MXPA99011635A - Low residue antiperspirant gel-solid stick compositions containing volatile nonpolar hydrocarbon solvents - Google Patents

Low residue antiperspirant gel-solid stick compositions containing volatile nonpolar hydrocarbon solvents

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Publication number
MXPA99011635A
MXPA99011635A MXPA/A/1999/011635A MX9911635A MXPA99011635A MX PA99011635 A MXPA99011635 A MX PA99011635A MX 9911635 A MX9911635 A MX 9911635A MX PA99011635 A MXPA99011635 A MX PA99011635A
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MX
Mexico
Prior art keywords
composition
gel
antiperspirant
solid
weight
Prior art date
Application number
MXPA/A/1999/011635A
Other languages
Spanish (es)
Inventor
John Guskey Gerald
Original Assignee
Procter & Gamble Company
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Publication date
Application filed by Procter & Gamble Company filed Critical Procter & Gamble Company
Publication of MXPA99011635A publication Critical patent/MXPA99011635A/en

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Abstract

Disclosed are anhydrous antiperspirant gel-solid sticks which comprise from about 0.5%to about 60%by weight of antiperspirant active;from about 1%to about 15%by weight of a gellant;from about 1%to about 50%by weight of nonpolar volatile hydrocarbon solvent having a solubility parameter of less than 8 (cal/cm3)0.5, a vapor pressure of from about 0.01 mmHg to about 6 mmHg, and an average boiling point of less than about 250°C;and from about 0.01%to about 10%by weight of a polar, water-miscible solvent having a solubility parameter of from 12.5 (cal/cm3)0.5 to about 25 (cal/cm3)0.5;wherein the composition has a visible residue index of from about 11 to about 30 L-value, a product hardness of from about 500 gram-force to about 5,000 gram-force, and a ratio of an elastic to viscous moduli of from about 0.1 to about 100. These compositions provide improved low residue performance, rheology, efficacy, stability and/or aesthetics from a composition having reduced raw material costs.

Description

ANTI-RANSPIRANT COMPOSITIONS IN GEL BAR - DO NOT LEAVE LITTLE RESIDUE AND CONTAIN VOLATILE NON-POLAR HYDROCARBONS TECHNICAL FIELD The present invention relates to antiperspirant compositions in the form of gel-solid sticks. In particular, the present invention relates to gel-solid stick compositions that provide better performance by leaving little residue and improving efficiency and aesthetics, and comprising a polar solvent miscible with water and a nonpolar, volatile hydrocarbonaceous solvent.
BACKGROUND OF THE INVENTION There are many types of topical antiperspirant products that are commercially available or are known in the antiperspirant art. Most of these products are formulated as sprays by pump or as aerosols, sprayable liquids, creams, emulsions, gels, gel-solids or other solid bar formulations, and comprise an astringent material, such as salts of zirconium or aluminum or combinations thereof, incorporated into a suitable carrier. These products are P957 4? They are designed to provide effective control of perspiration and odor while also being cosmetically acceptable during and after application on the axillary area or other areas of the skin. Within this group of products, solid antiperspirant bars have become especially popular with consumers. Most of these anhydrous bars contain up to 80% by weight of a volatile silicone fluid such as cyclomethicone. The volatile silicone provides the composition with an improved and drier perception of the skin during application and due to its volatility, evaporates quickly after application leaving the surface applied with a soft, dry feel. However, volatile silicones are expensive and add a considerable cost to the finished product. An attempt to reduce the cost of anhydrous antiperspirant sticks involves the use of volatile isoparaffins instead of some or all of the volatile silicones. Volatile isoparaffins are typically less expensive than volatile silicone fluids and, like volatile silicones, help to provide the composition with a dry feeling during and after application to the skin. Examples of isoparaffin-containing compositions are described in the Patent of the P957 United States 4,724,139, granted on February 9, 1988 to Palinczar and United States Patent 5,169,626 issued December 8, 1992 to Tanner et al. The compositions described by Palinczar leave on the skin, after application, a tendency to form a highly visible residue and tend to fracture during application due to their inherently and relatively high elastic content. It has now been found that a solid antiperspirant stick composition can be formulated to provide dry perception in the skin and that it uses low cost raw materials containing isoparaffin, those compositions exhibit low residue formation performance and good composition rheology. of gel-solid antiperspirant bar. This is achieved by formulating an anhydrous system with from about 0.5% to about 60% by weight of an antiperspirant active agent, from about 1% to about 15% by weight of a gellant, from about 1% to about 50% by weight of a nonpolar volatile hydrocarbon solvent having a solubility parameter of less than 8 (cal / cm3) 0.5, a vapor pressure of about 0.01 mmHg to about 6 mmHg at 25 ° C under one atmosphere, and a boiling point average of less than approximately 250 ° C and approximately 0.1% P957 to about 10% by weight of a polar solvent miscible in water having a solubility parameter of from 12.5 (cal / cm3) 0.5 to approximately 25 (cal / cm3) 0.5; wherein the composition has a visible residue index of between about 11 and about 30 of the L value, a product hardness of between about 500 grams force up to about 5,000 grams force, and a ratio between the elastic modulus (G1) and the modulus viscous (G ") from about 0.1 to about 100. Therefore, it is an object of the present invention to provide a gel-solid anhydrous antiperspirant stick composition containing volatile and non-polar hydrocarbon solvents, for example volatile isoparaffins and it also provides this composition with improved performance of low residue formation, good rheology, efficiency, stability and / or aesthetics, and also provides the composition with a reduced cost in raw materials.
SOMRRIQ OF THE INVENTION The present invention is directed to anhydrous antiperspirant gel-solid stick compositions, comprising from about 0.5% to about 60% by weight of a particulate antiperspirant active ingredient; from about 1% to about 15% by weight of a gellant; from about 1% to about 50% by weight of volatile and non-polar hydrocarbon solvent having a solubility parameter of less than 8 (cal / cm3) 0.5, a vapor pressure of between about 0.01 mmHg to about 6 mmHg at 25 ° C under an atmosphere and an average boiling point of less than about 250 ° C, and from about 0.01% to about 10% by weight of a polar solvent miscible with water having a solubility parameter of 12.5 (cal / cm3) 0.5 and approximately 25 (cal / cm3) 0.5; wherein the composition has a visible residue index of between about 11 to about 30 L-value, a product hardness of between about 500 grams-force to about 5,000 grams-force, and a ratio between elastic and viscous moduli of about 0.1 to about 100. It has been found that the gel-solid stick antiperspirant compositions of the present invention can comprise improved performance of leaving little residue, improved rheology, efficacy and aesthetics from a composition containing a volatile hydrocarbon solvent and not polar, as the isoparaffins selected. It has been found that these compositions exhibit a decreased Ostwald Ripening characteristic during prolonged storage, giving rise to a better stability of the product and a reduced syneresis of the solvent during this prolonged storage. All this is achieved by combining a volatile and non-polar hydrocarbon solvent with a water-miscible polar solvent, each having selected solubility parameters and other selected characteristics, incorporating the combined solvents into the gel-solid stick antiperspirant composition that is define here The compositions are formulated to have the required rheology and hardness profile which are also defined herein. The required hardness and rheology are preferably provided with a three-dimensional and non-polymeric crystal gel network formed of small elongated crystalline particles having an average particle size of less than about 1 μm and / or a particle morphology defined by a ratio dimensional of more than about 2.
DETAILED DESCRIPTION OF A NATION The antiperspirant gel-solid stick compositions of the present invention are anhydrous systems containing preserved antiperspirant active agent or contained within a gel-solid crystalline matrix. The antiperspirant active can be dissolved or in the form of solid particles.
The term "anhydrous" as used herein refers to gel-solid stick compositions of the present invention and, to the essential or optional components thereof other than the particulate antiperspirant active ingredient, which are essentially free of added water or free water. From a formulation point of view, this means that the antiperspirant gel-solid compositions of the present invention preferably contain less than about 5%, preferably less than about 3%, more preferably less than about 1%, still more preferably zero percent by weight of free or added water, other than water of hydration typically associated with the active particulate antiperspirant ingredient, prior to formulation. The term "low residue or leaving little residue" in the sense used herein generally refers to the visible residue remaining on the areas of skin on which the product is applied, during and immediately after application, and more specifically, it refers to the visible residue index of the composition as defined by the methodology described below. The term "environmental conditions" as used herein refers to the surrounding conditions which are from about one atmosphere of pressure, to about 50% relative humidity and about 25 ° C, unless otherwise specified. The term "substituted" as used herein, unless otherwise specified, refers to chemical entities or substituents known or suitable for binding to the compounds or other chemical materials described herein. These substituents include, but are not limited to, those listed and described in C. Hansch and A. Leo, Substi tuent Constants for Correlation Analysis in Chemistry and Biology (1979), whose listing and description are incorporated herein by reference. Examples of these substituents include, for example, alkyl, alkenyl, alkoxy, hydroxy, oxo, nitro, amino, aminoalkyl (for example aminomethyl, etc.), cyano, halo (for example chlorine, fluorine, bromine, iodine), carboxy, alkoxyaceil (for example carboethoxy, etc.), thiol, aryl, cycloalkyl, heteroaryl, heterocycloalkyl (for example piperidinyl, morpholinyl, pyrrolidinyl, etc.), imino, thioxo, hydroxyalkyl, aryloxy, arylalkyl, amides, esters, ethers, combinations of them and the like. The term "n-acyl amino acid derivatives" refers to gelling agents selected from the group consisting of n-acyl amino acid, n-acyl amino acid esters prepared from glutamic acid, lysine, glutamine, aspartic acid and combinations thereof, and that in particular are disclosed in U.S. Patent No. 5,429,816. The term "alkyl" and "alkenyl" as used herein, unless otherwise specified, refers to cyclic, linear or branched substituted or unsubstituted hydrocarbons having from 1 to about 22 carbon atoms. The gelling agent, the antiperspirant active ingredient and the solvents of the gel-solid stick compositions herein, preferably do not match in their refractive indices and, more preferably, at least two of these components have refractive indices ( ? \ D) that differ by at least about 0.02. The antiperspirant gel-solid stick compositions of the present invention may comprise, consist or consist essentially of the essential elements and limitations of the inventions described herein, as well as of any other additional or optional ingredient, component or limitation that is describe here All percentages, parts and proportions are given by weight of the total composition unless otherwise specified. All weights belong to the listed ingredients based on the specific level of the ingredient and, therefore, do not include the solvents, carriers, by-products, fillers or other minor ingredients that could be included in commercially available materials, unless another thing is specified.
