WO2007089337A2 - Cosmetic beads and method of making same - Google Patents

Cosmetic beads and method of making same Download PDF

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Publication number
WO2007089337A2
WO2007089337A2 PCT/US2006/047773 US2006047773W WO2007089337A2 WO 2007089337 A2 WO2007089337 A2 WO 2007089337A2 US 2006047773 W US2006047773 W US 2006047773W WO 2007089337 A2 WO2007089337 A2 WO 2007089337A2
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WO
WIPO (PCT)
Prior art keywords
acid
cosmetic
organic acid
ingredient
bead
Prior art date
Application number
PCT/US2006/047773
Other languages
French (fr)
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WO2007089337A3 (en
Inventor
Walter J. Carmody
Luciana Treubig
Original Assignee
Avon Products, 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 Avon Products, Inc. filed Critical Avon Products, Inc.
Publication of WO2007089337A2 publication Critical patent/WO2007089337A2/en
Publication of WO2007089337A3 publication Critical patent/WO2007089337A3/en

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Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11Encapsulated compositions
    • 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
    • A61K8/31Hydrocarbons
    • 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
    • A61K8/34Alcohols
    • A61K8/342Alcohols having more than seven atoms in an unbroken chain
    • 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
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/361Carboxylic acids having more than seven carbon atoms in an unbroken chain; Salts or anhydrides 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
    • A61K2800/40Chemical, 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

