ES2232566T3 - IMPROVED DETERGENT COMPOSITION. - Google Patents

Abstract

A molded detergent composition with a solids content of less than 30%, having an elastic resistance> 75 kPa in a temperature range of 20-40 ° C, comprising (i) 2-50% by weight of soap saturated fatty acid comprising one or more salts of C6-C24 fatty acids; (ii) 2-40% by weight of active detergent species (iii) 30-80% by weight of water and optionally one or more liquid beneficial agents, in which the composition does not show pure liotropic liquid crystalline phase in the temperature range of 20-100 ° C and forms an isotropic liquid phase or a dispersion of the liotropic liquid crystalline phase in a continuous medium of the isotropic liquid at a temperature within the range of 40-100 ° C, and in which the composition Contains less than 5% by weight of alcohols, propylene glycol and other polyols, and less than 1% by weight of saline electrolytes

Description

Improved detergent composition.

The present invention relates to compositions of solid detergent formed by melting in molds with a solids content less than 30% and very high water levels or beneficial liquid agents, but with high stiffness and good properties in use.

Detergent tablets are manufactured in a manner conventional by one of the two procedures (i) work to shear / homogenization of the formulation followed by extrusion and stamping, or (ii) molding.

In the manufacture of detergent tablets through shear and extrusion work, the amount of water that can be incorporated into the formulation is typically less than \ sim15%. These systems are multiphase composite materials that they have a morphology of the type "blocks suspended in mortar ". The blocks are solid particles, which in the case of Soaps for personal hygiene are crystalline salts of acids saturated long chain fatty acids, inorganic particles, etc. He mortar is a mixture of different liotropic crystalline liquids or phases in isotropic solution, comprising water, liquid additives, and relatively water-soluble soaps or surfactants. These compositions will typically comprise 40-60% of solids, 20-50% of liquid crystalline phases Liotropic and up to 10% isotropic fluid.

In the manufacture of detergent compositions by molding, the formulated system is brought to a fluid state increasing the temperature, the molds are filled and cooled. This technology is commonly used to make pills transparent for personal hygiene that typically contain other ingredients (such as soap or synthetic surfactants) a 15-50% of expensive alcoholic ingredients such as ethanol, polyhydric alcohols, sugars, etc., at the time of molding

US 4,165,293 (Amway, 1979) and WO 96/04361 (P&G, 1996) describe a solid transparent soap bar comprising soap, synthetic surfactants, and a water soluble organic solvent such as, for example, propylene glycol. The water level in these compositions is approximately one
10-32%

The problem in the manufacture of tablets non-transparent detergent by molding is that the compositions typical do not form a liquid that can be poured at high temperatures Document US 5,340,492 (P&G, 1994) claims a moldable composition comprising carboxylic acids neutralized crystals (soap), synthetic surfactants and high levels of water and other liquids. The prepared compositions as described in US 5,349,492 are soft, presenting an elastic resistance less than 75 kPa measured using a wire cutter for cheese, and therefore not suitable as firm pads that are rigid enough to hold in hand conveniently for use.

In order to increase the stiffness of the tablet, patent examples employ ingredients such as polyols (for example, propylene glycol) in the composition, under the appearance called "pill appearance aids". The patent does not describe any composition without the incorporation of "pill appearance aid" when they are also synthetic surfactants present in the composition. These Pill appearance adjuvants are expensive, reduce the amount and speed of the foam and, on the other hand, are fine known in the prior art (US 4,165,293, Document WO 96/04361).

In our pending application (717 / Bom / 99, Document WO-A-0130959) has been described that incorporating low amounts of electrolytes saline in melt molding detergent compositions that They comprise fatty acid soap, active detergent, very levels high water or liquid beneficial agents, results in rigid solid shaped articles that have a strength elastic greater than 75 kPa measured using a cutting device cheese wire These compositions can be held in the hand, they are economical, very sparkling and show good properties In use. The fatty acid soap according to the previous request is one or more of the C 6 -C 24 fatty acids neutralized

The prior art generally teaches use of additives such as polyols or saline electrolytes or others tablet appearance aids in compositions for melt molding comprising a fatty acid soap, detergent active, very high water levels or liquid beneficial agents to improve the stiffness of the tablet.

At present, it has been possible to obtain a composition of melt molding detergent using nothing or very low levels of additives, having a solids content less than 30% and high levels of water or other beneficial agents liquids, which are rigid and have an elastic resistance> 75 kPa in a temperature range between 20-40 ° C.