Product Characteristics The antiperspirant gel-solid stick composition of the present invention is defined in terms of an essential combination of selected ingredients and product characteristics, wherein the product characteristics are defined in terms of the hardness of the product, the index of visible residue and a rheology profile defined by a relationship between the elastic modulus and the viscous modulus. Each of these essential product features is defined below in greater detail.
A) Hardness The antiperspirant gel-solid stick compositions of the present invention have a product hardness of about 500 grams-force at about 5,000 grams-force, preferably from about 750 grams-force to about 2,000 grams-force, with greater preference of approximately 800 grams-force to approximately 1,400 grams-force.
The term "product hardness" as used herein is a reflection of how much force is required to move a cone of penetration at a specified distance and at a controlled rate within the antiperspirant gel-solid stick composition, according to following test conditions. Higher values represent a harder product and lower values represent a softer product. These values are measured at 27 ° C, 15% relative humidity, using a Texture Analyzer TA-XT2, available from Texture Technology Corp., Scarsdale, New York, U.S.A. The hardness value of the product as used herein represents the amount of force required to move a standard penetration cone at a 45 ° angle through the composition by a distance of 10 mm at a rate of 2 m / second. The standard cone is available from Texture Technology Corp., as part number TA-15 and has a total cone length of approximately 24.7 mm, an angled cone length of approximately 18.3 mm, a maximum diameter of the angled surface of the cone of approximately 15.5 mm. The cone is a smooth stainless steel construction and weighs approximately 17.8 grams.
B) Residue The antiperspirant gel-solid stick composition of this invention has an index of P957 visible residue of between 11 and about 30, value L, preferably between 11 and approximately 25 value L, more preferably between 11 and approximately 20 value L. The term "visible residue index" as used herein refers to General to the extent to which the composition of this invention is clearly visible as a thin topical film after application to the skin and, more specifically, refers to visible residue values (expressed as L value on the L-value scale). a, b) as measured according to the following methodology, developed at 27 ° C under atmospheric pressure and at 15% relative humidity in the antiperspirant stick composition having a product hardness of approximately 500 grams-force at approximately 5,000 grams -force. A piece of black felt of approximately 10 cm x 30 cm is attached to a movable horizontal slide to which it is movably attached or fixed to a larger mechanical unit. An example of a suitable piece of black felt that is used here is Supreme Robe Velor, FN-6554, Color 404L, Style 31854, available from So-Fro Fabrics, Evendale, Ohio, U.S.A. An example of the appropriate mechanical unit used here is the Adhesion and Release Tester No. A-14934 manufactured by Testing Machines, Inc., A ityville, New York, U.S.A., or a P957 Velmex Unislide Positioning System, from the Unislide series (MB6000), available from Velmex, Inc., Bloomfield, New York, U.S.A. An antiperspirant stick composition contained within about 0.5 cm from a conventional package or package and extending particularly at this length, is placed perpendicular to the piece attached to the felt and above it, so that the product extends out of the package or the package and is oriented towards the felt piece and the surrounding package is positioned away from the felt piece. The surrounding package is placed in place using a mechanical arm or other suitable device to apply the required movement to the product, as described herein. The antiperspirant stick composition then moves slowly towards the black felt piece and is allowed to gently contact it. A 500 gram weight is placed on the product mix so that the product continuously contacts the black felt piece during the test. The sample with the weight is then repeatedly moved back and forth through the piece of felt at a fixed speed (approximately 3 cm / sec) and with a fixed amount of applied pressure provided by the heavy product, until 1.4 grams of bar composition P957 antiperspirant are applied evenly over a 5 cm x 20 cm area of the piece of black felt. The piece of felt is carefully removed from the apparatus. Subsequently, a calibrated Minolta CR-300 chromameter (available from Minolta Corp., Ramsey, New Jersey, U.S.A.) is used to measure the L value (on the color scale L, a, b) of the applied surface area. First, a template is placed on the top of the felt piece to facilitate Minolta readings. The size of the template is 5 cm x 20 cm. The template has twelve circular openings (2.2 cm in diameter) placed inside it, each opening is placed centrally within adjacent areas of 6.5 cm2 of the surface of the template. The template is placed over the applied surface area of the felt piece, so that each of the twelve circular openings covers a non-overlapping area of the applied surface. The observation port of the chromameter is adjusted within each of the circular openings and the measurement of the L value is taken. An average L value is then determined for the twelve measurements (standard deviation of less than approximately 0.8) which then corresponds to the index of visible residue as described here. It has been found that there is a correlation between the range of the visible residue index defined here and the P957 average particle size of the crystalline gelling particles in the antiperspirant gel-solid stick composition of the present invention. In general, as the average particle size of the crystalline gelling particles of the composition decreases, the performance of little residue occurrence is improved. In particular, it has been found that a visible residue index of between about 11 and about 30 on the L-value scale, correlates with a crystalline, gelling particle size, average of less than about 1 μm and / or a morphology of crystallizing, gelling particle characterized by dimensional crystal growth so as to result in filaments, fibers, strands or other crystalline elongated particles, wherein the dimensional relationship that is defined by the major and minor axes of the crystalline particle is greater than about 2, preferably greater than about 6. Conversely, solid compositions containing crystalline gelling particles greater than 1 μm (average particle diameter) have a visible residue index greater than the L value of 30. In view of this correlation between the values of visible residue index and average crystalline particle size or elongated particle morphology, the measurement of the index from P957 visible residue can now be used as an alternative means to establish the average particle size of the crystalline gellant or the morphology thereof, at least insofar as this average particle size is less than about 1 μm.
C) Rheology The antiperspirant stick compositions of the present invention are gel-solid type having the selected rheology profile defined herein. The rheology profile is defined herein in terms of the relationship between the elastic modulus (Gt) and the viscous modulus (G ") (GdG") of the gel-solid stick composition. To provide the required rheology, gel-solid stick compositions must have a GdG ratio of between about 0.1 and about 100, preferably between about 0.1 and about 50, more preferably between about 1 and about 20, still with more preferred between about 5 and about 20. This ratio represents the extent to which the gel-solid stick compositions of the present exhibit solid characteristics and the extent to which the compositions exhibit liquid or fluid characteristics, and specifically refers to the numerical GdG ratio "which is determined by the following P957 methodology. The elastic modulus is a measurement that correlates with the solid character of the gel-solid stick compositions herein and the viscous modulus is a measurement that correlates the liquid or fluid character of the gel-solid stick compositions of the present. The measurements for G 'and G "for the purpose of defining the composition of the present invention are determined according to environmental conditions using conventional techniques well known in the art of formulations, for example, Bohlin Stress-Strain Rheometer, available from Bohlin Reologi, Cranberry, New Jersey can be used with a plate and cone configuration (approximately Io) Approximately 1.0 mg of the product is carefully removed from the composition with minimal application of shear and then placed between the cone and plate attachments. measure G 'and G ". It has been found that the gel-solid stick compositions of this invention exhibit improved development of low residue appearance when formulated as described herein, wherein the composition has the selected GdG ratio "as already described, especially when the defined rheology is associated with a crystalline gel matrix having a preferred small particle size and / or a particle morphology such as that P957 describes here. These gel-solid bar formulations are gently smeared onto the skin with low shear and melt rapidly during this operation to form a thin film that leaves little residue on the applied surface. In particular, it has been found that the gel-solid stick compositions of this invention have rheology characteristics that result in better performance, especially performance in terms of the little residue left. These selected gel-solid compositions that are defined herein behave as solids before being applied while remaining within a basket and other type of container, but behave as liquids or fluids during and immediately after being applied to the skin. In other words, the solid compositions become thin during application to the skin, melt or nearly melt (except for the active compound in particles that remains without melting) during the application of low shear, resulting in a liquid film or fluid, thin and that leaves little residue on the skin, during or immediately after topical application to the skin. The applied film is clear or has a very inconspicuous residue and remains essentially in that form for extended periods of time, after application.
P957 Essential Ingredients The gel-solid stick antiperspirant compositions of this invention have the aforementioned product characteristics and are further defined in terms of the select combination of essential ingredients resulting in the product characteristics mentioned above. The essential ingredients are antiperspirant active agent, primary gelling agent, non-polar volatile solvent and polar solvent miscible with water. Each of these essential ingredients is defined below in detail.
