US3018223A - Aluminum dihydroxy-titanium dilactate antiperspirant - Google Patents

Description

3,013,223 ALUMINUM DHYDRGXYEITANTJM DZLAC- TA'TE ANHPERSPIRANT Bernard Siegal, Elizabeth, NIL, assignor to Bristol-Myers Company, New York, N.Y., a corporation of Betaware No Drawing. Filed Feb. 24, 1958, Ser. No. 716,836 7 Claims. (Cl. 167-90) This invention pertains to antiperspirant compositions and more particularly to compositions for inhibiting or retarding the flow of perspiration, comprising the reaction product of titanium lactate and an aluminum-containing material.

Antiperspirants, as opposed to simple deodorants, which merely mask offensive odors, act to eliminate or retard the flow of perspiration from the sweat glands. Such materials, to be useful in commercial antiperspirant formulations, must be free of any tendency to cause skin irritation or sensitization and should not stain, weaken, char or otherwise damage clothing fabric with which they come into contact in the course of recurrent normal use.

Many prior art antiperspirants are commonly defective in one or more of the foregoing respects. For example, aluminum salts of strong inorganic acids, such as aluminum chloride and aluminum sulfate are effective antiperspirants by reason of their powerful astringent action but these salts, when present in effective concentrations, produce skin irritation and extensive fabric damage. Aluminum salts of some strong organic acids have also been suggested as antiperspirants, e.g., the sulfamate, sulfonate and alkyl sulfonates. Aluminum salts of other organic acids, previously suggested as antiperspirants, include the aluminum salts of such sulfonated organic acids as the phenolsulfonate (sulfocarbolate), the sulfoacetate, the methionate (methane disulfonate) or salts of Weaker organic acids, such as the acetate, lactate, acetotartrate, formate and palmitate. Various aluminum hydroxide derivatives have also been used or advanced as antiperspirants, e.g., aluminum chlorhydroxide, aluminum calcium chlorhydroxide complex, and aluminum chlorhydroxyacetate. Th aluminum salts of the weaker organic acids'have been found to be inferior in their antiperspirant activity as have certain of the aluminum hydroxide derivatives. Others of the latter type, notably aluminum chlorhydroxide, although efiicient antiperspirants, result in appreciable degrees of fabric damage and staining. The staining produced by aluminum chlorhydroxide and similar materials is believed to be due to a deposition upon the clothing fabric of aluminum hydroxide. The latter material, being relatively insoluble in water, is not removable by washing. This tendency to cause insoluble stains, together with the corrosive nature of the aluminum salts of strong acids, constitutes a major disadvantage when aluminum-containing compounds are considered for incorporation in antiperspirant compositions.

Therefore it is an object of the present invention to provide an aluminum-containing compound having a high antiperspirant activity but which does not possess the corrosive properties of prior art aluminum compounds.

It is another object of the present invention to provide an effective antiperspirant composition which is free from any tendency to stain or otherwise damage clothing fabrics.

It is a further object of the invention to provide an aluminum-containing antiperspirant composition which is free from any tendency to irriate or sensitize the skin.

It is still another object of the invention to provide an antiperspirant and deodorant compound which is watertates Patent 3,i8,223 Patented Jan. 23, 1962 soluble and compatible with the usual ingredients of antiperspirant cosmetic compositions.

Other objects and advantages of the invention will appear in the following description.

It has been disclosed in co-pending patent application Serial No. 691,131, of E. L. Saul and B, Siegal, filed October 21, 1957, that the titanium salts of lactic acid, hereinafter termed titanium lactate, possess antiperspirant activity. It has now been found that titanium lactate may be reacted with an aluminum-containing material to produce a reaction product, hereinafter referred to as aluminum titanium lactate, which possesses an antiperspirant activity substantially equal to or greater than most prior art antiperspirants with the exception of the more corrosive aluminum salts such as aluminum chloride or aluminum sulfate. However, aluminum titanium lactate exhibits few or none of the defects commonly found in such prior art antiperspirants. Aluminum titanium lactate is water-soluble and therefore lends itself readily to incorporation in aqueous based cosmetic compositions. Moreover, antiperspirant compositions containing aluminum titanium lactate do not irritate or sensitize the unbroken skin when repeatedly applied thereto.

