WO2015093324A1 - Powder composition which contains powder composited with lamellar phase, and process for manufacturing same - Google Patents

Powder composition which contains powder composited with lamellar phase, and process for manufacturing same Download PDF

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Publication number
WO2015093324A1
WO2015093324A1 PCT/JP2014/082293 JP2014082293W WO2015093324A1 WO 2015093324 A1 WO2015093324 A1 WO 2015093324A1 JP 2014082293 W JP2014082293 W JP 2014082293W WO 2015093324 A1 WO2015093324 A1 WO 2015093324A1
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powder
powder composition
surfactant
oil
lamellar phase
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PCT/JP2014/082293
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French (fr)
Japanese (ja)
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亘 堀江
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ポーラ化成工業株式会社
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Publication of WO2015093324A1 publication Critical patent/WO2015093324A1/en

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    • 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
    • A61K8/0216Solid or semisolid forms
    • A61K8/022Powders; Compacted Powders
    • 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
    • A61K8/55Phosphorus compounds
    • A61K8/553Phospholipids, e.g. lecithin
    • 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
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10General cosmetic use

Definitions

  • the present invention relates to a powder composition containing a powder in which a lamellar phase is complexed and a method for producing the same.
  • Powder powder is superior in portability and convenience compared to liquid cosmetics, but has a problem that it feels dry to the skin when used.
  • a technique of coating powder with an oil has been taken (for example, Patent Document 1).
  • a lamellar phase in which an aqueous phase and an oil phase are repeatedly overlapped.
  • This lamellar phase has a structure in which lipids, which are amphipathic molecules, are regularly arranged.
  • the water phase retains active ingredients such as lactic acid and amino acids to keep the skin moist.
  • the lamellar phase in the skin has a barrier function to protect the skin from harmful substances in the atmosphere.
  • cosmetics applying the active ingredient holding function, moisturizing function, and barrier function of this lamellar phase have been created.
  • Patent Document 2 discloses a humectant containing a lamellar phase and a sucrose fatty acid ester containing fatty acid monoglyceride as components.
  • Coating the powder with an oil agent is effective in reducing the dry feeling.
  • an oil agent used to improve the moisture retention, there is a problem that stickiness occurs during use. Therefore, there has been a demand for a technique for improving the moisturizing property of the powder cosmetic by a separate method other than increasing the amount of oil used. That is, the problem to be solved by the present invention is to provide a powder composition excellent in moisturizing property that does not cause dryness and stickiness during use.
  • the powder composing such a powder composition has excellent moisturizing properties because the surface has a lamellar phase.
  • “composite” means not only a state in which the entire surface of the powder base material is coated with a lamellar phase, but also a state in which the lamellar phase is partially adhered. Further, in this specification, the powder composition refers to a mixed composition of powder and other components.
  • the oil agent is selected from silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.
  • the powder composition contains water. Since the lamellar phase can retain moisture in the hydrophilic layer, by combining it with the powder base material in the oil agent, moisture and oil can coexist and the dry feeling during use is suppressed. Can moisturize the skin.
  • the powder composition contains water as described above, a water-soluble active ingredient may be included.
  • the hydrophilic active ingredient is taken into the layer in which the water in the lamellar phase is retained.
  • a powder composition becomes the outstanding thing which exhibits the effect which the active ingredient has other than moisture retention.
  • the powder composition of the present invention having such a form can enhance the effect of the active ingredient by efficiently infiltrating the active ingredient into the stratum corneum.
  • the surfactant is not particularly limited.
  • lecithin and / or a nonionic surfactant are preferably mentioned. Since the lamellar phase composed of these oil agents is more stable, it is possible to provide a powder cosmetic that maintains high moisture retention for a long time.
  • the present invention also relates to an external preparation for skin containing a powder composition.
  • Such an external preparation for skin has excellent moisturizing properties and can retain a water-soluble active ingredient in the lamellar phase, and therefore has an excellent skin care effect.
  • the present invention also relates to a method for producing the above powder composition, characterized in that a lamellar phase mainly composed of a surfactant in an oil agent is compounded on the surface of a powder base material. According to the production method of the present invention, the powder composition of the present invention can be produced.
  • the manufacturing method of the powder composition of this invention includes the process of mixing an oil agent, surfactant, and a powder base material. According to this form, the powder composition of the present invention can be produced efficiently.
  • the process which mixes an oil agent and surfactant and obtains a lamella phase dispersion solution and the process which mixes the said lamella phase dispersion solution and a powder base material are included.
  • the powder base material of the present invention can be produced efficiently and simply.
  • the manufacturing method of the present invention in this form is referred to as a dry manufacturing method.
  • the production method of the present invention comprises a step of mixing an oil agent, a surfactant, a volatile solvent, and a powder base material to obtain an intermediate powder composition; Volatilizing the volatile solvent in the intermediate powder composition.
  • the powder composition of the present invention including a powder base material in which lamella phases are uniformly combined can be efficiently and simply manufactured.
  • the manufacturing method of the present invention in this form is referred to as a wet manufacturing method.
  • a solvent selected from alcohols, hydrocarbons, aromatics, ketones, ethers, esters, volatile silicone oils, and isoparaffins as the volatile solvent.
  • the volatile solvent is volatilized under reduced pressure. By carrying out like this, a volatile solvent can be volatilized efficiently.
  • the present invention also relates to a method for producing an external preparation for skin, which comprises a step of mixing the powder composition produced by the production method of the present invention described above with other components.
  • the present invention is a method for producing a powder composition
  • a powder composition comprising a powder base material having a lamella phase mainly composed of a surfactant on the surface, wherein the surfactant is mainly contained in the oil.
  • the present invention also relates to a method for producing a powder composition, characterized in that a lamellar phase is combined with the surface of a powder substrate.
  • a volatile oil agent may be used as the oil agent.
  • a powder composition containing no oil agent can be produced by volatilizing the oil agent.
  • the powder composition of the present invention Since the powder base material is complexed with the lamellar phase, the powder composition of the present invention has the ability to retain moisture even in the oil, and can also retain water-soluble active ingredients at the same time. Moreover, if the powder composition of this invention is used, the skin external preparation excellent in moisture retention can be provided.
  • the powder composition of the present invention includes an oil agent, a surfactant, and a powder base material, and a lamellar phase mainly composed of the surfactant is compounded on the surface of the powder base material. It is characterized by.
  • each component which comprises this composition is demonstrated.
  • Oil Agent in the powder composition of the present invention can be mixed with a powder base material and a surfactant, and a lamellar phase mainly composed of a surfactant is formed in the continuous phase.
  • a powder base material and a surfactant there is no particular limitation as long as it can be used.
  • preferred examples of the oil include silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.
  • silicone oil examples include organopolysiloxanes such as dimethylpolysiloxane, methylphenylpolysiloxane, dimethylsiloxane / methylphenylsiloxane copolymer, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, etc.
  • organopolysiloxanes such as dimethylpolysiloxane, methylphenylpolysiloxane, dimethylsiloxane / methylphenylsiloxane copolymer, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, etc.
  • examples thereof include cyclic siloxane. Among these, the cyclic siloxane described above is preferably used.
  • Hydrocarbon oils include chain and cyclic hydrocarbons such as ⁇ -olefin oligomers, light isoparaffins, light liquid isoparaffins, squalane, liquid paraffin, liquid isoparaffins, hydrogenated isobutene, isooctane, decane, isododecane, isohexadecane, Polybutene etc. are mentioned.
  • Ester oils include dioctyl succinate, diisobutyl adipate, dioctyl adipate, di (2-heptylundecyl) adipate, diisopropyl sebacate, dioctyl sebacate, dibutyl octyl sebacate, diisostearyl malate, triethyl citrate , Ethylene glycol dioctanoate, neopentyl glycol dioctanoate, propylene glycol dicaprate, neopentyl glycol dicaprate, trimethylolpropane trioctanoate, trimethylolpropane triisostearate, pentaerythritol tetraoleate, ethyl acetate, butyl acetate, amyl acetate Octyldodecyl neopentanoate, cetyl ethylhexano
  • Natural animal and vegetable oils include avocado oil, almond oil, olive oil, wheat germ oil, safflower oil, jojoba oil, macadamia nut oil, cottonseed oil, coconut oil, and the like.
  • Fluorine oil includes perfluoro oils.
  • the powder composition of the present invention is produced by preparing a lamellar phase dispersion solution containing lecithin as a surfactant by the method described in the item ⁇ Preparation Method 1 of ⁇ 3-1-1> Lamellar Phase Dispersion Solution> described later.
  • an oil agent that is liquid at 25 ° C. with a molecular weight of greater than 114 g / mol.
  • the surfactant in the present invention is not particularly limited as long as it is an amphiphilic substance, and either an ionic surfactant or a nonionic surfactant can be used.
  • an ionic surfactant or a nonionic surfactant can be used.
  • lecithin which is an amphoteric surfactant is used.
  • Nonionic surfactants can also be preferably used.
  • silicone surfactants, polyoxyethylene alkyl ethers, sucrose fatty acid esters, sphingosines, fatty acids and the like can be preferably used.
  • Lecithin extracted from living bodies of plants, animals and microorganisms and purified as desired may be used, or synthesized.
  • plant-derived lecithin such as soybean, corn, peanut, rapeseed, and wheat
  • animal-derived lecithin such as egg yolk
  • the lecithin in the present invention includes phosphatidylcholine, phosphatidic acid, phosphatidylglycerol, phosphatidylinositol, phosphatidylethanolamine, phosphatidylmethylethanolamine, phosphatidylserine, bisphosphatidic acid, diphosphatidylglycerol (cardiolipin) and the like.
  • “lecithin” also includes hydrogenated lecithin, enzymatically decomposed lecithin, enzymatically decomposed hydrogenated lecithin, lysolecithin and the like.
  • the number of carbon atoms of the fatty acid constituting the hydrophobic group portion of lecithin is not particularly limited, and for example, those having 8 to 20 carbon atoms, preferably 16 to 18 carbon atoms can be mainly used.
  • the fatty acid may be saturated or unsaturated.
  • the fatty acid may be linear or branched.
  • lecithin can be used in the form of a single kind of the above-mentioned compound or in the form of a mixture of the above-mentioned plural kinds of phospholipids.
  • the composition of lecithin is preferably composed mainly of phosphatidylcholine, for example, 20% by mass or more, and preferably 50% by mass or more is phosphatidylcholine.
  • a commercially available lecithin can be used.
  • the following commercially available products can be used.
  • Resinol S-10 Nikko Chemicals (hydrogenated: ⁇ , PC (phosphatidylcholine) content: 25-30%)
  • Resinol S-10E Nikko Chemicals (hydrogenated: ⁇ , PC content: 75-85%)
  • Resinol S-10EX Nikko Chemicals (hydrogenated: ⁇ , PC content:> 95%)
  • Basis LP-20H Nisshin Oilio Co., Ltd.
  • lecithin When lecithin is mainly used, it can be combined with other auxiliary surfactants (nonionic surfactants, ionic surfactants). In this case, it is preferable that lecithin accounts for 60% by mass or more, more preferably 80% by mass or more of the surfactant forming the lamellar phase.
  • a silicone surfactant may be used as the surfactant in the present invention.
  • the silicone surfactant is a surfactant having a polyorganosiloxane (silicone chain) in a hydrophobic group.
  • the hydrophilic group is preferably selected from polyether or polyglycerin.
  • Preferred examples of the polyether include polyoxyethylene, polyoxypropylene, and oxyethylene / oxypropylene copolymers.
  • the average degree of polymerization of polyoxyethylene or polyoxypropylene, oxyethylene / oxypropylene copolymer, and polyglycerin is, for example, about 8 to 15.
  • the polyorganosiloxane may be linear or branched. A plurality of polyorganosiloxane chains may be cross-linked.
  • the silicone chain may be modified with an alkyl group.
  • the HLB of the silicone surfactant is preferably 3 to 13, more preferably 6 to 10.
  • the silicone surfactant is soluble or dispersible in the oil agent. Moreover, it is preferable that it is a liquid at room temperature.
  • the silicone surfactant can be used in the form of a single kind of the above compound, or in the form of a mixture of plural kinds.
  • silicone surfactants are known as cosmetic raw materials, and any of them can be used.
  • Commercially available silicone surfactants can be used.
  • the following commercially available products can be used.
  • ⁇ SH3772M PEG-12 dimethicone (polyoxyethylene type), HLB: 6, Toray Dow Corning)
  • SH3773M PEG-12 dimethicone (polyoxyethylene type), HLB: 8, Toray Dow Corning
  • FZ2222 Polysilicone-13 (oxyethylene / oxypropylene type), HLB: 6, Toray Dow Corning
  • KF6013 PEG-9 dimethicone ((polyoxyethylene type)
  • HLB 10, Shin-Etsu Silicone
  • KF6100 polyglyceryl 3 disiloxane dimethicone (polyglycerin), Shin-Etsu Silicone
  • Powder base material The powder base material in the present invention is not particularly limited as long as it is used as a powder for cosmetics. Even if the powder surface is hydrophilic, it is hydrophobic. May be sex.
  • the powder base material in the present invention for example, mica, talc, kaolin, synthetic mica, calcium carbonate, magnesium carbonate, anhydrous silicic acid (silica), aluminum oxide, barium sulfate, etc.
  • surface may be treated Powders; surface may be treated, bengara, yellow iron oxide, black iron oxide, cobalt oxide, ultramarine, bitumen, titanium oxide, zinc oxide inorganic pigments; surface may be treated, mica Pearls such as titanium, fish phosphorus foil, bismuth oxychloride; red 202, red 228, red 226, yellow 4, blue 404, yellow 5, red 505, which may be raked, Organic pigments such as red 230, red 223, orange 201, red 213, yellow 204, yellow 203, blue 1, blue 201, green 201, purple 201, red 204; Riechiren powder, can be used polymethyl methacrylate, nylon powder, organic powders such as organopolysiloxane elastomers. It is also possible to use a mixed powder containing two or more of the above powders.
  • the powder composition of the present invention may contain water.
  • the content of water in the whole powder composition is preferably 10% by mass or less, more preferably 0.05 to 5% by mass, and further preferably 0.1 to 1% by mass.
  • the weight ratio of water to the surfactant in the powder composition is preferably 1: 1 to 1:20, more preferably 1: 2 to 1:10, and even more preferably 1: 3 to 1: 5. is there.
  • Water-soluble active ingredient As described above, when water is contained in the powder composition of the present invention, a water-soluble active ingredient can be contained at the same time. That is, the layer in which water in the lamellar phase is retained can be in a form containing a hydrophilic active ingredient. By setting it as such a form, the effect which an active ingredient has can be heightened by making an active ingredient penetrate
  • Incorporation of the hydrophilic active ingredient into the layer in which water in the lamella phase is retained can be carried out by a method usually used in the cosmetics and pharmaceutical fields. That is, the active ingredient is dissolved in water to prepare an aqueous solution of the active ingredient. By stirring and mixing the aqueous solution and the surfactant, a dispersion solution of a lamellar phase containing an active ingredient in a layer in which moisture is retained can be obtained. And the powder composition which the lamellar phase which contains an active ingredient in the layer by which the water
  • maintained can be obtained by the dry manufacturing method or wet manufacturing method mentioned later using this dispersion solution.
  • the water-soluble active ingredient to be contained in the layer in which the water in the lamella phase is retained is not particularly limited as long as it is used for an external preparation for skin.
  • tranexamic acid, glycyrrhizic acid and its salt ascorbine Ascorbic acids such as acid, ascorbic acid phosphate ester, 3-O-ethylascorbic acid, ascorbic acid glucoside or salts thereof, ursolates such as arbutin and potassium ursolate phosphate, pyridoxine, riboflavin or salts thereof
  • Preferred examples include vitamin B, hyaluronic acid and salts thereof, fucoidan, sulfated trehalose or salts thereof, trehalose, amino acids and amino acid derivatives, esculetin glycosides, liquid or solid plant extracts, and the like.
  • dipotassium glycyrrhizinate, 2-glucoside ascorbic acid, and tranexamic acid can be remarkably improved in the penetration efficiency into the stratum corneum by being contained in a layer in which water in the lamellar phase is retained.
  • External preparation for skin also relates to an external preparation for skin containing the powder composition.
  • the external preparation for skin of the present invention may contain any commonly used optional component as long as the effects of the present invention are not impaired.
  • optional ingredients include macadamia nut oil, avocado oil, corn oil, olive oil, rapeseed oil, sesame oil, castor oil, safflower oil, cottonseed oil, jojoba oil, coconut oil, palm oil, liquid lanolin, and hardened coconut oil.
  • sorbitan fatty acid esters such as sorbitan monostearate and sorbitan sesquioleate
  • glycerin fatty acids such as glyceryl monostearate
  • propylene glycol fatty acid esters (monostearic acid) Propylene glycol, etc.)
  • hardened castor oil derivative glycerin alkyl ether
  • POE sorbitan fatty acid esters POE sorbitan monooleate, polyoxyethylene sorbitan monostearate, etc.
  • POE sorbite fatty acid esters POE-sorbite monolaurate, etc.
  • POE glycerol fatty acid esters POE-glycerol monoisostearate, etc.
  • POE fatty acid esters polyethylene glycol monooleate, POE distearate, etc.
  • POE alkyl ethers POE2-octyldodecyl ether, etc.
  • the external preparation for skin of the present invention can contain a powder having no lamellar phase adhering to the surface as long as the effects of the present invention are not impaired.
  • a powder base material may have a surface-treated powder such as mica, talc, kaolin, synthetic mica, calcium carbonate, magnesium carbonate, anhydrous silicic acid (silica), aluminum oxide, barium sulfate, etc.
  • the surface may be treated, inorganic pigments such as bengara, yellow iron oxide, black iron oxide, cobalt oxide, ultramarine, bitumen, titanium oxide, zinc oxide; the surface may be treated, mica titanium, Pearl agents such as fish phosphorus foil, bismuth oxychloride; red 202, red 228, red 226, yellow 4, blue 404, yellow 5, red 505, red 230 which may be raked No., Red No. 223, Orange No. 201, Red No. 213, Yellow No. 204, Yellow No. 203, Blue No. 1, Green No. 201, Purple No. 201, Red No. 204, etc .; , Polymethyl methacrylate, nylon powder, organic powders such as organopolysiloxane elastomers and the like can be preferably exemplified.
  • inorganic pigments such as bengara, yellow iron oxide, black iron oxide, cobalt oxide, ultramarine, bitumen, titanium oxide, zinc oxide
  • the surface may be treated, mica titanium
