WO2022220027A1 - Production method for solid composition, solid composition, and cosmetic - Google Patents

Production method for solid composition, solid composition, and cosmetic Download PDF

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Publication number
WO2022220027A1
WO2022220027A1 PCT/JP2022/013266 JP2022013266W WO2022220027A1 WO 2022220027 A1 WO2022220027 A1 WO 2022220027A1 JP 2022013266 W JP2022013266 W JP 2022013266W WO 2022220027 A1 WO2022220027 A1 WO 2022220027A1
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Prior art keywords
solid composition
wax
slurry
producing
composition according
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PCT/JP2022/013266
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French (fr)
Japanese (ja)
Inventor
健斗 鈴木
希佳 高橋
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株式会社資生堂
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Priority to JP2023514542A priority Critical patent/JPWO2022220027A1/ja
Publication of WO2022220027A1 publication Critical patent/WO2022220027A1/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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/31Hydrocarbons
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • 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
    • A61K8/60Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • 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
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • A61Q1/08Preparations containing skin colorants, e.g. pigments for cheeks, e.g. rouge
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • A61Q1/10Preparations containing skin colorants, e.g. pigments for eyes, e.g. eyeliner, mascara
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/12Face or body powders for grooming, adorning or absorbing

Definitions

  • the present invention relates to a method for producing a solid composition, a solid composition, and a cosmetic.
  • Patent Document 1 a cosmetic base material containing an organic layered powder and an oil agent is mixed with a solvent such as silicone oil, the mixture is filled in a container, and the solvent is removed in a liquid state.
  • a solid powder cosmetic is disclosed.
  • Non-volatile solvents such as silicone oil are difficult to remove during the production of cosmetics, and may reduce the quality of the resulting cosmetics.
  • An object of the present invention is to provide a solid composition that facilitates removal of non-volatile solvents and suppresses quality deterioration of cosmetics.
  • a method for producing a solid composition comprises steps of preparing a mixture containing powdered wax and liquid non-volatile hydrocarbon oil, and adding a non-volatile solvent to the mixture to prepare a slurry. aspirating and filling the slurry into a container; and heating the slurry in the container to a temperature above the melting temperature of the wax.
  • FIG. 1 is a flow chart for implementing a method for producing a solid composition according to an embodiment.
  • FIG. 1 is a flow chart for implementing a method for producing a solid composition according to an embodiment.
  • the method for producing a solid composition according to this embodiment includes a step of preparing a mixture containing powdered wax and liquid non-volatile hydrocarbon oil ( FIG. 1 , step S1).
  • a solid composition refers to a solid obtained by molding a given composition.
  • the powdered wax may be powdered by pulverizing solid wax, or may be powdered wax from the beginning.
  • the average particle size of the powdered wax is arbitrary, but preferably 1 ⁇ m or more and 1000 ⁇ m or less, more preferably 10 ⁇ m or more and 600 ⁇ m or less.
  • the average particle size is the particle size at which the volume-based cumulative distribution measured by a laser diffraction/scattering method is 50%.
  • the average particle size of the wax means the average particle size before being filled with the slurry, which will be described later.
  • the melting point of the wax is not particularly limited, it is preferably 55°C or higher and 90°C or lower, more preferably 60°C or higher and 85°C or lower, and still more preferably 65°C or higher and 80°C or lower.
  • the components of the wax are not particularly limited. Isopropyl lanolin fatty acid, hexyl laurate, reduced lanolin, jojoba ester (hydrogenated jojoba oil), hard lanolin, shellac wax, beeswax, microcrystalline wax, paraffin wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin Fatty acid polyethylene glycol, fatty acid glyceride, hydrogenated castor oil, POE hydrogenated lanolin alcohol ether, sucrose fatty acid ester (sucrose triacetate tetrastearate) and the like. These components may be used singly or in combination of two or more.
  • the amount of the wax to be blended is arbitrary, but can be 0.5% by mass or more and 10% by mass or less, preferably 1% by mass or more and 9% by mass or less, with respect to the resulting solid composition. It is preferably 1.5% by mass or more and 8% by mass or less, more preferably 2% by mass or more and 7% by mass or less.
  • a liquid non-volatile hydrocarbon oil indicates a hydrocarbon oil with a kinematic viscosity of 5 cSt (centistokes) or more.
  • the viscosity of the non-volatile hydrocarbon oil is not particularly limited, it is preferably 10 mPa s or more and 50 mPa s or less, more preferably 15 mPa s or more and 45 mPa s or less, and still more preferably 20 mPa s at 20°C. 40 mPa ⁇ s or less.
  • Components of the liquid non-volatile hydrocarbon oil are not particularly limited, but for example, paraffin oil, mineral oil, saturated or unsaturated dodecane, saturated or unsaturated tridecane, saturated or unsaturated tetradecane, saturated or unsaturated pentadecane, saturated or unsaturated At least one non-volatile hydrocarbon oil selected from unsaturated hexadecane, or mixtures thereof.
  • nonvolatile hydrocarbon oils paraffin oil and mineral oil are preferred.
  • paraffin oil examples include liquid paraffin.
  • mineral oils examples include hydrogenated polydecene and hydrogenated polyisobutene. Among these, hydrogenated polydecene is more preferable.
  • hydrogenated polydecene refers to hydrogenated products of ⁇ -olefin oligomers.
  • the amount of the non-volatile hydrocarbon oil to be blended is arbitrary, but can be 0.5% by mass or more and 20% by mass or less, preferably 1% by mass or more and 15% by mass or less, relative to the resulting solid composition. , more preferably 2% by mass or more and 10% by mass or less, and still more preferably 3% by mass or more and 8% by mass or less.
  • the mass ratio of the nonvolatile hydrocarbon oil to the wax is not particularly limited, but is preferably 1 or more and 6 or less, more preferably 1.3 or more and 5 or less, and still more preferably 1.5 or more and 4 or less. is.
  • a mixture containing powdery wax and liquid non-volatile hydrocarbon oil may contain spherical powder.
  • spherical powder refers to powder that is approximately spherical in shape and has an aspect ratio (ratio of major axis to minor axis) of 1.2 or less.
  • the amount of the spherical powder to be blended is arbitrary, but is preferably 0.1% by mass or more and 15% by mass or less, more preferably 1% by mass or more and 10% by mass or less, and even more preferably, based on the resulting solid composition. is 3% by mass or more and 8% by mass or less.
  • the average particle size of the spherical powder is arbitrary, but is preferably 1 ⁇ m or more and 10 ⁇ m or less, more preferably 2 ⁇ m or more and 9 ⁇ m or less, and still more preferably 3 ⁇ m or more and 8 ⁇ m or less.
  • the average particle size is the particle size at which the volume-based cumulative distribution measured by a laser diffraction/scattering method is 50%.
  • the mixture may contain components other than the above components within a range that does not impair the effects of the present invention.
  • components other than the above components include powders other than the above spherical powders, coloring materials, activators, antioxidants, moisturizing agents, and the like.
  • Components of powders other than the above-mentioned spherical powders are optional, and examples include talc, kaolin, mica, sericite, muscovite, phlogopite, synthetic mica, leprotite, biotite, permiculite, Magnesium carbonate, calcium carbonate, aluminum silicate, barium silicate, calcium silicate, magnesium silicate, strontium silicate, metal tungstate, magnesium, silica, zeolite, barium sulfate, calcined calcium sulfate (calcined gypsum), calcium phosphate, Fluoroapatite, hydroxyapatite, ceramic powder, silicone powder, magnesium myristate (magnesium myristate), zinc myristate, calcium palmitate, aluminum stearate, chlorphenesin, boron nitride and the like. These powders may be used singly or in combination of two or more. In addition, the amount of powder to be blended is
  • the components of the coloring material are optional, and examples include red iron oxide, yellow iron oxide, black iron oxide, inorganic white pigments (e.g., zinc oxide, etc.); inorganic red pigments (e.g., iron titanate, etc.); inorganic purple system pigments (e.g., mango violet, cobalt violet, etc.); inorganic green pigments (e.g., chromium oxide, chromium hydroxide, cobalt titanate, etc.); inorganic blue pigments (e.g., ultramarine, navy blue, etc.); metal powder pigments ( For example, aluminum powder, copper powder, etc.); organic pigments such as zirconium, barium or aluminum lakes (for example, Red No. 201, Red No.
  • Red No. 204 Red No. 205, Red No. 220, Red No. 226, Red No. 228) , Red No. 405, Orange No. 203, Orange No. 204, Yellow No. 205, Yellow No. 401, Organic pigments such as Blue No. 404, Red No. 3, Red No. 104, Red No. 106, Red No. 227, Red No. 230, Red 401, Red No. 505, Orange No. 205, Yellow No. 4, Yellow No. 5, Yellow No. 202, Yellow No. 203, Green No. 3, Blue No. 1, etc.); natural pigments (e.g., chlorophyll, ⁇ -carotene, etc.), etc. is mentioned. These coloring materials may be used singly or in combination of two or more. Note that the amount of the coloring material to be mixed is arbitrary.
