EA040324B1 - XANTHANE STRUCTURED LIQUID CLEANSER WITH HIGH POLYOHOLIC CONTENT - Google Patents

Description

The invention relates to personal care cleansing compositions containing foaming, preferably mild, surfactants and large amounts of polyhydric alcohol as a wetting agent. In addition, the invention relates to a method of structuring such compositions using structurants, as a rule, incompatible with such systems.

State of the art

Personal care compositions (which typically include rinse-on and rinse-off compositions suitable for application to mammalian keratin tissue) are used to cleanse and moisturize skin and/or hair, deliver actives, conceal blemishes, and reduce sebum/shine associated with skin fat.

Consumers generally prefer compositions that are gentle on the skin and/or provide a moisturizing sensation or other consumer benefits. Softness, in turn, can be associated, for example, with lower levels of skin irritation and lower levels of water loss (which can be measured, for example, using the Skicon device and/or the transepidermal water loss test known to those skilled in the art). ).

One way to meet these needs is to increase the deposition of polyols such as glycerol; emollient oils such as petroleum jelly or triglyceride oils; and most preferably enhancing deposition of both polyol and emollient oil, preferably from a mild surfactant system.

An increase in the functionality of polyols from a liquid cleanser can be achieved by using a high polyol content together with a specific mild surfactant(s) as described in EP 16190191.3 by Yang et al. which are N-acyl derivatives of mono- and/or dicarboxylic acids, in combination with a high content of glycerol, i.e. from 40 to 90 wt.% in the composition, it is possible to take advantage of the mild nature of surfactants, while at the same time providing improved glycerol deposition compared to other types of surfactants in the same high glycerol systems.

In general, high glycerin liquid cleansing compositions are known in the art.

US Pat. No. 5,716,919 to Sano discloses a mild cleansing composition containing 25 to 80 wt% polyols, a nonionic surfactant and an anionic surfactant for removing make-up from the skin, which provides a fresh and clean feeling after washing.

Roulier et al. US Pat. No. 6,303,108 claims an anhydrous, solid, self-heating, foaming composition. 20 to 85 wt % polyol is used as a binder for foaming surfactant powders to form an anhydrous solid foam composition and also provides self-heating advantage.

U.S. Patent No. 6,387,857 to Chambers et al. claims a personal care cleansing composition containing 30 to 50 wt% polyol to reduce the water activity of the cleansing composition to achieve an antimicrobial benefit.

US Pat. No. 7,879,780 to Tsaur describes a liquid cleansing composition containing a fatty acyl isethionate surfactant as the base surfactant and 10 to 60 wt % of a polyol such as glycerol or sorbitol. A high level of polyol is used in the invention to stabilize the liquid cleanser composition at both high and low storage temperatures.

Masaaki et al. EP 1237534B1 discloses 10 to 50% by weight of a polyol to stabilize a liquid cleansing composition containing a mixture of a sulfosuccinate surfactant and fatty acid soaps.

None of these references describe high levels of polyols (e.g., 40 to 75%, preferably 50 to 75% polyol) in cleansers formulated with xanthan gum, a builder generally incompatible with foaming liquid cleansers containing such amounts of polyol. . In addition, there is no description of the method of obtaining such compositions.

Delivery of an emollient oil from a liquid cleanser is also well known in the art. To stabilize softening oil droplets in liquid cleansers, polymers such as Carbopol, alkali-soluble acrylic emulsions, or xanthan gum are usually required to thicken and structure the liquid to stabilize suspended oil particles. In the presence of high levels of polyols and surfactants, polymeric thickeners either do not dissolve or do not fully swell and are unable to provide thickening efficiency due to low water activity. For example, xanthan gum is a widely used

- 1 040324 polysaccharide for thickening and structuring the water system for food, skin care or personal care products. As described in the 8th edition of the Xanthan Book published by Kelco, xanthan gum is incompatible with aqueous solutions containing 40% by weight polyols. or more preferably 50 wt.% or more. Its compatibility with the surfactant solution is from 5 to 25% by weight of the surfactant, depending on the type of surfactant.

Applicants have surprisingly found that xanthan gum can be used to thicken and structure high polyol liquid cleansers while maintaining a composition viscosity of 2000 cps or more (e.g. 2000 to 15000 cps), preferably 2500 cps or more (e.g. 2500 cps to 10000 cps), more preferably from 3000 to 10000 cps, using the methods described in this application. Applicants have also developed a process for the preparation of such high polyol compositions that are xanthan crosslinked and retain a minimum defined viscosity.

