PT99367A - METHOD FOR PREPARING A COMPOSITION FOR SKIN CLEANING IN THE FORM OF BAR BASED ON SYNTHETIC SURFACTANTS - Google Patents

Abstract

This invention is an improved mild personal cleansing syndet bar comprising: long chain alkyl sulfate having essentially saturated C15-C22, preferably C16-C18, alkyl chains, more preferably cetearyl sulfate, combined with a selected plasticizer.

Description

METHOD FOR THE PREPARATION OF A COMPOSITION FOR SKIN CLEANING IN THE FORM OF BAR BASED ON SURFACTANTS

TECHNICAL FIELD This invention relates to synthetic surfactant cleaning rods and the processes for producing them.

BACKGROUND OF THE INVENTION

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Synthetic surfactant-based skin cleansing bars have recently attracted a lot of interest because they tend to be softer to the skin than soap-based products. However, this softness has negative aspects both for the manufacturer and for the consumer. The manufacturer experiences difficulty in processability due to the sticky nature of such products as well as high raw material costs. The consumer experiences negative performance properties such as unpleasantness, bar softness and consequently high wear rates. There is a strong need to develop a soft bar product that is easily processable in conventional equipment while having acceptable wear characteristics. /

0BJECTIVES OF THE INVENTION

This invention relates to skin cleansing bar compositions which provide medicaments for the preparation of medicaments.

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And continue to maintain bar quality that is acceptable to the consumer. Accordingly, it is an object of this invention to provide a composition that exhibits improved processability _____

SUMMARY OF THE INVENTION

This invention is a " sindet " for improved skin cleansing comprising: at least about 18% by weight, long chain alkylsulphate having essentially saturated βâ, † alkyl chains; preferably preferably cetearylsulfate, in combination with a plasticizer selected, preferably, from paraffin, fatty acids and polyethylene glycols and mixtures thereof.

DETAILED DESCRIPTION OF THE INVENTION

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In order to develop a smooth, synthetic surfer-based bar without the negatives of processability and performance underlined it is advantageous to think of the bar as two separate components: the matrix and the active principles. The matrix provides the physical characteristics (processability and messiness) of the bar while the active ingredients provide foaming and softening properties. If the matrix is not chosen correctly, it may prevent foaming, cause poor bar probing, increase the wear rate beyond an acceptable level and / or reduce the softness of the product. Likewise, the active principles should be chosen so as to provide acceptable levels of foaming without having a negative impact on softness, a common balance in formulations.

It will be appreciated that the development of 35 1 1

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Mod. 71-20,000 eu. - an appropriate matrix and a delicate balance between plasticity and brittleness, while not compromising foaming performance. Typical matrix materials such as triglycerides, fatty alcohols, monoglycerides, etc., tend to form a sufficiently plastic matrix but also tend to lower the foam potential. Other materials commonly used in the matrix such as salts, sugars, polysaccharides, etc., tend to produce an excessively brittle and water soluble matrix inducing poor bar disarrangement. A " Sindet " comprising: (1) from about 18% to about 55%, preferably from about 20% to about 45%, essentially long, saturated, (C 1 -C 4) alkylsulphates, preferably C 16 -C 18 from about 10% to about 50%, preferably from 15% to 40%, of a plasticizer; (3) from about 45%, preferably from about 15% to about 40% soft surfactants, forming a high amount of foam; (4) from 0¾ to about 20¾, preferably from 5¾ to about 15%, of sodium soap; and (5) from about 2% to about 10%, preferably from about 3% to about 8%, of water.

Long chain alkylsulfates, defined herein, comprise long alkyl chains at a level of at least about 90%, preferably about 93%, and most preferably about 97%. Long chain alkylsulphates are derived from the corresponding saturated straight chain alcohols. Preferred alkyl sulfates have a ratio of from about 100% to about 100% of the weight by weight. A commercially available C 1 -C 6 alkylsulfate is SIPON® EC-111 (formerly SIPEX EC-111), sodium cetearylsulfate, which is about 60% Cg and 36% Cg. SIPON R EC-111 is sold by Alcolac Company, Baltimore, MD 21226. Another source is Henkel Corp. Ambler, PA 19002. The sodium cetearylsulfate of 4-35

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Henkel, LANETTE, is a 50-50% alkyl sulfate sold as an emulsifier. The terms " synthetic bar ", also " sindet bar ", mean that the bar has more synthetic surfactant than soap, unless otherwise specified. The term " sindet AS " means a " sindet " containing alkylsulfate surfactant. The term " long chain " means e and mixtures thereof. The percentages, ratios and parts included herein are listed as the total weight of the composition unless otherwise specified. All levels and ranges included herein are approximations, unless otherwise specified. It is noted that the softness of the surfactant can be measured by a skin barrier killing test, used to estimate the irritation potential of the surfactants. In this test, the milder the lower the risk, the lower the skin barrier destroyed. The destruction of the skin barrier is measured by the relative amount of the radiolabelled water (H2 O) passing from the test solution through the epidermis to the physiological buffer contained in the diffusion chamber. This test is described by T.J. Franz in JJ. Invest Dematol., 1975, 64 pp. 190-195; and in U.S. Pat. U.S.A. No. 4,673,525, Small et al., Issued June 16, 1987, hereby incorporated by reference, discloses a " simbarra " (synthetic bar) based on alkylglycerylether sulfonate (AGS) surfactant, comprising a mixture of alkylglycerylether sulfonate. " standard ". The barrier destruction test shows, surprisingly, that long chain alkylsulfates are softer than standard AGS. The long chain alkylsulfate comprises 18-55% by weight of the bars of this invention. Other - 5 - 35 1 5