  • the manufacturing method of the powder composition of the present invention is characterized in that a lamellar phase mainly containing a surfactant is compounded on the surface of a powder base material in an oil agent. And in the preferable form of this invention, the process of mixing an oil agent, surfactant, and a powder base material is included.
  • a dry manufacturing method and a wet manufacturing method according to the method for manufacturing a powder composition of the present invention will be described in detail.
  • the dry manufacturing method of the powder composition of the present invention includes a step of mixing an oil agent and a surfactant to obtain a lamellar phase dispersion solution, and a mixing of the lamellar phase dispersion solution and the powder base material. Including the step of:
  • the oil agent and surfactant in this production method those described in the above items ⁇ 1-1> to ⁇ 1-2> can be used.
  • the powder base material in the present production method the powder described in the above item ⁇ 1-3> can be used, and a composite powder containing two or more kinds of such powders may be used.
  • ⁇ 3-1-1> (1) to (3) describe the method for preparing the lamella phase dispersion solution
  • ⁇ 3-1-2> describe the step of mixing the lamella phase dispersion solution and the powder base material.
  • ⁇ 3-1-1> Preparation Method of Lamellar Phase Dispersion Solution
  • Preparation Method 1 of Lamellar Phase Dispersion Solution The step of mixing an oil agent and a surfactant to obtain a lamellar phase dispersion solution is performed by preparing a mixture by mixing the above-described surfactant, oil agent, and water as required, and then shaking or stirring the mixture. It can be carried out. Shaking can be performed using a shaker or the like. Stirring can be performed using an ultrasonic disperser or the like.
  • the step of obtaining a lamellar phase dispersion solution comprises dissolving a surfactant in a volatile solvent to obtain a first isotropic solution, mixing the first isotropic solution with an oil agent, 2 is a step of obtaining an isotropic solution, a step of volatilizing the volatile solvent in the second isotropic solution, and volatilization of the volatile solvent.
  • the volatile solvent in this case, those described in detail in the following ⁇ Wet production method> can be used.
  • the preparation method 2 of the lamellar phase dispersion solution will be described with reference to FIG.
  • the content of the surfactant in the first isotropic solution may be in a range where the surfactant is sufficiently dissolved.
  • the content of the surfactant can be 10 to 90% by mass. This is because when the amount is less than 10% by mass, the volatilization time of the volatile solvent may become long, and when it exceeds 90% by mass, the solution becomes viscous and may be difficult to dissolve.
  • the first isotropic solution may contain water. Since the preparation of a lamellar phase dispersion solution by volatilization of a volatile solvent is intended to form a lamellar phase regardless of conventional physical stirring, the presence of water is necessary for the purpose of assisting dispersion by physical stirring. Rather, it can be said that it is useful in a system with little water. However, in the preparation of a lamellar phase dispersion solution by volatilization of the volatile solvent, the presence of water may assist the formation of the lamellar phase. From these viewpoints, the present invention may contain water having a mass of 1 or less that of the surfactant. In this case, the surfactant can be mixed with water and mixed with a volatile solvent (FIG. 1 (a)). Of course, you may mix surfactant, water, and a volatile solvent.
  • the surfactant 1 is dissolved in the volatile solvent 2 to prepare a first isotropic solution 3.
  • This preparation can be performed by ordinary mixing and stirring.
  • the first isotropic solution 3 obtained by dissolving the surfactant 1 in the volatile solvent 2 is a state in which the surfactant 1 is monodispersed in the volatile solvent 2 or the interface in the volatile solvent 2.
  • a complex such as reverse micelle of the active agent 1 is formed (FIG. 1B).
  • Such an isotropic solution has a high fluidity and is easy to mix with a subsequent oil agent.
  • the mixing ratio of the first isotropic solution and the oil agent is such that the surfactant content in the produced lamellar phase dispersion solution is 0.1. It can be in the range of ⁇ 10% by mass.
  • an isotropic solution (second isotropic solution) 5 in which the surfactant 1 is dispersed in the oil agent 4 can be obtained.
  • the form of dispersion of the surfactant into the oil varies depending on the solubility of the volatile solvent used in the oil.
  • the first isotropic solution 3 is compatible with the oil agent to form a one-phase solution. That is, the surfactant 1 contained in the first isotropic solution 3 is present in a monodispersed state or in a state where a complex such as reverse micelle is formed in the one-phase solutions 2 and 4. (FIG. 1 (c)).
  • the first isotropic solution 3 is not compatible with the oil agent 4 and forms a two-phase solution. That is, the particles 31 of the first isotropic solution 3 are dispersed in the continuous phase of the oil agent 4 (FIG. 1D). As shown in FIG. 1 (d 2), the particles 31 are in a state where the surfactant 1 is monodispersed in the volatile solvent 2, or a complex such as reverse micelle of the surfactant 1 in the volatile solvent 2. It is in a formed state. This state can be easily formed by a normal shaking or stirring operation in the mixing step.
  • the component that is sparingly soluble in the oil agent is dissolved in a volatile solvent. It is also possible to dissolve in an oil and mix them.
  • the volatile solvent can be volatilized by a conventional method. That is, it can be performed by vaporizing the volatile solvent by reducing the pressure. Moreover, it is possible to carry out by heating a liquid mixture to the temperature which a volatile solvent vaporizes. Volatilization is preferably performed under reduced pressure. Moreover, when heating, it heats below the temperature which can maintain a lamellar phase, ie, below the temperature which does not phase-transform. When the above-mentioned second isotropic solution forms two phases, the first isotropic solution is sufficiently dispersed in the oil by shaking or stirring, and then this step is entered. Is preferred. It is also preferable to apply a stirring force during volatilization from the viewpoint of forming a fine lamellar phase.
  • the second isotropic solution 5 is phase-shifted to obtain a lamellar phase dispersion solution 8 in which the lamellar phase 7 is dispersed in the oil agent 4 (FIG. 1). (E)).
  • the state of the lamella phase formed may be either a single layer or multiple layers. Confirmation that the lamella phase is formed can be confirmed by performing microscopic observation under polarized light, for example.
  • the step of obtaining a lamellar phase dispersion solution can also be performed as follows. That is, a surfactant and an oil agent are mixed, heated to obtain an isotropic solution, a step of cooling the isotropic solution, and a lamellar phase mainly composed of the surfactant is formed by the cooling.
  • a lamellar phase dispersion solution can be obtained by the process of making it.
  • the preparation method 3 of the lamellar phase dispersion solution will be described with reference to FIG.
  • the mixing ratio of the surfactant and the oil agent is such that the content of the surfactant in the produced lamellar phase dispersion solution is as follows.
  • the range may be 0.1 to 10% by mass.
  • Heating may be performed until the surfactant lamellar (FIG. 2A) undergoes phase transition and the mixture becomes an isotropic solution. Whether or not it is an isotropic solution can be determined by observing the solution through a polarizing plate. Further, the isotropic solution obtained by heating may be one-phase or two-phase, but it is more preferable to heat it until it becomes one-phase (see FIG. 2B, L1). In addition, when the said oil agent contains 2 or more types of oil agents, it is preferable that the said surfactant is performed to the temperature which forms a one-phase isotropic solution with at least 1 type of the said oil agent.
  • the isotropic solution is one-phase or two-phase can be distinguished by observing the presence or absence of separation by leaving it at a constant temperature, or by measuring the light transmittance of the solution.
  • the phase transition temperature of the mixture varies depending on the combination of surfactant and oil used. Therefore, the heating temperature may be adjusted in consideration of the phase transition temperature according to these combinations. For example, when lecithin is used as a surfactant and squalane is used as an oil agent, a phase transition from a lamellar phase to a two-phase isotropic solution is observed at around 65 ° C., and a two-phase is obtained at around 90 ° C. A phase transition from an isotropic solution to a one-phase isotropic solution is seen.
  • the heating temperature in this case is preferably 65 ° C. or higher, more preferably 90 ° C. or higher.
  • the isotropic solution 3 obtained by heating the mixture of the surfactant 1 and the oil agent 2 is in a state in which reverse micelles of the bilayer membrane component 1 are formed in the oil agent 2 (FIG. 2B).
  • the heating is performed until a one-phase isotropic solution is obtained.
  • the heating is performed until the two-phase isotropic solution (L1 + L2) as shown in FIG. 2C is obtained. Form may be sufficient.
  • the highly viscous isotropic solution (L2) containing the reverse-like micelles of the surfactant 1 in the oil agent 2 is phase-separated from the oil agent (L1).
  • L1 the highly viscous isotropic solution
  • the mixture of the surfactant and the oil may further contain water.
  • the process of heating and cooling the mixture of surfactant and oil to obtain a lamellar phase dispersion solution is intended to form a lamellar phase without using conventional physical agitation.
  • the presence of water is not necessary, but rather it is useful in systems with little water.
  • the presence of water may assist the formation of the lamellar phase.
  • the present invention may contain water having a mass of 1 or less that of the surfactant. The smaller the water content, the lower the transition temperature to the isotropic solution. Therefore, when the production efficiency in the present invention is taken into consideration, it is advantageous that the water content is small.
  • the cooling method is not particularly limited, and examples thereof include a method of placing the isotropic solution at a temperature below room temperature and a method of cooling with a refrigerant. Moreover, it can cool by mixing the dilution solvent of temperature lower than the isotropic solution mixed. For example, you may mix the cooled oil agent as a dilution solvent.
  • the cooling temperature may be equal to or lower than the temperature at which the isotropic solution undergoes phase transition and the coexisting phase of the lamellar phase and the oil agent is formed.
  • cooling to about room temperature can be mentioned.
  • Step of mixing the lamellar phase dispersion solution and the powder base material In the step of mixing the lamellar phase dispersion solution obtained as described above and the powder base material, It can be carried out by a usual method of mixing oil. That is, it can be performed by pulverizing the powder base material with a pulverizer, adding a lamellar phase dispersion solution, and mixing with a Henschel mixer. At this time, the mixing ratio of the lamellar phase dispersion solution and the powder base material is preferably 1:99 to 30:70, more preferably 2:98 to 20:80, and further preferably 3:97 to 15:85. .
  • ⁇ 3-1-3> Method for producing powder composition containing no oil agent After the step of mixing the above lamellar phase dispersion solution and the powder base material, a step of volatilizing the oil agent in the powder composition is taken. Thus, a powder composition containing no oil agent can be produced.
  • a volatile oil agent is used as the oil agent.
  • the volatile oil include light isoparaffin, dimethicone and cyclomethicone having a boiling point of 150 to 250 ° C. In the case of dimethicone, the viscosity is 1 mPa ⁇ s or less in terms of viscosity.
  • the step of volatilizing the volatile oil from the mixture of the lamella phase dispersion solution and the powder base material is preferably performed at 50 to 100 ° C. for 6 to 48 hours.
  • the wet manufacturing method of the powder composition of the present invention comprises a step of mixing an oil agent, a surfactant, a volatile solvent, and a powder base material to obtain an intermediate powder composition, And volatilizing the volatile solvent in the intermediate powder composition.
  • the oil agent and surfactant in this production method those described in the above ⁇ 1-1> to ⁇ 1-2> can be used.
  • the powder base material in the present production method the powder described in the above item ⁇ 1-3> can be used, and a composite powder containing two or more kinds of such powders may be used.
  • a mixed powder When it is desired to obtain a powder composition containing two or more powder base materials in which lamella phases are combined, it is preferable to use a mixed powder.
  • the oil agent and the powder base material are mixed in advance, and the volatile solvent and the surfactant are mixed therewith.
  • a mixed solution of water can be added and mixed by stirring.
  • the content of the surfactant in the intermediate powder composition is preferably 0.05 to 10% by mass, more preferably 0.1 to 5% by mass, and still more preferably 0.2 to 2% by mass.
  • the content of the oil agent in the intermediate powder composition is preferably 0.1 to 20% by mass, more preferably 0.5 to 15%, and further preferably 1 to 10% by mass.
  • the content of the volatile solvent in the intermediate powder composition is preferably 10 to 70% by mass, more preferably 20 to 60% by mass, and still more preferably 30 to 50% by mass.
  • the content of the powder base material in the intermediate powder composition is preferably 20 to 90% by mass, more preferably 30 to 80% by mass, and further preferably 40 to 70% by mass.
  • volatile solvent examples include alcohols such as methanol, ethanol, propanol and isopropanol, hydrocarbons such as pentane, hexane and cyclopentane, aromatics such as benzene, ketones such as acetone, ethers and esters. And volatile silicone oils such as decamethylpentasiloxane, fluorocarbons, isoparaffins and the like. Of these, ethanol, propanol, acetone and the like are preferably used.
  • the volatile solvent can be volatilized by a conventional method. That is, it can be carried out by vaporizing a volatile solvent under reduced pressure. It can also be carried out by heating the intermediate powder composition to a temperature at which the volatile solvent vaporizes. Volatilization is preferably performed under reduced pressure. Moreover, when heating, it heats below the temperature which can maintain a lamellar phase, ie, below the temperature which does not phase-transform.
  • a powder composition containing no oil agent can be produced by volatilizing the volatile oil agent simultaneously by the volatilization step of the volatile solvent.
  • the volatile oil those described in the above ⁇ 3-1-3> can be used.
  • the powder composition manufactured by the manufacturing method of this invention can be used as a raw material of a skin external preparation.
  • the powder composition manufactured by such a method can also be used as a skin external preparation as it is.
  • the external preparation for skin include powder cosmetics such as foundation, teak, eye shadow, loose powder and pressed powder.
  • a powder cosmetic containing the powder composition of the present invention was produced by a dry production method.
  • Example 1 A powder foundation was produced according to the following formulation.
  • (A) Methyl methacrylate cross polymer 15 (A) Fluorine-treated mica 10
  • (A) Fluorine-treated sericite 10 (A) Methylparaben 0.3
  • C Silicone surfactant 1.6
  • C Water 0.4
  • Cetyl ethylhexanoate 2 D) Dimethicone 8 (Unit:% by mass)
  • the (C) and (D) groups were mixed and dissolved by heating at 80 ° C., and then the solution was cooled to prepare a lamellar phase dispersion solution (B) in advance.
  • (B) After mixing the components of (A) group and coarsely pulverizing with a pulverizer, (B) was added and mixed with a Henschel mixer. Thereafter, it was pulverized again with a pulverizer and cast into a metal pan to produce a powder foundation.
  • Loose powder was produced according to the following formulation.
  • (A) Methyl methacrylate cross polymer 10 (A) Mica 10
  • (A) Silicone resin powder 10 (A) Methylparaben 0.3
  • (B) Lamella phase dispersion solution 4 (C) Lecithin (Epikuron 200) 0.6
  • (D) Ethyl hexanoate cetyl 3 Unit:% by mass
  • the (C) and (D) groups were mixed to obtain a lamellar phase dispersion solution (B) by ultrasonic dispersion. After mixing the components of (A) group and coarsely pulverizing with a pulverizer, (B) was added and mixed with a Henschel mixer
  • Example 3 A powder foundation was produced according to the following formulation.
  • FIG. 3 shows a lamellar phase dispersion solution
  • FIG. 4 shows a small-angle X-ray scattering spectrum of the powder cosmetic of Example 3.
  • a powder sample 1 which is a powder composition of the present invention was prepared by the following method.
  • An intermediate solution was prepared by mixing 3 parts by mass of lecithin (Epicuron 200), 2 parts by mass of water, and 60 parts by mass of ethanol and stirring and dissolving at room temperature.
  • 88 parts by mass of talc was pulverized with a pulverizer, 7 parts by mass of cetyl ethylhexanoate was added thereto, and mixed with a Henschel mixer. Thereafter, the mixture was again pulverized to prepare a mixed powder.
  • a powder sample 1 was prepared by thoroughly mixing 65 parts by mass of the intermediate solution and 95 parts by mass of the mixed powder and volatilizing ethanol at 40 ° C.
  • FIG. 5 shows a photograph of the powder sample 1 taken with a transmission electron microscope. As shown in FIG. 5, in the powder sample 1, the lamellar phase is compounded on the surface of talc. In addition, talc which was not subjected to any treatment after being pulverized by a pulverizer was prepared as a comparative sample 1.
  • the plugability of the powder sample 1 was evaluated by the cup method as follows. Water was put into the cup, and filter paper moistened with a sebum component (oleic acid) was placed so as to close the opening. Comparative sample 1 or powder sample 1 in the same amount as the sebum component contained in the filter paper was further applied to the filter paper. Then, the cup was left at 35 ° C., and the water evaporation rate was calculated. As a result, the water evaporation rate when the comparative sample 1 was applied was 8.6 mg / cm 2 / h. On the other hand, the moisture evaporation rate when the powder sample 1 was applied was 4.6 mg / cm 2 / h (FIG. 6). This result has shown that the powder sample 1 is excellent in the obstruction
  • LPF lamellar phase coating foundation
  • SQL squalane coating foundation
  • the moisturizing properties of LPF and SQPF were evaluated as follows.
  • the water content of the facial skin of 20 subjects was measured with SKICON EX-200.
  • 20% glycerin aqueous solution was applied to the entire face, and LPF and SQPF were applied to each half face.
  • the entire face was washed with cleansing and face wash, and the moisture content was measured.
  • the moisture content of the skin before application of LPF and SQPF was 1, the moisture content of the skin after application was 1.21 and 1.04, respectively (FIG. 7). This result has shown that the skin external preparation of this invention is excellent in the moisture retention of skin.
  • a powder sample 2 was prepared by sufficiently mixing 65 parts by mass of the intermediate solution and 95 parts by mass of the mixed powder and volatilizing ethanol at 40 ° C. Moreover, comparative sample 2 was prepared by mixing 0.5 parts by mass of dipotassium glycyrrhizinate and 99.5 parts by mass of comparative sample 1.
  • the powder sample 2 and the comparative sample 2 were each applied at 5 mg / cm 2 to the forearms of 12 subjects and fixed with a film. After 6 hours, the powder sample 2 and the comparative sample 2 were wiped off, the stratum corneum was collected by tape stripping, and dipotassium glycyrrhizinate was quantitatively analyzed by HPLC. As a result, penetration of the stratum corneum of dipotassium glycyrrhizinate when the powder sample 2 and comparative sample 2 was applied, respectively, 0.28 .mu.g / cm 2, was 0.19 ⁇ g / cm 2. This result shows that according to the powder composition of the present invention, the penetration efficiency of the water-soluble active ingredient into the stratum corneum can be increased.
  • the present invention can be applied to powder cosmetics having excellent moisture retention.

