WO2023063116A1 - Water-in-oil emulsified cosmetic - Google Patents

Water-in-oil emulsified cosmetic Download PDF

Info

Publication number
WO2023063116A1
WO2023063116A1 PCT/JP2022/036741 JP2022036741W WO2023063116A1 WO 2023063116 A1 WO2023063116 A1 WO 2023063116A1 JP 2022036741 W JP2022036741 W JP 2022036741W WO 2023063116 A1 WO2023063116 A1 WO 2023063116A1
Authority
WO
WIPO (PCT)
Prior art keywords
oil
water
emulsified cosmetic
silicone
pigment
Prior art date
Application number
PCT/JP2022/036741
Other languages
French (fr)
Japanese (ja)
Inventor
喜郎 貞神
大輝 隈部
耕太郎 ▲高▼田
隆志 福原
Original Assignee
株式会社 資生堂
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 株式会社 資生堂 filed Critical 株式会社 資生堂
Publication of WO2023063116A1 publication Critical patent/WO2023063116A1/en

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
    • A61K8/04—Dispersions; Emulsions
    • A61K8/06—Emulsions
    • 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
    • A61K8/29—Titanium; Compounds thereof
    • 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
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • 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
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A61K8/894—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by a polyoxyalkylene group, e.g. cetyl dimethicone copolyol
    • 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

