CN103179943B - Hair maintenance compositions and correlation technique - Google Patents

Abstract

Hair maintenance compositions containing compound polyelectrolyte is disclosed herein.Also disclose their using method, their manufacture method, test the method for their effects, and relate to the medium method of hair nursing.

Description

Hair repair compositions and related methods

Cross References to Related Applications

This patent application claims priority to U.S. Provisional Patent Application 61/394,966, filed October 20, 2010, and International Application PCT/US10/53360, filed October 20, 2010, both of which are incorporated by reference in their entirety into this article.

Background of the invention

Hair care compositions are often formulated to have a variety of properties. For example, a conditioner can be formulated to condition the hair, and can also be formulated to repair the hair. Hair care compositions with a variety of properties are attractive to consumers because less composition needs to be applied to the hair to achieve the desired results. However, in order to formulate such hair care compositions, various components are often necessary. The long-term stability of such compositions may be compromised due to incompatibility between the numerous components.

Furthermore, due to the large number of components in many hair care compositions, formulators are faced with the challenge not only of finding the right components to provide the desired cosmetic properties, but also of manufacturing these complex compositions. Such challenges include developing production protocols to manufacture compositions, both for small-scale initial testing and for large-scale commercial markets. A greater number of components means that a greater number of manufacturing containers is required, which in itself means more time and expenditure required to produce the composition. Cosmetic compositions are thus complex mixtures of components and due to this complexity, careful consideration is required when developing production protocols.

Components of hair care compositions include conditioning agents, which are generally positively charged compounds. Hair fibers have a net negative charge. The positive charge of the conditioner is attracted to the overall negative charge of the hair fiber, making the positively charged conditioner substantive to the hair. This substantive property allows the conditioner to interact with the hair so that the conditioner provides its conditioning benefit. The conditioning action may include restoring the hair fiber after hair damage, eg repairing split ends.

Conditioners known in the art include quaternary ammonium nitrogen compounds known as "quats" and polymers comprising groups of such compounds known as "polyquaterniums". The polyquaternium includes polyquaternium-28, a vinylpyrrolidone/methacrylamidopropyltrimethylammonium chloride copolymer. It has been found that the combination of polyquaternium-28 and methyl vinyl ether/maleic acid copolymer (PVMMA) in specific ratios produces a polyelectrolyte complex (PEC) that repairs split-end damage (U.S. Patent Application Publication No. 2005/0089494 and 2006/0251603, both assigned to ISP Investments Inc.). However, in the complex environment of hair care formulations, the stability of PECs may be compromised by the presence of other components, especially charged compounds and polymers that can disrupt the structure of PECs. As such, the suitability of PECs may be limited by their compatibility with other ingredients desired to be included in hair care compositions. Because multiple properties are often desired in hair care compositions, it would be desirable to formulate hair care compositions that include stable combinations of PECs and other hair care ingredients that provide other desired properties.

Also, although PVMMA:Polyquaternium-28 PECs consist of only two constituent components, the method of making these PECs is described in the ISP Investment application as involving two or three separate containers. Such a method is cumbersome, not least due to the need for any additional containers to introduce the other components. Using two or three vessels to make one compound is inefficient and expensive in a large-scale production facility.

Additionally, when a consumer purchases a hair care product, the consumer does so based on the characteristics of the hair care product. For example, a consumer with frizzy hair might purchase a product for frizz-free hair, and a consumer with split-ends might purchase a product for repairing said split-ends. Accordingly, consumers may purchase hair care products with desired properties for a particular hair type or hair problem. In order for a consumer to compare hair care product compositions to make a decision about which to purchase, the beneficial properties of the composition should be clearly communicated to the consumer. One approach consists in using still photography, such as described in the ISP Investments application. However, other methods are needed.

Accordingly, it would be desirable to formulate stable hair care compositions comprising unaffected PEC together with other hair benefit agents, especially charged hair benefit agents. Furthermore, there is a need for more efficient methods for preparing PECs and hair care compositions comprising PECs. Furthermore, there is a need to develop test methods to show improved results in split end repair of hair care compositions so that the benefits of the hair care compositions can then be effectively communicated to consumers. There is also a need to develop other methods by which the benefits of hair care compositions can be demonstrated so that the benefits can then be effectively communicated to consumers. The present invention provides these advantages. Additional advantages of the invention, as well as additional inventive features, will become apparent from the description of the invention herein.

Summary of the invention

In one aspect, the present invention provides a hair care composition in the form of an emulsion comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, relative to a comparative composition comprising a plurality of such polyelectrolyte complexes, Has improved freeze-thaw stability.

In another aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, wherein the composition has a viscosity of greater than 3000 centipoise.

In another aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer; from about 1% to about 5% of a thickener; from about 10% or more propylene glycol; and about 5% or more of an emollient; wherein the percentages are based on the total weight of the composition.

In yet another aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer; from about 3% to about 5% of a thickener; and about 2% or Less emollient; where percentages are based on the total weight of the composition.

The present invention also provides methods of using the compositions described herein, including methods of conditioning hair fibers and methods of repairing split-ends of hair fibers.

In addition, the present invention provides a method for improving the freeze-thaw stability of a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer comprising adding about 1% to about 5% of Thickeners are added to the hair care composition, where percentages are based on the total weight of the composition.

Additionally, the present invention provides a method for improving the freeze-thaw stability of a hair care composition comprising a polyelectrolyte complex, the method comprising adding about 10% or more propylene glycol to the hair care composition , wherein the percentage is based on the total weight of the composition.

The present invention also provides methods of thermally protecting hair by applying a hair composition as described herein.

In addition, one aspect of the present invention provides a method for preparing a polyelectrolyte complex, the method comprising hydrating a methyl vinyl ether/maleic acid copolymer having a repeating unit of the following formula (Formula I) in a container

reacting the methyl vinyl ether/maleic acid copolymer in the vessel with a base in an amount sufficient to at least partially neutralize its acid groups to form an intermediate mixture; heating the intermediate mixture in the vessel; Add vinylpyrrolidone of the following formula (Formula II) to the intermediate mixture in the container

and methacrylamidopropyltrimethylammonium chloride of the following formula (formula III):

and mixing said polymer in said vessel under high shear and at a temperature of at least about 50-60° C. to prepare said polyelectrolyte complex.

The present invention also provides a method for preparing a polyelectrolyte complex, the method comprising hydrating a methyl vinyl ether/maleic acid copolymer having a repeating unit of formula I in a container; making the methyl vinyl ether/maleic acid copolymer The maleic acid copolymer is reacted in the vessel with, for example, a 20% solution of sodium hydroxide, wherein the sodium hydroxide is added in an amount sufficient to obtain a pH of, for example, about 6.5 to about 7.5, or about 6.9 to about 7.0, to forming an intermediate mixture; heating said intermediate mixture in said vessel to a temperature of about 50°C to about 60°C; mixing vinylpyrrolidone of formula II and methacrylamidopropyltrimethylammonium chloride of formula III to the intermediate mixture in the vessel; and mixing the polymer in the vessel at a temperature of at least about 50-60° C. for at least about 10 minutes to prepare The polyelectrolyte complex. In one embodiment, the method further comprises mixing the polyelectrolyte complex with one or more selected from aqueous carriers, surfactants, fragrances, conditioners, emollients, emulsifiers, thickeners , preservatives, gelling agents, silicones, hair fixatives, humectants and humectants are mixed to form a hair care composition. In one embodiment, the mixing is sufficient to allow sufficient incorporation of the one or more ingredients.

The present invention also provides a method for preparing a hair care composition comprising a polyelectrolyte complex, comprising the steps of: hydrating a methyl vinyl ether/maleic acid copolymer having a repeating unit of formula I in a container; The methyl vinyl ether/maleic acid copolymer is reacted in the vessel with an amount of base sufficient to at least partially neutralize its acid groups, for example 20% sodium hydroxide solution, for example wherein the sodium hydroxide is adding an amount sufficient to obtain a pH of, for example, from about 6.5 to about 7.5, or from about 6.9 to about 7.0, to form an intermediate mixture; heating the intermediate mixture in the vessel, for example, to a temperature of from about 50°C to about 60°C; A cationic copolymer of vinylpyrrolidone of formula II and methacrylamidopropyltrimethylammonium chloride of formula III is added to said intermediate mixture in said vessel; under high shear and at least about 50 Mix the polymers in the container at a temperature of -60°C to prepare the polyelectrolyte complex; one or more selected from aqueous carriers, surfactants, fragrances, conditioning agents, emollients, additional ingredients of emulsifiers, thickeners, preservatives, gelling agents, silicones, hair fixatives, humectants, and humectants are added to the polyelectrolyte complex in the container; and in the container The resulting composition is mixed. In one embodiment, the hair care composition prepared by the method is a shampoo, conditioner, leave-in treatment, cream, gel, mousse, serum, oil, gloss, or spray form.

The present invention also provides a process for the preparation of a hair care composition comprising the preparation of a methyl vinyl ether/maleic acid copolymer and a cationic copolymer of vinylpyrrolidone and methacrylamidopropyltrimethylammonium chloride A polyelectrolyte complex comprising the steps of: hydrating a methyl vinyl ether/maleic acid copolymer having a repeating unit of general formula I in a first container; making the methyl vinyl ether/maleic acid The copolymer is reacted in said first container with an amount of base, such as 20% sodium hydroxide, sufficient to at least partially neutralize its acidic groups, such as wherein the sodium hydroxide is sufficient to obtain, for example, about 6.5 to about 7.5, Alternatively, an amount at a pH of about 6.9 to about 7.0 is added to form an intermediate mixture; the intermediate mixture in the first vessel is heated, for example, to a temperature of about 50°C to about 60°C; the vinylpyrrolidone of formula II and A cationic copolymer of methacrylamidopropyltrimethylammonium chloride of formula III is added to said intermediate mixture in said first vessel; under high shear and at a temperature of at least about 50-60°C mixing the polymer in the first container to prepare the polyelectrolyte complex; in a second container, one or more selected from aqueous carriers, surfactants, fragrances, conditioning agents, emollients agent, emulsifier, thickener, preservative, gelling agent, silicone, hair fixative, humectant, and humectant; and mixing said second The polyelectrolyte complex of one container is mixed together with the mixing components of the second container. In one embodiment, the method produces a hair care composition in the form of a shampoo, conditioner, leave-in treatment, cream, gel, mousse, or spray.

In addition, the present invention provides a method of repairing split-ends of hair fibers by graphically reconstructing, said method comprising securing a hair fiber to a surface, wherein said hair fiber secured to said surface has a split-end or is located at said surface. said surface is damaged to produce a split-end; said surface is associated with a magnification device, wherein said split-end is placed in a field of view of said magnification device; an image capture device is associated with said magnification device linked so as to capture a magnified image of the field of view of the magnifying device; treating the split-end with a composition, wherein the composition repairs the split-end, and wherein the split-end fuses together; and An image of the repair of the split-end during processing of the composition is captured by the image capture device associated with the magnification device, and a representative image of the captured repair image is stored for subsequent retrieval. In one embodiment, the composition comprises, for example, from about 1% to about 5% of a thickener, about 10% or more of propylene glycol, and about 5% or more of an emollient, wherein the percentages are based on by total weight of the composition. In another embodiment, the composition comprises from about 3% to about 5% of a thickening agent, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition. In another embodiment, the degree of split-end hair fiber repair is communicated to the consumer.

The present invention also provides a method for quantitatively assessing the degree of repair of split-end hair fibers, said method comprising obtaining a bundle of hair, wherein said hair is twice bleached hair; combing and drying the bundle of hair so that at least one producing at least one split-end in the fiber; removing at least one hair fiber having a split-end from the bundle; optionally marking the at least one hair fiber; capturing the split-end of the at least one hair fiber a first image, and storing a representative image of said image, such as an electronic representative image; associating said hair fiber with a bundle from which said hair fiber was removed; treating said bundle and said hair fiber with a composition; removing said hair fiber from the processed bundle; capturing a second image of said hair fiber end removed from the processed bundle; assigning a value of 0 for said hair fiber as split-end not repaired, 1/2 for partial repair, or 1 for complete repair, to assess the degree of repair of the split-end of the hair fiber; and if multiple hair fibers are evaluated, optionally an average value is determined for the hair fibers evaluated. In one embodiment, the composition comprises, for example, from about 1% to about 5% of a thickening agent, about 10% or more of propylene glycol, and about 5% or more of an emollient, wherein the percentages are based on by total weight of the composition. In another embodiment, the composition comprises from about 3% to about 5% of a thickening agent, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition. In another embodiment, the degree of hair fiber repair at the split-end is communicated to the consumer.

One embodiment of the present invention provides a method of quantitatively assessing the degree of repair of split-end hair fibers, the method comprising obtaining a bundle of hair; producing at least one hair fiber in the bundle to have a split-end; removing at least one hair fiber having a split-end; optionally marking the at least one hair fiber; capturing a first image of the split-end of the at least one hair fiber, and storing a representative image of the image , such as an electronically representative image; associating said hair fiber with a strand from which said hair fiber was removed; treating said strand and said hair fiber with a composition, wherein said composition comprises a hair care composition, It comprises a polyelectrolyte complex of a cationic polymer and an anionic polymer, from about 1% to about 5% of a thickener, about 10% or more of propylene glycol, and about 5% or more of an emollient, The percentages therein are based on the total weight of the composition; the hair fibers are removed from the treated bundle; a second image is captured of the ends of the hair fibers removed from the treated bundle; a value of 0 is set for the hair fibers Designated as split-end unrepaired, 1/2 as partially repaired, or 1 as fully repaired to assess the degree of repair of the split-end of the hair fiber in question; and if multiple hair fibers are evaluated, then The fibers optionally determine the average value.

Another embodiment of the present invention provides a method of quantitatively assessing the extent of split-end hair fiber repair, the method comprising obtaining a bundle of hair; manufacturing at least one hair fiber of the bundle to have a split-end; bundle removing at least one hair fiber having a split-end; optionally marking the at least one hair fiber; capturing a first image of the split-end of the at least one hair fiber, and storing a representative image of the image , such as an electronically representative image; associating said hair fiber with a bundle from which said hair fiber was removed; treating said bundle and said hair fiber with a composition, wherein said composition comprises a hair care composition, It comprises a polyelectrolyte complex of a cationic polymer and an anionic polymer, from about 3% to about 5% of a thickener, and about 2% or less of an emollient, the percentages of which are based on the total weight of the composition ; remove the hair fiber from the processed bundle; capture a second image of the hair fiber end removed from the processed bundle; assign a value of 0 to the hair fiber as split-end unrepaired, 1/ 2 for partial repair, or 1 for complete repair, to assess the degree of repair of the split-end of the hair fiber; and if multiple hair fibers are evaluated, optionally an average of the hair fibers evaluated is determined.

Another embodiment of the present invention provides a method of quantitatively assessing the degree of repair of a split-ended hair fiber, the method comprising obtaining a bundle of hair; manufacturing at least one hair fiber of the bundle to have a split-end; The bundle removes at least one hair fiber having a split-end; optionally marking the at least one hair fiber; capturing a first image of the split-end of the at least one hair fiber, and storing a representative image of the image , such as an electronically representative image; associating said hair fiber with a strand from which said hair fiber was removed; treating said strand and said hair fiber with a composition, wherein said composition comprises a hair care composition, It comprises a polyelectrolyte complex of a cationic polymer and an anionic polymer, wherein the viscosity of the composition is greater than 3000 centipoise; removes the hair fiber from the treated strand; captures the hair fiber from the treated strand Second image of the removed hair fiber end; assign a value of 0 for split-end unrepaired, 1/2 for partial repair, or 1 for complete repair for the hair fiber to evaluate the split-end of the hair fiber and if multiple hair fibers are evaluated, optionally determine an average of the hair fibers evaluated.

Another embodiment of the present invention provides a method of quantitatively assessing the degree of repair of a split-ended hair fiber, the method comprising obtaining a bundle of hair; manufacturing at least one hair fiber in the bundle to have a split-end; The bundle removes at least one hair fiber having a split-end; optionally marking the at least one hair fiber; capturing a first image of the split-end of the at least one hair fiber, and storing the image a representative image, such as an electronic representative image; associating the hair fiber with the bundle from which the hair fiber was removed; treating the bundle and the hair fiber with a composition, wherein the composition comprises an emulsion form A hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, the hair care composition having improved freeze-thaw stability relative to a comparative composition comprising a plurality of such polyelectrolyte complexes ; remove the hair fiber from the processed bundle; capture a second image of the hair fiber end removed from the processed bundle; assign a value of 0 to the hair fiber as split-end unrepaired, 1/ 2 for partial repair, or 1 for complete repair, to assess the degree of repair of the split-ends of the hair fibers; and if multiple hair fibers are evaluated, optionally determine an average of the hair fibers evaluated.

Description of drawings

Figure 1 is a bar graph showing the percent repair determined with a rinse-off conditioner over three cycles using the method of the present invention. Values in parentheses are percent polyelectrolyte complex (PEC). The number of fibers tested was 20, 100 and/or 50 for different compositions.

Figure 2 is a bar graph showing the percent repair determined using the method of the present invention with a leave-on composition in one treatment. Twenty fibers were tested for each composition.

Figure 3 is a diagram showing the use of polyelectrolyte complexes (PECs) to repair split-ends. The figure shows a possible mechanism of split-end repair by PEC: the PEC attaches to the site of the split-end, forms a network with itself, the fibers assemble and shrink as they dry, thereby bonding the split-end from the inside.

Figures 4A-4D also show images of repairs of various split-end types.

Figure 5 also shows a still image taken from a repair video of a split-end during the repair process.

Fig. 6 is a schematic diagram of an image data acquisition system according to an embodiment of the present invention.

Figure 7 shows a line graph comparing the high humidity curl retention of exemplary compositions of the present invention.

Figure 8 shows thermal protection of hair using exemplary compositions of the present invention.

Figures 9-19 show freeze/thaw comparisons of the compositions described herein.

Figure 20 shows a split-end repaired by an exemplary composition of the invention.

Detailed description of the invention

The present invention is based on the surprising and unexpected discovery of stable compositions comprising a polyelectrolyte complex (PEC) and other hair benefit agents, especially charged species, wherein the PEC remains intact and exhibits hair restoration efficacy . The unexpected discovery that PECs can be combined with other charged hair benefit agents—that is, substances that have beneficial properties for or impart beneficial properties to hair, such as cationic conditioning agents—without disrupting the defined PEC structure compound. As a result of this unexpected discovery, the present invention provides compositions that not only provide the hair restoration benefits of PECs, but also provide the benefits of other hair benefit agents. Thus, the present invention provides compositions and methods comprising, for example, charged hair benefit agents such as quaternary ammonium salts, cationic conditioning polymers, and the like. Suitable hair benefit agents which may be combined with the PEC according to the invention include, for example, stearamidopropyldimethylamine, cocamidopropyl betaine, polyquaternium-37, polyquaternium-7, Polyquaternium-39, DC5-7113 (Siliconequat-16 and Undeceth-11 and Butyl Octanol and Undeceth-5), TQuat60 (polysiloxane quaternary ammonium salt-22), quaternary ammonium salt-80, 2001 (Polyquaternium-47), and Acrylic/VP Crosspolymer. Other suitable charged hair benefit agents are described herein.

The present invention also provides a single vessel process for the preparation of PEC. The method of the present invention also allows the preparation of PECs having the same particle size distribution as PECs prepared by conventional methods requiring the use of two or more separate vessels. Thus, the present invention provides a more efficient and cost-effective process for the preparation of PECs and hair care compositions comprising PECs.

The present invention also allows concentrations of PEC greater than 4% by weight, for example 8% by weight.

Additionally, the present invention has the advantage of providing a means by which the benefits of a hair care composition can be graphically illustrated so that the benefits can then be effectively communicated to consumers. Consumers purchase hair care products based on their properties. As such, it is important to effectively communicate the beneficial properties of hair care product compositions to these consumers so that consumers can make informed purchasing decisions when comparing competing hair care products.

The present invention still further has the advantage of providing a test method which allows showing improved results of split end repair of the hair care composition so that the benefits of the hair care composition can then be effectively communicated to the consumer. Most split-end repair testing methods use virgin hair whose ends have been mechanically induced to split. The use of virgin hair allows the ingredients of the split end repair composition to act only on mechanically induced damage. In other words, in virgin hair, there is no other damage other than the split ends. Thus, the repair composition directs its repair ability to act only on split-end damage. In this way, the repairing ingredients of the composition will not be wasted on other parts of the hair. However, it has surprisingly been found that hair with other damage (eg due to bleaching) can be used in place of the original hair in the split end repair test method. This is counter-intuitive, as it would be expected that any repair composition would have its repair components adsorb to other damage to the hair, not just the split ends, thereby reducing the amount of split-end repair. Applicants have found that the more damaged the hair, the better the repair of split ends. Furthermore, it has been found that with more severely damaged hair, high repair percentages can be achieved in rinse-off products, for example higher than 50%, which is the level achievable in leave-on products. In one aspect, the present invention provides a hair care composition in the form of an emulsion comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, which hair care composition is compared to a comparative composition (such as disclosed in U.S. Patent Application The PECs described in 2005/0089494 and 2006/0251603 formulated in conventional hair care base formulations) have improved freeze-thaw stability. In an embodiment, the composition comprises, for example, from about 1% to about 5% of a thickener, about 10% or more of propylene glycol, and about 5% or more of an emollient, wherein the percentages are based on the composition of total weight. In another embodiment, the composition comprises from about 3% to about 5% of a thickening agent, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition.

The compositions of the present invention provide unexpected freeze-thaw stability. Freeze-thaw stability is an important characteristic of hair care compositions, especially for transport and storage purposes which often expose the compositions to extremes of low temperature. Freeze-thaw stability is also important for outdoor products that remain on the hair and are thus exposed to extreme temperatures. Compositions containing PECs are not inherently unstable under freeze/thaw conditions. However, when combined with one or more fatty alcohols (cetyl, stearyl fatty alcohols, etc.) that have been used in the art to thicken conditioner compositions, for example at about 3 wt. % by weight), the formulation will be unstable during freeze/thaw. The composition will become grainy and chunky, which is unsatisfactory and likely to be rejected by the consumer.