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Abstract

Provided is a powder cosmetic which does not give a dry feeling in use and exhibits excellent moisturizing properties. This powder cosmetic contains, as an ingredient, a powder composition which comprises an oil, a surfactant and a powder base and which is characterized in that the surface of the powder base is composited with a lamellar phase comprising the surfactant as the main component.

Description

ラメラ相が複合化した粉体を含む粉体組成物とその製造方法POWDER COMPOSITION CONTAINING POWDER COMPOSED WITH LAMERA PHASE AND METHOD FOR PRODUCING SAME
 本発明は、ラメラ相が複合化した粉体を含む粉体組成物とその製造方法に関する。 The present invention relates to a powder composition containing a powder in which a lamellar phase is complexed and a method for producing the same.
 パウダー化粧料は液状の化粧料と比較して、携帯性や簡便性に優れているが、使用したとき肌に乾燥感を感じやすいという問題があった。従来、このような問題点を解決するために粉体を油剤で被覆する手法がとられてきた(例えば特許文献1)。 Powder powder is superior in portability and convenience compared to liquid cosmetics, but has a problem that it feels dry to the skin when used. Conventionally, in order to solve such problems, a technique of coating powder with an oil has been taken (for example, Patent Document 1).
 ところで、人間の皮膚を構成する細胞と細胞の隙間には、ラメラ相と呼ばれる水相と油相が繰り返し重なった層状構造が存在する。このラメラ相は両親媒性分子である脂質が規則正しく配列した構造をとっており、その水相に乳酸やアミノ酸等の有効成分を保持することで、皮膚の潤いを保っている。また、皮膚中のラメラ相は、大気中の有害物質から肌を守るバリア機能を有している。
 近年、このラメラ相の持つ有効成分の保持機能、保湿機能、バリア機能を応用した化粧料が作成されている。例えば、特許文献2には脂肪酸モノグリセリドを構成成分とするラメラ相とショ糖脂肪酸エステルを含有する保湿剤が開示されている。
By the way, in the gap between cells constituting human skin, there is a layered structure called a lamellar phase in which an aqueous phase and an oil phase are repeatedly overlapped. This lamellar phase has a structure in which lipids, which are amphipathic molecules, are regularly arranged. The water phase retains active ingredients such as lactic acid and amino acids to keep the skin moist. The lamellar phase in the skin has a barrier function to protect the skin from harmful substances in the atmosphere.
In recent years, cosmetics applying the active ingredient holding function, moisturizing function, and barrier function of this lamellar phase have been created. For example, Patent Document 2 discloses a humectant containing a lamellar phase and a sucrose fatty acid ester containing fatty acid monoglyceride as components.
特開2002-284644号公報JP 2002-284644 A 特開2009-298748号公報JP 2009-298748 A
 油剤による粉体の被覆は、乾燥感の軽減には有効である。しかし、保湿性を高めようと大量の油剤を用いると、使用時にべたつきを生じるという問題がある。そのため、用いる油剤の増量以外の別途の方法によってパウダー化粧料の保湿性を向上させる技術が求められてきた。すなわち、本発明の解決しようとする課題は、使用時に乾燥感及びべたつき感を生じない、保湿性に優れた粉体組成物を提供することである。 Coating the powder with an oil agent is effective in reducing the dry feeling. However, when a large amount of oil is used to improve the moisture retention, there is a problem that stickiness occurs during use. Therefore, there has been a demand for a technique for improving the moisturizing property of the powder cosmetic by a separate method other than increasing the amount of oil used. That is, the problem to be solved by the present invention is to provide a powder composition excellent in moisturizing property that does not cause dryness and stickiness during use.
 上記課題を解決する本発明は、油剤と界面活性剤と粉体基材を含み、粉体基材の表面に界面活性剤を主とするラメラ相が複合化していることを特徴とする、粉体組成物である。かかる粉体組成物を構成する粉体は、その表面にラメラ相が存在しているため、保湿性に優れたものとなる。
 ここで複合化とは、粉体基材の表面全体がラメラ相で被覆されている状態だけではなく、部分的にラメラ相が接着している状態のこともいう。
 また、本明細書において粉体組成物とは、粉体と他の成分の混合組成物のことをいう。
The present invention for solving the above-mentioned problems comprises a powder comprising an oil agent, a surfactant, and a powder base material, wherein a lamellar phase mainly comprising a surfactant is complexed on the surface of the powder base material. It is a body composition. The powder composing such a powder composition has excellent moisturizing properties because the surface has a lamellar phase.
Here, “composite” means not only a state in which the entire surface of the powder base material is coated with a lamellar phase, but also a state in which the lamellar phase is partially adhered.
Further, in this specification, the powder composition refers to a mixed composition of powder and other components.
 本発明の好ましい形態では、前記油剤が、シリコーン油、炭化水素油、エステル油、天然動植物油、フッ素油から選ばれる。
 これらの油剤を用いることで、粉体組成物の保湿性が向上する。
In a preferred embodiment of the present invention, the oil agent is selected from silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.
By using these oil agents, the moisture retention of the powder composition is improved.
 本発明の好ましい形態では、粉体組成物は水を含む。
 ラメラ相は親水性の層に水分を保持することができるため、これを油剤中で粉体基材に複合化させることにより、水分と油分を共存させることができ、使用時の乾燥感を抑え、肌に潤いを与えることができる。
In a preferred form of the invention, the powder composition contains water.
Since the lamellar phase can retain moisture in the hydrophilic layer, by combining it with the powder base material in the oil agent, moisture and oil can coexist and the dry feeling during use is suppressed. Can moisturize the skin.
 上記の様に粉体組成物が水を含む場合には、水溶性の有効成分を含ませてもよい。
 この場合、ラメラ相中の水分が保持されている層に親水性の有効成分が取り込まれる。このような形態とすることによって、粉体組成物は、保湿性の他、その有効成分の持つ効果を発揮する優れたものとなる。具体的には、このような形態の本発明の粉体組成物は、有効成分を効率よく角質層に浸透させることにより、有効成分の持つ効果を高めることができる。
When the powder composition contains water as described above, a water-soluble active ingredient may be included.
In this case, the hydrophilic active ingredient is taken into the layer in which the water in the lamellar phase is retained. By setting it as such a form, a powder composition becomes the outstanding thing which exhibits the effect which the active ingredient has other than moisture retention. Specifically, the powder composition of the present invention having such a form can enhance the effect of the active ingredient by efficiently infiltrating the active ingredient into the stratum corneum.
 本発明においては、界面活性剤は特に制限されないが、例えば、本発明の粉体組成物を化粧料の成分として応用する場合、レシチン及び/又は非イオン界面活性剤が好ましく挙げられる。これらの油剤からなるラメラ相はより安定性に優れるため、高い保湿性を長時間維持するパウダー化粧料を提供することができる。 In the present invention, the surfactant is not particularly limited. For example, when the powder composition of the present invention is applied as a cosmetic component, lecithin and / or a nonionic surfactant are preferably mentioned. Since the lamellar phase composed of these oil agents is more stable, it is possible to provide a powder cosmetic that maintains high moisture retention for a long time.
 本発明は粉体組成物を含む皮膚外用剤にも関する。
 かかる皮膚外用剤は保湿性に優れ、またラメラ相内に水溶性の有効成分を保持することができるため、優れたスキンケア効果を有するものとなる。
The present invention also relates to an external preparation for skin containing a powder composition.
Such an external preparation for skin has excellent moisturizing properties and can retain a water-soluble active ingredient in the lamellar phase, and therefore has an excellent skin care effect.
 本発明は、油剤中で界面活性剤を主とするラメラ相を粉体基材の表面に複合化させることを特徴とする、上記粉体組成物の製造方法にも関する。
 本発明の製造方法によれば、本発明の粉体組成物を製造することができる。
The present invention also relates to a method for producing the above powder composition, characterized in that a lamellar phase mainly composed of a surfactant in an oil agent is compounded on the surface of a powder base material.
According to the production method of the present invention, the powder composition of the present invention can be produced.
 また好ましい形態によれば、本発明の粉体組成物の製造方法は、油剤と界面活性剤と粉体基材を混合する工程を含む。
 かかる形態によれば、本発明の粉体組成物を効率よく製造することができる。
Moreover, according to a preferable form, the manufacturing method of the powder composition of this invention includes the process of mixing an oil agent, surfactant, and a powder base material.
According to this form, the powder composition of the present invention can be produced efficiently.
 本発明の製造方法のより好ましい形態によれば、油剤と界面活性剤を混合し、ラメラ相分散溶液を得る工程と、前記ラメラ相分散溶液と粉体基材を混合する工程を含む。
 上記工程を含む製造方法によれば、本発明の粉体基材を効率よく簡便に製造することができる。
 以下、かかる形態の本発明の製造方法のことを乾式製造方法という。
According to the more preferable form of the manufacturing method of this invention, the process which mixes an oil agent and surfactant and obtains a lamella phase dispersion solution, and the process which mixes the said lamella phase dispersion solution and a powder base material are included.
According to the production method including the above steps, the powder base material of the present invention can be produced efficiently and simply.
Hereinafter, the manufacturing method of the present invention in this form is referred to as a dry manufacturing method.
 また、乾式製造方法とは別の好ましい形態によれば、本発明の製造方法は、油剤と界面活性剤と揮発性溶媒と粉体基材を混合し、中間粉体組成物を得る工程と、前記中間粉体組成物中の前記揮発性溶媒を揮発させる工程と、を含む。
 上記工程を含む製造方法によれば、均一にラメラ相が複合化した粉体基材を含む本発明の粉体組成物を効率よく簡便に製造することができる。
 以下、かかる形態の本発明の製造方法のことを湿式製造方法という。
Further, according to a preferred embodiment different from the dry production method, the production method of the present invention comprises a step of mixing an oil agent, a surfactant, a volatile solvent, and a powder base material to obtain an intermediate powder composition; Volatilizing the volatile solvent in the intermediate powder composition.
According to the manufacturing method including the above steps, the powder composition of the present invention including a powder base material in which lamella phases are uniformly combined can be efficiently and simply manufactured.
Hereinafter, the manufacturing method of the present invention in this form is referred to as a wet manufacturing method.
 本発明の湿式製造方法では、前記揮発性溶媒として、アルコール類、炭化水素類、芳香族類、ケトン類、エーテル類、エステル類、揮発性シリコーン油、イソパラフィンから選ばれる溶媒を用いることが好ましい。
 揮発性溶媒として、上記のものを用いることにより、安全に効率よく粉体組成物を製造することができる。
In the wet manufacturing method of the present invention, it is preferable to use a solvent selected from alcohols, hydrocarbons, aromatics, ketones, ethers, esters, volatile silicone oils, and isoparaffins as the volatile solvent.
By using the above-mentioned volatile solvent, a powder composition can be produced safely and efficiently.
 また、本発明の湿式製造方法では、前記揮発性溶媒の揮発は、減圧下で行われる。こうすることで、効率的に揮発性溶媒を揮発させることができる。 In the wet manufacturing method of the present invention, the volatile solvent is volatilized under reduced pressure. By carrying out like this, a volatile solvent can be volatilized efficiently.
 本発明はまた、上述した本発明の製造方法により製造された粉体組成物を、他の成分と混合する工程を含む、皮膚外用剤の製造方法にも関する。 The present invention also relates to a method for producing an external preparation for skin, which comprises a step of mixing the powder composition produced by the production method of the present invention described above with other components.
 また、本発明は、表面に界面活性剤を主とするラメラ相が複合化している粉体基材を含む粉体組成物を製造する方法であって、油剤中で、界面活性剤を主とするラメラ相を粉体基材の表面に複合化させることを特徴とする、粉体組成物の製造方法にも関する。
 かかる製造方法では、油剤として揮発性油剤を使用してもよい。この場合、かかる油剤を揮発させて油剤を含まない粉体組成物を製造することもできる。
Further, the present invention is a method for producing a powder composition comprising a powder base material having a lamella phase mainly composed of a surfactant on the surface, wherein the surfactant is mainly contained in the oil. The present invention also relates to a method for producing a powder composition, characterized in that a lamellar phase is combined with the surface of a powder substrate.
In such a production method, a volatile oil agent may be used as the oil agent. In this case, a powder composition containing no oil agent can be produced by volatilizing the oil agent.
 本発明の粉体組成物は、粉体基材がラメラ相と複合化しているため、油剤中においても水分の保持能力を有し、同時に水溶性の有効成分も保持することができる。また、本発明の粉体組成物を使用すれば、保湿性に優れた皮膚外用剤を提供することができる。 Since the powder base material is complexed with the lamellar phase, the powder composition of the present invention has the ability to retain moisture even in the oil, and can also retain water-soluble active ingredients at the same time. Moreover, if the powder composition of this invention is used, the skin external preparation excellent in moisture retention can be provided.
ラメラ相分散溶液の調製方法2を示す概略工程図である。各工程における相の状態を併せて示す。It is a schematic process drawing which shows the preparation method 2 of a lamella phase dispersion solution. The phase state in each step is also shown. ラメラ相分散溶液の調製方法3を示す概略工程図である。各工程における相の状態を併せて示す。It is a schematic process drawing which shows the preparation method 3 of a lamella phase dispersion solution. The phase state in each step is also shown. レシチンと水を8:2で混合したラメラ相分散溶液の小角X線散乱による測定結果。縦軸は散乱強度、横軸は散乱ベクトルの大きさを表す。The measurement result by the small angle X ray scattering of the lamellar phase dispersion solution which mixed lecithin and water by 8: 2. The vertical axis represents the scattering intensity, and the horizontal axis represents the size of the scattering vector. 実施例3のパウダー化粧料の小角X線散乱スペクトルを表す図。縦軸は散乱強度、横軸は散乱ベクトルの大きさを表す。The figure showing the small angle X-ray-scattering spectrum of the powder cosmetics of Example 3. FIG. The vertical axis represents the scattering intensity, and the horizontal axis represents the size of the scattering vector. 粉体試料1を透過型電子顕微鏡によって撮影した写真である。It is the photograph which image | photographed the powder sample 1 with the transmission electron microscope. 粉体試料1と比較試料1の閉塞性の測定結果を示す。The measurement results of the occlusion property of the powder sample 1 and the comparative sample 1 are shown. ラメラ相コーティングファンデーション(LPF)及びスクワランコーティングファンデーション(SQPF)の保湿性の測定結果を示す。The measurement result of the moisture retention of a lamellar phase coating foundation (LPF) and a squalane coating foundation (SQPF) is shown.
 以下、本発明を実施するための形態について、詳述する。
<1>粉体組成物
 本発明の粉体組成物は、油剤と界面活性剤と粉体基材を含み、前記粉体基材の表面に前記界面活性剤を主とするラメラ相が複合化していることを特徴とする。
 以下、本組成物を構成する各成分について説明する。
Hereinafter, embodiments for carrying out the present invention will be described in detail.
<1> Powder Composition The powder composition of the present invention includes an oil agent, a surfactant, and a powder base material, and a lamellar phase mainly composed of the surfactant is compounded on the surface of the powder base material. It is characterized by.
Hereinafter, each component which comprises this composition is demonstrated.
<1-1>油剤
 本発明の粉体組成物における油剤としては、粉体基材及び界面活性剤と混合すことができ、界面活性剤を主とするラメラ相をその連続相中に形成することができるものであれば特に制限されない。本発明の粉体組成物を、化粧料など皮膚外用剤に応用する場合には、油剤として、シリコーン油、炭化水素油、エステル油、天然動植物油、フッ素油等が好ましく挙げられる。これらの油剤を使用することによって、粉体組成物の保湿性を高めることができる。
<1-1> Oil Agent The oil agent in the powder composition of the present invention can be mixed with a powder base material and a surfactant, and a lamellar phase mainly composed of a surfactant is formed in the continuous phase. There is no particular limitation as long as it can be used. When the powder composition of the present invention is applied to an external preparation for skin such as cosmetics, preferred examples of the oil include silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil. By using these oil agents, the moisture retention of the powder composition can be enhanced.
 シリコーン油の例としては、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、ジメチルシロキサン・メチルフェニルシロキサン共重合体等のオルガノポリシロキサン、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シロキサン等が挙げられる。
 中でも、上述した環状シロキサンが好ましく用いられる。
Examples of silicone oil include organopolysiloxanes such as dimethylpolysiloxane, methylphenylpolysiloxane, dimethylsiloxane / methylphenylsiloxane copolymer, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, etc. Examples thereof include cyclic siloxane.
Among these, the cyclic siloxane described above is preferably used.
 炭化水素油としては、鎖式及び環式の炭化水素、例えば、α-オレフィンオリゴマー、軽質イソパラフィン、軽質流動イソパラフィン、スクワラン、流動パラフィン、流動イソパラフィン、水添イソブテン、イソオクタン、デカン、イソドデカン、イソヘキサデカン、ポリブデン等が挙げられる。 Hydrocarbon oils include chain and cyclic hydrocarbons such as α-olefin oligomers, light isoparaffins, light liquid isoparaffins, squalane, liquid paraffin, liquid isoparaffins, hydrogenated isobutene, isooctane, decane, isododecane, isohexadecane, Polybutene etc. are mentioned.
 エステル油としては、コハク酸ジオクチル、アジピン酸ジイソブチル、アジピン酸ジオクチル、アジピン酸ジ(2-ヘプチルウンデシル)、セバシン酸ジイソプロピル、セバシン酸ジオクチル、セバシン酸ジブチルオクチル、リンゴ酸ジイソステアリル、クエン酸トリエチル、ジオクタン酸エチレングリコール、ジオクタン酸ネオペンチルグリコール、ジカプリン酸プロピレングリコール、ジカプリン酸ネオペンチルグリコール、トリオクタン酸トリメチロールプロパン、トリイソステアリン酸トリメチロールプロパン、テトラオレイン酸ペンタエリトリトール、酢酸エチル、酢酸ブチル、酢酸アミル、ネオペンタン酸オクチルドデシル、エチルヘキサン酸セチル、オクタン酸セチル、イソノナン酸イソノニル、イソノナン酸イソトリデシル、ジメチルオクタン酸ヘキシルデシル、ラウリン酸エチル、ラウリン酸ヘキシル、ミリスチン酸イソプロピル、ミリスチン酸ミリスチル、ミリスチン酸イソセチル、ミリスチン酸オクチルドデシル、パルミチン酸イソプロピル、パルミチン酸オクチル、パルミチン酸セチル、パルミチン酸イソセチル、パルミチン酸イソステアリル、ステアリン酸ブチル、ステアリン酸ヘキシルデシル、イソステアリン酸イソプロピル、イソステアリン酸イソセチル、オレイン酸デシル、オレイン酸オレイル、オレイン酸オクチルドデシル、リノール酸エチル、リノール酸イソプロピル、乳酸セチル、乳酸ミリスチル、ヒドロキシステアリン酸コレステリル、ラウロイルグルタミン酸ジオクチルドデシル、ラウロイルサルコシンイソプロピル、メトキシケイヒ酸エチルヘキシル等が挙げられる。 Ester oils include dioctyl succinate, diisobutyl adipate, dioctyl adipate, di (2-heptylundecyl) adipate, diisopropyl sebacate, dioctyl sebacate, dibutyl octyl sebacate, diisostearyl malate, triethyl citrate , Ethylene glycol dioctanoate, neopentyl glycol dioctanoate, propylene glycol dicaprate, neopentyl glycol dicaprate, trimethylolpropane trioctanoate, trimethylolpropane triisostearate, pentaerythritol tetraoleate, ethyl acetate, butyl acetate, amyl acetate Octyldodecyl neopentanoate, cetyl ethylhexanoate, cetyl octanoate, isononyl isononanoate, isotrideconate isononanoate Hexyldecyl dimethyloctanoate, ethyl laurate, hexyl laurate, isopropyl myristate, myristyl myristate, isocetyl myristate, octyldodecyl myristate, isopropyl palmitate, octyl palmitate, cetyl palmitate, isocetyl palmitate, palmitic acid Isostearyl, butyl stearate, hexyldecyl stearate, isopropyl isostearate, isocetyl isostearate, decyl oleate, oleyl oleate, octyldodecyl oleate, ethyl linoleate, isopropyl linoleate, cetyl lactate, myristyl lactate, hydroxystearic acid Cholesteryl, dioctyldecyl lauroyl glutamate, lauroyl sarcosine isopropyl, methoxysilicate Ethylhexyl and the like.