It has also been found that aluminum titanium lactate may be prepared in a number of difierent ways. A preferred method of preparing aluminum titanium lactate comprises reacting titanium lactate and aluminum hydroxide. For example, the following procedure was utilized in preparing an aluminum titanium lactate suitable for incorporation in an antiperspirant composition.

Fourteen (14) grams of titanium lactate powder were added to water in a sufiicient quantity to dissolve the titanium lactate. To the titanium lactate solution was added 20.33 grams of commercial aluminum hydroxide gel and the mixture stirred with heating to about C. until the reaction was substantially complete as indicated by the substantially complete disappearance of the insoluble aluminum hydroxide, A suitable titanium lactate is that manufactured and sold by the E. I. du Pont de Nemours & Co. under the trademark Tilac. A suitable aluminum hydroxide gel is manufactured and sold by the Reheis Co. under the designation Aluminum Hydroxide Wet Gel F500. The latter material contains about 9 percent by weight of aluminum oxide, A1 0 20.33 grams of the aluminum hydroxide gel thus contains about 1.83 grams of A1 0 This reaction resulted in the production of about 15.0 grams of aluminum titanium lactate in an aqueous solution. Such solutions may be used directly for the preparation of antiperspirant cosmetic compositions or they may be concentrated to any desired degree.

Suitable compositions have also been prepared in a similar manner using other commercially available aluminum hydroxide wet gels, such as Reheis Wet Gel F1000 containing from 9.5 to 10.5 percent by weight of aluminum oxide or Reheis Wet Gel F2000 containing from 12.5 to 13.5 percent by weight of aluminum oxide. Dried aluminum oxide gels may also be utilized, useful products having been obtained by reacting titanium lactate in water solution with Reheis Dried Gel F2000, containing a minimum of 50 percent by Weight of aluminum oxide and Reheis Dried Gel F1000, containing a minimum of 51.5 percent by weight of aluminum oxide.

Aluminum titanium lactate may also be prepared by the reaction, in aqueous solution between titanium lactate and an aluminum alkoxide, such as the methoxide, ethoxide, isopropoxide or t-butoxide. Thus, aluminum titanium lactate has been prepared by slowly adding aluminum isoproxide to an aqueous solution containing 40 percent, by weight thereof, of titanium lactate. The

reaction proceeds at ordinary temperatures until completion as indicated by the appearance of a precipitate of aluminum hydroxide caused by reaction of an excess of aluminum isopropoxide with water. Before the end point of the reaction is reached, the reaction mass remains clear due to the substantially instantaneous reaction with titanium lactate of the aluminum hydroxide produced by the decomposition of the aluminum alkoxide when contacted with Water.

Another useful procedure for the preparation of aluminum titanium lactate comprises reacting titanium lactate with a complex compound of an aluminum alkoxide chelated with an alkyl ester of a betaor gamma-ketocarboxylic acid. Suitable esters include the alkyl esters of acetoacetic acid or acetopropionic acid (levulinic acid). Both of the latter compounds have been chelated with aluminum isopropoxide and the chelated aluminum compound reacted, in aqueous solution, with titanium lactate to produce a water-soluble reaction product which possesses marked antiperspirant activity.

