GB2196980A - Hair care compositions containing purified cationic surfactant materials - Google Patents

Abstract

Compositions containing purified cationic surfactant materials (substantially free of undesirable solvents, including water) are for use as hair shampoos and/or hair conditioners. The purification may be made by washing the cationic surfactants with an organic solvent.

Description

SPECIFICATION Hair care compositions containing purified cationic surfactant materials Prem Sagar Juneja TECHNICAL FIELD This invention relates to processes for purifying cationic surfactant materials and compositions containing the purified cationic surfactant materials.

BACKGROUND OF THE INVENTION Cationic surfactant materials are widely known for use in softening, cleaning and cosmetic compositions.

Many hair care compositions, especially conditioning products, contain long chain quaternary ammonium compounds. Compositions are disclosed in U.S. Patent 3,155,591, Hilfer, issued November 3, 1964, and U.S. Patent 4,269,824, Villamarin et al., issued May 26, 1981. Hair care compositions have also been disclosed which contain quaternary ammonium salts and silicone materials in U.K. Patent Application 2,066,659, Abe, published July 15, 1981, all of which are incorporated herein by reference.

Cationic amines are disclosed in U.S. Patent 4,275,055, Nachtigel et al., issued June 23, 1981.

Although widely used, all of the problems of making compositions containing such cationic surfactant materials have not been solved.

It has been found that frequently commercial supplies of certain cationic surfactant materials contain levels of water and/or other solvents; the amount of which varies by lot of material.

Surprisingly, this has been found to adversely impact the stability and processing of certain compositions made therewith. The impure materials vary in color from off-white to brown; they vary in physical condition from partially dry sticky powders to pasty solids. The variation in level also renders measurement less accurate.

Applicant has now discovered that cationic surfactant materials purified by a process described herein, yield significantly improved physical properties, ease of handling and accuracy of processing.

It is therefore an object of the invention to provide stable compositions containing purified cationic surfactant materials.

It is a further object ofthe invention to provide purified cationic surfactant materials for use in such compositions.

It is a further object to provide purified cationic surfactant materials in the form of free-flowing powders.

These and other objects will be made clear from the description herein.

All percentages and ratios herein are by weight unless otherwise noted.

SUMMARY OF THE INVENTION The present invention provides hair care compositions comprising purified cationic surfactant materials. The invention also provides hair care compositions comprising cationic surfactant materials purified by a certain process.

DETAILED DESCRIPTION OF THE INVENTION Cationic Surfactant Materials Compositions of the invention comprise one or more purified cationic surfactant materials.

Such surfactant materials contain amino or quaternary ammonium hydrophilic moieties which are positvely charged when dissolved in the aqueous compositions of the present invention.

Cationic surfactant materials are those described in the following publications, all of which are incorporated herein by reference: McCutcheon's, Detergents & Emulsifiers (North American Ed.

1979); Schwartz et al., Surface Active Agents, Their Chemistry and Technology, New York: Interscience Publishers, 1949; U.S. Patent 3, 155,591, Hilfer, issued November 3, 1964; U.S.

Patent 3,929,678, Laughlin, issued May 25, 1976, and U.S. Patent 4,387,090, Bolich, Jr., issued June 7, 1983, and U.S. Patent 4,275,055, Nachtigel, issued June 23, 1981.

Quaternary ammonium-containing surfactant materials useful herein are those of the general formula:

(a) wherein R1 is an aliphatic group having from about 8 to about 22 carbon atoms, R2, R3 and R4 are hydrogen or short chain alkyl groups having from about 1 to about 4 carbon atoms, and X is an anion selected from the group consisting of acetate, halogen, phosphate, nitrate, and alkyl sulfate radicals, or (b) wherein R" R2 and R3 are aliphatic groups having from about 8 to about 22 carbons atoms, R4 is hydrogen or an alkyl group containing from about 1 to about 4 carbon atoms and X is as defined above.

Salts of primary, secondary and tertiary fatty amines are also useful cationic surfactant materials. The alkyl groups of such amines preferably have from 12 to 22 carbon atoms, and may be substituted or unsubstituted. Secondary and tertiary amines are preferred, tertiary amines are particularly preferred. Such amines, useful herein, include stearamido propyl dimethyl amine, diethyl amino ethyl stearamide, dimethyl stearamine, dimethyl soyamine, soyamine, myristyl amine, tridecyl amine, ethyl stearylamine, N-tallowpropane diamine, ethoxylated (5 moles E.O.) stearylamine, dihydroxy ethyl stearylamine, and arachidylbehenylamine. Suitable amine salts include the halogen, acetate, phosphate, nitrate, citrate, lactate and alkyl sulfate salts.Such salts include stearylamine hydrochloride, soyamine chloride, stearylamine formate and N-tallowpropane diamine dichloride and stearamidopropyl dimethylamine citrate.