 天然動植物油としては、アボカド油、アーモンド油、オリーブ油、小麦胚芽油、サフラワー油、ホホバ油、マカデミアナッツ油、綿実油、ヤシ油等が挙げられる。 Natural animal and vegetable oils include avocado oil, almond oil, olive oil, wheat germ oil, safflower oil, jojoba oil, macadamia nut oil, cottonseed oil, coconut oil, and the like.
 フッ素油としてはパーフルオロ類の油が挙げられる。 Fluorine oil includes perfluoro oils.
 後述する<3-1-1>ラメラ相分散溶液の調製方法1の項目に記載の方法によって、界面活性剤としてレシチンを含むラメラ相分散溶液を調整し、本発明の粉体組成物を製造する場合には、油剤としては分子量が114g/molより大きい25℃で液状のものを使用することが好ましい。 The powder composition of the present invention is produced by preparing a lamellar phase dispersion solution containing lecithin as a surfactant by the method described in the item <Preparation Method 1 of <3-1-1> Lamellar Phase Dispersion Solution> described later. In this case, it is preferable to use an oil agent that is liquid at 25 ° C. with a molecular weight of greater than 114 g / mol.
<1-2>界面活性剤
 本発明における界面活性剤としては、両親媒性物質であれば特に制限されず、イオン性界面活性剤、非イオン界面活性剤の何れをも用いることができる。好ましくは、両イオン性界面活性剤であるレシチンが挙げられる。また、非イオン性界面活性剤も好ましく用いることができ、例えば、シリコーン界面活性剤、ポリオキシエチレンアルキルエーテル、ショ糖脂肪酸エステル、スフィンゴシン類、脂肪酸などを好ましく用いることができる。
<1-2> Surfactant The surfactant in the present invention is not particularly limited as long as it is an amphiphilic substance, and either an ionic surfactant or a nonionic surfactant can be used. Preferably, lecithin which is an amphoteric surfactant is used. Nonionic surfactants can also be preferably used. For example, silicone surfactants, polyoxyethylene alkyl ethers, sucrose fatty acid esters, sphingosines, fatty acids and the like can be preferably used.
 レシチンは、植物、動物及び微生物の生体から抽出され、所望により精製したものを用いてもよいし、合成したものを用いても良い。好ましくは、大豆、トウモロコシ、落花生、ナタネ、麦等の植物由来レシチンや、卵黄等の動物由来レシチンなどを用いることができる。
 本発明におけるレシチンには、ホスファチジルコリン、ホスファチジン酸、ホスファチジルグリセリン、ホスファチジルイノシトール、ホスファチジルエタノールアミン、ホスファチジルメチルエタノールアミン、ホスファチジルセリン、ビスホスアチジン酸、ジホスファチジルグリセリン(カルジオリピン)等が含まれる。
 また、本発明において、「レシチン」には、水素添加レシチン、酵素分解レシチン、酵素分解水素添加レシチン、リゾレシチン等も含まれる。
Lecithin extracted from living bodies of plants, animals and microorganisms and purified as desired may be used, or synthesized. Preferably, plant-derived lecithin such as soybean, corn, peanut, rapeseed, and wheat, or animal-derived lecithin such as egg yolk can be used.
The lecithin in the present invention includes phosphatidylcholine, phosphatidic acid, phosphatidylglycerol, phosphatidylinositol, phosphatidylethanolamine, phosphatidylmethylethanolamine, phosphatidylserine, bisphosphatidic acid, diphosphatidylglycerol (cardiolipin) and the like.
In the present invention, “lecithin” also includes hydrogenated lecithin, enzymatically decomposed lecithin, enzymatically decomposed hydrogenated lecithin, lysolecithin and the like.
 レシチンの疎水基部分を構成する脂肪酸の炭素数は特に制限されず、例えば炭素数8~20、好ましくは16~18のものを主に用いることができる。また、脂肪酸は、飽和であっても不飽和であってもよい。また、脂肪酸は直鎖であっても分岐であっても良い。
 本発明において、レシチンは、上記化合物の単独種の形態で用いることもできるし、上述した複数種のリン脂質の混合物の形態で用いることも出来る。
 レシチンの組成としては、ホスファチジルコリンを主体としたものが好ましく、例えば20質量%以上、好ましくは50質量%以上がホスファチジルコリンであることが好ましい。
 レシチンは、市販のものを用いることができる。例えば、以下のような市販品を用いる
ことができる。
レシノールS-10、日光ケミカルズ社(水添:○、PC(ホスファチジルコリン)含有量:25~30%)
レシノールS-10E、日光ケミカルズ社(水添:○、PC含有量:75~85%)
レシノールS-10EX、日光ケミカルズ社(水添:○、PC含有量:>95%)
ベイシスLP-20、日清オイリオ社(水添:×、PC含有量:20~30%)
ベイシスLP-20H、日清オイリオ社(水添:○、PC含有量:未確認)
ベイシスLS-60HR、日清オイリオ社(水添:○、PC含有量:60~75%)
ベイシスLS-60、日清オイリオ社(水添:×、PC含有量:未確認)
Phospholipon85G、H.Holstein GmbH&Co.KG社((水添:×、PC含有量:>85%))
Phospholipon90G、H.Holstein GmbH&Co.KG社((水添:×、PC含有量:>94%))
Phospholipon75IP、H.Holstein GmbH&Co.KG社((水添:×、PC含有量:>70%))
Phospholipon90IP、H.Holstein GmbH&Co.KG社((水添:×、PC含有量:>90%))
Phospholipon80H、H.Holstein GmbH&Co.KG社((水添:○、PC含有量:>70%))
Phospholipon90H、H.Holstein GmbH&Co.KG社((水添:○、PC含有量:>90%))
Phospholipon75HIP、H.Holstein GmbH&Co.KG社((水添:○、PC含有量:>70%))
Phospholipon90HIP、H.Holstein GmbH&Co.KG社((水添:○、PC含有量:>90%))
LipoidE25、H.Holstein GmbH&Co.KG社((水添:×、PC含有量:>25%))
LipoidE80、H.Holstein GmbH&Co.KG社((水添:×、PC含有量:>80%))
LipoidE80S、H.Holstein GmbH&Co.KG社((水添:×、PC含有量:>64%))
LipoidEPCS、H.Holstein GmbH&Co.KG社((水添:×、PC含有量:>96%))
Epikron200、Cargill社(水添:×、PC含有量:>95%)
Epikron200SH、Cargill社(水添:○、PC含有量:未確認)
Epikron100P、Cargill社(水添:×、PC含有量:未確認)
Epikron100H、Cargill社(水添:○、PC含有量:未確認)
PhosphoLipidPCSH70、日本精化社(水添:○、PC含有量:約70%)
卵黄レシチンPL-100E、キューピー社(水添:○、PC含有量:約83%)
The number of carbon atoms of the fatty acid constituting the hydrophobic group portion of lecithin is not particularly limited, and for example, those having 8 to 20 carbon atoms, preferably 16 to 18 carbon atoms can be mainly used. The fatty acid may be saturated or unsaturated. The fatty acid may be linear or branched.
In the present invention, lecithin can be used in the form of a single kind of the above-mentioned compound or in the form of a mixture of the above-mentioned plural kinds of phospholipids.
The composition of lecithin is preferably composed mainly of phosphatidylcholine, for example, 20% by mass or more, and preferably 50% by mass or more is phosphatidylcholine.
A commercially available lecithin can be used. For example, the following commercially available products can be used.
Resinol S-10, Nikko Chemicals (hydrogenated: ○, PC (phosphatidylcholine) content: 25-30%)
Resinol S-10E, Nikko Chemicals (hydrogenated: ○, PC content: 75-85%)
Resinol S-10EX, Nikko Chemicals (hydrogenated: ○, PC content:> 95%)
Basis LP-20, Nisshin Oillio Co., Ltd. (hydrogenated: x, PC content: 20-30%)
Basis LP-20H, Nisshin Oilio Co., Ltd. (hydrogenated: ○, PC content: unconfirmed)
Basis LS-60HR, Nisshin Oilio Co., Ltd. (hydrogenated: ○, PC content: 60-75%)
Basis LS-60, Nisshin Oillio Co., Ltd. (hydrogenated: x, PC content: unconfirmed)
Phospholipon 85G, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 85%))
Phospholipon 90G, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 94%))
Phospholipon 75IP, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 70%))
Phospholipon 90IP, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 90%))
Phospholipon 80H, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: ○, PC content:> 70%))
Phospholipon 90H, H.P. Holstein GmbH & Co. KG ((hydrogenated: ○, PC content:> 90%))
Phospholipon 75HIP, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: ○, PC content:> 70%))
Phospholipon 90 HIP, H.P. Holstein GmbH & Co. KG ((hydrogenated: ○, PC content:> 90%))
Lipoid E25, H.I. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 25%))
Lipoid E80, H.I. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 80%))
Lipoid E80S, H.I. Holstein GmbH & Co. KG ((hydrogenated: x, PC content:> 64%))
Lipoid EPCS, H.C. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 96%))
Epikron 200, Cargill (hydrogenated: x, PC content:> 95%)
Epikron 200SH, Cargill (hydrogenated: ○, PC content: unconfirmed)
Epikron 100P, Cargill (hydrogenated: x, PC content: unconfirmed)
Epikron 100H, Cargill (hydrogenated: ○, PC content: unconfirmed)
PhosphoLipid PCSH70, Nippon Seika Co., Ltd. (hydrogenated: ○, PC content: about 70%)
Egg yolk lecithin PL-100E, Kewpie company (hydrogenated: ○, PC content: about 83%)
 また、レシチンを主体とする場合、他の補助界面活性剤(非イオン界面活性剤、イオン性界面活性剤)と組合せることもできる。
 この場合、ラメラ相を形成する界面活性剤のうち、レシチンが好ましくは60質量%以上、さらに好ましくは80質量%以上を占めることが好ましい。
When lecithin is mainly used, it can be combined with other auxiliary surfactants (nonionic surfactants, ionic surfactants).
In this case, it is preferable that lecithin accounts for 60% by mass or more, more preferably 80% by mass or more of the surfactant forming the lamellar phase.
 上述したように、本発明における界面活性剤として、シリコーン界面活性剤を使用しても良い。シリコーン界面活性剤は、ポリオルガノシロキサン(シリコーン鎖)を疎水基にもつ界面活性剤である。その親水基は、好ましくはポリエーテル又はポリグリセリンから選ばれる。ポリエーテルとしては、ポリオキシエチレン、ポリオキシプロピレン、又はオキシエチレン・オキシプロピレン共重合体が好ましく挙げられる。
 ポリオキシエチレン又はポリオキシプロピレン、オキシエチレン・オキシプロピレン共重合体、ポリグリセリンの平均重合度としては、たとえば8~15程度が挙げられる。
 ポリオルガノシロキサンは、直鎖であっても分岐であってもよい。また、複数のポリオルガノシロキサン鎖が架橋されていてもよい。また、シリコーン鎖はアルキル基で変性されていてもよい。
As described above, a silicone surfactant may be used as the surfactant in the present invention. The silicone surfactant is a surfactant having a polyorganosiloxane (silicone chain) in a hydrophobic group. The hydrophilic group is preferably selected from polyether or polyglycerin. Preferred examples of the polyether include polyoxyethylene, polyoxypropylene, and oxyethylene / oxypropylene copolymers.
The average degree of polymerization of polyoxyethylene or polyoxypropylene, oxyethylene / oxypropylene copolymer, and polyglycerin is, for example, about 8 to 15.
The polyorganosiloxane may be linear or branched. A plurality of polyorganosiloxane chains may be cross-linked. The silicone chain may be modified with an alkyl group.
 シリコーン界面活性剤のHLBは、好ましくは3~13、さらに好ましくは6~10である。 The HLB of the silicone surfactant is preferably 3 to 13, more preferably 6 to 10.
 シリコーン界面活性剤は、油剤に可溶性又は分散性であることが好ましい。また、室温で液体であることが好ましい。 It is preferable that the silicone surfactant is soluble or dispersible in the oil agent. Moreover, it is preferable that it is a liquid at room temperature.
 本発明において、シリコーン界面活性剤は、上記化合物の単独種の形態で用いることもできるし、複数種の混合物の形態で用いることも出来る。 In the present invention, the silicone surfactant can be used in the form of a single kind of the above compound, or in the form of a mixture of plural kinds.
 これらのシリコーン界面活性剤は、化粧料の原料として知られており、それらの何れも用いることができる。
 シリコーン界面活性剤は、市販のものを用いることができる。例えば、以下のような市販品を用いることができる。
・ SH3772M(PEG-12ジメチコン(ポリオキシエチレンタイプ)、HLB:6,東レ・ダウコーニング)
・ SH3773M(PEG-12ジメチコン(ポリオキシエチレンタイプ)、HLB:8,東レ・ダウコーニング)
・ FZ2222(ポリシリコーン-13(オキシエチレン・オキシプロピレンタイプ)、HLB:6,東レ・ダウコーニング)
・ KF6013(PEG-9ジメチコン((ポリオキシエチレンタイプ))、HLB:10,信越シリコーン)
・ KF6100(ポリグリセリルー3ジシロキサンジメチコン(ポリグリセリン)、信越シリコーン)
These silicone surfactants are known as cosmetic raw materials, and any of them can be used.
Commercially available silicone surfactants can be used. For example, the following commercially available products can be used.
・ SH3772M (PEG-12 dimethicone (polyoxyethylene type), HLB: 6, Toray Dow Corning)
・ SH3773M (PEG-12 dimethicone (polyoxyethylene type), HLB: 8, Toray Dow Corning)
・ FZ2222 (Polysilicone-13 (oxyethylene / oxypropylene type), HLB: 6, Toray Dow Corning)
・ KF6013 (PEG-9 dimethicone ((polyoxyethylene type)), HLB: 10, Shin-Etsu Silicone)
・ KF6100 (polyglyceryl 3 disiloxane dimethicone (polyglycerin), Shin-Etsu Silicone)
<1-3>粉体基材
 本発明における粉体基材としては、化粧料用の粉体として用いられているものであれば特に制限されず、粉体表面が親水性であっても疎水性であっても構わない。本発明における粉体基材としては、例えば、表面を処理されていても良い、マイカ、タルク、カオリン、合成雲母、炭酸カルシウム、炭酸マグネシウム、無水ケイ酸(シリカ)、酸化アルミニウム、硫酸バリウム等の粉体類;表面を処理されていても良い、ベンガラ、黄酸化鉄、黒酸化鉄、酸化コバルト、群青、紺青、酸化チタン、酸化亜鉛の無機顔料類;表面を処理されていても良い、雲母チタン、魚燐箔、オキシ塩化ビスマス等のパール剤類;レーキ化されていても良い赤色202号、赤色228号、赤色226号、黄色4号、青色404号、黄色5号、赤色505号、赤色230号、赤色223号、橙色201号、赤色213号、黄色204号、黄色203号、青色1号、緑色201号、紫色201号、赤色204号等の有機色素類;ポリエチレン末、ポリメタクリル酸メチル、ナイロン粉末、オルガノポリシロキサンエラストマー等の有機粉体類を用いることができる。
 また、上記粉体を2種以上含んだ混合粉体を用いることも可能である。
<1-3> Powder base material The powder base material in the present invention is not particularly limited as long as it is used as a powder for cosmetics. Even if the powder surface is hydrophilic, it is hydrophobic. May be sex. As the powder base material in the present invention, for example, mica, talc, kaolin, synthetic mica, calcium carbonate, magnesium carbonate, anhydrous silicic acid (silica), aluminum oxide, barium sulfate, etc. whose surface may be treated Powders; surface may be treated, bengara, yellow iron oxide, black iron oxide, cobalt oxide, ultramarine, bitumen, titanium oxide, zinc oxide inorganic pigments; surface may be treated, mica Pearls such as titanium, fish phosphorus foil, bismuth oxychloride; red 202, red 228, red 226, yellow 4, blue 404, yellow 5, red 505, which may be raked, Organic pigments such as red 230, red 223, orange 201, red 213, yellow 204, yellow 203, blue 1, blue 201, green 201, purple 201, red 204; Riechiren powder, can be used polymethyl methacrylate, nylon powder, organic powders such as organopolysiloxane elastomers.
It is also possible to use a mixed powder containing two or more of the above powders.
<1-4>水
 また、本発明の粉体組成物は水を含んでいても良い。この場合、粉体組成物全体における水の含有量は、好ましくは10質量%以下、より好ましくは0.05~5質量%、さらに好ましくは0.1~1質量%である。また、粉体組成物中における水と界面活性剤の重量比は、好ましくは1:1~1:20、より好ましくは1:2~1:10、さらに好ましくは1:3~1:5である。
<1-4> Water The powder composition of the present invention may contain water. In this case, the content of water in the whole powder composition is preferably 10% by mass or less, more preferably 0.05 to 5% by mass, and further preferably 0.1 to 1% by mass. The weight ratio of water to the surfactant in the powder composition is preferably 1: 1 to 1:20, more preferably 1: 2 to 1:10, and even more preferably 1: 3 to 1: 5. is there.
<1-5>水溶性の有効成分
 上述したように本発明の粉体組成物に水を含有させる場合には、同時に水溶性の有効成分を含有させることができる。すなわち、ラメラ相中の水分が保持されている層が親水性の有効成分を含有する形態とすることができる。
 このような形態とすることによって、有効成分を効率よく角質層に浸透させることにより、有効成分の持つ効果を高めることができる。
<1-5> Water-soluble active ingredient As described above, when water is contained in the powder composition of the present invention, a water-soluble active ingredient can be contained at the same time. That is, the layer in which water in the lamellar phase is retained can be in a form containing a hydrophilic active ingredient.
By setting it as such a form, the effect which an active ingredient has can be heightened by making an active ingredient penetrate | invade into a stratum corneum efficiently.
 ラメラ相中の水分が保持されている層への親水性の有効成分の取り込みは、通常化粧品、医薬品の分野で行われている方法により行うことができる。
 すなわち、有効成分を水に溶解し有効成分の水溶液を調製する。該水溶液と界面活性剤を撹拌混合することによって、水分が保持されている層に有効成分を含むラメラ相の分散溶液を得ることができる。
 そして、該分散溶液を用いて、後述する乾式製造方法又は湿式製造方法によって、水分が保持されている層に有効成分を含むラメラ相が複合化した粉体組成物を得ることができる。
Incorporation of the hydrophilic active ingredient into the layer in which water in the lamella phase is retained can be carried out by a method usually used in the cosmetics and pharmaceutical fields.
That is, the active ingredient is dissolved in water to prepare an aqueous solution of the active ingredient. By stirring and mixing the aqueous solution and the surfactant, a dispersion solution of a lamellar phase containing an active ingredient in a layer in which moisture is retained can be obtained.
And the powder composition which the lamellar phase which contains an active ingredient in the layer by which the water | moisture content was hold | maintained can be obtained by the dry manufacturing method or wet manufacturing method mentioned later using this dispersion solution.
 ラメラ相中の水分が保持されている層に含有させる水溶性の有効成分としては、皮膚外用剤に用いられるものであれば特に制限されないが、例えば、トラネキサム酸、及びグリチルリチン酸やその塩、アスコルビン酸、アスコルビン酸リン酸エステル、3-O-エチルアスコルビン酸、アスコルビン酸グルコシド或いはこれらの塩の様なアスコルビン酸類、アルブチン、ウルソール酸リン酸カリウムなどのウルソール酸塩、ピリドキシン、リボフラビン或いはこれらの塩の様なビタミンB類、ヒアルロン酸やその塩、フコイダン、硫酸化トレハロース或いはその塩、トレハロース、アミノ酸およびアミノ酸誘導体、エスクレチン配糖体、液状または固形状植物エキス等が好適に例示できる。
 特に、グリチルリチン酸ジカリウム、アスコルビン酸2-グルコシド、及びトラネキサム酸は、ラメラ相中の水分が保持されている層に含有させることにより、角層への浸透効率を著しく向上させることができる。
The water-soluble active ingredient to be contained in the layer in which the water in the lamella phase is retained is not particularly limited as long as it is used for an external preparation for skin. For example, tranexamic acid, glycyrrhizic acid and its salt, ascorbine Ascorbic acids such as acid, ascorbic acid phosphate ester, 3-O-ethylascorbic acid, ascorbic acid glucoside or salts thereof, ursolates such as arbutin and potassium ursolate phosphate, pyridoxine, riboflavin or salts thereof Preferred examples include vitamin B, hyaluronic acid and salts thereof, fucoidan, sulfated trehalose or salts thereof, trehalose, amino acids and amino acid derivatives, esculetin glycosides, liquid or solid plant extracts, and the like.
In particular, dipotassium glycyrrhizinate, 2-glucoside ascorbic acid, and tranexamic acid can be remarkably improved in the penetration efficiency into the stratum corneum by being contained in a layer in which water in the lamellar phase is retained.
<2>皮膚外用剤