In a first embodiment, the invention comprises a melt molding detergent composition that it is preferably a tablet with a solids content less than 30%, presenting an elastic resistance> 75 kPa in a temperature range between 20-40 ° C, comprising:

(to)

a 2-50% by weight of saturated fatty acid soap that comprises one or more fatty acid salts of C_ {6} -C_ {24}.

(b)

a 2-40% by weight of active detergent species, Y

(C)

a 30-80% by weight of water and optionally others Liquid beneficial agents.

characterized in that the composition does not show pure liotropic liquid crystalline phase in the temperature range of 20-100 ° C, and forms an isotropic liquid phase or a dispersion of the liotropic liquid crystalline phase in the continuous medium of isotropic liquid in the temperature range of 40-100 ° C and in which the composition contains less than 5% by weight, more preferably less than 1% by weight, even more preferably less than 0.5% by weight, and may even be totally free of polyhydric alcohols, and less than 1%, more preferably less than 0.5%, and conveniently can be totally free of saline electrolyte. It is preferred that the active ingredient of the detergent is predominantly non-soapy.

The presence of the isotropic liquid phase and the liquid crystalline phases in surfactant systems are preferably detected using the microscopy technique of optical polarization The liquid crystalline phases are inherently anisotropic, causing the refractive index depend on the orientation. In general, such systems birefringent change the plane of polarization of light polarized An isotropic liquid appears black between polarizers crossed, but a crystalline liquid system is more transparent, for example, lamellar liquid crystalline phases show malt crosses or oil grain textures (in the form of large loops), while hexagonal phases show textures in fan shape. It has been reported in the textures bibliography characteristics of various crystalline phases of liotropic liquids and its dispersions.

In accordance with another aspect of the invention, provides a process for manufacturing the composition of solid form detergent of the invention comprising the stages of:

a) manufacture a melt of the composition previous,

b) pour said melt into a mold to get the desired shape,

c) cool the mold under resting conditions to achieve solidification.

According to a preferred aspect of the invention, a method is provided for manufacturing a solid molding package detergent composition that It comprises the stages of:

a) manufacture a melt of the composition previous,

b) pour said melt into a mold of preformed polymer to obtain the desired shape,

c) seal the mold, and

d) cool the mold under resting conditions to achieve solidification.

The present invention relates to compositions of detergent that essentially have a behavior of specific phase that results in a rigid tablet for cast molding with a solids content of less than 30%, and very high levels of water or other beneficial liquid agents. The detergent composition is characterized in that the composition does not shows liquid crystalline phase in the range of temperature of 20-100 ° C and forms a liquid phase isotropic in the continuous medium of the isotropic fluid in the interval of temperature of 40-100ºC.

The presence of the isotropic liquid phase and the liquid crystalline phases in surfactant systems are preferably detected using the microscopy technique of optical polarization The liquid crystalline phases are inherently anisotropic, causing the refractive index depend on the orientation. In general, such systems birefringent change the plane of polarization of light polarized An isotropic liquid appears black between polarizers crossed, but a crystalline liquid system is more transparent, for example, lamellar liquid crystalline phases show malt crosses or oil grain textures (in the form of large loops), while hexagonal phases show textures in fan shape. Various structures have been observed in the inside the same phase structure.

Characteristic textures of various liquid crystalline phases in the following References: (i) "The Aqueous Phase Behavior of Surfactants" by Robert G. Laughlin, Academic Press, New York, 1994, Pages 538-542. (ii) "The Colloidal Domain Where Physics, Chemistry, Biology, and Technology Meet "by D. Fennell Evans, Hakan Wennerstrom, VCH Publishers, New York, 1994, Pages 251-252.

The solid shaped articles of the composition according to the invention are sufficiently rigid to hold by hand conveniently, economically, very foaming, and have good properties in use. The compositions have elastic resistance values greater than 75 kPa measured using the automatic penetrometer.

Saturated fatty acid soap is selected from preferably between one or more fatty acid salts C_ {6} -C_ {24} saturated The soap used can be a salt of sodium, potassium, magnesium, aluminum, calcium or lithium of saturated fatty acids. It is especially preferred to have a soap obtained as sodium salt or potassium fatty acid saturated.

The saturated fatty acid soap in the composition is preferably comprised between a 5-50% by weight and more preferably a 5-40% by weight.