Xanthan gum as a builder for use in liquid cleansers is known and described in the prior art, in patents such as US4728457; US4788006, US5948739 and US6001344. None of these patents describes or discloses a method to overcome the compatibility problem of xanthan gum with foaming liquid cleansers containing 40 wt.% or more polyols, or compositions derived from them. In addition, none of these references indicate that homogenization to produce xanthan gum of 50 microns or less is required to solve compatibility problems when used in systems with a high content of polyols.

Brief description of the invention

In one aspect, the present invention provides personal care cleansing compositions comprising:

a) from 40 to 75% by weight of a polyol;

b) 1 to 15% by weight of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants and mixtures thereof ;

c) from 0.1 to 1.5 wt.% particles of xanthan gum having a size of 50 micrometers or less;

d) 10 to 50% water; And

e) while the viscosity of the final composition, measured using spindle No. 5 at 20 rpm for 30 seconds, is from 2000 to 15000 centipoise.

In a second aspect, the present invention relates to a process for preparing a composition comprising:

a) from 40 to 75% by weight of a polyol;

b) 1 to 15% by weight of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants and mixtures thereof ;

c) from 0.1 to 1.5 wt.% xanthan gum;

d) 10 to 50% water; And

e) whereby the viscosity of the final composition, measured using spindle No. 5 at 20 rpm for 30 s, is from 2000 to 15000 cps, and this method includes:

1) adding and mixing all xanthan gum with 5-10 parts of polyol to obtain a homogeneous mixture;

2) separate addition and mixing of the remainder of the polyol, surfactant and water in a separate mixer;

3) adding xanthan gum in polyol mixture (1) to mixture (2) and homogenizing mixture (1) with (2) with suitable homogenization so that the xanthan particles in the final mixture have a size of 50 µm or less.

In a third aspect, the present invention relates to a method for preparing a composition comprising:

a) from 40 to 75% by weight of a polyol;

b) 1 to 15% by weight of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants and mixtures thereof ;

c) from 0.1 to 1.5 wt.% xanthan gum;

d) 10 to 50% water; And

e) while the viscosity of the final composition, measured using spindle No. 5 at 20

- 2 040324 rpm for 30 seconds, is from 2000 to 15000 cps, and this method includes:

1) pre-mixing from 4 to 8 wt.% xanthan gum with 10-20 wt.% polyol;

2) adding and mixing a mixture of xanthan polyol to a 75-90 wt.% solution of surfactant with a total level of surfactant of more than 15 wt.%;

3) homogenizing the predispersion (1) plus (2) under homogenizing conditions sufficient to obtain xanthan particles of 50 micrometers or less; And

4) adding and mixing xanthan gum pre-dispersion (3) in a mixer containing the remaining ingredients.

A homogenizer that can be used is, for example, a mechanical rotor-stator type homogenizer with a homogenization speed of more than 500 rpm, preferably 1500 rpm to 15000 rpm, for example, homogenization is carried out for four minutes or more, in depending on the diameter of the rotor and its speed of rotation, the distance between the rotor and the stator, the time in the mixer and the number of generators in the series. Variables include the number of rows of teeth, their angle, and the width of the holes between the teeth. The final particle size of the xanthan gum will depend on both the rate of homogenization and the mixing time. In general, a faster homogenization rate and/or a longer mixing time will create smaller xanthan gum particles.

Detailed description of the invention

Except in the examples or where expressly stated otherwise, all numbers in this specification indicating amounts of material or reaction conditions, physical properties of the materials, and/or application are to be understood as modified by the word approximately. All amounts are by weight based on the weight of the final composition, unless otherwise indicated.

It should be noted that in defining any concentration or amount range, any particular upper concentration may be associated with any particular lower concentration or amount.

For the avoidance of doubt, the word containing is intended to mean the term including, but does not necessarily mean consisting of or composed of. In other words, the steps or options listed are not meant to be exhaustive.

The disclosure of the invention that is found in this document should be considered as covering all embodiments that are in the claims, as multiply dependent on each other, regardless of the fact that the claims can be found without multiple dependence or redundancy.

The present invention provides compositions containing high levels of a polyol, preferably glycerol, in which xanthan gum can surprisingly be used as a builder and provide good viscosity. In particular, applicants have found that by preparing in a certain way (using homogenization) new compositions can be obtained.

