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WO1994024994A1 - Microcristallites de l'ingredient bicarbonate portant un revetement de polymere hydrophile - Google Patents

Microcristallites de l'ingredient bicarbonate portant un revetement de polymere hydrophile Download PDF

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Publication number
WO1994024994A1
WO1994024994A1 PCT/US1994/001193 US9401193W WO9424994A1 WO 1994024994 A1 WO1994024994 A1 WO 1994024994A1 US 9401193 W US9401193 W US 9401193W WO 9424994 A1 WO9424994 A1 WO 9424994A1
Authority
WO
WIPO (PCT)
Prior art keywords
powder composition
accordance
bicarbonate
hydrophilic polymer
particles
Prior art date
Application number
PCT/US1994/001193
Other languages
English (en)
Inventor
Richard T. Murphy
M. Stephen Lajoie
Original Assignee
Church & Dwight Company, Inc.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Church & Dwight Company, Inc. filed Critical Church & Dwight Company, Inc.
Priority to AU65485/94A priority Critical patent/AU6548594A/en
Priority to CA002144660A priority patent/CA2144660C/fr
Publication of WO1994024994A1 publication Critical patent/WO1994024994A1/fr

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11—Encapsulated compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/12—Face or body powders for grooming, adorning or absorbing
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q15/00—Anti-perspirants or body deodorants
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns

Definitions

  • Anhydrous antiperspirant stick systems have good consumer acceptance primarily due to the ease of application to the skin, good cosmetic esthetics and an acceptable degree of effectiveness.
  • anhydrous stick systems numerous water based systems were developed in which the active astringent salts were solubilized in a thickened or gelled composition.
  • Anhydrous stick compositions that suspend the aluminum salt in a hydrophobic matrix are described in U.S. 4,049,792. These compositions employ waxy materials and long chain fatty esters to form a stick that delivers the active astringent salts to the skin.
  • Cosmetic stick compositions made in accordance with these embodiments are greasy, and the active astringent salt is enveloped in a manner that prevents maximum performance.
  • volatile silicone fluids replacement of the less volatile long chain fatty esters is described in U.S. 4,126,679.
  • This disclosure teaches the advantage of utilizing a volatile non-staining liquid such as cyclic dimethylpolysiloxanes (referred to as volatile silicones) , in combination with various types of waxes, as a carrier for the active astringent salts in an antiperspirant stick composition.
  • volatile silicones cyclic dimethylpolysiloxanes
  • Similar antiperspirant stick compositions containing volatile silicones are described in United States Patent Numbers 4,511,554; 4,980,156; and 4,985,238.
  • One or more objects of the present invention are accomplished by the provision of a powder composition which is composed of particles having an average particle size between about
  • the particles comprise a hydrophilic polymer surface coating having an encapsulated core matrix content of at least two crystallites of water-soluble inorganic compound selected from alkali metal bicarbonate and ammonium bicarbonate.
  • particle size refers to the largest size dimension of a particle.
  • dimensional axial ratio refers to the ratio of the largest axial diameter to the other axial diameters.
  • water-soluble refers to a bicarbonate salt which has a solubility of at least about five grams per 100 grams of water at 25°C.
  • crystallite and “microcrystallite” as employed herein refer to micro-size crystalline particles of bicarbonate salt.
  • the encapsulated microcrystalline bicarbonate ingredient of an invention powder composition is selected from alkali metal and ammonium bicarbonates , such as sodium bicarbonate, potassium bicarbonate and ammonium bicarbonate, and mixtures thereof.
  • the encapsulated bicarbonate core matrix can contain up to about 30 weight percent, based on the weight of bicarbonate ingredient, of an alkali metal or ammonium carbonate compound in admixture with the bicarbonate crystallites.
  • the encapsulated bicarbonate crystallites in the core matrix have an average particle size between about 0.5-30 microns.
  • the encapsulated bicarbonate crystallites have a particle size distribution in which at least 80 percent of the particles have a particle size in the range between about 0.1-5 microns.
  • Fig. 1 is a Scanning Electron Microscope photomicrograph illustrating particles of starch- coated sodium bicarbonate deodorant.
  • the particle size distribution substantially is in the range between about 10-40 microns, and each particle contains an average of about 2-10 bicarbonate crystallites in the core matrix.
  • the bicarbonate crystallites are "sand ⁇ like" and approximately spherical in configuration.
  • Bicarbonate crystallites which are spheroidal in shape can be obtained by subjecting particulate bicarbonate to an air-jet pulverizing treatment, in which two air-jets containing entrained bicarbonate particles are impinged at high velocity. The resultant pulverized bicarbonate is recycled until the desired crystallite size distribution is obtained.
  • the pulverized bicarbonate product can be sized into fractions as suitable for end-use purposes.
  • the presence of at least two crystallites of bicarbonate salt in each hydrophilic polymer- coated core matrix is attributable to the micro-size of the crystallites.
  • Some of the microcrystallites aggregate to form crystallite agglomerates containing between about 2-10 primary crystallites. Coating of the agglomerates yield particles which contain between about 2-10 bicarbonate crystallites in the core matrix of hydrophilic polymer-coated particles.
  • Similar coated particles are obtained when during a coating procedure with a hydrophilic polymer solution two or more single bicarbonate crystallites, with a liquid surface coating of hydrophilic polymer solution, make contact and coelesce into coated particles containing two or more bicarbonate crystallites in the core matrix.
  • the application of the hydrophilic polymer coating to the core matrix particles is accomplished by conventional means such as pan coating, fluidized coating, centrifugal fluidized coating, and the like.
  • the coating polymer usually is dissolved in a suitable solvent such as water, methanol, ethanol, acetone, tetrahydrofuran, ethyl acetate, dimethylformamide, and the like, as appropriate for a selected polymer species.
  • a coating polymer also can be applied in the form of an emulsion or suspension. After the coating medium is applied to the particles, the solvent medium is removed by evaporation, thereby forming a continuous film coating which encapsulates the bicarbonate crystallites as demonstrated in Example I.