  • the active agent component is optional, for example, hydrogenated lecithin, sorbitan laurate, sorbitan palmitate, sorbitan oleate, sorbitan stearate, sorbitan isostearate, sorbitan sesquioleate, sorbitan trioleate, sorbitan tristearate. , sorbitan sesquiisostearate, and the like.
  • active agents may be used singly or in combination of two or more.
  • the compounding quantity of an active agent is arbitrary.
  • antioxidants are optional, and examples include ascorbic acid, ⁇ -tocopherol, dibutylhydroxytoluene, butylhydroxyanisole, and the like. These antioxidants may be used singly or in combination of two or more. In addition, the compounding quantity of antioxidant is arbitrary.
  • ingredients of the moisturizing agent are optional, and examples include polyhydric alcohol (1,3-butylene glycol, etc.), paraoxybenzoic acid ester, phenoxyethanol, octoxyglycerin, benzoic acid, salicylic acid, phenolic acid, sorbic acid, and parachlormetacresol. , hexachlorophene, benzalkonium chloride, chlorhexidine chloride, trichlorocarbanilide and the like.
  • a method for producing a solid composition according to the present embodiment includes a step of adding a non-volatile solvent to a mixture to prepare a slurry (Fig. 1, step S2).
  • slurry refers to a suspension in which a mixture containing powdered wax and liquid non-volatile hydrocarbon oil is dispersed in a non-volatile solvent.
  • a non-volatile solvent indicates a solvent having a kinematic viscosity of 5 cSt (centistokes) or more.
  • the component of the non-volatile solvent is not particularly limited, but is preferably silicone oil.
  • the silicone oil is an oily silicone having a relatively low degree of polymerization.
  • the silicone oil is not particularly limited, and examples thereof include dimethylpolysiloxane (dimethicone), methylphenylpolysiloxane, and methylhydrogenpolysiloxane. These components may be used singly or in combination of two or more. Among these silicone oils, dimethylpolysiloxane 6CS (INCI name) is preferred.
  • the non-volatile solvent may be added at any ratio to the mixture.
  • the method for producing a solid composition according to this embodiment includes a step of sucking the slurry and filling it into a container (Fig. 1, step S3).
  • aspiration of the slurry indicates removal of the non-volatile solvent in the slurry by aspiration.
  • the mode of sucking the slurry and filling it into the container is not particularly limited, and the container may be filled after sucking the slurry solvent, or the container may be filled while sucking the slurry solvent. The solvent of the slurry may be sucked after filling the container.
  • a method can be used in which the slurry is poured into an intermediate plate, compression-molded using a molding head, and simultaneously sucked from the back surface of the molding head.
  • a method can be used in which the slurry is poured into an intermediate plate and the slurry is degassed in a reduced pressure environment using a vacuum pump or the like.
  • a wet method commonly used can be applied.
  • the method for producing a solid composition includes a step of heating the slurry in the container to a temperature equal to or higher than the melting temperature of wax (Fig. 1, step S4).
  • the melting temperature of wax indicates the melting point of wax (the temperature at which wax melts). Heating to a temperature equal to or higher than the melting temperature means heating until the wax in the slurry is completely melted.
  • a slurry is prepared by adding a non-volatile solvent to a mixture containing powdered wax and liquid non-volatile hydrocarbon oil, and the non-volatile hydrocarbon oil in the slurry is and the compatibility with the non-volatile solvent can be reduced. This facilitates removal of the non-volatile solvent during molding of the solid composition. Therefore, it becomes difficult for the non-volatile solvent to remain in the obtained solid composition.
  • a slurry is formed in which powdery wax mixed with liquid nonvolatile hydrocarbon oil is dispersed in a nonvolatile solvent.
  • the nonvolatile solvent can be easily removed, and the solid composition obtained It is possible to suppress the deterioration of the quality of things.
  • the powdery wax and the non-volatile hydrocarbon oil are more easily mixed, thereby further facilitating the removal of the non-volatile solvent. It is possible to further suppress deterioration in the quality of the obtained solid composition.
  • the non-volatile hydrocarbon oil having a viscosity of 10 mPa s or more and 50 mPa s or less at 20 ° C., the non-volatile solvent can be removed more easily. and the quality deterioration of the obtained solid composition can be further suppressed.
  • the powdery wax and the non-volatile hydrocarbon oil are more easily mixed, so that the non-volatile hydrocarbon oil and the non-volatile solvent in the slurry compatibility with can be further reduced. This makes it easier to remove the non-volatile solvent during molding of the solid composition, and makes it less likely that the non-volatile solvent will remain in the obtained solid composition.
  • the use of hydrogenated polydecene as the non-volatile hydrocarbon oil makes it easier to remove the non-volatile solvent, and the quality of the resulting solid composition can be further suppressed.
  • silicone oil has poor compatibility with nonvolatile hydrocarbon oils.
  • the solvent becomes easier to remove. Therefore, it is possible to further suppress deterioration in the quality of products using the obtained solid composition.
  • the removal of the non-volatile solvent becomes easier, and the quality of the obtained solid composition does not deteriorate. can be suppressed further.
  • the solid composition according to the present embodiment is produced by the method for producing a solid composition described above. That is, a step of preparing a mixture containing a powdered wax and a liquid non-volatile hydrocarbon oil, a step of adding a non-volatile solvent to the mixture to prepare a slurry, and a step of sucking the slurry and filling it into a container. , and a step of heating the slurry in the container to a temperature equal to or higher than the melting temperature of the wax, the solid composition according to the present embodiment can be obtained.
  • the melted wax is dispersed in the solid composition as described above. Therefore, by using such a solid composition in a product such as cosmetics, it is possible to suppress deterioration in the quality of the product.
  • the solid composition according to the present embodiment is produced by heating a slurry prepared by adding a non-volatile solvent to a mixture containing powdered wax and liquid non-volatile hydrocarbon oil to a temperature equal to or higher than the melting temperature of the wax.
  • a slurry prepared by adding a non-volatile solvent to a mixture containing powdered wax and liquid non-volatile hydrocarbon oil to a temperature equal to or higher than the melting temperature of the wax.
  • the solid composition according to the present embodiment requires promptness due to the nature of the patent application. Carrying out the task of identifying the structure or properties of the structure would be significantly more expensive and time consuming. That is, it is impossible or impractical to specify the structure or characteristics of the solid composition according to the present embodiment.
  • the cosmetic according to this embodiment contains the solid composition described above. Since the above-mentioned solid composition has the effect of suppressing the deterioration of the quality of cosmetics, such an effect can be used to apply foundation, eye shadow, cheek color, body powder, perfume powder, baby powder, pressed powder, etc. It is suitably used for solid powder cosmetics such as powders, deodorant powders and face powders.
  • ⁇ Test body> After mixing the powder with a Henschel mixer, dimethylpolysiloxane 6CS as a solvent was added to the resulting mixture to prepare a slurry. The resulting slurry is poured into a mold (middle plate) while being sucked. The slurry filled in the mold is heated in a constant temperature bath at 70° C. for 1 hour. After that, the mold is taken out from the constant temperature bath and left in a room for 1 hour, and the obtained molded article (solid matter) is used as a test piece.
  • ⁇ Surface condition> The surface condition of the obtained molded article (solid matter) was visually observed. Evaluation criteria for the surface state are shown below. In the cases of A and B, the surface condition was evaluated as good, and in the case of evaluation C, the surface condition was evaluated as poor.
  • a test piece was dropped from a height of 30 cm onto a metal plate, and the number of times it dropped until it could no longer maintain a state such as falling out of the middle plate was examined.
  • the number of tests (N) is three. Evaluation criteria for impact resistance are shown below. In the cases of A and B, the impact resistance was evaluated as good, and in the case of the evaluation of C, the impact resistance was evaluated as poor.
  • C Less than 5 times
  • Table 1 below shows the composition of ingredients and the evaluation results for Examples and Comparative Examples.
  • the specifications of the blended non-volatile hydrocarbon oil are as follows.
  • Hydrogenated polydecene Olefin Oligomer 30 (manufactured by Nikko Chemicals Co., Ltd.) (viscosity at 20 ° C.: 25 to 37 mPa s)
  • Mineral oil liquid paraffin (viscosity 21 to 26 mPa s at 20°C)
  • Vaseline semi-solid
  • Triethylhexanoin RA-G-308 (manufactured by Nippon Fine Chemical Co., Ltd.) (viscosity at 20 ° C. 20 to 35 mPa s)
  • the particle size of the component means the average particle size of the wax before the slurry is filled into the mold.