More specifically, the new compositions according to this invention contain:

1) 40 to 75%, preferably 45 to 75%, more preferably 50 to 75% by weight of a polyol (preferably glycerol);

2) from 1% to 15% of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants and mixtures thereof; salts of N-acyl derivatives of a dicarboxylic amino acid (eg aspartic acid, glutamic acid) or salts of N-acyl derivatives of monocarboxylic acids (eg glycine, alanine), the derivatives being particularly preferred;

3) 0.1 to 1.5%, preferably 0.3 to 1.2% xanthan gum;

4) from 10 to 50% water; and

5) while the viscosity of the final composition, measured using spindle No. 5 at 20 rpm for 30 s, is from 2000 to 15000 cps, preferably from 3000 to 10000 cps.

Preferably, the xanthan gum particles are 50 microns or less, preferably 0.1 to 50 microns, preferably 0.5 to 40 microns.

The compositions according to the present invention contain, as noted, from 40 to 75%, preferably from 45 to 75% of the polyol. Although glycerol is the preferred polyol, other polyols may be used. These include sorbitol, propylene glycol, polypropylene glycol, and mixtures thereof (including, preferably, mixtures of one of these with glycerin).

The lower level of polyol used can be 40%, 45% or 50% (and all numbers in between) and is preferably 51% or more, including 51 to 60 and all numbers in between. The upper range can be from 60 to 75 and all numbers in between. Of course, any number between 41 and 74 could theoretically be an upper or lower limit. For example, 74% may be the lower limit and 75% may be the upper limit.

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Surprisingly, xanthan gum would be compatible with such high polyol systems. However, Applicants have further disclosed a method that allows such compositions to be made while maintaining excellent viscosity. It is not recognized that xanthan needs to be homogenized (by which we mean breaking down, whether in a mechanical rotor-stator mixer using RPM; or in a classic homogenizer using inlet pressure to homogenize) to obtain fine particles in order to achieve marked compatibility.

Surface-active substance

The composition may further contain 1 to 15%, preferably 2 to 12%, even more preferably 2 to 9% by weight of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants and mixtures thereof.

The active anionic detergent that can be used in the invention may be aliphatic sulfonates such as a primary alkane sulfonate (eg C8C ₁₂ ), a primary alkane disulfonate (eg C ₈ -C ₂₂ ), a C ₈ -C ₂₂ - sulfonate an alkene, a C ₈ -C ₂₂ hydroxyalkane sulfonate, or an alkyl glyceryl ether sulfonate (AGS), or aromatic sulfonates such as alkyl benzene sulfonate. The anion may also be an alkyl sulfate (eg C ₁₂ -C ₁₈ alkyl sulfate) or an alkyl ether sulfate (including alkyl glyceryl ether sulfates).

The solubilizing cation may include sodium, potassium, ammonium, or a substituted ammonium. Ammonium and sodium lauryl ether sulfates are preferred. The anion may also be alkyl sulfosuccinates (including mono- and dialkyl, eg C ₆ -C ₂₂ sulphosuccinates); alkyl and acyl taurates, alkyl and acyl sarcosinates, sulfoacetates, C ₈ -C ₂₂ alkyl phosphates and phosphates, esters of alkyl phosphates and alkoxyl alkyl phosphates, acyl lactates, C ₈ -C ₂₂ monoalkyl succinates and maleates, sulfoacetates, alkyl glucosides and acyl isethionates, and the like. The sulfosuccinates may be monoalkyl sulfosuccinates having the formula:

R ⁴ O ₂ CCH ₂ CH(SO ₃ M)CO2M;

and amide-MEA sulfosuccinates with the formula:

R ⁴ CONHCH ₂ CH ₂ O ₂ CCH ₂ CH(SO ₃ M)CO ₂ M, where R ⁴ is in the range of C ₈ -C ₂₂ -alkyl and M is a solubilizing cation.

Sarcosinates are usually denoted by the formula:

R ¹ CON(CH3)CH ₂ CO ₂ M, where R ¹ is in the range of alkyl C ₃ -C ₂₀ and M is a solubilizing cation.

Taurates are usually identified by the formula:

R ² CONR ³ CH ₂ CH ₂ SO ₃ M, where R ² is in the range of C3-C20 alkyl, R ³ is in the range of C1-C ₄ alkyl alkyl, and M is a solubilizing cation.

The cleansing composition according to the present invention may contain C ₈ -C ₁₈ -acyl isethionates. These esters are prepared by the reaction of an alkali metal isethionate with mixed aliphatic fatty acids having 6 to 18 carbon atoms and an iodine value of less than 20. At least 75% of the mixed fatty acids have 12 to 18 carbon atoms and up to 25% have 6 to 10 carbon atoms. The acyl isethionate may be an alkoxylated isethionate such as described by Ilardi et al. in U.S. Patent No. 5,393,466 entitled Fatty Acid Esters of Polyalkoxylated isethonic acid, issued Feb. by reference This compound has the general formula:

RC-0(0)-C(X)H-C(Y)H ₂ -(OCH-CH ₂ ) _m -SO ₃ M ⁺ , where R is an alkyl group having 8 to 18 carbon atoms, m is is an integer from 1 to 4, X and Y are hydrogen or an alkyl group having 1 to 4 carbon atoms, and M is a monovalent cation such as, for example, sodium, potassium or ammonium.