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% bar ingredients &quot; sindet &quot; are selected from: other surfactants, polyamine outlier auxiliaries, humidifiers, plasticizers, fillers, etc. A &quot; sindet &quot; The preferred composition comprises: about 20-45% cetearylsulfate; 5-15% soap; and about 1-35%, preferably about 5-30%, of hu-meter; 10-50% plasticizers; and 2-10%, preferably 3-8%, of water. To ensure smoothness and reliability? The synthetic detergent surfactant system in the bars must contain long chain alkyl sulfate. Other detergent surfactants may be used; particularly from about 10% to about 50%, preferably from about 15% to about 40% co-surfactant for foam reinforcement, e.g., sodium lauroyl sarcosinate, alkyl glycerylether sulfonate and sulphonated fatty acids. Numerous examples of other surfactants are disclosed in the patents incorporated herein by reference. They include limited amounts of other alkylsulfate surfactants, anionic acylsaroosinates, methyl acyltaurates, N-acylglutamates, acyl isethionates, alkylsulfosuccinates, alkylphosphate esters, ethoxylated alkyphosphate esters, tridecetosulfates, protein condensates, mixtures of ethoxylated alkylsulfates and oxides of alkylamines; betaines, sultaines, and mixtures thereof. Included in the surfactants are the alkyl ether sulphates having 1 to 12 ethoxy groups, especially sodium and ammonium laethyl ethers. The alkyl chains for these surfactants are preferably Câ, -Câ, ", Câ, â, <â," alkyl. The acylesters of the isethionic acid salts, with acyl isethionate esters Câ,,â, ... Câ, ... and g are not more than 25% or less, of C? acyl groups. The 3% C 4 es -tearoyl isethionate is preferred; 50% C6-6 and 47% C4-6. The alkyl glycosides and methylglucose esters are preferred, nonionic, soft surfactants which can be mixed with other anionic or amphoteric soft surfactants.

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in the compositions of this invention. The bars of this invention may have up to about 10% shorter or traditional chain alkyl sulfates (coconut) and still maintain the bar softness requirements. A second essential material of the present invention is a plastic binder, also referred to herein as a plasticizer. The &quot; sindet &quot; of this invention also comprises from about 10% to about 50%, preferably from about 15% to about 40%, of plasticizer. The plasticizer may be selected from the group, paraffin, fatty acid, fatty alcohols, polyethylene glycols, although it is not limited thereto. The above-mentioned nonionic surfactants, e.g. tallow alcohol ethoxylates (TAE), e.g. TAEgo 'TAE8' etc. * &gt; are also good plasticizers. Other (free) plasticizers are identified in the published literature such as J. Amer. Oil Chem. Soc. 1982, 59, 442. The preferred cation in the AS salt is sodium. However, other cations such as triethanolammonium (TEA), ammonium, and K, etc. may also be used. Nal &gt; As used herein the term "cationic polymer" includes naturally and synthetically derived cationic polymers. The abbreviation &quot; CN &quot; means coco and the "T" stands for tallow, unless otherwise specified. All percentages and proportions are by weight, unless otherwise specified.

One &quot; simbarra &quot; (or polyethylene glycol) and paraffin in a ratio of 3: 1 to 1: 1.

A preferred sindet AS bar also contains from about 10% to about 35% humectant, preferably one selected from glycerin and free fatty acid or mixtures thereof. In this case, the free fatty acid serves the purpose as the wetting and plasticizing ingredient.

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Mod. 71-20,000 ex. - 90/08 20 63,963 Case 4274 tificante. The &quot; sindet &quot; of this invention may comprise from 0% to about 5% of an adduct cationic polymer to provide rapid hydration. The polymers have molecular weights of from about 1000 to about 3,000.00). The cationic polymer (skin conditioning agent) is selected from the group which includes: (X) cationic polysaccharides; (II) cationic copolymers of synthetic cationic monomers and saccharides, and (III) synthetic polymers selected from the group including: (A) cationic polyalkylene-imines (B) cationic ethoxypolyalkylene-imines, and

25 (C) N- [3- (dimethylammonio) propyl] -N '- [3- (ethyleneoxy-ethylenedimethylammonium) propyl] ureic cationic dichloride. Specific examples of members of the cationic polysaccharide class include the cationic hydroxyethyl cellulose JR 400, produced by Union Carbide Corporation; the Stalok® 100, 200, 300 and 400 cationic starches produced by Staley, Inc., galactomannan based on the guar gum of the Galatosol 800 series from Henkel Inc. and the Jaguar Series from Celanese Corporation.