Still other aluminum compounds have been used in the preparation of aluminum titanium lactate. For example, an aqueous solution containing 15.2 grams of titanium lactate was partially neutralized to a pH of about 5.5 and 6.1 grams of anhydrous aluminum sulfate were added with agitation and heating to about 50 C. with the production of about 12.2 grams of aluminum titanium lactate. The latter material has been prepared in a similar manner with other aluminum salts substituted for aluminum sulfate. Thus, aluminum chloride, aluminum nitrate, aluminum sulfamate, aluminum chlorhydroxyacetate, aluminum sulfocarbolate and aluminum thiocyanate have all been used to prepare aluminum titanium lactate. For example, in the case of each of these aluminum salts, an aqueous solution containing 15 percent, by weight thereof, of titanium lactate was prepared and adjusted to a pH of about 7.0 by the addition of a suitable alkaline material, such as sodium hydroxide. Approximately 15 grams of sodium hydroxide were required per 100 grams of titanium lactate. To the partially neutralized titanium lactate solutions there was added, in the case of each of the aluminum salts, 5 percent, by weight of solution, of the aluminum salts and the solution was heated, with agitation to about 50 C. Addition of the acid salts lowered the pH values of the solutions to between about 2.7 and 3.2, depending upon the salt used.

These reaction masses may be used directly in the preparation of antiperspirant formulations. Each was found to have a high order of antiperspirant activity and, with the exception of the compositions prepared with aluminum chloride and with aluminum nitrate, to be substantially free of any tendency to damage fabric. The compositions containing the products of the reaction between titanium lactate and aluminum chloride or aluminum nitrate were found to possess some tendency to cause a weakening of fabric tensile strength. It is believed that this tendency is due to the presence, in the unpurified reaction masses, of the chloride and nitrate ions. The observed fabric weakening is not greaterthan that produced by prior art antiperspirant compositions containing these ions.

A still further procedure for preparing aluminum titanium lactate comprises the reaction of metallic aluminum, for example, in a powder or dust form, with titanium lactate in an aqueous solution. The titanium lactate concentration may vary from a fraction of a percent by weight of solution to substantial saturation, the amount of titanium lactate preferably being slighly in excess of the stoichiometric amount in order that completion of the reaction may become evident by the disappearance of the aluminum metal. Using aluminum powder, a temperature of 100 C. and a reaction time of 24 to 36 hours has been found to result in a sub- 4 stantially complete reaction of stoichiometric amounts of reactants.

It is believed that the reaction product of each of the aforementioned reactions is a compound wherein two aluminum atoms are combined with three titanium lactate moieties according to the following structural formula:

II o H CH3 3 This material, the aluminum salt of titanium lactate, herein termed aluminum titanium lactate, is more correctly identified as aluminum dihydroxytitanium dilactate. My belief that the foregoing formula accurately represents the chemical structure of the products of these reactions is substantiated by the results of quantitative analyses. Thus, a reaction mass was prepared by reacting, in 200 milliliters Water, 0.7 gram of aluminum dust and 11.6 grams of the aforementioned DuPont Tilac material which contained, by analysis, 86.5 percent by weight of titanium lactate. The reaction was continued, on a steam bath, for a period of approximately two and one-half weeks in order to insure con-- pletion of the reaction. Assuming that the reaction product, aluminum titanium lactate has the postulated molecular structure consisting of two aluminum atoms and three titanium lactate moieties and having a molecular weight of 834, the theoretical concentration of aluminum titanium lactate was 6.50 percent by weight of the reaction mass, i.e., 65 mg./ml. Titanium was separated and analyzed by the standard cupferron (ammonium N-nitrosophenylhydroxylamine) method, giving, for four separate analyses, an average titanium dioxide concentration of 1.980 percent by weight of solution. Based upon the postulated molecular structure, this corresponds to an average aluminum titanium lactate concentration of 6.88 percent, a deviation from the theoretical value which is within the limits of unavoidable experimental error.

Since the postulated three titanium lactate moieties contain a total of six reactive hydroxyl hydrogen atoms, it seems certain that two trivalent aluminum atoms are required per molecule of aluminum titanium lactate. This assumption is further substantiated by a representative laboratory experiment wherein a 1.0727 gram portion of the same aluminum dust-titanium lactate reaction product was titrated with 0.1 N sodium hydroxide solution. This titration gave a generally S-shaped titration curve, the data for which are given in Table I.