Amphoteric Surfactants

In this invention, one or more amphoteric surfactants are used. Such surfactants contain at least one acid group. This may be a carboxylic or sulfonic acid group. They contain quaternary nitrogen and are therefore quaternary amido acids. They will usually contain an alkyl or alkenyl group of 7-18 carbon atoms. They will usually follow the general structural formula:

R ¹ -4-C(O)-NH(CH ₂ )n.-] _m -N ⁺ -(R ² )(R^ where R ¹ is alkyl or alkenyl with 7-18 carbon atoms; R ² and R ³ each independently represents alkyl, hydroxyalkyl or carboxyalkyl with 1-3 carbon atoms, n is from 2 to 4, m is from 0 to 1;

X is a C1-C3 alkylene optionally substituted with hydroxyl,

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Y represents —CO2— or —SO ₃ —.

Suitable amphoteric surfactants with the above general formula include simple betaines with the formula:

R ¹ —N ⁺ —(R ² )(R ³ )CH ₂ CO ₂ — and amidobetaines with the formula:

R ¹ -CONH(CH2) „- N ⁺ -(R ² )(R ³ )CH2CO ₂ where n is 2 or 3.

In both formulas, R ¹ , R ² and R ³ have the meanings as previously defined. In particular, R ¹ may be a mixture of C ₁₂ and C ₁₄ alkyl groups derived from coconut oil, such that at least half, preferably at least three quarters of the R ¹ groups have from 10 to 14 carbon atoms. R ² and R ³ are preferably methyl.

Another possibility is that the amphoteric detergent is a sulfobetaine with the formula:

R ¹ —N ⁺ —(R ² )(R ³ )(CH ₂ )SO ₃ — or

R ¹ —CONH(CHz)m—N ⁺ —(R ² )(R ³ )(CH2)SO where m is 2 or 3 or variants thereof, in which ---(CH ₂ )380z is replaced by —CH ₂ C (OH)(H)CH ₂ SO ₃ -

In these formulas, R ¹ , R ² and R ³ are as previously discussed.

It is also contemplated that the amphoacetates and diamphoacetates are coated with possible zwitterionic and/or amphoteric compounds such as, for example, sodium lauroamphoacetate, sodium cocoamphoacetate and mixtures thereof and the like.

Nonionic Surfactants

One or more nonionic surfactants may be used in the cleansing composition of the present invention. Nonionic substances that can be used include, in particular, the reaction products of compounds having a hydrophobic group and a reactive hydrogen atom, for example, aliphatic alcohols, acids, amides or alkylphenols with alkylene oxides, especially ethylene oxide, either alone or mixed with propylene oxide. Specific nonionic detergent compounds are the condensation products of (C6-C ₂₂ )alkylphenols with ethylene oxide, the condensation products of aliphatic (C ₈ -C ₁₈ ) primary or secondary linear or branched alcohols with ethylene oxide, and the products obtained by the condensation of ethylene oxide with the reaction products of propylene oxide and ethylenediamine. Other so-called nonionic detergent compounds include long chain tertiary amine oxides, long chain tertiary phosphine oxides and dialkyl sulfoxide and the like.

In some forms, the compositions of the present invention may contain a surfactant selected from the group consisting of salts of N-acyl derivatives of a dicarboxylic amino acid (for example, aspartic acid, glutamic acid), salts of N-acyl derivatives of monocarboxylic acids (for example, glycine, alanine , sarcosine) and mixtures of such derivatives of mono- and dicarboxylic acids.

Preferred dicarboxylic amino acid surfactants are acylglutamate and acylaspartate surfactants. Preferred monocarboxylic amino acid surfactants are acylglycinate, acylalanate and acylsarcosinate. Preferably they are potassium and/or sodium salts of Nacyl amino acid derivatives.