  • Another method of invention powder composition preparation is by slow addition of an aqueous solution of bicarbonate salt to a water- miscible organic solvent solution of a hydrophilic polymer, to form a suspension of precipitated bicarbonate microcrystallites in the organic solvent medium. Removal of the solvent medium yields hydrophilic polymer-coated bicarbonate salt microcrystallites as demonstrated in Example III.
  • the solvent component of the suspension admixture is partially removed, and the remaining concentrated suspension admixture is blended as a deodorant ingredient with organic ingredients in the formulation of a cosmetic stick or roll-on personal care product.
  • the blending of the diverse miscibility phases serves to disperse the deodorant ingredient in the form of hydrophilic polymer-coated bicarbonate microcrystallites in accordance with the present invention.
  • the coating thickness on the particle surfaces typically will vary in the range between about 0.1-20 microns.
  • the coating can consist of a single layer or multiple layers.
  • the polymeric coating can constitute between about 5-50 weight percent of the total dry weight of the coated particles.
  • the hydrophilic polymer employed for coating the ingredient particles is selected from water-soluble and water-dispersible organic polymers. A mixture of polymers can be employed, and a content of between about 0.5-40 weight percent of a water-insoluble polymer, based on the coating weight, can be included.
  • hydrophilic refers to an organic polymer which has a water- solubility of at least about one gram per 100 grams of water at 25°C.
  • Suitable hydrophilic polymers for coating particles include gum arabic, gum karaya, gum tragacanth, guar gum, locust bean gum, xanthan gum, carrageenan, alginate salt, casein, dextran, pectin, agar, sorbitol, 2-hydroxyethyl starch, 2-aminoethyl starch, maltodextrin, amylodextrin, 2-hydroxyethyl cellulose, methyl cellulose, carboxymethyl cellulose salt, cellulose sulfate salt, polyvinylpyrrolidone, polyethylene glycol, polypropylene glycol, polyethylene oxide, polyvinyl alcohol/acetate, polyacrylamide, and the like.
  • Polyvinyl acetate is illustrative of a water- insoluble polymer which can be included as an additional coating component to moderate the hydrophilicity of the coating.
  • the rate of particle matrix bicarbonate release from the particle core under moisture conditions can be controlled by the quantity and type of hydrophilic polymer coating on the particle surfaces.
  • Low molecular weight hydrophilic polymers will release the particle matrix compound at a relatively fast rate in the presence of moisture.
  • High molecular weight polymers which are less hydrophilic will release at a relatively slow rate. Additional rate control is obtained by employing mixtures of polymer components of varied hydrophilicity.
  • Polyethylene glycol (M.W. of 4000) or polyvinyl alcohol will release particle matrix compound at a relatively fast rate.
  • Polyethylene oxide (M.W. of 4,000,000) or partially hydrolyzed polyvinyl acetate will release at a relatively slow rate.
  • Polyvinylpyrrolidone will release particle matrix compound at an immediate rate when in contact with underarm type of moisture.
  • a powder composition of the present invention includes a content of anti- caking ingredient, in a sufficient quantity to provide and maintain free-flow properties in the powder composition.
  • Suitable anti-caking agents include magnesium silicate, zinc silicate, calcium silicate, sodium aluminosilicate, silica aerogel, silica xerogel, bentonite, attapulgite clay, zinc stearate, magnesium palmitate, sodium phthalate, zinc sulfide, magnesium phosphate, zirconium oxychloride, and the like.
  • the present invention also contemplates the provision of a cosmetic powder such as a baby powder formulation.
  • a cosmetic powder such as a baby powder formulation.
  • Illustrative of a novel baby powder product is a formulation which comprises a blend of (1) a hydrophilic polymer-coated bicarbonate crystallite ingredient as described hereinabove, and (2) between about 5-70 weight percent of cosmetic grade talc.
  • this invention provides a powder composition which comprises a blend of (1) a hydrophilic polymer-coated bicarbonate crystallite ingredient, and
  • a biocidal ingredient such as 2,4,4'-trichloro-2'- hydroxydiphenyl ether (Triclosan) .
  • a preferred biocidal ingredient is zinc oxide having an average particle size less than about one micron.
  • the relative densities of liquid and solid phases in a cosmetic stick or roll-on product directly affects the stability and esthetics of the formulations. Density matching of inorganic and organic phases is a significant factor in cosmetic stick and roll-on products.
  • the present invention provides a hydrophilic polymer-coated bicarbonate deodorant ingredient of lower density which more closely matches the density of the organic matrix of a cosmetic stick or roll-on product than does uncoated bicarbonate ingredient.
  • a cosmetic stick or roll-on product has improved dimensional stability, and better esthetic appearance and "feel" when applied to human skin.
  • An antiperspirant-deodorant cosmetic stick or roll-on product in accordance with the present invention has exceptional properties for treating or preventing perspiration and malodor associated with human underarm perspiration.
  • a present invention cosmetic stick or roll-on product can be applied effectively with safety and comfort for reduction of underarm perspiration and offensive odors.
  • EXAMPLE I This Example illustrates a fluidized bed procedure for coating a particulate bicarbonate compound with a hydrophilic polymer in accordance with the present invention.