Examples of members of the class of copolymers of synthetic cationic monomers and saccharides include compounds of cellulose derivatives (e.g., hydroxyethylcellulose) and N, N-di-alkyl, N, N-

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dialkylammonium bromide available from National Starch Corporation under the tradename Celquat.

The useful cationic synthetic polymers in the present invention are cationic polyalkylene imines, ethoxypolyalkylene imines and N- [3- (dimethylammoniopropyl) -4-CS-ethyleneoxyethylenedimethylammonium) poly] dichloride, the latter of which is available from Miranol Chemical Company, Inc. under the trademark of Miranol A-15, CAS Ref. Nos. 68555-36-2. Preferred cationic polymeric skin conditioning agents in the present invention are the cationic polysaccharides of the cationic guar gum class with molecular weights of 1,000 to 3,000,000. The most preferred molecular weights range from 2,500 to 350,000. These polymers have a polysaccharide main structure consisting of galactomannan units and a degree of cationic substitution ranging from about 0.04 per unit of anhydrous glucose to about 0.80 per anhydrous unit, with the cationic group being the substituent and the adduct of 2, 3-epoxypropyltrimethylammonium chloride for the natural polysaccharide backbone. Examples are the Jaguar C-14-S, C-15 and C-17 sold by Celanese Corporation. In order to achieve the benefits described in this invention, the polymer must have both structural and physical characteristics that allow it to be adequately and completely hydrated and subsequently well incorporated into the soap matrix.

Other ingredients 30 of the present invention are selected for the various applications. For example, perfumes may be used in the skin cleanser formulation, generally at a level of about 0.1% to about 1.5% of the composition. Alcohols, hydrotropes, dyes and fillers such as talc, clay, calcium carbonate and dextrin may also be used. 0 - 9 - 1 63-963

Case 4274 5

Cetearyl alcohol is a mixture of the cetyl and esterylic alcohols. Preservatives, e.g., sodium ethylenediaminetetraacetate (EDTA), generally at a level of less than λ% of the composition, may be incorporated into preservatives to prevent color and odor degradation. Anti-batterians may also be incorporated, usually at levels up to 1,556. The following patents disclose or refer to such ingredients and formulations which may be used in soaps &quot; bars &quot; of this invention and are incorporated herein by reference:

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Pat. No. Concession Inventors 4,234,464 11/1980 Morshauser 4,061,602 12/1977 Oberstar et al. 4,472,297 9/1984 Bolich et al. 4,981,539 1/1985 Hoskins et al. 4,540,507 9/1985 Grollier 4,673,525 6/1987 Small et al. 4,704,224 11/1987 Saud 4.812.253 3/1989 Small et al. 4,820,447 4/1989 Medcalf et al. 4,954,282 9/1990 Rys et al. The &quot; sintet &quot; from 4 to 9 in 1% aqueous solution. more preferably about 7% of this invention have the preferred pH is Laboratory Evaluation for Evaluation. The following procedures are used for the crucial performance characteristics.

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n Ma! WMM

smoothness and processability.

Methodology of the Rotating Cylinder Adhesion Test (RCAT) The Rotating Cylinder Adhesion Test (RCAT) is performed to simulate the adhesion of the "sinbarra" formulation processed to the surfaces of the processing equipment (drying / flaking / extrusion / grinding / stamping). It has been shown to correlate with the tackiness of products during processing. This peg is inversely proportional to the overall processability of the bar. The &quot; shade &quot; of this invention has a Relative RCAT Value (Rotating Cylinder Adhesion Test) of less than 1, preferably less than 0.9, and most preferably less than 0.8. A Relative RCAT Value of 1 is assigned to a comparison bar produced without the processing aid. The equipment used for this test is as follows. An inclined plane (15 °) with raised edges is used as the basis for the rotating cylinder. The cylinder itself is made of Plexiglas tubing with the outer diameter of 1016 x 10 m (4 ") and overall length of 1116/8" (3,016 x 10-1m); it weighs 735.2 grams. All evaluations are conducted at constant ambient temperature / humidity at 80 ° F (26 ° C) and relative humidity of 15%. The product "sinbarra" to be tested is scraped into small pieces (about 2 mm in length). About 20 grams of the scraped product is spread evenly over the surface of the inclined plane (which is covered with freezer Kraft paper). The pre-weighed cylinder is then placed on top of the inclined plane and allowed to roll freely over the material until it reaches the end of the path. The cylinder is again weighed, corresponding to different to the weight of the material that adhered to it. - 11 - 35 1 63-963 Case 4274 5

The greater the amount of material adhered to the cylinder, the greater the stickiness of the product and the more difficult it is to process. Data are expressed as the percentage of material adhered to the cylinder (% of RCAT) relative to the amount of material available (20 grams).