Typically, amino acid surfactants are commercially available in two forms. One is the powder or flake form, which tends to be more expensive and of high purity. Examples of solid dicarboxylic amino acid surfactants include sodium N-cocoyl-L-glutamate (for example, Amisoft® CS-11 from Ajinomoto), sodium N-lauroyl-L-glutamate (for example, Amisoft® LS-11 from Ajinomoto), N -sodium myristoyl-L-glutamate (Amisoft® MS-11 from Ajinomoto), potassium N-cocoyl-1-glutamate (for example, Amisoft® CK-11 from Ajinomoto), potassium N-myristoyl-L-glutamate (Amisoft® MK-11 from Ajinomoto ), Potassium N-Lauroyl-L-Glutamate (Amisoft® LK-11 by Ajinomoto), Sodium Lauroyl Aspartate (AminoFoamer™ FLMS-P1 by Asahi Kasei Chemical Corporation), Monosodium Lauroyl Glutamate (Aminosurfact™ ALMS-P1/S1 by Asahi Kasei Chemical Corporation), monosodium myristoyl glutamate (Aminosurfact™ AMMS-P1/S1 from Asahi Kasei Chemical Corporation).

Examples of solid surfactant monocarboxylic amino acids include sodium cocoyl glycinate (eg Amilite® GCS-11 from Ajinomoto) potassium cocoyl glycinate (eg Amilite® GCK11 from Ajinomoto).

Preferably, the content of N-acylamino acid surfactant derivatives is between 50 and 100% of the total surfactant system.

The compositions additionally contain from 0.1 to 1.5 wt.%, preferably from 0.3 to 1.2 wt.% xanthan gum. Xanthan gums are polysaccharides that can be synthesized by the fermentation of certain sugars by microorganisms such as the bacterium Xanthomonas campestris. Xanthan consists of repeating pentasaccharide units consisting of two D-glucopyranosyl units, two D-mannopyranosyl units, and one D-glucopyranosyluronic acid unit with a molecular weight of 1 million to 50 million. Xanthan gums are widely used to thicken or stabilize an aqueous system due to their excellent compatibility with many chemicals such as salts, acids, bases and water-miscible solvents. Xanthan gums preferred for this invention are commercial products such as Keltrol CG-T, Keltrol CG-SFT or Keltrol-CG manufactured by Kelco, Vangan NF-C available from Vanderbilt and Minerals, Rhodopol 23 C from Solvay.

As stated, xanthan is not typically added as a structurant to high polyol systems, especially along with surfactants as claimed in this invention. However, due to the novel processing step of our invention, Applicants can create high polyol and xanthan gum systems that allow the xanthan to increase the viscosity of the personal liquid cleanser as claimed. The key is to recognize that the xanthan gum particles must be 50 microns or less in order to be compatible in such high polyol systems.

The composition additionally contains 10 to 50%, preferably 15 to 40% water.

In a second form, the invention includes a process which makes it possible to make novel compositions according to the invention.

In particular, this invention relates to a homogenization process (as noted earlier, homogenization refers to both the destruction by a mechanical device of the rotor-stator type used at certain speeds, and / or a classic homogenizer, which is based on pressure supply) for the preparation of a composition containing:

1) 40 to 75%, preferably 45 to 75%, more preferably 50 to 75% by weight of a polyol (preferably glycerol);

2) from 1% to 15% of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants and mixtures thereof; salts of N-acyl derivatives of a dicarboxylic amino acid (eg aspartic acid, glutamic acid) or salts of N-acyl derivatives of monocarboxylic acids (eg glycine alanine) and mixtures of such derivatives are particularly preferred;

3) 0.1 to 1.5%, preferably 0.3 to 1.2% xanthan gum;

4) from 10 to 50% water; and also where the viscosity of the final composition is from 2000 to 15000 centipoise, preferably from 3000 to 10000 centipoise, as measured using a No. 5 spindle at 20 rpm for 30 seconds; where preferably the particles of xanthan gum have a size of from 0.1 to 50 microns or from 0.5 to 40 microns; and where N-acylamino acid surfactants, if present, preferably make up the majority of the surfactant system, e.g., 50 to 100% of the surfactant system, or 60 to 100%, or 70 to 100 % surfactant system;

where said method includes:

1) adding and mixing the entire xanthan gum with 5-10 parts of a polyol (preferably glycerin) to form a homogeneous mixture;

2) separately adding and mixing the remainder of the polyol, surfactant and water in a separate mixer (eg, main mixer);

3) adding xanthan gum in a mixture of polyols (1) to mixture (2) and homogenizing mixture (1) with (2) using suitable homogenization so that the xanthan particles in the final mixture have a size of 50 microns or less, preferably from 0.5 up to 40 microns.

A homogenizer that can be used is a mechanical rotor-stator homogenizer with a homogenization speed of more than 500 rpm, preferably 1500 to 15000 rpm, for example, for four minutes or more.