Definitions

  • the present invention relates to cosmetic bead compositions, wherein a wide variety of lipophilic, active, functional, and cosmetic ingredients can be entrapped or encapsulated into spherical beads. More particularly, the present invention relates to methods for forming small, stable, substantially uniform cosmetic beads by adding a metal-donating basic material to an oil phase containing an organic acid, in an aqueous suspension.
  • Encapsulation techniques employed for cosmetic materials are usually divided into two techniques. In conventional encapsulation, the active material content is surrounded with an outer film or coating. In the second type of encapsulation, matrix encapsulation, the active materials are mingled with the film or coating materials. Encapsulation techniques make it possible to insulate the active materials that may, for example, have poor compatibility with the cosmetic base, within the film materials, so that their stability in. the cosmetics can be improved. Further, it is desirable that the encapsulated active materials be protected from any unfavorable outside factors, so they can better maintain their physical and chemical properties until they are applied to the skin. There is also greater ease in handling liquid active materials by encapsulating them. Additionally, encapsulation can also regulate the particle size or amount of the active ingredient, as well as the release speed of the capsule contents.
  • Encapsulation methods employed in the cosmetic art generally limit the kind of ingredients that can be encapsulated, either by the chemical or physical nature of the encapsulating or encapsulated ingredients. Furthermore, many encapsulating methods are expensive and/or time consuming. It would be desirable to have cosmetic beads and cosmetic encapsulation techniques that allow for a wide variety of ingredients to be quickly, easily, and inexpensively encapsulated in a chemical reaction. It would be further desirable that the beads or capsules impart a feeling to the touch that is as agreeable as possible.
  • a cosmetic bead having a shell that has an insoluble soap of an organic acid and a lipophilic ingredient encapsulated within the shell.
  • the lipophilic ingredient may further include ingredients capable of being combined with the lipophilic ingredient.
  • the organic acid has a carbon chain of C8-C30.
  • a preferred organic acid is stearic acid.
  • the shell is formed by reacting a functional carboxyl acid group, especially such group contained in a fatty acid of 8 to 30 carbons, with an inorganic basic material, such that the resulting soap is insoluble in water.
  • a method of making cosmetic beads includes reacting an organic acid in an oil-in-water suspension with a metal-donating inorganic basic material.
  • an encapsulation method comprises hydrating a functional suspending aid in water to form an aqueous phase; separately combining a lipophilic ingredient and an organic acid to form a lipophilic phase; combining the lipophilic phase and the aqueous phase with mixing to produce a uniform suspension; and adding a metal donating inorganic basic material to the uniform suspension to cause soap formation, whereby the cosmetic beads are formed having a water insoluble organic acid soap shell and a lipophilic ingredient core (or encapsulant) .
  • the uniform suspension may be incorporated directly into a cosmetic preparation, although more typically the resulting beads contained in the uniform suspension are separated from the aqueous phase prior to use.
  • the cosmetic beads are concentrated in the uniform suspension by removing water prior to use.
  • the aqueous phase and the lipophilic phase are both heated, if necessary, to ensure that their components are maintained in the liquid state, even following formation of the uniform suspension. After formation of the beads, the composition is cooled to return it to ambient temperature.
  • the lipophilic ingredients include one or more ingredients having a functional carboxylic acid group.
  • lipophilic materials or ingredients known in the cosmetic art can be entrapped or encapsulated into the spherical cosmetic beads of the present invention.
  • the ingredients encapsulated in the cosmetic beads of the invention are lipophilic ingredients, and may include ingredients that are capable of being combined with the lipophilic ingredients.
  • lipophilic ingredients include oils, waxes, and/or fluids, all of which may be are encapsulated by beads made in accordance with the methods herein disclosed.
  • lipophilic oils, waxes, and/or fluids examples include but are not limited to fragrances, emollients, sunscreens, insect repellents, vitamins, vitamin derivates, skin protectants, antimicrobial agents, warming agents, cooling agents, hair minimizing agents, botanicals, skin lightening ingredients, OTC drug actives, or any combinations thereof.
  • the cosmetic beads may also contain particulate materials that are incorporated into the lipophilic ingredient, for example pigments, abrasives, soft focus materials, pearlescents, fillers, and the like.
  • the cosmetic beads can be formulated to be hard in order to help control the release of the encapsulated ingredient or to provide a mechanical exfoliating effect.
  • the cosmetic beads can be formulated to be soft so as to add a tactile or visual appeal to the cosmetic product in which the bead is incorporated, as well as for easier blending into the skin.
  • the cosmetic beads can be used for cosmetic appeal or to control the release of an encapsulated ingredient.
  • the hardness of the cosmetic beads is to some degree a subjective tactile evaluation, the practitioner of skill in cosmetic science and skilled in the art of product evaluation can gauge processing parameters during manufacture to obtain beads of a desired hardness.
  • the hardness of a particular bead may also be modified by the choice of lipophilic material encapsulated in the bead or the melting point of the organic acid used to form the shell of -the bead. For example, a hard wax would be used as the lipophilic ingredient when a hard bead is desired.
  • the beads can be evaluated in the following manner: Subjectively determine the amount of pressure needed to break a bead during simulated use, for example, when a given bead is placed between an evaluator's fingertips or between a fingertip and the inner forearm of the opposing arm, and then rubbed.
  • Very soft beads almost no pressure is needed to break the beads. The beads break rapidly and liquefy instantly spreading out over the evaluator's skin.
  • Hard beads Considerable pressure is needed to break the beads. The beads break very slowly, taking several minutes to fully break down. With repeated rubbing the beads break down, but can leave a rough texture on the evaluators skin.
  • Very hard beads Very hard pressure is needed to break the beads. Under normal pressure the beads will not break but remain intact and are considerably rough to the skin.
  • lipophilic ingredients The following are non-limiting examples of lipophilic ingredients :
  • the cosmetic bead compositions of the present invention are prepared by hydrating a functional suspending aid in water to form an aqueous phase; separately combining a lipophilic ingredient and an organic acid to form a lipophilic phase,- combining the lipophilic phase and the aqueous phase with mixing to produce a uniform suspension; and adding a metal donating inorganic basic material to the uniform suspension to cause soap formation, whereby the cosmetic beads are formed having a water insoluble organic acid soap shell and a lipophilic ingredient core (or encapsulant) .
  • the uniform suspension may be incorporated directly into a cosmetic preparation, although more typically, the resulting beads contained in the uniform suspension are separated from the aqueous phase prior to use .
  • the cosmetic beads are concentrated in the uniform suspension by removing water prior to use.