 本発明は上記粉体組成物を含む皮膚外用剤にも関する。本発明の皮膚外用剤においては、本発明の効果を損ねない限度において、通常使用される任意成分を含有することもできる。この様な任意成分としては、例えば、マカデミアナッツ油、アボカド油、トウモロコシ油、オリーブ油、ナタネ油、ゴマ油、ヒマシ油、サフラワー油、綿実油、ホホバ油、ヤシ油、パーム油、液状ラノリン、硬化ヤシ油、硬化油、モクロウ、硬化ヒマシ油、ミツロウ、キャンデリラロウ、カルナウバロウ、イボタロウ、ラノリン、還元ラノリン、硬質ラノリン、ホホバロウ等のオイル、ワックス類;流動パラフィン、スクワラン、プリスタン、オゾケライト、パラフィン、セレシン、ワセリン、マイクロクリスタリンワックス等の炭化水素類;オレイン酸、イソステアリン酸、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、ウンデシレン酸等の高級脂肪酸類;セチルアルコール、ステアリルアルコール、イソステアリルアルコール、ベヘニルアルコール、オクチルドデカノール、ミリスチルアルコール、セトステアリルアルコール等の高級アルコール等;イソオクタン酸セチル、ミリスチン酸イソプロピル、イソステアリン酸ヘキシルデシル、アジピン酸ジイソプロピル、セバチン酸ジ-2-エチルヘキシル、乳酸セチル、リンゴ酸ジイソステアリル、ジ-2-エチルヘキサン酸エチレングリコール、ジカプリン酸ネオペンチルグリコール、ジ-2-ヘプチルウンデカン酸グリセリン、トリ-2-エチルヘキサン酸グリセリン、トリ-2-エチルヘキサン酸トリメチロールプロパン、トリイソステアリン酸トリメチロールプロパン、テトラ-2-エチルヘキサン酸ペンタンエリトリット等の合成エステル油類等の油剤類;脂肪酸セッケン(ラウリン酸ナトリウム、パルミチン酸ナトリウム等)、ラウリル硫酸カリウム、アルキル硫酸トリエタノールアミンエーテル等のアニオン界面活性剤類;塩化ステアリルトリメチルアンモニウム、塩化ベンザルコニウム、ラウリルアミンオキサイド等のカチオン界面活性剤類;イミダゾリン系両性界面活性剤(2-ココイル-2-イミダゾリニウムヒドロキサイド-1-カルボキシエチロキシ2ナトリウム塩等)、ベタイン系界面活性剤(アルキルベタイン、アミドベタイン、スルホベタイン等)、アシルメチルタウリン等の両性界面活性剤類;ソルビタン脂肪酸エステル類(ソルビタンモノステアレート、セスキオレイン酸ソルビタン等)、グリセリン脂肪酸類(モノステアリン酸グリセリン等)、プロピレングリコール脂肪酸エステル類(モノステアリン酸プロピレングリコール等)、硬化ヒマシ油誘導体、グリセリンアルキルエーテル、POEソルビタン脂肪酸エステル類(POEソルビタンモノオレエート、モノステアリン酸ポリオキエチレンソルビタン等)、POEソルビット脂肪酸エステル類(POE-ソルビットモノラウレート等)、POEグリセリン脂肪酸エステル類(POE-グリセリンモノイソステアレート等)、POE脂肪酸エステル類(ポリエチレングリコールモノオレート、POEジステアレート等)、POEアルキルエーテル類(POE2-オクチルドデシルエーテル等)、POEアルキルフェニルエーテル類(POEノニルフェニルエーテル等)、プルロニック型類、POE・POPアルキルエーテル類(POE・POP2-デシルテトラデシルエーテル等)、テトロニック類、POEヒマシ油・硬化ヒマシ油誘導体(POEヒマシ油、POE硬化ヒマシ油等)、ショ糖脂肪酸エステル、アルキルグルコシド等の非イオン界面活性剤類;ポリエチレングリコール、グリセリン、エリスリトール、ソルビトール、キシリトール、マルチトール、プロピレングリコール、2,4-ヘキサンジオール等の多価アルコール類;ピロリドンカルボン酸ナトリウム、乳酸、乳酸ナトリウム等の保湿成分類;パラアミノ安息香酸系紫外線吸収剤;アントラニル酸系紫外線吸収剤;サリチル酸系紫外線吸収剤;桂皮酸系紫外線吸収剤;ベンゾフェノン系紫外線吸収剤;糖系紫外線吸収剤;2-(2'-ヒドロキシ-5'-t-オクチルフェニル)ベンゾトリアゾール、4-メトキシ-4'-t-ブチルジベンゾイルメタン等の紫外線吸収剤類;エタノール、イソプロパノール等の低級アルコール類フェノキシエタノール等の抗菌剤などが好ましく例示できる。
<2> External preparation for skin The present invention also relates to an external preparation for skin containing the powder composition. The external preparation for skin of the present invention may contain any commonly used optional component as long as the effects of the present invention are not impaired. Examples of such optional ingredients include macadamia nut oil, avocado oil, corn oil, olive oil, rapeseed oil, sesame oil, castor oil, safflower oil, cottonseed oil, jojoba oil, coconut oil, palm oil, liquid lanolin, and hardened coconut oil. Oil, wax, oils such as beeswax, molasses, hydrogenated castor oil, beeswax, candelilla wax, carnauba wax, ibotarou, lanolin, reduced lanolin, hard lanolin, jojoba wax; liquid paraffin, squalane, pristane, ozokerite, paraffin, ceresin, petrolatum , Hydrocarbons such as microcrystalline wax; higher fatty acids such as oleic acid, isostearic acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, undecylenic acid; cetyl alcohol, stearyl alcohol, isostearyl Higher alcohols such as alcohol, behenyl alcohol, octyldodecanol, myristyl alcohol, cetostearyl alcohol; cetyl isooctanoate, isopropyl myristate, hexyldecyl isostearate, diisopropyl adipate, di-2-ethylhexyl sebacate, cetyl lactate, malic acid Diisostearyl, di-2-ethylhexanoic acid ethylene glycol, dicapric acid neopentyl glycol, di-2-heptyl undecanoic acid glycerin, tri-2-ethylhexanoic acid glycerin, tri-2-ethylhexanoic acid trimethylolpropane, tri Oil agents such as synthetic ester oils such as trimethylolpropane isostearate and pentane erythritol tetra-2-ethylhexanoate; fatty acid soap (sodium laurate) Anionic surfactants such as potassium lauryl sulfate, alkyl sulfate triethanolamine ether; cationic surfactants such as stearyltrimethylammonium chloride, benzalkonium chloride, laurylamine oxide; imidazoline-based amphoteric Amphoterics such as surfactants (2-cocoyl-2-imidazolinium hydroxide-1-carboxyethyloxy disodium salt, etc.), betaine surfactants (alkyl betaine, amide betaine, sulfobetaine, etc.), acylmethyl taurine, etc. Surfactants: sorbitan fatty acid esters (such as sorbitan monostearate and sorbitan sesquioleate), glycerin fatty acids (such as glyceryl monostearate), propylene glycol fatty acid esters (monostearic acid) Propylene glycol, etc.), hardened castor oil derivative, glycerin alkyl ether, POE sorbitan fatty acid esters (POE sorbitan monooleate, polyoxyethylene sorbitan monostearate, etc.), POE sorbite fatty acid esters (POE-sorbite monolaurate, etc.) POE glycerol fatty acid esters (POE-glycerol monoisostearate, etc.), POE fatty acid esters (polyethylene glycol monooleate, POE distearate, etc.), POE alkyl ethers (POE2-octyldodecyl ether, etc.), POE alkylphenyl ethers (POE nonylphenyl ether, etc.), Pluronic type, POE / POP alkyl ethers (POE / POP2-decyltetradecyl ether, etc.), Tetro Nonionic surfactants such as sucrose, POE castor oil / hardened castor oil derivatives (POE castor oil, POE hardened castor oil, etc.), sucrose fatty acid ester, alkyl glucoside; polyethylene glycol, glycerin, erythritol, sorbitol, xylitol , Polyhydric alcohols such as maltitol, propylene glycol, and 2,4-hexanediol; moisturizing ingredients such as sodium pyrrolidonecarboxylate, lactic acid, and sodium lactate; paraaminobenzoic acid ultraviolet absorbers; anthranilic acid ultraviolet absorbers; Salicylic acid UV absorbers; cinnamic acid UV absorbers; benzophenone UV absorbers; sugar UV absorbers; 2- (2′-hydroxy-5′-t-octylphenyl) benzotriazole, 4-methoxy-4 ′ -UV light such as t-butyldibenzoylmethane Adsorbents such; ethanol, lower alcohols antibacterial agents such phenoxyethanol such isopropanol can be preferably exemplified.
 また本発明の皮膚外用剤においては、本発明の効果を損ねない限度において、表面にラメラ相が付着していない粉体を含有させることができる。このような粉体基材としては、表面を処理されていても良い、マイカ、タルク、カオリン、合成雲母、炭酸カルシウム、炭酸マグネシウム、無水ケイ酸(シリカ)、酸化アルミニウム、硫酸バリウム等の粉体類;表面を処理されていても良い、ベンガラ、黄酸化鉄、黒酸化鉄、酸化コバルト、群青、紺青、酸化チタン、酸化亜鉛の無機顔料類;表面を処理されていても良い、雲母チタン、魚燐箔、オキシ塩化ビスマス等のパール剤類;レーキ化されていても良い赤色202号、赤色228号、赤色226号、黄色4号、青色404号、黄色5号、赤色505号、赤色230号、赤色223号、橙色201号、赤色213号、黄色204号、黄色203号、青色1号、緑色201号、紫色201号、赤色204号等の有機色素類;ポリエチレン末、ポリメタクリル酸メチル、ナイロン粉末、オルガノポリシロキサンエラストマー等の有機粉体類などが好ましく例示できる。 Further, the external preparation for skin of the present invention can contain a powder having no lamellar phase adhering to the surface as long as the effects of the present invention are not impaired. Such a powder base material may have a surface-treated powder such as mica, talc, kaolin, synthetic mica, calcium carbonate, magnesium carbonate, anhydrous silicic acid (silica), aluminum oxide, barium sulfate, etc. The surface may be treated, inorganic pigments such as bengara, yellow iron oxide, black iron oxide, cobalt oxide, ultramarine, bitumen, titanium oxide, zinc oxide; the surface may be treated, mica titanium, Pearl agents such as fish phosphorus foil, bismuth oxychloride; red 202, red 228, red 226, yellow 4, blue 404, yellow 5, red 505, red 230 which may be raked No., Red No. 223, Orange No. 201, Red No. 213, Yellow No. 204, Yellow No. 203, Blue No. 1, Green No. 201, Purple No. 201, Red No. 204, etc .; , Polymethyl methacrylate, nylon powder, organic powders such as organopolysiloxane elastomers and the like can be preferably exemplified.
<3>製造方法
 本発明の粉体組成物の製造方法は、油剤中で、界面活性剤を主とするラメラ相を粉体基材の表面に複合化させることを特徴とする。そして、本発明の好ましい形態では、油剤と界面活性剤と粉体基材を混合する工程を含む。
 以下、本発明の粉体組成物の製造方法に係る乾式製造方法と湿式製造方法の実施形態について詳述する。
<3> Manufacturing Method The manufacturing method of the powder composition of the present invention is characterized in that a lamellar phase mainly containing a surfactant is compounded on the surface of a powder base material in an oil agent. And in the preferable form of this invention, the process of mixing an oil agent, surfactant, and a powder base material is included.
Hereinafter, embodiments of a dry manufacturing method and a wet manufacturing method according to the method for manufacturing a powder composition of the present invention will be described in detail.
<3-1>乾式製造方法
 本発明の粉体組成物の乾式製造方法は、油剤と界面活性剤を混合し、ラメラ相分散溶液を得る工程と、ラメラ相分散溶液と粉体基材を混合する工程を含むことを特徴とする。
 本製造方法における油剤及び界面活性剤としては、上記<1-1>~<1-2>の項目で述べたものを用いることができる。また、本製造方法における粉体基材としては、上記<1-3>の項目で述べた粉体を用いることができ、かかる粉体を2種以上含む複合粉体を用いても良い。ラメラ相が複合化している粉体基材を2種以上含む粉体組成物を得たい場合には、混合粉体を用いることが好ましい。
<3-1> Dry Manufacturing Method The dry manufacturing method of the powder composition of the present invention includes a step of mixing an oil agent and a surfactant to obtain a lamellar phase dispersion solution, and a mixing of the lamellar phase dispersion solution and the powder base material. Including the step of:
As the oil agent and surfactant in this production method, those described in the above items <1-1> to <1-2> can be used. Further, as the powder base material in the present production method, the powder described in the above item <1-3> can be used, and a composite powder containing two or more kinds of such powders may be used. When it is desired to obtain a powder composition containing two or more powder base materials in which lamella phases are combined, it is preferable to use a mixed powder.
 以下<3-1-1>(1)~(3)においてラメラ相分散溶液を調整する方法について述べ、<3-1-2>においてラメラ相分散溶液と粉体基材を混合する工程について述べる。
<3-1-1>ラメラ相分散溶液の調製方法
(1)ラメラ相分散溶液の調製方法1
 油剤と界面活性剤を混合し、ラメラ相分散溶液を得る工程は、上述した界面活性剤、油剤、所望により水を混合して混合物を調製し、続いて該混合物を振とう又は撹拌することにより行うことができる。
 振とうは、振とう機等を用いて行うことができる。また、撹拌は、超音波分散機等を用いて行うことができる。
In the following, <3-1-1> (1) to (3) describe the method for preparing the lamella phase dispersion solution, and <3-1-2> describe the step of mixing the lamella phase dispersion solution and the powder base material. .
<3-1-1> Preparation Method of Lamellar Phase Dispersion Solution (1) Preparation Method 1 of Lamellar Phase Dispersion Solution
The step of mixing an oil agent and a surfactant to obtain a lamellar phase dispersion solution is performed by preparing a mixture by mixing the above-described surfactant, oil agent, and water as required, and then shaking or stirring the mixture. It can be carried out.
Shaking can be performed using a shaker or the like. Stirring can be performed using an ultrasonic disperser or the like.
(2)ラメラ相分散溶液の調製方法2
 また、ラメラ相分散溶液を得る工程は、界面活性剤を揮発性溶媒に溶解させて、第1の等方性溶液を得る工程と、前記第1の等方性溶液を油剤と混合し、第2の等方性溶液を得る工程と、前記第2の等方性溶液中の前記揮発性溶媒を揮発させる工程と、揮発性溶媒の揮発により行うことができる。
 この場合の揮発性溶媒については、下記<湿式製造方法>の項目において詳述するものを使用することができる。
 以下、ラメラ相分散溶液の調製方法2について図1を参照しながら説明する。
(2) Preparation method 2 of lamellar phase dispersion solution
Further, the step of obtaining a lamellar phase dispersion solution comprises dissolving a surfactant in a volatile solvent to obtain a first isotropic solution, mixing the first isotropic solution with an oil agent, 2 is a step of obtaining an isotropic solution, a step of volatilizing the volatile solvent in the second isotropic solution, and volatilization of the volatile solvent.
As the volatile solvent in this case, those described in detail in the following <Wet production method> can be used.
Hereinafter, the preparation method 2 of the lamellar phase dispersion solution will be described with reference to FIG.
 第1の等方性溶液における界面活性剤の含有量としては、界面活性剤が十分に溶解する範囲であればよい。例えば、界面活性剤の含有量は、10~90質量%を目安とすることができる。10質量%より少ない場合には、揮発性溶媒の揮発時間が長くなる場合があり、90質量%より多い場合には、溶液が粘稠性となり、溶解させにくくなる場合があるためである。 The content of the surfactant in the first isotropic solution may be in a range where the surfactant is sufficiently dissolved. For example, the content of the surfactant can be 10 to 90% by mass. This is because when the amount is less than 10% by mass, the volatilization time of the volatile solvent may become long, and when it exceeds 90% by mass, the solution becomes viscous and may be difficult to dissolve.
 また、第1の等方性溶液は、水を含んでいてもよい。
 揮発性溶媒の揮発によるラメラ相分散溶液の調製は、従来の物理的な撹拌によらずラメラ相を形成しようとするものであるため、物理的な撹拌による分散を助ける目的では水の存在は必要でなく、むしろ水が少ない系において、有用であるといえる。
 ただし、前記揮発性溶媒の揮発によるラメラ相分散溶液の調製において、水の存在はラメラ相の形成を補助し得る場合がある。
 これらの観点から、本発明においては、界面活性剤の1倍以下の質量の水を含んでいてもよい。また、この場合、界面活性剤を水と混合しておき、揮発性溶媒と混合することができる(図1(a))。もちろん、界面活性剤、水、揮発性溶媒を混合してもよい。
Further, the first isotropic solution may contain water.
Since the preparation of a lamellar phase dispersion solution by volatilization of a volatile solvent is intended to form a lamellar phase regardless of conventional physical stirring, the presence of water is necessary for the purpose of assisting dispersion by physical stirring. Rather, it can be said that it is useful in a system with little water.
However, in the preparation of a lamellar phase dispersion solution by volatilization of the volatile solvent, the presence of water may assist the formation of the lamellar phase.
From these viewpoints, the present invention may contain water having a mass of 1 or less that of the surfactant. In this case, the surfactant can be mixed with water and mixed with a volatile solvent (FIG. 1 (a)). Of course, you may mix surfactant, water, and a volatile solvent.
 前記揮発性溶媒の揮発によるラメラ相分散溶液の調製においては、前記界面活性剤1を前記揮発性溶媒2に溶解し、第1の等方性溶液3を調製する。この調製は、通常の混合、撹拌により行うことができる。
 界面活性剤1を前記揮発性溶媒2に溶解して得られる第1の等方性溶液3は、界面活性剤1が揮発性溶媒2中に単分散した状態、又は揮発性溶媒2中に界面活性剤1の逆ミセルなどの複合化体が形成した状態となる(図1(b))。
 このような等方性溶液は流動性が高いものであり、続く油剤との混合をしやすいものである。
In the preparation of a lamellar phase dispersion solution by volatilization of the volatile solvent, the surfactant 1 is dissolved in the volatile solvent 2 to prepare a first isotropic solution 3. This preparation can be performed by ordinary mixing and stirring.
The first isotropic solution 3 obtained by dissolving the surfactant 1 in the volatile solvent 2 is a state in which the surfactant 1 is monodispersed in the volatile solvent 2 or the interface in the volatile solvent 2. A complex such as reverse micelle of the active agent 1 is formed (FIG. 1B).
Such an isotropic solution has a high fluidity and is easy to mix with a subsequent oil agent.
 第2の等方性溶液を得る工程においては、前記第1の等方性溶液と、前記油剤との混合比は、製造されるラメラ相分散溶液における界面活性剤の含有量が、0.1~10質量%となる範囲とすることができる。 In the step of obtaining the second isotropic solution, the mixing ratio of the first isotropic solution and the oil agent is such that the surfactant content in the produced lamellar phase dispersion solution is 0.1. It can be in the range of ˜10% by mass.
 前記第1の等方性溶液3と油剤4を混合することにより、油剤4中に界面活性剤1が分散した等方性溶液(第2の等方性溶液)5を得ることができる。
 ここで、界面活性剤の油剤への分散の形態は、用いる揮発性溶媒の油剤に対する溶解性に応じて異なる。
 (i)揮発性溶媒2が油剤4に可溶である場合には、第1の等方性溶液3は油剤と相溶し、一相の溶液を形成する。すなわち、第1の等方性溶液3に含まれていた界面活性剤1は、一相の溶液2・4中に、単分散した状態、又は逆ミセルなどの複合化体が形成した状態で存在する(図1(c))。
 (ii)一方、揮発性溶媒2が油剤4に対して不溶又は難溶である場合には、第1の等方性溶液3は油剤4と相溶せず、二相の溶液を形成する。すなわち、油剤4の連続相中に、第1の等方性溶液3の粒子31が分散した状態となる(図1(d))。粒子31は、図1(d2)に示すように、界面活性剤1が揮発性溶媒2中に単分散した状態、又は揮発性溶媒2中に界面活性剤1の逆ミセルなどの複合化体が形成した状態となっている。
 なお、この状態は、混合の工程において、通常の振とう又は撹拌の操作により容易に形成することができる。
 また、界面活性剤として、油剤に難溶な成分と、油剤に可溶な成分を組み合わせて用いる場合には、油剤に難溶な成分を揮発性溶媒に溶解し、油剤に可溶な成分を油剤に溶解し、これらを混合することも可能である。
By mixing the first isotropic solution 3 and the oil agent 4, an isotropic solution (second isotropic solution) 5 in which the surfactant 1 is dispersed in the oil agent 4 can be obtained.
Here, the form of dispersion of the surfactant into the oil varies depending on the solubility of the volatile solvent used in the oil.
(I) When the volatile solvent 2 is soluble in the oil agent 4, the first isotropic solution 3 is compatible with the oil agent to form a one-phase solution. That is, the surfactant 1 contained in the first isotropic solution 3 is present in a monodispersed state or in a state where a complex such as reverse micelle is formed in the one- phase solutions 2 and 4. (FIG. 1 (c)).
(Ii) On the other hand, when the volatile solvent 2 is insoluble or hardly soluble in the oil agent 4, the first isotropic solution 3 is not compatible with the oil agent 4 and forms a two-phase solution. That is, the particles 31 of the first isotropic solution 3 are dispersed in the continuous phase of the oil agent 4 (FIG. 1D). As shown in FIG. 1 (d 2), the particles 31 are in a state where the surfactant 1 is monodispersed in the volatile solvent 2, or a complex such as reverse micelle of the surfactant 1 in the volatile solvent 2. It is in a formed state.
This state can be easily formed by a normal shaking or stirring operation in the mixing step.
In addition, when using a combination of a component that is sparingly soluble in an oil agent and a component that is soluble in an oil agent as a surfactant, the component that is sparingly soluble in the oil agent is dissolved in a volatile solvent. It is also possible to dissolve in an oil and mix them.
 揮発性溶媒を揮発させる工程において、揮発性溶媒の揮発は、常法により行うことができる。すなわち、減圧することにより揮発性溶媒を気化させることにより行うことができる。また、揮発性溶媒が気化する温度まで混合液を加温することにより行うことが可能である。揮発は、減圧下で行うことが好ましい。また、加温する場合には、ラメラ相を維持できる温度以下、すなわち相転移しない温度以下で加熱する。
 上述した第2の等方性溶液が二相を形成する場合には、振とう又は撹拌の操作により、油剤中に第1の等方性溶液を十分に分散させた後に、本工程に入ることが好ましい。
 また、揮発中に撹拌力を与えることも、微細なラメラ相を形成する観点から好ましい。