In another form, the method may include obtaining a concentrated pre-dispersion of xanthan gum containing all of the xanthan gum with part of the surfactant, polyol and water; homogenizing said pre-dispersion (using a rotor-stator mixer or pressure homogenizer) to produce xanthan particles of 50 µm or less, preferably 0.5-40 µm; and then mixing with other remaining ingredients.

The method includes:

1) pre-mixing from 4 to 8 wt.% xanthan gum with 10-20 wt.% polyol;

2) adding and mixing a mixture of xanthan with polyol to a 75-90 wt.% surfactant solution with a total surfactant content of more than 15 wt.%, preferably

- 6 040324 positively over 20%;

3) homogenizing the pre-dispersion (1) plus (2) under conditions sufficient to obtain xanthan particles of 50 µm or less, preferably 0.5-40 µm; And

4) adding and mixing xanthan gum predispersion (3) in a mixer containing the remaining ingredients, preferably mixing is carried out for 5 minutes or more.

Homogenization is a process using a device (e.g. of the rotorstator or classic homogenizer type as above) to break up xanthan gum particles, typically having a particle size of 100 to 400 µm, in said liquid personal care cleanser high in polyols with forming a fine dispersion of xanthan gum with a size of 50 µm or less, more preferably 0.5 to 40 µm. For the purposes of the present invention, many different laboratory and industrial homogenizers can be used using various physical technologies to micronize particles in a liquid. For example, the Silverson mixer-homogenizers are well-known rotor-stator mechanical homogenizers in the industry, and the Sonolator® is a high-pressure in-line homogenizer, also known in the industry.

The Pro300D homogenizer used to prepare the compositions of the examples of the present invention is a mechanical rotor-stator homogenizer from PRO Scientific.

Examples

Examples 1 and 2 and Comparative Examples A-F.

Table 1. Effect of Polyol Level and Processing on Liquid Cleanser Viscosity

Examples Obtaining by means of a homogenization process Comparative examples Obtaining Overhead Agitator Agitation Assistance (Except A) Example 1 Example 2 Comp. A Comp. IN Comp. WITH Comp. D Comp. E Comp. F Na cocoamidolrolyl betaine 1.5 1.5 1.5 1.5 1.5 1.5 1.5 1.5 Na lauroylglutamate 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 xanthan gum Keltrol CG-SFT 0.6 0.6 0.6 0.6 0.6 0.6 - - Carbopol Aqua SF1 - - - - - - 0.9 - Hydroxyethyl Cellulose Methocel 40-100 - - - - - - - 0.9 Glycerol 70 50 6 70 50 6 70 70 Guar hydroxypropyltrimonium chloride Jaguar C17 0.06 0.06 0.06 0.06 0.06 0.06 0.06 0.06 Perfume 0.8 0.8 0.8 0.8 0.8 0.8 0.8 0.8 Phenoxyethanol 0.6 0.6 0.6 0.6 0.6 0.6 0.6 0.6 RN 6.04 6.08 6.20 6.10 6.05 5.95 6.50 6.10 Viscosity, cP (centipoise) Brookfield rheometer #5 spindle 20 rpm, 30 s; sp 5020 7040 2340 330 1540 1940 125 The polymer settles on the bottom

The effect of the xanthan gum treatment process on the viscosity of a liquid cleanser containing various levels of glycerol is shown in Table 1. 1 above. All samples were prepared using the process described below, except for the end of processing. First, 6 parts of glycerol (polyol) were weighed and stored in a beaker. All surfactants, water and the rest of the glycerin were added to the main mixer and mixed until homogeneous for about 10 minutes at room temperature using an overhead mixer equipped with a 3-blade propeller. Xanthan gum and Jaguar C17 powders were added and dispersed in 6 parts of glycerin in a beaker. The xanthan gum dispersion was then added to the main mixer and mixed for 5 minutes at room temperature. Added perfume and phenoxyethanol and stirred for another 5 minutes. The pH of the cleanser was adjusted to a value in the range of 5.9 to 6.3 using a solution of 50 wt.% citric acid or 25 wt.% NaOH.