  • the cosmetic beads are removed from the aqueous phase and dried.
  • the beads can be incorporated into a variety of different product types, for example emulsions, sticks, creams, lotions, gels, and the like. Because the cosmetic beads are lighter than water, they can be easily removed from the aqueous phase by known techniques, for example, by simply skimming the beads from the top of the mixing vessel in which they are made, but also by filtering, and other known methods.
  • the aqueous phase and the lipophilic phase are both heated, if necessary, to ensure that their components are maintained in the liquid state, even following formation of the uniform suspension. After formation of the beads, the composition is cooled to return it to ambient temperature.
  • the lipophilic ingredients include one or more ingredients having a functional carboxylic acid group.
  • a suspending aid is used to maintain the oil phase in suspension when it is combined with the aqueous phase.
  • Any suspending aid that is useful in maintaining an oil phase suspended in an aqueous phase and without allowing the oil phase to agglomerate is suitable, so long as it is otherwise compatible with and does not destabilize the lipophilic phase, in particular the organic acid component.
  • the suspending aid should not interfere with the formation of the soap shell, that is, be incompatible with the inorganic base material .
  • the suspending agent is a nonsurfactant suspending agent, that is, should not possess surface active or tensid properties.
  • the functional suspending aid is a hydrocolloid gum.
  • gums examples include but are not limited to guar gum, cellulose and its derivatives, such as hydroxyethyl cellulose and hydroxypropyl cellulose, gum Arabic, gellan gum, xanthan gum, sclerotium gum, or any combinations thereof.
  • Other useful nonsurfactant suspending aids include pectin, agar, alginates, starches, and combinations thereof. See e.g., CTFA, International Cosmetic Ingredient Dictionary and Handbook, v. 4, Section 3, p.2835-6 (Ninth Edition 2002) .
  • the lipophilic phase is added to the aqueous phase and the phases are mixed to produce a uniform suspension.
  • the metal donating inorganic basic material is added to the uniform suspension to cause soap formation.
  • inorganic basic materials include but are not limited to calcium carbonate, magnesium carbonate, aluminum hydroxide, calcium hydroxide, magnesium hydroxide, or any combinations thereof. Soap is insoluble in water and is typically formed from alkaline earth metal salts, although other salts may be useful as well, such as aluminum hydroxide and manganese salts.
  • the resulting beads are then separated from the aqueous phase. Ingredients that are capable of being added to the lipophilic phase may also be added.
  • the lipophilic phase is preferably heated to ensure that its components are melted (liquefied) .
  • the aqueous phase is also typically heated because it is combined with the lipophilic phase. Additionally, some of the gums that may be used work best at elevated temperatures.
  • the lipophilic phase is preferably added to the aqueous phase, but there may be any order of addition.
  • Preferred organic acids as defined within the scope of this disclosure can be defined as have the general structure H 3 C- (CH 2 ) n-COOH wherein the molecule can have from 8 - 30 carbons with 10 - 18 carbons preferred.
  • the organic acid is a fatty acid of from 8 to 30 carbons.
  • the organic acid is an organic acid having a carbon chain of C8-C30. More preferably, the organic acid is an organic acid having a carbon chain of C12-C20.
  • encapsulated cosmetic bead compositions are formed by reacting an organic acid with a metal ion-donating inorganic basic material, so that the resulting chemical reaction between the organic acid and the inorganic base results in an insoluble soap composition.
  • the organic acid is stearic acid.
  • the metal ion-donating inorganic basic material is calcium carbonate.
  • Cosmetic oils, fluids, and/or waxes, alone or in combination, are combined with the organic acid and heated from about room temperature, preferably from about 120° F to about 190° F, and most preferably from about 145 to about 180° F, until all are melted, and suspended in a heated aqueous system such that small, uniform micelles are formed.
  • the encapsulation occurs due to the designed orientation of the organic acid prior to and during the reaction with the metal ions in a basic environment.
  • the hydrophilic acid functional group (head) of the organic acid tends to orientate towards the outer, water phase with the carbon chain tail oriented into the oil droplet.
  • the inorganic basic material is added to the heated aqueous/oil phase where the metal ions rapidly react with the organic acid functional group resulting in a layer of insoluble soap on the outer surface or shell of the beads .
  • the shell may have a silicone molecule with a functional carboxyl acid group.
  • the shell is formed by reacting the functional carboxyl acid group with an inorganic basic material such that the resulting soap is insoluble in water.
  • the inorganic basic material is added to the oil in water suspension containing the organic acid, the resulting soap is insoluble in water, and results in small, uniform bead formation.
  • the insoluble soap is present at about 20 wt% to about 80 wt%, based on the total weight of the bead composition.
  • the insoluble soap is present at about 20 wt% to about 50 wt%, based on the total weight of the composition.
  • the encapsulated ingredient is present at about 20 wt% to about 80 wt%, preferably 50 to 80%, based on the total weight of the bead composition.
  • the hardness/softness texture of the cosmetic beads can be modified by the selection of the various constituents of the oil phase or by selection of the organic acid used in the formation of the encapsulated outer shell of the beads. Suspending aids such as guar gum or hydroxyethyl cellulose are needed to successfully suspend the lipophilic phase.
  • suspending aids such as anionic, cationic, or nonionic surface active agents have been found to be detrimental to the encapsulation process, and should be avoided in preparing the uniform suspension used in the manufacture of the cosmetic beads. More specifically, typical surfactant emulsifiers known in the cosmetic art such as Stearth-2 and/or Steareth-21 are detrimental to or prevent the encapsulation process.
  • the metal-donating basic materials must be so selected such that the resulting metal-organic acid reaction results in an insoluble product.
  • Metal -donating salts such as sodium chloride or sodium hydroxide result in a water-soluble soap and no encapsulating will occur.
  • the metal donating salts are alkaline earth metal salts, but may also be other salts that will form insoluble soaps, for example, aluminum salts, in particular aluminum hydroxide and aluminum carbonate .
  • the cosmetic beads are incorporated into a cosmetic product.
  • the cosmetic product thus has the cosmetic beads of the present invention and a S cosmetic vehicle preferably having at least one cosmetic functional ingredient.
  • Suitable cosmetic functional ingredients include fragrances, emollients, sunscreens, insect repellents, vitamins, vitamin derivates, skin protectants, antimicrobial agents, warming agents, cooling agents, hair 0 minimizing agents, botanicals, skin lightening ingredients, OTC drug actives, or any combinations thereof.
  • one functional cosmetic ingredient can be present in the bead and a second cosmetic functional ingredient can be present in the vehicle outside the bead. 5
  • Phase B Separately combine Phase B and, while mixing, heat to 120 to 160° F or until melted.
  • Phase A While mixing Phase A, slowly add phase B and mix until uniform. 4) Pretnix Phase C, as required, and then add Phase C to Phase A and B mixture. Mix for 5 to 20 minutes.
  • a medium soft bead is obtained.
  • a medium hard bead is obtained.