In the step of volatilizing the volatile solvent, the volatile solvent can be volatilized by a conventional method. That is, it can be performed by vaporizing the volatile solvent by reducing the pressure. Moreover, it is possible to carry out by heating a liquid mixture to the temperature which a volatile solvent vaporizes. Volatilization is preferably performed under reduced pressure. Moreover, when heating, it heats below the temperature which can maintain a lamellar phase, ie, below the temperature which does not phase-transform.
When the above-mentioned second isotropic solution forms two phases, the first isotropic solution is sufficiently dispersed in the oil by shaking or stirring, and then this step is entered. Is preferred.
It is also preferable to apply a stirring force during volatilization from the viewpoint of forming a fine lamellar phase.
 上記のとおり、揮発性溶媒2を揮発させることにより、第2の等方性溶液5を相転移させ、油剤4中にラメラ相7が分散したラメラ相分散溶液8を得ることができる(図1(e))。形成されるラメラ相の状態は単層、多層を問わない。ラメラ相が形成されていることの確認は、例えば、偏光下で顕微鏡観察を行うことにより確認することができる。 As described above, by volatilizing the volatile solvent 2, the second isotropic solution 5 is phase-shifted to obtain a lamellar phase dispersion solution 8 in which the lamellar phase 7 is dispersed in the oil agent 4 (FIG. 1). (E)). The state of the lamella phase formed may be either a single layer or multiple layers. Confirmation that the lamella phase is formed can be confirmed by performing microscopic observation under polarized light, for example.
(3)ラメラ相分散溶液の調製方法3
 上述した手法とは別に、ラメラ相分散溶液を得る工程は以下のようにして行うこともできる。すなわち、界面活性剤及び油剤を混合し、加熱して等方性溶液を得る工程と、前記等方性溶液を冷却する工程と、前記冷却により、前記界面活性剤を主とするラメラ相を形成させる工程によりラメラ相分散溶液を得ることができる。
 以下、ラメラ相分散溶液の調製方法3について図2を参照しながら説明する。
(3) Preparation method 3 of lamellar phase dispersion solution
Apart from the above-described method, the step of obtaining a lamellar phase dispersion solution can also be performed as follows. That is, a surfactant and an oil agent are mixed, heated to obtain an isotropic solution, a step of cooling the isotropic solution, and a lamellar phase mainly composed of the surfactant is formed by the cooling. A lamellar phase dispersion solution can be obtained by the process of making it.
Hereinafter, the preparation method 3 of the lamellar phase dispersion solution will be described with reference to FIG.
 界面活性剤及び油剤を混合し、加熱して等方性溶液を得る工程においては、界面活性剤と、前記油剤との混合比は、製造されるラメラ相分散溶液における界面活性剤の含有量が、0.1~10質量%となる範囲とすることができる。 In the step of mixing the surfactant and the oil agent and heating to obtain the isotropic solution, the mixing ratio of the surfactant and the oil agent is such that the content of the surfactant in the produced lamellar phase dispersion solution is as follows. The range may be 0.1 to 10% by mass.
 加熱は、界面活性剤のラメラ(図2(a))が相転移し、混合物が等方性溶液となるまで行えばよい。等方性溶液となっているか否かは、偏光板を通して溶液を観察することにより行うことができる。
 また、加熱により得られる等方性溶液は、一相であっても二相であってもよいが、一相になるまで加熱することがより好ましい(図2(b)参照、L1)。なお、前記油剤が2種以上の油剤を含む場合には、前記界面活性剤は、前記油剤の少なくとも1種と一相の等方性溶液を形成する温度まで行われることが好ましい。
 等方性溶液が一相であるか二相であるかは、一定の温度で放置することによる分離の有無の観察、又は溶液の光透過率測定法により区別することができる。
 上記混合物の相転移温度は、用いる界面活性剤、油剤の組合せにより異なる。従って、これらの組合せに応じて、相転移温度を考慮して加熱温度を調整すればよい。
 例えば、界面活性剤としてレシチンを用い、油剤としてスクワランを用いる場合には、65℃付近で、ラメラ相から二相の等方性溶液への相転移が見られ、90℃付近で二相の等方性溶液から一相の等方性溶液への相転移が見られる。従って、この場合の加熱温度は、好ましくは65℃以上、さらに好ましくは90℃以上を目安とすることができる。
 界面活性剤1と油剤2の混合物を加熱して得られる等方性溶液3は、油剤2中に二分子膜成分1の逆ミセルが形成した状態となる(図2(b))。
 なお、本実施形態では、一相の等方性溶液となるまで加熱する形態を示しているが、図2(c)に示すような二相の等方性溶液(L1+L2)となるまで加熱する形態であってもよい。レシチンとスクワランの組合せでは、油剤2中に界面活性剤1の逆ひも状ミセルなどを含む粘性が高い等方性溶液(L2)が、油剤(L1)と相分離した状態となる。
 二相の等方性溶液を形成した場合は、冷却前および/又は冷却中に攪拌し、分散状態を得ることが重要である。
Heating may be performed until the surfactant lamellar (FIG. 2A) undergoes phase transition and the mixture becomes an isotropic solution. Whether or not it is an isotropic solution can be determined by observing the solution through a polarizing plate.
Further, the isotropic solution obtained by heating may be one-phase or two-phase, but it is more preferable to heat it until it becomes one-phase (see FIG. 2B, L1). In addition, when the said oil agent contains 2 or more types of oil agents, it is preferable that the said surfactant is performed to the temperature which forms a one-phase isotropic solution with at least 1 type of the said oil agent.
Whether the isotropic solution is one-phase or two-phase can be distinguished by observing the presence or absence of separation by leaving it at a constant temperature, or by measuring the light transmittance of the solution.
The phase transition temperature of the mixture varies depending on the combination of surfactant and oil used. Therefore, the heating temperature may be adjusted in consideration of the phase transition temperature according to these combinations.
For example, when lecithin is used as a surfactant and squalane is used as an oil agent, a phase transition from a lamellar phase to a two-phase isotropic solution is observed at around 65 ° C., and a two-phase is obtained at around 90 ° C. A phase transition from an isotropic solution to a one-phase isotropic solution is seen. Accordingly, the heating temperature in this case is preferably 65 ° C. or higher, more preferably 90 ° C. or higher.
The isotropic solution 3 obtained by heating the mixture of the surfactant 1 and the oil agent 2 is in a state in which reverse micelles of the bilayer membrane component 1 are formed in the oil agent 2 (FIG. 2B).
In this embodiment, the heating is performed until a one-phase isotropic solution is obtained. However, the heating is performed until the two-phase isotropic solution (L1 + L2) as shown in FIG. 2C is obtained. Form may be sufficient. In the combination of lecithin and squalane, the highly viscous isotropic solution (L2) containing the reverse-like micelles of the surfactant 1 in the oil agent 2 is phase-separated from the oil agent (L1).
When a two-phase isotropic solution is formed, it is important to stir before cooling and / or during cooling to obtain a dispersed state.
 また、上記界面活性剤と油剤の混合物は、さらに水を含んでいてもよい。
 界面活性剤及び油剤の混合物を加熱し冷却してラメラ相分散溶液を得る工程は、従来の物理的な撹拌によらずラメラ相を形成しようとするものであるため、物理的な撹拌による分散を助ける目的では水の存在は必要でなく、むしろ水が少ない系において、有用であるといえる。
 ただし、後述する冷却によるラメラ相の形成において、水の存在はラメラ相の形成を補助し得る場合がある。
 これらの観点から、本発明においては、界面活性剤の1倍以下の質量の水を含んでいてもよい。
 水の含有量は小さいほど、等方性溶液への転移温度を低くすることができる。従って、本発明における製造効率を考慮した場合にも、水の含有量は小さい方が有利である。
In addition, the mixture of the surfactant and the oil may further contain water.
The process of heating and cooling the mixture of surfactant and oil to obtain a lamellar phase dispersion solution is intended to form a lamellar phase without using conventional physical agitation. For the purpose of helping, the presence of water is not necessary, but rather it is useful in systems with little water.
However, in the formation of the lamellar phase by cooling described later, the presence of water may assist the formation of the lamellar phase.
From these viewpoints, the present invention may contain water having a mass of 1 or less that of the surfactant.
The smaller the water content, the lower the transition temperature to the isotropic solution. Therefore, when the production efficiency in the present invention is taken into consideration, it is advantageous that the water content is small.
 等方性溶液を冷却する工程においては、冷却方法は特に制限されず、等方性溶液を室温以下の温度下に置く方法、冷媒により冷却する方法などが挙げられる。また、混合される等方性溶液より低い温度の希釈溶媒を混合することにより冷却することができる。例えば、希釈溶媒として、冷却した油剤を混合してもよい。
 冷却温度は、等方性溶液が相転移して、ラメラ相と油剤の共存相が形成する温度以下であればよい。目安として、室温程度まで冷却することが挙げられる。
 また、冷却中に撹拌力を与えることも、微細なラメラ相を形成する観点から好ましい。
 また、冷却の速度は大きくするほど(急冷するほど)微細なラメラ相を形成することが可能となるので、このような形態も好ましい。
In the step of cooling the isotropic solution, the cooling method is not particularly limited, and examples thereof include a method of placing the isotropic solution at a temperature below room temperature and a method of cooling with a refrigerant. Moreover, it can cool by mixing the dilution solvent of temperature lower than the isotropic solution mixed. For example, you may mix the cooled oil agent as a dilution solvent.
The cooling temperature may be equal to or lower than the temperature at which the isotropic solution undergoes phase transition and the coexisting phase of the lamellar phase and the oil agent is formed. As a guide, cooling to about room temperature can be mentioned.
Moreover, it is also preferable to give a stirring force during cooling from the viewpoint of forming a fine lamellar phase.
Moreover, since it becomes possible to form a fine lamella phase, so that the rate of cooling becomes large (it quenches rapidly), such a form is also preferable.
<3-1-2>ラメラ相分散溶液と粉体基材を混合する工程
 上記のようにして得られたラメラ相分散溶液と、粉体基材を混合する工程においては、粉体基材と油剤を混合する通常の方法により行うことができる。すなわち、粉体基材をパルベライザーで粉砕した後、ラメラ相分散溶液を添加しヘンシェルミキサーで混合することにより行うことができる。
 この時、ラメラ相分散溶液と粉体基材の混合比は、好ましくは1:99~30:70、より好ましくは2:98~20:80、さらに好ましくは3:97~15:85である。
<3-1-2> Step of mixing the lamellar phase dispersion solution and the powder base material In the step of mixing the lamellar phase dispersion solution obtained as described above and the powder base material, It can be carried out by a usual method of mixing oil. That is, it can be performed by pulverizing the powder base material with a pulverizer, adding a lamellar phase dispersion solution, and mixing with a Henschel mixer.
At this time, the mixing ratio of the lamellar phase dispersion solution and the powder base material is preferably 1:99 to 30:70, more preferably 2:98 to 20:80, and further preferably 3:97 to 15:85. .
<3-1-3>油剤を含まない粉体組成物の製造方法
 上述のラメラ相分散溶液と粉体基材を混合する工程の後に、粉体組成物中の油剤を揮発させる工程を踏むことで、油剤を含まない粉体組成物を製造することができる。この場合、油剤としては、揮発性油剤を用いる。前記揮発性油剤としては、軽質イソパラフィン、ジメチコン、シクロメチコンの何れかであって、沸点が150~250℃のものが例示できる。ジメチコンであれば、粘度に換算して1mPa・s以下のものがこれに相当する。この様な揮発性油剤には既に化粧料原料として市販されているものが存し、この様な化粧品原料を購入して利用することができる。この様な市販品の内、好ましいものとしては出光興産社製の「IPソルベント1620MU」、信越シリコーン社製の「シリコーンKF96-1」などが例示できる。
 ラメラ相分散溶液と粉体基材の混合物から、揮発性油剤を揮発させる工程は、50~100℃で6~48時間の送風条件で行うことが好ましく例示できる。
<3-1-3> Method for producing powder composition containing no oil agent After the step of mixing the above lamellar phase dispersion solution and the powder base material, a step of volatilizing the oil agent in the powder composition is taken. Thus, a powder composition containing no oil agent can be produced. In this case, a volatile oil agent is used as the oil agent. Examples of the volatile oil include light isoparaffin, dimethicone and cyclomethicone having a boiling point of 150 to 250 ° C. In the case of dimethicone, the viscosity is 1 mPa · s or less in terms of viscosity. Some of these volatile oils are already commercially available as cosmetic raw materials, and such cosmetic raw materials can be purchased and used. Among such commercially available products, preferable examples include “IP Solvent 1620MU” manufactured by Idemitsu Kosan Co., Ltd. and “Silicone KF96-1” manufactured by Shin-Etsu Silicone.
Preferably, the step of volatilizing the volatile oil from the mixture of the lamella phase dispersion solution and the powder base material is preferably performed at 50 to 100 ° C. for 6 to 48 hours.
 上記の方法により製造された組成物中でラメラ相が形成されていることの確認は、例えば、偏光下で顕微鏡観察を行うことにより確認することができる。 Confirmation that a lamellar phase is formed in the composition produced by the above method can be confirmed, for example, by observing under a polarized light under a microscope.
<3-2>湿式製造方法
 本発明の粉体組成物の湿式製造方法は、油剤と界面活性剤と揮発性溶媒と粉体基材を混合し、中間粉体組成物を得る工程と、前記中間粉体組成物中の前記揮発性溶媒を揮発させる工程と、を含むことを特徴とする。
 本製造方法における油剤及び界面活性剤としては、上記<1-1>~<1-2>で述べたものを用いることができる。また、本製造方法における粉体基材としては、上記<1-3>の項目で述べた粉体を用いることができ、かかる粉体を2種以上含む複合粉体を用いても良い。ラメラ相が複合化している粉体基材を2種以上含む粉体組成物を得たい場合には、混合粉体を用いることが好ましい。
<3-2> Wet manufacturing method The wet manufacturing method of the powder composition of the present invention comprises a step of mixing an oil agent, a surfactant, a volatile solvent, and a powder base material to obtain an intermediate powder composition, And volatilizing the volatile solvent in the intermediate powder composition.
As the oil agent and surfactant in this production method, those described in the above <1-1> to <1-2> can be used. Further, as the powder base material in the present production method, the powder described in the above item <1-3> can be used, and a composite powder containing two or more kinds of such powders may be used. When it is desired to obtain a powder composition containing two or more powder base materials in which lamella phases are combined, it is preferable to use a mixed powder.
 油剤と界面活性剤と揮発性溶媒と粉体基材を混合し、中間粉体組成物を得る工程においては、予め油剤と粉体基材を混合し、そこへ揮発性溶媒及び界面活性剤と所望により水を混合した溶液を添加し、撹拌混合することにより行うことができる。
 また、油剤と揮発性溶媒と界面活性剤と所望により水を混合した溶液を粉体基材に添加するようにしても良い。
 中間粉体組成物中における界面活性剤の含有量は好ましくは0.05~10質量%、より好ましくは0.1~5質量%、さらに好ましくは0.2~2質量%である。同じく中間粉体組成物中における油剤の含有量は好ましくは0.1~20質量%、より好ましくは0.5~15%、さらに好ましくは1~10質量%である。同じく中間粉体組成物中における揮発性溶媒の含有量は好ましくは10~70質量%、より好ましくは20~60質量%、さらに好ましくは30~50質量%である。そして中間粉体組成物中における粉体基材の含有量は好ましくは20~90質量%、より好ましくは30~80質量%、さらに好ましくは40~70質量%である。
In the step of mixing the oil agent, the surfactant, the volatile solvent, and the powder base material to obtain the intermediate powder composition, the oil agent and the powder base material are mixed in advance, and the volatile solvent and the surfactant are mixed therewith. If desired, a mixed solution of water can be added and mixed by stirring.
Moreover, you may make it add the solution which mixed the oil agent, the volatile solvent, surfactant, and water as needed to a powder base material.
The content of the surfactant in the intermediate powder composition is preferably 0.05 to 10% by mass, more preferably 0.1 to 5% by mass, and still more preferably 0.2 to 2% by mass. Similarly, the content of the oil agent in the intermediate powder composition is preferably 0.1 to 20% by mass, more preferably 0.5 to 15%, and further preferably 1 to 10% by mass. Similarly, the content of the volatile solvent in the intermediate powder composition is preferably 10 to 70% by mass, more preferably 20 to 60% by mass, and still more preferably 30 to 50% by mass. The content of the powder base material in the intermediate powder composition is preferably 20 to 90% by mass, more preferably 30 to 80% by mass, and further preferably 40 to 70% by mass.
 揮発性溶媒としては、例えば、メタノール、エタノール、プロパノール、イソプロパノールなどのアルコール類、ペンタン、ヘキサン、シクロペンタンなどの炭化水素類、ベンゼンなどの芳香族類、アセトンなどのケトン類、エーテル類、エステル類、デカメチルペンタシロキサン等の揮発性シリコーン油、フルオロカーボン類、イソパラフィン等が挙げられる。
 中でも、エタノール、プロパノール、アセトン等が好ましく用いられる。
Examples of the volatile solvent include alcohols such as methanol, ethanol, propanol and isopropanol, hydrocarbons such as pentane, hexane and cyclopentane, aromatics such as benzene, ketones such as acetone, ethers and esters. And volatile silicone oils such as decamethylpentasiloxane, fluorocarbons, isoparaffins and the like.
Of these, ethanol, propanol, acetone and the like are preferably used.
 湿式製造方法において、前記揮発性溶媒の揮発は、常法により行うことができる。すなわち、減圧による揮発性溶媒の気化により行うことができる。また、揮発性溶媒が気化する温度まで中間粉体組成物を加温することにより行うことが可能である。揮発は、減圧下で行うことが好ましい。また、加温する場合には、ラメラ相を維持できる温度以下、すなわち相転移しない温度以下で加熱する。 In the wet manufacturing method, the volatile solvent can be volatilized by a conventional method. That is, it can be carried out by vaporizing a volatile solvent under reduced pressure. It can also be carried out by heating the intermediate powder composition to a temperature at which the volatile solvent vaporizes. Volatilization is preferably performed under reduced pressure. Moreover, when heating, it heats below the temperature which can maintain a lamellar phase, ie, below the temperature which does not phase-transform.
 上記油剤として揮発性油剤を用いれば、前期揮発性溶媒の揮発の工程によって同時に該揮発性油剤を揮発させることで油剤を含まない粉体組成物を製造することができる。揮発性油剤としては、上記<3-1-3>で述べたものを使用することができる。 If a volatile oil agent is used as the oil agent, a powder composition containing no oil agent can be produced by volatilizing the volatile oil agent simultaneously by the volatilization step of the volatile solvent. As the volatile oil, those described in the above <3-1-3> can be used.
<4>皮膚外用剤の製造方法
 本発明の製造方法により製造した粉体組成物は、皮膚外用剤の原料として用いることができる。もちろん、このような方法により製造した粉体組成物をそのまま皮膚外用剤として用いることもできる。
 この場合皮膚外用剤としては、ファンデーション、チーク、アイシャドウ、ルースパウダーやプレストパウダーのようなパウダー化粧料が挙げられる。
<4> Manufacturing method of skin external preparation The powder composition manufactured by the manufacturing method of this invention can be used as a raw material of a skin external preparation. Of course, the powder composition manufactured by such a method can also be used as a skin external preparation as it is.
In this case, examples of the external preparation for skin include powder cosmetics such as foundation, teak, eye shadow, loose powder and pressed powder.
<1>乾式製造方法
 乾式製造方法により本発明の粉体組成物を含むパウダー化粧料を製造した。
(実施例1)
 以下の処方によりパウダーファンデーションを製造した。
 