In addition to freeze/thaw instability, conventional compositions with PEC containing about 5% fatty alcohol do not have long term high temperature stability. The viscosity of such compositions continues to increase over time (e.g., over 100,000 centipoise after 2-3 months at 45° C.), which is unsatisfactory to consumers because it is too thick and hard Cannot be spread throughout the hair and may be repelled by consumers. The inventors have found The addition of <RTI ID=0.0>(R)</RTI> improves viscosity control; that is, controlling viscosity to maintain, for example, about 20,000-40,000 centipoise.

The compositions and methods of the invention may include thickeners. Thickeners increase the viscosity of a composition such that compositions with greater amounts of a given thickener have higher viscosities. The thickener may be, for example, a quaternary ammonium nitrogen compound or a polymer, such as polyquaternium-37, and for example wherein polyquaternium-37 is combined with propylene glycol dicaprylate/dicaprate and polypropylene glycol-1 Trideceth-6 (polypropyleneglycol-1trideceth-6) mixture. from /BASF, Basel, Switzerland SC96 is an example of such a mixture. SC96 is 65% Polyquaternium-37, 25% Propylene Glycol Dicaprylate/Dicaprate, 10% PPG-1 Trideceth-6. Other suitable thickeners may also be added to the compositions of the present invention including, for example, xanthan gum, acrylic/VP crosspolymers (e.g. Ultrathix ^™ P-100; ISP, Wayne, NJ, USA), PVP, PVPK -90, PEG-90M and Styrene/VP Copolymer.

In another aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, wherein the composition has a viscosity of greater than 3000 centipoise. In embodiments, such compositions may include, for example, from about 1% to about 5% of a thickener, about 10% or more of propylene glycol, and about 5% or more of an emollient, wherein the percentages are based on the Total weight meter. In another embodiment, such compositions may include, for example, from about 3% to about 5% of a thickener, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition.

The viscosity of the compositions of the present invention varies based on the amount of thickener and/or other components added. The compositions of the present invention may comprise a thickener at a concentration of from about 1% to about 10% by weight. The thickener may be present in wt %, for example, as set forth in the table below. In the table, an "X" indicates a range "from [the corresponding value in the first row] to [the corresponding value in the first column]". For example, the first "X" is in the range of "from about 1% to about 2% by weight".

Table 1

Thus, the viscosity may have a range between any of the aforementioned endpoints.

The viscosity of the compositions of the present invention may range, for example, from about 3000 centipoise to about 100,000 centipoise, or, for example, from about 20,000 centipoise to about 40,000 centipoise by RVT-B at 10 rpm at 25°C for viscosities less than 50,000 centipoise Tested for 1 minute, or by RVT-C at 5 rpm for 1 minute at 25°C for viscosities greater than 50,000 centipoise and less than 100,000 centipoise. Viscosity ranges for compositions of the invention may be, for example, as set forth in the table below. In the table, an "X" indicates a range "from [the corresponding value in the first row] to [the corresponding value in the first column]". For example, the first "X" is the range "from about 3000 centipoise to about 10,000 centipoise".

Table 2

Thus, the viscosity may have a range bounded by any two of the above endpoints.

In one aspect of the invention, the composition comprises a thickener, propylene glycol and a relatively high concentration of an emollient, for example in an amount of 5% by weight or higher. Suitable emollients may include, for example, one or more fatty alcohols. Consumers may find hair care products containing 10% by weight or more of propylene glycol unacceptable, they may perceive such products as having a heavy and sticky feel, and may notice that hair takes too long to dry ( Due to the moisturizing properties of diols), hair may also be noticed to be difficult to comb or lack luster. Surprisingly, however, it has now been found that including 10% or more propylene glycol according to the present invention not only provides acceptable freeze-thaw stability, but may provide a composition that is more likely to be acceptable to consumers. Additionally, applicants have found that emulsions of such compositions can accept high levels of diols and not be affected (eg viscosity changes, etc.). Applicants have found that other polyols, such as 5% by weight sorbitol and glycerol, do not provide acceptable freeze-thaw stability.

In certain embodiments, the compositions and methods of the present invention can include propylene glycol, for example, at about 10% by weight or greater, about 20% by weight or greater, about 30% by weight or greater, about 40% by weight or more Large, or concentrations of about 50% by weight or greater.

The present invention also provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer; about 1% to about 5% of a thickener; about 10% or more propylene glycol; and about 5% % or more of an emollient; wherein the percentages are based on the total weight of the composition.

In another aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, and from about 3% to about 5% of a thickener, and about 2% or more Minor emollient, where percentages are based on the total weight of the composition. In this aspect, the compositions of the invention are preferably substantially free of propylene glycol. As used herein, "substantially free of propylene glycol" means that the compositions of the present invention contain less than about 1% by weight propylene glycol, less than about 0.5% by weight propylene glycol, less than about 0.1% by weight propylene glycol, and more preferably 0% by weight or no propylene glycol.

One or more emollients may be present in the compositions and methods of the present invention. Emollients can, for example, soften and/or soothe the skin. Suitable emollients may include, for example, fatty alcohols. Fatty alcohols include, for example, cetyl alcohol, stearyl alcohol, and combinations thereof. Fatty alcohols are sometimes used to thicken the composition as well as to provide emollient properties. Applicants have surprisingly found that compositions of the invention, for example 5% fatty alcohol/1% SC96 and 1% Fatty Alcohol/5% SC96, exhibited approximately the same emulsion properties (eg viscosity, rheology, yield value, appearance, color). This is unexpected when the concentration of cetyl alcohol drops to only about 1% by weight. Furthermore, it has now been found that in compositions having 2% by weight of PEG, the emollient concentration can be reduced to about 1% by weight where the composition also has from about 3% to about 5% by weight of a thickener or lower. The weight % range of fatty alcohols can be increased when the concentration of PEC is lower. Even at low concentrations of emollient fatty alcohols, the PEC compositions were found to provide an acceptable sensory experience. This is unexpected in most hair care compositions, especially conditioners, which have higher concentrations of emollient fatty alcohols to provide a sensory experience for the consumer. Also, in combination with the thickener, the PEC composition maintained an acceptable viscosity. Additionally, the combination of low concentrations of emollient fatty alcohol and PEC with about 3% to about 5% by weight thickener provides sufficient white opacity not observed with any of these components alone.

The concentration of emollient in the compositions of the present invention may desirably be adjusted based on the concentration of thickener. Emollient concentration ranges can be, for example, listed in the table below, eg for 3-5% by weight thickener. In the table, "X" means the range "from [corresponding value in first row] to [corresponding value in first column]". For example, the first "X" is in the range of "from about 0% to about 0.1% by weight".

Thus, the concentration of emollient may have a range bounded by any two of the aforementioned endpoints. Alternatively, the emollient concentration can be, for example, about 5% by weight or greater, about 6% by weight or greater, about 7% by weight or greater, about 8% by weight, such as for 1-5% by weight thickener % or greater, about 9% by weight or greater, about 10% by weight or greater, about 20% by weight or greater, about 30% by weight or greater, about 40% by weight or greater, or about 50% by weight or larger.

Certain PECs are described in US Patent Application Publications 2005/0089494 and 2006/0251603, both of which are incorporated herein by reference in their entirety. As outlined in these publications, the formation of PECs is not simply due to the presence of oppositely charged polymers in the composition. A phase diagram can be made to show the polymer-polymer species that exist when the concentration of oppositely charged polymers is changed (thereby changing the ratio of polymers to each other). Based on the phase diagram, the ratios of the polymers in terms of weight percent, moles, etc. to form the PEC can be determined. For PVMMA/polyquaternium-28 PEC, a 1:9 weight ratio of PVMMA:polyquaternium-28 is preferred. However, PEC may be present at other weight percent ratios. For example, PVMMA/Polyquaternium-28 PEC can be formed at about a 1:9 weight percent ratio such that ratios slightly above or below 1:9 will have some amount of PEC present. The weight percent ratio may range from about 1:8 to about 1:10 PVMMA:Polyquaternium-28. Thus, the actives of the cationic polymer and the anionic polymer used in the compositions of the invention and in the methods of the invention are in a weight ratio of from about 1:8 to about 1:10.

In addition to weight percent ratios, the formation of PECs can be determined based on the charge-to-charge ratio of the polymer. PECs are typically formed when the charge-to-charge ratio of the polymer is 1:1. Thus, PECs are likely to form when each negative charge of a polymer is balanced by the positive charge of another polymer. However, PECs can exist at other charge-to-charge ratios. For example, PECs can be formed at about a 1:1 charge-to-charge ratio such that ratios slightly above or below 1:1 will have at least some amount of PEC present, e.g., at a cationic to anionic charge ratio such as 0.82 to 1.8 Down. Phase diagrams can be made to determine the presence of PECs at different charge-to-charge ratios.

The PECs of the present invention can be formed from polymers that include cationic charges as well as polymers that include anionic charges. However, as long as the polymers interact via ionic bonds, phase diagrams can be constructed to determine the suitability of any polymer-polymer system to form a PEC. The compositions and methods of the present invention may include polyelectrolyte complexes wherein the cationic polymer comprises one or more monomeric units having one or more quaternary ammonium nitrogen groups, such as vinylpyrrolidone/methacrylamide groups Propyltrimethylammonium Chloride Copolymer (Polyquaternium-28). Non-limiting examples of other cationic polymers that can be used to form PECs include other polyquaternium polymers, such as polyquaternium-7, polyquaternium-10, or polyquaternium-11. The compositions and methods of the invention may include polyelectrolyte complexes wherein the anionic polymer comprises monomeric units having ionizable carboxylic acid groups, such as methyl vinyl ether/maleic acid copolymers. Another example of an anionic polymer that can be used to form a PEC is a vinylpyrrolidone/acrylate/lauryl methacrylate copolymer.

Polymers with ionizable groups, such as carboxylic acid groups or tertiary amine groups, may require pH adjustment to form polyelectrolyte complexes. Adjustment of pH changes the percentage of ionizable groups that are ionized, and thus adjusts the number of groups that can interact through ionic bonds. Phase diagrams prepared at different pH's can be used to determine the appropriate pH for PEC formation. For PVMMA/polyquaternium-28 PEC, a pH range of about 6.5 to about 7.5 can be used to form the PEC. Suitable pH ranges may, for example, be listed in the table below. In the table, an "X" indicates a range "from [the corresponding value in the first row] to [the corresponding value in the first column]". For example, the first "X" is the range "from about pH 6.5 to about pH 6.6".

Table 4

Thus, the pH can have a range bounded by any two of the aforementioned endpoints.

The pH of the composition can be adjusted using neutralizing/buffering agents. For acidic groups such as carboxylic acids, basic neutralizing agents such as hydroxide compounds may be used. Suitable hydroxide compounds include strong bases such as sodium hydroxide. For basic groups, acid neutralizers such as citric acid can be used. Any suitable neutralizing agent concentration can be used, including for example those listed in the table below. In the table, "X" means the range "from [corresponding value in first row] to [corresponding value in first column]". For example, the first "X" is the range "from about 0.1% to about 1% by weight".

table 5

Accordingly, the concentration of the neutralizing agent may have a range bounded by any two of the aforementioned endpoints. As long as the PEC is formed under the desired pH conditions, the final pH of any resulting composition comprising the PEC may be the same as or different from the pH at which the PEC was formed, as long as the PEC remains intact.

The PVMMA/Polyquaternium-28PEC has the ability to repair split ends of hair fibers. Hair has a net negative charge. Without being bound by any particular theory, the PEC is believed to be substantive to the hair fiber and binds the ends of the split-ends together through bonding properties. The positive charge of the polyquaternium-28 polymer is attracted to the negatively charged hair fibers and is substantive to the hair. Because the negatively charged PVMMA polymer is complexed to polyquaternium-28, PVMMA is also attracted to the hair. The ends of the split-ends are then adhered together by the interaction of multiple PECs with the ends of the split-ends and/or with each other (e.g. in film formation where the film shrinks upon drying) . Additionally, the surface tension experienced by the ends of the split ends due to the interaction of water during film formation helps to bond the ends together.

As long as the PEC is in the form of suspended or emulsified particles, the particle size of the PEC should allow access of the PEC to the ends of split ends so that the PEC can repair damaged hair fibers. The particle size distribution may have any suitable average PEC particle size so long as the PEC is able to access the ends of the split ends. Suitable average PEC particle sizes may include, for example, those listed in the table below. In the table, an "X" indicates a range "from [the corresponding value in the first row] to [the corresponding value in the first column]". For example, the first "X" is in the range of "from about 0.5 μm to about 1 μm".

Table 6

about 0.5μm about 1μm about 2μm about 3μm about 5μm about 10μm about 20μm about 30μm about 1μm x about 2μm x x about 3μm x x x about 5μm x x x x about 10μm x x x x x about 20μm x x x x x x about 30μm x x x x x x x about 40μm x x x x x x x x

Thus, the average PEC particle size distribution may have a range bounded by any two of the aforementioned endpoints. In certain embodiments, the compositions and methods of the invention comprise a PEC particle distribution having an average PEC particle size of about 5 microns, eg, about 5 ± 3 microns, or about 5 ± 2 microns. The compositions and methods of the invention may also include PEC particles present in microgels, eg, interlocked microgel structures.

The compositions and methods of the invention may contain PEC at concentrations higher than previously considered achievable in the art. For example, a composition of the invention may include PEC of PVMMA/Polyquaternium-28 at a concentration of 8% by weight. The concentration of PEC in hair care compositions can vary. The compositions and methods of the present invention may contain the polyelectrolyte complex at a concentration of from about 1% to about 8%, based on the total weight of the composition. The compositions of the present invention may contain the polyelectrolyte complex at a concentration of from about 1% to about 3%, or from about 2% to about 4%, based on the total weight of the composition. The concentration of PEC can be, for example, as listed in the table below. In the table, an "X" indicates a range "from [the corresponding value in the first row] to [the corresponding value in the first column]". For example, the first "X" is the range "from about 0.1% to about 0.5%".

Table 7

about 0.1% about 0.5% about 1% about 2% about 3% about 4% about 5% about 6% about 7% about 0.5% x about 1% x x about 2% x x x about 3% x x x x about 4% x x x x x about 5% x x x x x x about 6% x x x x x x x about 7% x x x x x x x x about 8% x x x x x x x x x

Accordingly, the concentration of PEC may have a range bounded by any two of the aforementioned endpoints.

Formation of PECs can be confirmed using any suitable method. Examples of suitable methods include microscopy methods. Under an optical microscope, the structure of the polymer-polymer system can be studied, and sizing software can be used to determine the size of any particles present. Such a method can yield the particle size distribution of the PEC, provided that the presence of other components does not obscure the PEC structure. Another method involves the use of a Malvern particle size analyzer to determine the particle size distribution. Furthermore, the physical properties of the composition of only the PEC in the carrier solvent may indicate the presence of the PEC. For example, as the presence of PEC increases, the turbidity and opacity of such compositions increases. Furthermore, for a given polymer-polymer system, the minimum value to which the viscosity of such a composition is reduced corresponds to the presence of the greatest amount of PEC, where the PEC is the densest.

The compositions of the present invention are in the form of, and the methods of the present invention may manufacture or use, compositions in the form of, for example, shampoos, conditioners, gels, rinses, emulsions (oil-in-water, water-in-oil or multiphase ), lotions, creams, ointments, ointments, pomades, sprays (pressurized or unpressurized), injections, mousses, foams, shampoos, solutions and solids (e.g. viscous, semi-solid wait). Accordingly, the compositions of the invention are in the form, and the methods of the invention may make or use, the composition in the form of, for example, a cream, lotion, solution, ointment or gel. Accordingly, the hair care compositions and methods of the present invention may include other components that may be suitable for these types of compositions. Preferably, such components are compatible with the PEC because the components do not disrupt the PEC structure.

Compositions may be suitable for rinse-off, leave-on and/or overnight treatments. The methods and hair care compositions of the present invention may comprise mixing the polyelectrolyte complex with one or more agents selected from the group consisting of aqueous carriers, surfactants, neutralizing agents, fragrances, conditioners, emulsifiers, thickeners, preservatives , gelling agent, silicone, hair fixative, humectant and humectant are mixed to form a hair care composition. Accordingly, the compositions and methods of the present invention may include, for example, preservatives, neutralizing agents, fragrances, silicones, or combinations thereof. Those skilled in the art will recognize that the components identified herein may have various properties and thus may be adapted to various component classes, especially if it is a commercially available product with multiple ingredients.

The aqueous carrier can include any suitable amount of water, such as from about 25% to about 97% by weight water (eg, from about 30% to about 95% by weight water). The compositions of the present invention may comprise from about 30% to about 97% by weight water, from about 50% to about 80% by weight water, or from about 60% to about 70% by weight water. The water used in the compositions of the present invention may be deionized water.

Suitable emulsifiers may include, for example, PPG-3 benzyl ether myristate (e.g. Crodamol STS; Croda, Inc., Edison, NJ, USA), arachidyl and behenyl alcohols and arachidyl glucosides (e.g. Montanov 202; SEPPIC, Paris, France), polyacrylamide and C13-14 isoparaffin and laureth-7 (e.g. Sepigel™ 305; SEPPIC), glyceryl stearate, isoceteth-20, oleyl alcohol Polyether-2, Methoxy PEG/PPG-7/3 Aminopropyl Dimethicone, PEG/PPG-18/18 Dimethicone (eg DC-190; DowCorning), PEG -12 Dimethicone, PEG-40 Hydrogenated Castor Oil, PEG-6 Caprylic/Capric Triglyceride, Aminomethylpropanol (AMP-95), and Polyglyceryl-3 Distearate.

Suitable surfactants may be used, such as cleansing and/or detersive surfactants, including, for example, disodium laureth sulfosuccinate, sodium laureth sulfate, polysorbate 20, polysorbate 60, Cocamidopropyl Betaine and Stearalkonium Chloride. Such surfactants may be present in shampoo compositions. Conditioners are preferably substantially free of cleansing surfactants, unless the conditioner is a two-in-one combination of shampoo and conditioner. As used herein, "substantially free of cleansing surfactants" means that the compositions of the present invention contain less than about 2% by weight of cleansing surfactants, and more preferably less than about 1% by weight, such as 0% by weight or no Contains cleansing surfactants.

Suitable conditioning agents may include, for example, tertiary or quaternary amines such as stearamidopropyldimethylamine, polyquaternium-47 (such as Merquat 2001; Nalco, Naperville, IL, USA), Silicone Quat-22 (eg TQuat60; Evonik, Essen, Germany), cocamidopropyl betaine, polyquaternium-11, polyquaternium-39, polyquaternium-4 ( H-100; AkzoNobel, Amsterdam, Netherlands), polyquaternium-4 ( L-200; AkzoNobel) to 0.5% by weight, Polyquaternium-7, Polyquaternium-10 and Quaternium-80. Other suitable conditioners include, for example, AquD4272N-HanceSP100 (acrylamidopropyltrimonium chloride/acrylamide copolymer), distearylethyldimethylammonium chloride; cetearyl alcohol (Varisoft EQ65), RhodiaGuarS, Behentrimonium Chloride and Behentimonium Chloride/Cetearyl Alcohol. N-Hance SP100 copolymer has been found to be especially advantageous. Thus, the compositions and methods of the present invention may include, for example, acrylamidopropyltrimethylammonium chloride/acrylamide copolymer. As shown in Example 16 below, this copolymer provides additional split-end repair in PEC-containing compositions.

Although not required, an effective amount of at least one preservative can be incorporated into the composition. For example, a preservative can be selected to kill bacteria that might otherwise live or proliferate in the composition. Suitable preservatives may include, for example, DMDM hydantoin, disodium EDTA, Kathon ^™ CG (active ingredients: 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4 -isothiazolin-3-one), etc., and combinations thereof.

Suitable gelling agents may be used. Suitable gelling agents may include, for example, acrylic acid/VP crosslinked copolymers (eg Ultrathix ^™ P-100; ISP).

Suitable silicones may be added, for example, to improve hair conditioning. Suitable silicones may include, for example, polysiloxanes including dimethicone, dimethiconol, cyclopentasiloxane, and cyclohexasiloxane. These include for example phenyl trimethicone, OSW5 (84% Cyclopentasiloxane, 15% Dimethiconol, 1% Dimethicone; Evonik, Essen, Germany), DC-200 (Dimethicone; DowCorning, Midland, MI, USA), FluidBlend (80% Cyclomethicone, 20% Dimethicone), and DC-1501 (D5/Dimethicone; DowCorning) . Other suitable silicones include, for example, DC-556 (phenyl trimethicone; Dow Corning), and amino-functional silicones, such as DC-949 (31% amodimethylsiloxane, 1.9% Trideceth-12, 2.2% Cetyltrimethylammonium Chloride, 55-60% Water, 2.2% Cyclotetramethicone, 1.6% Cyclopentasiloxane, and <0.5% Sodium Benzoate; DowCorning), DC-8500 (82% Bis(C13-15 Alkoxy)PG-Amodimethicone, 18% C14-15 Alcohol; DowCorning), Aminopropyl Dimethicone, DC5-7113 Silicone Quat Microemulsion (66% Water, 25% Silicone Quat-16, 7.4% Undeceth-11, 4.5% Butyloctyl Alcohol, 3.5% Undeceth-5; Dow Corning), DC2-8566 (Amodimethicone; Dow Corning), and Amodimethicone (ADM1100; Wacker).

Suitable hair fixatives may be used. Suitable examples include, for example, VP/aminomethacrylic acid/vinylimidazole copolymers (e.g. Clear; BASF), acrylic acid/vinylpyrrolidone crosspolymer (e.g. Ultrathix TMP-100; ISP), vinylcaprolactam/VP/dimethylaminoethyl methacrylate copolymer ( S; ISP), and VP/VA copolymer.

Additional ingredients may be added including, for example, coconut palm (coconut) oil, mineral oil (liquid paraffin), sodium chloride, hydrolyzed silk protein, keratin amino acids, ascorbic acid, panthenol, tocopheryl acetate, biotin, tobacco Amides, Triethanolamine, Wheat Germ (Wheat) Flour Lipid, Ceramide 3, Avocado Oil, Tetrahexyldecyl Ascorbate, Soy Sterol, Alpha-Glucan Oligosaccharides, Ethylhexyl Methoxycinnamate , butylmethoxydibenzoylmethane, and tocopheryl acetate. Propellants may be used, for example in spray compositions including isobutane and propane and 152A (78.5% A46; 28.5% HFC152A). Fatty acids such as myristic acid, palmitic acid and stearic acid can be used.