A) Active Agent The anhydrous antiperspirant gel-solid stick compositions of the present invention comprise an antiperspirant active agent suitable for application to human skin. These active agents can be dissolved in the selected solvent or dispersed throughout the compositions as non-solubilized solids. The concentration of the antiperspirant active agent in the composition should be sufficient to provide the desired wetting of perspiration and odor control from the selected gel-solid stick antiperspirant formulation. The gel-solid stick compositions P957 antiperspirant according to the present invention preferably comprise particulate antiperspirant active agents at concentrations between about 0.5% and about 60%, more preferably between about 5% and about 35% by weight of the composition. These percentages by weight are calculated based on an anhydrous metal salt, excluding water and any other complexing agent such as glycine, glycine salts and other complexing agents. The particulate antiperspirant active agent, as it is in the composition, is in the form of dispersed solid particles having a preferred average particle size or a diameter less than about 100 μm, more preferably less than about 50 μm . Also preferred are dispersed solid particles having an average particle size or average diameter of less than about 2 μm, even more preferably less than about 0.4 μm. It has been found that the particles of the antiperspirant active within the preferred range of particle size provide a performance of less visible residue of the gel-solid compositions herein than other preferred smaller ranges of particle size. The antiperspirant active that is used in the antiperspirant gel-solid stick compositions of the P957 present invention include any compound, composition or material having antiperspirant activity. Preferred antiperspirant actives include astringent metal salts, especially organic and inorganic salts of aluminum, zirconium and zinc, as well as mixtures thereof. Particularly preferred are the aluminum and zirconium salts, for example aluminum halides, aluminum chlorohydrate, and aluminum hydroxyhalides, zirconyl oxyhalides, zirconyl hydroxyhalides and mixtures thereof. Preferred aluminum salts that are used in the antiperspirant gel-solid stick compositions include those that conform to the formula: Al2 (OH) aClb • x H20 wherein a is from about 2 to about 5; the sum of a and b is approximately 6; x is from about 1 to about 6 and where a, b and x can be non-integer values. Particular preference is given to aluminum chlorhydroxides referred to as "basic 5/6 chlorohydroxide" wherein a = 5 and "basic 2/3 chlorohydroxide" where a = 4. The processes for preparing the aluminum salts are set forth in the US Pat. the United States number 3,887,692 of Gilman granted on June 3, 1975; United States Patent number 3,904,741 of P957 Jones et al. granted on September 9, 1975; U.S. Patent No. 4,359,456 to Gosling et al. granted on November 16, 1982 and British Patent Specification number 2,048,229 of Fitzgerald et al. published December 10, 1980, all of which are incorporated herein by reference. Mixtures of aluminum salts are described in British Patent Specification No. 1,347,950 to Shin et al. published on February 27, 1974, which is incorporated herein by reference. Preferred zirconium salts that are used in antiperspirant gel-solid stick compositions include those that conform to the formula: ZrO (OH) 2.aCla • x H20 wherein a is from about 1.5 to about 1.87; x is from about 1 to about 7 and where a and x can be, the two values; not integers These zirconium salts are described in Belgian Patent 825,146 of Schmitz issued August 4, 1975, which is incorporated herein by reference. Particularly preferred zirconium salts are those complexes that additionally contain aluminum and glycine, commonly known as ZAG complex. These ZAG complexes contain aluminum chlorhydroxide and zirconyl hydroxy chloride which conform to the formulas described above. These ZAG complexes are P957 describe in U.S. Patent No. 3,679,068 to Luedders et al. granted on February 12, 1974, British Patent Application No. 2,144,992 of Callaghan et al. published March 20, 1985 and U.S. Patent No. 4,120,948 to Shelton published October 17, 1978, all of which are incorporated herein by reference. The gel-solid antiperspirant stick compositions of the present invention may also be formulated to comprise other dispersed solids or other materials in addition to or in place of the particulate antiperspirant active ingredient. These other dispersed solids and other materials include any known or suitable material for topical application to human skin. The gel-solid antiperspirant compositions can also be formulated as gel-solid stick compositions that do not contain antiperspirants or any other active material, in particles or in another form.
B) Gelifier The gel-solid antiperspirant stick compositions of this invention comprise a gellant suitable for topically applying to human skin.
These solid non-polymeric gelling agents must form within the composition a crystalline matrix within the P957 which is entrapped or contained an anhydrous liquid carrier or any other liquid component of the composition. These solid and non-polymeric gelling agents preferably form crystalline particles having an average particle diameter and a particle morphology as described below. The essential and optional features of the suitable gelling agents that are used in the gel-solid stick composition are described in detail below. 1) Description of gelling agent The concentration of gelling agents in the compositions can vary with each selected gel-solid antiperspirant stick formulation, especially with each anhydrous liquid carrier selected from the formulation, but these concentrations will generally vary from about 0.1%. and about 15%, preferably between about 1% and about 12%, more preferably between about 3% and about 12% by weight of the composition. The gelling agents must be solids under environmental conditions. The gelling agents that are used in the antiperspirant compositions are those that can P957 melt and form a solution and other homogeneous liquid or liquid dispersion with the selected anhydrous liquid carrier, and at the concentrations of the liquid carrier and the selected gellant, at a process temperature of from about 28 ° C to about 250 ° C, preferably from between about 28 ° C and 100 ° C, more preferably between about 28 ° C and about 78 ° C. The molten gellant is typically dissolved by the selected liquid carrier or dispersed therethrough to thereby form a solution or other homogeneous liquid. The solution or other homogeneous liquid and other optional and essential ingredients, preferably are combined according to the manufacturing method described herein or to other conventional or otherwise known techniques, and placed in a suitable package as a fluid solution or as a homogeneous liquid, and then allowed to solidify and form the desired solid-gel matrix within the composition, as the temperature returns to room temperature and falls below the solidification point of the selected gellant. When selecting a combination of gelling agent, water-miscible polar solvent and non-polar vola solvent for use in gel-solid antiperspirant stick compositions, the selected combination P957 should allow the development of a crystalline gelling matrix within the composition, wherein the crystalline particles of the component preferably have an average particle size of less than about 1 μm, more preferably less than about 0.4 μm, s more preferably less than about 0.2 μm, and s more preferably between about 0.001 μm and about 0.2 μm, and / or where the crystalline particles have the required elongated morphology that is described here, where the particle size is measured or determined by the methods described herein or by methods well known to those skilled in the art, such as electron or light microscopy. Gel-solid stick compositions can be prepared by methods well known in the art for formulation of gel solids having a minimum crystalline particle size or the preferred elongated particle morphology. The gel-solid stick compositions are preferably prepared by the selected methods described below, aimed at decreasing the crystalline particle size and / or establishing the preferred morphology of the crystalline particle. Suitable gelling agents that are used in the antiperspirant stick compositions of the present invention include fatty acid gelling agents, esters and P957 amides of fatty acid gelling agents, hydroxy acids, hydroxy fatty acids, cholesteric materials, lanolinol materials and other amide gelling agents that are known to be used as gelling agents or are described in other detail in detail below. The gelling agents can be used as a gelling agent or a combination of gelling agents. Other crystalline gelling agents can be used in the antiperspirant compositions of the present invention as long as these other gelling agents can be formulated to provide the required crystal gel matrix. Suitable amide gelling agents include branched or disubstituted monoamide gelling agents, branched or monosubstituted diamide gelling agents, triamide gelling agents, n-acyl amino acid derivatives and combinations thereof. Non-limiting examples of suitable secondary amide gelling agents include alkylamides of a di- and / or tri-basic carboxylic acid which conforms to the formula: P957 R. C '-C -N -R.
-X -Y - ZO II R- c, -C ~ N -R, 10 where a is a structure formed from the union of C ', C "and X and where: a) Ri is zero, hydroxy , hydrogen, aryl, siloxane or aryl substituted with C? -C22 alkyl or C? -C2 alkyl ethers, C? -C22 alkyl esters / C? -C2 alkoxy, C1-C22 alkenyl / C1-C22 alkyl / straight chain, cyclic or branched, substituted or unsubstituted, saturated or unsaturated, preferably C4-C18 alkyl, C4-Cis alkenyl, C4-C18 alkoxy, C4-C18 alkyl esters, C4-C18 alkyl ethers or C4-C18-substituted aryl, with higher preferably, C 2 -C 8 alkyl, C 2 -C 8 alkenyl, C 1 -C 8 alkoxy, C 12 -C 18 alkyl esters, C 12 -C 18 alkylethers or aryl substituted with C 2 -C 8 alkyl; b) R 2, R 4, R 5 and together or independently are hydrogen, hydroxy, aryl, aryl, siloxane or aryl substituted with C 1 -C 22 alkyl or C 1 -C 22 alkyl ethers / C 1 -C 22 alkylesters / C 1 -C 22 alkoxy / C 1 -C 22 alkenyl C1-C22 straight-chain, branched or cyclic alkyl, substituted or unsubstituted, saturated or unsaturated; preferably, C4-C10 alkyl, C4-C10 alkenyl, C4-C10 alkoxy, alkyl esters P957 C4-C10, C4-C10 alkyl ethers or aryl substituted with C4-C10 alkyl, more preferably C4-C8 alkyl, C4-C8 alkenyl, C4-C8 alkoxy, C-C8 alkylester, C4-C8 alkyl ether or substituted aryl with C4-C8 alkyl; c) R3, is zero, hydroxy, hydrogen, alkyl ethers C1-C4 or C1-C4 alkylesters, C1-C4 alkoxy, C1-C4 alkenyl, straight, branched or cyclic C 1 -C 4 alkyl, substituted or unsubstituted, saturated or unsaturated; preferably, C1-C4 alkoxy, hydroxy or hydrogen, more preferably, a hydroxy or hydrogen; d) R7 and R8 independently or together are, null, hydrogen, hydroxy, aryl, siloxane or aryl substituted with C1-C22 alkyl or C1-C22 alkyl ethers C1-C22 alkylester C1-C22 alkoxy, C1-C22 alkenyl / C1 alkyl -C22 straight chain, branched or cyclic, substituted or unsubstituted, saturated or unsaturated; preferably, C4-C10 alkyl, C4-C2 alkenyl, C4-C10 alkoxy, C4-C10 alkylester, C4-C10 alkyl ether or C4-C10 substituted aryl, more preferably C4-C8 alkyl, C4-alkenyl C8, C4-C8 alkoxy, C4-C8 alkyl esters, C4-C8 alkyl ethers or aryl substituted with C4-C8 alkyl; e) Rg is zero or hydrogen; f) Rio and R11 independently or together are, null, hydrogen, hydroxy, aryl, siloxane or aryl substituted with C? -C6 alkenyl or C? -C6 alkyl ethers, P957 Ci-Cβ alkylesters, Ci-Cg alkoxy, C?