Preferred cationic surfactant materials include lauryl trimethyl ammonium chloride, stearyl trime thyl ammonium chloride, tri C8 l0 methyl ammonium chloride, tricetyl methyl ammonium chloride, tri C13 amine, and stearamido propyl dimethyl amine. Tricetyl methyl ammonium chloride is most preferred. 4 The cationic surfactant materials described above are available in the impure form as products of commerce. Use of the impure materials in certain hair care compositions surprisingly results in more difficult handling and processing.

The purified cationic surfactant materials useful in compositions of the invention are substantially free of impurities such as water and solvents such as isopropyl alcohol. ''Substantially free" as used herein means that the purified materials have less than 1% water or other undesirable solvent.

Hair Care Compositions The hair care compositions of the invention are stable compositions, which may be in the form of shampoos, conditioning shampoos, hair conditioners, or rinses.

Hair care compositions of the invention comprise from about 0.05% to about 10% of a purified cationic surfactant material.

Preferred hair care compositions of the invention further comprise a silicone conditioning agent which impart conditioning benefits to human hair when applied in the present compositions. (As used herein, the term ''silicone conditioning agent" refers to such silicone conditioning materials, singly or in combination.) Non-volatile silicones are preferred.

Preferred silicone conditioning agents include the polydimethylsiloxanes, more preferably, the linear polydimethylsiloxanes of the general formula: (CH3)3 SiO [Si(CH3)2O]n Si(CH3)3 wherein n is from 1 to 15,000, preferably from 20 to 7000. Preferred polydimethylsiloxanes are unsubstituted or are vinyl, phenyl, carboxy, alkoxy, mercapto, alkyl, or amino substituted. Particularly preferred silicone conditioning agents include the unsubstituted and the amino or alkoxy substituted linear polydimethylsiloxanes, and mixtures thereof.

Example of silicone oils useful in the present invention include Dow Corning 200 Fluid and Dow Corning Q2-8075 Aminofunctional Fluid (manufactured by the Dow Corning Corporation); Silicone Copolymer F-755 (manufactured by SWS Silicones Corp.), and SE 76 Silicone Gum (manufactured by General Electric). Polydimethylsiloxane conditioning agents are also disclosed in the following documents, all incorporated by reference herein: U.S. Patent 4,387,097, Bolich, Jr., issued June 7, 1983; British Specification 2,066,659, Abe, published July 15, 1981; Wendel, et al, "Organofunctional Silicones for Personal Care Applications", 98 Cosmetics & Toiletries 103-106 (1983); and Todd, et al., "Volatile Silicone Fluids for Cosmetics", 91 Cosmetics & BR< Toiletries 27-32 (1976).

One particularly preferred composition is a conditioning shampoo comprising from about 0.1% to about 10% of a purified cationic surfactant material, from about 0.5% to about 50% of a synthetic anionic surfactant, and water.

Surfactants useful in the shampoo compositions herein may be anionic, nonionic or amphoteric, such as ceteareth-20, steareth-20, sorbitan monoesters, and tallow betaines. Optional surfactant materials are described in the following documents, all incorporated by reference herein: M.

C. Publishing Co., McCutcheon's Detergents & Emulsifiers, (North American edition, 1979); Schwartz, et al., Surface Active Agents, Their Chemistry and Technology (1949); and U.S.

Patent 3,929,678, Laughlin, et al., issued December 30, 1975.

Preferred surfactants in shampoo compositions of the invention are anionic surfactants, particularly alkyl and alkyl ether sulfates. These materials have the respective formulae ROSO3M and RO(C2H4O)xSO3M wherein R is alkyl or alkenyl of about 10 to about 20 carbon atoms, x is 1 to 10, and M is a water-soluble cation such as ammonium, sodium, potassium and triethanolamine.