ij u

\

Table 1, below, Examples 1-46 of &quot; sindet &quot; (described in more detail below in the Examples section of Table 5) are tested for tackiness using RCAT. Comparative Example 1 is a &quot; sindet &quot; bar, product of the current state of the art, similar to the exemplified bars of Small et al, supra. 15

Mod. 71-20,000 ex. - 90/08 20 25 30 TABLE 1 Test Values of Adhesion (Tackiness) to the Turning Cylinder (RCAT)

Example RCAT (50 RCAT King 1 56.5 1.0 ** 2 32.8 0.58 *** 3 18.5 0.33 4 17.5+ 0.31 6 23.8 0.42 7 25.7 0 , 45 8 18.9 0.33 9 17.2+ 0.30 10 18.2+ 0.3.3 11 19.2 0.34 12 28.1 0.50 15 18.1 0.32 - 12 - 35 63,963 Case 4274

SM 30, JA'I.199í TABLE 1 (eont.) Adhesion Test Values (Tackiness) to the Rotating Cylinder (RCAT)

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15 20 25 30

Example RCAT (%) 16 26.3 17 24.7 18 30.7 19 24.4 21 39.9 23 34.0 26 39.3 27 28.0 29 31.3 30 40.0 31 29.8 32 16.0+ 33 23.5 34 20.0 43 26.0 44 12.0+ 45 19.5 46 9.5+ * RCAT / 56.5 ** Barra &quot; sindet &quot; of the RCAT Rei? 0.47 0.44 0.54 0.43 0.710.60 0.70 0.50 0.55 0.71 0.530.28 0.42 0.35 0.460.21 0.35 0.17 product of the present state - 13 - 35 5

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Table 1 (cont.) *** &quot; sindet &quot;

+ Better bars of less stickiness.

RCAT data are a measure ofprocability since they correlate very well with stickiness during processing. Comparative Example 1 is difficult to process because the material adheres to the cooling, extrusion and stamping equipment during manufacture. Therefore, all formulas that have a relative RCAT value of less than 1.0 are easier to process. Of Examples 3-46, for which data are available, all have lower RCAT values and improved processability. Improving the processability of these formulas is a direct result of their lower hygroscopicity.

Hygroscopicity Test (Processability) Hygroscopicity is the tendency for a product to absorb water under equilibrium conditions. It is a factor that causes the tackiness of the materials. The higher the hygroscopicity the more sticky and difficult to process a material tends to be. Hygroscopicity is measured by scraping approximately one gram of a bar product accurately knowing the initial weight and moisture. The scraped product is placed in a constant temperature (80SF) and humidity (80% RH) environment. The weight of the sample is evaluated hourly until no more weight is gained. The difference between the initial weight and the final weight is the increase in the moisture content of the sample; this value, when combined with - 14 - 63,963 Case 4274 Λ

n, f 30: JN. 1992 //% 1 The initial moisture is hygroscopicity. In Table 2, the Examples correspond to those shown in Table 1 and are described in more detail in Table 5, below. The &quot; sindet &quot; have all improved hygroscopicity relative to the standard bar of Example 1.

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TABLE 2 Hygroscopicity Value Hygroscopicity (%) Relative Hygroscopicity

Mod. 71-20,000 ex. 20

25 30 35 1 26.83 1.0 16 9.24 0.34 23 9.29 0.35 24 7.59 0.28 25 9.54 0.32 26: 6: 6-9 0.25 27 '7' 73 0.29 28 7.73 0.29 29 8.12 0.30 30 8.42 0.31 31 9.28 0.35 32 7.40 0.28 33 8.69 0.32 34 9.70 0.36 * Hygroscopicity / 26.83 = Standard - 15 - 63.963

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Skin Barrier Penetration Test (Softness)

In Vitro

This test was performed according to the procedure described in U.S. Pat. U.S. Patent 4,812,253, Small et al., issued March 14, 1989, the said patent being incorporated herein by reference.

Frequently, materials that tend to improve processability also tend to have other negative aspects, particularly in terms of the smoothness of the product. Referring to Table 3, using the barrier destruction method to evaluate the softness of the product, the individual raw materials such as sodium cetearyl sulfate show to be surprisingly softer than the ultra smooth sodium cocoglycerylether sulfonate, and a shortened chain AS, sodium dodecylsulfate. The lower the number in Table 3, the softer the product. TABLE 3 3mg of -BUO Transported Water 0.137

Sodium Cetearylsulfate 0.302

Sodium Cocoglycerylether Sodium 0.458

Sodium Dodecylsulfate 1.289

Sodium Laurate 1,805 - 16 -

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Mixture

A &quot; Sindel &quot; 1. Add molten sodium cetearylsulfate to the mixer. 2. Add a pre-determined amount of Hamposyl L-30 solution to the existing mix in the mixer. 3. Add a predetermined amount of AGS paste to the water in the mixer. The AGS slurry may be at ambient temperature or preheated to 150 ° F (65 ° C). 4. Turn on the agitator and recirculation pump and maintain the temperature in the mixer at 130-150 ° F (54-65 ° C) by adjusting the steam and water valves. 5. Leave the contents of the existing mix in the mixer back to 130-150Â ° F (54-65Â ° C prior to the addition of the predetermined amount of stearic acid.) 6. Add a predetermined amount of soap or NaOH to the mixture in the heated mixer. 7. Allow the contents in the mixer to mix and / or react for about 15 minutes while maintaining the temperature at 130-150 ° F (54-65 ° C) 8. Add to the existing mix in the heated mixer the amount pre- The content in the mixer is allowed to mix for about 17 - 35-163,963