  • Examples 1 to 9 showed good solvent removal. Of these, Examples 3 to 9 had even better surface conditions, and Examples 3, 4 and 7 among them had even better impact resistance.
  • Comparative Examples 1 to 3 solvent removal was poor, and of these, Comparative Example 3 was further poor in both surface condition and impact resistance.

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Abstract

A production method for a solid composition, that includes: a step in which a mixture is prepared that includes a powdered wax and a liquid non-volatile hydrocarbon oil; a step in which a non-volatile solvent is added to the mixture and a slurry is prepared; a step in which the slurry is suctioned and a container is filled; and a step in which the slurry inside the container is heated to a temperature that is at least the melting temperature of the wax.

Description

固形組成物の製造方法、固形組成物、及び化粧料Method for producing solid composition, solid composition, and cosmetic
 本発明は、固形組成物の製造方法、固形組成物、及び化粧料に関する。 The present invention relates to a method for producing a solid composition, a solid composition, and a cosmetic.
 特許文献1には、有機積層粉末と油剤とを含有する化粧料基材と、シリコーン油等の溶媒とを混合し、該混合物を容器に充填し、前記溶媒を液状状態で除去して得られる固形粉末化粧料が開示されている。 In Patent Document 1, a cosmetic base material containing an organic layered powder and an oil agent is mixed with a solvent such as silicone oil, the mixture is filled in a container, and the solvent is removed in a liquid state. A solid powder cosmetic is disclosed.
特開2007-291074号公報JP 2007-291074 A
 シリコーン油等の不揮発性溶媒は、化粧料の製造時における除去がしづらく、得られる化粧料の品質を低下させるおそれがある。 Non-volatile solvents such as silicone oil are difficult to remove during the production of cosmetics, and may reduce the quality of the resulting cosmetics.
 本発明の課題は、不揮発性溶媒の除去を容易にし、化粧料の品質の低下を抑制する固形組成物を提供することである。 An object of the present invention is to provide a solid composition that facilitates removal of non-volatile solvents and suppresses quality deterioration of cosmetics.
 本発明の一態様に係る固形組成物の製造方法は、粉末状のワックス及び液状の不揮発性炭化水素油を含む混合物を調製する工程と、前記混合物に不揮発性溶媒を添加してスラリーを調製する工程と、前記スラリーを吸引し且つ容器に充填する工程と、前記容器内の前記スラリーを前記ワックスの溶融温度以上の温度に加熱する工程と、を含む。 A method for producing a solid composition according to an aspect of the present invention comprises steps of preparing a mixture containing powdered wax and liquid non-volatile hydrocarbon oil, and adding a non-volatile solvent to the mixture to prepare a slurry. aspirating and filling the slurry into a container; and heating the slurry in the container to a temperature above the melting temperature of the wax.
 本発明の一態様によれば、不揮発性溶媒の除去を容易にし、化粧料の品質の低下を抑制する固形組成物を提供することができる。 According to one aspect of the present invention, it is possible to provide a solid composition that facilitates removal of a non-volatile solvent and suppresses quality deterioration of cosmetics.
実施形態に係る固形組成物の製造方法を実施するフローチャートである。1 is a flow chart for implementing a method for producing a solid composition according to an embodiment.
 以下、本発明の実施の形態について、詳細に説明する。 Hereinafter, embodiments of the present invention will be described in detail.
<固形組成物の製造方法>
 図1は、実施形態に係る固形組成物の製造方法を実施するフローチャートである。本実施形態に係る固形組成物の製造方法は、粉末状のワックス及び液状の不揮発性炭化水素油を含む混合物を調製する工程を含む(図1、ステップS1)。本明細書において、固形組成物は、所定の組成物を成形して固形物にしたものを示す。
<Method for producing solid composition>
FIG. 1 is a flow chart for implementing a method for producing a solid composition according to an embodiment. The method for producing a solid composition according to this embodiment includes a step of preparing a mixture containing powdered wax and liquid non-volatile hydrocarbon oil ( FIG. 1 , step S1). As used herein, a solid composition refers to a solid obtained by molding a given composition.
 粉末状のワックスは、固形のワックスを粉砕して粉末状に調製したものでも、最初から粉末状に調整されたワックスでもよい。粉末状のワックスの平均粒子径は、任意であるが、好ましくは1μm以上1000μm以下、より好ましくは10μm以上600μm以下である。ここで、平均粒子径は、レーザー回折・散乱法により測定される体積基準の累積分布が50%となる粒子径である。また、ワックスの平均粒子径は、後述するスラリーの充填前の平均粒子径を意味する。 The powdered wax may be powdered by pulverizing solid wax, or may be powdered wax from the beginning. The average particle size of the powdered wax is arbitrary, but preferably 1 μm or more and 1000 μm or less, more preferably 10 μm or more and 600 μm or less. Here, the average particle size is the particle size at which the volume-based cumulative distribution measured by a laser diffraction/scattering method is 50%. Also, the average particle size of the wax means the average particle size before being filled with the slurry, which will be described later.
 ワックスの融点は、特に限定されないが、好ましくは55℃以上90℃以下であり、より好ましくは60℃以上85℃以下であり、さらに好ましくは65℃以上80℃以下である。 Although the melting point of the wax is not particularly limited, it is preferably 55°C or higher and 90°C or lower, more preferably 60°C or higher and 85°C or lower, and still more preferably 65°C or higher and 80°C or lower.
 ワックスの成分は、特に限定されず、例えば、ミツロウ、キャンデリラロウ、綿ロウ、カルナバロウ、ベイベリーロウ、イボタロウ、鯨ロウ、モンタンロウ、ヌカロウ(ライスロウ)、カポックロウ、モクロウ、酢酸ラノリン、液状ラノリン、サトウキビロウ、ラノリン脂肪酸イソプロピル、ラウリン酸ヘキシル、還元ラノリン、ホホバエステル(水素添加ホホバ油)、硬質ラノリン、セラックロウ、ビーズワックス、マイクロクリスタリンワックス、パラフィンワックス、POEラノリンアルコールエーテル、POEラノリンアルコールアセテート、POEコレステロールエーテル、ラノリン脂肪酸ポリエチレングリコール、脂肪酸グリセリド、硬化ヒマシ油、POE水素添加ラノリンアルコールエーテル、ショ糖脂肪酸エステル(トリ酢酸テトラステアリン酸スクロース)等が挙げられる。これらの成分は、1種または2種以上を混合して用いてもよい。 The components of the wax are not particularly limited. Isopropyl lanolin fatty acid, hexyl laurate, reduced lanolin, jojoba ester (hydrogenated jojoba oil), hard lanolin, shellac wax, beeswax, microcrystalline wax, paraffin wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin Fatty acid polyethylene glycol, fatty acid glyceride, hydrogenated castor oil, POE hydrogenated lanolin alcohol ether, sucrose fatty acid ester (sucrose triacetate tetrastearate) and the like. These components may be used singly or in combination of two or more.
 ワックスの配合量は、任意であるが、得られる固形組成物に対して、0.5質量%以上10質量%以下にすることができ、好ましくは1質量%以上9質量%以下であり、より好ましくは1.5質量%以上8質量%以下であり、さらに好ましくは2質量%以上7質量%以下である。 The amount of the wax to be blended is arbitrary, but can be 0.5% by mass or more and 10% by mass or less, preferably 1% by mass or more and 9% by mass or less, with respect to the resulting solid composition. It is preferably 1.5% by mass or more and 8% by mass or less, more preferably 2% by mass or more and 7% by mass or less.
 液状の不揮発性炭化水素油は、動粘度が5cSt(センチストークス)以上の炭化水素油を示す。不揮発性炭化水素油の粘度は、特に限定されないが、好ましくは20℃において10mPa・s以上50mPa・s以下であり、より好ましくは15mPa・s以上45mPa・s以下であり、さらに好ましくは20mPa・s以上40mPa・s以下である。 A liquid non-volatile hydrocarbon oil indicates a hydrocarbon oil with a kinematic viscosity of 5 cSt (centistokes) or more. Although the viscosity of the non-volatile hydrocarbon oil is not particularly limited, it is preferably 10 mPa s or more and 50 mPa s or less, more preferably 15 mPa s or more and 45 mPa s or less, and still more preferably 20 mPa s at 20°C. 40 mPa·s or less.