The alkyl ether sulfates useful in the present invention are condensation products of ethylene oxide and monohydric alcohols having about 10 to about 20 carbon atoms. Preferably, R has 14 to 18 carbon atoms in both the alkyl and alkyl ether sulfates. The alcohols can be derived from fats, e.g., coconut oil or tallow, or can be synthetic. Lauryl alcohol and straight chain alcohols derived from coconut oil are preferred herein. Such alcohols are reacted with 1 to 10, and especially 3, molar proportions of ethylen oxide and the resulting mixture of molecular species, having, for example, an average of 3 moles of ethylene oxide per mole of alcohol, is sulfated and neutralized.

Specific examples of alkyl ether sulfates of the present invention are sodium coconut alkyl trioxyethylene sulfate; lithium tallow alkyl trioxyqthylene sulfate; and sodium tallow alkyl hexaoxyethylene sulfate. Highly preferred alkyl ether sulfates are those comprising a mixture of individual compounds, said mixture having an average alkyl chain length of from about 12 to 16 carbon atoms and an average degree of ethoxylation of from about 1 to 4 moles of ethylene oxide.

Such a mixture also comprises from about 0 to 20% by weight C1213 compounds; from 60 to 100% by weight of C14 15 16 compounds, from about 0 to 20% by weight of C17 18 19 compounds; from about 3 to 30% by weight of compounds having a degree of ethoxylation of 0; from about 45 to 90% by weight of compounds having a degree of ethoxylation of from 1 to 4; from about 10 to 25% by weight of compounds having a degree of ethoxylation of from 4 to 8; and from about 0.1 to 15% by weight of compounds having a degree of ethoxylation greater than 8.

Additional examples of anionic synthetic detergents which come within the terms of the present invention are the reaction product of fatty acids esterified with isethionic acid and neutralized with sodium hydroxide where, for example, the fatty acids are derived from coconut oil; sodium or potassium salts of fatty acid amides of methyl tauride in which the fatty acids, for example, are derived from coconut oil. Other anionic synthetic detergents of this variety are set forth in U.S. Patents 2,486,921; 2,486,922; and 2,396,278.

Still other anionic synthetic detergents include the class designed as succinamates. This class includes such surface active agents as disodium N-octadecylsulfosuccinamate; tetrasodium N (1 ,2-dicarboxyethyl)-N-octadecylsulfo-succinamate; diamyl ester of sodium sulfosuccinic acid; dihexyl ester of sodium sulfosuccinic acid; dioctyl esters of sodium sulfosuccinic acid.

Other suitable anionic detergents utilizable herein are olefin sulfonates having about 12 to about 24 carbon atoms. The term "olefin sulfonates" is used herein to mean compounds which can be produced by the sulfonation of a-olefins by means of uncomplexed sulfur trioxide, followed by neutralization of the acid reaction mixture in conditions such that any sultones which have been formed in the reaction are hydrolyzed to give the corresponding hydroxy-alkanesulfonates. The sulfur trioxide can be liquid or gaseous, and is usually, but not necessarily, diluted by inert diluents, for example by liquid SO2, chlorinated hydrocarbons, etc., when used in the liquid form, or by air, nitrogen, gaseous SO2, etc., when used in the gaseous form.

The a-olefins from which the olefin sulfonates are derived are mono-olefins having 12 to 24 carbon atoms, preferably 14 to 16 carbon atoms. Preferably, they are straight chain olefins.

Examples of suitable 1-olefins include 1-dodecene; 1-tetradecene; 1-hexadecene; 1-octadecene; 1-cicosene and 1-tetracosene.

In addition to the true alkene sulfonates and a proportion of hydroxy-alkanesulfonates, the olefin sulfonates can contain minor amounts of other materials, such as alkene disulfonates depending upon the reaction conditions, proportion of reactants, the nature of the starting olefins and impurities in the olefin stock and side reactions during the sulfonation process.

A specific a-olefin sulfonate mixture of the above type is described more fully in the U.S.

Patent 3,332,880 of Philip F. Pflaumer and Adrian Kessler, issued July 25, 1967, titled "Detergent Composition", the disclosure of which is incorporated herein by reference.

Another class of anionic organic detergents are the ssalkyloxy alkane sulfonates. These compounds having the following formula:

where R, is a straight chain alkyl group having from 6 to 20 carbon atoms, R2 is a lower alkyl group having from 1 (preferred) to 3 carbon atoms, and M is a water-soluble cation as hereinbefore described.