Abstract

There are provided cosmetic bead compositions having a shell with a water-insoluble soap of an organic acid, and lipophilic encapsulated ingredients. There are also provide methods for making cosmetic beads by reacting an organic acid and a lipophilic ingredient mixture in an oil in water suspension with a metal-donating inorganic basic material.

Description

COSHETXC BEADS AND METHOD OF MAKIlTG SAME
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to cosmetic bead compositions, wherein a wide variety of lipophilic, active, functional, and cosmetic ingredients can be entrapped or encapsulated into spherical beads. More particularly, the present invention relates to methods for forming small, stable, substantially uniform cosmetic beads by adding a metal-donating basic material to an oil phase containing an organic acid, in an aqueous suspension.
2. Description of the Related Art
The encapsulation or microencapsulation of cosmetic or dermatological active agents to allow for better storage and/or sustained and controlled release is known in the cosmetic art. Generally, most conventional encapsulation processes are based on the use of polymers as constituent elements of the wall of the miσroparticle that isolates the active agent from the external medium.
Encapsulation techniques employed for cosmetic materials are usually divided into two techniques. In conventional encapsulation, the active material content is surrounded with an outer film or coating. In the second type of encapsulation, matrix encapsulation, the active materials are mingled with the film or coating materials. Encapsulation techniques make it possible to insulate the active materials that may, for example, have poor compatibility with the cosmetic base, within the film materials, so that their stability in. the cosmetics can be improved. Further, it is desirable that the encapsulated active materials be protected from any unfavorable outside factors, so they can better maintain their physical and chemical properties until they are applied to the skin. There is also greater ease in handling liquid active materials by encapsulating them. Additionally, encapsulation can also regulate the particle size or amount of the active ingredient, as well as the release speed of the capsule contents.
With conventional encapsulation means, when the encapsulating film material is water-soluble and easily swollen in water, water in the cosmetic base may easily penetrate into the capsule, or the active ingredient in the capsule may be released. That is, the presence of an aqueous phase outside the capsules or microcapsules necessitates excellent impermeability of the wall of the capsules in order to prevent the active ingredient from passing into the outer aqueous phase, which would negate all the benefits of the encapsulation. Further, in the matrix encapsulation techniques, the active ingredient may be released through the capillaries of the capsule particle. Thus, in the cosmetic field, capsules and microcapsules with an impermeable wall, which release the active ingredient only after application, for example, following the rupture or biodegradation of the envelope, are generally sought.
Encapsulation methods employed in the cosmetic art generally limit the kind of ingredients that can be encapsulated, either by the chemical or physical nature of the encapsulating or encapsulated ingredients. Furthermore, many encapsulating methods are expensive and/or time consuming. It would be desirable to have cosmetic beads and cosmetic encapsulation techniques that allow for a wide variety of ingredients to be quickly, easily, and inexpensively encapsulated in a chemical reaction. It would be further desirable that the beads or capsules impart a feeling to the touch that is as agreeable as possible.
SUMIlARy OP THE INVENTION
It is an object of the present invention to provide a cosmetic bead composition wherein a wide variety of lipophilic, active, functional, and cosmetic ingredients can be entrapped or encapsulated into a spherical bead .
It is another object of the present invention to provide a method of encapsulation that allows for quick and easy, chemically induced encapsulation of a wide variety of ingredients .
According to these and other objects and advantages of the present invention, there is provided a cosmetic bead having a shell that has an insoluble soap of an organic acid and a lipophilic ingredient encapsulated within the shell. The lipophilic ingredient may further include ingredients capable of being combined with the lipophilic ingredient. Preferably, the organic acid has a carbon chain of C8-C30. A preferred organic acid is stearic acid. The shell is formed by reacting a functional carboxyl acid group, especially such group contained in a fatty acid of 8 to 30 carbons, with an inorganic basic material, such that the resulting soap is insoluble in water. In another aspect of the invention, a method of making cosmetic beads includes reacting an organic acid in an oil-in-water suspension with a metal-donating inorganic basic material.
Further according to this and other objects and advantages of the present invention, there is also provided an encapsulation method. The method comprises hydrating a functional suspending aid in water to form an aqueous phase; separately combining a lipophilic ingredient and an organic acid to form a lipophilic phase; combining the lipophilic phase and the aqueous phase with mixing to produce a uniform suspension; and adding a metal donating inorganic basic material to the uniform suspension to cause soap formation, whereby the cosmetic beads are formed having a water insoluble organic acid soap shell and a lipophilic ingredient core (or encapsulant) . The uniform suspension may be incorporated directly into a cosmetic preparation, although more typically the resulting beads contained in the uniform suspension are separated from the aqueous phase prior to use. In another aspect of the invention the cosmetic beads are concentrated in the uniform suspension by removing water prior to use.