 液状の不揮発性炭化水素油の成分は、特に限定されないが、例えば、パラフィン油、鉱物油、飽和または不飽和ドデカン、飽和または不飽和トリデカン、飽和または不飽和テトラデカン、飽和または不飽和ペンタデカン、飽和または不飽和ヘキサデカン、またはそれらの混合物から選択される少なくとも一つの不揮発性炭化水素油が挙げられる。これらの不揮発性炭化水素油の中でもパラフィン油、鉱物油が好ましい。 Components of the liquid non-volatile hydrocarbon oil are not particularly limited, but for example, paraffin oil, mineral oil, saturated or unsaturated dodecane, saturated or unsaturated tridecane, saturated or unsaturated tetradecane, saturated or unsaturated pentadecane, saturated or unsaturated At least one non-volatile hydrocarbon oil selected from unsaturated hexadecane, or mixtures thereof. Among these nonvolatile hydrocarbon oils, paraffin oil and mineral oil are preferred.
 パラフィン油としては、例えば、流動パラフィンが挙げられる。また、鉱物油としては、例えば、水添ポリデセン、水添ポリイソブテンが挙げられる。これらの中でも水添ポリデセンがより好ましい。ここで、水添ポリデセンは、α-オレフィンオリゴマーの水素添加物を示す。 Examples of paraffin oil include liquid paraffin. Examples of mineral oils include hydrogenated polydecene and hydrogenated polyisobutene. Among these, hydrogenated polydecene is more preferable. Here, hydrogenated polydecene refers to hydrogenated products of α-olefin oligomers.
 不揮発性炭化水素油の配合量は、任意であるが、得られる固形組成物に対して、0.5質量%以上20質量%以下にすることができ、好ましくは1質量%以上15質量%以下であり、より好ましくは2質量%以上10質量%以下であり、さらに好ましくは3質量%以上8質量%以下である。 The amount of the non-volatile hydrocarbon oil to be blended is arbitrary, but can be 0.5% by mass or more and 20% by mass or less, preferably 1% by mass or more and 15% by mass or less, relative to the resulting solid composition. , more preferably 2% by mass or more and 10% by mass or less, and still more preferably 3% by mass or more and 8% by mass or less.
 また、ワックスに対する不揮発性炭化水素油の質量比は、特に限定されないが、好ましくは1以上6以下であり、より好ましくは1.3以上5以下であり、さらに好ましくは、1.5以上4以下である。 In addition, the mass ratio of the nonvolatile hydrocarbon oil to the wax is not particularly limited, but is preferably 1 or more and 6 or less, more preferably 1.3 or more and 5 or less, and still more preferably 1.5 or more and 4 or less. is.
 粉末状のワックス及び液状の不揮発性炭化水素油を含む混合物には、球状粉末が含まれていてもよい。本明細書において、球状粉末は、形状が略球形の粉末でアスペクト比(長径と短径の比)が1.2以下のものを示す。 A mixture containing powdery wax and liquid non-volatile hydrocarbon oil may contain spherical powder. In the present specification, spherical powder refers to powder that is approximately spherical in shape and has an aspect ratio (ratio of major axis to minor axis) of 1.2 or less.
 球状粉末の配合量は、任意であるが、得られる固形組成物に対して、好ましくは0.1質量%以上15質量%以下、より好ましくは1質量%以上10質量%以下であり、さらに好ましくは3質量%以上8質量%以下である。 The amount of the spherical powder to be blended is arbitrary, but is preferably 0.1% by mass or more and 15% by mass or less, more preferably 1% by mass or more and 10% by mass or less, and even more preferably, based on the resulting solid composition. is 3% by mass or more and 8% by mass or less.
 球状粉末の平均粒子径は、任意であるが、好ましくは1μm以上10μm以下、より好ましくは2μm以上9μm以下、さらに好ましくは3μm以上8μm以下である。ここで、平均粒子径は、レーザー回折・散乱法により測定される体積基準の累積分布が50%となる粒子径である。 The average particle size of the spherical powder is arbitrary, but is preferably 1 μm or more and 10 μm or less, more preferably 2 μm or more and 9 μm or less, and still more preferably 3 μm or more and 8 μm or less. Here, the average particle size is the particle size at which the volume-based cumulative distribution measured by a laser diffraction/scattering method is 50%.
 本実施形態に係る固形組成物の製造方法において、混合物には、本発明の効果を損なわない範囲で、上記成分以外の成分が含まれていてもよい。上記成分以外の成分としては、例えば、上記球状粉末以外の粉体、色材、活性剤、酸化防止剤、保湿剤等が挙げられる。 In the method for producing a solid composition according to the present embodiment, the mixture may contain components other than the above components within a range that does not impair the effects of the present invention. Examples of components other than the above components include powders other than the above spherical powders, coloring materials, activators, antioxidants, moisturizing agents, and the like.
 上記球状粉末以外の粉体の成分は、任意であり、例えば、タルク、カオリン、雲母(マイカ)、絹雲母(セリサイト)、白雲母、金雲母、合成雲母、紅雲母、黒雲母、パーミキュライト、炭酸マグネシウム、炭酸カルシウム、ケイ酸アルミニウム、ケイ酸バリウム、ケイ酸カルシウム、ケイ酸マグネシウム、ケイ酸ストロンチウム、タングステン酸金属塩、マグネシウム、シリカ、ゼオライト、硫酸バリウム、焼成硫酸カルシウム(焼セッコウ)、リン酸カルシウム、弗素アパタイト、ヒドロキシアパタイト、セラミックパウダー、シリコーンパウダー、ミリスチン酸マグネシウム(マグネシウムミリステート)、ミリスチン酸亜鉛、パルミチン酸カルシウム、ステアリン酸アルミニウム、クロルフェネシン、窒化ホウ素等が挙げられる。これらの粉体は、1種または2種以上を混合して用いてもよい。なお、粉体の配合量は、任意である。 Components of powders other than the above-mentioned spherical powders are optional, and examples include talc, kaolin, mica, sericite, muscovite, phlogopite, synthetic mica, leprotite, biotite, permiculite, Magnesium carbonate, calcium carbonate, aluminum silicate, barium silicate, calcium silicate, magnesium silicate, strontium silicate, metal tungstate, magnesium, silica, zeolite, barium sulfate, calcined calcium sulfate (calcined gypsum), calcium phosphate, Fluoroapatite, hydroxyapatite, ceramic powder, silicone powder, magnesium myristate (magnesium myristate), zinc myristate, calcium palmitate, aluminum stearate, chlorphenesin, boron nitride and the like. These powders may be used singly or in combination of two or more. In addition, the amount of powder to be blended is arbitrary.
 色材の成分は、任意であり、例えば、赤酸化鉄、黄酸化鉄、黒酸化鉄、無機白色顔料(例えば、酸化亜鉛等);無機赤色系顔料(例えば、チタン酸鉄等);無機紫色系顔料(例えば、マンゴバイオレット、コバルトバイオレット等);無機緑色系顔料(例えば、酸化クロム、水酸化クロム、チタン酸コバルト等);無機青色系顔料(例えば、群青、紺青等);金属粉末顔料(例えば、アルミニウムパウダー、カッパーパウダー等);ジルコニウム、バリウムまたはアルミニウムレーキ等の有機顔料(例えば、赤色201号、赤色202号、赤色204号、赤色205号、赤色220号、赤色226号、赤色228号、赤色405号、橙色203号、橙色204号、黄色205号、黄色401号、青色404号などの有機顔料、赤色3号、赤色104号、赤色106号、赤色227号、赤色230号、赤色401号、赤色505号、橙色205号、黄色4号、黄色5号、黄色202号、黄色203号、緑色3号、青色1号等);天然色素(例えば、クロロフィル、β-カロチン等)等が挙げられる。これらの色材は、1種または2種以上を混合して用いてもよい。なお、色材の配合量は、任意である。 The components of the coloring material are optional, and examples include red iron oxide, yellow iron oxide, black iron oxide, inorganic white pigments (e.g., zinc oxide, etc.); inorganic red pigments (e.g., iron titanate, etc.); inorganic purple system pigments (e.g., mango violet, cobalt violet, etc.); inorganic green pigments (e.g., chromium oxide, chromium hydroxide, cobalt titanate, etc.); inorganic blue pigments (e.g., ultramarine, navy blue, etc.); metal powder pigments ( For example, aluminum powder, copper powder, etc.); organic pigments such as zirconium, barium or aluminum lakes (for example, Red No. 201, Red No. 202, Red No. 204, Red No. 205, Red No. 220, Red No. 226, Red No. 228) , Red No. 405, Orange No. 203, Orange No. 204, Yellow No. 205, Yellow No. 401, Organic pigments such as Blue No. 404, Red No. 3, Red No. 104, Red No. 106, Red No. 227, Red No. 230, Red 401, Red No. 505, Orange No. 205, Yellow No. 4, Yellow No. 5, Yellow No. 202, Yellow No. 203, Green No. 3, Blue No. 1, etc.); natural pigments (e.g., chlorophyll, β-carotene, etc.), etc. is mentioned. These coloring materials may be used singly or in combination of two or more. Note that the amount of the coloring material to be mixed is arbitrary.