Specific examples of fi-alkyloxy-alkane- 1 -sulfonates, or alternatively 2-alkyloxy-alkane-1-suifon- ates, having low hardness (calcium ion) sensitivity useful herein to provide superior cleaning levels under household washing conditions include: potassium-/-methoxydecanesulfonate, sodium 2-methoxytridecanesulfonate, potassium 2-ethoxytetradecylsulfonate, sodium 2-isopropoxyhexadecylsulfonate, lithium 2-t-butoxytetradecylsulfonate, sodium fi-methoxyoctadecylsulfonate, and ammonium-n-propoxydo-decylsulfonate.

Another suitable class of anionic surfactants are the water-soluble salts of organic, sulfuric acid reaction products of the general formula: R,-SO3-M wherein R, is chosen from the group consisting of a straight or branched chain, saturated aliphatic hydrocarbon radical having from 8 to 24, preferably 12 to 18 carbon atoms; and M is a cation. Important examples are the salts of an organic sulfuric acid reaction product of a hydrocarbon of the methane series, including iso-, neo-, ineso-, and n-paraffins, having 8 to 24 carbon atoms, preferably 12 to 28 carbon atoms and a sulfonating agent e.g., SO,, H2S04, oleum, obtained according to known sulfonation methods, including bleaching and hydrolysis.

Preferred are alkali metal and ammonium sulfonated C,2 ,8-n-paraffins.

Nonionic surfactants may also be present. Such surfactants are most commonly produced by the condensation of an alkylene oxide (hydrophilic in nature) with an organic hydrophobic compound, which is usually aliphatic or alkyl aromatic in nature. The length of the hydrophilic or poly- alkylene moiety which is condensed with any particular hydrophobic compounds can be readily adjusted to yield a water-soluble compound having the desired degree of balance between hydrophilic and hydrophobic elements.Such nonionic surfactants include polyethylene oxide condensates of alkyl phenols, condensation products of aliphatic alcohols with ethylene oxide, condensation products of ethylene oxide with a hydrophobic base formed by condensation of propylene oxide with propylene glycol, and condensation products of ethylene oxide with the product resulting from the reaction of propylene oxide and ethylene diamine. Another variety of nonionic surfactant is the non-polar nonionic, typified by the amine oxide surfactants. Preferred nonionic surfactants include ceteareth-20, steareth-20 and ceceth-2.

Zwitterionic surfactants can be exemplified by those which can be broadly described as derivatives of aliphatic quaternary ammonium, phosphonium, and sulfonium compounds, in which the aliphatic radicals can be straight chain or branched, and wherein one of the aliphatic substituents contains from about 8 to 18 carbon atoms and one contains an anionic watersolubilizing group, e.g., carboxy, sulfonate, sulfate, phosphate, or phosphonate.A general formula for these compounds is:

wherein R2 contains an alkyl, alkenyl, or hydroxy alkyl radical of from about 8 to about 18 carbon atoms, from 0 to about 10 ethylene oxide moieties and from 0 to 1 glyceryl moiety; Y is selected from the group consisting of nitrogen, phosphorus, and sulfur atoms; R3 is an alkyl or monohydroxyalkyl group containing 1 to about 3 carbon atoms; X is 1 when Y is a sulfur atom and 2 when Y is a nitrogen or phosphorus atom; R4 is an alkylene or hydroxyalkylene of from 1 to about 4 carbon atoms and Z is a radical selected from the group consisting of carboxylate, sulfonate, sulfate, phosphonate, and phosphate groups.

Examples include: 4-[N,N-di(2-hydroxyethyl)-N-octadecylammonioj-butane 1 -carboxylate; 5-[S-3-hydroxypropyl-S-hexadecylsulfonio]-3-hydroxypentane- sulfate; 3-[P,P-diethyl-P-3,6,9-trioxatetradexocylphosphonio]-2-hydroxy-propane 1-phosphate; 3-[N, N-dipropyl-N-3-dodecoxy-2-hydroxypropylammonio]-propane- 1 -phosphonate; 3-(N ,N-dimethyl-N-hexadecylammonio)propane- 1 -sulfonate; 3-(N,N-dimethyl-N-hexadecylammonio)-2-hydroxypropane- 1 -sulfonate; 4-[N,N-di(2-hydroxyethyl)-N-(2-hydroxydodecyl)ammonio]-butane- 1 -carboxylate; 3-[S-ethyl-S-(3-dodecoxy-2-hydroxypropyl)sulfonio]-propane- 1-phosphate; 3-[P,P-dimethyl-P-dodecylphosphonio]-propane-1-phosphonate; and 5-[N,N-di(3-hydroxypropyl)-N-hexadecylammonio]-2-hydrnxypentane- sulfate.

