US3288681A - Anhydrous aluminum antiperspirant powder aerosol compositions and methods of preparation - Google Patents

Anhydrous aluminum antiperspirant powder aerosol compositions and methods of preparation Download PDF

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Publication number
US3288681A
US3288681A US191446A US19144662A US3288681A US 3288681 A US3288681 A US 3288681A US 191446 A US191446 A US 191446A US 19144662 A US19144662 A US 19144662A US 3288681 A US3288681 A US 3288681A
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United States
Prior art keywords
dispersion
propellent
antiperspirant
aluminum
parts
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US191446A
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English (en)
Inventor
Goldberg Melvin Arthur
Netzbandt William Roy
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Lever Brothers Co
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Lever Brothers Co
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Filing date
Publication date
Priority to GB1013386D priority Critical patent/GB1013386A/en
Application filed by Lever Brothers Co filed Critical Lever Brothers Co
Priority to US191446A priority patent/US3288681A/en
Priority to BR148796/63A priority patent/BR6348796D0/pt
Application granted granted Critical
Publication of US3288681A publication Critical patent/US3288681A/en
Anticipated expiration legal-status Critical
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Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q15/00Anti-perspirants or body deodorants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/30Characterized by the absence of a particular group of ingredients
    • A61K2800/31Anhydrous
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S8/00Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
    • Y10S8/10Polyvinyl halide esters or alcohol fiber modification