Definitions

  • the present invention relates to a water-in-oil emulsified cosmetic. More specifically, it relates to a water-in-oil emulsified cosmetic that is excellent in spreadability during application, uniform finish of makeup, and excellent emulsification stability.
  • a water-in-oil emulsified composition having an oil phase as an outer phase and an aqueous phase as an inner phase can efficiently spread oil-soluble active ingredients such as emollient oils, drugs, ultraviolet absorbers, etc. on the skin. It has a suitable dosage form and is widely used in make-up cosmetics such as foundation.
  • Makeup cosmetics such as foundations use white pigments such as zinc oxide and titanium oxide, and colored pigments such as iron oxide, which have the effect of correcting skin unevenness such as spots and freckles and skin unevenness such as pores. ing. In order to obtain a high corrective effect, etc., it is required that these pigments are highly blended in cosmetics.
  • the external oil phase contains solid oil such as wax, semi-solid oil, or macromolecules such as coating agents, these aggregates and the powder cause agglomeration, resulting in slow spreadability during application. As a result, the problem of non-uniform finish of makeup tends to occur.
  • Patent Document 2 discloses that an outer oil phase is thickened with (A) wax and (B) disteardimonium hectorite or It is suggested to solidify.
  • A wax and (B) disteardimonium hectorite or It is suggested to solidify.
  • non-hydrophobized powders tend to cause creaking over time after being applied to the skin.
  • the present invention has been made in view of the above-mentioned circumstances, and by stably dispersing a hydrophobized pigment in the internal water phase, the spreadability during application and the uniformity of the makeup finish are excellent, and the emulsion is emulsified. To provide a water-in-oil emulsified cosmetic excellent in stability.
  • the inventors of the present invention conducted intensive research to solve the above problems, and as a result, prepared an aqueous dispersion in which a hydrophobized pigment was dispersed in an aqueous component using a nonionic surfactant having a predetermined HLB.
  • a hydrophobized pigment was dispersed in an aqueous component using a nonionic surfactant having a predetermined HLB.
  • the hydrophobized pigment is stably dispersed inside the emulsified particles, i.e., in the internal water phase.
  • the inventors found that the spreadability during application, the uniformity of the makeup finish, and the emulsification stability were remarkably improved, leading to the completion of the present invention.
  • the present invention (A) a nonionic surfactant with an HLB of 9 or more; (B) a hydrophobized pigment, (C) a silicone emulsifier, and (D) a silicone oil,
  • a water-in-oil emulsified cosmetic containing (C) a 50% by mass solution of cyclopentasiloxane as a silicone emulsifier has a viscosity of 300 mPa s or more;
  • Silicone oil accounts for more than 50% by weight of the total liquid oil,
  • the gist of the present invention is a water-in-oil emulsified cosmetic in which (B) a hydrophobized pigment is dispersed in an internal water phase.
  • the water-in-oil emulsified cosmetic according to the present invention has the above-described structure, so that it does not give a powdery feel when applied and has excellent spreadability.
  • the finished product is uniform, and the emulsified particles are hard to break and excellent emulsification stability can be realized.
  • the water-in-oil emulsified cosmetic of the present invention contains (A) a nonionic surfactant having an HLB of 9 or more, (B) a hydrophobized pigment, (C) a silicone emulsifier, and (D) a silicone oil. contains.
  • polyoxyethylene may be abbreviated as "POE”, polyethylene glycol as “PEG”, and polypropylene glycol as "PPG”.
  • the (A) nonionic surfactant (hereinafter sometimes referred to as "(A) component") blended in the present invention adsorbs to the particle surface of the (B) hydrophobized pigment to make it hydrophilic, ( B) It has the effect of uniformly dispersing the hydrophobized pigment in the inner water phase.
  • the HLB of the nonionic surfactant is 7 or more, more preferably 8 or more, and still more preferably 9 or more. However, if the HLB is 7 or more, a sufficient effect can be obtained. It is preferable to blend (A) a nonionic surfactant with an HLB of 9 or more.
  • nonionic surfactants include fatty acid polyoxyalkylene glyceryl, polyoxyalkylene hydrogenated castor oil, polyoxyalkylene alkyl ether, fatty acid polyoxyalkylene sorbitan, polyoxyalkylene phytosterol, and polyoxyalkylene-modified silicone. etc. can be mentioned.
  • fatty acid polyoxyalkylene glyceryl such as PEG-20 glyceryl isostearate
  • Polyoxyalkylene hydrogenated castor oils such as PEG-40 hydrogenated castor oil, PEG-60 hydrogenated castor oil, PEG-100 hydrogenated castor oil
  • Polyoxyalkylene alkyl ethers such as PEG-20 oleyl ether, PEG-10 behenyl ether, PEG-20 behenyl ether, PEG-30 behenyl ether
  • fatty acid polyoxyalkylene sorbitan such as PEG-20 sorbitan monolaurate, PEG-20 sorbitan monostearate, PEG-20 sorbitan monooleate
  • Polyoxyalkylene phytosterols such as PEG-30 phytosterols
  • Polyoxyalkylene-modified silicones such as PEG-12 dimethicone; etc.
  • PEG-60 hydrogenated castor oil and PEG-100 hydrogenated castor oil are preferred.
  • One or two or more nonionic surfactants can be used, and the total content thereof is 0.01% by mass or more with respect to the total amount of the water-in-oil emulsified cosmetic. is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, and preferably 10% by mass or less, more preferably 8% by mass or less, and even more preferably 5% by mass or less.
  • the (B) hydrophobized pigment blended in the present invention (hereinafter sometimes referred to as "(B) component”) can be those commonly blended in cosmetics as a coloring material, and is particularly limited not a thing (B)
  • the hydrophobized pigment is a powder such as a hydrophobized pigment, and specifically includes titanium oxide, iron oxide, magnesium oxide, zinc oxide, calcium oxide, calcium phosphate, calcium carbonate, alumina, hydroxide.
  • a base such as aluminum, barium sulfate, a pearlescent pigment (titanium mica, bismuth oxychloride, etc.), talc, etc., or a composite material of these bases.
  • Hydrophobic treatment includes, for example, silicone treatment (silicone oils such as methylhydrogenpolysiloxane, dimethylpolysiloxane, and methylphenylpolysiloxane; methyltrimethoxysilane, ethyltrimethoxysilane, hexyltrimethoxysilane, octyltrimethoxysilane, etc.
  • silicone treatment silicone oils such as methylhydrogenpolysiloxane, dimethylpolysiloxane, and methylphenylpolysiloxane
  • methyltrimethoxysilane ethyltrimethoxysilane
  • hexyltrimethoxysilane octyltrimethoxysilane, etc.
  • fluoroalkylsilanes such as trifluoromethylethyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, etc.
  • fatty acid treatment palmitic acid, isostearic acid, stearic acid, lauric acid, myristic acid, behenic acid, treatment with oleic acid, rosin acid, 12-hydroxystearic acid, etc.
  • fatty acid soap treatment treatment with aluminum stearate, calcium stearate, 12-hydroxystearic acid, etc.
  • fatty acid ester treatment (dextrin fatty acid ester, cholesterol fatty acid ester, treatment with sugar fatty acid ester, starch fatty acid ester, etc.).
  • the average particle size of the hydrophobized pigment is preferably 200 to 10000 nm, more preferably 200 to 1000 nm.
  • the "average particle size” used herein is the number average size (average of 50 arbitrary particles) obtained by image analysis of transmission electron micrographs.
  • Hydrophobized pigments may be used alone or in combination of two or more, and the total content thereof is preferably 0.01% by mass or more relative to the total amount of the water-in-oil emulsified cosmetic. , more preferably 1% by mass or more, and more preferably 5% by mass or more. Moreover, it is preferably 25% by mass or less, more preferably 20% by mass or less, and even more preferably 15% by mass or less.
  • the (C) silicone-based emulsifier (hereinafter sometimes referred to as "(C) component”) blended in the present invention has an emulsifying action that allows fine droplets of the aqueous phase to enter the oil phase, which is the continuous phase. Disperse stably. Therefore, the HLB of (C) the silicone emulsifier is preferably 8 or less, more preferably 6 or less, and even more preferably 5 or less.
  • the silicone-based emulsifier has a viscosity at 25° C. of a solution obtained by dissolving the emulsifier in cyclopentasiloxane to a concentration of 50% by mass (hereinafter sometimes referred to as “viscosity of the emulsifier”) of 300 mPa ⁇ . s or more, preferably 320 mPa ⁇ s or more, and still more preferably 340 mPa ⁇ s or more.
  • the upper limit of the viscosity of the emulsifier is not particularly limited, but is preferably 60,000 mPa s or less, more preferably 30,000 mPa s or less, further preferably 10,000 mPa s or less, and 1,000 mPa s or less. is more preferable, and 500 mPa ⁇ s or less is even more preferable.
  • a silicone-based emulsifier having an emulsifier viscosity of 300 mPa ⁇ s or more as component (C) the aqueous phase can be more stably dispersed in the oil phase, and as a result, the hydrophobized pigment (B) can be obtained. It can be stably retained in the inner water phase.
  • the "viscosity of the emulsifier" is measured by rotor No. using a Brookfield viscometer. 1. Values measured under the conditions of 12 rpm for 1 minute.
  • silicone-based emulsifier examples include various polyether-modified silicones. Among them, cetyl PEG/PPG-10/1 dimethicone and PEG/PPG-19/19 dimethicone are particularly preferred.
  • a silicone-based emulsifier can also be a commercially available product, and specific examples thereof include cetyl PEG/PPG-10/1 dimethicone (eg, ABIL EM90; manufactured by Evonik Japan Co., Ltd.), PEG/PPG-19. /19 dimethicone (eg, BY11-030; manufactured by Dow Toray Industries, Inc.) and the like.
  • Silicone emulsifiers may be used alone or in combination of two or more, and the total content thereof is preferably 0.1% by mass or more relative to the total amount of the water-in-oil emulsified cosmetic, 1% by mass or more is more preferable, 2% by mass or more is more preferable, 10% by mass or less is preferable, 8% by mass or less is more preferable, and 6% by mass or less is even more preferable.
  • the (D) silicone oil blended in the present invention (hereinafter sometimes referred to as "(D) component") has the property of being difficult to mix with sebum, so it can impart a refreshing feeling.
  • (D) Silicone oil may be volatile or non-volatile.
  • the silicone oil (D) preferably has a viscosity (Brookfield viscometer) of 1 mPa ⁇ s or more and 500 mPa ⁇ s or less at 25° C., more preferably 1 mPa ⁇ s or more and 100 mPa ⁇ s or less.
  • the "viscosity" of (D) silicone oil is measured by rotor No. using a Brookfield viscometer. 1. Values measured under the conditions of 12 rpm for 1 minute.
  • silicone oils include linear polysiloxanes such as dimethylpolysiloxane (dimethicone), methylphenylpolysiloxane, diphenylpolysiloxane; octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane and alkyl-modified polysiloxanes such as caprylyl methicone. Among them, dimethicone is preferred.
  • silicone oils can be used, and the total content thereof is preferably 20% by mass or more, preferably 30% by mass, based on the total amount of the water-in-oil emulsified cosmetic. % or more, more preferably 40 mass % or more, preferably 90 mass % or less, more preferably 80 mass % or less, and even more preferably 70 mass % or less.
  • (D) silicone oil accounts for more than 50% by mass, more preferably 55% by mass or more, and still more preferably 60% by mass or more of the total liquid oil content.
  • total liquid oil refers to (D) a silicone oil as well as an oil that is liquid at 25°C and is commonly used in cosmetics. If this ratio ((D) silicone oil/total liquid oil content) is more than 50% by mass, excellent emulsification system stability can be achieved.
  • Oily components include not only oils such as hydrocarbon oils, fats, waxes, higher fatty acids, higher alcohols, and ester oils, but also the oil phase of general cosmetics such as oil-soluble polymers, ultraviolet absorbers, fragrances, and drugs. Components to be blended as components can be mentioned.
  • hydrocarbon oils examples include liquid paraffin, ozokerite, squalene, pristane, paraffin, ceresin, squalene, vaseline, and microcrystalline wax.
  • Fats and oils include avocado oil, camellia oil, evening primrose oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil, sasanqua oil, castor oil, and linseed oil.
  • oils and fats such as glycerin; cocoa butter, coconut oil, horse oil, hydrogenated coconut oil, palm oil, beef tallow, mutton tallow, hydrogenated beef tallow, palm kernel oil, lard, beef bone fat, Japanese wax kernel oil, hydrogenated oil, beef leg
  • solid oils such as fat, Japanese wax, and hydrogenated castor oil.
  • Waxes include, for example, beeswax, candelilla wax, cotton wax, carnauba wax, bayberry wax, wart wax, whale wax, montan wax, bran wax, lanolin, kapok wax, lanolin acetate, liquid lanolin, sugarcane wax, isopropyl lanolin fatty acid, hexyl laurate, Reduced lanolin, jojoba wax, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin fatty acid polyethylene glycol, POE hydrogenated lanolin alcohol ether and the like.
  • higher fatty acids examples include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, undecylenic acid, toric acid, isostearic acid, linoleic acid, linoleic acid, eicosapentaenoic acid (EPA), docosahexaenoic acid ( DHA) and the like.
  • Higher alcohols include, for example, straight-chain alcohols (e.g., lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol, etc.); branched-chain alcohols (e.g., monostearyl glycerin ether (bacyl alcohol ), 2-decyltetradecinol, lanolin alcohol, cholesterol, phytosterol, hexyldodecanol, isostearyl alcohol, octyldodecanol, etc.).
  • straight-chain alcohols e.g., lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol, etc.
  • branched-chain alcohols e.g., monostearyl glycerin ether (bacyl alcohol ), 2-decyltetradecinol,
  • Ester oils include pentaerythrityl tetraethylhexanoate, cetyl ethylhexanoate, di(phytosteryl/octyldodecyl) lauroyl glutamate, triisostearin, glyceryl diisostearate, triethylhexanoin, dimer dilinoleic acid (phytosteryl/behenyl), dimer Linoleic acid (phytosteryl/isostearyl/cetyl/stearyl/behenyl), isopropyl palmitate, macadamia nut fatty acid phytosteryl, tetra (behenate/benzoate/ethylhexanoate) pentaerythrityl, ethylhexyl palmitate, myristyl myristate, myristic acid Examples include isopropyl, tripropylene glycol dipivalate, diisopropyl sebac
  • the aqueous component is not particularly limited as long as it is an aqueous component used in the field of cosmetics, and water, as well as lower alcohols such as ethanol, propanol, isopropyl alcohol and butanol, as well as moisturizing agents and highly water-soluble Ingredients such as molecules, ultraviolet absorbers, sequestering agents, antioxidants, drugs, and the like, which are generally blended as aqueous phase components of cosmetics, can be mentioned.
  • the water-in-oil emulsified cosmetic composition according to the present invention contains a hydrophobized pigment in the internal water phase, it does not easily give a powdery feel when applied and is excellent in spreadability.
  • the hydrophobized pigment is dispersed in the internal water phase, the pigment is less likely to be affected by solid oil content, etc., and aggregation of the pigments is less likely to occur, thereby achieving a uniform makeup finish. Therefore, in order to maximize these effects, it is preferable that the water-in-oil emulsified cosmetic composition according to the present invention contains substantially no powder in the external oil phase. More preferably there is no powder in it.
  • the water-in-oil emulsified cosmetic according to the present invention can contain a sufficient amount of pigment in the inner water phase, that is, in the emulsified particles. It has excellent unevenness correction effect, and at the same time, it spreads well when applied and is excellent in uniform finish of makeup. Therefore, it can be widely applied to makeup cosmetics such as liquid foundation, concealer, makeup base, eye shadow, blush, and mascara.
  • the water-in-oil emulsified cosmetic according to the present invention is characterized by containing (B) a hydrophobized pigment in the internal water phase.
  • (B) a hydrophobized pigment in the internal water phase first, (A) the nonionic surfactant, (B) the hydrophobized pigment, and other aqueous components are mixed, followed by a bead mill or the like. It is necessary to prepare an aqueous dispersion in which the (B) hydrophobized pigment is dispersed in an aqueous component by treatment with a high-pressure homogenizer or the like.
  • the hydrophilicity of (A) the nonionic surfactant is applied to the particle surface of the (B) hydrophobized pigment. Since the oil group is adsorbed and the hydrophilic group faces outward, the (B) hydrophobized pigment can be blended with the aqueous component and dispersed uniformly. As a result, the hydrophobized pigment (B) is stably dispersed in the aqueous dispersion as fine particles, so that an aqueous dispersion with high Newtonian fluidity can be obtained.
  • the ratio of (B) the hydrophobized pigment to the total water phase component is preferably 50% by mass or less, more preferably 45% by mass or less, and even more preferably 40% by mass or less.
  • the “total aqueous phase components” include (A) nonionic surfactants, (B) hydrophobized pigments, water-soluble ultraviolet absorbers, moisturizing agents, and other components that make up the aqueous phase. including. If this ratio ((B) hydrophobized pigment/total aqueous phase component) is 50% by mass or less, an aqueous dispersion having extremely excellent dispersion stability can be obtained, which is preferable.
  • the resulting aqueous dispersion is added to an oil phase mixture obtained by mixing (C) a silicone emulsifier, (D) a silicone oil, and other oily components, and a general water-in-oil emulsification It may be emulsified by a method similar to the manufacturing method of cosmetics.
  • the following steps (1) to (3) (1) Aqueous dispersion in which (A) a nonionic surfactant having an HLB of 9 or more, (B) a hydrophobized pigment, and an aqueous component are mixed, and (B) the hydrophobized pigment is dispersed in the aqueous component preparing a product, (2) a step of mixing (C) a silicone emulsifier, (D) a silicone oil, and an oily component to prepare an oil phase mixture; (3) A step of adding the aqueous dispersion obtained in step (1) to the oil phase mixture obtained in step (2) for emulsification.
  • the present invention will be described in more detail below with reference to examples, but the present invention is not limited by these.
  • the blending amount is shown in % by mass with respect to the total amount of the water-in-oil emulsified cosmetic.
  • the hydrophobized pigment could not be wetted into the water phase and could not be sufficiently dispersed. Shear thinning was observed in samples 2, 4, 5 and 7. The reason for this is considered to be that the aggregation between the hydrophobized pigments was loosened by the flow. That is, the hydrophobized pigment was not sufficiently wetted with water and was not evenly dispersed. Newtonian flow was observed in samples 3, 6, 8-22. As a result, it was found that the hydrophobized pigment was sufficiently wetted with water and uniformly dispersed in the aqueous component. As described above, when a nonionic surfactant having an HLB of 9 or more was used, the hydrophobized pigment could be stably and well dispersed in the aqueous component in any case.
  • Aqueous dispersions were prepared by dispersing pigments with different hydrophobic treatment methods in an aqueous component, and dispersibility was evaluated.
  • any hydrophobized pigment could be well dispersed regardless of the surface treatment method (Samples 23 to 25).
  • Examples 1-2 and Comparative Examples 1-8> Water-in-oil emulsified cosmetics were prepared using various emulsifiers, and the emulsion stability was evaluated by the following method. Also, the viscosity of the emulsifier used was examined by the following method.
  • Emulsion stability After storing the prepared water-in-oil emulsified cosmetic in a constant temperature bath at 50°C for one month, the state of dispersion of the hydrophobized pigment was observed with an optical microscope and evaluated according to the following criteria.
  • Viscosity of Emulsifier The viscosity at 25° C. of a solution obtained by dissolving 50% by mass of an emulsifier in cyclopentasiloxane was measured using a Brookfield viscometer. 1. Measured under conditions of 12 rpm for 1 minute.
  • Example 14 and Comparative Example 15 As the pigment to be dispersed in the internal water phase, the following methods were used to evaluate the spreadability during application and the uniformity of the makeup finish in the case of using a hydrophobic treatment pigment and the case of using a hydrophilic treatment pigment. .
  • a panel of 10 cosmetic evaluation specialists used the water-in-oil emulsified cosmetics of Examples and Comparative Examples, and evaluated them according to the following criteria.
  • D Less than 1 panel judged that growth was good
  • Example 15 and Comparative Example 16 A water-in-oil emulsified cosmetic (Example 15) in which a hydrophobized pigment is dispersed in the inner water phase and an oil in which the hydrophobized pigment is dispersed in the outer oil phase, both of which have the same ingredients and amounts.
  • a medium-water emulsified cosmetic (Comparative Example 16) was prepared, and spreadability during application and uniformity of makeup finish were evaluated.
  • An oil phase mixture was prepared by heating and mixing components (1) to (5) in Table 9 at 80° C. or higher. Separately, the components (6) to (11) were heated and mixed and treated with a high-pressure homogenizer to prepare an aqueous dispersion (aqueous dispersion in which a hydrophobized pigment is dispersed in an aqueous component). Next, the aqueous dispersion was gradually added to the oil phase mixture, emulsified by a homomixer treatment, and then cooled to obtain a water-in-oil emulsified cosmetic.
  • Formulation example 1 Liquid foundation (ingredient name) Amount (% by mass) (1) Dimethicone 17 (2) diphenylsiloxyphenyl trimethicone 11 (3) PEG/PPG-19/19 dimethicone 4 (4) Ethylhexyl methoxycinnamate 2.5 (5) distearyldimonium hectorite 1.2 (6) Niacinamide 5 (7) Glycerin 5 (8) PEG-60 hydrogenated castor oil 1 (9) Dipropylene glycol 8 (10) Phenoxyethanol 0.5 (11) (dimethylacrylamide/acryloyldimethyltaurate Na) crosspolymer 0.05 (12) Hydrophobized pigment 10 (13) Water 34.75 Total 100
  • Formulation Example 2 Solid emulsified foundation (ingredient name) Blending amount (% by mass) (1) Dimethicone 30 (2) Cetyl PEG/PPG-10/1 Dimethicone 4 (3) Ethylhexyl methoxycinnamate 2.5 (4) Paraffin wax 5 (5) Microcrystalline wax 0.5 (6) distearyldimonium hectorite 1.2 (7) Niacinamide 5 (8) Glycerin 5 (9) PEG-60 hydrogenated castor oil 1 (10) dipropylene glycol 8 (11) Phenoxyethanol 0.5 (12) (dimethylacrylamide/acryloyldimethyltaurate Na) crosspolymer 0.05 (13) Hydrophobic treatment pigment 10 (14) Water 27.25 Total 100
  • Formulation Example 3 Concealer (ingredient name) Amount (% by mass) (1) Dimethicone 20 (2) Cetyl PEG/PPG-10/1 Dimethicone 4 (3) Ethylhexyl methoxycinnamate 2.5 (4) Paraffin wax 7 (5) Microcrystalline wax 0.7 (6) distearyldimonium hectorite 1.2 (7) Niacinamide 5 (8) Glycerin 5 (9) PEG-60 hydrogenated castor oil 1 (10) Dipropylene glycol 5 (11) Phenoxyethanol 0.5 (12) (dimethylacrylamide/acryloyldimethyltaurate Na) crosspolymer 0.05 (13) Hydrophobic treatment pigment 20 (14) Water 28.05 Total 100

Landscapes

  • 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)
  • Dispersion Chemistry (AREA)
  • Cosmetics (AREA)

Abstract

The purpose of the present invention is to provide a water-in-oil emulsified cosmetic having good spreadability during application, excellent uniformity of makeup finish, and excellent emulsion stability, by stably dispersing a hydrophobized pigment in an inner water phase.　This water-in-oil emulsified cosmetic contains (A) a nonionic surfactant having an HLB of at least 9, (B) a hydrophobized pigment, (C) a silicone-based emulsifier, and (D) a silicone oil, wherein a solution of 50 mass% of the silicone-based emulsifier (C) in cyclopentasiloxane has a viscosity of at least 300 mPa·s, the silicone oil (D) constitutes more than 50 mass% of the total liquid oil content, and the hydrophobized pigment (B) is dispersed in an inner water phase.