-C6 alkenyl, Ci-Cd straight-chain, branched or cyclic alkyl, substituted or unsubstituted, saturated or unsaturated; preferably, C 1 -C 4 alkyl, C 1 -C 4 alkenyl, C 1 -C 4 alkoxy, C 1 -C 4 alkyl esters / C 1 -C 4 alkyl ethers, aryl substituted with C 1 -C 4 alkyl or hydrogen, more preferably hydrogen; g) X is zero, nitrogen, aryl or -CH 2 -) - n / wherein n is an integer from 1 to 6, preferably, -CH 2 -) - n, where n is an integer from 1 to 3; h) Y is zero, acyl or carbonyl; i) Z is zero, hydrogen, hydroxy, aryl, siloxane, nitrogen or aryl substituted with C1-C22 alkyl or C1-C22 alkyl ethers / C1-C22 alkylesters / C? -C22 alkoxy, C1-C22 alkenyl C1-C22 alkyl chain straight, branched or cyclic, substituted or unsubstituted, saturated or unsaturated; preferably, C4-C10 alkyl, C4-C10 alkenyl, C4-C10 alkoxy, C4-C10 alkyl esters, C4-C10 alkyl ethers or C4-C10 substituted aryl, more preferably C4-C8 alkyl, C4-C8 alkenyl, C4-C8 alkoxy, C4-C8 alkyl esters, C4-C8 alkyl ethers or aryl substituted with C4-C8 alkyl; j) "a" is a double or simple link as long as: (i) when X and Z are not null and Y is null, X is directly bonded to Z; P957 (ii) when Z is zero, a hydrogen or a hydroxy, R7 and R8 are zero; and (iii) when "a" is a double bond, R3 and Rg are null. Specific examples of alkylamides of the di and tribasic carboxylic acids or anhydrides suitable for use in the gel-solid antiperspirant stick composition include cyclic acid alkylamides., tricarballylic acid, aconitic acid, nitrilotriacetic acid, succinic acid and itaconic acid, for example 1,2,3-propane tributylamide, 2-hydroxy-l, 2,3-propane tributylamide, 1-propene-1, 2, 3- trioctylamide, N, N'N "-tri (methyl disyl) ida, 2-dodecyl-N, N'-dibutyl succinamide and combinations thereof. N, N'-dibutylsuccinamide Non-limiting examples of the n-acylamino acid derivatives include n-acylamino acid esters and n-acylamino acid amides, specific examples of these include N-lauroyl-glutamic acid diethylamide, N-dibutylamide -lauroyl-glutamic acid, N-lauroyl-glutamic acid dihexylamide, N-lauroyl-glutamic acid dioctylamide, N-lauroyl-glutamic acid didecylamide, N-lauroyl-glutamic acid didodecylamide, N-lauroyl-glutamic acid ditetradecylamide, P957 N-lauroyl-glutamic acid dihexadecyl amide, N-lauroyl-glutamic acid distearyl amide, N-stearoyl-glutamic acid dibutyl amide, N-stearoyl-glutamic acid dihexylamide, N-stearoyl glutamic acid diheptylamide, dioctylamide N-stearoyl-glutamic acid, N-stearoyl-glutamic acid didecylamide, N-stearoyl-glutamic acid didodecylamide, N-stearoyl-glutamic acid ditetradecylamide, N-stearoyl-glutamic acid dihexadecylamide and N-stearoyl-glutamic acid distearylamide. glutamic The dibutyl amide of n-lauroyl-glutamic acid, n-stearyl-glutamic acid dihexylamide and combinations thereof are preferred. The selected alkylamide gelling agents are preferably synthesized by direct amidation of the corresponding di- or tri-basic organic acids with the appropriate alkylamine under the appropriate reaction temperatures, followed by removal of the excess amine from the resulting mixture which contains the alkylated amide gelling agents. Select alkylamide gelling agents can also be synthesized by esterification of the corresponding di or tribasic organic acid with methanol using a boron trifluoride catalyst, followed by removal of excess methanol and catalyst. He The resulting p957 trimethylester is then amidated as described in the previous step process, using the appropriate alkylamine followed by removal of excess amine. The resulting alkylamides that are used in the composition must be non-polymeric. Suitable fatty acid gelling agents include, but are not limited to, hydroxy fatty acids including alpha-hydroxy acids and 12-hydroxystearic acid and derivatives thereof (which include amides and esters thereof), fatty acids having from about 10 to about 40 carbon atoms (for example behenic acid, erucic acid, stearic acid) and related gelling agents, some preferred examples are disclosed in U.S. Patent 5,429,816, issued to Hofrichter et al. on July 4, 1995; and U.S. Patent 5,552,136, issued to Motley on September 3, 1996, the exhibits of which are incorporated herein by reference. Preferred is 12-hydroxystearic acid and derivatives thereof. Preferred antiperspirant compositions are those comprising a gelling system containing hydroxy fatty acid gellant as described herein, in combination with an n-acyl amino acid derivative as a secondary gellant, wherein the ratio between the hydroxy acid gellant fat and the P957 secondary gelling agent is from about 1: 2 to about 20: 1, preferably between about 2: 1 and about 5: 1. Most preferred are the dibutylamide combinations of n-lauroyl-glutamic acid and 12-hydroxystearic acid. Examples of these preferred gelling systems are described in U.S. Patent 5,429,816. 2) Preferred enantiomeric gelling agents Preferred gelling agents which are used herein include those enantiomeric compounds or enantiomeric materials which contain at least one asymmetric (chiral) carbon atom. Non-limiting examples of these preferred enantiomeric gelling agents include 12-hydroxystearic acid, other hydroxy acids such as for example alpha hydroxy acid, cholesterols, lanolin and derivatives thereof. It has been found that these preferred enantiomeric gelling agents, when used in the gel-solid antiperspirant compositions of the anhydrous type herein, provide the composition with the required hardness of the product, the required values of visible residue index and the properties Rheological requirements (GdG). It is believed that these enantiomeric gelling agents are especially effective in forming P957 one-dimensional elongated particles in the form of filaments, fibrils or strands that twist or twist simply to form a crystalline matrix, three-dimensional, stable in the gel-solid composition. These elongated particles have a dimensional ratio of greater than about 2, preferably greater than about 6. These gelling agents are considered to form elongated crystalline particles resulting in a stable crystalline matrix which, in part because of the small size and elongated morphology of these particles cause less diffusion of light when applied to the skin in the antiperspirant composition, which results in a lower visible residue after application. 3) Preferred morphology of the particles The gelling agents used herein include the crystalline gelling agents which inherently form or can be formulated or are made to form elongated crystalline particles having a dimensional ratio of greater than about 2, preferably greater than about 6. These elongated crystals preferably have an average particle size, measured along a minor axis of the elongated crystal, of less than 1 μm, more preferably, less than about P957 0.4 μm, still more preferably, less than about 0.2 μm, preferably superlative between about 0.2 μm and about 0.001 μm. Gel-solid stick compositions containing these preferred elongated crystals can be prepared by the methods described herein or by methods otherwise known in the art of formulating to make gel matrices comprising these elongated crystalline particles. The "dimensional relationship" as used herein to define the preferred embodiments of the gel-solid stick compositions herein can be determined by measuring or otherwise determining the ratio between the length of the major axis of the crystalline particles and the length of the minor axis of the crystalline particles. This ratio of lengths between the major axis and the minor axis is characterized by the dimensional relationship referred to herein. The dimensional relationship can be determined by conventional methods or by known methods of electron microscopy or light, where the crystalline particles are measured in the dimensions of the major axis and the minor axis, or by these methods it is observed that they clearly have a structure elongated crystal with a dimensional ratio substantially greater than about 2, preferably, P957 greater than about 6. It has been found that these crystalline gelling agents having the selected dimensional ratios that are defined herein provide the gel-solid antiperspirant stick compositions with a three-dimensional crystal structure which can provide the composition with the characteristic of leaving little residue , a ratio of elastic modulus to viscous required and the required hardness of the product, as defined herein. This crystalline morphology is considered to be especially effective in providing a crystalline matrix within the composition that provides a tightly bonded gel-solid matrix network, but also comprises crystalline particles that are small enough to contribute minimally to visible residue when applied topically to the skin. In particular, it has been found that a visible residue index of between about 11 and about 30 of the L value correlates with an average particle size of the crystalline gellant of less than about 1 μm and / or a particle morphology of the crystalline gelling agent characterized by a dimensional crystal growth, such as that which results in crystalline filaments, crystalline fibers, strands or P957 other elongated particles, wherein the dimensional ratio as defined by the major axis and minor axis of the crystalline particle is greater than about 2, preferably greater than about 6. 4) Optional ratio of dimer to monomer The gellant of the gel-solid antiperspirant stick composition of the present invention preferably comprises a fatty acid gellant, as the primary gelling agent, having a selected ratio of dimer to monomer. The fatty acid gelling agents having the required ratio of dimer to monomer can be used alone or in combination with an additional or secondary gellant of the composition. The dimer to monomer ratio selected helps to provide the gel-solid stick compositions herein with a low residue performanceImproved efficiency and aesthetics and especially provides a better performance of little appearance of residue and better hardness of the product. The fatty acid gelling agents of the gel-solid antiperspirant stick composition, when used in combination with additional or secondary gelling agents, have a selected ratio of dimer to monomer of between about 1: 1 to about 25: 1, preferably, from about 1.5: 1 to about P957 25: 1, more preferably, from about 2.5: 1 to about 20: 1, still more preferably, between about 3: 1 to about 10: 1. The higher dimer to monomer ratios are preferred. The dimer to monomer ratio of the fatty acid gellant can be determined by methods or techniques well known in the field of formulations, including infrared methods such as Fourier Transform Infrared Spectroscopy (FTIR). These methods are discussed in The Infared Spectra of Complex Molecules, L.J. Bellamy, 2nd. Edition, 1958, Introduction to Infared and Raman Spectroscopy, N.B. Colthup, et al., 3a. Edition, and Fourier Transform Infared Spectroscopy, P.R. Griffiths, et al., 1986, which are incorporated herein by reference. According to these methods or techniques, fatty acids are normally characterized by their carbonyl elongation frequencies, which are measured as absorption bands between 1740 cm "1 and 1680 cm" 1. The fatty acid gellant of the antiperspirant compositions of the present invention comprises fatty acid monomers and fatty acid dimers which are components of the carbonyl absorption band. However, due to the formation of hydrogen-bonded dimers, the fatty acid dimer component can travel to frequencies 30 cm "1 lower than the frequency of the acid monomer P957 fatty. With the use of infrared spectral data, the dimer to monomer ratio is determined by calculating the ratio of the peak area of the band derived from the second dimer bound to hydrogen about 1696 cm "1 with respect to the peak area of the band derived from the second fatty acid monomer about 1712 cm "1. According to the following methodology, an infrared spectrum is recorded using an Attenuated Total Reflectance ("ATR") crystal of 45 ° ZnSe and a horizontal ATR apparatus (which is obtained from Spectra Tech. Inc., Shelton, Connecticut, U.S.A.) attached to a Nicolet 20scx Spectrometer FTIR. The Nicolet 20scx FTIR spectrometer is obtained from Nicolet Instrument Corporation, Madison, Wisconsin, U.S.A. The Nicolet 205scx FTIR Spectrometer is equipped with a narrowband cadmium and mercury telluride detector with which an average of 256 scans are co-added to generate the infrared spectra. The infrared spectra are then imported into the software program of the computer, for example GRAMS / 386 (obtained from Galactic Industries Corporation, Salem, New Hampshire, USA) to calculate the ratio of dimer to monomer using a second derivative algorithm. 5 points, which is a mathematical procedure defined by Savistsky-Gola.