Other zwitterionics such as betaines are also useful in the present invention. Examples of betaines useful herein include the high alkyl betaines such as coco dimethyl carboxymethyl betaine, lauryl dimethyl carboxymethyl betaine, lauryl dimethyl alpha-carboxy-ethyl betaine, cetyl dimethyl carboxymethyl betaine, lauryl bis-(2-hydroxy-ethyl) carboxy methyl betaine, stearyl bis (2-hydroxy-propyl) carboxymethyl betaine, oleyl dimethyl gamma-carboxypropyl betaine, lauryl bis (2-hydroxypropyl) alpha-carboxyethyl betaine, etc. The sulfobetaines may be represented by coco dimethyl sulfopropyl betaine, stearyl dimethyl sulfopropyl betaine, lauryl dimethyl sulfoethyl betaine, lauryl bis-(2-hydroxy-ethyl) sulfopropyl betaine and the like; amido betaines and amidosulfobetaines, wherein the RCONH(CH)23 radical is attached to the nitrogen atom of the betaine are also useful in this invention.The amido betaines are preferred for use in some of the compositions of this invention. A particularly preferred composition utilizes an amido betaine, a quaternary compound, a silicone, a suspending agent and has a pH of from about 2 to about 4.

Example of amphoteric surfactants which can be used in the compositions of the present invention are those which can be broadly described as derivatives of aliphatic secondary and tertiary amines in which the aliphatic radical can be straight chain or branched and wherein one of the aliphatic substitutents contains from about 8 to about 18 carbon atoms and one contains an anionic water solubilizing group, e.g., carboxy, sulfonate, sulfate, phosphate, or phosphonate.

Examples of compounds falling within this definition are sodium 3-dodecylaminopropionate, sodium 3-dodecylaminopropane sulfonate, N-alkyltaurines such as the one prepared by reacting dodecylamine with sodium isethionate according to the teaching of U.S. Patent No. 2,658,072, N-higher alkyl aspartic acids such as those produced according to the teaching of U.S. Patent No. 2,438,091, and the products sold under the trade name "Miranol" and described in U.S.

Patent 2,528,378.

Another useful component of the silicone containing shampoo composition of the present invention is a suspending agent. Two preferred materials are xanthan gum and long chain acyl derivatives as well as other long chain materials.

Xanthan gum is an agent which can be used in the present compositions to suspend the silicone fluid. This biosynthetic gum material is commercially available and is a heteropolysaccharide with a molecular weight of greater than 1 million. It contains D-glucose, D-mannose and Dglucuronate in the molar ratio of 2.8:2.0:2.0. The polysaccharide is partially acetylated with 4.7% acetyl. This information and other is found in Whistler, Roy L. Editor Industrial Gums-Polysaccharides and Their Derivatives New York: Academic Press, 1973. Kelco, a Division of Merck & Co., Inc. offers xanthan gum as Keltrol. The gum is present at a level of from about 0.4% to about 3%, preferably from about 0.6% to about 1.2% in the compositions of the present invention.

Another suspending agent useful in the present compositions is any of several long chain acyl derivative materials or mixtures of such materials. Included are ethylene glycol esters of fatty acids having from about 16 to about 22 carbon atoms. Preferred are the ethylene glycol stearates, both mono and distearate, but particularly the distearate containing les than abut 7% of the monostearate. Other suspending agents found useful are alkanol amides of fatty acids, having from about 16 to about 22 carbon atoms, preferably about 16 to 18 carbon atoms.

Preferred alkanol amides are stearic monoethanolamide, stearic diethanolamide, stearic monoisopropanolamide and stearic monoethanolamide stearate.

Still other suitable non-acyl derivative suspending agents are alkyl (C 16-22) dimethyl amine oxides such as stearyl dimethyl amine oxide.

The suspending agent or mixture of agents is present at a level of from about 0.4% to about 5%, preferably from about 0.5% to about 2.5%. The suspending agent serves to assist in suspending the silicone material and may also give pearlescence to the product.

Another preferred hair care composition herein is a conditioning composition for human or animal hair. Such compositions also comprise from about 0.1% to about 5% of a purified cationic surfactant material. The conditioning compositions further comprise from about 0. 1 % to about 10% of a silicone conditioning agent and from about 0.1% to about 10% of a lipid vehicle material.