  • a fluidized bed vessel is utilized which is equipped with a Wurster air-suspension coater system (WARF) as described in U.S. 4,568,559 and U.S. 4,877,621.
  • a coating solution is prepared by dissolving polyethylene glycol (45 g, Poly-G 2000, Olin Corp.), and propylene glycol butyl ether (10 g, PPG 14, Americol) in ethanol (500 g)/water (75 g).
  • Sodium bicarbonate is utilized as the core matrix particles.
  • the sodium bicarbonate (Particle Size Technology, Inc.) has an average particle size of about 5 microns, and 90 percent of the particles have a diameter less than 20 microns.
  • the sodium bicarbonate powder is charged into the coating chamber of the coater system.
  • Compressed air is introduced into the coating chamber, and the polymeric coating solution is sprayed on the air-suspended bicarbonate core matrix particles, until the coating weight is about 30% of the total dry weight of the coated particles.
  • the procedure is repeated, except that Hydroxypropylmethylcellulose (Methocel 60 HG, Dow Chemical Co.) is employed as the hydrophilic polymer.
  • the procedure is repeated, except that multiodextrin (Lodex 10; Durkee Foods) or amylodextrin is employed as the water-soluble polymer, and 0.5 g of a surfactant is included in the solution (polyoxyethylenesorbitan monolaurate; Tween 20; ICI Americas, Inc.)
  • the coated particles consist of a hydrophilic polymer coating on an inner core of 2-10 crystallites of sodium bicarbonate.
  • the coated particles have an average particle size of about 35 microns.
  • EXAMPLE II This Example illustrates a procedure for the preparation of an antiperspirant-deodorant cosmetic stick product in accordance with the present invention.
  • a stainless steel tank is provided which is equipped with turbine agitation.
  • Silicone oil DC 245 400 lbs, Dow Corning
  • Dow DC 200 37.50 lbs, Dow Corning
  • Agitation 55-65 RPM
  • heating the liquid medium to 176°F is commenced.
  • the mixture is stirred at 176°F for about 30 minutes until the ingredients are melted and the liquid medium is homogeneous.
  • the stirring speed is reduced to about 35 RPM, then Cyprus Supra A Talc 1625 (18.75 lbs, Cyprus) and Reach AZP 908 aluminum- zirconium tetrachlorohydrex glycine (312.50 lbs, Reheis) are added.
  • the temperature is maintained at 176°F for about 40 minutes until the fluid medium is uniform, and then the temperature is lowered to 154°F.
  • Polymer-coated sodium bicarbonate (140 lbs.) and Sobica F41 fragrance (6.25 lbs, Takasago) respectively are added with stirring to Silicone oil DC 245 (200 lbs, Dow Corning) in a second mixing tank at a temperature of 154°F to form a homogeneous suspension medium.
  • the sodium bicarbonate particles are pre-coated with amylodextrin as described in Example I.
  • the contents of the two mixing tanks which contain heated fluid medium are transferred to separate fill tanks through a Greer mill, and the fill tanks are connected to a mixing and dispensing nozzle device, of the type described in U.S. 5,094,276.
  • the nozzle device is adapted for homogeneously blending the two separate streams of fluid media, and dispensing a predetermined quantity of the blended fluid.
  • Plastek 2 oz. bottom-fill stick containers are filled with the blended fluid.
  • the container contents are cooled to a room temperature solid stick over a period of about 45 minutes.
  • the average hardness value of the solid sticks is 7 (ASTM Method D5) .
  • EXAMPLE III This Example illustrates a precipitation procedure for forming microcrystallites of potassium bicarbonate, and coating the microcrystallites with a hydrophilic polymer in accordance with the present invention.
  • a coating solution is prepared by dissolving polyethylene glycol (10 g, Poly-G 2000, Olin Corp.), propylene glycol butyl ether (5 g, PPG 14, Americol) , and polyoxyethylenesorbitan monqlaurate (l.o g; Tween 20; ICI Americas, Inc.) in 1-propanol (300 g) .
  • a solution of potassium bicarbonate (30 g) in water (100 g) is prepared.
  • the potassium bicarbonate solution is added dropwise to the coating solution with high speed stirring.
  • the admixture which forms is a suspension of potassium bicarbonate microcrystallites in the liquid medium.
  • the liquid medium is concentrated to dryness by removal of water/1-propanol azeotrope under vacuum at 60°C in a rotating evaporator.
  • the resultant dry powder is composed of particles which consist of a 33% by weight coating on an inner core of 2-10 microcrystallites of potassium bicarbonate.
  • the microcrystallites have a particle size distribution substantially in the range of 0.1-5 microns.
  • the potassium bicarbonate suspension admixture is concentrated until all of the water is removed azeotropically.
  • the remaining liquid concentrate is utilized as a deodorant ingredient in a cosmetic stick or roll-on formulation.
  • the blending of the liquid concentrate with the other formulation ingredients disperses the deodorant ingredient in the form of hydrophilic polymer-coated potassium bicarbonate particles, which are similar to the encapsulated bicarbonate crystallites described in Example I.
  • EXAMPLE IV This Example illustrates the preparation of an antiperspirant-deodorant roll-on product in accordance with the present invention.
  • a roll-on formulation is prepared by blending the following proportions of ingredients:
  • the roll-on formulation exhibits excellent dimensional stability when packaged and maintained under storage conditions for six months.