 活性剤の成分は、任意であり、例えば、水素添加レシチン、ラウリン酸ソルビタン、パルミチン酸ソルビタン、オレイン酸ソルビタン、ステアリン酸ソルビタン、イソステアリン酸ソルビタン、セスキオレイン酸ソルビタン、トリオレイン酸ソルビタン、トリステアリン酸ソルビタン、セスキイソステアリン酸ソルビタン等が挙げられる。これらの活性剤は、1種または2種以上を混合して用いてもよい。なお、活性剤の配合量は、任意である。 The active agent component is optional, for example, hydrogenated lecithin, sorbitan laurate, sorbitan palmitate, sorbitan oleate, sorbitan stearate, sorbitan isostearate, sorbitan sesquioleate, sorbitan trioleate, sorbitan tristearate. , sorbitan sesquiisostearate, and the like. These active agents may be used singly or in combination of two or more. In addition, the compounding quantity of an active agent is arbitrary.
 酸化防止剤の成分は、任意であり、例えば、アスコルビン酸、α-トコフェロール、ジブチルヒドロキシトルエン、ブチルヒドロキシアニソール等が例示される。これらの酸化防止剤は、1種または2種以上を混合して用いてもよい。なお、酸化防止剤の配合量は、任意である。 The components of the antioxidant are optional, and examples include ascorbic acid, α-tocopherol, dibutylhydroxytoluene, butylhydroxyanisole, and the like. These antioxidants may be used singly or in combination of two or more. In addition, the compounding quantity of antioxidant is arbitrary.
 保湿剤の成分は、任意であり、例えば、多価アルコール(1,3-ブチレングリコール等)、パラオキシ安息香酸エステル、フェノキシエタノール、オクトキシグリセリン、安息香酸、サリチル酸、石炭酸、ソルビン酸、パラクロルメタクレゾール、ヘキサクロロフェン、塩化ベンザルコニウム、塩化クロルヘキシジン、トリクロロカルバニリド等が挙げられる。 Ingredients of the moisturizing agent are optional, and examples include polyhydric alcohol (1,3-butylene glycol, etc.), paraoxybenzoic acid ester, phenoxyethanol, octoxyglycerin, benzoic acid, salicylic acid, phenolic acid, sorbic acid, and parachlormetacresol. , hexachlorophene, benzalkonium chloride, chlorhexidine chloride, trichlorocarbanilide and the like.
 本実施形態に係る固形組成物の製造方法は、混合物に不揮発性溶媒を添加してスラリーを調製する工程を含む(図1、ステップS2)。本明細書において、スラリーは、粉末状のワックス及び液状の不揮発性炭化水素油を含む混合物が不揮発性溶媒に分散された懸濁液を示す。不揮発性溶媒は、動粘度が5cSt(センチストークス)以上の溶媒を示す。 A method for producing a solid composition according to the present embodiment includes a step of adding a non-volatile solvent to a mixture to prepare a slurry (Fig. 1, step S2). As used herein, slurry refers to a suspension in which a mixture containing powdered wax and liquid non-volatile hydrocarbon oil is dispersed in a non-volatile solvent. A non-volatile solvent indicates a solvent having a kinematic viscosity of 5 cSt (centistokes) or more.
 不揮発性溶媒の成分は、特に限定されないが、好ましくはシリコーン油である。ここで、シリコーン油は、比較的重合度の低いシリコーンで油状のものを示す。 The component of the non-volatile solvent is not particularly limited, but is preferably silicone oil. Here, the silicone oil is an oily silicone having a relatively low degree of polymerization.
 シリコーン油としては、特に限定されず、例えば、ジメチルポリシロキサン(ジメチコン)、メチルフェニルポリシロキサン、メチルハイドロジェンポリシロキサン等が挙げられる。これらの成分は、1種または2種以上を混合して用いてもよい。これらのシリコーン油の中でも、ジメチルポリシロキサン6CS(INCI名)が好ましい。 The silicone oil is not particularly limited, and examples thereof include dimethylpolysiloxane (dimethicone), methylphenylpolysiloxane, and methylhydrogenpolysiloxane. These components may be used singly or in combination of two or more. Among these silicone oils, dimethylpolysiloxane 6CS (INCI name) is preferred.
 なお、不揮発性溶媒は、混合物に対して任意の比率で添加してよい。 The non-volatile solvent may be added at any ratio to the mixture.
 本実施形態に係る固形組成物の製造方法は、スラリーを吸引し且つ容器に充填する工程を含む(図1、ステップS3)。本明細書において、スラリーの吸引は、スラリー中の不揮発性溶媒を吸引により除去することを示す。 The method for producing a solid composition according to this embodiment includes a step of sucking the slurry and filling it into a container (Fig. 1, step S3). As used herein, aspiration of the slurry indicates removal of the non-volatile solvent in the slurry by aspiration.
 スラリーを吸引し且つ容器に充填する態様は、特に限定されず、スラリーの溶媒を吸引した後に容器に充填してもよく、スラリーの溶媒を吸引しながら容器に充填してもよく、また、スラリーを容器に充填した後にスラリーの溶媒を吸引してもよい。 The mode of sucking the slurry and filling it into the container is not particularly limited, and the container may be filled after sucking the slurry solvent, or the container may be filled while sucking the slurry solvent. The solvent of the slurry may be sucked after filling the container.
 スラリーを吸引し且つ容器に充填する態様としては、例えば、スラリーを中皿に流し込み、成形ヘッドを用いて圧縮成形し、同時に成形ヘッドの裏面から吸引する方法を用いることができる。また、スラリーを中皿に流し込み、真空ポンプ等を用いてスラリーを減圧環境で脱気する方法を用いることができる。さらに、通常用いられる湿式法を適用することができる。 As a mode of sucking the slurry and filling it into a container, for example, a method can be used in which the slurry is poured into an intermediate plate, compression-molded using a molding head, and simultaneously sucked from the back surface of the molding head. Alternatively, a method can be used in which the slurry is poured into an intermediate plate and the slurry is degassed in a reduced pressure environment using a vacuum pump or the like. Furthermore, a wet method commonly used can be applied.
 本実施形態に係る固形組成物の製造方法は、容器内のスラリーをワックスの溶融温度以上の温度に加熱する工程を含む(図1、ステップS4)。本明細書において、ワックスの溶融温度とは、ワックスの融点(ワックスが溶解する温度)を示す。溶融温度以上の温度に加熱するとは、スラリー中のワックスが溶解しきるまで加熱することを示す。 The method for producing a solid composition according to this embodiment includes a step of heating the slurry in the container to a temperature equal to or higher than the melting temperature of wax (Fig. 1, step S4). As used herein, the melting temperature of wax indicates the melting point of wax (the temperature at which wax melts). Heating to a temperature equal to or higher than the melting temperature means heating until the wax in the slurry is completely melted.
 本実施形態に係る固形組成物の製造方法では、粉末状のワックスと液状の不揮発性炭化水素油を含む混合物に不揮発性溶媒を添加してスラリーを調整することにより、スラリーにおける不揮発性炭化水素油と不揮発性溶媒との相溶性を低下させることができる。これにより、固形組成物の成形時における不揮発性溶媒の除去が容易である。そのため、得られた固形組成物中に不揮発性溶媒が残存しにくくなる。 In the method for producing a solid composition according to the present embodiment, a slurry is prepared by adding a non-volatile solvent to a mixture containing powdered wax and liquid non-volatile hydrocarbon oil, and the non-volatile hydrocarbon oil in the slurry is and the compatibility with the non-volatile solvent can be reduced. This facilitates removal of the non-volatile solvent during molding of the solid composition. Therefore, it becomes difficult for the non-volatile solvent to remain in the obtained solid composition.
 また、本実施形態に係る固形組成物の製造方法では、液状の不揮発性炭化水素油が混ざり合った粉末状のワックスが不揮発性溶媒に分散するスラリーが形成される。このようなスラリーを、固形組成物の成形時に不揮発性溶媒が除去された状態で、ワックスの溶融温度以上の温度に加熱することで、得られた固形組成物では、溶けたワックスを固形組成物中に分散させることができる。 In addition, in the method for producing a solid composition according to the present embodiment, a slurry is formed in which powdery wax mixed with liquid nonvolatile hydrocarbon oil is dispersed in a nonvolatile solvent. By heating such a slurry to a temperature equal to or higher than the melting temperature of the wax in a state in which the non-volatile solvent has been removed during molding of the solid composition, the resulting solid composition has the melted wax dissolved in the solid composition. can be dispersed in
 本実施形態に係る固形組成物の製造方法では、このような固形組成物を化粧料等の製品に用いることで、不揮発性溶媒の除去を容易にし、製品の品質の低下を抑制することができる。 In the method for producing a solid composition according to the present embodiment, by using such a solid composition in products such as cosmetics, it is possible to facilitate removal of the nonvolatile solvent and suppress deterioration in product quality. .