Description

油中水型乳化化粧料Water-in-oil emulsified cosmetic
　本発明は、油中水型乳化化粧料に関する。より詳しくは、塗布中の伸びの良さ、化粧の仕上がりの均一さ、及び、乳化安定性に優れた油中水型乳化化粧料に関する。 The present invention relates to a water-in-oil emulsified cosmetic. More specifically, it relates to a water-in-oil emulsified cosmetic that is excellent in spreadability during application, uniform finish of makeup, and excellent emulsification stability.
　油相を外相、水相を内相とした油中水型の乳化組成物は、油溶性の有効成分、例えばエモリエント油、薬剤、紫外線吸収剤等を効率的に皮膚上に展開できることから皮膚外用剤に適した剤型であり、ファンデーション等のメーキャップ化粧料に広く活用されている。 A water-in-oil emulsified composition having an oil phase as an outer phase and an aqueous phase as an inner phase can efficiently spread oil-soluble active ingredients such as emollient oils, drugs, ultraviolet absorbers, etc. on the skin. It has a suitable dosage form and is widely used in make-up cosmetics such as foundation.
　ファンデーション等のメーキャップ化粧料には、シミ、そばかす等の肌の色むらや毛穴等の肌の凹凸を補正する効果を有する酸化亜鉛や酸化チタン等の白色顔料や酸化鉄等の着色顔料が用いられている。高い補正効果等を得るにはこれらの顔料を化粧料に高配合することが求められている。 Makeup cosmetics such as foundations use white pigments such as zinc oxide and titanium oxide, and colored pigments such as iron oxide, which have the effect of correcting skin unevenness such as spots and freckles and skin unevenness such as pores. ing. In order to obtain a high corrective effect, etc., it is required that these pigments are highly blended in cosmetics.
　油中水型乳化化粧料に顔料を配合するにあたっては、表面を疎水化処理した顔料を外油相に分散させるのが一般的である。例えば、特許文献１には、優れた貯蔵安定性と皮膚への均一なメイクアップを可能にするファンデーション組成物を得るために、アルキルジメチコーンコポリオール、ジメチコーンコポリオール、疎水性被覆顔料、及び大量の揮発性油の混合物を使用することが提案されている。しかし、外油相に疎水化処理顔料を分散させると、肌に塗布する際に粉ぎしみ（なめらかさが欠けてくる感触）を生じやすく、使用感触に劣る傾向がある。また、外油相にワックス等の固形油分や半固形油分、被膜剤などの高分子を含む場合には、これらと粉末とが凝集を起こし、この凝集物に起因して塗布時ののびが重くなり、化粧の仕上がりが不均一になるという問題も生じやすい。 When blending a pigment into a water-in-oil emulsified cosmetic, it is common to disperse the pigment whose surface has been hydrophobized in the outer oil phase. For example, in Patent Document 1, alkyldimethicone copolyol, dimethicone copolyol, hydrophobic coated pigment, and It has been proposed to use mixtures of large amounts of volatile oils. However, when the hydrophobic treated pigment is dispersed in the external oil phase, it tends to cause a chalky feeling (feeling lacking in smoothness) when applied to the skin, and tends to be inferior to the feel of use. In addition, when the external oil phase contains solid oil such as wax, semi-solid oil, or macromolecules such as coating agents, these aggregates and the powder cause agglomeration, resulting in slow spreadability during application. As a result, the problem of non-uniform finish of makeup tends to occur.
　そこで、塗布時の伸びやみずみずしさといった使用感触の改善を図るために、内水相に顔料を分散させる試みもなされている。
　例えば、特許文献２には、内水相に疎水化処理されていない粉末を安定に分散配合するために、外油相を（Ａ）ワックス及び（Ｂ）ジステアルジモニウムヘクトライトで増粘又は固化することが提案されている。しかし、疎水化処理されていない粉末は、皮膚に塗布した後に経時的に粉ぎしみを生じやすい傾向がある。 Therefore, attempts have been made to disperse pigments in the internal water phase in order to improve the feeling of use such as spreadability and freshness during application.
For example, Patent Document 2 discloses that an outer oil phase is thickened with (A) wax and (B) disteardimonium hectorite or It is suggested to solidify. However, non-hydrophobized powders tend to cause creaking over time after being applied to the skin.
　一方、内水相に疎水化処理顔料を分散させることも考えられるが、疎水化処理顔料は水との親和性が悪いために、通常、安定に分散させることは不可能である。
　また、一般に、乳化化粧料の内相、すなわち乳化粒子の内部に顔料を分散させると、顔料自身あるいはその分散剤の界面活性によって油水界面張力が低下し、乳化粒子が壊れやすくなる傾向がある。 On the other hand, it is conceivable to disperse a hydrophobized pigment in the inner water phase, but it is usually impossible to stably disperse the hydrophobized pigment because of its poor affinity with water.
In general, when a pigment is dispersed in the internal phase of an emulsified cosmetic, that is, inside emulsified particles, the surface activity of the pigment itself or its dispersant lowers the oil-water interfacial tension, and the emulsified particles tend to break easily.
特開２００４－０２６８３３号公報JP-A-2004-026833 特開２０１７－０３１１４９号公報JP 2017-031149 A
　本発明は、前記実情に鑑みてなされたものであり、内水相に疎水化処理顔料を安定に分散させることによって、塗布中の伸びの良さや化粧の仕上がりの均一さに優れ、なおかつ、乳化安定性にも優れた油中水型乳化化粧料を提供することを目的とする。 The present invention has been made in view of the above-mentioned circumstances, and by stably dispersing a hydrophobized pigment in the internal water phase, the spreadability during application and the uniformity of the makeup finish are excellent, and the emulsion is emulsified. To provide a water-in-oil emulsified cosmetic excellent in stability.
　本発明者らは上記の課題を解決すべく鋭意研究を行った結果、所定のＨＬＢを有する非イオン性界面活性剤を用いて水性成分に疎水化処理顔料を分散させた水性分散物を調製し、この水性分散物をシリコーン油を含む油性成分中に所定の粘度を示すシリコーン系乳化剤を用いて乳化させることにより、乳化粒子の内部、すなわち内水相中に疎水化処理顔料を安定に分散させることができ、それによって塗布中の伸びの良さ、化粧の仕上がりの均一さ、乳化安定性が格段に向上することを見出し、本発明を完成するに至った。 The inventors of the present invention conducted intensive research to solve the above problems, and as a result, prepared an aqueous dispersion in which a hydrophobized pigment was dispersed in an aqueous component using a nonionic surfactant having a predetermined HLB. By emulsifying this aqueous dispersion in an oil component containing silicone oil using a silicone emulsifier exhibiting a predetermined viscosity, the hydrophobized pigment is stably dispersed inside the emulsified particles, i.e., in the internal water phase. As a result, the inventors found that the spreadability during application, the uniformity of the makeup finish, and the emulsification stability were remarkably improved, leading to the completion of the present invention.
　すなわち、本発明は、
（Ａ）ＨＬＢが９以上の非イオン性界面活性剤、
（Ｂ）疎水化処理顔料、
（Ｃ）シリコーン系乳化剤、及び
（Ｄ）シリコーン油、
を含有する油中水型乳化化粧料であって、
（Ｃ）シリコーン系乳化剤のシクロペンタシロキサンにおける５０質量％溶液の粘度が３００ｍＰａ・ｓ以上であり、
（Ｄ）シリコーン油が全液状油分の５０質量％より多くを占め、
かつ
（Ｂ）疎水化処理顔料が内水相に分散されている、油中水型乳化化粧料を要旨とするものである。 That is, the present invention
(A) a nonionic surfactant with an HLB of 9 or more;
(B) a hydrophobized pigment,
(C) a silicone emulsifier, and (D) a silicone oil,
A water-in-oil emulsified cosmetic containing
(C) a 50% by mass solution of cyclopentasiloxane as a silicone emulsifier has a viscosity of 300 mPa s or more;
(D) Silicone oil accounts for more than 50% by weight of the total liquid oil,
The gist of the present invention is a water-in-oil emulsified cosmetic in which (B) a hydrophobized pigment is dispersed in an internal water phase.
　本発明に係る油中水型乳化化粧料は、上記構成とすることにより、塗布の際に粉っぽい感触を生じにくく伸びの良さに優れ、顔料が凝集することなく安定に分散するため化粧の仕上がりが均一であり、しかも、乳化粒子が壊れにくく優れた乳化安定性を実現することができる。 The water-in-oil emulsified cosmetic according to the present invention has the above-described structure, so that it does not give a powdery feel when applied and has excellent spreadability. The finished product is uniform, and the emulsified particles are hard to break and excellent emulsification stability can be realized.
　本発明の油中水型乳化化粧料は、（Ａ）ＨＬＢが９以上の非イオン性界面活性剤、（Ｂ）疎水化処理顔料、（Ｃ）シリコーン系乳化剤、及び、（Ｄ）シリコーン油を含有する。
　なお、以下において、ポリオキシエチレンを「ＰＯＥ」、ポリエチレングリコールを「ＰＥＧ」、ポリプロピレングリコールを「ＰＰＧ」と略記する場合がある。 The water-in-oil emulsified cosmetic of the present invention contains (A) a nonionic surfactant having an HLB of 9 or more, (B) a hydrophobized pigment, (C) a silicone emulsifier, and (D) a silicone oil. contains.
In the following, polyoxyethylene may be abbreviated as "POE", polyethylene glycol as "PEG", and polypropylene glycol as "PPG".
＜（Ａ）非イオン性界面活性剤＞
　本発明に配合される（Ａ）非イオン性界面活性剤（以下、「（Ａ）成分」と称する場合がある）は、（Ｂ）疎水化処理顔料の粒子表面に吸着して親水化し、（Ｂ）疎水化処理顔料を内水相に均一に分散させる作用を有する。
　（Ａ）非イオン性界面活性剤のＨＬＢは、７以上であり、より好ましくは８以上であり、さらに好ましくは９以上である。ただし、ＨＬＢが７以上であれば十分な効果が得られるが、内水相を構成する水性成分中に（Ｂ）疎水化処理顔料を凝集させることなく、より確実かつ良好に分散させるには、ＨＬＢが９以上の（Ａ）非イオン性界面活性剤を配合するのが好ましい。 <(A) nonionic surfactant>
The (A) nonionic surfactant (hereinafter sometimes referred to as "(A) component") blended in the present invention adsorbs to the particle surface of the (B) hydrophobized pigment to make it hydrophilic, ( B) It has the effect of uniformly dispersing the hydrophobized pigment in the inner water phase.
(A) The HLB of the nonionic surfactant is 7 or more, more preferably 8 or more, and still more preferably 9 or more. However, if the HLB is 7 or more, a sufficient effect can be obtained. It is preferable to blend (A) a nonionic surfactant with an HLB of 9 or more.
　（Ａ）非イオン性界面活性剤としては、例えば、脂肪酸ポリオキシアルキレングリセリル、ポリオキシアルキレン水添ヒマシ油、ポリオキシアルキレンアルキルエーテル、脂肪酸ポリオキシアルキレンソルビタン、ポリオキシアルキレンフィトステロール、ポリオキシアルキレン変性シリコーン等を挙げることができる。
　より具体的には、
イソステアリン酸ＰＥＧ－２０グリセリル等の脂肪酸ポリオキシアルキレングリセリル；
ＰＥＧ－４０水添ヒマシ油、ＰＥＧ－６０水添ヒマシ油、ＰＥＧ－１００水添ヒマシ油等のポリオキシアルキレン水添ヒマシ油；
ＰＥＧ－２０オレイルエーテル、ＰＥＧ－１０ベヘニルエーテル、ＰＥＧ－２０ベヘニルエーテル、ＰＥＧ－３０ベヘニルエーテル等のポリオキシアルキレンアルキルエーテル；
モノラウリン酸ＰＥＧ－２０ソルビタン、モノステアリン酸ＰＥＧ－２０ソルビタン、モノオレイン酸ＰＥＧ－２０ソルビタン等の脂肪酸ポリオキシアルキレンソルビタン；
ＰＥＧ－３０フィトステロール等のポリオキシアルキレンフィトステロール；
ＰＥＧ－１２ジメチコン等のポリオキシアルキレン変性シリコーン；
等である。
　なかでも、ＰＥＧ－６０水添ヒマシ油、ＰＥＧ－１００水添ヒマシ油が好ましい。 (A) Examples of nonionic surfactants include fatty acid polyoxyalkylene glyceryl, polyoxyalkylene hydrogenated castor oil, polyoxyalkylene alkyl ether, fatty acid polyoxyalkylene sorbitan, polyoxyalkylene phytosterol, and polyoxyalkylene-modified silicone. etc. can be mentioned.
More specifically,
fatty acid polyoxyalkylene glyceryl such as PEG-20 glyceryl isostearate;
Polyoxyalkylene hydrogenated castor oils such as PEG-40 hydrogenated castor oil, PEG-60 hydrogenated castor oil, PEG-100 hydrogenated castor oil;
Polyoxyalkylene alkyl ethers such as PEG-20 oleyl ether, PEG-10 behenyl ether, PEG-20 behenyl ether, PEG-30 behenyl ether;
fatty acid polyoxyalkylene sorbitan such as PEG-20 sorbitan monolaurate, PEG-20 sorbitan monostearate, PEG-20 sorbitan monooleate;
Polyoxyalkylene phytosterols such as PEG-30 phytosterols;
Polyoxyalkylene-modified silicones such as PEG-12 dimethicone;
etc.
Among them, PEG-60 hydrogenated castor oil and PEG-100 hydrogenated castor oil are preferred.
　（Ａ）非イオン性界面活性剤は、１種又は２種以上を用いることができ、その合計含有量は、油中水型乳化化粧料の全量に対して０．０１質量％以上であるのが好ましく、０．１質量％以上がより好ましく、０．５質量％以上がさらに好ましく、また、１０質量％以下が好ましく、８質量％以下がより好ましく、５質量％以下がさらに好ましい。 (A) One or two or more nonionic surfactants can be used, and the total content thereof is 0.01% by mass or more with respect to the total amount of the water-in-oil emulsified cosmetic. is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, and preferably 10% by mass or less, more preferably 8% by mass or less, and even more preferably 5% by mass or less.
＜（Ｂ）疎水化処理顔料＞
　本発明に配合される（Ｂ）疎水化処理顔料（以下、「（Ｂ）成分」と称する場合がある）は、色材として通常化粧料に配合されているものを使用でき、特に限定されるものではない。
（Ｂ）疎水化処理顔料は、疎水化処理された顔料等の粉末であり、具体的には、酸化チタン、酸化鉄、酸化マグネシウム、酸化亜鉛、酸化カルシウム、リン酸カルシウム、炭酸カルシウム、アルミナ、水酸化アルミニウム、硫酸バリウム、真珠光沢顔料（雲母チタン、オキシ塩化ビスマス等）、タルク等の基剤、又はこれら基剤の複合材料からなる粉末の表面を疎水化処理した粉末である。 <(B) Hydrophobic treatment pigment>
The (B) hydrophobized pigment blended in the present invention (hereinafter sometimes referred to as "(B) component") can be those commonly blended in cosmetics as a coloring material, and is particularly limited not a thing
(B) The hydrophobized pigment is a powder such as a hydrophobized pigment, and specifically includes titanium oxide, iron oxide, magnesium oxide, zinc oxide, calcium oxide, calcium phosphate, calcium carbonate, alumina, hydroxide. It is a powder obtained by hydrophobizing the surface of a powder composed of a base such as aluminum, barium sulfate, a pearlescent pigment (titanium mica, bismuth oxychloride, etc.), talc, etc., or a composite material of these bases.
　疎水化処理としては、例えば、シリコーン処理（メチルハイドロジェンポリシロキサン、ジメチルポリシロキサン、メチルフェニルポリシロキサン等のシリコーン油；メチルトリメトキシシラン、エチルトリメトキシシラン、ヘキシルトリメトキシシラン、オクチルトリメトキシシラン等のアルキルシラン；トリフルオロメチルエチルトリメトキシシラン、ヘプタデカフルオロデシルトリメトキシシラン等のフルオロアルキルシラン等による処理）、脂肪酸処理（パルミチン酸、イソステアリン酸、ステアリン酸、ラウリン酸、ミリスチン酸、ベヘニン酸、オレイン酸、ロジン酸、１２－ヒドロキシステアリン酸等による処理）、脂肪酸石鹸処理（ステアリン酸アルミニウム、ステアリン酸カルシウム、１２－ヒドロキシステアリン酸等による処理）、脂肪酸エステル処理（デキストリン脂肪酸エステル、コレステロール脂肪酸エステル、ショ糖脂肪酸エステル、デンプン脂肪酸エステル等による処理）等が挙げられる。これらの疎水化処理は、常法に従って行うことができる。 Hydrophobic treatment includes, for example, silicone treatment (silicone oils such as methylhydrogenpolysiloxane, dimethylpolysiloxane, and methylphenylpolysiloxane; methyltrimethoxysilane, ethyltrimethoxysilane, hexyltrimethoxysilane, octyltrimethoxysilane, etc. treatment with fluoroalkylsilanes such as trifluoromethylethyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, etc.), fatty acid treatment (palmitic acid, isostearic acid, stearic acid, lauric acid, myristic acid, behenic acid, treatment with oleic acid, rosin acid, 12-hydroxystearic acid, etc.), fatty acid soap treatment (treatment with aluminum stearate, calcium stearate, 12-hydroxystearic acid, etc.), fatty acid ester treatment (dextrin fatty acid ester, cholesterol fatty acid ester, treatment with sugar fatty acid ester, starch fatty acid ester, etc.). These hydrophobizing treatments can be carried out according to conventional methods.