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Cosmetics (AREA)

Abstract

Cette invention concerne une composition pulvérulente de particules qui sont constituées d'un revêtement en un polymère hydrophile et d'une matrice centrale encapsulée contenant au moins deux microcristallites d'un composé minéral hydrosoluble tel que le bicarbonate de sodium. Une forme d'exécution d'une composition de poudre de la présente invention contient des microcristallites de bicarbonate avec un revêtement de polymère hydrophile et un agent antiadhésif acceptable sur le plan cosmétique tel que le talc. Cette composition est utile comme poudre pour bébé.
PCT/US1994/001193 1993-04-27 1994-02-08 Microcristallites de l'ingredient bicarbonate portant un revetement de polymere hydrophile WO1994024994A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU65485/94A AU6548594A (en) 1993-04-27 1994-02-08 Hydrophilic polymer-coated microcrystallites of bicarbonate ingredient
CA002144660A CA2144660C (fr) 1993-04-27 1994-02-08 Microcristaux hydrophiles d'un ingredient a base de bicarbonate avec revetement polymerique hydrophile

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US5383493A 1993-04-27 1993-04-27
US053,0834 1993-04-27

Publications (1)

Publication Number Publication Date
WO1994024994A1 true WO1994024994A1 (fr) 1994-11-10

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PCT/US1994/001193 WO1994024994A1 (fr) 1993-04-27 1994-02-08 Microcristallites de l'ingredient bicarbonate portant un revetement de polymere hydrophile

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AU (1) AU6548594A (fr)
CA (1) CA2144660C (fr)
WO (1) WO1994024994A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2737134A1 (fr) * 1995-07-27 1997-01-31 Bionatec Sarl Procede de fabrication de granules et granules ainsi obtenus
WO2001083603A1 (fr) * 2000-05-04 2001-11-08 Elementis Uk Ltd Agent biostatique
WO2002034189A3 (fr) * 2000-10-25 2002-06-20 Kimberly Clark Co Article pour l'apprentissage de la proprete contenant un agent effervescent
US7002055B2 (en) 2004-04-13 2006-02-21 Kimberly-Clark Worldwide, Inc. Toilet training article containing a foaming agent
GB2452118A (en) * 2007-06-26 2009-02-25 Nano4M Ltd Powder and its method of manufacture
WO2010072637A1 (fr) * 2008-12-23 2010-07-01 Basf Se Cristaux mixtes, leur procédé de fabrication et leur utilisation dans la production de produits de boulangerie-pâtisserie

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2837088A1 (de) * 1977-08-26 1979-03-08 Unilever Nv Antitranspirant-mittel

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2837088A1 (de) * 1977-08-26 1979-03-08 Unilever Nv Antitranspirant-mittel

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2737134A1 (fr) * 1995-07-27 1997-01-31 Bionatec Sarl Procede de fabrication de granules et granules ainsi obtenus
WO1997004861A1 (fr) * 1995-07-27 1997-02-13 Bionatec (S.A.R.L.) Procede de fabrication de granules et granules ainsi obtenues
US5965165A (en) * 1995-07-27 1999-10-12 Bionatec Process for the production of granules, and granules thus obtained
WO2001083603A1 (fr) * 2000-05-04 2001-11-08 Elementis Uk Ltd Agent biostatique
WO2002034189A3 (fr) * 2000-10-25 2002-06-20 Kimberly Clark Co Article pour l'apprentissage de la proprete contenant un agent effervescent
US6576810B1 (en) 2000-10-25 2003-06-10 Kimberly-Clark Worldwide, Inc. Toilet training article containing an effervescent agent
US7705194B2 (en) 2000-10-25 2010-04-27 Kimberly-Clark Worldwide, Inc. Article for assisting in toilet training
US7002055B2 (en) 2004-04-13 2006-02-21 Kimberly-Clark Worldwide, Inc. Toilet training article containing a foaming agent
GB2452118B (en) * 2007-06-26 2010-04-14 Nano4M Ltd A pharmaceutical compact and its method of manufacture
GB2452118A (en) * 2007-06-26 2009-02-25 Nano4M Ltd Powder and its method of manufacture
GB2465115A (en) * 2007-06-26 2010-05-12 Nano4M Ltd Powder and its method of manufacture
GB2465115B (en) * 2007-06-26 2011-08-24 Nano4M Ltd A novel powder and its method of manufacture
US9889097B2 (en) 2007-06-26 2018-02-13 Nano4M Limited Powder and its method of manufacture
WO2010072637A1 (fr) * 2008-12-23 2010-07-01 Basf Se Cristaux mixtes, leur procédé de fabrication et leur utilisation dans la production de produits de boulangerie-pâtisserie
EP2204095A1 (fr) 2008-12-23 2010-07-07 Basf Se Cristaux mélangés, leur procédé de fabrication et d'utilisation dans la fabrication de produits cuits
US9894905B2 (en) 2008-12-23 2018-02-20 Basf Se Mixed crystals, method for the production thereof and use thereof in the production of baked goods
US10609931B2 (en) 2008-12-23 2020-04-07 Basf Se Mixed crystals, method for the production thereof and use thereof in the production of baked goods

Also Published As

Publication number Publication date
AU6548594A (en) 1994-11-21
CA2144660A1 (fr) 1994-11-10
CA2144660C (fr) 2001-05-29

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