P957 The required dimer to monomer ratio can be established with the fatty acid gelling agents described herein, which include alpha-hydroxy fatty acids and fatty acids having from about 10 to about 40 carbon atoms, examples of which include -hydroxystearic acid, 12-hydroxylauric acid, 16-hydroxyhexadecanoic acid, behenic acid, euricic acid, stearic acid, caprylic acid, lauric acid, isostearic acid and combinations thereof. Examples of some of the suitable fatty acid gelling agents are described in U.S. Patent No. 5,429,816, issued to Hofrichter et al. on July 4, 1995; and in U.S. Patent No. 5,552,136 issued to Motley on September 3, 1996, which are incorporated herein by reference. The 12-hydroxystearic acid is the most preferred. The required dimer to monomer ratio can also be established with the fatty acid gelling agents described herein, in combination with an additional or secondary gelling agent, wherein the molar ratio of the fatty acid gelling agent to the additional or secondary gelling agent is thus less 0.5: 1, preferably at least 3: 1 and typically no more than about 20: 1. Anyone with average skill in the chemical or formulation technique can formulate these P957 fatty acid gelling systems to control or obtain the proportion described.
C) Non-Polar and Volatile Hydrocarbon Solvent The gel-solid bar composition of the present invention comprises a non-polar and volatile hydrocarbon solvent having a selected vapor pressure and a select solubility parameter. The concentration of the volatile and non-polar hydrocarbon solvent in the gel-solid stick composition varies between about 1% and about 50%, preferably between about 10% and about 40%, more preferably between about 20% and about 40%. %, and preferably superlative between about 30% and about 40% by weight of the composition. The term "volatile" which is used in this context refers to the volatile and non-polar hydrocarbon solvent of the gel-solid stick composition of the present invention and in this context refers specifically to non-polar hydrocarbon solvents having a Vapor pressure measured at 25 ° C of between about 0.01 mmHg to about 6.0 mmHg, preferably from about 0.02 mmHg to about 2.0 mmHg and an average boiling point under a pressure atmosphere (1 atm) of less than about P957 250 ° C, preferably less than about 235 ° C, under 1 atmosphere of pressure (atm). The term "non-polar" which is used in this context refers to non-polar and volatile hydrocarbon solvents of the gel-solid stick composition of this invention and in this context specifically refers to volatile solvents having a solubility parameter less than 8.0 (cal / cm3) 0.5, preferably from about 5.0 (cal / cm3) 0.5 to less than 8.0 (cal / cm3) 0.5, more preferably 6.0 (cal / cm3) 0 ' 5 to about 7.60 (cal / cm3) 0.5. The solubility parameters for the volatile and non-polar hydrocarbon solvents and for other materials described herein are determined by methods well known in the chemical area to establish the relative polar character of a solvent or other material. A description of the solubility parameters and the means to determine them is described by C.D. Vaughan, "Solubility Effects in Product, Package, Penetration and Preservation" 103 Cosmetics and Toiletries 47-69, October 1988; and C.D. Vaughan, "Using Solubility Parameters in Cosmetics Formulation", 36 J. Soc. Cosmetic Chemists 319-333, September / October 1988, the descriptions of which are incorporated herein by reference. Volatile hydrocarbon solvents and not P957 polar suitable for use in gel-solids bar compositions are those solvents having the vapor pressure described above and the solubility parameters described above, which include hydrocarbons such as, for example, some isoparaffins and petroleum distillates having the pressure of steam required and the required solubility parameter. Preferred are non-polar hydrocarbon solvents which may be of cyclic, branched or chain configuration, more preferably branched chain hydrocarbons. The non-polar volatile hydrocarbon solvent is more preferably a branched chain hydrocarbon having the required vapor pressure and solubility parameter and having from about 4 to about 30 carbon atoms, preferably from about 4 to about 20 carbon atoms. carbon atoms, more preferably from about 6 to about 20 carbon atoms. The gel-solid stick antiperspirant composition most preferably comprises a combination of two or more of the aforementioned branched-chain hydrocarbons, wherein these two or more hydrocarbons have different molecular weights, different numbers of carbon atoms and / or different chain configurations. The specific non-limiting examples of these combinations more Preferred P957 hydrocarbon solvents include isoparaffins available from Exxon Chemical Company, Baytown, Texas USA, such as Isopar M (Isoparaffin C13-C14), Isopar C (Isoparaffin C7-C8), Isoparaffin C8-C9 (Isopar E), Isopar G (Isoparaffin C10-11), Isopar L (Isoparaffin CUCO), Isopar H (C11-C12 Isoparaffin) and combinations thereof. Other non-limiting examples of suitable branched chain hydrocarbons include Permethyl 99A (isododecane), Permethyl 102A (isoeicosane), Permethyl 101A (isohexadecane) and combinations thereof. The Permethyl series are available from Preperse, Inc., South Plainfield, New Jersey, E.U.A. Other non-limiting examples of suitable branched chain hydrocarbons include petroleum distillates such as those available from Phillips Chemical such as Soltrol 130, Soltrol 170 and those available from Shell as Shell Sol 70, -71 and -2033. Non-limiting examples of other suitable volatile and non-polar hydrocarbon solvents include dodecane, octane, decane and combinations thereof and the Norpar paraffin series available from Exxon Chemical Company such as Norpar 12, -13 and -15. Still other examples include Cn-Cis alkanes / cycloalkanes such as those available from Exxon such as Exxsol D80.
P957 D) Water Miscible Polar Solvents The gel-solid stick composition of this invention comprises one or more polar water-miscible solvents having a selectively high solubility parameter. The concentration of the water-miscible polar solvent in the gel-solid antiperspirant stick composition will vary with the specific combination of water-miscible polar solvent, gelling agent, volatile non-polar hydrocarbon solvent and other solvents or gelling agents of the composition, but will not exceed about 10% by weight of the composition, preferably from about 0.1% to about 5%, more preferably from about 0.1% to about 4%, even more preferably from about 0.1% to about 3% by weight of the composition of gel-solid antiperspirant bar, wherein the polar solvent miscible in water has a solubility parameter of at least 12.5 (cal / cm3) 0.5, preferably 12.5 (cal / cm3) ° 5 to approximately 25 (cal / cm3) 0.5, more preferably from 12.5 (cal / cm3) 0.5 to approximately 17.0 (cal / cm3) 0.5. Non-limiting examples of water miscible polar solvents suitable for antiperspirant gel-solid stick compositions include monohydric alcohols, polyhydric alcohols and combinations of the P957 themselves, specific examples include, but are not limited to, glycerin, propylene glycol, dipropylene glycol, ethanol, tripropylene glycol, butylene glycol, hexylene glycol, 1,2-hexanediol, propylene carbonate and combinations thereof. Propylene glycol, dipropylene glycol, propylene carbonate, glycerin and combination thereof are preferred. The most preferred is glycerin.
E) Optional Solvents The gel-solid anhydrous antiperspirant gel compositions of this invention may further comprise an optional liquid carrier in addition to the non-polar volatile solvents and water miscible polar solvents described above. The concentrations of the optional liquid carrier in the gel-solid stick compositions will vary mainly with the type and amount of liquid carrier, the type and amount of volatile non-polar and polar miscible solvents in water described above, the gelling agent and the solubility of the gellant in the optional liquid carrier and other solvents. Preferred concentrations of the combination of solvents and optional liquid carrier are between about 10% and about 80%, preferably, between about 10% and about 70%, by weight of the composition.
P957 The optional liquid carrier preferably includes a modified silicone carrier at a concentration ranging from about 0.1% to about 75%, preferably from about 0.1% to about 50%, more preferably from about 1% to about 20%, and even more preferably between about 1% and about 10% by weight of the gel-solid stick antiperspirant composition. The optional liquid carrier may include one or more liquid carriers suitable for topical application to human skin and may include solvents or organic liquid carriers, may contain silicone or fluorine, may be volatile or non-volatile, may be polar or non-polar, provided that when the resulting combination of the optional liquid carrier and other solvents forms a solution or other type of homogeneous liquid or liquid dispersion with the selected non-polymeric gellant at the selected gelling concentration, at a temperature between about 28 ° C to about 250 ° C , preferably, between about 28 ° C and about 100 ° C, more preferably, about 28 ° C and about 78 ° C. Optional liquid carriers include silicone carriers, as long as they are liquid P957 environmental conditions and have a viscosity less than about 100,000 centistokes, preferably less than about 500 centistokes, more preferably from about 1 and 50 centistokes, and still more preferably between about 1 and 20 centistokes. These modified silicone carriers are generally known in the chemical field, some examples of which are described in Cosmetics, Science and Technology 27-104 M. Balsam and E. Sagarin