The aqueous phase and the lipophilic phase are both heated, if necessary, to ensure that their components are maintained in the liquid state, even following formation of the uniform suspension. After formation of the beads, the composition is cooled to return it to ambient temperature. The lipophilic ingredients include one or more ingredients having a functional carboxylic acid group.
DETAILED DESCRIPTION OF THE INVENTION
It was surprisingly found that there could be a cosmetic bead composition wherein a wide variety of lipophilic, active, functional, and cosmetic ingredients can be entrapped or encapsulated into a spherical bead. It was further surprisingly found that the addition of a metal ion donating basic material can cause an oil solution containing an organic acid in an aqueous suspension, to rapidly react and form small, stable, uniform cosmetic beads.
A wide variety of lipophilic materials or ingredients known in the cosmetic art can be entrapped or encapsulated into the spherical cosmetic beads of the present invention. The ingredients encapsulated in the cosmetic beads of the invention are lipophilic ingredients, and may include ingredients that are capable of being combined with the lipophilic ingredients. Preferably, lipophilic ingredients include oils, waxes, and/or fluids, all of which may be are encapsulated by beads made in accordance with the methods herein disclosed. Examples of such lipophilic oils, waxes, and/or fluids that can be encapsulated into the cosmetic beads include but are not limited to fragrances, emollients, sunscreens, insect repellents, vitamins, vitamin derivates, skin protectants, antimicrobial agents, warming agents, cooling agents, hair minimizing agents, botanicals, skin lightening ingredients, OTC drug actives, or any combinations thereof. The cosmetic beads may also contain particulate materials that are incorporated into the lipophilic ingredient, for example pigments, abrasives, soft focus materials, pearlescents, fillers, and the like.
The cosmetic beads can be formulated to be hard in order to help control the release of the encapsulated ingredient or to provide a mechanical exfoliating effect. Alternatively, the cosmetic beads can be formulated to be soft so as to add a tactile or visual appeal to the cosmetic product in which the bead is incorporated, as well as for easier blending into the skin. The cosmetic beads can be used for cosmetic appeal or to control the release of an encapsulated ingredient.
While the hardness of the cosmetic beads is to some degree a subjective tactile evaluation, the practitioner of skill in cosmetic science and skilled in the art of product evaluation can gauge processing parameters during manufacture to obtain beads of a desired hardness. The hardness of a particular bead may also be modified by the choice of lipophilic material encapsulated in the bead or the melting point of the organic acid used to form the shell of -the bead. For example, a hard wax would be used as the lipophilic ingredient when a hard bead is desired.
Below is a subjective tactile scale useful in determining a bead's hardness, as well as the melting points of some typical waxes used as lipophilic ingredients.
The beads can be evaluated in the following manner: Subjectively determine the amount of pressure needed to break a bead during simulated use, for example, when a given bead is placed between an evaluator's fingertips or between a fingertip and the inner forearm of the opposing arm, and then rubbed.
Very soft beads: almost no pressure is needed to break the beads. The beads break rapidly and liquefy instantly spreading out over the evaluator's skin.
Medium soft beads: little pressure is needed to break the beads. The beads break quickly and within seconds liquefy easily spreading out over the evaluator's skin. Soft beads: Some pressure, over several seconds, is needed to break the beads . The beads break slowly and remain
Figure imgf000008_0001
intact for several seconds until smoothing out and being absorbed into the skin .
Medium hard beads: Considerable pressure, and up to one minute, is needed to fully break the beads. The beads break slowly and remain intact with noticeable roughness to the evaluator's skin. Over time and with pressure, the beads smooth out and are absorbed into the skin .
Hard beads: Considerable pressure is needed to break the beads. The beads break very slowly, taking several minutes to fully break down. With repeated rubbing the beads break down, but can leave a rough texture on the evaluators skin.
Very hard beads: Very hard pressure is needed to break the beads. Under normal pressure the beads will not break but remain intact and are considerably rough to the skin.
The following are non-limiting examples of lipophilic ingredients :
The cosmetic bead compositions of the present invention are prepared by hydrating a functional suspending aid in water to form an aqueous phase; separately combining a lipophilic ingredient and an organic acid to form a lipophilic phase,- combining the lipophilic phase and the aqueous phase with mixing to produce a uniform suspension; and adding a metal donating inorganic basic material to the uniform suspension to cause soap formation, whereby the cosmetic beads are formed having a water insoluble organic acid soap shell and a lipophilic ingredient core (or encapsulant) . The uniform suspension may be incorporated directly into a cosmetic preparation, although more typically, the resulting beads contained in the uniform suspension are separated from the aqueous phase prior to use . In another aspect of the invention, the cosmetic beads are concentrated in the uniform suspension by removing water prior to use. Preferably, the cosmetic beads are removed from the aqueous phase and dried. In this form the beads can be incorporated into a variety of different product types, for example emulsions, sticks, creams, lotions, gels, and the like. Because the cosmetic beads are lighter than water, they can be easily removed from the aqueous phase by known techniques, for example, by simply skimming the beads from the top of the mixing vessel in which they are made, but also by filtering, and other known methods.