Definitions

  • This invention relates to an antiperspirant; and more particularly, it is concerned with an aerosol antiperspirant powder spray.
  • an aerosol antiperspirant powder spray can be provided by forming a dispersion comprising an altuninum compound, an alcohol and a propellent. This dispersion is passed through a screen and the screened dispersion is subsequently packaged in an aerosol can under pressure. A spray of anti-perspirant is dispensed therefrom as desired and a substantially dry product is provided when it strikes the skin.
  • an aluminum compound which is in fine particulate form and of a size sufficiently small to provide adequate coverage of the treated skin area.
  • An aluminum compound which has a particulate size to pass through a 200 mesh or finer screen, is suitable; however, finer sizes are preferred for better skin coverage and less likelihood of valve clogging.
  • the preferred aluminum compounds pass through a 325 or finer mesh screen which avoids clogging in the currently available valves.
  • an aluminum compound is defined herein as a compound which is not soluble in propellant and which has antiperspirant and astringent properties.
  • Preferred compounds are aluminum chlorhydrate (aluminum chlorhydroxide complex) and aluminum sulfate.
  • Aluminum chloride is also suitable for use in the practice of the invention provided that the dispersion is prepared and packed under strictly anhydrous conditions. It is also critical to use from about 4 to 10% of the aluminum compound, e.g., aluminum chlorhydrate, based upon the total weight of the aerosol antiperspirant powder spray. A larger amount is too dusty when sprayed and clogs the aerosol valve; and a smaller amount is relatively ineffective as an antiperspirant.
  • R is an aliphatic hydrocarbon group having 12 to 18 carbon atoms; R is selected from the group con sisting of an aliphatic hydrocarbon having 3 to 18 carbon atoms and an alkyleneoxy group having a terminal OH and having the formula (R"O) H wherein R" is an alkylene having at least 2 carbon atoms, n is an integer from 1 to 9, and the product of R" and n is from 3 to 18; and the sum of carbon atoms in R and R is from 15 to 34.
  • Specific esters within this generic structure include isopropyl myristate-palmitate, propylene glycol monooleate and stearyl palmitate.
  • esters within critical limits facilitates dispersion of the powder and in particular makes it easier to re-disperse any powder that may settle on standing. It has been found that from 2 to 5% esters based upon total weight of spray is the operable range; more than 5%, e.g., 6%, provides a powder film which is too wet and less than 2%, e.g., 1%, provides little observable benefit.
  • Alcohol is also a critical component in the instant dispersion. Any known commercial alcohol, e.g., an admixture of 5 parts of methyl alcohol and 100 parts of 200 proof ethyl alcohol, is applicable. However, the range of alcohol required for the success of the present invention is 2 to 4 wt. percent based upon the total spray. The resultant spray is too wet if a higher alcohol c0n tent is employed and there is powder agglomeration if a lower alcohol content is used.
  • the lower aliphatic alcohols are suitable provided the alcohol is soluble in propellent which includes the following: methanol, ethanol, n-propanol, isopropanol, propylene glycol, diethylene glycol and mixtures thereof.
  • the dispersion generally has a non-irritating germicide included therein within the range of 0.05 to 1.5 wt. percent based upon the total spray.
  • the following germicides among others are suitable: 3,4,5 tribromosalicylanilide, hexachlorophene [2,2'-methylene-bis(3,4,6-trichlorophenol)], benzalkonium chloride (alkyl-dimethylbenzyl-ammonium chloride), 3,4,4'-trichlorocarbanilide and 2,2,3,4-tetrabromosalicylanilide.
  • a liquefied gaseous propellent it is critical in the instant invention to add at least one liquefied gaseous propellent to the dispersion prior to the screening operation.
  • Dichlorodifluoromethane and 1,2-dichloro-l,1,2,2-tetrafluoroethane are suitable and either of them can be used as the only propellent in the system.
  • Trichloromonofiuoromethane is also suitable but it must be employed in an admixture with another propellent, e.g., an admixture of 50% dicholrodifiuoromethane and 50% trichloromonofluoromethane.
  • the trichloromonofluorometh-ane may also contain 0.3 nitromethane to inhibit acid formation.
  • the aforementioned propellents e.g., halogenated hydrocarbon propellents, comprise the balance of the aerosol antiperspirant powder spray, which is generally between 79 and based upon the total weight of the spray.
  • a perfume compound is usually included in the dispersion within 813 the range of .01 to .04%.
  • the perfume can be any one which is known in the art.
  • the following perfumes are satisfactory: oil of lavender; oil of sandalwood; ylang-ylang; geranium; patchouli; and mixtures thereof. These perfumes can be employed alone or in blends with other materials.
  • the dispersion with the aforementioned components After the dispersion with the aforementioned components has been formed, it is passed through a screen, such as a stainless steel screen with a mesh of at least 325. During this screening operation, the absorption of moisture should be avoided and agitation should be provided.
  • a screen such as a stainless steel screen with a mesh of at least 325.
  • Sufiicient dry powder can be screened for small batches if ample time is available for the screening operation, but it is impossible with the large scale production of the instant composition.
  • a dispersion can be screened readily on a large scale; this overcomes the necessity of screening the dry powder and makes this invention commercially feasible.
  • the screened dispersion is generally collected in a jacketed holding tank. However, a plain tank may be used with the screened dispersion being recirculated through a heat exchanger. The dispersion is thereby cooled to the desired temperature, e.g., 20 F. or less.
  • the cooled dispersion is subsequently incorporated into an aerosol can.
  • Additional propellents besides those included in the dispersion, may also be independently incorporated into the can. For example, if trichloromonofluoromethane is employed in the dispersion, dichlorodifluoromethane may be added to the aerosol can after the dspersion is packaged therein.
  • a valve is then crimped on the aerosol can containing the dispersion and, optionally, the additional propellents.
  • the additional propellents are introduced through the valve after crimping, the dispersion need not be cooled below room temperature. As desired, the contents in the can are dispensed therefrom to provide an aerosol antiperspirant powder spray on the skin.
  • an antiperspirant which is an aerosol powder spray.
  • Some of the components in the instant end product have been used in other forms of antiperspirant (U.S. Pat. Nos. 2,492,085 and 2,890,087).
  • the success of this invention is dependent upon adhering to the critical limits of components therein and by following the required processing conditions. For example, it is essential that the dispersion be eflicient enough to prevent rapid settling of the solid particles.
  • Example 'I The following components were used to prepare an aerosol antiperspirant powder spray.