Case 4274 of 20 minutes while maintaining the temperature at 130-150Â ° F (54-65Â ° C). 9. Add plasticizer sodium chloride and titanium dioxide to the mixture in the heated blender. 10. Add lauric acid and / or

to the mixture in the mixer and allow the contents to mix for about 15 minutes while maintaining the temperature at 130-150Â ° F (54-65Â ° C).

Drying 15

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The blender mixture is dried and cooled using a combination of &quot; flaSh &quot; and coating cylinder or coating tape. The mixture in the mixer is initially heated to about 300 ° F (149 ° C) through a heat exchanger then is flash-dried (&quot; flash &quot;) on top of the cooling cylinder or cooling belt. The cooling cylinder or cooling belt provides a product in the form of uniform, thin, cold flakes or flakes (85-95Â ° F, 29-35Â ° C). ) The typical humidity of the flake is 1-10%, preferably about 2-4.55 °. The ways to regulate the humidity, in order of preference, are (1) to increase or decrease the vapor pressure in the heat exchanger (3) increasing or decreasing the temperature of the mixture in the mixer with the heat exchanger, (3) increasing or decreasing the temperature of the mixture in the mixer with the heat exchanger,

Amalgamation 35

The flakes are weighed and blended into one

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amalgamator to achieve a uniform flake size. Pre-weighed perfume is added to the flakes and blended into the amalgamator to obtain the desired perfume level in the finished product. The perfumed flakes are transferred to the mixing hopper or directly to the extruder.

Crushing (Optional)

The three soap roller crushers are assembled, with the first roll at 120Â ° F (49Â ° C) and the other two grinders at about 44Â ° F (72c). The material is passed through the crushers several times to provide a homogeneous mixture of perfume and dry flakes.

Extrusion and Stamping

The extruder is set to the body temperature at about 125Â ° F (52Â ° C) and the end temperature at 120Â ° F (49Â ° C). The ideal extruder is a double-stage extruder which allows to use a vacuum of about 5.1 x 10-8.5 x 10-8 Pa (15-25 inches) of H 2 O. The dies should be cut into sections of 1.27-10 m (5M) and stamped with a cold template using a liquor matrix such as alcohol, if appropriate.

EXAMPLES

The following examples are illustrative and are not intended to limit the scope of the invention (s). Detailed processes for producing crushed bars are well known. All levels and ranges, temperatures, results, etc., used herein are approximations unless otherwise specified. The formulations illustrated in Examples 1 and 2 included comparative examples for illustrative purposes.

63,963 Case 4274 (%). Example 1 is a product of the current state of the art based on AGS, while Example 2 is an estimated bar formulation &quot; sindet &quot; Colgate-Palmolive VEL with £ 15.0% sodium cetearylsulfate. Examples 3-49 contain 26-46% sodium cetearylsulfate and represent the broad range of acceptable formulations within the matrix of this invention. Sodium cetearylsulfate contains primary 5 'alkyl chains. COMPARATIVE EXAMPLE 1

Mod. 71-20,000 ex. Comparative Example 1 is the control rod for evaluating the processability of the bars of this invention. See Table 4. Using this comparative example, it will be shown that the bars described below have improved processability without sacrificing softness or other bar performance properties. COMPARATIVE EXAMPLE 2

Comparative Example 2 is a &quot; sindet &quot; standard manufactured by Colgate-Palmolive Co. under the designation VEL ^. This product contains sodium cetearylsulfate estimated at 10% to 15%, significantly less than the levels required in the present invention. Additionally, the VEL bar has unacceptable bar use properties such as foam volume and grease. - 20 - 35 10 15

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TABLE 4 (% Weight) Comparative Examples 1 and 2

Ingredient EX.1 57.3 Sodium Cocoglycerylether Sodium Lauroylsarcosinate 12.5 Sodium Soap 7.2 Sodium Cocomonoglyceryl Sulfate Sodium Cetearylsulfate Getearyl Alcohol Stearic Acid 9.8 Lauric Acid 6.5 Coconut Oil Coconut Fatty Acid Sodium Chloride Sodium Sulphate Polyquaternium-7 Polyquatermium-10 Water

Ext 2 40-45 10-1515.0 4.0 1.0 0.5 4.0 EXAMPLES 3-49 5.0 2.4 10.9 6.3 1.0

Examples 3-49 are all based on a matrix composed of sodium cetearylsulfate (26-465 nu) and 21 21-35 1 63.963 /