  (A)シリコーン処理顔料色素(酸化チタン、酸化鉄)  15
  (A)シリコーン処理タルク              37.7
  (A)メタクリル酸メチルクロスポリマー        15
  (A)フッ素処理マイカ                10
  (A)フッ素処理セリサイト              10
  (A)メチルパラベン                  0.3
  (B)ラメラ相分散溶液                12
   (C)シリコーン界面活性剤              1.6
   (C)水                       0.4
   (D)エチルヘキサン酸セチル             2
   (D)ジメチコン                   8
(単位:質量%)
 
(C)、(D)群を混合し、80℃で加熱溶解したのち、溶液を冷却することでラメラ相分散溶液(B)を予め調製した。(A)群の成分を混合してパルベライザーで粗粉砕した後、(B)を添加しヘンシェルミキサーで混合した。その後、再びパルベライザーで粉砕し、金皿に打型してパウダーファンデーションを製造した。
<1> Dry production method A powder cosmetic containing the powder composition of the present invention was produced by a dry production method.
Example 1
A powder foundation was produced according to the following formulation.

(A) Silicone-treated pigment dye (titanium oxide, iron oxide) 15
(A) Silicone-treated talc 37.7
(A) Methyl methacrylate cross polymer 15
(A) Fluorine-treated mica 10
(A) Fluorine-treated sericite 10
(A) Methylparaben 0.3
(B) Lamellar phase dispersion solution 12
(C) Silicone surfactant 1.6
(C) Water 0.4
(D) Cetyl ethylhexanoate 2
(D) Dimethicone 8
(Unit:% by mass)

The (C) and (D) groups were mixed and dissolved by heating at 80 ° C., and then the solution was cooled to prepare a lamellar phase dispersion solution (B) in advance. After mixing the components of (A) group and coarsely pulverizing with a pulverizer, (B) was added and mixed with a Henschel mixer. Thereafter, it was pulverized again with a pulverizer and cast into a metal pan to produce a powder foundation.
(実施例2)
 以下の処方によりルースパウダーを製造した。
 
  (A)シリコーン酸処理顔料色素(酸化チタン、酸化鉄)  1
  (A)アミノ酸処理タルク               60.7
  (A)メタクリル酸メチルクロスポリマー        10
  (A)マイカ                     10
  (A)シリコーン樹脂粉末               10
  (A)メチルパラベン                  0.3
  (B)ラメラ相分散溶液                 4
   (C)レシチン(Epikuron 200)      0.6
   (C)10%水酸化カリウム水溶液           0.3
   (C)アスコルビン酸グルコシド            0.1
   (D)エチルヘキサン酸セチル             3
(単位:質量%)
 
(C)、(D)群を混合して、超音波分散でラメラ相分散溶液(B)を得た。(A)群の成分を混合してパルベライザーで粗粉砕した後、(B)を添加しヘンシェルミキサーで混合した。その後、再びパルベライザーで粉砕して、ルースパウダーを製造した。
(Example 2)
Loose powder was produced according to the following formulation.

(A) Silicone acid-treated pigment dye (titanium oxide, iron oxide) 1
(A) Amino acid-treated talc 60.7
(A) Methyl methacrylate cross polymer 10
(A) Mica 10
(A) Silicone resin powder 10
(A) Methylparaben 0.3
(B) Lamella phase dispersion solution 4
(C) Lecithin (Epikuron 200) 0.6
(C) 10% aqueous potassium hydroxide solution 0.3
(C) Ascorbic acid glucoside 0.1
(D) Ethyl hexanoate cetyl 3
(Unit:% by mass)

The (C) and (D) groups were mixed to obtain a lamellar phase dispersion solution (B) by ultrasonic dispersion. After mixing the components of (A) group and coarsely pulverizing with a pulverizer, (B) was added and mixed with a Henschel mixer. After that, the powder was pulverized again to produce loose powder.
<2>湿式製造方法
 湿式製造方法により本発明の粉体組成物を含むパウダー化粧料を製造した。
(実施例3)
 以下の処方によりパウダーファンデーションを製造した。
 
  (A)パウダーファンデーション母体          95
   (B)シリコーン処理顔料色素(酸化チタン、酸化鉄) 15
   (B)シリコーン処理タルク             47.7
   (B)メタクリル酸メチルクロスポリマー       10
   (B)タルク/酸化チタン/アルミナ/シリカ混合粉体  5
   (B)雲母チタン                  10
   (B)メチルパラベン                 0.3
   (C)エチルヘキサン酸セチル             7
  (D)中間溶液                    65
   (E)レシチン(Epikuron 200)      3
   (E)水                       2
   (F)エタノール                  60
(単位:質量%)
 
(E)、(F)群を混合して、室温にて撹拌溶解した溶液(D)を予め調製した。(B)群の成分を混合してパルベライザーで粗粉砕した後、(C)を添加しヘンシェルミキサーで混合した。その後、再びパルベライザーで粉砕して(A)を得た。(A)と(D)とを十分に混合し、40℃でエタノールを揮発させて得たサンプルを金皿に打型してパウダーファンデーションを製造した。
<2> Wet manufacturing method The powder cosmetics containing the powder composition of this invention were manufactured with the wet manufacturing method.
Example 3
A powder foundation was produced according to the following formulation.