  • Wt. percent 1 Consists of 200 proof ethyl alcohol containing 5 gallons of methyl alcohol for every '100 gallons of ethyl alcohol appearance, clear, colorless liquid odor, equal approved sample specific gravity, .7938 wt./gallon, 6.60 pounds ethyl alco- 1101 by volume, 95.2% moisture 0.00, 0. 1%.
  • Example 11 An aerosol antiperspirant spray was provided from the ingredients listed herebelow.
  • Aluminum chlorhydroxide complex analysis shows aluminum oxide (A1203), 47.0i-1.0% chlorides (*CI), 16.3% i0.5%; sulphates (S04), .05% max.; heavy metals (as Pb), p.p.m. max. arsenic (AS203), 2 ppm. max.; iron (as Fe), 0.1% max; Al Cl atomic ratio, 2.1: 1; pH of 15 sol.,h4.5 m1n.; specific gravity, 1.9 and 97% passes thru 325 mes Givaudan Delawanna predominantly isopropyl myris ta'te, with a small amount of isopropyl esters of other saturated fatty acids; color, colorless liquid; odor, practically odorless; Sp.
  • the TBS was dissolved in the alcohol while warming slightly.
  • the Deltyl and perfume were added with subsequent cooling to below 74 F.
  • Liquefied propellent 11 and chlorhydrol were consecutively incorporated into the system in conjunction with agitation.
  • the resultant dispersion was passed through a 325 mesh stainless steel screen with continuous stirring into a jacketed holding tank which was also equipped with an agitator.
  • the screened dispersion was cooled to 20 F. and loaded into aerosol cans.
  • Liquefied propellent 12 was then added to the cans. Immediately thereafter, valves were crimped onto the cans.
  • a suitable packaged end product was obtained in this example.
  • Example III An aerosol antiperspirant powder spray was formed from the components indicated herebelow following the same procedures described in Example II.
  • Example IV Antiperspirants (Wt. percent) Ingredients Aluminum chlorhydratc Alcohol per Example I Freon ll-3 1 Propellent 1 Isopropyl myristate. Stearyl palrnitate Z Propylene glycol monooleate.
  • Antiperspirants D, E, F, G and H were formed from dispersions with the following ingredients therein.
  • Antiperspirant (Wt. percent) Ingredients D E F G H Chlorhydrol 8. 10. 00 8. 00 8. 00 8. 00 Isopropyl myristate 2. 0O 2. 00 2. 00 2. 00 2. 00 Alcohol per Example L- 4. 00 4 00 4. 00 4. 00 Talc 8. 00 Gll TB S. 0. lerfume. 0. 01 Propellent l1 38. 54 Propellent 12 42. 945 26. 39 25 79 34. 42 39. 40 Propellent 114 2 51. 46
  • Example II After screening and cooling as described in Example II, the dispersions were incorporated into aerosol containers by gravity flow. Cold propellent 12 was then incorporated into the containers and valves were crirnped thereon.
  • the containers were subjected to steam testing at 125 to 135 F., and then to water-bath testing at about 95 F. After being subjected to these tests, the containers were capped.
  • Example VI The following components were used to form an aerosol antiperspirant powder spray.
  • a commercially suitable antiperspirant in the form of a powder spray was obtained when the contents were dispersed from the aerosol can.
  • a composition under pressure for providing an aerosol antiperspirant powder spray on the skin which comprises about 4 to 10 parts of an aluminum compound which is not soluble in propellent and which has antiperspirant properties, said aluminum compound being aluminum chlorhydroxide complex, aluminum sulfate or aluminum chloride; about 2 to 4 parts of a lower aliphatic alcohol; and 79 to 94 parts of a liquefied gaseous propellent; said composition having been screened as an anhydrous dispersion of aluminum compound in propellent with a screen not larger than 200 mesh.
  • composition according to claim 1 which also contains a germicide, a perfume and an ester having the general structure:
  • R is an aliphatic hydrocarbon group having 12 to 18 carbon atoms; R is an aliphatic hydrocarbon having 3 to 18 carbon atoms; and the sum of carbon atoms in R and R is from 15 to 34.
  • a composition under pressure which comprises about 4 to 10 parts of an aluminum compound which is not soluble in propellentand which has antiperspirant properties, said aluminum compound being aluminum chlorhydroxide complex, aluminum sulfate or aluminum chloride; about 2 to 5 parts of an ester which is isopropyl myristatepalmitate, propylene glycol monooleate or stearyl palmitate; about 2 to 4 parts of a lower aliphatic alcohol; about 0.05 to 1.5 parts of a gennicide; about 0.01 to 0.04 part of a perfume; and about 79 to 94 parts of a liquefied gaseous propellent; said composition having been passed through a screen not larger than 325 mesh as an anhydrous dispersion of aluminum compound in propellent; said composition being packaged in an aerosol container for dispensing a dry antiperspirant powder spray on the skin.
  • a composition under pressure for providing a dry aerosol antiperspirant powder spray on the skin which comprises 8 parts of aluminum chlorhydroxide complex which is not soluble in propellent and which has antiperspirant properties, 2 parts of isopropyl myristate, 0.03 part of perfume, 4 parts of ethyl alcohol, 0.08 parts of 2,2-methy1ene-bis(3,4,6-trichlorophenol) and 42.945 parts of liquefied gaseous trichlor-omon-ofiuoromethane as a pro pellent; said composition having been passed through a 325 mesh screen as an anhydrous dispersion of said aluminum compound in said propellent and subsequently cooled; said composition being packaged in an aerosol container with 42.945 parts of liquefied gaseous dichlorodifiuoromethane.
  • a process for forming an aerosol antiperspirant powder spray for dispensing from an aerosol container to provide a dry antiperspirant on the skin which comprises preparing an anhydrous dispersion comprising about 4 to 10 parts of an aluminum compound which is not soluble in propellent and which has antiperspirant properties, said aluminum compound being aluminum chlorhydroxide complex, aluminum sulfate or aluminum chloride, about 2 to 4 parts of a lower aliphatic alcohol and about 79 to 94 parts of a liquefied gaseous propellent; passing said dispersion through a screen not larger than 200 mesh; and packaging said screened dispersion in an aerosol container.
  • R is an aliphatic hydrocarbon group having 12 to 18 carbon atoms; R is an aliphatic hydrocarbon having 3 to 18 carbon atoms; and the sum of carbon atoms in R and R is from 15 to 34.
  • a process for forming an aerosol antiperspirant powder spray for dispensing from an aerosol container to provide a dry antiperspirant on the skin which comprises preparing an anhydrous dispersion comprising about 4 to 10 parts of an aluminum compound which is not soluble in propellent and which has antiperspirant properties, said aluminum compound being aluminum chlorhydroxide complex, aluminum sulfate or aluminum chloride, about 2 to 5 parts of an ester which is isopropyl myristatepalrnitate, propylene glycol monooleate or stearyl palmitate, about 2 to 4 parts of a lower aliphatic alcohol, about 0.05 to 1.5 parts of a germicide, about 0.1 to 0.4 part of a perfume and a liquefied gaseous first propellent; passing said dispersion through a screen not larger than 325 mesh; cooling said screened dispersion to a temperature below 20 F.; packaging said cooled dispersion in an aerosol container; and incorporating subsequently a liquefied gaseous second propellent into said