A curve erected upon the data of Table I shows two separate inflection points, at pH values of approximately 7.2 and 10.3 corresponding, respectively, to alkaline volumes of 2.50 ml. and 5.00 ml. This double inflection in the titration curve is believed to result from the neutralization, at each inflection point of one-half of the compound being titrated. Moreover the concentration of aluminum titanium lactate calculated from the data of Table I is 6.46 percent by weight of solution, which agrees, within the limits of experimental error, with the theoretical value for a molecule of the postulated structure. Similar analyses of aluminum titanium lactate made in accordance with the other procedures described herein also give results which indicate that the actual structure of aluminum titanium lactate is substantially as postulated.

Inasmuch as aluminum titanium lactate is extremely soluble in water, its antiperspirant properties may be utilized to advantage by dissolving the compound in water or other suitable solvent, such as water-alcohol mixtures. Such compositions containing upwards of from about 5 percent by weight thereof of aluminum titanium lactate are especially useful and those having an aluminum titanium lactate concentration of from about to about 20 percent by weight are particularly desirable, an aluminum titanium lactate concentration of about percent by weight being preferred. The pH of a substantially impurity-free aqueous solution of aluminum titanium lactate varies very little with concentration. Thus, the pH of aqueous solutions containing from about 5 to about 45 percent by weight of aluminum titanium lactate has been observed to vary between about 3.8 and about 4.0.

The aqueous reaction masses containing aluminum titanium lactate may be used directly in the preparation of antiperspirant compositions. Moreover, it is not necessary that the reactants be present in stoichiometric amounts. Thus, highly useful compositions may be produced by using less than the stoichiometric amount of aluminum-containing material, thereby resulting in mixtures of aluminum titanium lactate with titanium lactate and/ or the neutralized salts thereof.

Fabric damage tests show that, with the aforementioned exception in respect to compositions containing chloride or nitrate ions, compositions containing aluminum titanium lactate, as well as compositions containing mixtures of aluminum titanium lactate with titanium lactate and/or a neutralized salt thereof, such as sodium titanium lactate, exhibit very little fabric damage, and, in this respect, represent a marked advance over a great many prior art antiperspirant compounds. Thus, tests were performed comparing the weight load necessary to break fabrics treated, on the one hand, with the novel compositions of this invention, and, on the other hand, with aluminum chlor'nydroxide, a common ingredient in commercial antiperspirant compositions. These tests, given in Table H below, were performed with an Amthor Tensile Strength Tester, Type 254, sold by Amthor Testing Instrument Co., Inc. of Brooklyn, New York. The testing machine was set for a capacity of O to 100 lbs. Ten (10) strips of cotton fabric measuring inches x 4 inches, were used for each test solution and the average loss of tensile strength determined. In Table II the breaking load is given in arbitrary scale units and the concentrations of the test compositions, which are simple aqueous solutions, are expressed in percent by weight.

It will be noted that the reduction of the average percent loss of strength of the fabrics treated with the novel compositions of the invention, as compared to the fabrics treated with aluminum chlorhydroxide, varies from over eight-fold for a composition comprising a 5050 mixture of titanium lactate and aluminum titanium lactate to sixty-fold for a composition comprising aluminum titanium lactate. The pH of the aluminum chlorhydroxide solution used for the tests reported in Table II was about 3.9. The pH of the aluminum titanium lactate solutions was about 4.0 and that of the mixtures of aluminum titanium lactate and titanium lactate was about 3.2.