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Stearic acid (0-20%). A number of foam forming surfactants such as sodium lauroylsilosinate (0-20%) were added to this matrix; sodium cocoglycerylether sulfonate (0-355%), sodium cocoyl thioate (4-0-17%); and sodium soap (0-155¾). The lauric acid (0-205¾), together

with stearic acid, are added to ensure a product pH of less than or equal to 7.5. Processing aids such as plasticizers (paraffin, cottonseed oil and PEG-8000) and fillers, calcium carbonate and dextrins are added (0-1555) to reduce tackiness and improve extrusion. TABLE 5

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Ex.3 ingredient (55 P) Sodium Cetearylsulfate •: U6., Sodium Lauroylsarcosinate 15.0 Sodium Cocoglycerylether Sodium Cocoylsethionate 15.0 Sodium Soap - Stearic Acid 20.0 Water 4.0 Total 100.0

Ex. 5 Ex. 6 (55 P) (5 P) (55 P) 36.0 36.0 36.0 15.0 15.0 15.0 15.0 15.0 17.3 - 10.0 7.5 8.0 20.0 20.0 20.0 4.0 4.3 4.0 100, 100.0 100.0 22-35

63,963

Sase 4274 TABLE 5 (Cont.)

(% P) (S p) (% P) Cetearylsulfate 38.0 38.0 36.2 36.0 Sodium Lauroyl sarcosinate 12.5 15, 5 12.1 11.9 Sodium Cocoglyceryl ether 17.5 11.0 17.0 16.5 Sodium sulfate Sodium soap 8.0 8.0 7.3 7.1 Stearic acid 20T0 20.0 19 , 4 19.0 Sodium Chloride - 4.0 3.0 5.0 Water 4.0 4.0 5.0 5.0 Total 100.0 100.0 100.0 100.0 TABLE 5 (Cntnt) Ex.11 Ex. 12 Ex. 13 Ex. 14 Ingredient (IP) (% p) (% P) (2 P) Sodium Cetearylsulfate 34, 34.0 36.0 35.0. Sodium laurolilsarcosinate 11.5 11.5 15.0 15.0 Sodium cocoglyceryl ether sulfonate - 15.7 15.7 17.0 9.0 Sodium cocoyl isothionate - - - 9.0 - 23 - 63.963

Case 4274 * Table 5 (Contd.) 10 i 15 20

J 25 30

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Ex.11 Ex. 12 Ex. 13 Ex. 14 Ingredient (% P) (% P) (% P) Sodium soap 6.9 6.9 8.0 8.0 Stearic acid 18.4 18 , 4 20.0 14.0 Lauric acid: - - - 6.0 Sodium chloride 8.0 8.0 - - Water 5.1 5.1 4.0 4.0 Total 100.0 100.0 100, (% P) (% P) (% P) Sodium Cetearylsulfate 35.3 35.3 35, 3 45.0 Lauroylsarcosine to Sodium 15.0 15.0 14.3 5.0 Sodium cocoglyceryl ether sulfonate 9.0 9.0 8.6 17.5 Sodium cocoyl isethionate 9.0 9.0 8.6 _ Sodium Soap 7.5 7.5 7.1 7.5 Sodium Lauryl Sulfate - 5.0 5.0 Stearic Acid 14.0 14.0 13.3 16.0 Lauric Acid 6.0 6.0 , 7.0 4.0 Water 4.3 4.3 4.0 5.0 Total 100.0 100.0 100.0 100.0 - 24 35 63.963 Case 4274 tb______________________________________ tb *. t'-k

V% TABLE 5 (Cont.)

Mod. 71-20,000 ex. - 90/08

Ex. 19 Ex.21 Ex.22 Ingredient (* P) (% P) (% P) (% P) Sodium Cetearylsulfate 40.0 40.0 45.0 45.0 Sodium Lauroylsarcosinate 8 , 0 10.0 Sodium cocoglycerylether sulfonate 14.5 12.5 14.5 14.5 Sodium soap 7.5 7.5 7.5 7.5 Sodium laurilsulfate 5.0 5.0 8.0 8.0 Stearic Acid 18.0 18.0 18.0 18.0 Lauric Acid 2.0 2.0 2.0 2.0 Water 5.0 5.0 5.0 5.0 Total 100.0 100, 0 100.0 100.0 TABLE 5 (Cont.) Ex.23 Ex. 24 Ex.25 Ex.26 Ingredient (* P) (* P) (% P) (56 P) Sodium Cetearylsulfate 26.3 32, 0 32.0 26.3 Sodium lauroylsarcosinate 15.0 13.8 13.8 15.0 Sodium cocoglyceride ether sulphate 9.0 8.3 8.3 18.0-25-il 63.963 Case 4274 ; Table 5 (Cont'd) Ex.23 Ex. 24 Ex. 25 Ex. 26 5 Ingredient% P (% P) (% P) Sodium cocoyl isothionate 9.0 8.38, 3 - 10 Sodium Soap 7.5 6.9 6.9 7.5 Stearic Acid 14.0 12.9 12.9 14.0 Lauric Acid 4.0 5.5 5.5 4.0 Paraffin 10.0 - - 10.0 15 Calcium Carbonate - 7.5 - - Dextrin - - 7.5 - Water 5.3 4.8 4.8 5.2 Total 100.0 100.0 100.0 100.0 20 TABLE (% P) (wt) Sodium Cetearylsulfate 26.3 36.3 34.3 45.0 (%) Ex. Sodium lauroyl sarcosylate 15.0 10.0 7.0 6.5 Sodium cocoglierylether sulfonate 18.0 18.0 18.0 28.5 Sodium soap 7.5 7.5 7.5 - 35 Stearic Acid 14.0 14.0 14.0 - - 26 - 63.963