　（Ｂ）疎水化処理顔料の平均粒子径は、２００～１００００ｎｍが好ましく、さらに好ましくは２００～１０００ｎｍである。
　なお、本明細書における「平均粒子径」は透過電子顕微鏡写真の画像解析による個数平均径（任意の５０個の粒子の平均）である。 (B) The average particle size of the hydrophobized pigment is preferably 200 to 10000 nm, more preferably 200 to 1000 nm.
The "average particle size" used herein is the number average size (average of 50 arbitrary particles) obtained by image analysis of transmission electron micrographs.
　（Ｂ）疎水化処理顔料は、１種又は２種以上を用いることができ、その合計含有量は、油中水型乳化化粧料の全量に対して０．０１質量％以上であるのが好ましく、１質量％以上がより好ましく、５質量％以上がさらに好ましい。また、２５質量％以下が好ましく、２０質量％以下がより好ましく、１５質量％以下がさらに好ましい。 (B) Hydrophobized pigments may be used alone or in combination of two or more, and the total content thereof is preferably 0.01% by mass or more relative to the total amount of the water-in-oil emulsified cosmetic. , more preferably 1% by mass or more, and more preferably 5% by mass or more. Moreover, it is preferably 25% by mass or less, more preferably 20% by mass or less, and even more preferably 15% by mass or less.
＜（Ｃ）シリコーン系乳化剤＞
　本発明に配合される（Ｃ）シリコーン系乳化剤（以下、「（Ｃ）成分」と称する場合がある）は、その乳化作用により、水相の微小液滴を連続相である油相の中に安定に分散させる。このため、（Ｃ）シリコーン系乳化剤のＨＬＢは、８以下であることが好ましく、より好ましくは６以下、さらに好ましくは５以下である。 <(C) Silicone emulsifier>
The (C) silicone-based emulsifier (hereinafter sometimes referred to as "(C) component") blended in the present invention has an emulsifying action that allows fine droplets of the aqueous phase to enter the oil phase, which is the continuous phase. Disperse stably. Therefore, the HLB of (C) the silicone emulsifier is preferably 8 or less, more preferably 6 or less, and even more preferably 5 or less.
　また、（Ｃ）シリコーン系乳化剤は、乳化剤をシクロペンタシロキサン中に５０質量％となるように溶解させた溶液の２５℃における粘度（以下、「乳化剤の粘度」と称する場合がある）が３００ｍＰａ・ｓ以上を示すものが好ましく、より好ましくは３２０ｍＰａ・ｓ以上、さらに好ましくは３４０ｍＰａ・ｓ以上を示すものである。乳化剤の粘度の上限は特に限定されるものではないが、６０，０００ｍＰａ・ｓ以下が好ましく、３０，０００ｍＰａ・ｓ以下がさらに好ましく、１０，０００ｍＰａ・ｓ以下がさらに好ましく、１，０００ｍＰａ・ｓ以下がさらに好ましく、５００ｍＰａ・ｓ以下がさらに好ましい。
（Ｃ）成分として乳化剤の粘度が３００ｍＰａ・ｓ以上を示すシリコーン系乳化剤を用いることにより、油相中に水相をより安定に分散させることができ、その結果、（Ｂ）疎水化処理顔料を内水相に安定に保持することができる。
　なお、「乳化剤の粘度」は、Ｂ型粘度計を用いて、ローターＮｏ．１、回転数１２ｒｐｍ、１分間の条件で測定した数値である。 In addition, (C) the silicone-based emulsifier has a viscosity at 25° C. of a solution obtained by dissolving the emulsifier in cyclopentasiloxane to a concentration of 50% by mass (hereinafter sometimes referred to as “viscosity of the emulsifier”) of 300 mPa·. s or more, preferably 320 mPa·s or more, and still more preferably 340 mPa·s or more. The upper limit of the viscosity of the emulsifier is not particularly limited, but is preferably 60,000 mPa s or less, more preferably 30,000 mPa s or less, further preferably 10,000 mPa s or less, and 1,000 mPa s or less. is more preferable, and 500 mPa·s or less is even more preferable.
By using a silicone-based emulsifier having an emulsifier viscosity of 300 mPa·s or more as component (C), the aqueous phase can be more stably dispersed in the oil phase, and as a result, the hydrophobized pigment (B) can be obtained. It can be stably retained in the inner water phase.
In addition, the "viscosity of the emulsifier" is measured by rotor No. using a Brookfield viscometer. 1. Values measured under the conditions of 12 rpm for 1 minute.
　（Ｃ）シリコーン系乳化剤の好ましい態様としては、各種のポリエーテル変性シリコーン等が挙げられる。なかでも、セチルＰＥＧ／ＰＰＧ－１０／１ジメチコン、ＰＥＧ／ＰＰＧ－１９／１９ジメチコンが特に好ましい。
　（Ｃ）シリコーン系乳化剤は、市販品を使用することもでき、その具体例としては、セチルＰＥＧ／ＰＰＧ－１０／１ジメチコン（例えば、ＡＢＩＬ　ＥＭ９０；エボニックジャパン株式会社製）、ＰＥＧ／ＰＰＧ－１９／１９ジメチコン（例えば、ＢＹ１１－０３０；ダウ・東レ株式会社製）等が挙げられる。 (C) Preferred embodiments of the silicone-based emulsifier include various polyether-modified silicones. Among them, cetyl PEG/PPG-10/1 dimethicone and PEG/PPG-19/19 dimethicone are particularly preferred.
(C) A silicone-based emulsifier can also be a commercially available product, and specific examples thereof include cetyl PEG/PPG-10/1 dimethicone (eg, ABIL EM90; manufactured by Evonik Japan Co., Ltd.), PEG/PPG-19. /19 dimethicone (eg, BY11-030; manufactured by Dow Toray Industries, Inc.) and the like.
　（Ｃ）シリコーン系乳化剤は、１種又は２種以上を用いることができ、その合計含有量は、油中水型乳化化粧料の全量に対して０．１質量％以上であるのが好ましく、１質量％以上がより好ましく、２質量％以上がさらに好ましく、また、１０質量％以下が好ましく、８質量％以下がより好ましく、６質量％以下がさらに好ましい。 (C) Silicone emulsifiers may be used alone or in combination of two or more, and the total content thereof is preferably 0.1% by mass or more relative to the total amount of the water-in-oil emulsified cosmetic, 1% by mass or more is more preferable, 2% by mass or more is more preferable, 10% by mass or less is preferable, 8% by mass or less is more preferable, and 6% by mass or less is even more preferable.
＜（Ｄ）シリコーン油＞
　本発明に配合される（Ｄ）シリコーン油（以下、「（Ｄ）成分」と称する場合がある）は、皮脂と混ざりにくい性質を有するため、さっぱりとした使用感を付与することができる。
　（Ｄ）シリコーン油は揮発性油でも不揮発性油でもよい。また、（Ｄ）シリコーン油は、２５℃における粘度（Ｂ型粘度計）が、１ｍＰａ・ｓ以上５００ｍＰａ・ｓ以下であるものが好ましく、１ｍＰａ・ｓ以上１００ｍＰａ・ｓ以下であるものがより好ましい。なお、（Ｄ）シリコーン油の「粘度」は、Ｂ型粘度計を用いて、ローターＮｏ．１、回転数１２ｒｐｍ、１分間の条件で測定した数値である。 <(D) Silicone oil>
The (D) silicone oil blended in the present invention (hereinafter sometimes referred to as "(D) component") has the property of being difficult to mix with sebum, so it can impart a refreshing feeling.
(D) Silicone oil may be volatile or non-volatile. The silicone oil (D) preferably has a viscosity (Brookfield viscometer) of 1 mPa·s or more and 500 mPa·s or less at 25° C., more preferably 1 mPa·s or more and 100 mPa·s or less. In addition, the "viscosity" of (D) silicone oil is measured by rotor No. using a Brookfield viscometer. 1. Values measured under the conditions of 12 rpm for 1 minute.
　（Ｄ）シリコーン油の具体例としては、ジメチルポリシロキサン（ジメチコン）、メチルフェニルポリシロキサン、ジフェニルポリシロキサン等の鎖状ポリシロキサン；オクタメチルシクロテトラシロキサン、デカメチルシクロペンタシロキサン、ドデカメチルシクロヘキサシロキサン等の環状ポリシロキサン、カプリリルメチコン等のアルキル変性ポリシロキサンが挙げられる。なかでもジメチコンが好ましい。 (D) Specific examples of silicone oils include linear polysiloxanes such as dimethylpolysiloxane (dimethicone), methylphenylpolysiloxane, diphenylpolysiloxane; octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane and alkyl-modified polysiloxanes such as caprylyl methicone. Among them, dimethicone is preferred.
　（Ｄ）シリコーン油は、１種又は２種以上を用いることができ、その合計含有量は、油中水型乳化化粧料の全量に対して、２０質量％以上であるのが好ましく、３０質量％以上がより好ましく、４０質量％以上がさらに好ましく、また、９０質量％以下が好ましく、８０質量％以下がより好ましく、７０質量％以下がさらに好ましい。 (D) One or two or more silicone oils can be used, and the total content thereof is preferably 20% by mass or more, preferably 30% by mass, based on the total amount of the water-in-oil emulsified cosmetic. % or more, more preferably 40 mass % or more, preferably 90 mass % or less, more preferably 80 mass % or less, and even more preferably 70 mass % or less.
　また、（Ｄ）シリコーン油は、全液状油分の５０質量％より多くを占め、より好ましくは５５質量％以上、さらに好ましくは６０質量％以上を占める。ここで、本発明における「全液状油分」とは、（Ｄ）シリコーン油のほか、化粧料に通常用いられる２５℃で液状の油分を指す。
　この比率（（Ｄ）シリコーン油／全液状油分）が５０質量％より多ければ、優れた乳化系安定性を実現することができる。 In addition, (D) silicone oil accounts for more than 50% by mass, more preferably 55% by mass or more, and still more preferably 60% by mass or more of the total liquid oil content. Here, the term "total liquid oil" as used in the present invention refers to (D) a silicone oil as well as an oil that is liquid at 25°C and is commonly used in cosmetics.
If this ratio ((D) silicone oil/total liquid oil content) is more than 50% by mass, excellent emulsification system stability can be achieved.
＜任意配合成分＞
　本発明の油中水型乳化化粧料には、上記（Ａ）～（Ｄ）成分以外に、本発明の効果を妨げない範囲で、油中水型乳化化粧料に通常用いられる種々の油性成分、水性成分等を配合することができる。 <Optional ingredients>
In the water-in-oil emulsified cosmetic composition of the present invention, in addition to the above components (A) to (D), various oily components commonly used in water-in-oil emulsified cosmetic compositions, within a range that does not interfere with the effects of the present invention. , an aqueous component, and the like.
　油性成分としては、炭化水素油、油脂、ロウ類、高級脂肪酸、高級アルコール、エステル油等の油分はもちろん、例えば、油溶性高分子、紫外線吸収剤、香料、薬剤等の一般に化粧料の油相成分として配合される成分を挙げることができる。 Oily components include not only oils such as hydrocarbon oils, fats, waxes, higher fatty acids, higher alcohols, and ester oils, but also the oil phase of general cosmetics such as oil-soluble polymers, ultraviolet absorbers, fragrances, and drugs. Components to be blended as components can be mentioned.
　炭化水素油としては、流動パラフィン、オゾケライト、スクワレン、プリスタン、パラフィン、セレシン、スクワレン、ワセリン、マイクロクリスタリンワックスなどが例示される。 Examples of hydrocarbon oils include liquid paraffin, ozokerite, squalene, pristane, paraffin, ceresin, squalene, vaseline, and microcrystalline wax.
　油脂としては、アボカド油、ツバキ油、月見草油、タートル油、マカデミアナッツ油、トウモロコシ油、ミンク油、オリーブ油、ナタネ油、卵黄油、ゴマ油、パーシック油、小麦胚芽油、サザンカ油、ヒマシ油、アマニ油、サフラワー油、綿実油、エノ油、大豆油、落花生油、茶実油、カヤ油、コメヌカ油、シナギリ油、日本キリ油、ホホバ油、胚芽油、トリグリセリン、トリオクタン酸グリセリン、トリイソパルミチン酸グリセリン等の液体油脂；カカオ脂、ヤシ油、馬油、硬化ヤシ油、パーム油、牛脂、羊脂、硬化牛脂、パーム核油、豚脂、牛骨脂、モクロウ核油、硬化油、牛脚脂、モクロウ、硬化ヒマシ油等の固体油脂などが例示される。 Fats and oils include avocado oil, camellia oil, evening primrose oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil, sasanqua oil, castor oil, and linseed oil. , safflower oil, cottonseed oil, perilla oil, soybean oil, peanut oil, tea seed oil, kaya oil, rice bran oil, sinagiri oil, Japanese paulownia oil, jojoba oil, germ oil, triglycerin, glyceryl trioctanoate, triisopalmitic acid Liquid oils and fats such as glycerin; cocoa butter, coconut oil, horse oil, hydrogenated coconut oil, palm oil, beef tallow, mutton tallow, hydrogenated beef tallow, palm kernel oil, lard, beef bone fat, Japanese wax kernel oil, hydrogenated oil, beef leg Examples include solid oils such as fat, Japanese wax, and hydrogenated castor oil.
　ロウ類としては、例えば、ミツロウ、キャンデリラロウ、綿ロウ、カルナウバロウ、ベイベリーロウ、イボタロウ、鯨ロウ、モンタンロウ、ヌカロウ、ラノリン、カポックロウ、酢酸ラノリン、液状ラノリン、サトウキビロウ、ラノリン脂肪酸イソプロピル、ラウリン酸ヘキシル、還元ラノリン、ホホバロウ、硬質ラノリン、セラックロウ、ＰＯＥラノリンアルコールエーテル、ＰＯＥラノリンアルコールアセテート、ＰＯＥコレステロールエーテル、ラノリン脂肪酸ポリエチレングリコール、ＰＯＥ水素添加ラノリンアルコールエーテル等が挙げられる。 Waxes include, for example, beeswax, candelilla wax, cotton wax, carnauba wax, bayberry wax, wart wax, whale wax, montan wax, bran wax, lanolin, kapok wax, lanolin acetate, liquid lanolin, sugarcane wax, isopropyl lanolin fatty acid, hexyl laurate, Reduced lanolin, jojoba wax, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin fatty acid polyethylene glycol, POE hydrogenated lanolin alcohol ether and the like.
　高級脂肪酸としては、例えば、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン
酸、ベヘン酸、オレイン酸、ウンデシレン酸、トール酸、イソステアリン酸、リノール酸、リノレイン酸、エイコサペンタエン酸（ＥＰＡ）、ドコサヘキサエン酸（ＤＨＡ）等が挙げられる。 Examples of higher fatty acids include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, undecylenic acid, toric acid, isostearic acid, linoleic acid, linoleic acid, eicosapentaenoic acid (EPA), docosahexaenoic acid ( DHA) and the like.
　高級アルコールとしては、例えば、直鎖アルコール（例えば、ラウリルアルコール、セチルアルコール、ステアリルアルコール、ベヘニルアルコール、ミリスチルアルコール、オレイルアルコール、セトステアリルアルコール等）；分枝鎖アルコール（例えば、モノステアリルグリセリンエーテル(バチルアルコール)、２－デシルテトラデシノール、ラノリンアルコール、コレステロール、フィトステロール、ヘキシルドデカノール、イソステアリルアルコール、オクチルドデカノール等）等が挙げられる。 Higher alcohols include, for example, straight-chain alcohols (e.g., lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol, etc.); branched-chain alcohols (e.g., monostearyl glycerin ether (bacyl alcohol ), 2-decyltetradecinol, lanolin alcohol, cholesterol, phytosterol, hexyldodecanol, isostearyl alcohol, octyldodecanol, etc.).
　エステル油としては、テトラエチルヘキサン酸ペンタエリスリチル、エチルヘキサン酸セチル、ラウロイルグルタミン酸ジ（フィトステリル／オクチルドデシル）、トリイソステアリン、ジイソステアリン酸グリセリル、トリエチルヘキサノイン、ダイマージリノール酸（フィトステリル／ベヘニル）、ダイマージリノール酸（フィトステリル／イソステアリル／セチル／ステアリル／ベヘニル）、パルミチン酸イソプロピル、マカダミアナッツ脂肪酸フィトステリル、テトラ（ベヘン酸／安息香酸／エチルヘキサン酸）ペンタエリスリチル、パルミチン酸エチルヘキシル、ミリスチン酸ミリスチル、ミリスチン酸イソプロピル、ジピバリン酸トリプロピレングリコール、セバシン酸ジイソプロピル、ネオペンタン酸イソデシル等が例示できる。 Ester oils include pentaerythrityl tetraethylhexanoate, cetyl ethylhexanoate, di(phytosteryl/octyldodecyl) lauroyl glutamate, triisostearin, glyceryl diisostearate, triethylhexanoin, dimer dilinoleic acid (phytosteryl/behenyl), dimer Linoleic acid (phytosteryl/isostearyl/cetyl/stearyl/behenyl), isopropyl palmitate, macadamia nut fatty acid phytosteryl, tetra (behenate/benzoate/ethylhexanoate) pentaerythrityl, ethylhexyl palmitate, myristyl myristate, myristic acid Examples include isopropyl, tripropylene glycol dipivalate, diisopropyl sebacate, and isodecyl neopentanoate.