 本実施形態に係る固形組成物の製造方法では、上述のように、平均粒子径が1μm以上1000μm以下のワックスを用いることで、不揮発性溶媒の除去を容易にすることができ、得られる固形組成物の品質の低下を抑制することができる。 In the method for producing a solid composition according to the present embodiment, as described above, by using a wax having an average particle size of 1 μm or more and 1000 μm or less, the nonvolatile solvent can be easily removed, and the solid composition obtained It is possible to suppress the deterioration of the quality of things.
 本実施形態に係る固形組成物の製造方法では、上述のように、ワックスに対する不揮発性炭化水素油の質量比が1以上6以下に調整された該ワックスと不揮発性炭化水素油を用いることで、不揮発性溶媒の除去がさらに容易になり、得られる固形組成物の品質の低下をさらに抑制することができる。 In the method for producing a solid composition according to the present embodiment, as described above, by using the wax and the non-volatile hydrocarbon oil in which the mass ratio of the non-volatile hydrocarbon oil to the wax is adjusted to 1 or more and 6 or less, Removal of the non-volatile solvent is further facilitated, and deterioration in quality of the obtained solid composition can be further suppressed.
 また、本実施形態に係る固形組成物の製造方法では、上述のように、粉末状のワックスと不揮発性炭化水素油がより混合しやすくなることで、不揮発性溶媒の除去がさらに容易になり、得られる固形組成物の品質の低下をさらに抑制することができる。 In addition, in the method for producing a solid composition according to the present embodiment, as described above, the powdery wax and the non-volatile hydrocarbon oil are more easily mixed, thereby further facilitating the removal of the non-volatile solvent. It is possible to further suppress deterioration in the quality of the obtained solid composition.
 本実施形態に係る固形組成物の製造方法では、上述のように、粘度が20℃において10mPa・s以上50mPa・s以下の不揮発性炭化水素油を用いることにより、不揮発性溶媒の除去がさらに容易になり、得られる固形組成物の品質の低下をさらに抑制することができる。 In the method for producing a solid composition according to the present embodiment, as described above, by using a non-volatile hydrocarbon oil having a viscosity of 10 mPa s or more and 50 mPa s or less at 20 ° C., the non-volatile solvent can be removed more easily. and the quality deterioration of the obtained solid composition can be further suppressed.
 また、本実施形態に係る固形組成物の製造方法では、上述のように、粉末状のワックスと不揮発性炭化水素油がより混合しやすくなることで、スラリーにおける不揮発性炭化水素油と不揮発性溶媒との相溶性をさらに低下させることができる。これにより、固形組成物の成形時における不揮発性溶媒の除去がさらに容易になり、得られた固形組成物中に不揮発性溶媒が残存しにくくなる。 Further, in the method for producing a solid composition according to the present embodiment, as described above, the powdery wax and the non-volatile hydrocarbon oil are more easily mixed, so that the non-volatile hydrocarbon oil and the non-volatile solvent in the slurry compatibility with can be further reduced. This makes it easier to remove the non-volatile solvent during molding of the solid composition, and makes it less likely that the non-volatile solvent will remain in the obtained solid composition.
 本実施形態に係る固形組成物の製造方法では、上述のように、不揮発性炭化水素油に水添ポリデセンを用いることで、不揮発性溶媒の除去がさらに容易になり、得られる固形組成物の品質の低下をさらに抑制することができる。 In the method for producing a solid composition according to the present embodiment, as described above, the use of hydrogenated polydecene as the non-volatile hydrocarbon oil makes it easier to remove the non-volatile solvent, and the quality of the resulting solid composition can be further suppressed.
 本実施形態に係る固形組成物の製造方法では、上述のように、不揮発性溶媒としてシリコーン油を用いることにより、シリコーン油は不揮発性炭化水素油と相溶性が悪いため、固形組成物において不揮発性溶媒がさらに除去しやすくなる。そのため、得られた固形組成物を用いた製品の品質の低下をさらに抑制することができる。 In the method for producing a solid composition according to the present embodiment, as described above, by using silicone oil as a nonvolatile solvent, silicone oil has poor compatibility with nonvolatile hydrocarbon oils. The solvent becomes easier to remove. Therefore, it is possible to further suppress deterioration in the quality of products using the obtained solid composition.
 本実施形態に係る固形組成物の製造方法では、上述のように、混合物に球状粉末が含まれていると、不揮発性溶媒の除去がさらに容易になり、得られる固形組成物の品質の低下をさらに抑制することができる。 In the method for producing a solid composition according to the present embodiment, as described above, if the mixture contains spherical powder, the removal of the non-volatile solvent becomes easier, and the quality of the obtained solid composition does not deteriorate. can be suppressed further.
 本実施形態に係る固形組成物の製造方法では、上述のように、平均粒子径が1μm以上10μm以下の球状粉末を用いることにより、不揮発性溶媒の除去がさらに容易になり、得られる固形組成物の品質の低下をさらに抑制することができる。 In the method for producing a solid composition according to the present embodiment, as described above, by using spherical powder having an average particle size of 1 μm or more and 10 μm or less, the removal of the nonvolatile solvent becomes easier, and the obtained solid composition quality deterioration can be further suppressed.
<固形組成物>
 本実施形態に係る固形組成物は、上述の固形組成物の製造方法によって製造される。すなわち、粉末状のワックス及び液状の不揮発性炭化水素油を含む混合物を調製する工程と、混合物に不揮発性溶媒を添加してスラリーを調製する工程と、スラリーを吸引し且つ容器に充填する工程と、容器内のスラリーをワックスの溶融温度以上の温度に加熱する工程と、を実行することで、本実施形態に係る固形組成物を得ることができる。
<Solid composition>
The solid composition according to the present embodiment is produced by the method for producing a solid composition described above. That is, a step of preparing a mixture containing a powdered wax and a liquid non-volatile hydrocarbon oil, a step of adding a non-volatile solvent to the mixture to prepare a slurry, and a step of sucking the slurry and filling it into a container. , and a step of heating the slurry in the container to a temperature equal to or higher than the melting temperature of the wax, the solid composition according to the present embodiment can be obtained.
 このようにして得られる固形組成物は、上述のように、溶けたワックスが固形組成物中に分散している。そのため、このような固形組成物を化粧料等の製品に用いることで、製品の品質の低下を抑制することができる。 In the solid composition thus obtained, the melted wax is dispersed in the solid composition as described above. Therefore, by using such a solid composition in a product such as cosmetics, it is possible to suppress deterioration in the quality of the product.
 なお、本実施形態に係る固形組成物は、粉末状のワックス及び液状の不揮発性炭化水素油を含む混合物に不揮発性溶媒を添加して調整したスラリーをワックスの溶融温度以上の温度に加熱して得られるが、得られた固形組成物においてワックスの粉末状態は消失している。そのため、固形組成物の製造前の状態(例えば、粉末状のワックス及び液状の不揮発性炭化水素油を含む混合物、または該混合物に不揮発性溶媒を添加して調整したスラリー等の性状)を解析しても、本実施形態に係る固形組成物の構造または特性を特定することは現時点で技術的に困難である。 The solid composition according to the present embodiment is produced by heating a slurry prepared by adding a non-volatile solvent to a mixture containing powdered wax and liquid non-volatile hydrocarbon oil to a temperature equal to or higher than the melting temperature of the wax. However, the powdered state of the wax has disappeared in the resulting solid composition. Therefore, the state before production of the solid composition (for example, the properties of a mixture containing powdered wax and liquid non-volatile hydrocarbon oil, or a slurry prepared by adding a non-volatile solvent to the mixture) is analyzed. However, it is currently technically difficult to specify the structure or properties of the solid composition according to this embodiment.
 また、何らかの方法によって本実施形態に係る固形組成物の構造または特性を解析でき得るとしても、特許出願の性質上、迅速性等を必要とすることに鑑みて、本実施形態に係る固形組成物の構造または特性を特定する作業を行うことには著しく過大な経済的支出や時間を要することになる。すなわち、本実施形態に係る固形組成物をその構造または特性を明記して特定することには、不可能・非実際的事情が存在する。 In addition, even if the structure or characteristics of the solid composition according to the present embodiment can be analyzed by some method, the solid composition according to the present embodiment requires promptness due to the nature of the patent application. Carrying out the task of identifying the structure or properties of the structure would be significantly more expensive and time consuming. That is, it is impossible or impractical to specify the structure or characteristics of the solid composition according to the present embodiment.