Additional components and/or ingredients may be provided to impart beneficial properties to the hair, for example for imparting softness to the hair after drying, providing moisture to the hair, providing a pleasing uniformity/viscosity of the composition, and providing volume to the hair Components and/or ingredients for fullness.

Fragrances may be provided in the compositions of the present invention. A non-limiting example of a fragrance is flower extract. Any particular fragrance may be used, and those skilled in the art will recognize that a particular consistent fragrance is not critical. In fact, it is possible to provide compositions of the invention without fragrance.

Embodiments of the compositions of the present invention may include, for example, 1-2% by weight of PVMMA copolymer and PEC of polyquaternium-28 in a 1:9 ratio. Such a compound may be prepared in a side vessel and added to the main batch vessel after the milk phase is prepared and when said milk phase is cooled to 45-65°C. About 1-2% by weight of a tertiary or quaternary amine may be included in the emulsion phase and neutralized to a pH of about 4.0-6.0. Fatty alcohols (such as cetyl alcohol and/or stearyl alcohol) and low HLB co-emulsifiers, such as glycerol monostearate, distearate, etc., may be included in a ratio of about 3-7% by weight, And can be included in the emulsion phase. Silicones or mixtures of dimethicone, cyclomethicone, phenyl and/or amino functional silicones may be included, for example, from 0.1 to 10% by weight. Emollient esters such as PPG-3 benzyl ether myristate (eg Crodamol STS) may be added at eg 1-4% by weight to enhance product spreadability as well as enhance shine and hair feel. 10% propylene glycol may be included to improve freeze/thaw stability. can also include SC-96, which can be added after the emulsion phase and when the batch is cooled to 45-65°C, for example, at 0.1-5% by weight to increase viscosity, improve conditioning feel in hair, and improve long-term stability and viscosity control. Another embodiment of the composition of the present invention may comprise, for example, the same composition, except with about 1% fatty alcohol, without the emollient ester, and SC-96 is, for example, 1-7% by weight. An embodiment of a composition having about 3-7% by weight of fatty alcohol may include a PEC compound that has first been prepared in a main container, and then the remainder of the composition is prepared in the same container, wherein SC-96 has been increased to, for example, 1-7% by weight. An embodiment of a composition having about 1% by weight of fatty alcohol may include a PEC compound that has first been prepared in a main container, and then the remainder of the composition is prepared in the same container, wherein SC-96 is increased to, for example, 3-10% by weight.

The present invention includes hair care compositions formed from any suitable components described herein. In an embodiment, the present invention comprises polyquaternium-28 and methyl vinyl ether/maleic acid copolymer; about 1% to about 5% thickener; about 10% or more propylene glycol; and A hair care composition comprising about 5% or more of an emollient, where the percentages are based on the total weight of the composition. In an embodiment, the present invention comprises polyquaternium-28 and methyl vinyl ether/maleic acid copolymer; from about 3% to about 5% of a thickener; and about 2% or less of an emollient The hair care composition formed by the agent, wherein the percentage is based on the total weight of the composition. In an embodiment, the present invention includes a hair care composition formed from polyquaternium-28 and methyl vinyl ether/maleic acid copolymer, wherein the viscosity of the composition is greater than 3000 centipoise. In an embodiment, the present invention includes a hair care composition in the form of an emulsion formed from polyquaternium-28 and methyl vinyl ether/maleic acid copolymer, relative to a comparative polyelectrolyte complex containing a plurality of such polyelectrolyte complexes. Compositions having improved freeze-thaw stability. In an embodiment, the present invention includes a hair care composition formed from polyquaternium-28, methyl vinyl ether/maleic acid copolymer, and polyvinylpyrrolidone.

The present invention also provides embodiments of hair care formulations and methods of their use that do not increase the force required to comb the hair; do not increase detachment compared to untreated hair The force required for the adhesion of two hair fibers; compared with untreated hair, does not increase the "three-point bending" force; compared with untreated hair, does not increase Young's modulus; compared with untreated hair Does not reduce hair shine/shine compared to natural hair; or impart other quantifiable "negative" attributes.

The compositions of the present invention may be used in any suitable method of treating hair. For example, the compositions described herein can be used to condition hair fibers by applying the composition to the hair fibers and rinsing the hair fibers with water. After rinsing, the hair fibers can be dried using a blow dryer, combed and/or styled using a styling product or composition. Additionally, the compositions described herein can be used to repair split ends of hair fibers by applying the composition to the split ends and rinsing the split ends with water. This method can also be followed by blow drying, brushing and/or styling. The compositions described herein are also useful in a method of strengthening hair fibers by applying a composition of the invention to the hair fibers and rinsing the hair with water. In other embodiments, the compositions of the present invention may be used for hair styling, for example when the composition includes a hair styling benefit agent. For example, the composition may be a setting spray (aerosol and non-aerosol). In other embodiments, the compositions of the present invention, when formulated as a shampoo, can be used to shampoo the hair. Other styling products may include leave-in conditioners, overnight conditioning treatments, styling lotions/balms/balms, styling gels, styling mousses, serums, hair oils, glosses and conditioning sprays (aerosol and non-aerosol).

Freeze-thaw stability of hair care compositions comprising polyelectrolyte complexes of cationic and anionic polymers can be improved by adding from about 1% to about 5% of a thickener to the hair care composition, wherein Percentages are based on the total weight of the composition. Thickeners may contain quaternary ammonium nitrogen compounds or polymers. The quaternary ammonium nitrogen compound or polymer can be, for example, polyquaternium-37. Polyquaternium-37 can be in a blend with propylene glycol dicaprylate/dicaprate and polypropylene glycol-1 trideceth-6. Alternatively, the freeze-thaw stability of a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer can be improved by adding about 10% or more propylene glycol to the hair care composition, wherein the percentage Based on the total weight of the composition.

The present invention provides thermal protection of the hair. When a leave-on composition having a PEC described herein is applied to hair, the PEC protects the hair shaft from heat-induced damage (eg, fiber breakage). The heat can be from any source including, for example, a hair dryer, a flatiron, or a heat styling tool.

The method of the present invention allows the preparation of PEC in one vessel. Therefore, one aspect of the present invention provides a method for preparing a polyelectrolyte complex, the method comprising hydrating a methyl vinyl ether/maleic acid copolymer having a repeating unit of the following formula (Formula I) in a container

reacting the methyl vinyl ether/maleic acid copolymer in the vessel with a base (such as sodium hydroxide) in an amount sufficient to at least partially neutralize its acidic groups to form an intermediate mixture; heating the The intermediate mixture; the vinylpyrrolidone of the following formula (formula II)

and methacrylamidopropyltrimethylammonium chloride of the following formula (formula III):

The cationic copolymer of is added to the intermediate mixture in the container; and the polyelectrolyte composite is prepared by mixing the various polymers in the container under high shear force and a temperature of at least about 50-60°C.

Additionally, another aspect of the present invention allows for the preparation of hair care compositions by combining the PEC prepared according to the present invention with other hair benefit agents. According to the method of the present invention, such hair care compositions may be prepared by combining the PEC prepared according to the present invention with other hair benefit agents in a single container. Accordingly, the present invention also provides a process for the preparation of a hair care composition comprising the manufacture of a polyelectrolyte complex, comprising the step of hydrating a methyl vinyl ether/maleic acid copolymer having repeating units of formula I in a container reacting the methyl vinyl ether/maleic acid copolymer in a container with an amount of base, such as sodium hydroxide (for example 20% aqueous sodium hydroxide solution) sufficient to at least partially neutralize its acidic groups (for example by Add sufficient base to obtain a pH of about 6.5 to about 7.5, or about 6.9 to about 7.0), to form an intermediate mixture, heat the intermediate mixture in the vessel, for example, to a temperature of about 50°C to about 60°C; formula II A cationic copolymer of vinylpyrrolidone and methacrylamidopropyltrimethylammonium chloride of formula III is added to the intermediate mixture in the vessel; and under high shear and for example about 50-60°C Polyelectrolyte complexes are prepared by mixing the various polymers in the vessel at temperature. The method of the present invention optionally comprises further adding one or more agents selected from the group consisting of aqueous carriers, surfactants, fragrances, conditioners, emollients, emulsifiers, thickeners, preservatives, gelling agents, silicone Additional ingredients of alkanes, hair fixatives, humectants, and humectants are added to the polyelectrolyte complex in the container; and the resulting composition is mixed in the container.

The present invention also allows the hair care composition to be prepared in two containers, the PEC being prepared in one container and the remaining ingredients of the composition being prepared in a second container, wherein the PEC and other components are then combined. In this aspect, the present invention also provides a process for the preparation of a hair care composition comprising methyl vinyl ether/maleic acid copolymer and vinylpyrrolidone with methacrylamidopropyltrimethylammonium chloride The cationic copolymer of the polyelectrolyte complex is prepared, and it comprises the steps: the methyl vinyl ether/maleic acid copolymer hydration with the repeating unit of formula I in the first container; Methyl vinyl ether/maleic acid copolymer The maleic acid copolymer is reacted in a first vessel with a base, such as sodium hydroxide, in an amount sufficient to at least partially neutralize its acidic groups to form an intermediate mixture; the intermediate mixture in the first vessel is heated; the ethylene of formula II 1-pyrrolidone and cationic copolymer of methacrylamidopropyltrimethylammonium chloride of formula III is added to the intermediate mixture in the first vessel; mixed under high shear and at a temperature of at least about 50-60°C polymer in the first container to prepare the polyelectrolyte complex; in a second container mix one or more selected from aqueous carriers, surfactants, fragrances, conditioners, emollients, emulsifiers, thickeners , preservatives, gelling agents, silicones, hair fixatives, humectants, and humectants; and mixing the polyelectrolyte complex of the first container with the composition of the second container in the first or second container Mix together.

As described above, phase diagrams can be generated to determine the conditions for PEC formation, including polymer:polymer weight ratios as well as charge-to-charge ratios. Additional conditions may also be varied, including temperature, solvent system, and the like. Each of these conditions can be varied to determine their effect on PEC formation. Therefore, the preparation of PECs can be complex and difficult due to the different conditions required for the preparation of PECs and the large number of variables involved. Especially where a specific particle size is desired, as in the preparation of PVMMA/Polyquaternium-28PEC that can repair split-end damaged hair. In addition to polymer:polymer weight ratios and/or charge-to-charge ratios, etc., the specific preparation method used can also affect the average particle size distribution of the PEC. For example, mixing speed and/or mixing time during addition of one polymer to another, as well as mixing speed and/or mixing time after such addition, can affect the PEC particle size distribution. Other process variables such as temperature, pH, and the presence of other charged compounds may also have an impact during PEC formation. The composition of the present invention can be prepared by a method that allows large-scale production of PECs in which the correct particle size distribution for repairing split-ends can be obtained.

The formation of PECs can be promoted by applying heat at specific stages, for example when neutralizing the anionic polymer with a base and/or when adding a cationic polymer to an anionic polymer to prepare a complex. The composition may be preheated prior to combining the polymers, may be heated with one or a subset of the polymers, or may be heated during or after combining all of the polymers for PEC formation. For PVMMA/polyquaternium-28 PEC, it has now been found that it is advantageous to heat the neutralized PVMMA prior to adding the polyquaternium-28, for example at a temperature of at least 50°C to 60°C or greater. Such temperature ranges are listed, for example, in the table below. In the table, an "X" indicates a range "from [the corresponding value in the first row] to [the corresponding value in the first column]". For example, the first "X" is the range "from about 50°C to about 51°C".

Table 8

Accordingly, the temperature may have a range bounded by any two of the aforementioned endpoints.

The compositions of the present invention may be prepared in a single container or may be prepared in separate containers, eg the PEC is prepared separately from the other ingredients and then the PEC is combined with the other ingredients. The methods described herein produce PECs with the same size, morphology and stability as conventional methods, but in doing so can reduce the number of containers.

The step of adding the cationic polymer to the intermediate mixture may comprise adding a solution, such as an aqueous solution, of the cationic polymer to the intermediate mixture. The cationic polymer can be added to the intermediate mixture at any suitable rate, which can include, for example, about 0.3 kg/minute per minute to about 1.0 kg/minute per minute (e.g., if the addition period is 10 minutes, The rate would then be about 3 kg/minute to about 10 kg/minute), and may include, for example, those listed in the table below. In the table, an "X" indicates a range "from [the corresponding value in the first row] to [the corresponding value in the first column]". For example, the first "X" is in the range of "from about 0.3 kg/minute per minute to about 0.4 kg/minute per minute".

Table 9

Thus, an addition can have a range bounded by any two of the aforementioned endpoints.

When one polymer is added to another, the formation of PEC depends on the mixing speed and mixing duration. High shear forces can be used to accomplish mixing. However, for proper PEC formation, the mixing speed may have to be adjusted depending on the polymer-polymer system. For PVMMA/Polyquaternium-28 PEC, Polyquaternium-28 can be mixed first eg 5 minutes, 10 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes or 60 minutes before adding PVMMA. Polyquaternium-28 can be added to the PVMMA over a period of, for example, 5 minutes, 10 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes, or 60 minutes. Polyquaternium-28 can be added to the PVMMA over a period of 30 minutes. The rate of addition can be any suitable rate at which PEC is formed. The rate can be determined based on the time required for addition. For example, the rate may be based on the amount added per minute in the added period per minute. For PVMMA/Polyquaternium-28 PEC this may be about 0.4 kg/min to 1.0 kg/min. Thus, if the addition period is 10 minutes, the rate will be about 4 kg/minute to about 10 kg/minute. Mixing may continue for a period of time such as 5 minutes, 10 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes or 60 minutes after adding the polymer. Mixing can include combinations of mixing before, during, and/or after adding the polyquaternium-28. Thus, the intermediate mixture of PVMMA can be mixed for at least about 10 minutes before adding the cationic polymer, for at least about 10 minutes after adding the cationic polymer, or a combination thereof.

Certain embodiments of the compositions of the present invention include compositions having formulations of PVMMA and Polyquaternium-28 as in Table 10.

Table 10

PEC active ingredient wt% 1% 2% 4% 6% 8% water 7.775 15.55 31.1 46.65 62.2 PVM/MA copolymer 0.1 0.2 0.4 0.6 0.8 Sodium Hydroxide, Water (20% active ingredients) 0.125 0.25 0.5 0.75 1 Polyquaternium-28, Water (20% active ingredients) 4.5 9 18 27 36 *remaining ingredients of the composition* 87.5 75 50 25 0 Total 100 100 100 100 100

The present invention provides mixing with additional ingredients after formation of the PEC, wherein the mixing is sufficient to allow sufficient incorporation of one or more ingredients.

The present invention provides a single-vessel process for the preparation of PECs that is highly efficient, low-cost, and eliminates the additional process of transferring material from one vessel to another as is done in conventional PEC production methods. time and labor. Accordingly, the process of the present invention is particularly useful for preparing PEC and hair care compositions containing PEC on a commercial scale, eg, from about 500 to about 10,000 gallons.

The method of the present invention further provides for the preparation of PEC compositions at concentrations significantly exceeding those of conventionally prepared PEC compositions (for example, 8% by weight). There are several advantages to increasing the concentration when preparing PEC. Higher concentrations allow the use of smaller premix containers and the combination of PEC with other ingredients to make hair care compositions such as conditioners. Also, PEC can be prepared and stored for future use, and for more concentrated feedstock, less storage space is required. In addition, fewer quality control steps are required because one batch of PEC can be prepared and tested at a higher concentration, rather than multiple batches prepared at a lower concentration, which would require additional testing. Additionally, if the PEC raw material is used to make a hair care composition, the PEC raw material will not require as much volume in the processing vessel, which allows for the addition of larger volumes of other ingredients and allows for higher concentrations of other ingredients. Element. For example, Applicants have discovered that to prepare PVMMA/Polyquaternium-28 PECs, dilution of Polyquaternium-28 is not necessary (eg, ConditionezeNT-20, which is commercially available at a concentration of 20% active ingredient). More appropriately, according to the present invention, PVMMA/Polyquaternium-28PEC can be prepared in a single vessel by adding undiluted ConditionezeNT-20 directly to the PVMMA copolymer, which surprisingly produces stable high Concentration PEC. Furthermore, applicants have found that higher concentrations of PEC in compositions prepared according to the present invention are substantially more likely to be compatible with the preparation of hair care compositions, such as conditioners, relative to lower concentrations of conventional PEC compositions. The other ingredients together form a stable emulsion.

The present invention provides a method for graphically reconfiguring the repair process in repairing split-ends of hair fibers. In one embodiment, the method comprises securing hair fibers to a surface, wherein the hair fibers secured to the surface have split-ends or are damaged while on the surface to produce split-ends; A magnifying device is associated, wherein the split-end is placed in the field of view of the magnifying device; an image capture device is associated with the magnifying device, thereby capturing a magnified image in the field of view of the magnifying device; the split-end is treated with a composition, wherein The composition repairs the split-end, and wherein the split-end is fused together; and by an image capture device associated with the magnification device, capturing a repaired image of the split-end during treatment with the composition, and storing the captured A representative image of the inpainted image for subsequent retrieval. The method of graphically reconstructing hair restoration according to the present invention includes using video to record the hair restoration process in real time. Ideally, the hair restoration process is recorded at a magnification sufficient to observe the restoration process with the naked eye, for example at a magnification of 20-50 times, using video equipment suitable for recording the restoration process in real time. The video can be stored on a recording medium for subsequent retrieval using methods known to those skilled in the art.

Additionally, the methods of the present invention may comprise securing hair fibers to a surface, wherein the hair fibers secured to the surface have split-ends or are damaged while on the surface to produce split-ends. Thus, the hair fiber may have a split-end before it is secured to the surface, or the split-end may be induced to form (eg by mechanical means) after the hair fiber is secured to the surface. A surface may be any surface capable of being associated with a magnification device. Such surfaces may include, for example, table tops or microscope slides. The properties of the surface can be determined by the type of magnification device used. For example, if using an optical microscope, where light is passed through the sample, then a transparent surface, such as a microscope slide, can be used. As another example, the surface may be a mirror stand on which hair fibers will rest. As yet another example, if the magnifying device is a simple lens, such as a magnifying glass, then the surface could be a tabletop. Nothing should interfere with the repair of the split end. For example, coverslips for microscope slides should not be used if the coverslip will prevent the ends of split ends from coming together.

The hair fibers may be secured by any suitable means including, for example, the use of one or more clamps. The hair fibers can also be secured using tape, for example, when using a tabletop or microscope slide. Any suitable means may be used to fasten (eg fix) the hair fiber to the surface as long as the split ends of the hair fiber can be observed with a magnifying device.

The method of the invention may comprise associating the surface with a magnification device, wherein the split end is placed in the field of view of the magnification device. The magnifying device may be eg a magnifying glass, a microscope (eg an optical microscope). Each magnification device has a field of view. "Field of view" refers to the area of an image that is magnified by a magnifying device for viewing. The split-end is placed in the field of view so that the split-end is magnified for viewing.

Methods of the invention may include associating an image capture device with a magnification device, thereby capturing a magnified image of a field of view of the magnification device. The image capture device may be, for example, a digital recorder. The image capture device may also be an analog device. Non-limiting examples of image capture devices also include cameras, video cameras, charge-coupled device (CCD) cameras, digital cameras, and/or camcorders, or any other similar recording devices.

The methods of the invention may comprise treating the split-end with a composition, wherein the composition repairs the split-end, and wherein the split-end fuses together. Treatment may include, for example, massaging the composition into the hair. Treatment may also include, for example, rinsing the hair to remove the composition, for example with a rinse-off composition. The composition can be allowed to remain on the hair, for example when using a leave-on composition. The method of treatment can be any suitable method, including those described herein. The composition can be any suitable composition, including those described herein.

The method of the invention may comprise the steps of capturing, by means of an image capture device associated with a magnification device, a repaired image of the split-end during treatment with said composition, and storing a representative image of the captured repaired image , for subsequent retrievals. The image capture device may use any suitable means to capture the repair of the split-end. For example, if the image capture device is a digital recorder, then the digital recorder can generate the electronic document. As another example, if the image capture device is a camera, the camera may use film to capture the restoration.

Storing the captured representation of the repaired image for subsequent retrieval may be by any suitable means. For example, this may include storing an electronic representation of the image, such as using an electronic file accessible on a digital camera and/or computer. This can also be through the use of film.

Furthermore, the present invention may be used in any method of communication to consumers. These may include, for example, the use of still photographs (e.g. before and after photographs); diagrams, traces and/or diagrams; computer visualizations; and/or in vivo/in vitro/ In situ video. Additionally, the method of communication can be print, television, web, in-store, in-person demonstration (eg, live demonstration), and/or public media. The method of the invention can also be used to explain bonding mechanisms (eg PEC shrinkage to bring together two ends of a split-end).

The present invention also provides a method for quantitatively assessing the degree of repair of split-end hair fibers, the method comprising obtaining a bundle of hair, preferably twice bleached hair; producing a split-end of at least one hair fiber in the bundle (e.g. by sufficiently combing and/or drying the bundle to produce split-ends); removing at least one hair fiber having a split-end from the bundle; optionally marking the at least one removed hair fiber; capturing the at least one A first image of a split end of a removed hair fiber; associating the hair fiber with a bundle from which the hair fiber was removed; treating the bundle and the hair fiber with a composition; removing the hair fiber from the bundle removed; capture a second image of the end of the hair fiber, where the end is the same end as the first image used to capture the split end of at least one removed hair fiber; assign a value of 0 as a split The ends were not repaired, 1/2 was partially repaired, or 1 was fully repaired; and the assigned values for all marked hair fibers were summed and the sum was divided by the total number of marked hair fibers. When evaluated according to this method, exemplary compositions of the invention can obtain average values of, for example, an evaluation based on 20 fibers of 0.85 or greater, such as 0.925, 0.95 and even 0.975.

The methods of the invention may include generating a split-end. This may include combing or drying the bundle of hair to produce at least one hair fiber of the bundle with split ends. Other methods include selecting naturally forked ends. For example, a hair sample can be obtained from a biopsy where the hair has been split. However, this approach may result in poor reproducibility of the data due to diversity.

The method of the invention may comprise marking at least one removed hair fiber in the bundle of hair. The split end can start marking just at the beginning of the split. If the markings disappear after treatment with the composition, this may indicate that the split ends have broken the hair fiber. This fiber can then be excluded when assigning a value to a hair fiber because the split end is neither maintained as a split end nor repaired. Thus, for example, false positives can be avoided when assessing the repair capacity of a composition.