　水性成分は、化粧料分野において用いられる水性成分であれば特に限定されるものでなく、水はもちろん、例えば、エタノール、プロパノール、イソプロピルアルコール、ブタノール等の低級アルコールのほか、保湿剤、水溶性高分子、紫外線吸収剤、金属イオン封鎖剤、酸化防止剤、薬剤等の一般に化粧料の水相成分として配合される成分を挙げることができる。 The aqueous component is not particularly limited as long as it is an aqueous component used in the field of cosmetics, and water, as well as lower alcohols such as ethanol, propanol, isopropyl alcohol and butanol, as well as moisturizing agents and highly water-soluble Ingredients such as molecules, ultraviolet absorbers, sequestering agents, antioxidants, drugs, and the like, which are generally blended as aqueous phase components of cosmetics, can be mentioned.
＜油中水型乳化化粧料＞
　本発明に係る油中水型乳化化粧料は、疎水化処理顔料を内水相中に含むため、塗布の際に粉っぽい感触を生じにくく、伸びの良さに優れている。また、疎水化処理顔料が内水相中に分散されていることから、顔料が固形油分等の影響を受けにくく、顔料同士の凝集が発生しにくいため、化粧の均一な仕上がりを実現できる。従って、これらの効果を最大限に実現するには、本発明に係る油中水型乳化化粧料が、外油相中に粉末を実質的に含まないことが好ましく、さらに言えば、外油相中に粉末を全く含まないことがより好ましい。 <Water-in-oil emulsified cosmetic>
Since the water-in-oil emulsified cosmetic composition according to the present invention contains a hydrophobized pigment in the internal water phase, it does not easily give a powdery feel when applied and is excellent in spreadability. In addition, since the hydrophobized pigment is dispersed in the internal water phase, the pigment is less likely to be affected by solid oil content, etc., and aggregation of the pigments is less likely to occur, thereby achieving a uniform makeup finish. Therefore, in order to maximize these effects, it is preferable that the water-in-oil emulsified cosmetic composition according to the present invention contains substantially no powder in the external oil phase. More preferably there is no powder in it.
　本発明に係る油中水型乳化化粧料は、内水相、すなわち乳化粒子内に十分な量の顔料を含有できるため、皮膚上の小皺や毛穴等の凹凸を自然にぼかし、目立たなくさせる皮膚の凹凸補正効果に優れていると同時に、塗布時の伸びの良さと化粧の仕上がりの均一性に優れている。このため、リキッドファンデーション、コンシーラー、化粧下地、アイシャドウ、チーク、マスカラ等のメイクアップ化粧料に幅広く応用できる。 The water-in-oil emulsified cosmetic according to the present invention can contain a sufficient amount of pigment in the inner water phase, that is, in the emulsified particles. It has excellent unevenness correction effect, and at the same time, it spreads well when applied and is excellent in uniform finish of makeup. Therefore, it can be widely applied to makeup cosmetics such as liquid foundation, concealer, makeup base, eye shadow, blush, and mascara.
＜製法＞
　本発明に係る油中水型乳化化粧料は、（Ｂ）疎水化処理顔料を内水相中に含むことを特徴とする。内水相に（Ｂ）疎水化処理顔料を分散させるには、先ず、（Ａ）非イオン性界面活性剤と、（Ｂ）疎水化処理顔料と、他の水性成分とを混合し、ビーズミルや高圧ホモジナイザー等で処理することにより、（Ｂ）疎水化処理顔料が水性成分に分散した水性分散物を調製する必要がある。 <Manufacturing method>
The water-in-oil emulsified cosmetic according to the present invention is characterized by containing (B) a hydrophobized pigment in the internal water phase. In order to disperse (B) the hydrophobized pigment in the internal water phase, first, (A) the nonionic surfactant, (B) the hydrophobized pigment, and other aqueous components are mixed, followed by a bead mill or the like. It is necessary to prepare an aqueous dispersion in which the (B) hydrophobized pigment is dispersed in an aqueous component by treatment with a high-pressure homogenizer or the like.
　水性成分中で（Ａ）非イオン性界面活性剤と（Ｂ）疎水化処理顔料とを混合することにより、（Ｂ）疎水化処理顔料の粒子表面に（Ａ）非イオン性界面活性剤の親油基が吸着し親水基が外側に向くため、（Ｂ）疎水化処理顔料を水性成分に馴染ませ、均一に分散させることができる。これにより、水性分散物中に（Ｂ）疎水化処理顔料が微細な粒子のまま安定に分散するため、ニュートン流動性が高い水性分散物を得ることができる。 By mixing (A) a nonionic surfactant and (B) a hydrophobized pigment in an aqueous component, the hydrophilicity of (A) the nonionic surfactant is applied to the particle surface of the (B) hydrophobized pigment. Since the oil group is adsorbed and the hydrophilic group faces outward, the (B) hydrophobized pigment can be blended with the aqueous component and dispersed uniformly. As a result, the hydrophobized pigment (B) is stably dispersed in the aqueous dispersion as fine particles, so that an aqueous dispersion with high Newtonian fluidity can be obtained.
　なお、（Ｂ）疎水化処理顔料は、全水相成分に対する比率が５０質量％以下であることが好ましく、より好ましくは４５質量％以下、さらに好ましくは４０質量％以下である。ここで、「全水相成分」とは、（Ａ）非イオン性界面活性剤、（Ｂ）疎水化処理顔料のほか、水溶性の紫外線吸収剤、保湿剤等の水相を構成するあらゆる成分を含む。この比率（（Ｂ）疎水化処理顔料／全水相成分）が５０質量％以下であれば、分散安定性に非常に優れた水性分散物を得ることができ好ましい。 The ratio of (B) the hydrophobized pigment to the total water phase component is preferably 50% by mass or less, more preferably 45% by mass or less, and even more preferably 40% by mass or less. Here, the "total aqueous phase components" include (A) nonionic surfactants, (B) hydrophobized pigments, water-soluble ultraviolet absorbers, moisturizing agents, and other components that make up the aqueous phase. including. If this ratio ((B) hydrophobized pigment/total aqueous phase component) is 50% by mass or less, an aqueous dispersion having extremely excellent dispersion stability can be obtained, which is preferable.
　次いで、得られた水性分散物を、（Ｃ）シリコーン系乳化剤、（Ｄ）シリコーン油、及び、他の油性成分を混合して得られた油相混合物中に、一般的な油中水型乳化化粧料の製法と同様の方法で乳化させればよい。 Next, the resulting aqueous dispersion is added to an oil phase mixture obtained by mixing (C) a silicone emulsifier, (D) a silicone oil, and other oily components, and a general water-in-oil emulsification It may be emulsified by a method similar to the manufacturing method of cosmetics.
　具体的な製造方法としては、以下の工程（１）～（３）：
（１）（Ａ）ＨＬＢが９以上の非イオン性界面活性剤、（Ｂ）疎水化処理顔料、及び、水性成分を混合して、（Ｂ）疎水化処理顔料が水性成分に分散した水性分散物を調製する工程、
（２）（Ｃ）シリコーン系乳化剤、（Ｄ）シリコーン油、及び、油性成分を混合して油相混合物を調製する工程、
（３）工程（２）で得られた油相混合物に工程（１）で得られた水性分散物を添加して乳化させる工程
を含む。 As a specific manufacturing method, the following steps (1) to (3):
(1) Aqueous dispersion in which (A) a nonionic surfactant having an HLB of 9 or more, (B) a hydrophobized pigment, and an aqueous component are mixed, and (B) the hydrophobized pigment is dispersed in the aqueous component preparing a product,
(2) a step of mixing (C) a silicone emulsifier, (D) a silicone oil, and an oily component to prepare an oil phase mixture;
(3) A step of adding the aqueous dispersion obtained in step (1) to the oil phase mixture obtained in step (2) for emulsification.
　以下に実施例を挙げて本発明をさらに詳述するが、本発明はこれらにより何ら限定されるものではない。配合量は特記しない限り、油中水型乳化化粧料の全量に対する質量％で示す。 The present invention will be described in more detail below with reference to examples, but the present invention is not limited by these. Unless otherwise specified, the blending amount is shown in % by mass with respect to the total amount of the water-in-oil emulsified cosmetic.
＜試料１～２２＞
　種々のタイプの非イオン性界面活性剤を用いて、疎水化処理顔料を水性成分に分散させた水性分散物を調製した。以下の方法で分散性を調べ、非イオン性界面活性剤による分散性を評価した。 <Samples 1 to 22>
Various types of nonionic surfactants were used to prepare aqueous dispersions of hydrophobized pigments dispersed in an aqueous component. Dispersibility was examined by the following method, and dispersibility with a nonionic surfactant was evaluated.
（１）分散性
　各試料の水性分散物のレオロジー特性をコーンプレート型レオメータで測定し、せん断速度とせん断応力との関係を調べた。
［分散性の評価基準］
Ａ：ニュートン流動（せん断応力とせん断速度の間に比例関係があり、粘性はせん断速度によらず一定）を示した
Ｂ：シアシニング（せん断速度が高いほど粘性が下がる）を示した
Ｃ：疎水化処理顔料が水相へ湿潤できず、分散できなかった (1) Dispersibility The rheological properties of the aqueous dispersion of each sample were measured with a cone-plate rheometer to investigate the relationship between shear rate and shear stress.
[Evaluation Criteria for Dispersibility]
A: Newtonian flow (there is a proportional relationship between the shear stress and the shear rate, and the viscosity is constant regardless of the shear rate) B: Shear thinning (the higher the shear rate, the lower the viscosity) C: Hydrophobization The treated pigment could not wet into the water phase and could not be dispersed
Figure JPOXMLDOC01-appb-T000001
 ＊１　ラウロイルグルタミン酸Ｎａ／リシン／塩化Ｍｇ処理酸化チタン
Figure JPOXMLDOC01-appb-T000001
 *1 Na lauroyl glutamate/lysine/Mg chloride treated titanium oxide
Figure JPOXMLDOC01-appb-T000002
 ＊１　ラウロイルグルタミン酸Ｎａ／リシン／塩化Ｍｇ処理酸化チタン
Figure JPOXMLDOC01-appb-T000002
 *1 Na lauroyl glutamate/lysine/Mg chloride treated titanium oxide
　試料１は、疎水化処理顔料が水相へ湿潤できず、十分に分散できなかった。
　試料２、４、５、７は、シアシニングが観察された。これは、流れによって疎水化処理顔料間の凝集がほぐれたことが原因と考えられる。すなわち、これらも疎水化処理顔料が十分に水に濡れず、均一に分散されなかった。
　試料３、６、８～２２は、ニュートン流動が観察された。これにより、疎水化処理顔料が十分に水に濡れ、水性成分に均一に分散されていることがわかった。
　以上から、非イオン性界面活性剤としてＨＬＢが９以上のものを用いれば、いずれの場合も疎水化処理顔料を水性成分に安定かつ良好に分散できた。 In sample 1, the hydrophobized pigment could not be wetted into the water phase and could not be sufficiently dispersed.
Shear thinning was observed in samples 2, 4, 5 and 7. The reason for this is considered to be that the aggregation between the hydrophobized pigments was loosened by the flow. That is, the hydrophobized pigment was not sufficiently wetted with water and was not evenly dispersed.
Newtonian flow was observed in samples 3, 6, 8-22. As a result, it was found that the hydrophobized pigment was sufficiently wetted with water and uniformly dispersed in the aqueous component.
As described above, when a nonionic surfactant having an HLB of 9 or more was used, the hydrophobized pigment could be stably and well dispersed in the aqueous component in any case.
＜試料２３～２５＞
　疎水化処理方法の異なる顔料を水性成分に分散させた水性分散物を調製し、分散性を評価した。 <Samples 23 to 25>
Aqueous dispersions were prepared by dispersing pigments with different hydrophobic treatment methods in an aqueous component, and dispersibility was evaluated.
Figure JPOXMLDOC01-appb-T000003
 ＊１　ラウロイルグルタミン酸Ｎａ／リシン／塩化Ｍｇ処理酸化チタン
＊２　トリエトキシカプリリルシラン処理酸化チタン
＊３　テトラヒドロテトラメチルシクロテトラシロキサン処理酸化チタン
Figure JPOXMLDOC01-appb-T000003
 *1 Na lauroyl glutamate/lysine/Mg chloride-treated titanium oxide *2 Triethoxycaprylylsilane-treated titanium oxide *3 Tetrahydrotetramethylcyclotetrasiloxane-treated titanium oxide
　ＨＬＢが１６．５である非イオン性界面活性剤を用いることにより、表面処理方法によらずいずれの疎水化処理顔料も良好に分散することができた（試料２３～２５）。 By using a nonionic surfactant with an HLB of 16.5, any hydrophobized pigment could be well dispersed regardless of the surface treatment method (Samples 23 to 25).
＜実施例１～２及び比較例１～８＞
　種々の乳化剤を用いて油中水型乳化化粧料を調製し、以下の方法で乳化安定性を評価した。また、使用した乳化剤の粘度を以下の方法で調べた。 <Examples 1-2 and Comparative Examples 1-8>
Water-in-oil emulsified cosmetics were prepared using various emulsifiers, and the emulsion stability was evaluated by the following method. Also, the viscosity of the emulsifier used was examined by the following method.
（１）乳化安定性
　調製した油中水型乳化化粧料を５０℃の恒温槽に１カ月保管した後、疎水化処理顔料の分散状況を光学顕微鏡で観察し、以下の基準で評価した。
［乳化安定性の評価基準］
Ａ：疎水化処理顔料が内水相中に分散
Ｂ：疎水化処理顔料が内水相と外油相の両方に分散
Ｃ：疎水化処理顔料が外油相に分散 (1) Emulsion stability After storing the prepared water-in-oil emulsified cosmetic in a constant temperature bath at 50°C for one month, the state of dispersion of the hydrophobized pigment was observed with an optical microscope and evaluated according to the following criteria.
[Evaluation Criteria for Emulsion Stability]
A: Hydrophobized pigment dispersed in internal water phase B: Hydrophobized pigment dispersed in both internal water phase and external oil phase C: Hydrophobized pigment dispersed in external oil phase
（２）乳化剤の粘度
　乳化剤をシクロペンタシロキサン中に５０質量％となるように溶解させた溶液の２５℃における粘度を、Ｂ型粘度計を用いてローターＮｏ．１、回転数１２ｒｐｍ、１分間の条件で測定した。 (2) Viscosity of Emulsifier The viscosity at 25° C. of a solution obtained by dissolving 50% by mass of an emulsifier in cyclopentasiloxane was measured using a Brookfield viscometer. 1. Measured under conditions of 12 rpm for 1 minute.
Figure JPOXMLDOC01-appb-T000004
 ＊１　ラウロイルグルタミン酸Ｎａ／リシン／塩化Ｍｇ処理酸化チタン
Figure JPOXMLDOC01-appb-T000004
 *1 Na lauroyl glutamate/lysine/Mg chloride treated titanium oxide
Figure JPOXMLDOC01-appb-T000005
 ＊１　ラウロイルグルタミン酸Ｎａ／リシン／塩化Ｍｇ処理酸化チタン
Figure JPOXMLDOC01-appb-T000005
 *1 Na lauroyl glutamate/lysine/Mg chloride treated titanium oxide
　水性分散物を油性成分に分散させる乳化剤として、乳化剤の粘度が３００ｍＰａ・ｓ以上を示すシリコーン系乳化剤を用いた場合には、乳化粒子が壊れることなく、疎水化処理顔料を内水相に閉じ込めたまま安定に分散させることができた（実施例１、２）。なお、使用する乳化剤のＨＬＢは乳化安定性に直接影響しないことが認められた。
　一方、シリコーン系乳化剤であっても、乳化剤の粘度が３００ｍＰａ・ｓ未満のものを用いた場合には、一部の乳化粒子が壊れて疎水化処理顔料が外油相に流出し、その結果、疎水化処理顔料が内水相と外油相の両方に分散していた（比較例１～３）。
　また、炭化水素系乳化剤を用いた場合には、乳化粒子が壊れ、疎水化処理顔料が外油相に流出してしまった（比較例４～８）。 When a silicone-based emulsifier exhibiting a viscosity of 300 mPa·s or more is used as the emulsifier for dispersing the aqueous dispersion in the oily component, the emulsified particles are not broken, and the hydrophobized pigment is confined in the internal water phase. It was possible to disperse stably as it was (Examples 1 and 2). It was found that the HLB of the emulsifier used does not directly affect the emulsion stability.