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  • Animal Behavior & Ethology (AREA)
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US191446A 1962-05-01 1962-05-01 Anhydrous aluminum antiperspirant powder aerosol compositions and methods of preparation Expired - Lifetime US3288681A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
GB1013386D GB1013386A (hu) 1962-05-01
US191446A US3288681A (en) 1962-05-01 1962-05-01 Anhydrous aluminum antiperspirant powder aerosol compositions and methods of preparation
BR148796/63A BR6348796D0 (pt) 1962-05-01 1963-04-30 Composicao anti-sudorifera e processo de preparacao

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3472928A (en) * 1968-02-08 1969-10-14 Chase Products Co Antiperspirant composition containing aluminum hydroxychloride
US3863005A (en) * 1970-03-05 1975-01-28 Aerosol Tech Inc Dual astringent composition
US3876758A (en) * 1969-12-01 1975-04-08 Stewart M Beekman Process for preparing alcohol solutions of aluminum chlorhydroxides for antiperspirant use and for other uses and compositions containing the same
US3920807A (en) * 1970-08-18 1975-11-18 Lever Brothers Ltd Antiperspirant and deodorant compositions
US3968203A (en) * 1965-10-01 1976-07-06 Jerome G. Spitzer Aerosol astringent composition
US4010252A (en) * 1974-12-19 1977-03-01 Colgate-Palmolive Company Antimicrobial compositions
US4018887A (en) * 1969-12-29 1977-04-19 The Procter & Gamble Company Amide-stabilized dry powder aerosol antiperspirant compositions and method of preparation
US4018888A (en) * 1969-12-29 1977-04-19 The Procter & Gamble Company Amine-stabilized dry powder aerosol antiperspirant compositions and method of preparation
US4045548A (en) * 1974-02-13 1977-08-30 The Procter & Gamble Company Aerosol antiperspirant containing emollients
US4305930A (en) * 1977-10-20 1981-12-15 Armour-Dial, Inc. Synergistic deodorant compositions
US4411883A (en) * 1973-02-05 1983-10-25 Colgate-Palmolive Company Antiperspirant
US5605682A (en) * 1992-04-16 1997-02-25 Colgate-Palmolive Company Antiperspirant aerosol composition with high solids content
WO2002065997A1 (en) * 2001-02-21 2002-08-29 Unilever Plc Antiperspirant or deodorant compositions