The method of the present invention may comprise capturing an image of the split-end of at least one removed hair fiber. Examples of such capture methods are described herein. This step may include storing an electronic representation of the image, for example using an electronic file accessible on a digital camera and/or computer.

The method of the invention may comprise associating at least one marked hair fiber with the bundle from which the hair fiber was removed. Returning the removed hair fibers to the tress provided a more natural environment for testing the restorative capabilities of the compositions. Hair fibers with split-ends are kept together with other hair fibers that do not have split-ends and remain in larger groups of hair fibers. This situation better simulates normal hair strands, such as the environment on a human head. Simply removing hair fibers with split ends and testing compositions on these removed fibers will only provide results based on artificial circumstances. Thus, when using this method to test compositions intended for consumer use, the present invention allows the reporting of results that are meaningful to those consumers, for example reporting results regarding the repair of hair fibers in circumstances that are important to consumers .

The method of the invention may comprise treating the strand and the at least one marked hair fiber with a composition. The treatment may include, for example, massaging the composition into the hair. The treatment may also include, for example, rinsing the hair to remove the composition, for example with a rinse-off composition. The composition may be allowed to remain on the hair, for example when using a leave-on composition. The treatment method can be any suitable method, including those described herein. The composition can be any suitable composition, including the compositions described herein.

The methods of the invention may include determining parameters of hair restoration. For example, the rate at which split-ends are repaired can be determined under defined conditions, such as those described herein. The compositions can then be compared to determine which provides faster repair of the split-end. The split-end repair efficiency of the compositions used and/or tested can also be determined, for example, using the video methods described herein. Repair of the split-end is preferably within 1 hour, less than 50 minutes, less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, less than 5 minutes, or less than 1 minute. The degree or amount of restoration may be 10% or greater, 20% or greater, 30% or greater, 40% or greater, 50% or greater, 60% or greater, 70% or greater, 80% or greater, 90% or greater, or complete (eg, about 100%). Repair can be measured relative to a negative control or untreated, where treated split-ends can show a statistically significant improvement in split-end repair (e.g., faster and/or greater repair or complete repair Spend).

The method of the present invention also includes assigning a value of 0 as split-end unrepaired, 1/2 as partially repaired, or 1 as fully repaired, and summing the assigned values for all marked hair fibers and dividing the sum by Total number of labeled hair fibers. Thus, for example, where there is a statistic for all split-ends of a bundle, the value obtained will give the ability of the composition to repair split-ends. A composition with poor repair ability will have a low and/or near zero value, while a composition with better repair ability will have a higher and/or near 1 value. Compositions can thus be compared using the method of the invention, wherein compositions leading to higher values provide better repair than compositions leading to lower values.

Any type of split-end can be repaired by the method of the present invention. One type of split-end includes, for example, a primary split-end. In this type of split-end, the hair fiber contains a single split along the longitudinal axis of the hair fiber, resulting in two ends of the hair fiber. Another example of a split-end includes a double Y split-end resulting from additional splits along the longitudinal axis of the primary split-end. A tree-like split-end is an example of a split-end where there are several double Y-shaped splits in one hair fiber. Another example of a split-end is the end of a hair fiber with many feathery short splits, which often result in a change in the thickness of the fiber shaft. Another example of a split-end is a long split-end, wherein one side of the primary split-end is significantly longer than the other (eg, one side is broken off). A tapered split-end is another example of a split-end where only a portion of the hair fiber remains at the end. Split-ends can also be characterized, for example, by the number of ends, eg a three-furnished end with two split hair fibers. A deep split end is an example of a split that occurs at the midpoint of the hair shaft (not necessarily the end). A lightly split end is an example of a split end that has only slight splits in the hair fiber. As used herein, the term "split ends" may include split ends that do not extend to the ends of the hair fibers. An example of such a fork is an incomplete fork. Figures 4A-4D show some types of split ends.

The hair fibers used in the methods of the present invention may be any mammalian hair. In one embodiment, the hair is human hair. Human hair of any country, region or race can be used, such as European, Asian, African or Caucasian. In one embodiment, the hair is European hair. The hair may have any type of damage due to, for example, one bleaching, two bleachings, more than two bleachings, coloring or mechanical damage. The hair fiber may not have any damage, just like the original hair. Additionally, the hair type used in the methods of the present invention may vary from one run of the method to another. Such hair changes may correspond to the use and testing of different compositions, which may for example depend on what type of result is desired to be communicated to the consumer. Varying the hair type and/or composition will allow the results to be communicated for any hair type and any hair care composition.

One aspect of the invention involves selecting hair fibers having split ends and cutting them to lengths (measured from the side of the split ends), for example, of about 1-1.5 inches. Small pieces of scotch tape can be used to secure the fibers to eg a glass slide. The slide can be placed under a microscope having, for example, 50X magnification and linked to a camera and computer. Lighting and focus can be adjusted accordingly. Depending on the setup, the recording can take place within a computer interface, or the camera can be set up, for example, on a tripod pointed at the computer screen. Recorded by a camera, a drop of the composition, for example containing 2% of the active complex, can be applied to the split-end using a micropipette. The lighting and focus can further be adjusted accordingly, and the hair dryer can be turned on, for example, on medium heat and aimed at the split ends. Recording can be done in between, and until the split-end has been fully or partially repaired.

Another aspect of the invention involves taking human hair, preferably damaged, most preferably twice bleached European hair, and assembling, for example, a wax-bonded strip, which may be, for example, 1-1.5 inches wide . These bundles are then combed thousands of times while pointing the hair dryer vertically in the direction of combing to create the proper number of split ends. A selected number (eg, 10-20) of fibers with split ends are selected and withdrawn from the fiber population. Photographs of each fiber end were taken by microscope at 20-50X magnification. A brass hoop was clamped over the end of each fiber opposite the split end. These brass hoops were then marked and placed between two pieces of masking tape. The set was then inserted into the middle of the tress and secured with a paper clip to hold the set in place. The bundle is then treated with a rinse-off split-end repair composition for a series of cycles, for example three cycles. After the final cycle, the clamps were removed and new pictures of the split ends were taken. By comparing the before and after photos, the assessor can assign a value of "0" for no restoration, "1/2" for partial restoration, and "1" for complete restoration. These values were summed and divided by the total number of fibers to express the extent of split-end repair.

As noted above, an image capture system is used in embodiments of the present invention to generate representative images of the appearance of a split-end before and after a repair or attempted repair. While a variety of such image capture systems are possible within the scope of the teachings herein, an exemplary such system is shown in FIG. 6 . Specifically, FIG. 6 is a schematic diagram showing an image data capture system in which the described image capture and processing steps can be performed.

The illustrated system 600 includes several interacting components, including a sample support device 601 , such as a platform or surface adapted to support a sample 602 . The sample support 601 may be transparent to allow downlighting by the light source 603 . The light source 603 can also be arranged above the support device 601 to provide illumination through reflection.

An electronic image capture device 604 is provided for capturing enlarged images or video sequences of the sample 602 as it is being processed. In this regard, the magnification device 605 is adjacent to the sample support device 601 , between the sample support device 601 and the image capture device 604 . Image capture device 604 may also be a still camera or video camera adapted to capture a sequence of images. The magnifying device 605 may be an optical magnifying glass or lens device such as an optical microscope, or may be an electronic magnifying device such as an electron microscope or the like. In embodiments of the invention, image capture device 604 and/or magnification device 605 may be scannable to capture images of different regions or sections of sample 602 .

An auxiliary computing and data capture device 606 is provided to control and receive data from the image capture device 604 . Auxiliary computing and data capture device 606 is a computing processing device capable of receiving electronic image data from image capture device 604 and sending control signals to image capture device 604 to capture an image. The auxiliary computing and data capture device 606 may also control the lighting device 603 .

In an embodiment of the invention, the auxiliary computing and data capture device 606 is communicatively connected to the electronic database 607 by wire or wirelessly, locally or remotely. In this way, secondary computing and data capture device 606 is capable of collecting data from image capture device 604 and storing the collected data in electronic database 607 for subsequent analysis, manipulation, and/or redistribution, such as to a printing or publishing device (not shown).

The auxiliary computing and data capture device 606 may be a computer, such as a personal computer, a laptop, a workstation, etc., and operates by the computer executing computer-readable instructions stored on a computer-readable medium. Computer readable media are tangible media such as magnetic or optical disk systems, flash drives, PROs, and the like. Accordingly, steps discussed herein involving data capture, manipulation and/or transmission are performed in this manner. User interface 608 allows a user to receive information from auxiliary computing and data capture device 606 in a human-understandable manner, and to provide input to the device in a computer-understandable manner. In an embodiment of the present invention, the user interface 608 includes an on-screen graphical user interface as well as a keyboard, keys, pad, mouse, and/or other user input mechanisms.

In an embodiment of the invention, the image capture device is a video camera adapted to record in real time the repair of one or more hair shafts, for example a hair shaft comprising one or more split ends. Ideally, the video is recorded at a magnification sufficient to observe the hair restoration process in real time with the naked eye. Suitable magnifications may include, for example, 20-50X magnification.

The invention is further described by the following examples but, of course, should not be construed as limiting the scope of the invention in any way.

Example 1

This example illustrates the use of a two-container process to prepare a hair care composition comprising a polyelectrolyte complex.

Compositions 1A-1C

For the mixers listed in this and other examples, one skilled in the art will be able to determine the proper RPM setting based on identifying the particular vessel to be used and following the experimental protocols listed.

In a suitable, stainless steel premix vessel, charge water set to 113-131°F (45-55°C). Begin vigorous turbo mixing (turbine mixer on vigorous clockwise; side sweep mixer off). Once the batch temperature reaches 86°F (30°C) or higher, and with vigorous mixing, the PVMMA copolymer ( S-97BF; ISP, Wayne, NJ, USA) was slowly added to the premix vessel. Adjust mixing accordingly to obtain vigorous stirring without creating excess foam on the surface of the liquid. Once all the powder has been added, rinse the mixing blade and sidewall with water set at 113-131°F (45-55°C). Once the rinse is complete, turn on the side sweep agitator and begin heating to 122-131°F (50-55°C). (Clubs will disperse faster when premixed at 113-131°F (45-55°C)). Continue heating and maintain this temperature throughout the mixing period. Set mixer (turbine mixer at vigorous counterclockwise; side sweep mixer at moderate clockwise).

The batch was mixed for at least 20 minutes, or until no particles or lumps were present.

Once premix is homogeneous and free of lumps, reduce turbo mix to medium. Add sodium hydroxide to the premix container and mix for 10 minutes. The solution will have low viscosity and will appear slightly cloudy (mixer settings: turbo mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Mix the batch for at least 10 minutes or until completely homogeneous.

Once the batch is homogeneous, samples are subjected to an in-process pH test. Continue to repeat the test sample until a stable pH reading of 6.9-7.0 is obtained. If the pH is low, add an additional 20% sodium hydroxide to meet the specified range. Mix again and sample again. If the pH is high, add additional aspartic acid to meet the specified range. Mix again and sample again.

Once the Gantrez has been fully hydrated and the pH is within specification, check that the premix temperature is 122-131°F (50-55°C). Apply heat if necessary. Once premixed at 122-131°F (50-55°C), turn off side sweep mixer, reverse turbine direction and increase turbine mix speed to create a vortex (turbine mixer at strong clockwise direction; side sweep mixer off ).

Slowly add polyquaternium-28 ( NT-20 (20% active ingredient); ISP, Wayne, NJ, USA) to the premix container. Add slowly to the premix vessel to obtain the proper particle size of the polyelectrolyte complex. Use the drum spout to adjust the addition flow rate. Do not pour the entire open container into the premix container at once. During the addition of this material, the premix will become very viscous and begin to turn white. Once all the materials have been added, the solution will be diluted again and will be milky in appearance.

Reverse turbine direction and turn on side sweep agitator. Mix vigorously for 20 minutes or until premix is completely homogeneous (turbine mixer at vigorous counterclockwise, side sweep mixer at moderate clockwise). The batch was mixed for at least 20 minutes or until there were no visible particles or lumps.

Once the mixing is complete, a sample is taken and the premix is visually inspected. Check that it is completely white and not cloudy or dull. Also check that the premix viscosity is thin and milky and not too viscous. If the premix is not thin and milky, continue mixing vigorously for an additional 20 minutes and sample again.

Once the premix is completely homogeneous, reduce agitation and begin cooling, to 86-113°F (30-45°C). Maintain mixing and temperature until the premix is about to be added to the main compounding vessel (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction).

In the main stainless steel composite vessel, fill with water set at 180-185°F (82-85°C) with moderate mixing (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise direction). Slowly add disodium EDTA and aspartic acid to the main compounding container. After the ingredients have been added, begin heating the batch to 180-185°F (82-85°C), as needed (turbine mixer in moderate counterclockwise direction). Continue heating the batch to 180-185°F (82-85°C). The batch was mixed for at least 5 minutes or until the solids were completely dissolved.

Once the batch temperature is 176°F (80°C) or higher, add stearamidopropyldimethylamine to the main compounding vessel and mix until completely melted (turbine mixer at moderate counterclockwise; side sweep mixer on moderate clockwise). Continue heating the batch to 180-185°F (82-85°C). The batch was mixed for at least 5 minutes or until the solids were completely melted.

Once the batch temperature is 180-185°F (82-85°C), add the following ingredients to the main compounding tank: Cetyl Alcohol, Stearyl Alcohol, Glyceryl Stearin for Composition 1A (Conditioner) Cetyl Alcohol, Glyceryl Stearate, and Aminopropyl Dimethicone for Composition 1B (overnight cream); for Composition 1C (Leave-on Cream) of Cetyl Alcohol and Glyceryl Stearate. Once the batch temperature is again at 180-185°F (82-85°C), maintain this temperature and mix for at least 30 minutes (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Mix the batch while maintaining it between 180-185°F (82-85°C).

Take a sample from the main compounding vessel and visually inspect that all solids have melted and the batch is smooth and homogeneous. Continue vigorous mixing and sample again if any undissolved material or particles are present.

Begin cooling the batch to 104-113°F (40-45°C) and reduce turbine and side sweep agitator speeds to moderate/slow to help degas the batch (turbine mixer at moderate counterclockwise; side sweep mixer in a slow clockwise direction). Once the batch temperature is 167°F (75°C) or less during cooling, add propylene glycol to the main compounding vessel (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). For Composition 1C (leave-on cream), glycerin was also added at this mixing speed.

Turn off side sweep agitator once main batch temperature is 150°F (65°C) or lower for Composition 1A (conditioner) or 131°F (55°C) or lower for cream , reverse direction of turbo mixer, and intensify mixing to create a slight vortex (turbine mixer at moderate clockwise; side sweep mixer off). Will SC-96 (65% Polyquaternium-37, 25% Propylene Glycol Dicaprylate/Dicaprate, 10% PPG-1 Trideceth-6; Ciba/BASF, Basel, Switzerland ) to the main compounding vessel and continue cooling to 104-113°F (40-45°C). (Mix well in its container before adding to the batch SC-96).

Once all the ingredients have been incorporated into the batch and are no longer on the surface, reverse the turbine agitator and turn on the side sweep agitator (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise direction).

Once the main batch temperature is 150°F (65°C) or less for Composition 1A (conditioner) or 131°F (55°C) or less for Composition 1B (overnight cream), and the premix is ready, it is added to the main compounding container. While the premix was being added, the turbine mixer was turned off or slowed to slow so that the liquid level was set above the top of the turbine blades to minimize aeration. Once the premix has been added, rinse the premix container with water set at 77-95°F (25-35°C) and add it to the main compounding container. As the premix is mixed into the batch, the viscosity of the batch will decrease. Adjust mixer speed accordingly to avoid splashing (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise).

For Composition 1A (conditioner), mix the batch for at least 15 minutes or until the batch is homogeneous. Once the main batch temperature is 122°F (50°C) or lower, add the LluidBlend directly to the main compounding tank. Mix well during addition. Intensify mixing as needed to incorporate silicone (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise).

For creams, water set at 77-95°F (25-35°C) is added if possible once all of the premix has been added, this is done below the surface of the batch to minimize aeration. Mix the batch for at least 15 minutes or until the batch is homogeneous. Continue cooling to 104-113°F (40-45°C). In a suitable stainless steel phase vessel or container, premix the following silicone ingredients under vigorous agitation: OSW5 (84% Cyclopentasiloxane, 15% Dimethiconol, 1% Dimethicone) and Dimethicone (60,000cst); used in Composition 1C ( Leave-on Cream), Dimethicone (60,000cst), Phenyl Trimethicone (DC-556; DowCorning) and D5 Dimethiconol (DC-1501) . Once the silicone premix is homogeneous, add it to the main compounding container and allow as much of the silicone premix container to drain as possible into the main batch container. Intensify mixing as needed to incorporate silicone (turbine mixer on vigorous counterclockwise; side sweep mixer on moderate clockwise).

When the batch temperature is 113°F (45°C) or less, add the following ingredients to the main compounding tank: fragrance (fragrance), DMDM hydantoin, coconut palm oil, keratin amino acids, flower / leaf extract. For Composition 1B (overnight cream), DC-8500 (82% bis(C13-15 alkoxy) PG-amodimethicone, 18% C14-15 alcohol; Dow Corning, Midland, MI, USA). Continue mixing and cooling to 95-104°F (35-40°C).

Mix vigorously for at least 45 minutes or until all lumps have been removed and the batch is smooth and uniform. The batch can be recirculated by passing this final mixture through an 80 mesh filter to help break up lumps. Minimize aeration as much as possible (turbine mixer at vigorous counterclockwise; side sweep mixer at moderate clockwise), although shear (intensive mixing and/or recirculation) is required to break up the agglomerates ). Mix for at least 45 minutes.

Samples were analyzed when the batch temperature was 95-104°F (35-40°C). Stop mixing and cool.

Adjustments can be made as follows. If the pH is low, add sodium hydroxide (20%) at a maximum of 5% of the total batch requirement. Mix again and sample again. If the pH is high, add aspartic acid at a maximum of 7.5% of the total batch requirement. Mix again and sample again. If viscosity is low, mix for an additional 60 minutes and resample. The batch can also be recirculated through an 80 mesh filter.

Pumps that should be used to pump material into containers include diaphragm and positive displacement. Filters that should be used include 80 mesh for all transfer operations. Fill temperature should be 90-99°F (32-37°C). If the product temperature drops below 90°F (32°C), there is no need to reheat the batch.

Composition 1D

In the main stainless steel composite vessel, fill the water set at 95-104°F (30-35°C) and begin vigorous agitation (turbine mixer at vigorous counterclockwise direction, if available; side sweep mixer at Moderately clockwise). Do not heat the water to maintain temperature. Slowly add the following ingredients in order to the main compounding vessel and mix vigorously (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available) for 10 minutes or until batch The feed is completely homogeneous and no lumps present: PVM/MA copolymer (Oantrez S97BF), NaOH, Polyquaternium-28 (Conditioneze). The batch was mixed for at least 10 minutes or until the batch was completely homogeneous and no lumps were present.

With vigorous mixing (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available), add the following ingredients to the main compounding tank: PVP, Disodium EDTA. Mix the batch for at least 15 minutes or until the solids are completely dissolved and the batch is homogeneous.

After mixing, take a sample from the main compounding container and check that no lumps or particles are present and that the batch is smooth and uniform. If lumps or particles are present, continue mixing and resampling until the batch is smooth and uniform.

Begin heating the batch to 170-175°F (76-79°C) with vigorous agitation (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available). Once the batch temperature reaches 150°F (65°C) or higher, add the following ingredients to the main compounding tank: Stearyldimethylbenzylammonium chloride. Keep the batch between 170-175°F (76-79°C) while mixing it. The batch was mixed for at least 60 minutes.

A sample was taken from the main compounding vessel and visually inspected for the absence of lumps or particles, and the batch was homogeneous. If lumps or particles are present, continue to mix vigorously and resample until the batch is uniform.

Slow agitation to moderate (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction, if applicable) and begin cooling the batch to 90-95°F (32-35°C).

While cooling, add the following ingredients, in order, to the main compounding container. Mix well after each addition of: DC949 Cationic Emulsion; Glycerin USPVEG; PEG-12 Dimethicone; Propylene Glycol; Triethanolamine; Citric Acid.

Once the batch temperature is 113°F (45°C) or lower, add the following ingredients to the main compounding container in order: DMDM Hydantoin; Hydrolyzed Silk Protein; Vitamin Blend; Polyglyceryl-3 Distearate mixture.

In a separate stainless steel vessel or container equipped with an electric or air mixer, premix the following ingredients: Polysorbate 20; Fragrance. Blend this premix vigorously until all fragrance is dissolved and the premix is homogeneous and clear. Load this premix into the main compounding vessel with moderate agitation. Rinse the premix vessel/container with cold water set at 60-80°F (15-27°C) and add to the main compounding container. Mix (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction, if applicable) for at least 20 minutes or until the batch is completely homogeneous.

Adjustments can be made as follows. If the pH is low, add the triethanolamine solution in increments of 0.20% solution. If the pH is high, add the citric acid solution in increments of 0.20% solution.

Pumps that should be used to pump material into the container include diaphragm and positive displacement types. Filters that should be used include 80 mesh for all transfer operations. Fill temperature should be ambient temperature. The batch can be cooled as needed to facilitate filling.

Composition 1E

In the main stainless steel composite vessel, where applicable, add water set to 68-86°F (20-30°C) and begin vigorous agitation (turbine mixer at vigorous counterclockwise direction; side sweep mixer in a moderate clockwise direction).

Slowly add the following ingredients in order to the main compounding vessel and mix vigorously (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction) for 5 minutes or until batch is completely uniform and not Blocks are present: PVM/MA Copolymer (Gantrez S97BF), Sodium Hydroxide (20%), Polyquaternium-28 (Conditioneze). The batch was mixed for at least 5 minutes or until the batch was completely homogeneous and no lumps were present.

Once the batch is uniform, slowly spray the following ingredients into the main compounding tank: Polyquaternium-10. Where possible, use vigorous mixing to obtain a vortex. Rinse the inside of the container and mixer blades with water (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction).

Begin heating the batch to 113-122°F (45-50°C). Mix while heating for at least 20 minutes, or until the polymer is fully hydrated and the solution is clear and homogeneous.