The compositions according to the invention they also comprise detergents with active ingredients that can be based or not on soap. It is preferable to use detergents with non-soapy active ingredients that are selected from anionic, nonionic, cationic, amphoteric or Zwitterionic, or mixtures thereof.

Anionic active detergent compounds suitable are water soluble salts of reaction products of the sulfuric organic acids that have a molecular structure in alkyl radical containing between 8 and 22 carbon atoms, and a radical chosen from ester radicals of sulfonic acid or sulfuric acid, and mixtures of the above. Some examples of Active compounds of synthetic anionic detergent are alkyl linear benzene sulphonate, sodium lauryl sulfate, lauryl ether sodium sulfate, alpha olefin sulphonate, alkyl ether sulfate, ester fatty acid methyl sulfonate, alkyl isethionate, etc.

The most suitable cations in species Previous detergent active agents are sodium, potassium, ammonium, and various amines, for example monoethanol amine, diethanolamine, and triethanolamine

Non-ionic active detergent compounds suitable can be described broadly as the compounds produced by the condensation of alkylene oxide groups, which are hydrophilic by nature, with a hydrophobic compound organic that can be aliphatic or aromatic alkyl. Common non-ionic surfactants are the products of condensation of aliphatic alcohols having between 8 and 22 atoms carbon, in the configuration of the chain both linear and branched, with ethylene oxide, such as oil condensate of coconut with ethylene oxide that has between 2 and 15 moles of oxide of ethylene per mole of coconut alcohol. Some examples of nonionic surfactants are condensed alkyl phenol oxide ethylene (EO), tallow alcohol condensate 10 EO, alkyl oxides dimethyl amine, lauryl monoethanolamide, sugar esters, etc.

Some examples of detergents with ingredients Amphoteric assets are coco amidopropyl betaine, cocobetaine, etc.

It is also possible to optionally include detergents with cationic or zwitterionic active ingredients in the compositions according to the invention.

Additional examples of active species of Suitable detergents are given in the following reference "Handbook of Surfactants" M. R. Porter, Chapman and Hall, New York, 1991.

The active ingredient of the detergent to be used in the detergent composition of this invention is, of preferably, anionic, and will usually be contained up to 40% and more preferably between 2 and 30%.

According to a preferred aspect of the invention, liquid materials are incorporated into the composition beneficial for the skin, such as moisturizers, emollients, sunscreens, and anti-aging compounds. The examples Moisturizers and humectants include polyols, glycerols, alcohol of cetyl, Carbopol 934, ethoxylated castor oil, oils paraffin, lanolin and its derivatives. You can also include silicone compounds such as silicone surfactants such as the DC3225C (Dow Corning) and / or silicone emollients, oil silicone (DC-200 marketed by Dow Corning). Sunscreens such as 4-tert butyl-4'-methoxy dibenzoylmethane (available under the trade name Parsol 1789, from Givaudan) and / or 2-ethyl hexyl methoxy cinnamate (available under the trade name Parsol MCX, from Givaudan) or other protectors UV-A and UV-B. Can be incorporated also in the composition other beneficial agents for the skin such as polyethylene glycol (PEG).

Others may be incorporated into the composition. optional ingredients such as conditioning agents hair, fillers, color, perfume, opaquents, preservatives, one or more water insoluble particulate materials such as talc, kaolin, polysaccharides and other conventional ingredients.

A preferred method of the invention may be a manufacturing process in which a melt is prepared of the detergent composition comprising a 2-50% by weight of saturated fatty acid soap, a 2-40% by weight of an active detergent ingredient non-soapy and 30-80% water or other agents beneficial liquids, characterized in that the composition does not shows pure liotropic liquid crystalline phase in the range of temperature of 20-100 ° C, and forms a liquid phase isotropic or a dispersion of the liquid crystal phase liotropic in the continuous medium of the isotropic liquid in the range of temperature of 40-100 ° C. In the procedure, this molten is poured into any suitable mold or in a preformed polymer mold to obtain the desired shape, the mold It is sealed and cooled under resting conditions to achieve solidification.

The mold can be selected appropriately to produce a tablet with almost net forms or produce pads / blocks The pads / blocks can be made up of Additional way in the detergent article.

If the solid detergent article is produced using a thermoformed polymer with almost net shapes, the mold is seal to obtain a detergent composition molded into package. To obtain a molded detergent composition in package, the mold is preferably sealed immediately after the filling of the mold.