The lipid vehicle materials used in conditioning compounds herein are essentially water insoluble and contain hydrophobic and hydrophilic moieties. Lipid vehicle materials include naturally or synthetically-derived acids, acid derivatives, alcohols, esters, ethers, ketones, and amides with carbon chains of from 12 to 22, preferably from 16 to 18, carbon atoms in length. Fatty alcohols and fatty esters are preferred; fatty alcohols are particularly preferred.

Lipid vehicle materials among those useful herein are disclosed in Baileys Industrial Oil and Fat Products, (3rd edition, D. Swern, ed. 1979) (incorporated by reference herein). Fatty alcohols included among those useful herein are disclosed in the following documents, all incorporated by reference herein: U.S. Patent 3, 155,591, Hilfer, issued November 3, 1964; U.S. Patent 4,165,369, Watanabe, et al., issued August 21, 1979; U.S. Patent 4,269,824, Villamarin, et al., issued May 26, 1981; British Specification 1,532,585, published November 15, 1978; and Fukushima, et al., "The Effect of Cetostearyl Alcohol in Cosmetic Emulsions", 98 Cosmetics & BR< Toiletries 89-102 (1983). Fatty esters included among those useful herein are disclosed in U.S.

Patent 3,341,465, Kaufman, et al., issued September 12, 1967 also incorporated by reference herein.

Preferred esters for use herein include cetyl palmitate and glycerolmonostearate. Cetyl alcohol and stearyl alcohols are preferred alcohols. A particularly preferred lipid vehicle material is comprised of a mixture of cetyl alcohol and stearyl alcohol containing from abut 55% to about 65% (by weight of mixture) of cetyl alcohol.

The preferred conditioning compositions of the present invention further comprise a silicone containing material (specifically a polyalkylene oxide modified dimethylpolysiloxane, herein referred to as "dimethicone copolyol") which acts as an anti-resoiling agent. These dimethicone copolyols reduce deposition of lipid materials and cationic surfactant materials onto the hair.The dimethicone copolyols include those polyalkylene oxide modified dimethylpolysiloxanes of the following formulae:

and R'-Si(CH3)2-((O (CH3)2-[(O Si(CH3) ( C28i4)a ( C3H6)b R 3 wherein R is hydrogen, an alkyl group having from 1 to about 12 carbon atoms, an alkoxy group having from 1 to about 6 carbon atoms or a hydroxyl group; R' and R" are alkyl groups having from 1 to about 12 carbon atoms; x is an integer of from 1 to 100, preferably from 20 to 30; y is an integer of 1 to 20, preferably from 2 to 10; and a and b are integers of from 0 to 50, preferably from 20 to 30.

Optional Materials The hair care compositions of this invention preferably contain optional components in addition to those already discussed which may modify the physical and performance characteristics of the conditioning product. Such components include salts, buffers, thickeners, solvents, opacifiers, pearlescent aids, preservatives, fragrance, colorants, dyes, pigments, chelators, sunscreens, vitamins, and medicinal agents. Optional components that are among those useful herein are disclosed in U.S. Patent 4,387,090, Bolich, Jr., issued June 7, 1983, incorporated by reference herein.

Salts and buffers may be added to conditioning compositions in order to modify the product rheology. For example, salts such as potassium chloride and sodium chloride, may be added at levels of from about 0.001% to about 1%. Buffers, such as citrate or phosphate buffers, may also be used. Preferably the pH of the present conditioner compositions is from about 3 to about 10, more preferably from about 3 to about 7.

Thickening agents are also preferred optional components useful in hair care compositions herein. Such thickeners include nonionic thickening agents, incorporated at levels from about 0.1% to about 8%. Such agents are polymers which exhibit viscosities exceeding about 200 poises at lower shear (about 10-2 sec-1). Included among such polymers are polyoxyethylene, guar gum, methylcellulose, methyl hydroxy propyl cellulose, polypropyl cellulose, polypropyl hydroxy ethyl cellulose, hydroxy ethyl cellulose, starches and starch derivatives, and mixtures thereof.

Purification Process Solvent Acetonitrile is the preferred solvent for use in the purification process. Other solvents such as acetone or diethyl ether may also be used; however, larger amounts of these solvents are required to remove a like amount of impurity from the cationic surfactant material. Where acetonitrile is the sole solvent, at least about 0.5 mis/gm is required to achieve substantial purification. Below this level inadequate dissolution results in separation difficulties. Preferred processes use at least 5 ml/gm acetonitrile, more preferably at least 7 ml/gm.