The aluminum titanium lactate used in the test compositions of Table II was prepared by reacting with titanium lactate Reheis Aluminum Hydroxide Wet Gel F500. The aluminum titanium lactate compositions of Table II contain antiperspirant compounds in the amount of only 15 percent, as compared to the aluminum chlorhydroxide composition which contained 20 percent of the antiperspirant compound. However, it has been found that, in the case of compositions containing aluminum titanium lactate alone or in admixture with titanium lactate or mixtures of titanium lactate and the sodium salt thereof, where the aluminum titanium lactate constitutes at least about 50 percent by weight of the total antiperspirant ingredients, an increase of total antiperspirant content above about 15 percent does not increase antiperspirant activity to a degree sufiicient to economically warrant the use of substantially higher concentrations. On the other hand, current commercial aluminum chlorhydroxide-contain'mg antiperspirant compositions commonly utilize about 20 percent by weight of the active ingredient. Hence, the data given in Table II represent realistic comparisons of practical value. An average loss of 20 percent, as determined by this particular test, is considered acceptable by nationally recognized standards.

In determining the relative freedom from damage of clothing fabrics treated with compositions of the invention as compared to the damage caused by several prior art compositions, such as aluminum chloride, aluminum sulfate and aluminum chlorhydroxide, further tests were employed to duplicate actual use conditions. Thus, samples of cotton fabric were washed, rinsed, dried, ironed, and then treated with predetermined amounts of test compositions. The treated cloth was then dried under controlled conditions and inspected for damage after which it was again rinsed with water, dried, ironed and again inspected for damage. Using such a test procedure, it was shown that the antiperspirant compositions containing aluminum titanium lactate were substantially free from any tendency to damage fabric in contradistinction to the prior art antiperspirants tested which resulted in various degrees of severe fabric damage.

A similar use test procedure was established to determine the fabric staining propensities of the compositions of the invention and these tests showed that the compositions are essentially free of any tendency to stain fabrics to which they are applied. Whatever slight staining is caused by the novel compositions of the invention is easily removable by washing the fabric with water due to the high degree of water-solubiL ty of these compositions.

Other fabrics may be substituted for the cotton fabric in the above tests with similar results.

The *antiperspirant activity of aluminum titanium lactate has been established by a great number of human in vivo tests. For example, the results of the topical application to the skin of aluminum titanium lactate, in a simple water solution containing 15 percent by weight of the antiperspirant compound, are given in Table III wherein the antiperspirant activity of aluminum titanium lactate is compared to that of aluminum chlorhydroxide, an effective antiperspirant in common use, and also to that of a partially neutralized aqueous solution of titanium lactate. The compositions containing the latter two compounds were also in the form of aqueous solutions containing 15 percent by weight of the active ingredient.

TABLE III TABLE V Composition Titanium LactnterAlurninum Titanium Lactate Ratio Subject No. Subject No. Aluminum Aluminum Partially Chlor- Titanium N eutrali zed 1:1 1/3:'1 0:1 hydroxide Lactate Titanium Lactate The antiperspirant activities of the test solutions were established by means of a standardized test procedure wherein an area of the forearm of a test subject was exposed for 1 hour to the test solution contained in an inverted cup which was held against the arm. The forearm was then washed and an anhydrous mixture containing castor oil, iodine and starch was applied whereupon a dark blue spot appeared at the site of each active sweat gland.

The measurement of antiperspirant activity depends on many variables, a number of which depend on the individual test subject and are therefore not susceptible to easy reproduction in a large test population. In order to minimize this dilficulty, the activity values given in Table III are based upon the measured activity, for each individual test subject, of aluminum chlorhydroxide. The activity of the latter compound was arbitrarily assigned a value of 100, hence the antiperspirant activity values of a test composition may be determined by use of Equation I:

a=100x/N (I) where a is the activity value of the composition under test, x is the number of dark spots observed in ,an area of a certain size treated with the test composition and N is the number of dark spots produced in an area of an equal size treated with aluminum chlorhydroxide.

The partially neutralized titanium lactate composition of Table III had a pH of 3.2 and consisted of a mixture of titanium lactate and its sodium salt in a ratio of about 66 parts of titanium lactate to about 34 parts of the sodium salt.