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3638327A (en) * 1969-04-17 1972-02-01 Gillette Co Process for producing aluminum chlorhydroxides
GB9604340D0 (en) * 1996-02-29 1996-05-01 Unilever Plc Antiperspirant aerosol composition and method of making same

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2823169A (en) * 1955-05-23 1958-02-11 Reheis Company Inc Substituted aluminum alcoholates and methods of making same
US2872379A (en) * 1955-04-22 1959-02-03 Thomae Gmbh Dr K Aerosol antiperspirant composition preparation
US2959325A (en) * 1954-04-29 1960-11-08 Risdon Mfg Co Method and apparatus for dispensing dry powders
US3014844A (en) * 1957-01-31 1961-12-26 Riker Laboratories Inc Self-propelling powder dispensing compositions
US3088874A (en) * 1960-05-23 1963-05-07 Union Carbide Corp Powder aerosol

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2959325A (en) * 1954-04-29 1960-11-08 Risdon Mfg Co Method and apparatus for dispensing dry powders
US2872379A (en) * 1955-04-22 1959-02-03 Thomae Gmbh Dr K Aerosol antiperspirant composition preparation
US2823169A (en) * 1955-05-23 1958-02-11 Reheis Company Inc Substituted aluminum alcoholates and methods of making same
US3014844A (en) * 1957-01-31 1961-12-26 Riker Laboratories Inc Self-propelling powder dispensing compositions
US3088874A (en) * 1960-05-23 1963-05-07 Union Carbide Corp Powder aerosol

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3968203A (en) * 1965-10-01 1976-07-06 Jerome G. Spitzer Aerosol astringent composition
US3472928A (en) * 1968-02-08 1969-10-14 Chase Products Co Antiperspirant composition containing aluminum hydroxychloride
US3876758A (en) * 1969-12-01 1975-04-08 Stewart M Beekman Process for preparing alcohol solutions of aluminum chlorhydroxides for antiperspirant use and for other uses and compositions containing the same
US4018887A (en) * 1969-12-29 1977-04-19 The Procter & Gamble Company Amide-stabilized dry powder aerosol antiperspirant compositions and method of preparation
US4018888A (en) * 1969-12-29 1977-04-19 The Procter & Gamble Company Amine-stabilized dry powder aerosol antiperspirant compositions and method of preparation
US3863005A (en) * 1970-03-05 1975-01-28 Aerosol Tech Inc Dual astringent composition
US3920807A (en) * 1970-08-18 1975-11-18 Lever Brothers Ltd Antiperspirant and deodorant compositions
US4411883A (en) * 1973-02-05 1983-10-25 Colgate-Palmolive Company Antiperspirant
US4045548A (en) * 1974-02-13 1977-08-30 The Procter & Gamble Company Aerosol antiperspirant containing emollients
US4010252A (en) * 1974-12-19 1977-03-01 Colgate-Palmolive Company Antimicrobial compositions
US4305930A (en) * 1977-10-20 1981-12-15 Armour-Dial, Inc. Synergistic deodorant compositions
US5605682A (en) * 1992-04-16 1997-02-25 Colgate-Palmolive Company Antiperspirant aerosol composition with high solids content
WO2002065997A1 (en) * 2001-02-21 2002-08-29 Unilever Plc Antiperspirant or deodorant compositions

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BR6348796D0 (pt) 1973-07-03

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