After all ingredients were added and the pH of the liquid was adjusted, the compositions of Examples 1-2 and Comparative A were homogenized using Pro300D from Pro Scientific Inc. at 5500 rpm for 5-7 minutes. The formulations of Comparative Examples B and C (composition similar to those of Examples 1-2 and Comparative Example A) were mixed using an overhead agitator equipped with a 3-blade propeller providing mixing at 700-750 rpm for 10 minutes. The composition according to comparative example A was mixed in a homogenizer, but it should be considered comparative, since it used a much lower content of polyol. The viscosity of the prepared liquid was measured approximately 2 hours after preparation using a Brookfield rheometer with No. 5 spindle at 20 rpm for

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With. The results are shown in table. 1. The results clearly show that the xanthan gum treatment has a large effect on the fluid viscosity for fluids with a high content of polyol (eg, glycerol). For liquids with a high content of glycerol (examples 1 and 2), the homogenization process gives a significantly higher viscosity compared to a similar liquid mixed using an overhead stirrer (comparative examples B and C). For liquids with a low glycerol content (Comparative Example A and Comparative Example D), there was not much difference in the final viscosity with different mixing methods. Surprisingly, it was found that the compositions according to examples 1 and 2 with a high content of glycerol have a significantly higher viscosity compared to comparative example A with a low content of glycerol, although in both cases a homogenization process is used. Using the method of the present invention, the compatibility problem of xanthan gum with a high glycerin liquid cleanser can be solved; and the effectiveness of the gum for thickening the liquid cleanser is also greatly improved.

Compositions according to two other examples (comparative examples E and F) were also prepared using other conventional polymer thickeners, Carbopol Aqua SF1 and Methocel 40100, for comparison. Both samples were prepared using an overhead mixer equipped with a 3-blade propeller and in the same manner as described above, without homogenization. The viscosity of the sample with Aqua SF1, as shown in the table, is very low, 125 cP, compared to example 1 of the present invention, even if a higher polymer content than xanthan gum is used (0.9% vs. 0.6%). The sample containing Methocel 40-100 showed phase separation 2 hours after preparation. Methocel 40-100 will precipitate out of the liquid and form sticky, sticky clumps at the bottom of the liquid during storage.

Examples 3A-3F. Influence of speed and time of homogenization.

Table 2. Influence of speed , and time .of homogenization on the viscosity of a liquid cleanser

Example FOR | ExampleZV Speed and time gs predisp Mixing speed 5600 rpm 5600 rpm Mixing time 1 min 3 min Of course Rheometer Brookfil, Viscosity (cP) Same day after preparation Viscosity too low for measurement. 3380 Viscosity (cP) Aged 5 days at room temperature The xanthan gum gel fell to the bottom of the product jar. 4440

Example3S |ExampleZO Example 3E emogenization of xanthan gum in the version of surfactants 5600 rpm 4500 rpm 3000 rpm 6 min 3 min 3 min <liquid viscosity Yes; spindle #5, 20 rpm, 30 sec 4470 3520 3580 4780 4150 4280

Five (5) samples with the same formulations as in Example 1 were prepared using xanthan gum in a surfactant pre-dispersion instead of adding the entire ingredient to the blender and homogenizing the entire batch as described in Example 1. This is the second defined method according to the invention. The details of the procedure are described below.

First, a glutamate/betaine surfactant premix was prepared containing 17.8 wt% Na lauroylglutamate and 5.93 Na cocoylpropyl betaine with a pH of about 5.9. Six (6) parts xanthan gum powder was mixed with 18 parts glycerin. The mixture was then added to 76 parts of the glutamate/betaine surfactant premix and homogenized at various rates and times as indicated in Table 1. 2 (eg 3000 to 5600 rpm) using a Pro300D homogenizer to convert the xanthan gum into a surfactant pre-dispersion.

The final composition was then made by adding 68.2 parts of glycerol, 0.05 parts of Jaguar C17, 2.48 parts of deionized water, 17.68 parts of the glutamate/betaine surfactant premix described above, 1 part of perfume and 0.6 parts of phenoxyethanol in a mixer equipped with an overhead stirrer. The mixture was agitated using a 3-blade propeller at 600 rpm for 10 minutes, followed by the addition of 10 parts of xanthan gum in the surfactant predispersion prepared earlier. Stirring was continued for another 10 minutes at 600-700 rpm. The viscosity of the liquid was measured approximately 2 hours after preparation, and also measured again 5 days after preparation. Both results are shown in table. 2. Viscosity data shows that the homogenization process is very reliable in controlling the final viscosity of the liquid cleanser. With sufficient agitation, all liquids have the same viscosity after 5 days of storage at room temperature.

Examples 4-6.

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Table 3

Example 4 Example 5 Example 6 Na cocoamidopropyl betaine 2.25 1.5 1.5 Na lauroylglutamate 6.75 4.5 4.5 Glycerol 60 50 50 Guar hydroxypropyltrimonium chloride Jaguar С17 0.1 0.1 0.1 xanthan gum Keltro CG-SFT 1.0 0.8 0.8 Petrolatum - 5 - Sunflower oil - - 5 Perfume 1.0 1.0 1.0 Glydant plus 0.3 0.3 0.3 Deionized water Up to 100 Up to 100 Up to 100

The pH of the liquid is from 5.9 to 6.2.