On the other hand, even if a silicone emulsifier is used, if the viscosity of the emulsifier is less than 300 mPa·s, some of the emulsified particles will break and the hydrophobized pigment will flow out into the external oil phase, resulting in The hydrophobized pigment was dispersed in both the inner water phase and the outer oil phase (Comparative Examples 1 to 3).
Also, when a hydrocarbon emulsifier was used, the emulsified particles were broken, and the hydrophobized pigment flowed out into the external oil phase (Comparative Examples 4 to 8).
＜実施例３～１０及び比較例９～１２＞
　各乳化剤について、疎水化処理顔料の配合量を変更して油中水型乳化化粧料を調製し、乳化安定性を評価した。 <Examples 3 to 10 and Comparative Examples 9 to 12>
For each emulsifier, water-in-oil emulsified cosmetics were prepared by changing the blending amount of the hydrophobized pigment, and the emulsification stability was evaluated.
Figure JPOXMLDOC01-appb-T000006
 ＊１　ラウロイルグルタミン酸Ｎａ／リシン／塩化Ｍｇ処理酸化チタン
Figure JPOXMLDOC01-appb-T000006
 *1 Na lauroyl glutamate/lysine/Mg chloride treated titanium oxide
　乳化剤としてＰＥＧ－１０ジメチコン（乳化剤の粘度＝９８ｍＰａ・ｓ）を用いた場合には、疎水化処理顔料の配合量を少量に抑えても乳化粒子の合一や破壊が見られ、疎水化処理顔料が外油相に流出してしまった（比較例９～１２）。
　一方、乳化剤としてセチルＰＥＧ／ＰＰＧ－１０／１ジメチコン（乳化剤の粘度＝３４４ｍＰａ・ｓ）又はＰＥＧ／ＰＰＧ－１９／１９ジメチコン（乳化剤の粘度＝５１８００ｍＰａ・ｓ）を用いた場合には、疎水化処理顔料の配合量を変更しても、乳化粒子に合一や破壊を引き起こすことなく、疎水化処理顔料を内水相に閉じ込めたまま安定に分散させることができた（実施例３～１０）。 When PEG-10 dimethicone (viscosity of emulsifier = 98 mPa s) was used as an emulsifier, coalescence and destruction of emulsified particles were observed even when the blending amount of the hydrophobized pigment was reduced to a small amount. flowed out into the external oil phase (Comparative Examples 9 to 12).
On the other hand, when cetyl PEG/PPG-10/1 dimethicone (viscosity of emulsifier = 344 mPa s) or PEG/PPG-19/19 dimethicone (viscosity of emulsifier = 51800 mPa s) is used as an emulsifier, hydrophobic treatment Even when the blending amount of the pigment was changed, the emulsified particles did not coalesce or break, and the hydrophobized pigment could be stably dispersed while confined in the inner water phase (Examples 3 to 10).
＜実施例１１～１３及び比較例１３～１４＞
　全液状油分に対するシリコーン油の比率（シリコーン油／全液状油分）を変更して油中水型乳化化粧料を調製し、乳化安定性を評価した。 <Examples 11-13 and Comparative Examples 13-14>
Water-in-oil emulsified cosmetics were prepared by changing the ratio of silicone oil to total liquid oil (silicone oil/total liquid oil), and the emulsion stability was evaluated.
Figure JPOXMLDOC01-appb-T000007
 ＊１　ラウロイルグルタミン酸Ｎａ／リシン／塩化Ｍｇ処理酸化チタン
Figure JPOXMLDOC01-appb-T000007
 *1 Na lauroyl glutamate/lysine/Mg chloride treated titanium oxide
　全液状油分に対するシリコーン油の比率が５０質量％より多い場合には、乳化粒子が壊れることなく、疎水化処理顔料を内水相に閉じ込めたまま安定に分散させることができた（実施例１１～１３）。
　一方、この比率が５０質量％以下の場合には、一部又は全ての乳化粒子が壊れて疎水化処理顔料が外油相に流出してしまった（比較例１３～１４）。 When the ratio of the silicone oil to the total liquid oil content was more than 50% by mass, the emulsified particles did not break, and the hydrophobized pigment could be stably dispersed while confined in the internal water phase (Examples 11- 13).
On the other hand, when this ratio was 50% by mass or less, some or all of the emulsified particles were broken and the hydrophobized pigment flowed out into the external oil phase (Comparative Examples 13 and 14).
＜実施例１４及び比較例１５＞
　内水相に分散させる顔料として、疎水化処理顔料を用いた場合と、親水化処理顔料を用いた場合について、以下の方法で、塗布中の伸びの良さ、化粧の仕上がりの均一さを評価した。 <Example 14 and Comparative Example 15>
As the pigment to be dispersed in the internal water phase, the following methods were used to evaluate the spreadability during application and the uniformity of the makeup finish in the case of using a hydrophobic treatment pigment and the case of using a hydrophilic treatment pigment. .
（１）塗布中の伸びの良さ
　化粧品評価専門パネル１０名に実施例及び比較例の油中水型乳化化粧料を使用してもらい、以下の基準に従って評価した。
Ａ：８人以上のパネルが、伸びが良いと判断した
Ｂ：５人～７人のパネルが、伸びが良いと判断した
Ｃ：２人～４人のパネルが、伸びが良いと判断した
Ｄ：１人以下のパネルが、伸びが良いと判断した (1) Good spreadability during application A panel of 10 cosmetic evaluation specialists used the water-in-oil emulsified cosmetics of Examples and Comparative Examples, and evaluated them according to the following criteria.
A: A panel of 8 or more people judged that the growth was good B: A panel of 5 to 7 people judged that the growth was good C: A panel of 2 to 4 people judged that the growth was good D : Less than 1 panel judged that growth was good
（２）化粧の仕上がりの均一さ
　化粧品評価専門パネル１０名に実施例及び比較例の油中水型乳化化粧料を使用してもらい、以下の基準に従って評価した。
Ａ：８人以上のパネルが、仕上がりが均一であると判断した
Ｂ：５人～７人のパネルが、仕上がりが均一であると判断した
Ｃ：２人～４人のパネルが、仕上がりが均一であると判断した
Ｄ：１人以下のパネルが、仕上がりが均一であると判断した (2) Uniformity of makeup finish A panel of 10 cosmetic evaluation specialists used the water-in-oil emulsified cosmetics of Examples and Comparative Examples, and evaluated them according to the following criteria.
A: A panel of 8 or more people judged that the finish was uniform B: A panel of 5 to 7 people judged that the finish was uniform C: A panel of 2 to 4 people had a uniform finish D: 1 panel or less judged that the finish was uniform
Figure JPOXMLDOC01-appb-T000008
 ＊１　ラウロイルグルタミン酸Ｎａ／リシン／塩化Ｍｇ処理酸化チタン
＊２　シリカ処理酸化チタン
Figure JPOXMLDOC01-appb-T000008
 *1 Na lauroyl glutamate/lysine/Mg chloride treated titanium oxide *2 Silica treated titanium oxide
　顔料として疎水化処理顔料を用いた場合には、伸びの良さと仕上がりの良さのいずれにも優れていた（実施例１４）。
　一方、親水化処理顔料を用いた場合には、いずれの評価項目も十分な結果を示さなかった（比較例１５）。 When a hydrophobized pigment was used as the pigment, both good spreadability and good finish were obtained (Example 14).
On the other hand, when the hydrophilized pigment was used, none of the evaluation items showed sufficient results (Comparative Example 15).
＜実施例１５及び比較例１６＞
　配合成分及び配合量が同一であって、疎水化処理顔料を内水相に分散させた油中水型乳化化粧料（実施例１５）と、疎水化処理顔料を外油相に分散させた油中水型乳化化粧料（比較例１６）をそれぞれ調製し、塗布中の伸びの良さ、化粧の仕上がりの均一さを評価した。 <Example 15 and Comparative Example 16>
A water-in-oil emulsified cosmetic (Example 15) in which a hydrophobized pigment is dispersed in the inner water phase and an oil in which the hydrophobized pigment is dispersed in the outer oil phase, both of which have the same ingredients and amounts. A medium-water emulsified cosmetic (Comparative Example 16) was prepared, and spreadability during application and uniformity of makeup finish were evaluated.
（実施例１５の製法）
　表９の（１）～（５）成分を８０℃以上で加熱混合して油相混合物を調製した。別途、（６）～（１１）成分を加熱混合し、高圧ホモジナイザーで処理して水性分散物（疎水化処理顔料が水性成分に分散した水性分散物）を調製した。次いで、水性分散物を徐添により油相混合物に加え、ホモミキサー処理により乳化後、冷却し、油中水型乳化化粧料を得た。 (Manufacturing method of Example 15)
An oil phase mixture was prepared by heating and mixing components (1) to (5) in Table 9 at 80° C. or higher. Separately, the components (6) to (11) were heated and mixed and treated with a high-pressure homogenizer to prepare an aqueous dispersion (aqueous dispersion in which a hydrophobized pigment is dispersed in an aqueous component). Next, the aqueous dispersion was gradually added to the oil phase mixture, emulsified by a homomixer treatment, and then cooled to obtain a water-in-oil emulsified cosmetic.
（比較例１６の製法）
　表９の（１）～（５）及び（１０）成分を８０℃以上で加熱混合し、高圧ホモジナイザーで処理して油性分散物（疎水化処理顔料が油性成分に分散した油性分散物）を調製した。別途、（６）～（９）及び（１１）成分を加熱混合して水性混合物を調製した。次いで、水性混合物を徐添により油性分散物に加え、ホモミキサー処理により乳化後、冷却し、油中水型乳化化粧料を得た。 (Manufacturing method of Comparative Example 16)
Components (1) to (5) and (10) in Table 9 were heated and mixed at 80° C. or higher and treated with a high-pressure homogenizer to prepare an oil dispersion (an oil dispersion in which a hydrophobized pigment is dispersed in an oil component). bottom. Separately, components (6) to (9) and (11) were heated and mixed to prepare an aqueous mixture. Next, the aqueous mixture was gradually added to the oily dispersion, emulsified by a homomixer treatment, and cooled to obtain a water-in-oil emulsified cosmetic.
Figure JPOXMLDOC01-appb-T000009
 ＊１　ラウロイルグルタミン酸Ｎａ／リシン／塩化Ｍｇ処理酸化チタン
Figure JPOXMLDOC01-appb-T000009
 *1 Na lauroyl glutamate/lysine/Mg chloride treated titanium oxide
　疎水化処理顔料を内水相に分散させた場合には、伸びの良さと仕上がりの良さのいずれにも優れていた（実施例１５）。
　一方、疎水化処理顔料を外油相に分散させた場合には、いずれの評価項目も十分な結果を示さなかった（比較例１６）。 When the hydrophobized pigment was dispersed in the internal water phase, both good spreadability and good finish were obtained (Example 15).
On the other hand, when the hydrophobized pigment was dispersed in the external oil phase, none of the evaluation items showed satisfactory results (Comparative Example 16).
　以下に、本発明の油中水型乳化化粧料の処方を例示する。本発明はこれらの処方例によって何ら限定されるものではなく、請求の範囲によって特定されるものであることはいうまでもない。なお、配合量は全て油中水型乳化化粧料全量に対する質量％で表す。 The formulation of the water-in-oil emulsified cosmetic of the present invention is exemplified below. It goes without saying that the present invention is not limited at all by these formulation examples, but is specified by the claims. All blending amounts are represented by % by mass relative to the total amount of the water-in-oil emulsified cosmetic.
処方例１：リキッドファンデーション
（成分名）　　　　　　　　　　　　　　　　　　　　配合量（質量％）
（１）ジメチコン　　　　　　　　　　　　　　　　　　　　　１７
（２）ジフェニルシロキシフェニルトリメチコン　　　　　　　１１
（３）ＰＥＧ／ＰＰＧ－１９／１９ジメチコン　　　　　　　　　４
（４）メトキシケイヒ酸エチルヘキシル　　　　　　　　　　　　２．５
（５）ジステアリルジモニウムヘクトライト　　　　　　　　　　１．２
（６）ナイアシンアミド　　　　　　　　　　　　　　　　　　　５
（７）グリセリン　　　　　　　　　　　　　　　　　　　　　　５
（８）ＰＥＧ－６０水添ヒマシ油　　　　　　　　　　　　　　　１
（９）ジプロピレングリコール　　　　　　　　　　　　　　　　８
（１０）フェノキシエタノール　　　　　　　　　　　　　　　　０．５
（１１）（ジメチルアクリルアミド／アクリロイルジメチルタウリンＮａ）クロスポリマー　　　　　　　　　　　　　　　　　　　　　　　　　　　　　０．０５
（１２）疎水化処理顔料　　　　　　　　　　　　　　　　　　１０
（１３）水　　　　　　　　　　　　　　　　　　　　　　　　３４．７５
合計　　　　　　　　　　　　　　　　　　　　　　　　　　１００ Formulation example 1: Liquid foundation (ingredient name) Amount (% by mass)
(1) Dimethicone 17
(2) diphenylsiloxyphenyl trimethicone 11
(3) PEG/PPG-19/19 dimethicone 4
(4) Ethylhexyl methoxycinnamate 2.5
(5) distearyldimonium hectorite 1.2
(6) Niacinamide 5
(7) Glycerin 5
(8) PEG-60 hydrogenated castor oil 1
(9) Dipropylene glycol 8
(10) Phenoxyethanol 0.5
(11) (dimethylacrylamide/acryloyldimethyltaurate Na) crosspolymer 0.05
(12) Hydrophobized pigment 10
(13) Water 34.75
Total 100
処方例２：固形乳化ファンデーション
（成分名）　　　　　　　　　　　　　　　　　　　　配合量（質量％）
（１）ジメチコン　　　　　　　　　　　　　　　　　　　　　３０
（２）セチルＰＥＧ／ＰＰＧ－１０／１ジメチコン　　　　　　　４
（３）メトキシケイヒ酸エチルヘキシル　　　　　　　　　　　　２．５
（４）パラフィンワックス　　　　　　　　　　　　　　　　　　５
（５）マイクロクリスタリンワックス　　　　　　　　　　　　　０．５
（６）ジステアリルジモニウムヘクトライト　　　　　　　　　　１．２
（７）ナイアシンアミド　　　　　　　　　　　　　　　　　　　５
（８）グリセリン　　　　　　　　　　　　　　　　　　　　　　５
（９）ＰＥＧ－６０水添ヒマシ油　　　　　　　　　　　　　　　１
（１０）ジプロピレングリコール　　　　　　　　　　　　　　　８
（１１）フェノキシエタノール　　　　　　　　　　　　　　　　０．５
（１２）（ジメチルアクリルアミド／アクリロイルジメチルタウリンＮａ）クロスポリマー　　　　　　　　　　　　　　　　　　　　　　　　　　　　　０．０５
（１３）疎水化処理顔料　　　　　　　　　　　　　　　　　　１０
（１４）水　　　　　　　　　　　　　　　　　　　　　　　　２７．２５
合計　　　　　　　　　　　　　　　　　　　　　　　　　　１００ Formulation Example 2: Solid emulsified foundation (ingredient name) Blending amount (% by mass)
(1) Dimethicone 30
(2) Cetyl PEG/PPG-10/1 Dimethicone 4
(3) Ethylhexyl methoxycinnamate 2.5
(4) Paraffin wax 5
(5) Microcrystalline wax 0.5
(6) distearyldimonium hectorite 1.2
(7) Niacinamide 5
(8) Glycerin 5
(9) PEG-60 hydrogenated castor oil 1
(10) dipropylene glycol 8
(11) Phenoxyethanol 0.5
(12) (dimethylacrylamide/acryloyldimethyltaurate Na) crosspolymer 0.05
(13) Hydrophobic treatment pigment 10
(14) Water 27.25
Total 100
処方例３：コンシーラー
（成分名）　　　　　　　　　　　　　　　　　　　　配合量（質量％）
（１）ジメチコン　　　　　　　　　　　　　　　　　　　　　２０
（２）セチルＰＥＧ／ＰＰＧ－１０／１ジメチコン　　　　　　　４
（３）メトキシケイヒ酸エチルヘキシル　　　　　　　　　　　　２．５
（４）パラフィンワックス　　　　　　　　　　　　　　　　　　７
（５）マイクロクリスタリンワックス　　　　　　　　　　　　　０．７
（６）ジステアリルジモニウムヘクトライト　　　　　　　　　　１．２
（７）ナイアシンアミド　　　　　　　　　　　　　　　　　　　５
（８）グリセリン　　　　　　　　　　　　　　　　　　　　　　５
（９）ＰＥＧ－６０水添ヒマシ油　　　　　　　　　　　　　　　１
（１０）ジプロピレングリコール　　　　　　　　　　　　　　　５
（１１）フェノキシエタノール　　　　　　　　　　　　　　　　０．５
（１２）（ジメチルアクリルアミド／アクリロイルジメチルタウリンＮａ）クロスポリマー　　　　　　　　　　　　　　　　　　　　　　　　　　　　　０．０５
（１３）疎水化処理顔料　　　　　　　　　　　　　　　　　　２０
（１４）水　　　　　　　　　　　　　　　　　　　　　　　　２８．０５
合計　　　　　　　　　　　　　　　　　　　　　　　　　　１００ Formulation Example 3: Concealer (ingredient name) Amount (% by mass)
(1) Dimethicone 20
(2) Cetyl PEG/PPG-10/1 Dimethicone 4
(3) Ethylhexyl methoxycinnamate 2.5
(4) Paraffin wax 7
(5) Microcrystalline wax 0.7
(6) distearyldimonium hectorite 1.2
(7) Niacinamide 5
(8) Glycerin 5
(9) PEG-60 hydrogenated castor oil 1
(10) Dipropylene glycol 5
(11) Phenoxyethanol 0.5
(12) (dimethylacrylamide/acryloyldimethyltaurate Na) crosspolymer 0.05
(13) Hydrophobic treatment pigment 20
(14) Water 28.05
Total 100