<化粧料>
 本実施形態に係る化粧料は、上述の固形組成物を含む。上述の固形組成物は、化粧料の品質の低下を抑制する効果が得られるため、このような効果を利用して、ファンデーション、アイシャドウ、チークカラー、ボディーパウダー、パフュームパウダー、ベビーパウダー、プレスドパウダー、デオドラントパウダー、おしろい等の固形粉末化粧料に好適に用いられる。
<Cosmetics>
The cosmetic according to this embodiment contains the solid composition described above. Since the above-mentioned solid composition has the effect of suppressing the deterioration of the quality of cosmetics, such an effect can be used to apply foundation, eye shadow, cheek color, body powder, perfume powder, baby powder, pressed powder, etc. It is suitably used for solid powder cosmetics such as powders, deodorant powders and face powders.
 以下、本発明について、さらに実施例を用いて説明する。なお、表1、表2における各成分の数値は、「質量%」を単位とする。また、各種の試験および評価は、下記の方法にしたがって行った。 The present invention will be further described below using examples. In addition, the numerical value of each component in Table 1 and Table 2 uses "mass %" as a unit. Various tests and evaluations were conducted according to the following methods.
 <試験体>
 ヘンシェルミキサーで粉末を混合した後、得られた混合物に溶媒であるジメチルポリシロキサン6CSを添加し、スラリーを調製した。得られたスラリーを吸引しながら成形型(中皿)に流し込む。成形型に充填されたスラリーを、恒温槽で70℃、1時間加熱する。その後、成形型を恒温槽から取り出し、室内に1時間放置して、得られた成形体(固形物)を試験体とする。
<Test body>
After mixing the powder with a Henschel mixer, dimethylpolysiloxane 6CS as a solvent was added to the resulting mixture to prepare a slurry. The resulting slurry is poured into a mold (middle plate) while being sucked. The slurry filled in the mold is heated in a constant temperature bath at 70° C. for 1 hour. After that, the mold is taken out from the constant temperature bath and left in a room for 1 hour, and the obtained molded article (solid matter) is used as a test piece.
 <溶媒抜け>
 得られたスラリーを吸引した際の揮発性溶媒のティッシュへの広がり具合から、不揮発溶媒の除去のしやすさ(溶媒抜け)を評価した。溶媒抜けの評価基準を以下に示す。なお、A、Bの場合は、溶媒抜けが良好であると評価し、評価がCの場合は、溶媒抜けが不良であると評価した。
 A:とても広がりがよい
 B:やや広がりがよい
 C:広がりが悪い
<Solvent removal>
Ease of removal of the non-volatile solvent (solvent removal) was evaluated from the degree of spread of the volatile solvent on the tissue when the obtained slurry was sucked. Evaluation criteria for solvent removal are shown below. In addition, in the cases of A and B, it was evaluated that solvent removal was good, and in the case of evaluation C, it was evaluated that solvent removal was poor.
A: Very good spread B: Slightly good spread C: Poor spread
 <表面状態>
 得られた成形体(固形物)の表面状態を目視で観察した。表面状態の評価基準を以下に示す。なお、A、Bの場合は、表面状態が良好であると評価し、評価がCの場合は、表面状態が不良であると評価した。
 A:表面がとても平滑である
 B:表面がやや平滑である
 C:表面に凹凸がある
<Surface condition>
The surface condition of the obtained molded article (solid matter) was visually observed. Evaluation criteria for the surface state are shown below. In the cases of A and B, the surface condition was evaluated as good, and in the case of evaluation C, the surface condition was evaluated as poor.
A: Very smooth surface B: Somewhat smooth surface C: Rough surface
 <耐衝撃性>
 試験体を30cmの高さから金属板上に落下させ、中皿から抜ける等の状態が維持できなくなるまでの落下の回数を調べた。試験数(N)は3である。耐衝撃性の評価基準を以下に示す。なお、A、Bの場合は、耐衝撃性が良好であると評価し、評価がCの場合は、耐衝撃性が不良であると評価した。
 A:10回以上
 B:5回以上10回未満
 C:5回未満
<Impact resistance>
A test piece was dropped from a height of 30 cm onto a metal plate, and the number of times it dropped until it could no longer maintain a state such as falling out of the middle plate was examined. The number of tests (N) is three. Evaluation criteria for impact resistance are shown below. In the cases of A and B, the impact resistance was evaluated as good, and in the case of the evaluation of C, the impact resistance was evaluated as poor.
A: 10 times or more B: 5 times or more and less than 10 times C: Less than 5 times
 以下、実施例及び比較例について、成分の配合と評価の結果を表1に示す。 Table 1 below shows the composition of ingredients and the evaluation results for Examples and Comparative Examples.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
 表1において、機能性粉末(パール剤)の仕様は、以下の通りである。
・合成金雲母・酸化チタン・酸化スズ※1:TWINCLEPEARL(登録商標)400(日本光研工業社製)
・合成金雲母・酸化チタン・酸化スズ※2:TWINCLEPEARL(登録商標)500(日本光研工業社製)
In Table 1, specifications of the functional powder (pearl agent) are as follows.
・ Synthetic phlogopite ・ Titanium oxide ・ Tin oxide * 1: TWINCLEPEARL (registered trademark) 400 (manufactured by Nihon Koken Kogyo Co., Ltd.)
・ Synthetic phlogopite ・ Titanium oxide ・ Tin oxide * 2: TWINCLEPEARL (registered trademark) 500 (manufactured by Nihon Koken Kogyo Co., Ltd.)
 表1において、配合されるワックスの仕様は、以下の通りである。
・ホホバエステル:フローラエステル70HG(FLORATECH社製)(平均粒子径10~100μm)
In Table 1, the specifications of the wax to be blended are as follows.
・ Jojoba ester: Flora Ester 70HG (manufactured by FLORATECH) (average particle size 10 to 100 μm)
 表1において、配合される不揮発性炭化水素油の仕様は、以下の通りである。
・水添ポリデセン:オレフィンオリゴマー30(日光ケミカルズ社製)(20℃粘度25~37mPa・s)
・ミネラルオイル:流動パラフィン(20℃粘度21~26mPa・s)
・ワセリン:半固形
・トリエチルヘキサノイン:RA-G-308(日本精化社製)(20℃粘度20~35mPa・s)
In Table 1, the specifications of the blended non-volatile hydrocarbon oil are as follows.
・ Hydrogenated polydecene: Olefin Oligomer 30 (manufactured by Nikko Chemicals Co., Ltd.) (viscosity at 20 ° C.: 25 to 37 mPa s)
・Mineral oil: liquid paraffin (viscosity 21 to 26 mPa s at 20°C)
・ Vaseline: semi-solid ・ Triethylhexanoin: RA-G-308 (manufactured by Nippon Fine Chemical Co., Ltd.) (viscosity at 20 ° C. 20 to 35 mPa s)
 表1において、配合される不揮発性溶媒の仕様は、以下の通りである。
・ジメチルポリシロキサン6CS:シリコーンKF-96A-6T(後添加)(信越化学工業社製)
なお、表1におけるジメチルポリシロキサン6CSは、上述のように、混合物に溶媒として添加されたものであるが、吸引により一部が除去され、最終的に得られた固形物中に油分として残存するものである。
In Table 1, specifications of the non-volatile solvent to be blended are as follows.
・ Dimethylpolysiloxane 6CS: Silicone KF-96A-6T (post-addition) (manufactured by Shin-Etsu Chemical Co., Ltd.)
As described above, the dimethylpolysiloxane 6CS in Table 1 was added to the mixture as a solvent, but part of it was removed by suction and remained as oil in the finally obtained solid. It is.
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
 表2において、機能性粉末(パール剤)の仕様は、表1の合成金雲母・酸化チタン・酸化スズ※1、※2と同様である。 In Table 2, the specifications of the functional powder (pearl agent) are the same as the synthetic phlogopite/titanium oxide/tin oxide *1, *2 in Table 1.
 表2において、配合されるワックスの仕様は、以下の通りである。
・ホホバエステル※1:フローラエステル70HG(FLORATECH社製)(融点65℃、平均粒子径550μm)
・ホホバエステル※2:フローラエステル70HG(FLORATECH社製)(融点65℃、平均粒子径10~100μm)
・パラフィンワックス:プレスエイド(登録商標)(プレスパース社製)(融点105~125℃、平均粒子径6~7.5μm)
・パルミチン酸:融点58~68℃、平均粒子径800μm
・ポリエチレンワックス:パフォーマレンPL(ニューフェーズテクノロジー社製)(融点83~90℃、平均粒子径870μm)
・ミリスチン酸ミリスチル:融点41~45℃、平均粒子径100~300μm
・トリ酢酸テトラステアリン酸スクロース:シュガーワックス(登録商標)A-10E(第一工業製薬社製)(融点44~50℃、平均粒子径500μm)
・パラフィン・マイクロクリスタリンワックス:パーミック160(日興リカ社製)(融点66~73℃、平均粒子径3000~5000μm)
In Table 2, the specifications of the wax to be blended are as follows.