ed. 1972); U.S. Patent No. 4,202,879, issued to Shelton on May 13, 1980; U.S. Patent No. 5,084,577, issued to Bolich on January 28, 1992; which are incorporated here as a reference. Modified silicone carriers suitable for use in gel-solid antiperspirant stick compositions include, but are not limited to, compounds or materials as defined above and which are generally characterized in the following manner: silicone polyethers or silicone glycols (for example dimethicone copolyol); silicone polyethers bound to alkyl (for example, Goldschmidt EM-90 or EM-97); siloxane surfactants of a hanging / rake / comb configuration, silicone surfactants of a trisiloxane configuration and silicone surfactants of ABA / alf -omega block copolymers (as for example, P957 polyoxyalkylene, polyoxyethylene or ethoxylated, polyoxyethylene / polyoxypropylene or ethoxylated / propoxylated); silicone emollients substituted with aromatic groups (for example, phenyl, alpha-methyl styryl, styryl, methylphenyl, alkylphenyl); silicone copolymers with other functional groups including: hydrogen, alkyl, methyl, amino, trifluoropropyl, vinyl, alkoxy, arylalkyl, aryl, phenyl, styryl, polyethers, esters, carboxylic compounds; alkylmethylsiloxanes or silicone waxes (for example, hexyl, octyl, lauryl, cetyl, stearyl); nonionic functional siloxane copolymers with silanol or trimethylsiloxy end groups; nonionic functional siloxanes with main structure groups which are linked with trisiloxane or methicone; nonionic silicone surfactants; tetraethoxysilane; tetramethoxysilane; hexametoxy silicone; oximetoxitrisiloxane; silicone emulsifiers; siloxane or silicone resins; alkyl silicone resins; polyoxyalkylene silicone resins; MQ resins such as those of Shiseido / Shin-etsu, for example Publication of Japanese Patent JP86143760 or from Waiker Chem. 6MBH (described in EP722970); alkoxysiloxanes; alkoxysilanes; methicones (polymethylalkysiloxanes); and combinations thereof. Non-limiting examples of carriers of P957 suitable modified silicones that are used in the gel-solid antiperspirant stick compositions herein include the following modified silicones available from Dow Corning: DC-556, Cosmetic Grade Fluid (phenyl trimethicone); DC-704 Diffusion Pump Fluid (Tetramethyl-Tetraphenyl-Trisiloxane); DC-705 Diffusion Pump Fluid; DC-1784 Emulsion; DC-AF Emulsion; DC-1520-US Emulsion; DC-593 Fluid (Dimethicone [and] Trimethylsiloxysilicate); DC-3225C Fluid (Cyclomethicone [and] Dimethicone Copolyol); DC-190 Fluid (Dimethicone Copolyol); DC-193 Fluid (Dimethicone Copolyol); DC-1401 (Cyclomethicone [and] Dimethiconol); DC-5200 Fluid (Copolyol from Laurylmethicone); DC-6603 Polymer Powder; DC-5640 Powder; DC-Q2-5220 (Dimethicone Copolyol); DC Q2-5324 (Dimethicone Copolyol); DC-2501 Cosmetic Wax (Dimethicone Copolyol); DC-2502 Fluid (Cetil Dimethicone); DC-2503 Wax (Stearyl Dimethicone); DC-1731 Volatile Fluid (Caproil Trimethicone); DC-580 Wax (Stearoxytrimethylsilane [and] Stearyl Alcohol); DC-1-3563 (Dimethiconal); DC-X2-1286 (Dimeticonol); DC-X2-1146A (Cyclomethicone [and] Dimethiconol); DC-8820 Fluid (with Amino functional group); DC Q5-0158A wax (stearoxitrimethylsilane); DC-Q2-8220 (Trimethylsilyllamodimethicone); DC-7224 (Trimethylsilyllamodimethicone); DC-X2-1318 Fluid (Cyclomethicone [y] Vinyl dimethicone); DC-QF1-3593A fluid P957 (Trimethylsiloxysilicate) and combinations thereof. Other non-limiting examples of suitable modified silicone carriers that are used in the gel-solid antiperspirant stick compositions herein include the following modified silicones available from General Electric: GE SF-1023 (Dimeti1-Diphenyl Siloxane); GE SF-1142 (Methylphenyl Siloxane Fluid); GE SF-1153 (Dimethyl-diphenyl-Siloxane); GE SF-1265 (Diphenyl-Dimethyl-Siloxane); GE SF-1328; GE SF-1188 (Dimethicone Copolyol); GE SF-1188A (Silicone and polyether copolymer); GE SF-1288 (silicone-polyether copolymer, dimethyl-methyl-3-hydroxypropyl ethoxylate); GE SF-1318 (Methylester Siloxane); GE SF-1328 (silicone surfactant, ethoxylated-propoxylated dimethyl-methyl-3-hydroxypropyl); GE SF-1550 (methylphenyl siloxane, hexamethyl-3-phenyl-3- [[trimethylsilyl] oxy] trisiloxane); GE SF-1632 (silicone wax); GE SS-4265 (Dimethicone [and] Trimethylsiloxysilicate) and combinations thereof. Other non-limiting examples of suitable modified silicone carriers that are used in the gel-solid antiperspirant stick compositions herein include the following modified silicones that are obtained from Goldschmidt; Abil EM-90 (silicone emulsifier); Abil EM-97 (polyether siloxane); Abil Cera 9810 (silicone wax or methicone C24-28); Abil Cera 2434 P957 (Stearoxi Dimethicone); Abil Cera 9800D (Stearil Dimethicone); Tegomer H-Si 2111, H-Si 2311, A-Si 2120, A-Si 2320, C-Si-2141, C-Si 2341, E-Si 2130, E-Si 2330, V-Si 2150, V-Si 2550, H-Si 6420, H-Si 6440, H-Si 6460 (Copolymers of Dimethicone Alpha-Omega) and combinations thereof. Other non-limiting examples of suitable modified silicone carriers that are used in gel-solid antiperspirant stick compositions include the following: Masil 756 from PPG Industries (Tetrabutoxypropyl Trisiloxane); bis-phenylhexameticone (from Silbione Oils 70633 V30 from Rhone-Poulenc); Silbione Oils 70646 (dimethicone copolyols from Rhone-Poulenc); silicone L-711, L-720, L-721 and L722 (dimethicone copolyols from Union Carbide); Silicone L-7000, L-7001, L-7002, L-7004, L-7500, L-7600, L-7602, L-7604, L-7605 and L-7610 (Dimethicone copolyols from Union Carbide); Unisil SF-R (UPI dimethiconol); Olin Silicate Clod (Tris [Tributoxyloxy] Methylsilane); silicone copolymer F-754 (dimethicone copolyol from SWS Silicones); and combinations thereof. Antiperspirant gel-solid stick compositions preferably contain, as an optional carrier liquid, a volatile silicone carrier. These volatile silicone carriers can be silicones of P957 cyclic, linear or branched chain that have the required volatility that is defined here. Non-limiting examples of suitable volatile silicones are described in Todd et al., "Volatile Silicone Fluids for Cosmetics", Cosmetics and Toiletries, 91: 27-32 (1976), which is incorporated herein by reference. Preferred volatile silicones are cyclic silicones having from about 3 to about 7, more preferably, from about 4 to 5 silicon atoms. Preferred are those that conform to the general formula: wherein n is from about 3 to about 7, preferably from about 4 to about 5, more preferably is 5. Volatile cyclic silicones in general have a viscosity value of less than about 10 centistokes. All viscosity values described herein are measured or determined at ambient conditions unless otherwise specified. Suitable volatile silicones used herein include, but are not limited to, cyclomethicone D-5 (commercially available from G. E. Silicones); Dow Corning 344 and Dow Corning 345 (obtained from Dow P957 Corning Corp.); GE 7207; GE 7158 and Silicone Fluids SF-1202 and SF-1173 (obtained from General Electric Co.); SWS-03314, SWS-03400, F-222, F-223, F-250, F-251 (available from SWS Silicones Corp.); Volatile Silicas 7158, 7207, 7349 (available from Union Carbide); Masil SF-V (available from Mazer) and combinations thereof. The optional liquid carrier may also comprise a non-volatile silicone carrier, preferably in combination with a volatile silicone carrier and, more preferably with a volatile silicone carrier and a modified silicone carrier, as described herein. These non-volatile silicone carriers are preferably linear silicones that include, but are not limited to, those that conform to any of the following formulas: CH, - wherein n is greater than or equal to 1. These linear silicone materials will generally have viscosity values of up to about 100,000 centistoke, preferably less than about 500 centistoke, more preferably, between about 1 and 200 centistoke, still with higher preference, between approximately 1 and 50 P957 centistoke, measured at environmental conditions. Examples of suitable linear and non-volatile silicones which are used in antiperspirant compositions include, but are not limited to, Dow Corning 200, hexamethyldisiloxane, Rhodorsil Oils 70047 which is obtained from Rhone-Poulenc, SF Masil Fluid which is obtained from Mazer, Dow Corning 225, Dow Corning 1732, Dow Corning 5732, Dow Corning 5750 (obtained from Dow Corning Corp.); SF-96, SF-1066 and SF18 (350) as Silicone Fluids (from G.E Silícones); Velvasil and Viscasil (available from General Electric Co.) and Silicone L-45, Silicone L-530, Silicone L-531 (from Union Carbide) and Siloxane F-221 and Slicone Fluid SWS-101 (from SWS Silicones). The optional liquid carriers may further comprise other non-polar and non-volatile liquid solvents or carriers such as, for example, mineral oil, petrolatum, and any other known non-volatile carrier liquid or solvent or that is safe and effective for topical application to the skin. human The optional liquid carrier may also comprise fluorochemicals such as fluorosurfactants, fluorotelémeros and perfluoropoliéteres, some examples of which are described in Cosmetics & Toiletries, Using Fluorinated Compounds in Topical Preparations, Vol. 111, p. 47-62, (October 1996) which is incorporated herein by reference. Specific examples of suitable fluorochemicals include, but are not limited to, perfluoropolymethyl isopropyl ethers, perfluoropolypropyl ethers, fluorinated telomer of acrylamide, fluorinated amide surfactants, perfluorinated thiol surfactants. Other more specific examples include, but are not limited to, polyperfluoroisopropyl ethers available from Dupont Performance Chemicals under the tradename Fluortress® PFPE oils, and the series of fluorosurfactants from Dupont Performance Chemicals under the tradename Zonyl® Fluorosurfactants.