Claims (7)

  1. （Ａ）ＨＬＢが９以上の非イオン性界面活性剤、
    （Ｂ）疎水化処理顔料、
    （Ｃ）シリコーン系乳化剤、及び
    （Ｄ）シリコーン油、
    を含有する油中水型乳化化粧料であって、
    （Ｃ）シリコーン系乳化剤のシクロペンタシロキサンにおける５０質量％溶液の粘度が３００ｍＰａ・ｓ以上であり、
    （Ｄ）シリコーン油が全液状油分の５０質量％より多くを占め、
    かつ
    （Ｂ）疎水化処理顔料が内水相に分散されている、油中水型乳化化粧料。     (A) a nonionic surfactant with an HLB of 9 or more;
    (B) a hydrophobized pigment,
    (C) a silicone emulsifier, and (D) a silicone oil,
    A water-in-oil emulsified cosmetic containing
    (C) a 50% by mass solution of cyclopentasiloxane as a silicone emulsifier has a viscosity of 300 mPa s or more;
    (D) Silicone oil accounts for more than 50% by weight of the total liquid oil,
    and (B) a water-in-oil emulsified cosmetic in which a hydrophobized pigment is dispersed in an internal water phase.
  2. （Ｃ）シリコーン系乳化剤が、ポリエーテル変性シリコーンから選択される、請求項１に記載の油中水型乳化化粧料。 (C) The water-in-oil emulsified cosmetic composition according to claim 1, wherein the silicone emulsifier is selected from polyether-modified silicones.
  3. （Ｃ）シリコーン系乳化剤が、セチルＰＥＧ／ＰＰＧ－１０／１ジメチコン、又は、ＰＥＧ／ＰＰＧ－１９／１９ジメチコンである、請求項２に記載の油中水型乳化化粧料。 (C) The water-in-oil emulsified cosmetic composition according to claim 2, wherein the silicone emulsifier is cetyl PEG/PPG-10/1 dimethicone or PEG/PPG-19/19 dimethicone.
  4. 外油相に粉末を含まない、請求項１に記載の油中水型乳化化粧料。 The water-in-oil emulsified cosmetic according to claim 1, wherein the external oil phase does not contain powder.
  5. （Ｂ）疎水化処理顔料の平均粒子径が２００～１０００ｎｍの範囲である、請求項１に記載の油中水型乳化化粧料。 (B) The water-in-oil emulsified cosmetic composition according to claim 1, wherein the average particle size of the hydrophobized pigment is in the range of 200 to 1000 nm.
  6. （Ｂ）疎水化処理顔料の含有量が油中水型乳化化粧料全量に対して０．０１質量％以上かつ２５質量％以下である、請求項１に記載の油中水型乳化化粧料。 2. The water-in-oil emulsified cosmetic according to claim 1, wherein the content of (B) the hydrophobized pigment is 0.01% by mass or more and 25% by mass or less relative to the total amount of the water-in-oil emulsified cosmetic.
  7. 請求項１～６のいずれか一項に記載の油中水型乳化化粧料の製造方法であって、
    （１）（Ａ）ＨＬＢが９以上の非イオン性界面活性剤、（Ｂ）疎水化処理顔料、及び、水性成分を混合して、（Ｂ）疎水化処理顔料が水性成分に分散した水性分散物を調製する工程、
    （２）（Ｃ）シリコーン系乳化剤、（Ｄ）シリコーン油、及び、油性成分を混合して油相混合物を調製する工程、
    （３）工程（２）で得られた油相混合物に工程（１）で得られた水性分散物を添加して乳化させる工程
    を含む、製造方法。     A method for producing a water-in-oil emulsified cosmetic according to any one of claims 1 to 6,
    (1) Aqueous dispersion in which (A) a nonionic surfactant having an HLB of 9 or more, (B) a hydrophobized pigment, and an aqueous component are mixed, and (B) the hydrophobized pigment is dispersed in the aqueous component preparing a product,
    (2) a step of mixing (C) a silicone emulsifier, (D) a silicone oil, and an oily component to prepare an oil phase mixture;
    (3) A production method comprising a step of adding the aqueous dispersion obtained in step (1) to the oil phase mixture obtained in step (2) to emulsify.
PCT/JP2022/036741 2021-10-14 2022-09-30 Water-in-oil emulsified cosmetic WO2023063116A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2021-168832 2021-10-14
JP2021168832 2021-10-14