・ Jojoba ester * 1: Flora ester 70HG (manufactured by FLORATECH) (melting point 65 ° C., average particle size 550 μm)
・Jojoba Ester *2: Flora Ester 70HG (manufactured by FLORATECH) (melting point 65 ° C, average particle size 10 to 100 μm)
・ Paraffin wax: Press Aid (registered trademark) (manufactured by Presperse Co., Ltd.) (melting point 105 to 125 ° C., average particle size 6 to 7.5 μm)
・Palmitic acid: Melting point 58-68°C, average particle size 800μm
・ Polyethylene wax: Performalen PL (manufactured by New Phase Technology) (melting point 83-90 ° C., average particle size 870 μm)
・Myristyl myristate: Melting point 41 to 45°C, average particle size 100 to 300 µm
・ Sucrose triacetate tetrastearate: Sugar Wax (registered trademark) A-10E (manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) (melting point 44 to 50 ° C., average particle size 500 μm)
・ Paraffin/microcrystalline wax: Permic 160 (manufactured by Nikko Rica) (melting point 66-73° C., average particle size 3000-5000 μm)
 表2において、配合される不揮発性炭化水素油の仕様は、表1の水添ポリデセンと同様である。 In Table 2, the specifications of the non-volatile hydrocarbon oil to be blended are the same as those of hydrogenated polydecene in Table 1.
 表2において、配合される不揮発性溶媒の仕様は、表1のジメチルポリシロキサン6CSと同様である。 In Table 2, the specifications of the non-volatile solvent to be blended are the same as those of dimethylpolysiloxane 6CS in Table 1.
 また、表2において、成分の粒径は、スラリーが成形型に充填される前のワックスの平均粒子径を意味する。 Also, in Table 2, the particle size of the component means the average particle size of the wax before the slurry is filled into the mold.
 表1、表2より、実施例1~9は、溶媒抜けが良好であった。このうち実施例3~9は、さらに表面状態が良好であり、中でも実施例3、4、7は、さらに耐衝撃性が良好であった。 From Tables 1 and 2, Examples 1 to 9 showed good solvent removal. Of these, Examples 3 to 9 had even better surface conditions, and Examples 3, 4 and 7 among them had even better impact resistance.
 これに対して、比較例1~3は、溶媒抜けが不良であり、このうち比較例3は、さらに表面状態と耐衝撃性がいずれも不良であった。 On the other hand, in Comparative Examples 1 to 3, solvent removal was poor, and of these, Comparative Example 3 was further poor in both surface condition and impact resistance.
 これらの結果から、粉末状のワックス及び液状の不揮発性炭化水素油を含む混合物を調製する工程と、混合物に不揮発性溶媒を添加してスラリーを調製する工程と、スラリーを吸引し且つ容器に充填する工程と、容器内のスラリーをワックスの溶融温度以上の温度に加熱する工程と、を含む固形組成物の製造方法により、不揮発性溶媒の除去が容易になり、化粧料の品質の低下を抑制する固形組成物が得られることが判った。 From these results, the steps of preparing a mixture containing powdered wax and liquid non-volatile hydrocarbon oil, adding a non-volatile solvent to the mixture to prepare a slurry, sucking the slurry and filling it into a container and the step of heating the slurry in the container to a temperature equal to or higher than the melting temperature of the wax. It has been found that a solid composition which does well is obtained.
 以上、本発明の実施形態について説明したが、本発明は特定の実施形態に限定されるものではなく、請求の範囲に記載された発明の範囲内において、種々の変形、変更が可能である。 Although the embodiments of the present invention have been described above, the present invention is not limited to specific embodiments, and various modifications and changes are possible within the scope of the invention described in the claims.
 本出願は、2021年4月16日に出願された日本国特許出願2021-69865号に基づく優先権を主張するものであり、その全内容をここに援用する。 This application claims priority based on Japanese Patent Application No. 2021-69865 filed on April 16, 2021, the entire contents of which are incorporated herein.

Claims (10)

  1.  粉末状のワックス及び液状の不揮発性炭化水素油を含む混合物を調製する工程と、
     前記混合物に不揮発性溶媒を添加してスラリーを調製する工程と、
     前記スラリーを吸引し且つ容器に充填する工程と、
     前記容器内の前記スラリーを前記ワックスの溶融温度以上の温度に加熱する工程と、を含む、
     固形組成物の製造方法。
    preparing a mixture comprising powdered wax and liquid non-volatile hydrocarbon oil;
    adding a non-volatile solvent to the mixture to prepare a slurry;
    aspirating the slurry and filling a container;
    heating the slurry in the container to a temperature equal to or higher than the melting temperature of the wax;
    A method for producing a solid composition.
  2.  前記ワックスの平均粒子径が1μm以上1000μm以下である、請求項1に記載の固形組成物の製造方法。 The method for producing a solid composition according to claim 1, wherein the wax has an average particle size of 1 µm or more and 1000 µm or less.
  3.  前記ワックスに対する前記不揮発性炭化水素油の質量比が、1以上6以下である、請求項1または2に記載の固形組成物の製造方法。 The method for producing a solid composition according to claim 1 or 2, wherein the mass ratio of said non-volatile hydrocarbon oil to said wax is 1 or more and 6 or less.
  4.  前記不揮発性炭化水素油の粘度が、20℃において10mPa・s以上50mPa・s以下である、請求項1乃至3のいずれか一項に記載の固形組成物の製造方法。 The method for producing a solid composition according to any one of claims 1 to 3, wherein the nonvolatile hydrocarbon oil has a viscosity of 10 mPa·s or more and 50 mPa·s or less at 20°C.
  5.  前記不揮発性炭化水素油が、水添ポリデセンである、請求項1乃至4のいずれか一項に記載の固形組成物の製造方法。 The method for producing a solid composition according to any one of claims 1 to 4, wherein the non-volatile hydrocarbon oil is hydrogenated polydecene.
  6.  前記不揮発性溶媒がシリコーン油である、請求項1乃至5のいずれか一項に記載の固形組成物の製造方法。 The method for producing a solid composition according to any one of claims 1 to 5, wherein the non-volatile solvent is silicone oil.
  7.  前記混合物に球状粉末が含まれている、請求項1乃至6のいずれか一項に記載の固形組成物の製造方法。 The method for producing a solid composition according to any one of claims 1 to 6, wherein the mixture contains spherical powder.
  8.  前記球状粉末の平均粒子径が1μm以上10μm以下である、請求項7に記載の固形組成物の製造方法。 The method for producing a solid composition according to claim 7, wherein the spherical powder has an average particle size of 1 µm or more and 10 µm or less.
  9.  請求項1乃至8のいずれか一項に記載の製造方法によって製造された固形組成物。 A solid composition produced by the production method according to any one of claims 1 to 8.
  10.  請求項9に記載の固形組成物を含む化粧料。 A cosmetic containing the solid composition according to claim 9.
PCT/JP2022/013266 2021-04-16 2022-03-22 Production method for solid composition, solid composition, and cosmetic WO2022220027A1 (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10338618A (en) * 1997-06-04 1998-12-22 Kose Corp Oily solid cosmetic
JP2007291074A (en) * 2006-03-31 2007-11-08 Kose Corp Solid powder cosmetic and method for manufacturing solid powder cosmetic
JP2011105605A (en) * 2009-11-12 2011-06-02 Key Tranding Co Ltd Manufacturing method of solid powdery cosmetic
JP2020183352A (en) * 2019-05-07 2020-11-12 花王株式会社 Solid powder cosmetic
JP2021020867A (en) * 2019-07-26 2021-02-18 日本メナード化粧品株式会社 Solid powder cosmetic

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10338618A (en) * 1997-06-04 1998-12-22 Kose Corp Oily solid cosmetic
JP2007291074A (en) * 2006-03-31 2007-11-08 Kose Corp Solid powder cosmetic and method for manufacturing solid powder cosmetic
JP2011105605A (en) * 2009-11-12 2011-06-02 Key Tranding Co Ltd Manufacturing method of solid powdery cosmetic
JP2020183352A (en) * 2019-05-07 2020-11-12 花王株式会社 Solid powder cosmetic
JP2021020867A (en) * 2019-07-26 2021-02-18 日本メナード化粧品株式会社 Solid powder cosmetic

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