Case 4274 H 3Μί I99 | . (I.e.

%

Table 5 (Cont.)

Mod. 71-20,000 ex. - 90/08

Ex. 27 Ex.28 Ex. 29 Ex.30 Ingredient (% P) (% P) (% P) 5 Lauric Acid 4.0 4.0 4.0 - Paraffin - 5.0 - 15 , PEG-8000 10.0 - 10.0 - 10 Water 5.2 IU IV) 5.2 5.2 Total 100.0 100.0 100.0 100, TABLE 5 (C3nt.) 15 Ex.31 Ex (% P) (% P) 20 Sodium Cetearylsulfate 45.0 ± 30.5 37.5 Sodium Lauroylsarcosinate 10.0 12.5 12, 0 10.0 Cocoglycerylether- 25 Sodium 25-sulphonate 28.5 27.5 16.0 25.0 Sodium Soap - - 7.5 - Stearic Acid - - 13.0 - Lauric Acid - - 6.0 - 30 Paraffin 11.5 - - - Carbonate de. Calcium - - - 7.5 PEG-8000 - 15.0 10.0 15.0 Water 5.0 5.0 5.0 5.0 35 Total 100.0 100.0 100.0 100.0 27 - 1 5

15 63-963 Case 4274 H '

¹H-NMR (CDCl3):?

Mod. 71-20,000 ex. - 90/08 20

(% P) (* P) (% P) Sodium Cetearylsulfate 30.5 30.5 33.5 μm IV) o Sodium lauroxlsarcosinate 12.0 12.0 6.0 7.5 Sodium cocoglyceryl ether sulfonate 16.0 16.0 19.0 18.3 Sodium soap 7.55 7.5 7.5 7.5 Stearic Acid 6.0 9.5 6.0 6.0 Lauric Acid 13.0 9.5 13.0 13.0 PEG-8000 10, 10.0 10.0 10.0 Water 5.0 5 , 0 5.0 5.0 Total 100.0 100.0 100.0 100.0 TABLE 5 ('Ex.39 Ex, 40 Cont.) Ex. 41 Ex.42 Ingredient% P) (% P) ( * P) Sodium Cetearylsulfate 32.0 30.5 20.0 30.0 Sodium Laurylsarcosine 9.0 12.0 12.0 7.2 Sodium Cocoglycerylether Sodium 17.5 16, 0 11.0 33.0 Sodium Soap 7.5 7.5 12.0 4.3 - 28 - 35 63.963

Case 4274

Table 5 (Cont.)

5

15

Mod. 71 · 20,000 ex. - 90/08 20

25 30

Ex-39 Ex.40 Ex.41 Ex.42 Ingredient (% P) (% P) (% P) (% P) Stearic acid 6.0 6.0 12.0 5.9 Lauric acid 13.0 13, 0 18.0 3.9 Paraffin - 10.0 - - PEG-8000 10.0 - 10.0 10.0 Water 5.0 5.0 5.0 5.0 Total 100.0 100.0 100.0 (% P) (% P) (% P) Sodium Cetearylsulfate 30.0 25.0 32.0 Ex. Sodium lauroyl sarcosine 14.0 14.0 14.0 14.0 Sodium cocoglycerylether sulfonate 7.0 7.0 7.0 7.0 Sodium soap 10.0 10.0 10.0 10.0 Stearic Acid 20.0 20.0 20.0 5.0 Lauric Acid 5.0 5.0 5.0 20.0 Calcium Carbonate - 5.0 5.0 - PEG-8000 10.0 10.0 10, 0 10.0 Water 5.0 5.0 5.0 5.0 Total 100.0 100.0 100.0 100.0 29 - 35 30. Μ1992 63,963

Case 4274

Moà. 71 - 20,000 βχ. (56 P) (56 P) Sodium Cetearylsulfate 25.0 28.1 29.5 10 • Lauroyl sarcosinate of Sodium Cocoglycerylether 13.0 11.1 14.0 Sodium Sulfate 16.0 14.7 7.0 15 Sodium Soap 10.0 6.0 10.0 Stearic Acid 20.0 12.0 20.0 Acid Lauric 5.0 5.5 5.0 Calcium Carbonate - 7.5 - 20 PEG-8000 7.0 9.2 10.0 JR-400 - - 0.5 φ Water 5.0 5.0 5.0 25 Total 100.0 100.0 100.0 Examples 33, 43 and 49 are highly preferred &quot; sindet &quot; bars, easy to process and si- multaneously with good performance in terms of bar properties.