Table IV shows that aluminum titanium lactate in a concentration of about percent by weight is comparable in antiperspirant activity to higher concentrations of the other antiperspirant compounds of Table III. Thus, in the compositions of Table IV, the aluminum titanium lactate compositions had an active ingredient concentration of 15 percent whereas the compositions containing aluminum chlorhydroxide and titanium lactate-sodium titanium lactate mixtures had active ingredient concentrations of percent.

The antiperspirant effectiveness of compositions containing both aluminum titanium lactate and titanium lactate is illustrated in Table V wherein the activities are given for aqueous compositions containing 15 percent by weight of total antiperspirant, and having titanium lactate: aluminum titanium lactate ratios of 1:1, 1/3:1 and 0.1 respectively. In each instance, the reported activity is in reference to a standard aluminum chlorhydroxide activity value of 100.

TABLE VI Test No Composition I Activity 1 {12% Aluminum titanium lactate 1 100 3% Partially neutralized titanium lactate-..

(a) 12% Aluminum titanium lactate 1 89 2 3% Partially neutralized titamum lactate- (b) 12% Aluminum titanium lactate 100 3% Titanium lactate 3 {12% Aluminum titanium lactate Z 3% Titanium lactate (a) 12% Aluminum titanluml tate 3 %Titanium lactate 4 (b) 7.5% Aluminum titanium lactate 95 7.5% Titanium lactate (c) 15% Aluminum titanium lactate L Reaction product of titanium lactate and aluminum sult 2 Reaction product of titanium lactate and alummum oxide.

The material designated in Table VI as Partially neutralized titanium lactate was actually present as a mix ture of titanium lactate and the mono-sodium salt thereof clue to the equilibrium between these species at the pH of the solution. The relative amounts of titanium lactate and the sodium salt at the specified pH are determinable by the procedure disclosed in the aforementioned copending patent application Serial No. 691,131. Thus, the specific Partially neutralized titanium lactate composition given in Table VI, consisted of a mixture of about 66 parts by Weight of titanium lactate to about 34 parts of mono-sodium titanium lactate.

Although the observed test results reported in Tables III-VI show, in some instances, antiperspirant activities for the novel compositions less than that of the reference material, aluminum chlorhydroxide, it should be recognized that in tests of this nature the measurable antiperspirant activities are subject to wide limits of experimental error. Moreover, even if the observed values accurately represent the actual activity values of the novel compositions, these values are substantial and are soiliciently great to make the use of these materials desirable in antiperspirant formulations. Moreover the extremely small extent of any deleterious eifects upon clot-hing fabric to which the novel compositions are applied renders these compositions highly superior to many prior art compositions which result in varying degrees of severe fabric damage or staining.

Furthermore, although many prior art antiperspirants are highly irritating to the skin, the novel compositions of the invention have been found to be free of such defects. Thus, Draize repeat insult patch test studies were performed wherein a cosmetic formulation, having an antiperspirant content in accordance with compositions 1 and 2(a) of'Table VI, was successively applied to the intact skin of 25 human subjects on alternate days for a total of 15 applications, each application being of 48 hours duration. The cosmetic vehicle was that given in Example IV hereinbelow. No irritation or sensitization was observed.