The aqueous phase and the lipophilic phase are both heated, if necessary, to ensure that their components are maintained in the liquid state, even following formation of the uniform suspension. After formation of the beads, the composition is cooled to return it to ambient temperature. The lipophilic ingredients include one or more ingredients having a functional carboxylic acid group.
A suspending aid is used to maintain the oil phase in suspension when it is combined with the aqueous phase. Any suspending aid that is useful in maintaining an oil phase suspended in an aqueous phase and without allowing the oil phase to agglomerate is suitable, so long as it is otherwise compatible with and does not destabilize the lipophilic phase, in particular the organic acid component. Additionally, the suspending aid should not interfere with the formation of the soap shell, that is, be incompatible with the inorganic base material . The suspending agent is a nonsurfactant suspending agent, that is, should not possess surface active or tensid properties. Preferably, the functional suspending aid is a hydrocolloid gum. Examples of gums that may be used include but are not limited to guar gum, cellulose and its derivatives, such as hydroxyethyl cellulose and hydroxypropyl cellulose, gum Arabic, gellan gum, xanthan gum, sclerotium gum, or any combinations thereof. Other useful nonsurfactant suspending aids include pectin, agar, alginates, starches, and combinations thereof. See e.g., CTFA, International Cosmetic Ingredient Dictionary and Handbook, v. 4, Section 3, p.2835-6 (Ninth Edition 2002) .
Preferably, the lipophilic phase is added to the aqueous phase and the phases are mixed to produce a uniform suspension. The metal donating inorganic basic material is added to the uniform suspension to cause soap formation. Examples of inorganic basic materials that may be used include but are not limited to calcium carbonate, magnesium carbonate, aluminum hydroxide, calcium hydroxide, magnesium hydroxide, or any combinations thereof. Soap is insoluble in water and is typically formed from alkaline earth metal salts, although other salts may be useful as well, such as aluminum hydroxide and manganese salts. The resulting beads are then separated from the aqueous phase. Ingredients that are capable of being added to the lipophilic phase may also be added.
Although the beads may be formed at ambient temperature, the lipophilic phase is preferably heated to ensure that its components are melted (liquefied) . The aqueous phase is also typically heated because it is combined with the lipophilic phase. Additionally, some of the gums that may be used work best at elevated temperatures. The lipophilic phase is preferably added to the aqueous phase, but there may be any order of addition.
Preferred organic acids as defined within the scope of this disclosure can be defined as have the general structure H3C- (CH2) n-COOH wherein the molecule can have from 8 - 30 carbons with 10 - 18 carbons preferred. Preferably, the organic acid is a fatty acid of from 8 to 30 carbons. The following list gives examples within this disclosure and is not intended to limit the scope of applicable organic acids:
Scientific Nomenclature Common Name Number of Carbons
Octanoic Acid Caprylic Acid 8
Decanoic Acid Capric Acid 10
Tetradecanoic Acid Myristic Acid 14 Octadecanoic Acid Stearic Acid 18
Docosanoic Acid Behenic Acid 22
Preferably, the organic acid is an organic acid having a carbon chain of C8-C30. More preferably, the organic acid is an organic acid having a carbon chain of C12-C20.
In a preferred aspect of the present invention, encapsulated cosmetic bead compositions are formed by reacting an organic acid with a metal ion-donating inorganic basic material, so that the resulting chemical reaction between the organic acid and the inorganic base results in an insoluble soap composition. Preferably, the organic acid is stearic acid. Preferably, the metal ion-donating inorganic basic material is calcium carbonate. Cosmetic oils, fluids, and/or waxes, alone or in combination, are combined with the organic acid and heated from about room temperature, preferably from about 120° F to about 190° F, and most preferably from about 145 to about 180° F, until all are melted, and suspended in a heated aqueous system such that small, uniform micelles are formed.
The encapsulation occurs due to the designed orientation of the organic acid prior to and during the reaction with the metal ions in a basic environment. The hydrophilic acid functional group (head) of the organic acid tends to orientate towards the outer, water phase with the carbon chain tail oriented into the oil droplet. The inorganic basic material is added to the heated aqueous/oil phase where the metal ions rapidly react with the organic acid functional group resulting in a layer of insoluble soap on the outer surface or shell of the beads .
In a further aspect of the invention, the shell may have a silicone molecule with a functional carboxyl acid group. The shell is formed by reacting the functional carboxyl acid group with an inorganic basic material such that the resulting soap is insoluble in water. When the inorganic basic material is added to the oil in water suspension containing the organic acid, the resulting soap is insoluble in water, and results in small, uniform bead formation.