Lisbon, 50.JAÍÍ.1992

By THE PROCTER &amp; GAMBLE CQMPANY

ENG · ΜΔΝϋξΤ ΜΟΓ AOP Deputy! Eng. ° Vasco Leite Are © Conceição, 3-1o ° 11G0 LISBOA - 30 - 35

Claims (1)

η Λ 63,963 Case 4274 Λ f: 3ϋΛΚΝί 1992 ¾ = CLAIMS = 5 15 Mod. 71-20,000 ex. - 90/08 20 A process for the preparation of a skin cleansing composition in the form of a bar and based on synthetic surfactants, characterized in that it comprises: from about 18% to about 55% of essentially C15 -C22 alkyl sulphate saturated with long chain; from 0% to about 20% soap .; and from about 10% to about 50% of a plastic binder selected from the group consisting of: paraffin waxes, fatty acids, said plastic binder having a melting point of from about 232 ° C to about 110 ° C, and the pH of the composition from about 4.0 to about 8.5. 2. A process according to claim 1 wherein the level of long chain alkyl sulfate is from about 20% to about 45% by weight of said composition and said soap is from about 5% to about about 15% by weight of said composition, and wherein said melting point of the plastic binder is about 3020 to about 100 ° C and wherein said long chain &quot; A process according to claim 1, characterized in that it mainly comprises: from about 15% to about 40% of said plastic binder; and said long chain alkylsulfonate is present at a level of from about 20% to about 40% and is a long chain alkyl sulfate surfactant of saturated alkyl chains, from about 16 to about 18 carbon atoms; and about 15% to about 40% of a mild co-surfactant. 4. A composition according to claim 3, wherein the mild co-surfactant is selected from the group consisting of sodium lauryl sarcosine, alkyl glyceryl ether sulfonate, cocoyl isethio-31 15 Mod. 71-20,000 ex. - 90/08 25 30 35 n n, The composition of the present invention comprises the steps of: (a) converting the surfactant into a surfactant having a high foam composition, and comprising from about 2.0% to about 10% water, and said bar composition being based on synthetic surfactants having a pH of about 5 to about 8, and the bar being polished. Process according to claim 1, characterized in that said synthetic soap bar composition contains further components selected from: humectants, dyes, solvents, fillers, other surfactants, polymeric sensitivity and skin sensitivity aids, perfumes and preservatives; and water at a level of from about 3% to about 8%, and also contain said alkyl and C 1-4 chains having a ratio of about 4: 1 to about 1: 4. 6. A process as claimed in claim 2, wherein said long chain alkylsulphate is at least 90% by weight of the process according to claim 1, characterized in that it comprises: from about 18 to about 55% of essentially long chain saturated C 15 -C 18 alkyl sulfate: from 0% to about 20% soap; and from about 10% to about 50% of a plastic binder selected from the group consisting of: paraffin waxes, fatty acids, said plastic binder having a melting point of from about 232 ° C to about 110 ° C, said plastic binder selected from the group consisting of: paraffin, nonionic surfactants, fatty acids, fatty alcohols and polyethylene glycols and mixtures thereof; and the pH of the composition being from about 4.0 to about 8.5. 8 - a process according to claim 32, 15 Mod. 71 -> .000 ex. - 90/08 20 Wherein the level of long chain alkylsulfate is from about 20% to about 45% by weight of said bar composition and said soap is from about 5% to about 155% , by weight of said bar composition; and said melting point of the plastic binder being from about 30% to about 100% and said long chain being cetearyl. A process according to claim 8, wherein said melt composition bar comprises mainly: from about 15% to about 40% of said plastic binder; and in that said long chain alkylsulphate is present at a level of about 20% to about 40% and is a long chain alkyl sulfate surfactant of saturated alkyl chains of about 16 to about 18 carbon atoms; and from about 15% to about 40% of a mild co-surfactant selected from the group consisting of sodium lauroylsarcosinate, alkylglycerol ether sulphonate, sodium cocoyl isethionate, matroelysethionate, and mixtures thereof, and from about 2.0% to about 10% water; and said polished bar being said pH of the composition of from about 5 to about 8; and said composition containing said C ge alquilo cade alkyl chains having a ratio of about 4: 1 to about 1: 4 and containing from about 15% to about 40% of a mixture of paraffin and free fatty acids in a ratio from about 3: 1 to about 1: 1. A process according to claim 8, characterized in that said plastic binder is a mixture of polyethylene glycol and free fatty acid in a ratio of about 3: 1 to about 1: 1. Lisbon, 30. M1992 By THE PROCTER &amp; GAMBLE CQMPANY //: ENG. »MANUEM & IONIZ PEREIRA Deputy of ΔΟΡΙ Eng. ° Basque milk Arco da Conceição, 3-1 = ° - 1100 LISBOA • 3 0 35