Various forms of antiperspirant formulations, other than simple water solutions may be prepared by utilizing, as the active antiperspirant ingredient, the novel compositions of the invention. For example, cosmetic formulations in the form of creams, alcohol sprays, clear or emulsified lotions and semi-solid sticks may be made. The cream and lotion formulations may be in the form of thickened aqueous compositions or, if desired, they may be in the form of emulsions of either the water-in-oil or oil-in-water type, wherein the antiperspirant component is dissolved in the aqueous phase. The oil phase of such emulsions may comprise materials commonly used in the cosmetic arts, such as natural synthetic oil, fats or waxes, such as mineral oil, various vegetable oils, polyglycols, silicon es, stearic acid, cocoa butter, lanolin, paraffin, ceresin wax, spermaceti, beeswax,.a higher fatty alcohol, such as cetyl alcohol, glycostearin, certain polyethylene glycols or various synthetic hydrocarbon waxes. Any compatible emulsifying agent may be utilized to stabilize such emulsions and may be, for example, of the non-ionic type such as partial esters of fatty acids with glycerol, glycols or other polyhydric alcohols, the polyoxyethylene ethers, polyoxyethylene glycol fatty acid esters, sorbitan esters of fatty acids and polyethylene propylene oxides. Anionic emulsifiers are also useful, for example, alkali metal, alkaline earth metal or amine salts of alkyl sulfuric acid, such as sodium laurylsulfate, magnesium laurylsnlfate or triethanolamine laurylsulfate. The emulsifiers may also be of the cationic type such as various salts of polyoxyethylene amines. Suitable humectants, perfumes or coloring matter may be added as desired. Various devices of suitable nature may be utilized for the packaging and dispensing of these compositions. For example, roller type dispensers are admirably suited for the packaging and dispensing of the lotion and emulsion type formulations. The relatively fluid water and water-alcohol based formulations may be effectively packaged in pressurized containers and dispensed therefrom in the form of aerosols, foams or liquid drops or streams.

Useful antiperspirant formulations including aluminum titanium lactate are described in the following specific examples wherein the amounts of the various ingredients are given in percentage by weight.

A trademark of Atlas Powder Co., Wilmington, Delaware, for a polyoxyethylene ether.

The composition of Example I is an alcohol spray and may be prepared by forming an aqueous solution of aluminum titanium lactate by the aluminum oxide or aluminum metal method described hereinabove. The polyoxyethylene ether is dissolved in the remainder of the water and the glycerine, alcohol, the trichlorophenol derivative and perfume are added, each ingredient being dissolved before the next is added. The latter solution is then added, with stirring, to the aluminum titanium lactate while stirring and dissolving each ingredient before the next is added.

Example II Component Percent Aluminum titanium lactate 12.0 Sodium titanium lactate 3.0 Sodium sulfate 5.0 Glyceryl monostearate 20.0 Cetyl palmitate 3.0 Petrolatum 2.0 Cetyl alcohol 1.5 Beeswax 1.0 Glycerine 4.0 Perfume 0.3 Water 48.2

The formulation of Example II is a cream and may be prepared by heating the glyceryl monostearate, cetyl palmitate, petrolatum, cetyl alcohol and beeswax to 75 C. with stirring until melted. The glycerine is heated, to gether with a portion of water, to 75 C. and this mixture is added to the aforementioned non-aqueous mixture with continuous stirring. To the remaining portion of the Water there is added 15 grams, per 100 grams of the final composition, of sodium titanium lactate, together with 5 grams, per 100 grams of the final composition, of aluminum sulfate and the solution heated to 50C. The aluminum sulfate thereby reacts with a portion of the sodium titanium lactate to form about 12 grams of aluminum titanium lactate and 5 grams of sodium sulfate, the sodium titanium lactate remaining unreacted to the extent of about 3 grams. The solution containing aluminum titanium lactate is then added to the emulsion and the mixture cooled with stirring to 40 C. at which point the perfume may be added.

Example III Component: Percent Aluminum titanium lactate 15.0 Glyceryl monostearate 3.5 Brij 35 3.5 Perfume 0.3 Water 77.7

The composition of Example 111 is an emulsified lotion and may be prepared by heating a portion of the Water to C. and adding thereto with stirring the glyceryl monostearate and the fatty ether derivative. The resulting emulsion is cooled to 50 C. at which time the remainder of the Water containing the aluminum titanium lactate dissolved therein is added with stirring. The mixture is then cooled to 40 C. and the perfume added.

A trademark of Atlas Powder (30., Wilmington, Delaware, for polyoxyethylene sorbitan fatty acid ester.