(A) Powder foundation matrix 95
(B) Silicone-treated pigment dye (titanium oxide, iron oxide) 15
(B) Silicone-treated talc 47.7
(B) Methyl methacrylate cross polymer 10
(B) Talc / Titanium oxide / Alumina / Silica mixed powder 5
(B) Mica titanium 10
(B) Methylparaben 0.3
(C) Cetyl ethylhexanoate 7
(D) Intermediate solution 65
(E) Lecithin (Epikuron 200) 3
(E) Water 2
(F) Ethanol 60
(Unit:% by mass)

A solution (D) in which the groups (E) and (F) were mixed and dissolved by stirring at room temperature was prepared in advance. (B) The components of the group were mixed and coarsely pulverized with a pulverizer, and then (C) was added and mixed with a Henschel mixer. Thereafter, the mixture was again pulverized with a pulverizer to obtain (A). (A) and (D) were mixed thoroughly, and a sample obtained by volatilizing ethanol at 40 ° C. was molded into a metal pan to produce a powder foundation.
<3>ラメラ相の観察
 上記の実施例1~3のパウダー化粧料について、粉体基材の表面がラメラ相によりコーティングされているか否かについて観察した。ラメラ相の状態評価には、ラメラ相の異方性を観察できる偏光顕微鏡、及びラメラ構造の規則構造を断定できる小角X線散乱を用いた。小角X線散乱を行う際には、対照実験としてレシチン(Epikuron200)と水を8:2で混合したラメラ相分散溶液の観察も行った。
 偏光顕微鏡による観察の結果、実施例1~3のパウダー化粧料における粉体基材は、ラメラ相によりコーティングされていることが確認できた。
 また、小角X線散乱の結果、実施例1~3のパウダー化粧料の何れにおいても、ピーク比が1:2となるラメラ相特有の散乱スペクトルが観察された。図3にラメラ相分散溶液、図4に実施例3のパウダー化粧料の小角X線散乱スペクトルを示す。
<3> Observation of Lamellar Phase Regarding the powder cosmetics of Examples 1 to 3 above, whether the surface of the powder base material was coated with the lamellar phase was observed. For the evaluation of the state of the lamella phase, a polarizing microscope that can observe the anisotropy of the lamella phase and small-angle X-ray scattering that can determine the regular structure of the lamella structure were used. When small-angle X-ray scattering was performed, a lamellar phase dispersion solution in which lecithin (Epikuron 200) and water were mixed at 8: 2 was also observed as a control experiment.
As a result of observation with a polarizing microscope, it was confirmed that the powder base material in the powder cosmetics of Examples 1 to 3 was coated with a lamellar phase.
As a result of small-angle X-ray scattering, a scattering spectrum peculiar to the lamellar phase having a peak ratio of 1: 2 was observed in any of the powder cosmetics of Examples 1 to 3. FIG. 3 shows a lamellar phase dispersion solution, and FIG. 4 shows a small-angle X-ray scattering spectrum of the powder cosmetic of Example 3.
<4>試験例
(1)閉塞性の検討
 以下の方法により、本発明の粉体組成物である粉体試料1を調製した。
 レシチン(Epikuron 200)3質量部、水2質量部、及びエタノール60質量部を混合して、室温にて撹拌溶解した中間溶液を調製した。
 タルク88質量部をパルベライザーにて粉砕し、ここへエチルヘキサン酸セチル7質量部を添加し、ヘンシェルミキサーで混合した。その後、再びパルベライザーで粉砕して混合粉体を調製した。
 中間溶液65質量部と、混合粉体95質量部とを十分に混合し、40℃でエタノールを揮発させることで、粉体試料1を調製した。
 図5に、粉体試料1を透過型電子顕微鏡によって撮影した写真を示す。図5に示す通り、粉体試料1においては、タルクの表面にラメラ相が複合化している。
 なお、パルベライザーで粉砕した後に何ら処理を施していないタルクを比較試料1として調製した。
<4> Test Example (1) Examination of Occlusion A powder sample 1 which is a powder composition of the present invention was prepared by the following method.
An intermediate solution was prepared by mixing 3 parts by mass of lecithin (Epicuron 200), 2 parts by mass of water, and 60 parts by mass of ethanol and stirring and dissolving at room temperature.
88 parts by mass of talc was pulverized with a pulverizer, 7 parts by mass of cetyl ethylhexanoate was added thereto, and mixed with a Henschel mixer. Thereafter, the mixture was again pulverized to prepare a mixed powder.
A powder sample 1 was prepared by thoroughly mixing 65 parts by mass of the intermediate solution and 95 parts by mass of the mixed powder and volatilizing ethanol at 40 ° C.
FIG. 5 shows a photograph of the powder sample 1 taken with a transmission electron microscope. As shown in FIG. 5, in the powder sample 1, the lamellar phase is compounded on the surface of talc.
In addition, talc which was not subjected to any treatment after being pulverized by a pulverizer was prepared as a comparative sample 1.
 粉体試料1の閉塞性を以下の通りカップ法により評価した。
 カップに水を入れ、開口部を塞ぐように皮脂成分(オレイン酸)で湿らせた濾紙を載せた。濾紙が含む皮脂成分と同量の比較試料1、又は粉体試料1をさらに濾紙に塗布した。そして、カップを35℃に放置し、水の蒸散速度を算出した。
 その結果、比較試料1を塗布した場合の水分蒸散速度は、8.6mg/cm/hであった。一方、粉体試料1を塗布した場合の水分蒸散速度は、4.6mg/cm/hであった(図6)。
 この結果は、粉体試料1は水分の閉塞性に優れていることを示している。
 以上より、本発明の粉体組成物は肌からの水分蒸散を防ぐことができ、保湿性に優れることがわかった。
The plugability of the powder sample 1 was evaluated by the cup method as follows.
Water was put into the cup, and filter paper moistened with a sebum component (oleic acid) was placed so as to close the opening. Comparative sample 1 or powder sample 1 in the same amount as the sebum component contained in the filter paper was further applied to the filter paper. Then, the cup was left at 35 ° C., and the water evaporation rate was calculated.
As a result, the water evaporation rate when the comparative sample 1 was applied was 8.6 mg / cm 2 / h. On the other hand, the moisture evaporation rate when the powder sample 1 was applied was 4.6 mg / cm 2 / h (FIG. 6).
This result has shown that the powder sample 1 is excellent in the obstruction | occlusion property of a water | moisture content.
From the above, it was found that the powder composition of the present invention can prevent moisture transpiration from the skin and is excellent in moisture retention.
(2)保湿性の検討
 表1の処方に従って、本発明の皮膚外用剤であるラメラ相コーティングファンデーション(LPF)と、比較のための皮膚外用剤であるスクワランコーティングファンデーション(SQPF)を、実施例3に準じた方法により調製した。
(2) Examination of moisturizing properties According to the formulation of Table 1, lamellar phase coating foundation (LPF) which is an external preparation for skin of the present invention and squalane coating foundation (SQPF) which is an external preparation for comparison are described in Example 3. It was prepared by the method according to
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
 LPFとSQPFの保湿性は以下のように評価した。
 被験者20名の、顔面の肌の水分量をSKICON EX-200で測定した。次に、20%グリセリン水溶液を全顔に塗布し、LPFとSQPFを半顔ずつ塗布した。塗布から4時間後、クレンジングと洗顔料で全顔を洗浄し、水分量を測定した。
 その結果、LPF及びSQPFの塗布前の肌の水分量を1とした場合の、塗布後の肌の水分量はそれぞれ1.21及び1.04であった(図7)。
 この結果は、本発明の皮膚外用剤は肌の保湿性に優れることを示している。
The moisturizing properties of LPF and SQPF were evaluated as follows.
The water content of the facial skin of 20 subjects was measured with SKICON EX-200. Next, 20% glycerin aqueous solution was applied to the entire face, and LPF and SQPF were applied to each half face. Four hours after application, the entire face was washed with cleansing and face wash, and the moisture content was measured.
As a result, when the moisture content of the skin before application of LPF and SQPF was 1, the moisture content of the skin after application was 1.21 and 1.04, respectively (FIG. 7).
This result has shown that the skin external preparation of this invention is excellent in the moisture retention of skin.
(3)乾燥感の感じにくさ
 LPFとSQPFについて以下の方法により乾燥感の感じにくさを評価した。
 被験者20名にLPFとSQPFをそれぞれ使用させ、乾燥感を感じにくいファンデーションを選択させるアンケートを実施した。その結果、LPFと答えた被験者は14名で、SQPFと答えた被験者は5名、同等と答えた被験者は1名だった。
 この結果は、本発明の皮膚外用剤は使用時に乾燥感を感じにくいことを示している。
(3) Difficulty in feeling of dryness For LPF and SQPF, the difficulty of feeling of dryness was evaluated by the following method.
A questionnaire was conducted in which 20 subjects used LPF and SQPF respectively, and selected a foundation that did not feel dry. As a result, 14 subjects replied LPF, 5 subjects replied SQPF, and 1 subject replied.
This result indicates that the external preparation for skin of the present invention hardly feels dry when used.
(4)水溶性の有効成分の角層への浸透量の評価
 以下の方法で粉体試料2及び比較試料2を調製した。
 レシチン(Epikuron 200)3質量部、グリチルリチン酸ジカリウム0.5質量部、純水1.5質量部、及びエタノール60質量部を混合して、室温にて撹拌溶解した中間溶液を調製した。
 タルク88質量部をパルベライザーにて粉砕し、ここへエチルヘキサン酸セチル7質量部を添加し、ヘンシェルミキサーで混合した。その後、再びパルベライザーで粉砕して混合粉体を調製した。
 中間溶液65質量部と、混合粉体95質量部とを十分に混合し、40℃でエタノールを揮発させることで、粉体試料2を調製した。
 また、グリチルリチン酸ジカリウム0.5質量部と、99.5質量部の比較試料1を混合することにより、比較試料2を調製した。
(4) Evaluation of penetration amount of water-soluble active ingredient into stratum corneum Powder sample 2 and comparative sample 2 were prepared by the following method.
3 parts by mass of lecithin (Epicuron 200), 0.5 parts by mass of dipotassium glycyrrhizinate, 1.5 parts by mass of pure water, and 60 parts by mass of ethanol were mixed to prepare an intermediate solution that was stirred and dissolved at room temperature.
88 parts by mass of talc was pulverized with a pulverizer, 7 parts by mass of cetyl ethylhexanoate was added thereto, and mixed with a Henschel mixer. Thereafter, the mixture was again pulverized to prepare a mixed powder.
A powder sample 2 was prepared by sufficiently mixing 65 parts by mass of the intermediate solution and 95 parts by mass of the mixed powder and volatilizing ethanol at 40 ° C.
Moreover, comparative sample 2 was prepared by mixing 0.5 parts by mass of dipotassium glycyrrhizinate and 99.5 parts by mass of comparative sample 1.
 12名の被験者の前腕部に、粉体試料2及び比較試料2をそれぞれ5mg/cm塗布し、フィルムで固定化した。6時間後に粉体試料2及び比較試料2をふき取り、テープストリッピングで角層を採取し、HPLCでグリチルリチン酸ジカリウムを定量分析した。
 その結果、粉体試料2及び比較試料2を塗布した時のグリチルリチン酸ジカリウムの角層への浸透量は、それぞれ、0.28μg/cm、0.19μg/cmであった。
 この結果は、本発明の粉体組成物によれば、水溶性の有効成分の角層への浸透効率を高めることができることを示している。
The powder sample 2 and the comparative sample 2 were each applied at 5 mg / cm 2 to the forearms of 12 subjects and fixed with a film. After 6 hours, the powder sample 2 and the comparative sample 2 were wiped off, the stratum corneum was collected by tape stripping, and dipotassium glycyrrhizinate was quantitatively analyzed by HPLC.
As a result, penetration of the stratum corneum of dipotassium glycyrrhizinate when the powder sample 2 and comparative sample 2 was applied, respectively, 0.28 .mu.g / cm 2, was 0.19μg / cm 2.
This result shows that according to the powder composition of the present invention, the penetration efficiency of the water-soluble active ingredient into the stratum corneum can be increased.
 本発明は保湿性に優れたパウダー化粧料に応用できる。 The present invention can be applied to powder cosmetics having excellent moisture retention.

Claims (14)

  1. 油剤と界面活性剤と粉体基材を含み、前記粉体基材の表面に前記界面活性剤を主とするラメラ相が複合化していることを特徴とする、粉体組成物。 A powder composition comprising an oil agent, a surfactant, and a powder base material, wherein a lamellar phase mainly comprising the surfactant is complexed on a surface of the powder base material.
  2. 前記油剤が、シリコーン油、炭化水素油、エステル油、天然動植物油、フッ素油から選ばれる請求項1に記載の粉体組成物。 The powder composition according to claim 1, wherein the oil agent is selected from silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.
  3. さらに、水を含む、請求項1又は2に記載の粉体組成物。 Furthermore, the powder composition of Claim 1 or 2 containing water.
  4. さらに、水溶性の有効成分を含む、請求項3に記載の粉体組成物。 Furthermore, the powder composition of Claim 3 containing a water-soluble active ingredient.
  5. 前記界面活性剤は、レシチン及び/又は非イオン界面活性剤を含む、請求項1~4の何れかに記載の粉体組成物。 The powder composition according to any one of claims 1 to 4, wherein the surfactant comprises lecithin and / or a nonionic surfactant.
  6. 請求項1~5の何れかに記載の粉体組成物を含む、皮膚外用剤。 An external preparation for skin comprising the powder composition according to any one of claims 1 to 5.
  7. 油剤中で、界面活性剤を主とするラメラ相を粉体基材の表面に複合化させることを特徴とする、請求項1~6の何れかに記載の粉体組成物の製造方法。 The method for producing a powder composition according to any one of claims 1 to 6, wherein a lamellar phase mainly comprising a surfactant is compounded on the surface of the powder base material in an oil agent.
  8. 油剤と界面活性剤と粉体基材を混合する工程を含む、請求項7に記載の粉体組成物の製造方法。 The manufacturing method of the powder composition of Claim 7 including the process of mixing an oil agent, surfactant, and a powder base material.
  9. 油剤と界面活性剤を混合し、ラメラ相分散溶液を得る工程と、
    前記ラメラ相分散溶液と粉体基材を混合する工程を含むことを特徴とする、請求項7又は8に記載の粉体組成物の製造方法。
    A step of mixing an oil agent and a surfactant to obtain a lamellar phase dispersion solution;
    The method for producing a powder composition according to claim 7 or 8, comprising a step of mixing the lamellar phase dispersion solution and a powder base material.
  10. 油剤と界面活性剤と揮発性溶媒と粉体基材を混合し、中間粉体組成物を得る工程と、
    前記中間粉体組成物中の前記揮発性溶媒を揮発させる工程と、
    を含むことを特徴とする、請求項7又は8に記載の粉体組成物の製造方法。
    Mixing an oil agent, a surfactant, a volatile solvent, and a powder base material to obtain an intermediate powder composition;
    Volatilizing the volatile solvent in the intermediate powder composition;
    The method for producing a powder composition according to claim 7 or 8, characterized by comprising:
  11.  前記揮発性溶媒が、アルコール類、炭化水素類、芳香族類、ケトン類、エーテル類、エステル類、揮発性シリコーン油、イソパラフィンから選ばれる、請求項10に記載の粉体組成物の製造方法。 The method for producing a powder composition according to claim 10, wherein the volatile solvent is selected from alcohols, hydrocarbons, aromatics, ketones, ethers, esters, volatile silicone oil, and isoparaffin.
  12.  前記揮発性溶媒の揮発は、減圧下で行われる、請求項10又は11に記載の粉体組成物の製造方法。 The method for producing a powder composition according to claim 10 or 11, wherein the volatile solvent is volatilized under reduced pressure.
  13.  請求項7~12の何れかに記載の粉体組成物の製造方法により製造された粉体組成物を、他の成分と混合する工程を含む、皮膚外用剤の製造方法。 A method for producing an external preparation for skin, comprising a step of mixing the powder composition produced by the method for producing a powder composition according to any one of claims 7 to 12 with other components.
  14. 表面に界面活性剤を主とするラメラ相が複合化している粉体基材を含む粉体組成物を製造する方法であって、
     油剤中で、界面活性剤を主とするラメラ相を粉体基材の表面に複合化させることを特徴とする、粉体組成物の製造方法。
    A method for producing a powder composition comprising a powder base material in which a lamellar phase mainly comprising a surfactant is complexed on the surface,
    A method for producing a powder composition, comprising laminating a lamellar phase mainly comprising a surfactant on the surface of a powder base material in an oil agent.
PCT/JP2014/082293 2013-12-18 2014-12-05 Powder composition which contains powder composited with lamellar phase, and process for manufacturing same WO2015093324A1 (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0848612A (en) * 1994-08-05 1996-02-20 Noevir Co Ltd Humectant powder and powdery cosmetic containing the same powder
JPH09175931A (en) * 1995-12-21 1997-07-08 L'oreal Sa Microparticles coated with lamellar phase based on silicone surfactant and composition containing the same
JP2001213722A (en) * 1999-11-25 2001-08-07 Shiseido Co Ltd Method of manufacturing solid powder cosmetic
JP2002020236A (en) * 2000-05-19 2002-01-23 L'oreal Sa Composition for make-up and/or make-up care in powdery form and containing specific binder
JP2006056851A (en) * 2004-08-23 2006-03-02 Shu Uemura:Kk Cosmetic
WO2006028311A1 (en) * 2004-09-07 2006-03-16 Lg Household & Health Care Ltd. Cosmetic powder, its preparing method and make-up cosmetic composition comprising the same
WO2014103742A1 (en) * 2012-12-25 2014-07-03 ポーラ化成工業株式会社 Reverse vesicle composition and method for producing same

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0848612A (en) * 1994-08-05 1996-02-20 Noevir Co Ltd Humectant powder and powdery cosmetic containing the same powder
JPH09175931A (en) * 1995-12-21 1997-07-08 L'oreal Sa Microparticles coated with lamellar phase based on silicone surfactant and composition containing the same
JP2001213722A (en) * 1999-11-25 2001-08-07 Shiseido Co Ltd Method of manufacturing solid powder cosmetic
JP2002020236A (en) * 2000-05-19 2002-01-23 L'oreal Sa Composition for make-up and/or make-up care in powdery form and containing specific binder
JP2006056851A (en) * 2004-08-23 2006-03-02 Shu Uemura:Kk Cosmetic
WO2006028311A1 (en) * 2004-09-07 2006-03-16 Lg Household & Health Care Ltd. Cosmetic powder, its preparing method and make-up cosmetic composition comprising the same
WO2014103742A1 (en) * 2012-12-25 2014-07-03 ポーラ化成工業株式会社 Reverse vesicle composition and method for producing same

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