The insoluble soap is present at about 20 wt% to about 80 wt%, based on the total weight of the bead composition. Preferably, the insoluble soap is present at about 20 wt% to about 50 wt%, based on the total weight of the composition. The encapsulated ingredient is present at about 20 wt% to about 80 wt%, preferably 50 to 80%, based on the total weight of the bead composition. The hardness/softness texture of the cosmetic beads can be modified by the selection of the various constituents of the oil phase or by selection of the organic acid used in the formation of the encapsulated outer shell of the beads. Suspending aids such as guar gum or hydroxyethyl cellulose are needed to successfully suspend the lipophilic phase. These gums do not interfere with the encapsulation process. It has also been found that suspending aids such as anionic, cationic, or nonionic surface active agents have been found to be detrimental to the encapsulation process, and should be avoided in preparing the uniform suspension used in the manufacture of the cosmetic beads. More specifically, typical surfactant emulsifiers known in the cosmetic art such as Stearth-2 and/or Steareth-21 are detrimental to or prevent the encapsulation process. Additionally, it has been found that the metal-donating basic materials must be so selected such that the resulting metal-organic acid reaction results in an insoluble product. Metal -donating salts such as sodium chloride or sodium hydroxide result in a water-soluble soap and no encapsulating will occur. Typically, the metal donating salts are alkaline earth metal salts, but may also be other salts that will form insoluble soaps, for example, aluminum salts, in particular aluminum hydroxide and aluminum carbonate .
The following materials are non-limiting examples of basic compounds suitable to neutralize the organic acid:
Magnesium Carbonate MgCO3 Magnesium Hydroxide Mg(OH)2
Magnesium Amide Mg (NH2) 2
Calcium Carbonate CaCO3
Calcium Hydroxide Ca(OH)2
Calcium Amide Ca (NH2) 2 Aluminum Carbonate Al2 (CO3) 3
Aluminum Hydroxide Al (OH) 3
Aluminum Amide Al (NH2) 3 In another aspect of the invention the cosmetic beads are incorporated into a cosmetic product. The cosmetic product thus has the cosmetic beads of the present invention and a S cosmetic vehicle preferably having at least one cosmetic functional ingredient. Suitable cosmetic functional ingredients include fragrances, emollients, sunscreens, insect repellents, vitamins, vitamin derivates, skin protectants, antimicrobial agents, warming agents, cooling agents, hair 0 minimizing agents, botanicals, skin lightening ingredients, OTC drug actives, or any combinations thereof. Thus, one functional cosmetic ingredient can be present in the bead and a second cosmetic functional ingredient can be present in the vehicle outside the bead. 5
The following are examples of products of the present invention and are not to be construed as limiting. Unless otherwise indicated, all percentages and parts are by weight. Concentrations are on a 100 percent weight/weight basis. All 0 ingredients are "as is" unless otherwise noted.
The following formulations were prepared. The ingredients were as set forth in Examples 1 to 3 below. The methods to produce the Examples are commonly known to those 5 skilled in the art.
Procedure :
1) Combine Phase A and, while mixing, heat to 120 to 160° F 0 or to match the temperature of the lipophilic phase B.
2) Separately combine Phase B and, while mixing, heat to 120 to 160° F or until melted.
3) While mixing Phase A, slowly add phase B and mix until uniform. 4) Pretnix Phase C, as required, and then add Phase C to Phase A and B mixture. Mix for 5 to 20 minutes.
5) Separate beads from the water phase and dry.
EXAMPLE 1
Ingredients Coneentration
Phase A Demineralized Water 80.00% Guar HPT Chloride Gum 0.10%
Phase B Isopropyl Palmitate 9.40% Stearic Acid 9.40%
Phase C Calcium Hydroxide 1.10%
100.00%
A soft bead resulted.
EXAMPLE 2
Ingredients Concentration
Phase A
Demineralized Water 69 .50% Hydroxyethyl Cellulose 0. 10%
Phase B
Decaraethylcyclopentasiloxan Lee 20 .00% Stearic Acid 10 .00%
Phase C
Calcium Carbonate 0. 40%
100.00% A very soft bead was obtained. EXAMPLE 3
Ingredients Concentration
Phase A
Demineralized Water 65.14%
Guar HPT Chloride Gum 0.06%
Phase B
Isopropyl Palmitate 9.00%
Vanillyl Butyl Ether 0.05%
Myristyl Myristate 5.00%
Methylparaben 0.20%
Stearic Acid 10.00%
Pheπoxyethanol 0.30%
Phase C
Demineralized Water 10.00%
Magnesium Carbonate 0.25%
100.00%
A medium soft bead is obtained.
Example 4
Ingredients Concentration
Phase A
Demineralized Water 70.21%
Guar HPT Chloride Gum 0.06%
Phase B
Hydrogenated Castor Oil 1.00%
Stearic Acid 9.00%
Methylparaben 0.20%
Phenoxyethno1 0.30%
Cyclopentasiloxane 14.00%
Phase C
Demineralized Water 5.00%
Calcium Carbonate 0.23%
100.00%
A soft bead is obtained. Example 5
Ingredients Concentration
Phase A
Demineralized Water 70.15%
Guar HPT Chloride Gum 0.06%
Phase B
Vanillyl Butyl Ether 0.05%
Hydrogenated Castor Oil 5.00%
Stearic Acid 10.00%
Dimethicone 9.00%
Methylparaben 0.20%
Phenoxyethanol 0.30%
Phase C
Demineralized Water 5.00%
Magnesium Carbonate 0.24%
100.00%
A medium hard bead is obtained.
Example 6
Ingredients Concentration
Phase A Demineralized Water 66.79% Guar HPT Chloride Gum 0.06%
Phase B Vanillyl Butyl Ether 0.05% Hydrogenated Castor Oil 5.00% Stearic Acid 19.00% Petrolatum 3.00%
Methylparaben 0.20% Phenoxyethanol 0.30%
Phase C Demineralized Water 5.00% Aluminum Hydroxide 0.60%
100.00%
A hard bead is obtained. It should be understood that the foregoing description is only illustrative of the present invention. Various alternatives and modifications can be devised by those skilled in the art without departing from the invention. Accordingly, the present invention is intended to embrace all such alternatives, modifications and variances that fall within the scope of the appended claims.