The formulation given in Example IV is a clear lotion and may be prepared by dispersing the hydroxyethylcellulose in a portion of the Water with stirring. The fatty ester and perfume are dissolved in the remaining water in which the aluminum titanium lactate is also dissolved, and this solution is then added, with stirring, to the dispersion.

1 1 Example V Components: Percent Aluminum titanium lactate 15.0 Emcol 64 1 25.0 Ethanol 20.0 Propylene glycol 2.0

Polyethylene glycol (average molecular weight 350) 6.0 Perfume 0.3 Water 31.7

A trademark of Emulsol Corp., Chicago, Illinois, for a fatty acid amine condensate.

The formulation of Example V is a semi-solid cream stick and may be prepared by melting fatty acid amine condensate and adding thereto the propylene glycol and polyethylene glycol while maintaining the mixture at a temperature of 63 C. To this mixture is added, with stirring, a solution of the aluminum titanium lactate in the water Which has been heated to 65 C. This solution may be prepared by adding to the Water about 14.0 grams of titanium lactate and about 3.7 grams of Reheis aluminum hydroxide Dried Gel No. F2000, the latter containing a minimum of 50 percent by weight of aluminum oxide. These materials react to form about 15 grams of aluminum titanium lactate. The alcohol and perfume are then added and the mixture stirred until homogeneous after which it may be poured into stick molds at a temperature from about 60 to about 63 C.

It is to be understood that the foregoing examples and description are given merely to illustrate the novelty and utility of the invention and are not to be construed as limiting the broad principles thereof which may be modified by those skilled in the art without departing from the spirit and scope of the invention.

What is claimed is:

1. Aluminum dihydroxytitanium dilactate.

2. An antiperspirant composition comprising aluminum dihydroxytitanium dilactate and a carrier therefor.

5 3. An antiperspirant composition comprising aluminum dihydroxytitanium dilactate and an aqueous carrier therefor.

4. An antiperspirant and deodorant composition comprising a cosmetic aqueous-containing carrier having as the active ingredient an antiperspirantly effective amount of aluminum dihydroxytitanium dilactate dissolved in the aqueous portion thereof.

5. A composition according to claim 4 wherein the aluminum dihydroxytitanium dilactate comprises at least about 5 percent by weight of the aqueous portion of the carrier.

6. The method of inhibiting perspiration which comprises applying to the skin a composition comprising aluminum dihydroxytitanium dilactate.

7. The method of inhibiting perspiration which comprises topically applying to the skin an aqueous composition comprising at least about 5 percent, by weight of the composition, of aluminum dihydroxytitanium dilactate.

References Cited in the file of this patent UNITED STATES PATENTS 2,236,387 Wallace Mar. 25, 1941 2,707,667 Severn May 3, 1955 OTHER REFERENCES Grote: Drug and Cos. Ind. 59:6, December 1946, pp. 776, 777, 872-875. De Navarre: The Chemistry and Manuf. of Cosmetics,

D D. Van Nostrand Co., New York, 1941, page 261.

UNITED STATES PATENT OFFICE CERTIFICATION OF CORRECTION Patent No. 3 018 a 223 Bernard Siegal January 23, 1962 It is hereby certified that error appears in the above numbered patent requiring correction and that the said Letters Patent should read as corrected below.

Column 1 line 69, for "irriate" read irritate column 2, line 71 for "isoproxide" read isopropoxide column 3, line 70, for "slighly" read slightly column 4, lines 7 to 15, the structural formula should appear as shown below instead of as in the patent:

column 7, lin e 41, for "sodium" read mono-sodium Signed and sealed this 26th da of June 1962,

(SEAL) Attest:

ERNEST W. SWIDER Attesting Officer DAVID L. LADD Commissioner of Patents

Claims (2)

1. ALUMINUM DIHYDROXYTITANIUM DILACTATE.

2. AN ANTIPERSPIRANT COMPOSITION COMPRISING ALUMINUM DIHYDROXYTITANIUM DILACTATE AND A CARRIER THEREFOR.