F) Optional Nucleating Agents The gel-solid antiperspirant stick compositions of the present invention may preferably further comprise a nucleating agent to decrease the particle size of the gellant and / or to obtain the preferred morphology of the gelling particle that is described here . The optional nucleating agent that is used in the antiperspirant compositions of this invention should be a solid material at ambient conditions and have a solubility in the selected solvents less than the solubility of the gellant in the selected solvents or be in the form of a micronized particulate, P957 insoluble and inorganic. The nucleating agent typically crystallizes, gels, solidifies (except when the nucleating agent is an insoluble and micronized inorganic material) or acts as a core (eg promotes the formation of a small gelling nucleus) for the gelling agent just before, almost or at the same time in which the crystallization of the gellant is carried out in the selected solvents. The molar ratio of the solid gelling agent to the nucleating agent is between about 10: 1 and about 1000: 1, preferably between about 10: 1 and about 100: 1. These selected molar proportions will typically give rise to nucleating agent concentrations of between about 0.0001% to about 5%, preferably from about 0.001% to about 2%, more preferably from about 0.01% to about 1%. Preferred nucleating agents are those having a melting point of between about 40 ° C and about 200 ° C, more preferably between about 20 ° C below and 100 ° C above the melting point of the selected gellant. Antiperspirant compositions containing optionally optional nucleating agent are prepared by the following: 1) combining the gellant, the selected solvents and an optional nucleating agent as described herein; 2) heating the components or the combination of components to form a solution or another type of liquid dispersion or homogeneous liquid; and 3) solidifying the combination of components by cooling it below the solidification point of the solid gellant, to form the antiperspirant composition of the present invention. The nucleating agent used in the antiperspirant compositions includes fatty alcohols, fatty alcohol esters, ethoxylated fatty alcohols, esters or fatty acid ethers including waxes and triglycerides, silica, titanium dioxide, solid polyol and carboxylic acid polyesters and mixtures thereof. Suitable fatty alcohols which are used as optional nucleating agents include monohydric alcohols, ethoxylated fatty alcohols and fatty alcohol esters. Specific examples of the commercially available fatty alcohol nucleating agents include, but are not limited to, Unilin 550, Unilin 700, Unilin 425, Unilin 400, Unilin 350 and Unilin 325, all supplied by Petrolite. Suitable ethoxylated fatty alcohols include, but are not limited to, Unithox 325, Unithox 400 and Unithox 450, Unithox 480, P957 Unithox 520, Unithox 550, Unithox 720, Unithox 750, all of which are available from Petrolite. Non-limiting examples of suitable fatty alcohol esters include tri-isostearyl citrate, ethylene glycol di-12-hydroxystearate, tristearyl citrate, stearyl octanoate, stearyl heptanoate, and trilauryl citrate. Suitable fatty acid esters which are used as optional nucleating agents include esters of esters, monoglycerides, diglycerides, triglycerides and mixtures thereof. Glyceride esters are preferred. Non-limiting examples of suitable ester waxes include stearyl stearate, stearyl behenate, palmityl stearate, stearyl octyldodecanol, cetyl esters, cetearyl behenate, behenyl behenate, ethylene glycol distearate, ethylene glycol dipalmitate and beeswax. Examples of the commercial ester waxes include Kester waxes from Koster Keunen, Crodamol SS from Croda and Demalcare SPS from Rhone Poulenc. Preferred triglyceride nucleating agents include, but are not limited to, tristearin, tribehenate, behenyl palmityl behenyl triglyceride, palmityl stearyl palmityl triglyceride, hydrogenated vegetable oil, hydrogenated rapeseed oil, castor wax, fish oils, tripalmiten, Syncrowax HRC and Syncrowax. HGL-C P957 (Syncrowax is obtained from Croda, Inc.). Other suitable glycerides include, but are not limited to, glyceryl stearate and glyceryl distearate. Preferably, the optional nucleating agent is a solid polyester of polyol and carboxylic acid. Suitable solid polyol and carboxylic acid polyesters include those which are polyol esters or polyesters wherein the carboxylic acid ester groups of the polyester comprise a combination of: (a) long chain unsaturated carboxylic acid entities or a mixture of long chain unsaturated carboxylic acid and short chain saturated carboxylic acid entities; and (b) long chain saturated carboxylic acid entities, the ratio between (a) and (b) is about 1 to 15 to about 2 to 1. At least about 15%, preferably at least about 30. %, more preferably at least about 50% and still more preferably at least about 60% by weight of the total carboxylic acid entities of the polyesters are C20 or higher saturated carboxylic acid entities. The long chain unsaturated carboxylic acid entities are typically straight chain and contain at least about 12, preferably about 12 to about 26, most preferably P957 about 18 to about 22 carbon atoms. The most preferred unsaturated carboxylic acids are C18 mono- and / or di-unsaturated carboxylic acids. The short chain saturated carboxylic acids are typically unbranched and contain from about 2 to about 12 carbon atoms, preferably from about 6 to about 12 and more preferably from about 8 to about 12 carbon atoms. The long chain saturated carboxylic acids are typically straight chain and contain at least about 20, preferably about 20 to about 26 carbon atoms and more preferably about 22 carbon atoms. The molar ratio of the group (a) of carboxylic acid entities to Group (b) of carboxylic acid entities in the polyester molecule is between about 1:15 and about 2: 1, preferably between about 1: 7 to about 5. : 3, and more preferably between about 1: 7 and about 3: 5. The average degree of esterification of these carboxylic acid esters is such that at least about 2 of the hydroxyl groups of the polyol are esterified. In the case of sucrose polyesters of between about 7 to about 8 of the hydroxyl groups of the polyol are preferably P957 esterified. Typically, practically all hydroxyl groups of the polyol are esterified, for example, at least about 85% and preferably at least about 95%. The preferred polyols of the polyol carboxylic acid esters, solids, are sugars, including monosaccharides and disaccharides and trisaccharides, containing from about 4 to about 11 hydroxyl groups. The most preferred sugars are those containing from about four to about 8, more preferably from about 6 to about 8 hydroxyl groups. Examples of those containing four hydroxyl groups are the monosaccharides of xylose, arabinose and combinations thereof. Suitable polyols containing five hydroxyl groups are monosaccharides of galactose, fructose, mannose, glucose and combinations thereof. Examples of disaccharide polyols that can be used include maltose, lactose, sucrose and combinations thereof, all of which contain eight hydroxyl groups. The preferred polyol is sucrose. Examples of long chain unsaturated carboxylic acid entities include, but are not limited to, lauroleate, myristoleate, palmitoleate, oleate, elaidate, erucate, linoleate, linolenate, arachidonate, eicosapentaentoate and docosahexaenoate. For P957 oxidative stability are preferred mono and diunsaturated fatty acid entities. Examples of suitable short chain saturated carboxylic acid entities include, without limitation, acetate, caproate, caprylate, caprate and laurate. Examples of suitable saturated, long chain carboxylic acid entities include, without limitation, arachididate, behenate, lignocerate and cerotate. Of course, the long chain unsaturated carboxylic acid entities can be used alone or in mixtures with each other or in mixtures with saturated and short chain carboxylic acid entities, in all proportions. Similarly, the long chain saturated carboxylic acid entities can be used in combination with each other, in all proportions. Caboxylic acid entities mixed from source oils containing substantial amounts of the desired saturated or unsaturated acids can be used as the acid entities to prepare the compounds that are used as nucleating agents herein. The mixed carboxylic acids of the oils should contain at least about 30%, preferably at least about 50% and, more preferably, at least about 80% of the desired, saturated acids P957 or unsaturated. For example, rapeseed oil fatty acids or soybean oil fatty acids can be used in place of pure unsaturated fatty acids from C? 2 to Ci6- The higher fatty acids, rape seed oil, euricic, hydrogenated, can be used in place of the pure saturated acids of C2o to C26 - Preferably, C2o and higher acids, or their derivatives, for example methyl or other lower alkyl esters, are concentrated, for example, by distillation. Fatty acids from palm kernel oil or coconut oil can be used as a source of C8 to C12 acids. An example of the use of source oils to make solid polyol polyesters which are used in the antiperspirant compositions herein is the preparation of solid sucrose polyester, which employs fatty acids of the higher oleic sunflower oil and rapeseed oil, euricic, superior, substantially hydrogenated in its entirety. When the sucrose is virtually completely esterified with a 1: 3 weight mixture of methyl esters of the fatty acids of these two oils, the resulting sucrose polyester will have a molar ratio of unsaturated Cis-acid radicals to higher saturated acid radicals C20 of about 1: 1 and about 28.6 weight percent of the total fatty acids in the P957 polyester will be C22 fatty acids • The higher the unsaturated and saturated acid ratios desired in the carboxylic acid raw materials used to make solid polyester polyols, the more efficient the ester's ability to function as a nucleating agent . Examples of solid polyol carboxylic acid polyester nucleating agents that are used in the antiperspirant compositions herein include, without limitation, the octaester of raffinose, wherein the esterifying carboxylic acid entity is linoleate and behenate in a molar ratio of 1: 3, the maltose heptaester wherein the esterifying carboxylic acid entities are fatty acids from sunflower seed oil and lignocerate in a molar ratio of 3: 4; the octaester of sucrose wherein the esterifying carboxylic acid entities are oleate and behenate in a molar ratio of 2: 6, and the octaester of sucrose wherein the esterifying carboxylic acid entities are laurate, linoleate and behenate in a molar ratio of 1 : 3: 4 A preferred material is the sucrose polyester wherein the degree of esterification is 7-8 and wherein the fatty acid entities are mono and / or di-unsaturated, C18 and behenic, in a molar ratio of P957 unsaturated: behenic from 1: 7 to 3: 5. The particularly preferred nucleating agent of polyol ester is the octaester of sucrose wherein there are approximately 7 behenic fatty acid entities and about 1 oleic entity in the molecule. The solid carboxylic acid polyesters herein can be made according to prior art methods to prepare polyol polyesters. See, for example, U.S. Patent No. 5,306,516 to Letton et al., Issued April 26, 1994; U.S. Patent No. 5,306,515 to Letton et al., Issued April 26, 1994; U.S. Patent No. 5,305,514 to Letton et al., Issued April 26, 1994; U.S. Patent No. 4,797,300 to Jandacek et al., Issued January 10, 1989; U.S. Patent No. 3,963,699 to Rizzi et al., Issued June 15, 1976, U.S. Patent No. 4,518,772 to Volpenhein, issued May 21, 1995 and U.S. Patent No. 4,517,360 Volpenhein, granted on May 21, 1985, all of which are incorporated as a reference. The non-solubilized, micronized, inorganic nucleating agents suitable for the antiperspirant compositions of the present invention include materials such as silica, titanium dioxide and combinations P957 of them. These materials contain submicron particles (average particle size, generally less than about 1 μm, preferably less than about 0.2 μm) that aid in the production of small crystals or gelling particles. Preferred nucleating agents and preferred concentrations of nucleating agents that are used in the antiperspirant compositions include succinic acid Cis (0.1%), 1, 9-nonanodioc acid (0.1%), Teflon (0.1%), silica (0.1%), copolymer of polysiloxane (2%), sucrose octabehenate (0.5%, 0.75%, 1.0%), Unilin 350 (0.1%), Unilin 550 (0.1%), Unilin 700 (0.1%), trihydroxystearin (0.1%) and combinations of the same.