After mixing, take a sample from the main compounding container and check that no lumps or particles are present and that the batch is smooth and uniform. If lumps or particles are present, continue mixing and resampling until the batch is smooth and uniform. While continuing to heat, reduce turbine agitation (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise) and add the following ingredients in order to the main compounding vessel: Cocamidopropyl Betaine, Disodium EDTA, Citric Acid, USP. Mix for at least 10 minutes or until the batch is uniform and all components are completely dissolved.

Check that the batch temperature is 113-122°F (45-50°C). Then, add the following ingredients to the main compounding vessel in order with moderate agitation (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Work carefully to avoid aeration and slow down mixing if necessary during addition: Sodium Laureth Sulfate; Disodium Laureth Sulfosuccinate; Ethylene Glycol Distearate, Cocamidopropyl Betaine, Cocamide MEA, Water Blend; PEG-6 Caprylic/Capric Triglyceride. As the liquid level rises in the vessel, reduce the speed of the turbo mixer to slow as the liquid level approaches the vanes. Once the blades are fully covered with the batch, increase the turbo mixer speed back to moderate. This will help reduce aeration of the batch. Keep the batch between 113-122°F (45-50°C) while mixing it. Mix for at least 20 minutes or until the batch is smooth and completely homogeneous.

Degas the batch by reducing turbine and side sweep agitation to slow (turbine mixer at slow counterclockwise direction; side sweep mixer at slow clockwise direction) and begin cooling the batch to 95-104°F (35-40°C).

Once the batch temperature is 113°F (45°C) or lower, increase the agitation of the turbine and side sweep to moderate (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise), and Add the following ingredients in order to the main compounding container: Fragrance; Methylchloroisothiazolinone, Methylisothiazolinone, Water Mix; Coconut Oil; Keratin Amino Acids, Flower Extract.

In a separate stainless steel vessel or container, mix the sodium chloride and water set at 95-104°F (35-40°C) until the salt is completely dispersed. The salt may not dissolve completely because the amount of water may not be sufficient. Mix until the salt is fully dispersed and then continue.

Once the premix of the salt is ready, add it to the main compounding tank and mix until the batch is completely uniform (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise) . Rinse premixed vessels or containers with cold water and flush transfer lines. Add this rinse/rinse water to the main compounding tank. Mix for at least 30 minutes or until the batch is completely uniform. The composition was sampled. Stop mixing and let cool (if applicable).

Adjustments can be made as follows. If the viscosity is low, add sodium chloride. The total sodium chloride level in the formulation should not exceed 2.00%. If the viscosity is high, add propylene glycol. Sodium hydroxide (20%) was added if the pH was low. If the pH is high, add citric acid.

Aerated Batch: Reheat batch to 120-125°F (48-52°C) and mix slowly for 20 minutes. Cool back to 95-100°F (35-38°C), add 10% preservative, and add flavor if necessary.

Pumps that should be used to pump material into the container include diaphragm and positive displacement types. Filters that should be used include 80 mesh for all transfer operations. Fill temperature should be 90-100°F (32-38°C). The batch can be heated to this temperature range to help facilitate filling.

Composition 1F

Mix well in its container before being weighed and added to the batch SC-96.

In a suitable, stainless steel premix vessel, charge water set at 113-131°F (45-55°C). Begin vigorous turbo mixing (turbine mixer on vigorous clockwise; side sweep mixer off).

Once the batch temperature is 86°F (30°C) or higher, and with vigorous mixing, slowly add the PVM/MA copolymer (Gantrez S-97BF) to the premix vessel. Adjust mixing accordingly for vigorous stirring without creating excess foam on the surface of the liquid. Once all the powder has been added, rinse the mixing blade and sidewall with water set at 113-131°F (45-55°C). Once the rinse is complete, turn on the side sweep agitator (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise) and begin heating to 122-131°F (50-55°C). When the premix is 113-131°F (45-55°C), the powder clumps will disperse faster. Continue heating and maintain this temperature throughout the mixing period. The batch was mixed for at least 20 minutes or until no particles or lumps were present.

Once premix is homogeneous and free of lumps, reduce turbo mixing to medium (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise). Add sodium hydroxide to the premix container and mix for 10 minutes. The solution will have low viscosity and will appear slightly cloudy. Mix the batch for at least 10 minutes or until completely homogeneous.

Once the batch is homogeneous, samples are taken for an in-process pH test. Continue to repeatedly test the sample until a stable pH reading is obtained. If the pH is low, add additional sodium hydroxide (20%) to meet the specified range. Mix again and sample again. If the pH is high, add aspartic acid to meet the specified range. Mix again and sample again.

Once the Gantrez has been fully hydrated and the pH is within specification, check that the premix temperature is 122-131°F (50-55°C). Heat if necessary.

Once premix is 122-131°F (50-55°C), turn off side sweep mixer, reverse turbine direction and increase turbine mix speed to create a vortex (turbine mixer at moderate clockwise direction; side sweep mixer off ). Add Polyquaternium-28 (Conditioneze NT-20) slowly to the premix vessel. Add slowly to premix container to achieve proper compound particle size. This addition should take 10-15 minutes to complete. Use the drum spout to adjust the addition flow rate. Do not pour the entire open container into the premix container at once.

During this material addition, the premix will become very viscous and begin to turn white. Once all the materials have been added, the solution will be diluted again and will appear milky in appearance.

Reverse turbine direction and turn on side sweep mixer (turbine mixer at vigorous counterclockwise; side sweep mixer at moderate clockwise). Mix vigorously for 20 minutes or until the premix is completely homogeneous. The batch was mixed for at least 20 minutes or until no particles or lumps were present. Once mixing is complete, a sample is taken and the premix is visually inspected. Check that it is completely white and not cloudy or dull. Also check that the premix viscosity is thin and milky and not overly viscous. If the pre-mix is not thin Wagyu milky white, continue mixing vigorously for an additional 20 minutes and sample again.

Once the premix is completely uniform, reduce agitation (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise) and begin cooling to 86-113°F (30-45°C). Maintain mixing and temperature until the premix is ready to be added to the main compounding container.

In the main stainless steel composite vessel, fill with water set at 180-185°F (82-85°C) with moderate mixing (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise direction).

Slowly add the following components to the main compounding tank: Disodium EDTA; Aspartic Acid. After the components were added, begin heating the batch to 180-185°F (82-85°C), as needed. (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise). Continue heating the batch to 180-185°F (82-85°C). Mix the batch for at least 5 minutes or until the solids are completely dissolved.

Once the batch temperature is 176°F (80°C) or higher, add stearamidopropyldimethylamine to the main compounding vessel and mix until completely melted (turbine mixer at moderate counterclockwise; side Swipe mixer in a moderate clockwise direction). Continue heating the batch to 180-185°F (82-85°C). The batch was mixed for at least 5 minutes or until the solids were completely melted.

Once the batch temperature is 180-185°F (82-85°C), add the following ingredients to the main compounding container: Cetyl Alcohol, Glyceryl Stearate, Aminopropyl Dimethicone.

Once the batch temperature is again at 180-185°F (82-85°C), maintain this temperature and mix for 30 minutes (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Mix the batch while maintaining it between 180-185°F (82-85°C). The batch was mixed for at least 30 minutes.

After hot mixing, take a sample from the main compounding vessel and visually inspect that all solids have melted and the batch is smooth and homogeneous. If there is still any undissolved material or particles, continue mixing vigorously and resampling periodically until all wax and particles are dissolved and the batch is uniform.

After hot mixing, begin to cool the batch to 104-113°F (40-45°C) and reduce the turbine and side sweep mixer speeds to moderate/slow to help degas the batch (turbine mixer at moderate counterclockwise ; side sweep mixer in a slow clockwise direction).

While cooling and once the batch temperature is 167°F (75°C) or less, add the propylene glycol to the main compounding vessel (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction) .

Once the main batch temperature is 150°F (65°C) or lower, turn off the side sweep agitator, reverse the direction of the turbine agitator and intensify mixing to create a slight vortex (turbine mixer at moderate clockwise; side sweep the mixer off). Will Add SC-96 to the main compounding vessel and continue cooling to 104-113°F (40-45°C).

Once all the ingredients have been incorporated into the batch and are no longer on the surface, reverse the turbo mixer and turn on the side sweep agitator (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise direction).

Once the main batch temperature is 131°F (55°C) or less and the PEC active premix has been prepared, add the premix to the main compounding tank. While the premix was being added, the turbine mixer was turned off or slowed to slow when the liquid level was set past the top of the turbine blades to minimize aeration.

Once the premix has been added, rinse the premix container with cold water set at 77-95°F (25-35°C) and add it to the main compounding container. As the PEC active ingredient premix is mixed into the batch, the viscosity of the batch will decrease. Adjust mixer speed accordingly to avoid splashing (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise).

Once all of the PEC active ingredient premix has been added, if possible, fill the batch below the surface with cold water set at 77-95°F (25-35°C), which minimizes aeration. Mix the batch for at least 15 minutes or until the batch is homogeneous. Continue cooling to 104-113°F (40-45°C).

In a suitable stainless steel phase vessel or container, premix the following components with vigorous agitation: Cyclopentasiloxane Mixture; Dimethicone. Once the premix is homogeneous, add it to the main compounding vessel and allow as much of the premix vessel to drain as possible into the main batch vessel (turbine mixer at vigorous counterclockwise; side sweep mixer at moderate clockwise). clockwise), mixing more intensively as needed to incorporate the silicone.

When the batch temperature is 113°F (45°C) or lower, add the following ingredients to the main compounding container: DC-8500; Fragrance; DMDM Hydantoin, Coconut Oil, Keratin Amino Acids, Flower Extract mixture of substances. Continue mixing and cooling to 95-104°F (35-40°C).

Mix vigorously (turbine mixer at vigorous counterclockwise; side sweep mixer at moderate clockwise) for at least 45 minutes or until all lumps have been removed and batch is smooth and homogeneous. Batch material can be recirculated through an 80 mesh filter throughout this final blend to help break up lumps. Aeration should be minimized as much as possible, although shearing (enhanced mixing and/or recirculation) should be used to break up the pieces. Mix for at least 45 minutes. Compositions were sampled when the batch temperature was 95-104°F (35-40°C). Stop mixing and let cool.

Adjustments can be made as follows. If the pH is low, add sodium hydroxide (20%) at a maximum of 5% of the total batch requirement. Mix again and sample again. If the pH is high, add aspartic acid at a maximum of 7.5% of the total batch requirement. Mix again and sample again. If viscosity is low, mix for an additional 60 minutes and sample again. The batch can also be recycled through an 80 mesh filter.

Pumps that should be used to pump material into the container include diaphragm and positive displacement types. Filters that should be used include 80 mesh for all transfer operations. Fill temperature should be 90-99°F (32-37°C). If the product temperature drops below 90°F (32°C), do not reheat the batch.

Example 2

This example illustrates the preparation of a hair care composition comprising a polyelectrolyte complex using a one-vessel process.

The method of Example 1 describes a two-vessel process where the polyelectrolyte complex is prepared in one vessel, the remaining components are mixed in a separate vessel, and the polyelectrolyte complex and remaining components are combined. In order to simplify the process into one vessel, the process was carried out as described in Example 1, except that the polyelectrolyte complex was first prepared in the vessel, and the other components were added directly to the polyelectrolyte complex after formation. in the same container. The final viscosity of the composition may be lower than if prepared in two containers. To compensate, add an additional SC96.

Example 3

This example illustrates the compatibility of polyelectrolyte complexes (PECs) with certain charged compounds and polymers.

Visual Appearance: The visual appearance of PECs in solutions containing charged particles was characterized. When PVMMA and Polyquaternium-28 were solvated individually in water, the composition was clear. When PVMMA and Polyquaternium-28 are present as PEC solvated in water, the composition becomes cloudy and/or milky in appearance. After adding another charged species to the PEC that yields a clear composition when solvated in water, the milky/cloudy opacity is expected to decrease (and in some cases turn back to clear). This is a visual indication of the reversal of the PEC compounding process. The milky opaque appearance of 1 wt.% and 2 wt.% PVMMA/polyquaternium-28 PEC was greater than that of 0.5 wt.% polyquaternium-4 ( L-200; AkzoNobel, Amsterdam, Netherlands) will disappear in the presence of. This indicates that the structure of the PEC has been disrupted. Less than 0.5% by weight of At L-200, the PEC will not be destroyed. 0.5% by weight H-100 does not destroy PEC. L-200 and H-100 are similar, but L-200 has a lower viscosity and higher cationic activity.

Thickening: Tinovis GTC/Acrylates/Beheneth-25 Methacrylate Copolymer (2.3%) was tested in compositions with and without PEC. Compositions without PEC gave viscosities of 40,000-60,000 centipoise. Compositions containing PEC are water-diluted. Since Tinovis is an associative thickener, and compositions without PEC would not be thickened, it is believed that Tinovis is rendered ineffective by PEC.

Split-end repair: Table 11 shows charged compounds and polymers that bind to PECs. These compositions did not show detrimental effects on split-end repair.

Table 11

Example 4

This example describes a preparation comprising a polyelectrolyte complex and a charged polymer.

All compositions 4B-4E exhibited freeze-thaw stability. The inventors also surprisingly found that relative to compositions 4B, 4C and 4E, comprising Composition 4D of SC96 exhibited excellent long-term controllable viscosity (wherein the viscosity remained stable over long-term).

Comparative Composition 4A did not include PEC, while Compositions 4B-4E included PVMMA:Polyquaternium-28PEC and charged compounds and/or polymers. All compositions are rinse-off conditioners. Adjust with sodium hydroxide/citric acid/aspartic acid to obtain proper pH if necessary.

"MS" indicates compliance with the standard.

Compositions 4A-4E

Target Spec 4A:

pH: 4.00-5.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C):

Bulk viscosity: 5,000-9,000 centipoise

w/shear viscosity (finished product): 10,000-30,000 centipoise

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque emulsion

Target Specification 4B:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C):

Bulk viscosity: 7,000-15,000 centipoise

w/shear viscosity (finished product): 20,000-35,000 centipoise

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque emulsion

Target Specification 4C:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C):

Bulk viscosity: 7,000-15,000 centipoise

w/shear viscosity (finished product): 20,000-35,000 centipoise

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque emulsion

Target Specification 4D.

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C):

Bulk viscosity: 7,000-15,000 centipoise

w/shear viscosity (finished product): 20,000-35,000 centipoise

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque emulsion

Target Specification 4E:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C):

Bulk viscosity: 7,000-15,000 centipoise

w/shear viscosity (finished product): 20,000-35,000 centipoise

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque emulsion

Example 5

This example illustrates the method of preparing the composition of Example 4.

For Comparative Composition 4A, the vessel was initially heated to 80-85°C and the following ingredients were added: deionized water, citric acid, and disodium EDTA. Check that the temperature is 80-85°C and add the following ingredients: Quaternium-18/water, Stearamidopropyl Dimethylamine, Cetyl Alcohol and Stearyl Alcohol. Mix vigorously for 30 minutes at 80-85°C. Cool the mixture. At 57-60°C, add L-aspartic acid slowly. At 45°C or less, add the following ingredients: Isostearamidopropylethyl Dimethyl Ammonium Ethyl Sulfate/PEG-9, Cyclopentasiloxane/Cyclohexasiloxane/Dimethicone Silicone, Fragrance and DMDM Hydantoin.

Compositions 4B, 4C and 4E were prepared using two phases. For Composition 4B, 52.05% by weight (of the final total weight % of the composition) of deionized water was added to the main phase. Begin heating to 80-85°C. Add the following ingredients one at a time and mix until completely dissolved and the solution becomes clear: Disodium EDTA and L-Aspartic Acid. Add the following ingredients one at a time at 80-85°C and mix until melted: stearamidopropyldimethylamine (check to make sure solution becomes clear), cetyl alcohol and glyceryl stearate. Mix vigorously for 30 minutes at 80-85°C. After 30 minutes, the heat was turned off, the mixing speed was reduced, and the composition was allowed to cool slowly. In the secondary phase, 15.5% by weight (of the final total weight % of the composition) of deionized water was added, and the following ingredients were slowly added and mixed until hydrated: PVMMA copolymer (( S-97BF; ISPCorp., Wayne, NJ, USA) and sodium hydroxide (20% active ingredient). The solution will thicken slightly. The in-process pH should be 6.90-7.00. Heat the secondary phase to 50-55°C. Slowly add Polyquaternium-28 ( NT-20; ISPCorp.). The solution will turn opaque and become less viscous. The secondary phase was cooled and 0.05% by weight (of the final total weight % of the composition) of DMDM hydantoin was added at < 45°C. Slowly add the side phase to the main phase at < 45 °C. Then add the following ingredients: TQuat60 (Siloxane Quaternium-22; Evonik, Essen, Germany), propylene glycol, fragrance and (of the final total weight % of the composition) 0.15% by weight of DMDM hydantoin.

For Composition 4C, 52.45% by weight (of the final total weight % of the composition) of deionized water was added to the main phase. Begin heating to 80-85°C. Add the following ingredients one at a time and mix until completely dissolved and the solution becomes clear: Disodium EDTA and L-Aspartic Acid. Add the following ingredients one at a time at 80-85°C and mix until melted: Stearamidopropyldimethylamine (check to make sure the solution turns clear), Cetyl Alcohol and Glyceryl Stearate. Mix vigorously for 30 minutes at 80-85°C. After 30 minutes, the heat was turned off, the mixing speed was reduced, and the composition was allowed to cool slowly. In the secondary phase, 15.5% by weight (of the final total weight % of the composition) of deionized water was added, and the following ingredients were slowly added and mixed until hydrated: PVMMA copolymer ( S-97BF; ISPCorp., Wayne, NJ, USA) and sodium hydroxide (20% active ingredient). The solution will thicken slightly. The in-process pH should be 6.90-7.00. Heat the secondary phase to 50-55°C. Slowly add Polyquaternium-28 ( NT-20; ISPCorp.). The solution will turn opaque and become less viscous. The secondary phase was cooled and 0.05% by weight (of the final total weight % of the composition) of DMDM hydantoin was added at < 45°C. Slowly add the minor phase to the major phase at < 45°C. Premix the Quaternium-80/Propylene Glycol and Dimethicone and then add to the combined Major and Secondary phases. Then add the following ingredients: DC-8500 (bis(C13-15 alkoxy) PG-amodimethicone, DowComing, Midland, MI, USA), propylene glycol, fragrance and (composition final total weight %) 0.15% by weight of DMDM hydantoin.

For composition 4D, 40% by weight (of the final total weight % of the composition) of deionized water was added. Slowly add the following ingredients and mix until hydrated: PVMMA Copolymer ( S-97BF (ISP)) and sodium hydroxide (20% active ingredient). The solution will thicken slightly. The in-process pH should be 6.90-7.00. Heat to 50-55°C and slowly add Polyquaternium-28 ( NT-20; ISPCorp.). The solution will turn opaque and become less viscous. Begin heating to 80-85°C and add the following ingredients one at a time, mixing until fully dissolved: Disodium EDTA, L-Aspartic Acid, and (of the final total weight % of the composition) 22.95% by weight of deionized water. Add the following ingredients one at a time at 80-85°C and mix until melted: Stearamidopropyldimethylamine, Cetyl Alcohol, Stearyl Alcohol, Glyceryl Stearate, Crodamol STS (PPG-3 Benzyl Ether Myristate esters; Croda, Inc., Edison, NJ, USA), SC96 (65% Polyquaternium-37, 25% Propylene Glycol Dicaprylate/Dicaprate, 10% PPG-1 Trideceth-6; /BASF, Basel, Switzerland). Mix vigorously for 30 minutes at 80-85°C. Reduce mixing speed and allow composition to cool. When the temperature is ≤45°C, add the following ingredients: D5/D6/Dimethicone, Propylene Glycol, Fragrance and DMDM Hydantoin.

For Composition 4E, 50.47% by weight (of the final total weight % of the composition) of deionized water was added to the main phase. Begin heating to 80-85°C. Add the following ingredients one at a time and mix until completely dissolved and the solution becomes clear: Disodium EDTA and L-Aspartic Acid. Add the following ingredients one at a time at 80-85°C and mix until molten: Stearamidopropyldimethylamine (check to make sure the solution becomes clear), Cetyl Alcohol, Glyceryl Stearate, 202 (arachidyl and behenyl alcohols and arachidyl glucoside; SEPPIC, Paris, France), and aminopropyl dimethicone. Mix vigorously for 30 minutes at 80-85°C. After 30 minutes, the heat was turned off, the mixing speed was reduced, and the composition was allowed to cool slowly. In the secondary phase, 15.5% by weight (of the final total weight % of the composition) of deionized water was added, and the following ingredients were slowly added and mixed until hydrated: PVMMA copolymer ( S-97BF; ISPCorp., Wayne, NJ, USA) and sodium hydroxide (20% active ingredient). The solution will thicken slightly. The in-process pH should be 6.90-7.00. Heat the secondary phase to 50-55°C. Slowly add Polyquaternium-28 ( NT-20; ISPCorp.). The solution will turn opaque and become less viscous. The secondary phase was cooled and 0.05% by weight (of the final total weight % of the composition) of DMDM hydantoin was added at < 45°C. Slowly add the minor phase to the major phase at < 45°C. Add at 45°C or lower 2001 (Polyquaternium-47; Nalco, Naperville, IL, USA). Premix D5/Dimethiconol and Dimethicone and then add to the combined Major and Secondary phases. Then add the following ingredients: DC-8500 (bis(C13-15 alkoxy) PG-amodimethicone, DowComing, Midland, MI, USA), propylene glycol, fragrance and (composition final total weight %) 0.15% by weight of DMDM hydantoin.

Example 6

This example illustrates the repair of split-ends of hair fibers using the test method of the present invention.

The compositions used in this study, which are shown in Figure 1, are compared below. Adjust with sodium hydroxide/aspartic acid to obtain proper pH if necessary.

Compositions 6A-6D

The compositions used in this study are compared below, as shown in Figure 2. if necessary,

Adjust with sodium hydroxide/citric acid/aspartic acid to obtain proper pH.

Compositions 6E-6J

Figure 1 shows the results of conditioner restoration when twice bleached European hair with mechanically fabricated split-ends was used. The results show that about 80% repair was obtained in three cycles with the rinse-off conditioner.