The compositions according to examples 4, 5 and 6 corresponding to the present invention, the composition of which is presented in table 3, were prepared using xanthan gum in the process of pre-dispersion of the surfactant described in example 3 above. The composition according to example 4 is characterized by a high total content of surfactant compared to the composition according to example 1, namely 9% versus 6%. The compositions according to examples 5 and 6 contain emollient oil, petrolatum and sunflower oil, respectively. Both oils were added after adding the xanthan gum to the surfactant pre-dispersion and mixed at 700-750 rpm for 10 minutes. The composition according to example 5, containing petrolatum, was obtained at 50°C, and the composition according to example 6, containing sunflower oil, was mixed at room temperature. All samples are viscous and well structured. Both petroleum jelly and sunflower oil are stably suspended in a liquid cleanser without phase separation at both high and low storage temperatures.

Claims (13)

CLAIM 1) pre-mixing from 4 to 8 wt.% xanthan gum with 10-20 wt.% polyol; 1) adding and mixing all xanthan gum with 5-10 parts of polyol to obtain a homogeneous mixture; 1. Cleansing composition for personal hygiene, containing: a) from 40 to 75% by weight of a polyol; b) 1 to 15% by weight of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants and mixtures thereof ; c) 0.1 to 1.5% by weight of xanthan gum particles having a size of 50 µm or less; d) 10 to 50% water; And e) while the viscosity of the final composition, measured using spindle No. 5 at 20 rpm for 30 seconds, is from 2000 to 15000 centipoise. 2) adding and mixing a mixture of xanthan polyol to a 75-90 wt.% solution of surfactant with a total level of surfactant of more than 15 wt.%; 2) separate addition and mixing of the remainder of the polyol, surfactant and water in a separate mixer; 2. The composition of claim 1 wherein said surfactant comprises a surfactant selected from the group consisting of dicarboxylic acid N-acyl salts or monocarboxylic acid N-acyl salts and mixtures thereof. 3) homogenizing the pre-dispersion (1) plus (2) under homogenizing conditions sufficient to obtain xanthan particles of 50 µm or less; And 3) adding xanthan gum in polyol mixture (1) to mixture (2) and homogenizing mixture (1) with (2) with suitable homogenization so that the xanthan particles in the final mixture have a size of 50 µm or less. 3. Composition according to claim 1 or 2, wherein the polyol is glycerol. 4) adding and mixing xanthan gum pre-dispersion (3) in a mixer containing the remaining ingredients. 4. Method for obtaining a composition containing: a) from 40 to 75% by weight of a polyol; b) 1 to 15% by weight of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants and mixtures thereof ; c) from 0.1 to 1.5 wt.% xanthan gum; d) 10 to 50% water; And e) whereby the viscosity of the final composition, measured using spindle No. 5 at 20 rpm for 30 s, is from 2000 to 15000 cps, and this method includes: 5. Process according to claim 4, wherein the xanthan particles in the final mixture are between 0.5 and 40 µm in size. 6. The method according to claim 4 or 5, wherein the homogenization is carried out using a rotorstator type mixer and is carried out at a homogenization speed exceeding 500 rpm for four minutes or more. 7. The method according to any one of claims 4 to 6, wherein the surfactant of (2) comprises a surfactant selected from the group consisting of N-acyl salts of dicarboxylic acid derivatives or salts of N-acyl derivatives of monocarboxylic acid, and their mixtures. 8. The method according to any one of claims 4 to 7, wherein the polyol is glycerol. 9. A method of obtaining a composition containing: a) from 40 to 75 wt.% polyol; b) 1 to 15% by weight of a surfactant selected from the group consisting of anionic surfactants, nonionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants and mixtures thereof ; c) from 0.1 to 1.5% by weight of xanthan gum; d) 10 to 50% water; And e) whereby the viscosity of the final composition, measured using spindle No. 5 at 20 rpm for 30 s, is from 2000 to 15000 cps, and this method includes: - 9 040324 10. The method of claim 9 wherein the total surfactant level in step (2) is greater than 20%. 11. The method according to claim 9 or 10, wherein the particle size of the xanthan in step (3) is 0.5-40 µm or less. 12. The method according to any one of claims 9 to 11, wherein the mixing in step (4) is carried out for more than 5 minutes. 13. The method according to any one of claims 9 to 12, wherein the homogenization is carried out using a rotor-stator type mixer at a homogenization speed of more than 500 rpm for four minutes or more. Eurasian Patent Organization, EAPO Russia, 109012, Moscow, Maly Cherkassky per., 2