Publications (1)

Publication Number Publication Date
WO2023063116A1 true WO2023063116A1 (en) 2023-04-20

Family

ID=85988537

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2022/036741 WO2023063116A1 (en) 2021-10-14 2022-09-30 Water-in-oil emulsified cosmetic

Country Status (1)

Country Link
WO (1) WO2023063116A1 (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004026833A (en) * 2002-06-26 2004-01-29 L'oreal Sa Water in oil emulsion foundation
JP2008208045A (en) * 2007-02-23 2008-09-11 Shiseido Co Ltd Water-in-oil type emulsion composition
JP2019073460A (en) * 2017-10-13 2019-05-16 花王株式会社 Production method of water-in-oil type emulsion cosmetic

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004026833A (en) * 2002-06-26 2004-01-29 L'oreal Sa Water in oil emulsion foundation
JP2008208045A (en) * 2007-02-23 2008-09-11 Shiseido Co Ltd Water-in-oil type emulsion composition
JP2019073460A (en) * 2017-10-13 2019-05-16 花王株式会社 Production method of water-in-oil type emulsion cosmetic

Similar Documents

Publication Publication Date Title
JP5047369B2 (en) Method for producing O / W fine emulsion external preparation
US5015469A (en) Water-in-oil emulsion type cosmetics
JP4853974B2 (en) Self-tanning cosmetics
TWI693945B (en) Water-in-oil emulsion solid cosmetic
JP5394424B2 (en) Solid emulsified cosmetic
WO2011027812A1 (en) Method for producing o/w cream having high viscosity
WO2014010622A1 (en) Water-in-oil emulsion cosmetic
TW201831165A (en) Water-in-oil type cosmetic emulsion preparation
US20100233220A1 (en) Sol Composition Containing Organically Modified Clay Mineral Having Platy Particle Structure, Oily Gel Composition, And W/O Type Emulsion Composition Containing The Same
JP6864898B2 (en) Aqueous composition, its production method, and aqueous cosmetics and emulsified cosmetics containing it.
JPH09165317A (en) Oil-in-water type emulsifying composition
JP2006273747A (en) O/w/o type emulsion cosmetic
JP5228139B2 (en) Oil-in-water emulsified cosmetic
JP4786172B2 (en) Solid powder cosmetic
JP5491688B2 (en) Sol composition containing organically modified clay mineral having plate-like particle structure, oil-based gel composition containing the same, and W / O emulsion composition
WO2023063116A1 (en) Water-in-oil emulsified cosmetic
JP3312371B2 (en) Makeup cosmetics
JP2006241038A (en) Emulsion cosmetic
JP2000063231A (en) Aqueous cosmetic
JP2018199657A (en) Water-in-oil emulsion cosmetic
JPH0892059A (en) Transparent face lotion
WO2023085106A1 (en) Water-in-oil emulsion cosmetic
CN113301964A (en) Cosmetic base containing lecithin and cosmetic containing the same
JP5492373B2 (en) Oily gel composition containing organically modified clay mineral having plate-like particle structure, and W / O type emulsified composition using the same
JPH08259432A (en) Water-in-oil type emulsion preparation

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 22880812

Country of ref document: EP

Kind code of ref document: A1

WWE Wipo information: entry into national phase

Ref document number: 2023554397

Country of ref document: JP