Figure 2 shows the results for various compositions when using twice bleached European hair with mechanically produced split-ends. This result is based on the assumption that all formulations were leave-on formulations including overnight repair. The results show that all leave-on compositions repaired greater than 80% in one treatment.

Example 7

This example illustrates the repair of split-ends of hair fibers using the test method of the present invention.

The compositions used in this study are compared below. Adjust with sodium hydroxide/aspartic acid to obtain proper pH if necessary.

Compositions 7A-7D

Target Spec 7A:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 5,000-15,000 centipoise

Color: White (MS)

Smell: MS

Appearance: Opaque emulsion

Target Spec 7B:

pH: 5.5-6.5

Viscosity (LVT/spindle 4/30rpm/1min, 25°C): 15,000-20,000 centipoise

Color: White/Beige (MS)

Smell: MS

Appearance: Viscous, opaque emulsion

Target Spec 7C:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 15,000-25,000 centipoise

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque emulsion

Target Spec 7D:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 10,000-20,000 centipoise

Color: White (MS)

Smell: MS

Appearance: Opaque emulsion

Fifty hair fibers containing split ends were removed from the tress. The hair fiber samples were placed on a glass slide, aligned along a strip of double-sided tape for optical imaging. Prior to product application, each selected fiber with a split-end was imaged individually using a WILD stereomicroscope at approximately 25X magnification with transmitted light emission, and the image was stored. The fiber was also rotated prior to image capture to ensure the split-end was in view.

Follow the product application schedule outlined below. In each case, 50 selected fibers with split ends were each arranged in five different tresses, and the product was then applied. Optical images of the tip of each selected fiber were again obtained to examine and assess the extent of split-end repair. The results are shown in Table 12.

Table 12 shows a summary of the split-end data study comparing the total number of split-ends before treatment (50) to the number of repaired split-ends after treatment. (split-ends for replicate studies (category 6) were prepared by a separate method).

Table 12

All categories showed the ability to repair split ends in hair fibers, with three of them showing an improvement of 90% or greater.

Product application plan

Protocols are listed in the order shown in Table 12. For some compositions (noted below), the drying time was varied from 5 minutes to 20 minutes by the characteristics of the hair dryer (gentle air flow) in order to obtain 80% dry strands.

A. Pre-wash hair

1. Wash wax bound bleached silver (2X) hair by soaking in 5% w/w sodium lauryl ether sulfate (1M) solution. The solution to hair ratio was 40:1. Soak at room temperature for 30 minutes, and then massage the hair by hand for 3 minutes, then rinse with tap water at 40°C until all foam is rinsed off.

2. Blot dry hair with tissue or towel, comb straight, and allow the hair to dry overnight at ambient room temperature.

B. Mechanical generation of split ends

1. The bundle is sampled by International Hair Importers in a manner linear in the density of the hair. Five 1.5" wide tresses were prepared, cut and tied so that each tress had 6 g of hair.

2. Attach each tress to a repeat comber and comb the tress 1500 times on each side for a total of 3000 combs per tress.

3. During the combing process, the blow dryer was held 8 inches from the tresses and turned on the high heat setting. Directing the air flow towards the base of the tresses causes the hair to be pushed towards the comb during repeated brushing cycles.

C. Select split ends from hair strands and acquire initial images

1. Using a magnifying glass, examine the ends of the tresses to find hair fibers with split ends. Fifty fibers with split ends were selected and removed by root from the tress. 10 split-end fibers were selected from each tress so that 50 fibers could be pulled from five tresses.

2. Use a metal crimp to crimp the fibers at the tip, then line up the crimps to be placed on the tape so that there are 10 fibers on each tape. Use another tape to cover the curls so they can be easily lifted together.

3. Number all 50 fibers and collect optical images of 10 of the 50 hair fibers for before and after comparison photos.

4. Using a red permanent marker, mark each of the 50 selected fibers up to the start of the split.

5. Acquire optical images of 10 split-ends by mounting the split-ends on a glass slide. Images were acquired at 50× magnification using a stereomicroscope emitting transmitted light from beneath the stage of the microscope.

6. Use the stereomicroscope to examine the other 40 fibers with split ends, but they do not need to be photographed.

7. A strip of tape containing split ends is placed in the middle of the 1.5" tress.

8. Use large clips, such as binder clips, to hold tresses with split-ended fibers.

D. Composition Application - Category 1

1. Wet tresses in 35-40°C water at 1 GPM for 30 seconds.

2. Apply 1.5 ml of non-conditioning shampoo to 1.5 inch tresses and massage for 1 minute.

3. Rinse the tresses in 35-40°C water at 1 GPM for 30 seconds.

4. Lime off excess water by sliding hair tress between fingers.

5. Attach the top of the tress to the stand for drying.

6. Use bobby pins to pinch the strands 3/4 of the way down the length to avoid hair migration.

7. Blow dry the tresses on medium heat with a dryer 2 feet away from the tresses for about 3 minutes.

8. Apply 1.5 ml of Composition 7A (Leave-in Treatment) evenly to both sides of a 1.5 inch damp tress. Massage in primarily on ends and split-end prone areas for 1 minute.

9. Comb once on each side of the tresses.

10. Attach the top of the tress to the stand for drying.

11. Clip the tress 3/4 of its length with bobby pins to avoid hair migration.

12. Blow dry the tress on medium heat (gentle air stream) 2 feet away from the tress for about 20 minutes until it is 80% dry.

13. After blow drying, comb through the tresses once on each side.

D. Composition Application - Category 2

1. Wet tresses in 35-40°C water at 1 GPM for 30 seconds.

2. Apply 1.5 ml of Composition 7B (shampoo) to a 1.5 inch tress and massage for 1 minute.

3. Rinse tresses in 35-40°C water at 1 GPM for 30 seconds.

4. Wring out excess water by sliding hair strands between fingers.

5. Apply 1.5 ml of Composition 7C (Conditioner) to a 1.5 inch tress and tap the tress 9 times from top to bottom and allow to sit for 1 minute.

6. Rinse the tresses in 35-40°C water at 1 GPM for 30 seconds.

7. Gently blot dry strands with KimWipes.

8. Attach the top of the tress to the stand for drying.

9. Use bobby pins to pinch the tress 3/4 of its length to avoid hair migration.

10. Blow dry the tresses on medium heat for about 3 minutes with a dryer 2 feet away from the tresses.

11. Apply 1.5 ml of Composition 7A (Leave-in Treatment) to 1.5 feet of damp tresses. Massage in primarily on ends and split-end prone areas for 1 minute.

12. Comb once on each side of the tress.

13. Attach the top of the tress to the stand for drying.

14. Use bobby pins to pinch the tress 3/4 of its length to avoid hair migration.

15. Blow dry the tress on medium heat (gentle air stream) 2 feet away from the tress for about 20 minutes until it is 80% dry.

16. After blow drying, comb through the tresses twice on each side.

D. Composition Application - Category 3

1. Wet tresses in 35-40°C water at 1 GPM for 30 seconds.

2. Apply 1.5 ml of non-conditioning shampoo to 1.5 inch tresses and massage for 1 minute.

3. Rinse the tresses in 35-40°C water at 1 GPM for 30 seconds.

4. Wring out excess water by sliding hair strands between fingers.

5. Attach the top of the tress to the stand for drying.

6. Use bobby pins to pinch the strands 3/4 of the way down the length to avoid hair migration.

7. Blow dry the tresses on medium heat for about 3 minutes with a dryer 2 feet away from the tresses.

8. Apply 1.5 ml of Composition 7D (overnight treatment) to both sides of a 1.5 foot damp tress. Massage in primarily on ends and split-end prone areas for 1 minute.

9. Comb once on each side of the tresses.

10. Since this is an overnight treatment, leave the composition on the hair for 8 hours.

11. Use bobby pins to pinch the tress 3/4 of its length to avoid hair migration.

D. Composition Application - Category 4

1. Wet tresses in 35-40°C water at 1 GPM for 30 seconds.

2. Apply 1.5 ml of non-conditioning shampoo to 1.5 inch tresses and massage for 1 minute.

3. Rinse the tresses in 35-40°C water at 1 GPM for 30 seconds.

4. Wring out excess water by sliding hair strands between fingers.

5. Apply 1.5 ml of Composition 7C to a 1.5 inch tress and tap the tress 9 times from top to bottom and allow to sit for 1 minute.

6. Rinse the tresses in 35-40°C water at 1 GPM for 30 seconds.

7. Gently blot dry strands with KimWipes.

8. Attach the top of the tress to the stand for drying.

9. Use bobby pins to pinch the tress 3/4 of its length to avoid hair migration.

10. Blow dry the tress on medium heat with a dryer 2 feet away from the tress for about 5 minutes until it is 80% dry.

11. Comb through the tresses twice on each side.

12. Apply red marker again on fiber after blow drying.

13. Repeat steps 1-12 again for an additional 2 cycles for a total of three treatments.

D. Composition Application - Category 5

1. Wet tresses in 35-40°C water at 1 GPM for 30 seconds.

2. Apply 1.5 ml of Composition 7B (shampoo) to a 1.5 inch tress and massage for 1 minute.

3. Rinse the tresses in 35-40°C water at 1 GPM for 30 seconds.

4. Wring out excess water by sliding hair strands between fingers.

5. Apply 1.5 ml of Composition 7C (Conditioner) to a 1.5 inch tress and tap the tress 9 times from top to bottom and allow to sit for 1 minute.

6. Rinse the tresses in 35-40°C water at 1 GPM for 30 seconds.

7. Gently blot dry strands with KimWipes.

8. Comb through the tresses once on each side.

9. Attach the top of the tress to the stand for drying.

10. Use bobby pins to pinch the tress 3/4 of its length to avoid hair migration.

11. Blow dry the tress on medium heat (gentle air stream) 2 feet away from the tress for about 20 minutes until it is 80% dry.

12. Comb twice on each side.

13. Repeat steps 1-12 again for an additional two cycles for a total of three treatments.

E. Select the split ends from the hair bundle and capture the final image

1. Remove the strip containing the split ends from the middle of the 1.5" tress.

2. Using a stereomicroscope, take processed optical images of 10 hair fibers with split-ends by mounting the split-ends on a glass slide.

3. Examine the other 40 fibers with split ends using a stereomicroscope.

4. Count the number of fibers that have been repaired to determine % Repair.

Example 8

This example illustrates a method of communicating split-end repair status to consumers.

Figure 3 is a schematic diagram showing the use of polyelectrolyte complexes (PECs) to repair split ends. A possible mechanism of action for PECs is shown here, in which they attach to the site of the split-ends, form a network with themselves and assemble with the fibers, and shrink as they dry, thereby bonding the split-ends from within.

4A-4D show still images of repairing various types of split-ends with the compositions described herein using the methods described herein.

Figure 5 shows a still frame from a video of a split-end being repaired by the process of the repair method described herein.

Example 9

This example illustrates other compositions of the invention.

Composition 9A

Target Spec 9A:

pH: 6.0-7.0

Viscosity (RVT-C, 5rpm, 1 minute, 25°C): 40,000-80,000

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque (cloudy) gel

Compositions 9B-1 and 9B-2

Target Spec 9B:

Composition 9C-1

Target Specification 9C-1:

pH: 4.0-5.0

Colour: cloudy/pale

Smell: Matching Reference

Appearance: milky liquid

Composition 9C-2

Target Spec 9C:

pH: 4.5-6

color: White

Smell: Matching Reference

Appearance: milky liquid

Compositions 9D-1 and 9D-2

Target Spec 9D:

ontology

Color: Beige (MS)

Smell: MS

Appearance: cloudy liquid

pH: 5.0-6.5

Specific gravity: ^* 0.986

Non-volatile content: 4.4-4.9%

(T=4.66)

finished product

Color: White (MS)

Smell: MS

Appearance: dense foam, non-watery, not runny

pH: 5.0-6.5

Foam stability: 200 seconds minutes

Foam density: ^* 0.039g/mL

Specific gravity: ^* 0.941

4.3-4.8%

Non-volatile components: (T=4.58)

^* for reference

Composition 9E

Target Spec 9E:

pH: 6.0-7.0

Viscosity (RVT-C, 5rpm, 1 minute, 25°C): 40,000-80,000

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque (cloudy) gel

Compositions 9F-1 to 9F-4

Target Spec 9F:

pH: 7.00-7.50

Viscosity (RVT-C, 5rpm, 1 minute, 25°C): 50,000-100,000cps

Color: Transparent - Matte White

Smell: MS

Appearance: thick gel

Compositions 9G-1 to 9G-4

Target Spec 9G:

pH: 5.00-6.50

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 20,000-40,000cps

Color: Translucent White (MS)

Smell: MS

Appearance: Viscous, opaque gel

Compositions 9H-1 to 9H-2

Target Specification 9H:

pH: 5.00-6.50

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 5,000-15,000cps

Color: Translucent White (MS)

Smell: MS

Appearance: viscous, milky liquid

Compositions 9I-1 to 9I-3

Target Specification 9I:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 20,000-30,000cps

Color: White (MS)

Smell: MS

Appearance: viscous, opaque emulsion

Compositions 9J-1 to 9J-3

Target Specification 9J:

pH: 7.0-8.0

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 5,000-15,000cps

Color: colorless - pale yellow

Smell: MS

Appearance: Slightly cloudy oily liquid

Compositions 9K-1 to 9K-3

Target Spec 9K:

pH: 7.0-8.0

Viscosity (RVT-C, 10rpm, 1 minute, 25°C): 50,000-100,000cps

Color: transparent - matte white

Smell: MS

Appearance: thick gel-thin liquid

Composition 9L

Target specification 9L:

pH: 3.20-4.50

Penetration (50g weight w/cone): 18-24mm

Color: colorless

Smell: MS

Appearance: thick gel

Composition 9M

Element weight% main phase Deionized water 31.2837 PVM/MA Copolymer (Gantrez S-97BF(ISP)) 0.001 Sodium hydroxide, 20% 0.00125 Add the following ingredients and mix vigorously Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active ingredient) 0.045 Slowly add the following ingredients, mixing until hydrated Polyquaternium 10 0.8 Heat to 50°C and mix until clear Disodium EDTA 0.1 Cocamidopropyl Betaine (about 30% active ingredients), water, sodium chloride 8.2 NaOH, 20% 0.14875 Sodium Laureth Sulfate - 1 Mole (25%) 32 Disodium Laureth Sulfosuccinate (approx. 34% active ingredients) 12.8

Styrene/VP Copolymer (40%), Water 0.75 PEG-6 caprylic/capric triglycerides 0.6 Kathon CG 0.07 Fragrance 0.7 Coconut Palm (Coconut) Oil 0.0001 Keratin Amino Acids 0.0001 flower/leaf extract 0.0001 Premix the following components and add to the batch Deionized water 10 Sodium chloride 2.5

Target Specification 9M:

pH: 5.5-6.5

Viscosity (LVT/rotor 4/30rpm/1min, 25°C): 15,000-20,000cps

Color: White/Beige (MS)

Smell: MS

Appearance: viscous, opaque liquid

Compositions 9N-1 and 9N-2

Target Spec 9N:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 15,000-25,000cps

Color: White (MS)

Smell: MS

Appearance: viscous, opaque emulsion

Composition 9O

Target Specification 9O:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 5,000-15,000cps

Color: White (MS)

Smell: MS

Appearance: opaque emulsion

Composition 9P

Target Spec 9P:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C): 10,000-20,000cps

Color: White (MS)

Smell: MS

Appearance: opaque emulsion

Composition 9Q

Element weight% main phase Deionized water 52.8

Disodium EDTA 0.05 L-Aspartic Acid 0.75 Add the following one at a time at 80-85°C and mix until melted/homogeneous stearamidopropyl dimethylamine 2 cetyl alcohol 1 Glyceryl Stearate 0.2 Aminopropyl Dimethicone 0.5 Mix vigorously for 30 minutes at 80-85°C Slow down the mixing speed and allow to cool deputy phase Deionized water 15.5 Slowly add the following ingredients, mixing until hydrated PVM/MA Copolymer (Gantrez S-97BF(ISP)) 0.2 Sodium Hydroxide (20% active ingredient) 0.25 (solution will thicken slightly) In-process pH regulation: 6.90-7.00 Heat the secondary phase to 50-55°C Slowly add the following ingredients with very vigorous mixing Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active ingredient) 9 (solution will become opaque and less viscous) Add the following components at ≤45°C DMDM hydantoin 0.05 Slowly add the secondary phase to the primary phase at ≤45°C ＜45℃ premix the next two DS, polydimethylsiloxane 2 Polydimethylsiloxane (60,000cst) 1 DC-8500 1 Propylene Glycol 10

Fragrance 0.5 DMDM hydantoin 0.2 Salcare SC-96 3

Target Spec 9Q:

pH: 4.50-6.00

Viscosity (RVT-8, 10rpm, 1 minute, 25°C):

Bulk viscosity: 7,000-15,0000cps

Color: White (MS)

Smell: MS

Appearance: opaque emulsion

Composition 9R

Element weight% main phase Deionized water 40.55 Slowly add the following ingredients, mixing until hydrated PVM/MA Copolymer (Gantrez S-97BF(ISP)) 0.2 Sodium Hydroxide (20% active ingredient) 0.25 (solution will thicken slightly) In-process pH regulation: 6.90-7.00 Heat to 50-55°C Slowly add the following ingredients with very vigorous mixing Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active ingredient) 9 (solution will become opaque and less viscous) Start heating to 80-85°C Add the following components one at a time, mixing until completely dissolved Disodium EDTA 0.05 L-Aspartic Acid 0.75 Deionized water 20.27

Add the following components one at a time at 80-85°C and mix until melted/homogeneous stearamidopropyl dimethylamine 2 cetyl alcohol 4 "Montanov 202" 1.18 Glyceryl Stearate 0.80 "Crodamol STS" (benzyl ether myristate) 2 Salcare SC-96 1 Aminopropyl Dimethicone 0.75 Mix vigorously for 30 minutes at 80-85°C Slow down the mixing speed and allow to cool ＜45℃ premix the next two DS, polydimethylsiloxane 3 Polydimethylsiloxane 1.5 DC 2-8566 (Amodimethicone) 2 Propylene Glycol 10 Fragrance 0.5 DMDM hydantoin 0.2

Target Spec 9R:

pH: 4.50-6.00

Viscosity (RVT-8, 10rpm, 1 minute,

25°C):

Bulk viscosity: 15,000-25,000cps

Color: White (MS)

Smell: MS

Appearance: opaque emulsion

Compositions 9S-1 to 9S-6

Target specification 9S (also for composition 6J):

Composition 9T

Element weight%

main phase Deionized water 40.55 Slowly add the following ingredients, mixing until hydrated PVM/MA Copolymer (Gantrez S-97BF(ISP)) 0.2 Sodium Hydroxide (20% active ingredient) 0.25 (solution will thicken slightly) In-process pH regulation: 6.90-7.00 Record pH: 6.95 Heat to 50-55°C Slowly add the following ingredients with very vigorous mixing Polyquaternium-28 (Conditioneze NT-20(ISP)) 9 (solution will become opaque and less viscous) Deionized water 39.05 Disodium EDTA 0.05 Salcare SC-96 3 mix until homogeneous ＜45℃ Polydimethylsiloxane (DC-200, 20cst) 3 Phenyltrimethicone (DC-556) 2 Cyclopentasiloxane, Dimethicone 1 glycerin 1 Propylene Glycol 0.5 Fragrance 0.2 DMDM hydantoin 0.2

Target Spec 9T:

pH: 5.00-6.50

Viscosity (RVT-B, 10rpm, 1 minute, 25°C)

Bulk viscosity: 7,000-15,000cps

Color: Translucent White (MS)

Smell: MS

Appearance: Viscous, milky fluid

Composition 9U

Element weight% main phase Deionized water 60.85 Disodium EDTA 0.05 L-Aspartic Acid 0.75 Add the following components one at a time at 80-85°C and mix until melted/homogeneous stearamidopropyl dimethylamine 2 cetyl alcohol 1 Glyceryl Stearate 0.2 Mix vigorously for 30 minutes at 80-85°C Reduce mixing speed; allow to cool and reduce foam deputy phase Deionized water 15.50 Slowly add the following ingredients; mix until hydrated PVM/MA Copolymer (Gantrez S-97BF(ISP)) 0.2 Sodium Hydroxide (20% active ingredient) 0.25 (solution will thicken slightly) In-process pH regulation: 6.90-7.00 Heat the secondary phase to 50-55°C Slowly add the following ingredients with very vigorous mixing Polyquaternium-28 (Conditioneze NT-20(ISP)) 9 (solution will become opaque and less viscous) (Mix ~ 10 minutes) Add the following components at ≤45°C DMDM hydantoin 0.05

Slowly add the secondary phase to the primary phase at ≤45°C ＜45℃ Silicone Premix Polydimethylsiloxane (60,000cst) 2 Phenyl trimethicone (DC-556) 2 DS, polydimethylsiloxane (DC-1501) 1 glycerin 1 Propylene Glycol 0.5 Fragrance 0.5 DMDM hydantoin 0.15 Salcare SC-96 3

Target Specification 9U:

pH: 4.5-6.50

Viscosity (RVT-B, 10rpm, 1 minute, 25°C)

Bulk viscosity: 8,000-16,000cps

Color: White (MS)

Smell: MS

Appearance: opaque emulsion

Compositions 9V-1 to 9V-3

Target Spec 9V:

pH: 6.5-7.5

Viscosity (RVT-C, 5rpm, 1 minute, 25°C):

Volume: 40,000-90,000

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque gel

Compositions 9W-1 to 9W-3

Target specification 9W:

pH: 4.5-6.00

Viscosity (RVT-8, 10rpm, 1 minute, 25°C): 15,000-25,000cps

Color: White (MS)

Smell: MS

Appearance: viscous, opaque emulsion

Compositions 9X-1 and 9X-2

Target Spec 9X:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1 minute, 25°C):

Bulk viscosity: 7,000-15,000cps

w/shear viscosity (finished product): 20,000-35,000cps

Color: White (MS)

Smell: MS

Appearance: viscous, opaque emulsion

Example 10

This example illustrates exemplary addition rates, addition times, temperatures, mixing speeds, and mixing times for preparing PEC.

- Water Density: Perry's Chemical Engineer's Handbook.

- NaOH 20% Density = 1.2191 kg/L and Conditioneze Density = 1.042 kg/L.