Where other solvents are selected, at least about 2 mis/gm is required, preferably at least 10 mis/gm, more preferably at least 15 mis/gm for purification. Mixtures of acetonitrile and another solvent, an intermediate level may be acceptable, varying with the percentage of acetonitrile.

Mixtures containing 50% acetontrile or more are preferred.

Procedure The cationic surfactant materials of the invention are rendered substantially free of undesirable solvents, including water and other impurities by the following procedure.

The impure material is stirred with the requisite amount of solvent for from about 60 to about 120 minutes. The mixture is then filtered and washed with additional solvent. Suction is applied for from about 30 to about 60 minutes, during which time a filter cake is formed. The solid is then dried. A free-flowing white powder is left on the filter.

METHODS OF MANUFACTURE The processes for making compositions of the invention may be any of the conventional means known in the art with the purified cationic surfactant material used in place of impure material. Preferred methods are described in the examples.

EXAMPLE 1 About 1000 grams of unpurified tricetyl methyl ammonium chloride material was placed in a glass container. Acetonitrile (7000 ml) was added to the beaker and the mixture vigorously stirred, using a mechanical stirrer, for one hour. This mixture was then filtered on a Buchner funnel. The solid in the funnel was washed with additional 400-500 ml of acetonitrile. Suction was continued until the solid was essentially dry. It was removed from the funnel and spread in a flat glass pan and allowed to air dry for about 24 hours. Yield of the purified material was about 896 grams.

EXAMPLES Il-VII The following shampoo compositions representative for the present invention are prepared.

Component II Ill IV V VI vlrr Ammonium Lauryl Sulfate 12.00 12.00 12.00 15.00 8.00 8.00 Ammonium Laureth (3) Sulfate 4.00 4.00 4.00 4.00 8.00 8.00 Ammonium Xylene Sulfonate 2.20 2.20 2.20 3.00 -- - Cetearyl Alcohol 1.00 1.00 0.10 0.50 1.00 1.00 Giycol Distearate 0.75 2.50 0.75 0.75 0.75 0.75 Cocamide MEA 1.00 1.50 1.00 1.00 1.00 1.00 Xanthan Gum 0.75 -- 0.75 0.75 0.75 0.75 Dimethicone Fluid Viscosity 350 centistokes 1.80 1.80 1.80 1.80 1.80 1.80 Silicone Gum 1.00 1.00 1.00 1.00 1.00 1.00 lauryl Trimethyl Ammonium Chloride (purified) -- -- 0.75 0.75 -- - Tricetyl Methyl Ammonium Chloride (purified) 1.00 0.50 0.50 0.50 -- - Tri C8 1 0 Methyl Ammonium Chloride (purified) -- -- -- -- 2.00 - Tri C13 Amine ( pu ri fied ) -- -- -- -- -- 2.00 Color, Perfume, Preservative pH control2 and Water q.s. 100% These compositions all deliver good hair conditioning while also providing good cleaning.

EXAMPLE VIII A hair conditioner, according to the present invention, was made comprising: Component Weight % D5 cyclomethicone 2.00 SE-76 Silicone Gum 1 0.15 Silicone Copolymer F-755 2 0.50 Dow Corning 190 Silicone Surfactant 3 0.50 cetyl alcohol 1.25 stearyl alcohol 1.25 Lexamine S-13 (purified) 0.75 hydroxyethyl cellulose 0.50 fragrance 0.25 citric acid 0.13 preservative 0.03 distilled water q.s. 100% ': dimethicone gum, sold by General Electric stearoxydimethicone, sold by SWS Silicones Corporation 3: dimethicone copolyol 4 steramidopropyl dimethylamine All materials, except the preservative and fragrance, were added to the distilled water, maintained at a temperature of from 65"C to 740C. This mixture was then stirred for 15 minutes.

After the solution was cooled to approximately 49"C, the fragrance and preservative were added. The mixture was then cooled to approximately 38"C and milled under high shear for approximately 2 minutes using a conventional milling apparatus.

Approximately 20 g. of the hair conditioning product thus formed is applied to freshly shampooed and rinsed hair. The composition is then spread over the hair and allowed to stand for approximately 1 minute. Thereafter, the product is rinsed from the hair, leaving the hair with conditioning benefits.

In the above example, stearylamine, diethylaminopropyl stearamide, dimethyl stearamine, tridecylamine, ethyl stearamine, N-tallowpropane diamine, myristylamine, ethoxylated stearylamine, dihydroxyethyl stearylamine and arachidylbehenylamine are substituted, respectively, for the Lexamine S-13 stearamidopropyl dimethylamine, with substantially similar results.