The invention will now be illustrated with respect to The following non-limiting examples.

Examples Example 1 Selection of compositions with respect to their behavior phase

The composition according to the invention is characterized in that the composition does not show liquid crystalline phase pure liotropic in the temperature range of 20-100 ° C and forms an isotropic liquid phase or a dispersion of the liquid crystalline phase in the medium continuous isotropic fluid in the temperature range of 40-100 ° C. The examples are presented in Table 1 comparatives according to the invention and beyond the invention.

to. Phase characterization

The characterization of the phase of the compositions was carried out using the technique of optical polarization microscopy. A drop of the composition melt was transferred at an elevated temperature of 80 ° C on a microscope holder and covered with a cover. The edges of the cover were sealed using UV glue to minimize moisture loss. The slide was mounted on the microscope slide provided with a controlled heating / cooling installation. The system was heated at 110 ° C at a rate of 1 ° C per minute. The temperature at which the isotropic liquid phase or its dispersion was formed, or the liquid crystalline phase was then noted.
pure.

The system was then cooled to achieve solidification at the rate of 1 ° C per minute to check that pure liquid crystalline phases form during the cooling The liquid crystalline phases are inherently anisotropic, causing the refractive index depend on the orientation. In general, these systems birefringent change the plane of polarization of light polarized An isotropic liquid appears black between polarizers crossed, but a liquid crystalline system is more transparent, for example, lamellar liquid crystalline phases show malt crosses or oil grain textures (in the form of large loops), while hexagonal phases show textures in fan shape, not geometric.

Various textures have been observed within the Same phase structure. Textures reported characteristics of various liquid crystal phases liotropic (and their dispersions) in the following references: (i) "The Aqueous Phase Behavior of Surfactants "by Robert G. Laughlin, Academic Press, New York, 1994, Pages 538-542. (ii) "The Colloidal Domain Where Physics, Chemistry, Biology, and Technology Meet "by D. Fennell Evans, Hakan Wennerstrom, VCH Publishers, New York, 1994, Pages 251-252.

b. Determination of solids content

The low field NMR technique was used to determine the solids content in detergent compositions using the procedure described in the following reference: Suresh M. Nadakatti, "Modified Data Handling for Rapid Low Field NMR Characterization of Lyotropic Liquid Crystal Composites ", J. Surfactants and Detergents, Vol. 2, No. 4, pp. 515-521, 1999.

C. Preparation of the detergent tablet

A melt of the composition of detergent at an elevated temperature of 80 ° C in a rectangular mold with dimensions of 75 mm (L) x 55 mm (W) x 40 mm (A). Left cool the composition to achieve solidification and obtained the detergent tablet

d. Elastic Strength Measurement

The detergent tablets were kept at continued in ovens maintained at 25ºC and 40ºC respectively for 4 hours and allowed to reach equilibrium. The elastic strength of the pads at 25 ° C and 40 ° C using a automatic penetrometer using the procedure described previously.

The automatic penetrometer used for measurements of the elastic resistance was the PNR 10 model from M / s Petrotest Instruments Gmbh. The hollow standardized cone was used (part # 18-0101 according to ASTM D 217 - IP 50) together with a piston (part of 18-0042) for measurements. The cone it consisted of a conical brass body with a detachable tip of hardened steel. The total mass of the cone was 102.5 g. Mass Total mobile piston was 47.5 g. The total mass of the cone and the plunger that falls on the detergent tablet was therefore of 150 g Additional weights of 50 g and 100 g were also used (making that the total weight that fell on the sample was 200 g and 250 g respectively). The elastic resistance values of the sample at 25 ° C and 40 ° C were measured using the standardized protocol which included the following stages:

1. The detergent tablet was placed on the penetrometer table

2. The penetrometer measuring device is lowered in order for the tip of the penetrometer to touch the tablet, but without penetrating.

3. The measurement operation began by pressing the "start" key

4. The penetration depth was read in mm as it appears on the screen.

5. The measured penetration depth value it was used to calculate the elastic strength of the tablet detergent using the following equation:

resistance \ elastic = Force \ applied / projected \ area \ of the cone = (m \ x \ g) \ x \ 10 ^ 3 / [\ pi \ (p \ tan \ ^ {1} / {2} \ theta \ + \ 1 \ / 2 \ del \ diameter \ de \ la \ tip) 2]

in the that:

the elastic resistance is in kPa

m = total mass that falls on the flat surface of the tablet in kg

g = acceleration due to gravity in m / s2

p = penetration achieved in mm

the = cone angle (30 °)

tip diameter = 0.359 mm.