One 270-kg batch

PEC compound in 113 liter/30 gal premix vessel with center turbine agitator only

Main batch in 227l/60gal mixing vessel with center turbine and side sweep agitator

Processing parameters of PEC compound:

Initial water loading = 42.02L (41.85kg)

Addition rate = 28L/min (28kg/min)

Total addition time = 1.5min

Initial water temperature = 29°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

PVM/MA copolymer (GantrezS-97BF) = 0.54kg (solid)

Addition rate = 0.6kg/min

Total addition time = 1min

Temperature = 30°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Dispersion and mixing time = 30min

Sodium hydroxide, 20% = 0.55L (0.675kg)

Addition rate = 0.6L/min (0.7kg/min)

Total addition time = 1min

Temperature = 30°C

Center Turbo Agitator = Slow (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Hydration mixing time = 20min

In-Process pH Check = 6.90

Heat the premix for 10 minutes to 51°C

Polyquaternium 28 (ConditionezeNT-20) ＝23.32L (24.30kg)

Addition rate = 3.33L/min (3.47kg/min)

Total addition time = 7min

Temperature = 49°C

Center Turbo Agitator = Moderate/Strong (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Compound mixing time = 40min

premix cooling

Cool to 29°C

Center turbine agitator = very slow (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Cooling and mixing time = 60min ^*

( ^* Note: Mixing time reflects the time required to bring the main batch to the point of addition of the PEC premix)

One 11,800-kg batch

PEC compound in 5,678 liter / 1,500 gallon premix vessel with center turbine and side sweep agitator

Main batch in M0112, 113 liter / 3,200 gal mixing vessel with center turbine and side sweep agitator

Processing parameters of PEC compound:

Initial water loading = 1840.9L (1835kg)

Addition rate = 526L/min (524kg/min)

Total addition time = 3.5min

Temperature = 26°C

Central turbine agitator = 25RPM counterclockwise

Side sweep agitator = 7RPM clockwise

PVM/MA copolymer (GantrezS-97BF) = 23.6kg (solid)

Addition rate = 7.87kg/min

Total addition time = 3min

Temperature = 27°C

Central turbine agitator = 20RPM counterclockwise

Side sweep agitator = 7RPM clockwise

Dispersion mixing time = 30min

Sodium hydroxide, 20% = 24.2L (29.5kg)

Addition rate = 12.1L/min (14.75kg/min)

Total addition time = 2min

Temperature = 27°C

Central turbine agitator = 20RPM counterclockwise

Side sweep agitator = 7RPM clockwise

Hydration mixing time = 10min

In-process pH check = 6.72. An additional 118 grams (0.001 wt %) of NaOH was added and pH = 6.80. An additional 118 grams (0.001 wt %) of NaOH was added and pH = 6.90. A total of 29.736kg of NaOH

Heat the premix for 18 minutes to 55°C

Polyquaternium 28 (ConditionezeNT-20) = 1019L (1062kg)

Addition rate = 29.1L/min (30.0kg/min)

Total addition time = 35min

Temperature = 54°C

Central turbine agitator = 28RPM counterclockwise

Side sweep agitator = 7RPM clockwise

Compound mixing time = 30min

premix cooling

Cool to 35°C

Central turbine agitator = 18RPM counterclockwise

Side sweep agitator = 7RPM clockwise

Cooling and mixing time = 240min ^*

( ^* Note: Mixing time reflects the time required to bring the main batch to the point of addition of the PEC premix)

One 270-kg batch

PEC compound in 113 liter/30 gal premix vessel with center turbine agitator only

Main batch in 227l/60gal mixing vessel with center turbine and side sweep agitator

Processing parameters of PEC compound:

Initial water filling volume = 42.04L (41.84kg)

Addition rate = 28L/min (28kg/min)

Total addition time = 1.5min

Initial water temperature = 31°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep agitator = not included in pilot mixing vessel

Heat the premix for 10 minutes to 52°C

PVM/MA copolymer (GantrezS-97BF) = 0.54kg (solid)

Addition rate = 0.6kg/min

Total addition time = 1min

Temperature = 52°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Dispersion mixing time = 25min

Sodium hydroxide, 20% = 0.56L (0.688kg)

Addition rate = 0.6L/min (0.7kg/min)

Total addition time = 1min

Temperature = 52°C

Center Turbo Agitator = Slow (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Hydration mixing time = 15min

In-Process pH Check = 6.93

Polyquaternium 28 (ConditionezeNT-20) ＝23.32L (24.30kg)

Addition rate = 4.66L/min (4.86kg/min)

Total addition time = 5min

Temperature = 53°C

Center Turbo Agitator = Moderate/Strong (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Compound mixing time = 40min

premix cooling

Cool to 29°C

Center turbine agitator = very slow (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Cooling and mixing time = 100min ^*

( ^* Note: Mixing time reflects the time required to bring the main batch to the point of addition of the PEC premix)

One 270-kg batch

PEC compound in 113 liter/30 gal premix vessel with center turbine agitator only

Main batch in 227l/60gal mixing vessel with center turbine and side sweep agitator

PEC compound processing parameters:

Initial water filling volume = 42.03L (41.85kg)

Addition rate = 28L/min (28kg/min)

Total addition time = 1.5min

Initial water temperature = 30°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

PVM/MA copolymer (GantrezS-97BF) = 0.54kg (solid)

Addition rate = 0.6kg/min

Total addition time = 1min

Temperature = 30°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Dispersion mixing time = 30min

Sodium hydroxide, 20% = 0.56L (0.68kg)

Addition rate = 0.6L/min (0.7kg/min)

Total addition time = 1min

Temperature = 31°C

Center Turbo Agitator = Slow (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Hydration mixing time = 6min

In-progress pH check = initial 6.83. An additional 2.7 grams (0.001 wt %) of NaOH was added and pH = 6.95. Total 682.7g NaOH

Heat the premix for 10 minutes to 57°C

Polyquaternium 28 (ConditionezeNT-20) ＝23.32L (24.30kg)

Addition rate = 3.33L/min (3.47kg/min)

Total addition time = 7min

Temperature = 56°C

Center Turbo Agitator = Moderate/Strong (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Compound mixing time = 30min

premix cooling

Cool to 27°C

Center turbine agitator = very slow (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Cooling and mixing time = 120min ^*

( ^* Note: Mixing time reflects the time required to bring the main batch to the point of addition of the PEC premix)

One 1,250-kg batch

PEC compound in 379 liter/100 gallon premix vessel with center turbine and side sweep agitator

Main batch in 1,893 liter / 500 gal mixing vessel with center turbine and side sweep agitator

Processing parameters of PEC compound:

Initial water loading = 195.2L (194.4kg)

Addition rate = 97.6L/min (97.2kg/min)

Total addition time = 2min

Initial water temperature = 29°C

Central turbine agitator = 60RPM counterclockwise

Side sweep agitator = 10RPM clockwise

PVM/MA copolymer (GantrezS-97BF) = 2.5kg (solid)

Addition rate = 1.3kg/min

Total addition time = 2min

Temperature = 31°C

Central turbine agitator = 60RPM counterclockwise

Side sweep agitator = 10RPM clockwise

Dispersion mixing time = 26min

Sodium hydroxide, 20% = 2.56L (3.125kg)

Addition rate = 3L/min (4kg/min)

Total addition time = 1min

Temperature = 33°C

Central turbine agitator = 20RPM counterclockwise

Side sweep agitator = 10RPM clockwise

Hydration mixing time = 11min

In-Process pH Check = 6.90

Heat the premix for 10 minutes to 52°C

Polyquaternium 28 (ConditionezeNT-20) ＝108.0L (112.5kg)

Addition rate = 9.0L/min (9.4kg/min)

Total addition time = 12min

Temperature = 54°C

Central turbine agitator = 58RPM counterclockwise

Side sweep agitator = 15RPM clockwise

Compound mixing time = 31min

premix cooling

Cool to 35°C

Central turbine agitator = 18RPM counterclockwise

Side sweep agitator = 8RPM clockwise

Cooling and mixing time = 135min ^*

( ^* Note: Mixing time reflects the time required to bring the main batch to the point of addition of the PEC premix)

One 270-kg batch

PEC compound in 113 liter/30 gal premix vessel with center turbine agitator only

Main batch in 227l/60gal mixing vessel with center turbine and side sweep agitator

Processing parameters of PEC compound:

Initial water filling volume = 42.01L (41.84kg)

Addition rate = 28L/min (28kg/min)

Total addition time = 1.5min

Initial water temperature = 29°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Heat the premix for 10 minutes to 52°C

PVM/MA copolymer (GantrezS-97BF) = 0.54kg (solid)

Addition rate = 0.6kg/min

Total addition time = 1min

Temperature = 52°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Dispersion mixing time = 25min

Sodium hydroxide, 20% = 0.57L (0.69kg)

Addition rate = 0.6L/min (0.7kg/min)

Total addition time = 1min

Temperature = 53°C

Center Turbo Agitator = Slow (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Hydration mixing time = 5min

pH check in process = 6.95

Polyquaternium 28 (ConditionezeNT-20) ＝23.32L (24.30kg)

Addition rate = 4.66L/min (4.86kg/min)

Total addition time = 5min

Temperature = 53°C

Center Turbo Agitator = Moderate/Strong (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Compound mixing time = 35min

premix cooling

Cool to 30°C

Center turbine agitator = very slow (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Cooling and mixing time = 90min ^*

( ^* Note: Mixing time reflects the time required to bring the main batch to the point of addition of the PEC premix)

One 270-kg batch

PEC compound in 113 liter/30 gal premix vessel with center turbine agitator only

Main batch in 227l/60gal mixing vessel with center turbine and side sweep agitator

Processing parameters of PEC compound:

Initial water filling volume = 42.01L (41.84kg)

Addition rate = 28L/min (28kg/min)

Total addition time = 1.5min

Initial water temperature = 29°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

PVM/MA copolymer (GantrezS-97BF) = 0.54kg (solid)

Addition rate = 0.6kg/min

Total addition time = 1min

Temperature = 30°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Dispersion mixing time = 30min

Sodium hydroxide, 20% = 0.56L (0.68kg)

Addition rate = 0.6L/min (0.7kg/min)

Total addition time = 1min

Temperature = 30°C

Center Turbo Agitator = Slow (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Hydration mixing time = 20min

In-progress pH check = initial 6.81. An additional 3.4 grams (0.00126 wt %) of NaOH was added and pH = 6.92. Total 683.4g NaOH

Heat the premix for 10 minutes to 54°C

Polyquaternium 28 (ConditionezeNT-20) ＝23.32L (24.30kg)

Addition rate = 3.33L/min (3.47kg/min)

Total addition time = 7min

Temperature = 54°C

Center Turbo Agitator = Moderate/Strong (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Compound mixing time = 35min

premix cooling

Cool to 35°C

Center turbine agitator = very slow (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Cooling and mixing time = 260min ^*

( ^* Note: Mixing time reflects the time required to bring the main batch to the point of addition of the PEC premix)

A 3,772-kg batch

PEC compound in 1,893 liter/500 gallon premix vessel with center turbine and side sweep agitator

Main batch in 3,785 L/1000 gal mixing vessel with center turbine and side sweep agitator

Processing parameters of PEC compound:

Initial water filling amount = 588.93L (586.546kg)

Addition rate = 392.6L/min (391kg/min)

Total addition time = 1.5min

Initial water temperature = 29°C

Central turbine agitator = 46RPM counterclockwise

Side sweep agitator = 10RPM clockwise

PVM/MA copolymer (GantrezS-97BF) = 7.544kg (solid)

Addition rate = 3.77kg/min

Total addition time = 2min

Temperature = 29°C

Central turbine agitator = 46RPM counterclockwise

Side sweep agitator = 10RPM clockwise

Dispersion mixing time = 60min

Sodium hydroxide, 20% = 7.735L (9.430kg)

Addition rate = 3.9L/min (4.7kg/min)

Total addition time = 2min

Temperature = 30°C

Central turbine agitator = 25RPM counterclockwise

Side sweep agitator = 10RPM clockwise

Hydration mixing time = 10min

In-Process pH Check = 6.91

Heat the premix for 10 minutes to 52°C

Polyquaternium 28 (ConditionezeNT-20) ＝325.80L (339.48kg)

Addition rate = 16.3L/min (17.0kg/min)

Total addition time = 20min

Temperature = 50°C

Central turbine agitator = 35RPM counterclockwise

Side sweep agitator = 6RPM clockwise

Compound mixing time = 40min

premix cooling

Cool to 40°C

Center turbine agitator = 14RPM counterclockwise

Side sweep agitator = 6RPM clockwise

Cooling and mixing time = 55min ^*

( ^* Note: Mixing time reflects the time required to bring the main batch to the point of addition of the PEC premix)

One 270-kg batch

PEC compound in 113 liter/30 gal premix vessel with center turbine agitator only

Main batch in 227l/60gal mixing vessel with center turbine and side sweep agitator

Processing parameters of PEC compound:

Initial water filling volume = 42.01L (41.84kg)

Addition rate = 28L/min (28kg/min)

Total addition time = 1.5min

Initial water temperature = 29°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Heat the premix for 10 minutes to 52°C

PVM/MA copolymer (GantrezS-97BF) = 0.54kg (solid)

Addition rate = 0.6kg/min

Total addition time = 1min

Temperature = 52°C

Center Turbo Agitator = moderate (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Dispersion mixing time = 20min

Sodium hydroxide, 20% = 0.57L (0.69kg)

Addition rate = 0.6L/min (0.7kg/min)

Total addition time = 1min

Temperature = 53°C

Center Turbo Agitator = Slow (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Hydration mixing time = 6min

In-Process pH Check = 6.98

Polyquaternium 28 (ConditionezeNT-20) ＝23.32L (24.30kg)

Addition rate = 4.66L/min (4.86kg/min)

Total addition time = 5min

Temperature = 53°C

Center Turbo Agitator = Moderate/Strong (RPM) Clockwise

Side sweep mixer = not included in pilot premix vessel

Compound mixing time = 35min

premix cooling

Cool to 29°C

Center turbine agitator = very slow (RPM) clockwise

Side sweep mixer = not included in pilot premix vessel

Cooling and mixing time = 100min ^*

( ^* Note: Mixing time reflects the time required to bring the main batch to the point of addition of the PEC premix)

Example 11

This example describes exemplary compositions of the invention (Compositions 11A-11G).

The hair restoration efficacy of certain of these compositions (along with Composition 1C) is summarized in Tables 13 and 14. The high humidity curl retention for some of these compositions is shown in FIG. 7 .

Composition 11A

Target Spec 11A:

pH: 5.00-6.50

Viscosity (RVT-B, 10rpm, 1min, 25°C): 20,000-40,000cps

Color: Matt White (MS)

Smell: MS

Appearance: Viscous, opaque gel

Composition 11B

Target Specification 11B:

pH: 6.0-7.5

Viscosity (RVT-C, 5rpm, 1min, 25℃): 50,000-100,000cps

Color: matte white

Smell: MS

Appearance: thick gel

Composition 11C

Target Spec 11C:

pH: 5.00-6.50

Viscosity (RVT-B, 10rpm, 1min, 25°C): 5,000-15,000cps

Color: Translucent White (MS)

Smell: MS

Appearance: viscous, milky liquid

Composition 11D

Target Spec 11D:

pH: 4.50-6.00

Viscosity (RVT-B, 10rpm, 1min, 25°C): 20,000-30,000cps

Color: White (MS)

Smell: MS

Appearance: Viscous opaque emulsion

Composition 11E

Target Spec 11E:

pH: 6.5-7.5

Viscosity (RVT-B, 10rpm, 1min, 25°C): 5,000-15,000cps

Color: colorless - light yellow

Smell: MS

Appearance: Slightly cloudy oily liquid

Composition 11F

Target Spec 11F:

pH: 6.5-7.5

Viscosity (RVT-C, 5rpm, 1min, 25℃): 50,000-100,000cps

Color: colorless - light yellow

Smell: MS

Appearance: Slightly cloudy viscous wax

Compositions 11G-1 to 11G-4

Target Specifications, Ontology:

pH: 5.0-6.5

Color: Beige (MS)

Smell: MS

Appearance: cloudy liquid

Target specification, finished product:

pH: 5.0-6.5

Color: White (MS)

Smell: MS

Appearance: dense foam, non-watery, not runny

Foam stability: 200 seconds minutes

Spray Diameter (at 8"): Foam

Spray Pattern (at 8"): Foam

Table 13

Table 14

Example 12

This example demonstrates that the composition of the present invention reduces hair weakening caused by hot ironing boards.

Comparative Composition 12A

Target Spec 12A:

pH: 6.0-7.0

Viscosity (RVT-C, 5rpm, 1min, 25°C): 40,000-80,000

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque (cloudy) gel

Comparative Composition 12B

components weight% Water (Aqua, Eau) 39.52699 Aminomethyl propanol, water (about 5% water) 0.02 Acrylic/VP Crosspolymer 1 Water (Aqua, Eau) 23.2 Aminomethyl propanol, water (about 5% water) 0.44 Water (Aqua, Eau) 20 Water (Aqua, Eau) 0.013 dye 0.000013 Polyquaternium-4 0.5 Disodium EDTA 0.05 PVP (20%), Water (Aqua, Eau) 4 VP/methacrylamide/vinylimidazole copolymer (about 20%), water 3.5 Polyquaternium-39 (8.58%), water 0.5 Propylene Glycol 1 Sorbitol, water (30% water) 0.5 Aminomethyl propanol, water (about 5% water) 0.15 Water (Aqua, Eau) 4.8 Oleth-20 0.45 Fragrance 0.15 DMDM Hydantoin (55%), Water 0.2

In the main stainless steel composite vessel, under vigorous agitation (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction), add cold water at 68-86°F (20-86°C).

Add the first aminomethylpropanol (AMP-95) to the main compounding tank and mix until fully dispersed.

Next, slowly blend the acrylic/VP crosspolymer powder into the Spray into main compounding container. A jet pump or any other in-line disperser can be used for this addition. Be careful during the addition of the powder as it will clump if added too quickly. The batch was mixed for at least 45 minutes or until the polymer was fully dispersed and there were no more particles or lumps. While mixing, begin to prepare the Celquat premix.

Take a sample from the main compounding vessel and visually inspect that all polymer has dispersed and no more particles or lumps are present. If particles or lumps remain, continue vigorous mixing and resample periodically until the batch is uniform.

Next, after dispersion has been visually confirmed, the main compounding tank is charged with deionized water under moderate agitation (turbine mixer at moderate counterclockwise direction; side sweep mixer at slow clockwise direction). Be careful when filling with water, and mix slowly to avoid aeration. This filling of water should bring the level of the batch material above the top of the vanes to avoid splashing and aeration during the neutralization step. Mix the batch for at least 15 minutes or until the batch is smooth and uniform.

Once the batch is homogeneous after the deionized water charge, continue mixing moderately (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise direction) and add the second aminomethylpropanol ( AMP-95) was added to the main compounding tank to neutralize the polymer. The solution will eventually become clear and the viscosity will increase dramatically. Mix the batch for at least 20 minutes or until the batch is homogeneous.

In a suitable stainless steel premix vessel, fill with cold water set at 68-86°F (20-30°C) as follows. Begin mixing vigorously (turbine mixer at vigorous counterclockwise speed; side sweep mixer at moderate clockwise speed up, if available).

In suitable stainless steel containers, dyes are premixed in warm water set at 104-113°F (40-45°C), where applicable. Mix until the dye is completely dissolved and homogeneous. Mix until the premix is homogeneous and does not contain any undissolved particles. Once the dye premix is ready, add this solution to the phase container.

Next, with vigorous agitation (vortex when possible; vigorous counterclockwise with turbo mixer; moderate clockwise with side sweep mixer) slowly spray Polyquaternium-4 powder over the in the container. A jet pump or any other in-line disperser can be used for this addition. Be careful during the addition of the powder as it will clump if added too quickly. The batch was mixed for at least 30 minutes or until no more particles or lumps remained.

Take a sample from the phase container and inspect visually that all polymer has dispersed and no particles or lumps are present. If particles or lumps remain, continue mixing vigorously and resample periodically until the batch is uniform.

Once the phase is clear and homogeneous, add the following ingredients to the premix vessel (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available): Disodium EDTA; PVPK -90 (20% solution); VP/methacrylamide/vinylimidazole copolymer; polyquaternium-39; propylene glycol;

Once the premix is ready, add it to the main compounding container. Rinse premix container with cold water set at 68-86°F (20-30°C) and add to main compounding container (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise ). Mix the batch for at least 20 minutes or until the batch is homogeneous.

In a suitable, clean container equipped with an electric or air mixer prepare the following fragrance premixes: Oleth-20; fragrance. For uniformity and ease of handling, oleth-20 should be premelted at 95-104°F (35-40°C). Do not mix this component with the fragrance if it is above 110°F (43°C) or the fragrance will flash off. The premix was mixed vigorously until it was clear and did not contain any undissolved material. Visually inspect it to be clear and free of particles, and then add it to the main compounding container with moderate agitation.

Check batch temperature is 104°F (40°C) or lower (cool batch if necessary), and then under moderate agitation (turbine mixer at moderate counterclockwise; side sweep mixer at moderate clockwise) direction) Add DMDM Hydantoin to the main compounding container. Mix for at least 30 minutes or until the batch is completely homogeneous. Compositions were sampled. Stop mixing and let cool (if applicable).

Adjustments can be made as follows. If the pH is low, add aminomethyl propanol at a maximum of 5% of the total batch requirement. If the pH is high, add citric acid first premixed (20% solution) in water at a maximum of 0.1% of the total batch. If viscosity is low, mix for an additional 60 minutes and sample again. Pumps that should be used to pump material to the container include diaphragm and positive displacement types. Filters that should be used include 80 mesh for all transfer operations. Fill temperature should be 68-95°F (20-35°C).

Composition 12C

Target Spec 12C:

pH: 6.0-7.0

Viscosity (RVT-C, 5rpm, 1min, 25°C): 40,000-80,000

Color: White (MS)

Smell: MS

Appearance: Viscous, opaque (cloudy) gel

Comparative composition 12D: Rhodapex ES-2 (sodium laureth sulfate) from Rhodia, diluted with water to 12% active ingredient.

Quantification of fiber debris:

Shampoo with Sodium Laureth Sulfate.

A predetermined amount of test material is applied to damp hair and distributed evenly.

Blow dry tresses without brushing.