EXAMPLE IX A hair conditioner, according to the present invention, is made comprising: Component Weight % D5 cyclomethicone 8.00 dimethicone oil 1.00 cetyl palmitate 1.00 glycerol monostearate 3.00 tristearyi methyl ammonium chloride (purified) 2.00 perfume 0.50 colorant 0.11 preservative 0.03 distilled water 84.36 A conditioning product, as comprised above, is made in a manner similar to that described in Example VIII. This product, when applied to human hair, is useful as a hair conditioner.

EXAMPLE X A hair conditioner, according to the present invention, is made comprising: Component Weight % stearoxy dimethicone 1.00 dimethicone oil (12,500 cs) 1.00 cetearyl alcohol 3.00 cetyl trimethyl ammonium chloride (purified) 2.00 hydroxy ethyl cellulose 0.50 Peptein 2000 1 0.50 Panthenol 2 0.50 fragrance 0.50 titanium dioxide 0.10 phosphoric acid 0.05 preservative 0.05 colorant 0.05 distilled water 90.75 hydrolyzed animal protein, sold by Geo. A. Hormel & Co.

2: pantothenyl alcohol, provitamin of the B-complex vitamin pantothenic acid, sold by Hoffman LaRoche, Inc.

A hair conditioning product is made in a manner similar to that described in Example Veil, except for processing of the cyclomethicone/dimethicone gum materials. These silicone agents are premixed under heat and agitation to form a gum solution. The gum solution is added to the conditioning product batch mix after the batch solution is cooled to approximately 48"C. The final product, when applied to human hair, is useful as a conditioning agent.

Claims (12)

1. A hair care composition comprising a purified cationic surfactant material selected from the group consisting of:

wherein R, is an aliphatic group having from about 8 to about 22 carbon atoms, R2, R3 and R4 are hydrogen or short chain alkyl groups having from about 1 to about 4 carbon atoms, and X is an anion selected from the group consisting of acetate, halogen, phosphate, nitrate, and alkyl sulfate radicals;

wherein R1, R2 and R3 are aliphatic groups having from about 8 to about 22 carbon atoms, R4 is hydrogen or an alkyl group containing from about 1 to about 4 carbon atoms and X is as defined above; (c) salts of primary amines; (d) salts of secondary amines; (e) salts of tertiary amines; (f) and mixtures thereof, wherein said material is substantially free of solvents and water.

2. A hair composition according to Claim 1 in the form of a shampoo.

3. A shampoo composition according to Claim 2 comprising from about 0.05% to about 10% of a purified cationic surfactant material.

4. A shampoo composition according to Claim 1 wherein the purified cationic surfactant material is selected from the group consisting of tricetyl methyl ammonium chloride, lauryl trimethyl ammonium chloride, and tri C8-Cl9 methyl ammonium chloride and mixtures thereof.

5. A shampoo composition according to Claim 4 wherein the purified cationic surfactant material is tricetyl methyl ammonium chloride.

6. A shampoo composition comprising: (a) from about 0.1 h to about 5% of a purified cationic surfactant material according to Claim 4; (b) from about 0.5% to about 5% of a siloxane conditioning compound; (c) from about 5% to about 50% of a synthetic anionic surfactant; (d) from about 0.4% to about 5% of a suspending agent; and (e) water.

7. A hair care composition according to Claim 1 in the form of a conditioner.

8. A conditioning composition according to Claim 7 comprising from about 0.5% to about 10% of the purified cationic surfactant material.

9. A conditioning composition comprising: (a) from about 0. 1 % to about 5% of a purified cationic surfactant material (b) from about 0.1% to about 10% of a silicone conditioning agent; and (c) from about 0.1 vó to about 10% of a lipid vehicle material.

10. A conditioning composition according to Claim 9 additionally comprising from about .01% to about 10% of a dimethicone copolyol.

11. A hair care composition comprising a purified cationic surfactant material according to Claim 1 wherein the material is purified by a process comprising the steps of: (a) washing an impure cationic surfactant material with an organic solvent; (b) apply suction to remove the filtrate; and (c) drying the solid.

12. A shampoo composition comprising: (a) from about 0.5% to about 5% of a purified cationic surfactant material, purified according to Claim 11; (b) from about 0.5% to about 5% of a siloxane conditioning compound; (c) from about 5% to about 50% of a synthetic anionic surfactant; (d) from about 0.4% to about 5% of a suspending agent; and (e) water.