Claims

WHAT IS CLAIMED IS
1. A cosmetic bead comprising:
a shell having an insoluble soap of an organic acid; and
a lipophilic ingredient encapsulated within the shell.
2. The cosmetic bead of claim 1, wherein said lipophilic ingredient is selected from the group consisting of oil, wax, fluid, and any combinations thereof.
3. The cosmetic bead of claim 2, wherein said lipophilic ingredient is selected from the group consisting of fragrance, emollient, sunscreen, insect repellent, vitamin, vitamin derivate, skin protectant, antimicrobial agent, warming agent, cooling agent, hair minimizing agent, botanical, skin lightening ingredient, OTC drug active, and any combinations thereof.
4. The cosmetic bead of claim 1, wherein the ingredient further comprises a functional ingredient capable of being combined with the lipophilic ingredient.
5. The cosmetic bead of claim 1, wherein said organic acid has a carbon chain of C8-C30.
6. The cosmetic bead of claim 1, wherein said organic acid has a carbon chain of C12-C20.
7. The cosmetic bead of claim 1, wherein said organic acid is a fatty acid of from 8 to 30 carbons.
8. The cosmetic bead of claim 7, wherein said organic acid is selected from the group consisting of caprylic acid, capric acid, myristic acid, stearic acid, behenic acid, and any combinations thereof.
9. The cosmetic bead of claim 8, wherein said organic acid is stearic acid.
10. The cosmetic bead of claim 1, wherein said shell further comprises a silicone molecule with a functional carboxyl acid group.
11. The cosmetic bead of claim I, wherein said shell is formed by reacting a functional carboxyl acid group with an inorganic basic material such that the resulting soap is insoluble in water.
12. The cosmetic bead of claim 11, wherein said inorganic basic material is an alkaline earth metal salt.
13. The cosmetic bead of claim 11, wherein said inorganic basic material is selected from the group consisting of calcium carbonate, magnesium carbonate, aluminum hydroxide, calcium hydroxide, magnesium hydroxide, magnesium amide, calcium amide, aluminum carbonate, aluminum amide, and any combinations thereof.
14. The cosmetic bead of claim 13, wherein said inorganic basic material is calcium carbonate.
15. The cosmetic bead of claim 1, wherein said insoluble soap is present at about 20 wt% to about 80 wt%, based on the total weight of the composition.
16. The cosmetic bead of claim 1, wherein said insoluble soap is present at about 20 wt% to about 50 wt%, based on the total weight of the composition.
17. The cosmetic bead of claim 1, wherein said ingredient is present at about 20 wt% to about 80 wt%, based on the total weight of the composition.
18. An encapsulation method comprising:
hydrating a functional suspending aid in water to form an aqueous phase,-
separately combining a lipophilic ingredient and an organic acid to form a lipophilic phase;
combining the lipophilic phase and the aqueous phase with mixing to produce a uniform suspension; and
adding a metal-donating inorganic basic material to the uniform suspension to cause soap formation.
19. The encapsulation method of claim 18, wherein said functional suspending aid is a gum.
20. The encapsulation method of claim 19, wherein said gum is selected from the group consisting of guar gum, cellulose and its derivatives, hydroxyethyl cellulose, hydroxypropyl cellulose, gum Arabic, gellan gum, xanthan gum, sclerotium gum, and any combinations thereof.
21. The encapsulation method of claim 18, wherein said organic acid has a carbon chain of C8-C30.
22. The encapsulation method of claim 18, wherein said organic acid has a carbon chain of C12-C20.
23. The encapsulation method of claim 18, wherein said organic acid is selected from the group consisting of caprylic acid, capric acid, myristic acid, stearic acid, behenic acid, and any combinations thereof.
24. The encapsulation method of claim 23, wherein said organic acid is stearic acid.
25. The encapsulation method of claim 18, wherein said inorganic basic material is an alkaline earth metal salt.
26. The encapsulation method of claim 18, wherein said inorganic basic material is selected from the group consisting of calcium carbonate, magnesium carbonate, aluminum hydroxide, calcium hydroxide, magnesium hydroxide, magnesium amide, calcium amide, aluminum carbonate, aluminum amide, and any combinations thereof.
27. A method of making cosmetic beads comprising:
forming an oil in water suspension wherein the oil phase comprises an organic acid, and
reacting the organic acid with a metal-donating inorganic basic material .
28. The method of claim 27, wherein said organic acid has a carbon chain of C8-C30.
29. The method of claim 27, wherein said organic acid has a carbon chain of C12-C20.
30. The method of claim 27, wherein said organic acid is selected from the group consisting of caprylic acid, capric acid, myristic acid, stearic acid, behenic acid, and any combinations thereof .
31. The method of claim 30, -wherein said organic acid is stearic acid.
32. The method of claim 27, wherein said inorganic basic material is an alkaline earth metal salt.
33. The method of claim 27, wherein said inorganic basic material is selected from the group consisting of calcium carbonate, magnesium carbonate, aluminum hydroxide, calcium hydroxide, magnesium hydroxide, magnesium amide, calcium, amide, aluminum carbonate, aluminum amide, and any combinations thereof .
34. The method of claim 27, further comprising combining an encapsulated ingredient with said organic acid to form a mixture .
35. The method of claim 34, wherein said encapsulated ingredient is selected from the group consisting of a lipophilic ingredient, an ingredient capable of being combined with a lipophilic ingredient, and any combinations thereof.
36. The method of claim 34, wherein said encapsulated ingredient is selected from the group consisting of fragrance, emollient, sunscreen, insect repellent, vitamin, vitamin derivate, skin protectant, antimicrobial agent, warming agent, cooling agent, hair minimizing agent, botanical, skin lightening ingredient, OTC drug active, and any combinations thereof .
37. The method of claim 34, further comprising heating said mixture from about 120° F to about 190° F.
38. A cosmetic composition comprising the cosmetic bead of claim 1, a cosmetically acceptable vehicle, and at least one cosmetic active present in the cosmetically acceptable vehicle.
PCT/US2006/047773 2005-12-30 2006-12-14 Cosmetic beads and method of making same WO2007089337A2 (en)

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Publication number Priority date Publication date Assignee Title
WO2011082032A1 (en) * 2009-12-30 2011-07-07 Avon Products, Inc. Cosmetic powder bead compositions
US10822442B2 (en) 2017-07-17 2020-11-03 Ecolab Usa Inc. Rheology-modifying agents for slurries
CN113712824A (en) * 2021-09-27 2021-11-30 苏州睿粼材料科技有限公司 Soft bead body for cosmetics and preparation method thereof

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US5268180A (en) * 1990-11-09 1993-12-07 L'oreal Cosmetic pharmaceutical or foodstuff composition comprising an aqueous dispersion of lipidic vesicles
US20040224012A1 (en) * 2001-10-05 2004-11-11 Pichit Suvanprakorn Topical application and methods for administration of active agents using liposome macro-beads
US20050069704A1 (en) * 2003-09-25 2005-03-31 Thomas Rathschlag Encapsulated pigments

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US5268180A (en) * 1990-11-09 1993-12-07 L'oreal Cosmetic pharmaceutical or foodstuff composition comprising an aqueous dispersion of lipidic vesicles
US20040224012A1 (en) * 2001-10-05 2004-11-11 Pichit Suvanprakorn Topical application and methods for administration of active agents using liposome macro-beads
US20050069704A1 (en) * 2003-09-25 2005-03-31 Thomas Rathschlag Encapsulated pigments

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011082032A1 (en) * 2009-12-30 2011-07-07 Avon Products, Inc. Cosmetic powder bead compositions
US8658187B2 (en) 2009-12-30 2014-02-25 Avon Products Inc. Cosmetic powder bead compositions
US10822442B2 (en) 2017-07-17 2020-11-03 Ecolab Usa Inc. Rheology-modifying agents for slurries
CN113712824A (en) * 2021-09-27 2021-11-30 苏州睿粼材料科技有限公司 Soft bead body for cosmetics and preparation method thereof

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