J) Other Optional Components The gel-solid antiperspirant stick compositions of this invention may further comprise one or more optional components that may modify the physical, chemical or aesthetic characteristics of the composition or serve as additional "active" components, when deposited on the skin. The compositions may also comprise other optional inert ingredients. Many of these optional materials are already known in the antiperspirant art and can be used in the compositions P957 of this, as long as these optional materials are compatible with the essential materials described here, or do not unduly diminish the performance of the product. Non-limiting examples of optional materials include active components such as bacteriostats and fungistatics, and "non-active" components such as dyes, perfumes, emulsifiers, chelants, distributing agents, preservatives, agents in waste scavengers, process aids such as viscosity modifiers and washing elimination aids. Examples of these optional materials are described in U.S. Patent No. 4,049,792 to Elsnau, issued September 20, 1977; Canadian Patent No. 1,164,347 to Beckmeyer et al., issued March 27, 1984; U.S. Patent No. 5,019,375 to Tanner et al., Issued May 28, 1991; and U.S. Patent No. 5,429,816 to Hofrichter et al., issued July 4, 1995, the disclosures of which are incorporated herein by reference. Other non-limiting examples of the optional materials include various processing aids, especially chelants such as those described in U.S. Patent 5,516,511, issued to Motley et al. on May 14, 1996 that is incorporated here by P957 reference. The concentration of the chelants in the composition ranges from about 0.01% to about 10%, preferably from about 0.05% to about 5%, more preferably from about 0.01% to about 2% by weight of the composition. Non-limiting examples of suitable chelants include acetylacetone, ethylene diamino-N, N, N ', N' -tetraacetic acid (EDTA) nitrilotriacetic acid, oxalate, citric acid, 1,2-diaminocyclohexane acid, N, N, N ', N'-tetraacetic, 4,5-dihydroxybenzene-1,3-disulfonic acid, pyrocatechol-3,5'-disulfonate, salicylic acid, 5-sulfosalicylic acid, xylenol orange, aurintricarboxylic acid, 2,2'-pyridyl ethylenediamine, glycine , 8-hydroxyquinoline-5-sulfonic acid, lactic acid, 1,10-phenanthroline, pyridine, pridine-2,6-dicarboxylic acid, 8-quinolinol, succinic acid, tartaric acid, thioglycolic acid, 1, 1, 1-trifluoro -3, 2 'teniacetone, triethylene tetramine and combinations thereof. EDTA is preferred. Optional chelators can be used in their salt form. Preferred salts include mono and divalent cations and combinations thereof to provide a total charge of between 0 and about 4. The most preferred salts are Na +, K +, Li + and Mg ++ and mixtures thereof, preferably Na + and K + Y P957 mixtures thereof. More preferably, EDTA is disodium. Antiperspirant gel-solid stick compositions can further comprise up to about 5%, typically between about 0.05% and about 4% by weight of known or suitable perfumes or fragrances for application to human skin. These perfumes or fragrances may be selected to provide the composition or the applied surface with the desired aroma, or they may be selected to mask malodours associated with human perspiration or malodor inherently associated with the gel-solid stick antiperspirant composition (hereinafter he refers to them as odor masking fragrances). Some non-limiting examples of suitable odor masking fragrances that are used in gel-solid antiperspirant compositions are described in U.S. Patent No. 5,554,588, U.S. Patent No. 4,278,658, U.S. Pat. No. 5,501,805 and EP Patent Application No. 684 037 Al, all of which are hereby incorporated by reference in their entirety. Preferred odor masking fragrances are those having a deodorizing value of at least about 0.25, preferably between about 0.25 and about 3.5, including P957 greater preference between about 0.9 and about 3.5, as measured by the deodorant value test described in Patent Application EP 684 037 Al. The gel-solid antiperspirant stick compositions of this invention can also be formulated to comprise other dispersed solids or other materials in addition to or in place of the particulate antiperspirant actives. These other dispersed solids or other materials include any material known or that is suitable for topical application to human skin. The gel-solid antiperspirant stick compositions can also be formulated as gel-solid stick compositions that do not contain antiperspirant or any other active, particulate or otherwise material.
Manufacturing Method The gel-solid antiperspirant stick compositions of this invention can be prepared by any effective method or technique, suitable for providing a gel-solid antiperspirant stick composition having the required crystalline matrix and other product characteristics described here. These methods involve the formulation of the essential components of the composition to form a gel-solid that P957 has the required ratio of elastic modulus to viscous modulus, product hardness and visible residue index, wherein the crystalline matrix within the composition comprises elongated, non-polymeric gelling crystals having a dimensional ratio greater than about 2, preferably greater than about 6 and an average particle diameter that is minimized (preferably to less than about 1 μm) through techniques aimed at minimizing the crystalline particle size in a composition. The crystalline particle size in the preferred embodiments of this invention can be determined by techniques well known in the art, including electron or light microscopy of the composition, wherein the composition is formulated for analytical purposes without active particulate antiperspirant or other particles solid. Without this reformulation, it is more difficult to directly determine and directly distinguish the crystalline particle size of the gellant and the morphology from the particle size and morphology with which other non-gelling particles contribute. The reformulated composition is then evaluated by electron or light microscopy or by other similar methods. The techniques for preparing the compositions of P957 gel-solid antiperspirant stick of this invention include those methods suitable for formulating compositions containing small gelling crystalline particles. Appropriate techniques to decrease the size of crystalline gelling particle include the use of nucleating agents, the formulation with selected carriers or gelling agents or carrier / gellant combinations, the control of the crystallization rates including controlling the formulation, the flow regime of the process and the process temperatures and other methods described herein. All of these methods should be applied to the formulation to control or minimize the particle size of the gelling crystal and / or to form the desired elongated crystalline particles, so as to form the desired crystalline matrix of the composition.
Method of Use The gel-solid antiperspirant stick compositions can be applied topically to the armpit or to any other area of the skin in an amount effective to treat or reduce malodour or moisture by perspiration. The composition preferably is applied in an amount ranging from about 0.1 grams to about 20 grams, more preferably, between P957 about 0.1 grams to about 10 grams, still more preferably, between about 0.1 grams to about 1 gram to the desired area of the skin. The compositions are preferably applied to the armpit or to another area of the skin once or twice a day, preferably once a day, to achieve effective control of perspiration and odor for a prolonged period of time.
EXAMPLES The following non-limiting examples illustrate the specific embodiments of the gel-solid antiperspirant stick compositions of this invention, including the methods of manufacture and use. Each of the exemplified compositions is prepared by combining all listed components, except the antiperspirant active ingredient and other materials such as optional perfumes, optional chelating agents and optional inorganic particles. The combined components are heated to about 100 ° C with agitation to form a hot liquid, after which all the materials are added to the hot liquid. The hot liquid is allowed to cool with stirring just before the solidification point, at which point the liquid composition is cooled and poured into the liquid.
P957 applicator containers and allow to cool and solidify to the required product hardness. Each of the exemplified compositions comprises a crystalline gel matrix comprising crystalline particles with a dimensional ratio greater than about 6, and an average particle size of crystalline gelling agent of less than about 1 μm. Each of the exemplified compositions also has a visible residue index of between about 11 and about 30 in L-value, a product hardness of between about 500 and 5,000 grams "force and a G '/ G ratio" between about 0.1 and about 100. Each of the antiperspirant and anti-perspirant compositions are applied topically to the armpit area of the skin, according to the methods of use described herein, and improved performance is provided with little appearance of residue, greater efficacy, stability and Aesthetics All the exemplified amounts are percentages by weight based on the total weight of the antiperspirant gel-solid stick composition, unless otherwise specified.
P957 TABLE 1 1. Fluid 245 Dow Corning; General Electric SF 1202 2. Sucrose octa ester predominantly esterified with portions of behenic acid.
P957 TABLE 2 1. Fluid 245 Dow Corning; General Electric SF 1202 2. Sucrose octa ester predominantly esterified with portions of behenic acid.
P957

Claims (10)

  1. CLAIMS: 1. An anhydrous antiperspirant gel-solid stick composition comprising: (a) from about 0.5% to about 60% by weight of an antiperspirant active agent; (b) from 1% to 15% by weight of a primary gelling agent; (c) from 1% to 50% by weight of a non-polar volatile hydrocarbon solvent having a solubility parameter of less than 8 (cal / cm3) 0.5, a vapor pressure of between 0.01 mmHg and 6 mmHg and an average boiling point of less than 250 ° C; and (d) from 0.01% to 10% by weight of a polar solvent miscible in water having a solubility parameter of between 12.5 (cal / cm3) 0 * 5 to 25 (cal / cm3) 0 * 5; where the composition has a visible residual index of between 11 to 30 of the L value, a product hardness of between 500 grams force and 5,000 grams force and a ratio of elastic modulus to viscous modulus of between 0.1 to 100.
  2. 2. The The composition according to claim 1, wherein the primary gelling agent is selected from the group consisting of 12-hydroxystearic acid, esters of 12-hydroxystearic acid, amides of 12-hydroxystearic acid and combinations thereof. P957
  3. 3. The composition according to any of the preceding claims, wherein the composition further comprises a secondary gellant selected from the group consisting of: n-acylamino acid amides, n-acylamino acid esters and combinations thereof, wherein the ratio in The weight of the primary gellant relative to the secondary gellant is between 1: 2 and 20: 1.
  4. 4. The composition according to any of the preceding claims, wherein the non-polar volatile hydrocarbon solvent is a branched chain volatile hydrocarbon having from 4 to 40 carbon atoms, a solubility parameter of between 5 (cal / cm3) 0 * 5 to less than 8.0 (cal / cm3) 0 * 5 and a vapor pressure of between 0.02 mmHg and 2.0 mmHg at 25 ° C.
  5. The composition according to any of the preceding claims, wherein the composition comprises a combination of two or more branched chain volatile hydrocarbons having different molecular weights, each of which has from 6 to 20 carbon atoms.
  6. 6. The composition according to any of the preceding claims, wherein the branched chain volatile hydrocarbon is selected from the group consisting of C13-C14 Isoparaffin, C7-Cs Isoparaffin, Cs-Cg Isoparaffin, C-O-11 Isoparaffin, Isoparaffin Cn -C? 3, P957 Isoparaffin Cn-C? 2 and combinations thereof.
  7. The composition according to any of the preceding claims, wherein the water-miscible polar solvent is selected from the group of glycerin, propylene glycol, dipropylene glycol, ethanol, tripropylene glycol, butylene glycol, hexylene glycol, 1,2-hexanediol, propylene carbonate and combinations thereof .
  8. The composition according to any of the preceding claims, wherein the composition further comprises 0.01% to 10% by weight of a chelating agent.
  9. The composition according to any of the preceding claims, wherein the primary gelling agent consists of elongated crystalline particles having a dimensional ratio of at least 2, and wherein the hardness of the product is between 800 grams strength and 1,400 grams strength and the The ratio between the elastic modulus and the viscous modulus is between 0.1 and 50.
  10. 10. A method for treating or reducing moisture by perspiration and odor, which comprises applying the desired skin area from 0.1 grams to 20 grams of the composition of any of the preceding claims. P957
MXPA/A/1999/011635A 1997-06-23 1999-12-14 Low residue antiperspirant gel-solid stick compositions containing volatile nonpolar hydrocarbon solvents MXPA99011635A (en)

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