According to the previous equation if the measured penetration depth is <10 mm for a total mass of 200 g falling on the sample, then the elastic resistance of the detergent tablet is> 75 kPa. Three were calculated Elastic strength values for 150 g, 200 g, and 250 g of dough total that falls on the detergent tablet, and the average of the three values was used as the elastic strength of the tablet Detergent.

and. Examples of tablet compositions of Detergent

The data presented in Table 1 show that only the composition described in Ex 1.1, which satisfies the phase characterization according to the invention, formed a rigid detergent tablet presenting an elastic resistance > 75 kPa The compositions of Examples 1.2 and 1.3 are soft because they form a pure liotropic liquid crystalline phase in the temperature range of 35-75 ° C and do not form phase Isotropic liquid or its dispersion in the temperature range of 40-100 ° C In Example 1.4, the temperature at which the isotropic phase or its dispersion formed during heating it was within the range specified in the invention, but it formed pure liquid crystalline phase during cooling, and in Consequently, the tablet was soft. This shows that it is essential to satisfy both phase behavior criteria to get pads that are rigid and show resistance elastic> 75 kPa.

TABLE 1

one

Additional examples of the compositions that present the behavior of the phase of according to the invention and Table 3 shows those that do not they present the phase behavior according to the invention. All the examples in table 2 have less than 20% solids and however it forms rigid pads presenting a resistance elastic> 75 kPa at 25 ° C. The examples described in Table 3, on the contrary, they are soft.

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2

TABLE 3

3

Example 2 Procedure for preparing the detergent tablet

According to the selection procedure described in Example 1, a fatty acid mixture corresponding to the Examples 1.5 to 1.11 in two two-liter round bottom flasks capacity and mixed with detergent active ingredient no soapy and water. The batch temperature was increased to 80 ° C. Be added the aqueous sodium hydroxide solution to the mixture to neutralize fatty acids. The batch temperature was maintained at 80 ° C, so that a transparent isotropic solution was obtained. The melt of the detergent composition at 80 ° C was poured into a thermoformed polymer mold, and the mold inlet was sealed. Be let the mold cool to achieve solidification of the soap, and In this way, a molded detergent tablet was obtained in package.

Claims (7)

1. A detergent composition molded into cast with a solids content of less than 30%, presenting a elastic resistance> 75 kPa in a temperature range of 20-40 ° C, which comprises (i) 2-50% by weight of soap saturated fatty acid comprising one or more fatty acid salts of C 6 -C 24; (ii) 2-40% by weight of species detergent active (iii) 30-80% by weight of water and optionally one or more liquid beneficial agents, in which the composition does not show pure liotropic liquid crystalline phase in the temperature range of 20-100 ° C and forms an isotropic liquid phase or a dispersion of the liquid crystalline phase in a medium continuous isotropic fluid at a temperature within the range from 40-100 ° C, and in which the composition contains less than 5% by weight of alcohols, propylene glycol and other polyols, and less than 1% by weight of electrolytes saline 2. A detergent composition molded into molten according to claim 1 wherein the water and of optional liquid beneficial agents are present in an amount of 60-80% by weight of the composition. 3. A detergent composition molded into cast according to any preceding claim, wherein active detergent species are a non detergent soapy. 4. A detergent composition molded into cast according to any preceding claim, wherein fatty acid soap is a sodium or potassium salt of acid fatty. 5. A detergent composition molded into cast according to any preceding claim, wherein The liquid beneficial agent is selected from moisturizers, moisturizers, emollients, sunscreens and compounds anti-aging 6. A procedure for the preparation of a cast molded detergent composition according to a any one of claims 1 to 5, the process It includes: (i) manufacture a melt of the composition of Detergent; (ii) pour the melt inside a suitable mold to obtain the desired shape; Y (iii) make or allow the mold to cool by means from which a detergent composition is produced solid. 7. A procedure in accordance with the Claim 6 wherein step (ii) includes the sub-stages (iia) pour the melt inside a preformed polymer mold to obtain the desired shape; Y (iib) seal the mold, to produce whereby a Solid detergent composition molded into a package.