Iron at 205°C. Pull ironing board from top to bottom of tress in about 12 seconds; repeat 5 times for a total time of 1 minute. Allow tresses to cool. The heat treatment was repeated for an additional 3 (total of 4 minutes).

Repeat all the above steps three times.

Shampoo with Sodium Laureth Sulfate.

blow dry w/o comb

Place translucent plastic under the hair strands.

Comb 100 times with a five-toothed comb (actually tapping, ie tapping rate).

Tape the plastic to secure the pieces.

Number all hair fragments collected.

Calculate the percentage reduction in hair breakage (protection):

Hair breakage reduction%=[(C-T)/C]×100

C = number of hair fragments collected for control

T = number of hair fragments collected for testing

The equipment used for tryptophan degradation fluorescence spectrometry is Spectrofluorometer-HoribaJobinYvonFluoroMax4. The test was performed at five different locations on the top or root of the tress in a window 2.3 cm wide and 1.7 cm high, with the tress 2 inches from the bottom of the bonded tress to the midpoint of the window. During the test the equipment was set as:

Excitation: 290nm wavelength; 5mm slit

Emission: from 300-400 nm; 5 mm slit; 1 nm increments Measurements of the emission spectrum from 300-400 nm were recorded in 1 nm increments. Five measurements at 336 nm (maximum point of tryptophan emission) were then averaged. Calculations are made for initial readings and after the hot ironing process. The percent degradation is calculated as follows:

[(average of 5 emission readings at 336 nm before treatment - average of 5 emission readings at 336 nm after treatment)/average of 5 emission readings at 336 nm before treatment] x 100%

The protection percentage is calculated as follows:

[(Degradation % of Control - Degradation % of Test)/Degradation % of Control] × 100%

Humidity Conditions: The tresses were stored overnight at 22% RH (dry bulb 76°C; wet bulb 54°C). The carding test was performed at 30% RH (dry bulb 75°C; wet bulb 56°C).

Tables 15 and 16 show the breakage resistance data. Table 15 shows the values for hair fragments. Table 16 shows the percent reduction in breakage relative to composition 12D.

Table 15

situation hair bundle 1 hair bundle 2 hair bundle 3 hair bundle 4 hair bundle 5 12A 352 338 408 202 140 12B 327 294 241 272 172 12C 154 82 157 121 128 12C 412 503 234 289 342

Table 16

situation Average (n=5) standard deviation % reduction relative to 12D 12A 288.0 112.1 19.1 12B 261.2 58.9 26.6 12C 128.4 30.3 63.9 12D 356.0 105.3

Figure 8 shows the percent thermal protection measured by tryptophan. Composition 12C significantly reduced tryptophan degradation. Also, trends in percent tryptophan loss correlate well with quantification of fiber debris.

This example shows that gels containing PEC significantly reduce the percentage of fiber debris and tryptophan loss from carding.

Example 13

This example illustrates the freeze-thaw stability of exemplary compositions of the invention.

Compositions 13A-13D

Compositions 13E-13G

Composition 13H-13K

Composition 13L-13N

Composition 13O-13R

Composition 13S-13V

Composition 13W-13Z

Composition 13AA-13CC

Composition 13DD-13EE

Composition 13FF-13HH

Composition 13II-13LL

The procedure for freeze/thaw stability studies is as follows:

1. Fill the finished product in a glass bottle. If testing package stability, the product is filled in appropriately packaged containers.

2. After the bottles and packages have been filled, label each. Tape around the markers to ensure they remain in place throughout the stability study.

The initial pH, viscosity, appearance, color and odor of the batches were recorded prior to placement in the freezer.

3. Place all vials/packages in the freezer for 24 hours.

4. Take samples from the freezer after 24 hours and place them in a stock box on the rack or on paper towels. The samples were allowed to thaw for 24 hours.

5. Examine the samples for appearance, color and odor after an additional 24 hours. Measure pH and viscosity, if available. Record the results.

Viscosity was measured using the following parameters: RV, T-barB, 10 rpm, 60 seconds, 25°C (except when 40,000 cps was exceeded, the method was RV, T-barC, 5 rpm, 60 seconds, 25°C).

Tables 17-20 show the viscosity (cps) and pH readings for several of the compositions shown above.

Table 17

13A 13B 13C 13D 13E 13F 13G initial pH 4.92 4.94 4.88 4.79 4.69 4.77 4.75 viscosity 22,000 20,000 19,600 18,200 15,600 16,800 19,200 24 hours pH 4.90 4.91 4.86 4.77 4.73 4.73 4.81 viscosity 25,200 24,800 23,600 19,600 22,800 29,600 31,600

Table 18

13I 13J 13K 13L 13M 13N 24 hours pH 4.90 4.87 4.93 4.86 5.04 4.90 viscosity 20,600 22,000 26,400 23,600 28,400 35,600

Table 19

n/a=greater than 1MM

Table 20

Regarding compositions 13O-13R, Recommended amount of SC-96: use 1-5% for 13O, 0.5-3% for 13P, 2-10% for 13Q, 2-12% for 13R.

Figure 9 shows the results of a comparison to determine the freeze/thaw stability effectiveness of compositions 13H-13J and 13EE with different diols. Composition 13H did not exhibit freeze-thaw stability. Addition of 5% propylene glycol (composition 13I) did not greatly improve freeze/thaw stability. Add 10% propylene glycol (composition 13J) or reduce cetyl alcohol to 1% and contain SC-96 (composition 13EE) exhibited freeze/thaw stability.

Figure 10 shows a comparison of compositions 13K-13N. Different glycols such as glycerin and sorbitol were not as effective at improving freeze/thaw stability as propylene glycol.

Figure 11 shows a comparison of compositions 13A-13C. Reducing the polyelectrolyte complex to 1% showed less severe freeze/thaw instability, but the freeze/thaw stability was not optimal (13A vs. 13H). 5% propylene glycol (13B) showed some improvement; 10% (13C) showed positive results.

Figure 12 shows a comparison of compositions 13D-13G. Addition of glycerol and sorbitol did not show freeze/thaw stability, not even when the polyelectrolyte complex was reduced to 1%.

Figure 13 shows a comparison of compositions 13S-13U. Adding the polyelectrolyte complex to the emulsion "breaks" the viscosity (13S (without PEC) vs. 13T (with PEC) vs. 13U (with PEC)). Adding the polyelectrolyte after the milk phase was complete (13U) was slightly less effective than adding it before (13T).

Figure 14 shows a comparison of compositions 13V-13X. When adding the polyelectrolyte complex before or after the emulsion (13W and 13X vs. 13T and 13U), adding Salcare SC-96 before the emulsion phase can be used to thicken the emulsion. However, the initial viscosity is low and the final viscosity takes 72 hours to build, which is not preferred in a production environment. Also, 13X is not preferred in a production environment because the batch is too thick and difficult to mix during the milk phase (without additional water and PEC to reduce the viscosity of the batch). Freeze/thaw stability and spreadability can be improved by adding propylene glycol or CrodamolSTS.

Figure 15 shows a comparison of compositions 13FF-13HH. Addition of propylene glycol and Crodamol STS did not adversely affect the emulsion viscosity (13V, 13W, 13X had similar results except the initial viscosity was thicker). 13GG is a candidate for single vessel processing, however, its final viscosity is lower than 13DD/13KK. 13HH is still not preferred in production because the batch is too thick during the milk phase.

Figure 16 shows a comparison of compositions 13Y-13AA. When adding the polyelectrolyte complex before or after the emulsion (13Z and 13AA vs. 13T and 13U), add after the emulsion phase SC-96 can be used to thicken emulsions. 13AA is preferred over 13X from a production standpoint because the batch is less thick and can be mixed properly. For thick finished products, the polyelectrolyte complex can be added after the emulsion (13AA vs. 13Z). Similar to 13W and 13X, freeze/thaw stability and spreadability can be improved by adding propylene glycol or CrodamolSTS.

Figure 17 shows a comparison of compositions 13II-13KK. Addition of propylene glycol and Crodamol STS improved initial and final emulsion viscosities (13JJ and 13KK vs. 13Z and 13AA). Adding the complex before the emulsion is not preferred because of the thin viscosity (13JJ vs. 13KK).

Figure 18 shows a comparison of compositions 13BB-13DD. Both propylene glycol and Crodamol STS individually and collectively increased viscosity.

Figure 19 shows a comparison of compositions 13EE and 13LL. CrodamolSTS and propylene glycol can be removed if cetyl alcohol is reduced to 1% and SalcareSC-96 is increased to 5% (13EE). Exclusion of cetyl alcohol resulted in a product lacking essential "conditioner properties" (opacity, emulsion bulk) (13LL).

Example 14

This example demonstrates split-end repair with exemplary compositions of the invention.

Composition 14A

I, prepare the PVM/MA copolymer of 2% active component

Part A

describe % Deionized water 94.4 20%NaOH 3.6 GANTREZ S-97BF Polymer 2

If necessary, adjust the pH to 6.95 +/- 0.05 with NaOH.

II. Preparation of 2% active ingredient polyquaternium-28

Part B

describe % Deionized water 90.25 CONDITIONEZE NT-20 9.755

III. Merge A&B (compound concentrate)

Part C

describe %

Part A 5 Part B 45

IV, preparation of conditioner preparation

Part D

describe % Start heating to 75-80°C Deionized water 39.67 L-Aspartic Acid 0.8 Hydroxyethyl cellulose 0.5 xanthan gum 0.05 Disodium EDTA 0.03 Complex Concentrate ( ^* Part C) 50.1 In a separate container heat the following ingredients to 80°C cetyl alcohol 5 stearamidopropyl dimethylamine 2 Glyceryl Stearate 0.2 Then add back to the water phase and mix at 75-80°C Add to; Cocamidopropyl Betaine 1 Cool to 45°C, then add remaining components DMDM 0.2 Fragrance 0.45 Adjust to about pH=5 with citric acid

This "complex free" composition was prepared as above, but using water in place of Part C. The control was Tresemme Anti-Breakage Conditioner.

Method: Using five 1" wide, bleached, damaged hair tresses (from Int'1 Hari Importers), 10 fibers were snipped from each sample with split ends and labeled appropriately. Raw photographs were collected under a microscope .Shampoo using standard procedure (1 mL on 1" tress, 1 min contact time, 10 strokes per side, 20 sec rinse, 35-40°C water temperature, 2 gal/min rate). Conditioning (use 1mL on a 1" tress, 1min contact time, 10 strokes per side, 20sec rinse, 35-40°C water temperature, 2gal/min rate). End comb another time. Blow dry on high heat until completely dry, then comb twice again, once with the wide-toothed end and once with the narrow-toothed end. Calculate the amount of fiber repair after the third and sixth treatments . Capture the final photo.

calculate:

Repair % = [(total number of fibers cut before treatment - number of broken fibers after treatment) - number of split ends after treatment]/(total number of fibers cut before treatment - number of broken fibers after treatment)

Disconnected % = 100 × (number of disconnected fibers/total number of fibers cut before treatment)

Table 21 shows the results.

Table 21

Example 15

This example demonstrates split-end repair with exemplary compositions of the invention.

Compositions 15A-15D

Composition 15A15B15C15D

PEC%0.5123

I, prepare the PVM/MA copolymer of 4% active component

Part A

II. Preparation of 4% active ingredient polyquaternium-28

Part B

III. Merge A&B (compound concentrate)

Part C

IV, preparation of conditioner preparation

Part D

Composition 15E

I, prepare the PVM/MA copolymer of 4% active component

Part A

II. Preparation of 4% active ingredient polyquaternium-28

Part B

describe % Deionized water 80.49 CONDITIONEZE NT-20 19.51

III. Merge A&B (compound concentrate)

Part C

describe % Part A 5 Part B 45

IV, preparation conditioner formula

Part D

test 1

From 1" wide brown hair tresses, fibers with split ends were cut and initial photographs were taken. The tresses were individually shampooed with a control shampoo (Alberto VO5 Normal Shampoo), followed by the corresponding conditioner treatment. Repeat washing for at least two times. Hair tresses were blow-dried and air-dried for 24 hours. Final photographs were taken of each cut fiber.

The results of Test 1 are shown in Figure 20, which shows the following processing:

Fiber 1 on tress 1: water treatment

Fiber 2 on tress 2: Control Shampoo - Control VO5 plus Body Conditioner

Fiber 3 on tress 3: Control Shampoo - Composition 15C

Fiber 4 on tress 3: Control Shampoo - Composition 15C

test 2

From a 1" wide tress of brown hair, five fibers with split ends were snipped and an initial photograph was taken. The tresses were individually shampooed with a control shampoo followed by the corresponding conditioner treatment. (According to standard wash program: 1 mL , 1 min contact time, 20 sec rinse, 35-40°C water temperature). Apply Composition 15E to one tress and Composition 15C to the other tress at a rate of 2 gal/min. Repeat wash at least twice. Blow dry The tresses were air dried for 24 hours. Final photographs were taken of each cut fiber.

Not much conditioning benefit was provided by the addition of silicone, but split-end repair was still evident.

test 3

Using three 1" wide brown hair tresses, 10 fibers with split ends were cut from each sample and marked appropriately. Shampoo the tresses using standard procedures (use 1 mL on 1" tresses, 1 min contact time , 10 taps per side, 20 sec rinse, 35-40°C water temperature, 2 gal/min rate). Condition with Composition 15C (use 1 mL on a 1" tress, 1 min contact time, 10 strokes per side, 20 sec rinse, 35-40°C water temperature, 2 gal/min rate). Comb through wet hair using wide-toothed ends once, and comb another time using the narrow end. After drying, comb through twice more, once using the wide-toothed end and once using the narrow-toothed end. Repeat as necessary. Count the number of fibers repaired after each treatment.

The results are shown in Table 22.

Table 22

Processing times 1 2 3 4 5 6 7 8 9 10 repair percentage 17% 26% 57% 57% 57% 57% 61% 61% 61% 61%

test 4

Using five 1" wide bleached, damaged hair tresses (from Int'1 Hair Imports), 10 fibers with split ends were clipped from each sample and labeled appropriately. Initial photographs were taken under a microscope. Using standard Program tresses (use 1 mL on 1" tress, 1 min contact time, 10 strokes per side, 20 sec rinse, 35-40°C water temperature, 2 gal/min rate). Conditioning (use 1 mL on a 1" tress, 1 min contact time, 10 strokes per side, 20 sec rinse, 35-40°C water temperature, 2 gal/min rate). Comb wet hair once with wide-toothed ends, and use Narrow end comb another time. Blow dry on high heat until completely dry, then comb two more times, once with the wide-toothed end and once with the narrow end. Calculate repair after third, sixth and tenth treatments The number of fibers. The final picture is taken.

calculate

Repair % = 100 * number of split ends after treatment / initial number of cut split end fibers

Disconnected % = 100*Number of disconnected fibers/Initial number of split-end fibers cut before treatment

The results are shown in Table 23.

Table 23

Composition 15C provided excellent conditioning to bleached tresses with easy wet combing.

test 5

Two 1" wide bleached, damaged hair tresses were used per treatment. Ten fibers with split ends were clipped from each sample and labeled appropriately. Initial photographs were taken under a microscope. Standard procedures were used to separate Shampoo tresses (use 1 mL on 1" tresses, 1 min contact time, 10 strokes per side, 20 sec rinse, 35-40°C water temperature, 2 gal/min rate). The tresses were individually conditioned with Compositions 15B, 15C, or 15D (use 1 mL on 1" tresses, 1 min contact time, 10 strokes per side, 20 sec rinse, 35-40°C water temperature, 2 gal/min rate). Comb through wet hair once using the wide-toothed end and another time using the narrow end. Blow dry on high heat until completely dry, then comb twice again, once with the wide-toothed end and once with the narrow end. At the appropriate number of treatments The number of restoration fibers is then counted. The final photograph is taken.

The results are shown in Table 24.

Table 24

test 6

Using three 1" wide brown hair tresses, 10 fibers with split ends were cut from each sample and marked appropriately. Shampoo the tresses individually using standard procedures (use 1 mL on 1" tresses, contact time 1 min, 10 taps per side, 20 sec rinse, 35-40°C water temperature, 2 gal/min rate). Hair tresses were individually conditioned with Control 1 (Nexxus commercial formulation), Control 2, Compositions 15A, 15B, 15C, or 15D (use 1 mL on 1" tresses, 1 min contact time, 10 strokes per side, 20 sec rinse , 35-40°C water temperature, rate of 2 gal/min). Comb wet hair once with the wide-tooth end and another time with the narrow end. After blow drying, comb twice again, once with the wide-tooth end and once with the narrow end Repeat the above steps as needed. Count the number of repaired fibers after each treatment. Count the number of disconnected fibers after each treatment.

Control 2 composition

describe % Start heating to 75-80°C Deionized water 89.77 L-Aspartic Acid 0.8 Hydroxyethyl cellulose 0.5 xanthan gum 0.05 Disodium EDTA 0.03 In a separate container heat the following ingredients to 80°C cetyl alcohol 5 stearamidopropyl dimethylamine 2 Glyceryl Stearate 0.2 Then add to the water phase and mix for 15 minutes at 75-80°C Add to; Mackam CB35 (coco betaine) 1

Cool to 45°C before adding remaining components DMDM 0.2 Fragrance 0.45

Adjust to about pH=5 with citric acid

Specification

pH4.35

Viscosity (RVT-B, 10rpm, 1min, 25°C) 4,800

The results are shown in Tables 25 and 26.

Table 25

Table 26

Example 16

This example demonstrates split-end repair with exemplary compositions of the invention.

Composition 16A

Mixing steps:

1. Premix - Add ingredients #1-2 and mix until hydrated

2. Use ingredient #3 to adjust pH to 6.9-7, then heat to 50-55°C

3. Slowly add ingredient #4 with very vigorous mixing, mix for about 10 minutes

4. In the main container, add ingredient #5 and begin heating to 80-85°C

5. Add ingredients #6-7. When the batch reached 80°C, add #8-10 and mix for 30 minutes.

6. Begin to cool the batch, and when below 45°C, add the premix and remaining ingredients from steps 1-3.

Target Specifications:

Appearance - opaque, viscous liquid

Odor-matching criteria

pH-4.5-5.5

Viscosity-10,000-15,000cpsRTV-B10rpm, 60 seconds

Comparative Composition 16B

Mixing steps:

1. In the main container, add ingredients #1-2 and begin heating to 80-85°C

2. Add ingredient #3 when no block exists

3. When 1-3 does not have blocks, continue heating to 80-85°C

4. When the batch reaches 80-85°C, add ingredients #4-17 and mix for 30 minutes

5. Start to cool the batch, when it is lower than 45°C, add 11-18

Target Specifications:

Appearance - opaque, viscous liquid

Odor-matching criteria

pH-4.5-5.5

Viscosity-10,000-15,000cpsRTV-810rpm, 60 seconds

Composition 16A had a pH of 4.92 and a viscosity of 10,800 cps. Composition 16B had a pH of 4.95 and a viscosity of 7,200 cps.

Wet and dry combing of Composition 16A was much better when compared to the control.

Give twice-bleached tresses a heavy blow plus blow-dry to create split ends. Cut ten split ends in each of four 11/2-inch-wide sections. Both tresses were then washed with Alberto VO5 Normal Shampoo and conditioned with Composition 16A. Both tresses were washed with Alberto VO5 Normal shampoo and conditioned with comparative composition 16B.

Composition 16A gave 90% split-end repair, while comparative composition 16B gave 63% split-end repair. Adding N-Hance SP-100 to the formulation improved the repair ability of the final formulation.

All references, including publications, patent applications, and patents, cited herein are hereby incorporated by reference to the same extent as if each were individually and specifically indicated to be incorporated by reference, and in its entirety All presented in this article.

Use of the terms "a" and "an" and "the/the" and similar expressions in the context of describing the present invention (especially in the context of the following claims) shall be construed to cover both the singular and the plural. or unless otherwise indicated herein or otherwise clearly contradicted by context. The terms "comprising", "having", "including" and "containing" are to be construed as open-ended terms (ie meaning "including but not limited to") unless otherwise stated. Recitation of ranges of values herein are merely intended to serve as a shorthand method of referring individually to each separate value falling within the range, unless otherwise indicated herein, and each separate value is incorporated into the specification as if it were individually recited herein. In this article. All methods described herein can be performed in any suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (eg, "such as") provided herein, is intended merely to better illuminate the invention and does not pose a limitation on the scope of the invention unless otherwise stated. No language in the specification should be construed as indicating any non-claimed element as essential to the practice of the invention.

Preferred embodiments of this invention are described herein, including the best mode known to the applicants for carrying out the invention. Variations on those preferred embodiments may become apparent to those skilled in the art upon reading the foregoing description. The inventors expect skilled artisans to employ such modifications as appropriate, and the inventors intend for the invention to be practiced otherwise than as expressly described herein. Accordingly, this invention includes all modifications and equivalents of the subject matter recited in the claims appended hereto as permitted by applicable law. Moreover, any combination of the above-described elements in its stated possible variations is encompassed by the invention unless otherwise indicated herein or otherwise clearly contradicted by context.

Claims (6)

1. hair care composition, it comprises:

Based on compositions gross weight 1% to 8% compound polyelectrolyte, it comprises cation type polymer and anionic polymer, wherein said cation type polymer comprises one or more monomeric units with one or more quaternary nitrogen group, and described anionic polymer is methyl vinyl ether/maleic acid;

The thickening agent of 3% to 5%, it comprises quaternary nitrogen compounds or quaternary nitrogen polymer; And

2% or less emollient, wherein said emollient is fatty alcohol;

Percentage ratio wherein based on the total weight of compositions,

The viscosity of wherein said compositions is 3000 to 100,000cps, and

Wherein said compositions demonstrates stability in freeze-thaw stability test.

2. the compositions of claim 1, wherein, described quaternary nitrogen polymer is polyquaternary ammonium salt-37.

3. the compositions of claim 1, wherein, described quaternary nitrogen polymer is the mixture of polyquaternary ammonium salt-37 and propylene/dicaprate and polypropylene glycol-1 trideceth-6.

4. the compositions of claim 1, wherein, described fatty alcohol is spermol, stearyl alcohol or its combination.

5. the compositions of claim 1, wherein, the consumption of described compound polyelectrolyte is 1% to 3% of the gross weight based on compositions.

6. the compositions of claim 1, wherein, described cation type polymer is polyquaternary ammonium salt.