WO2024095598A1 - Method for producing oily dispersion, and cosmetic material having said oily dispersion blended therein - Google Patents

Method for producing oily dispersion, and cosmetic material having said oily dispersion blended therein Download PDF

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Publication number
WO2024095598A1
WO2024095598A1 PCT/JP2023/032178 JP2023032178W WO2024095598A1 WO 2024095598 A1 WO2024095598 A1 WO 2024095598A1 JP 2023032178 W JP2023032178 W JP 2023032178W WO 2024095598 A1 WO2024095598 A1 WO 2024095598A1
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Prior art keywords
oil
dispersion
inorganic oxide
oxide powder
producing
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PCT/JP2023/032178
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French (fr)
Japanese (ja)
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昇 長谷
昌平 中村
純也 中野
萌 秦
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日光ケミカルズ株式会社
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Publication of WO2024095598A1 publication Critical patent/WO2024095598A1/en

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/27—Zinc; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29—Titanium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons

Definitions

  • the present invention relates to a method for producing an oil dispersion and a cosmetic containing the oil dispersion. More specifically, the present invention relates to a method for producing an oil dispersion that can be dispersed in an oil even if it has a high solid content by adding inorganic oxide powder to a fatty acid ester oil at a specific temperature, and to a cosmetic containing the oil dispersion produced by this production method.
  • oil dispersions for cosmetics are made by pre-dispersing pigments in an oily medium, which are blended into makeup cosmetics such as foundation, eye shadow, and blush, as well as basic cosmetics such as sunscreen cosmetics, hair cosmetics, milky lotions, and creams.
  • makeup cosmetics such as foundation, eye shadow, and blush
  • basic cosmetics such as sunscreen cosmetics, hair cosmetics, milky lotions, and creams.
  • inorganic oxide powders have strong cohesive forces between the powders, making them difficult to disperse in oil as is. Therefore, pigments used in oil dispersions are widely subjected to hydrophobic treatment in order to make it easier to disperse the inorganic oxide powder in oil.
  • a method is known in which the pigment surface is coated with silicones such as higher fatty acids, higher alcohols, hydrocarbons, silicone oils, and silicone resins to impart hydrophobicity.
  • silicones such as higher fatty acids, higher alcohols, hydrocarbons, silicone oils, and silicone resins to impart hydrophobicity.
  • many methods have been established to date for hydrophobizing pigments using silicones as surface treatment agents (see, for example, Patent Documents 1 and 2), and oil dispersions using these methods are also widely known (see, for example, Patent Documents 3, 4, and 5).
  • inorganic oxide powders have strong cohesive forces between the powder particles, it is common to disperse the inorganic oxide powder by adding silicone-based dispersants such as polyether-modified silicone or surfactants in order to suppress re-agglomeration after dispersion and maintain dispersion stability (see, for example, Patent Documents 6 and 7).
  • the method of hydrophobizing inorganic oxide powder requires a step of first treating the inorganic oxide powder with a surface treatment agent before an oil-based dispersion can be produced, which is problematic in terms of its complexity.
  • the present invention was made in consideration of the problems described above, and aims to provide a method for producing an oil dispersion that does not require prior surface treatment of the inorganic oxide powder to enhance its dispersibility in oil agents, and that can obtain an oil dispersion with excellent dispersibility of inorganic oxide powder without the addition of a dispersant, and a cosmetic that contains the oil dispersion produced by this production method.
  • an oil-based dispersion with high powder dispersibility can be obtained by heating an ester oil of a fatty acid having 8 to 22 carbon atoms at a temperature of 70°C to 120°C while adding an inorganic oxide powder, and further, that an oil-based dispersion capable of maintaining high pigment dispersibility can be obtained without using a dispersant, thus completing the present invention.
  • the method for producing an oil-based dispersion according to one embodiment of the present invention is characterized by including a step (1) of gradually adding inorganic oxide powder to an ester oil of an ester oil of a fatty acid having 8 to 22 carbon atoms while heating the ester oil at a temperature of 70°C to 120°C, and a step (2) of further mixing the dispersion to which the entire amount of inorganic oxide powder has been added at a temperature of 70°C to 120°C.
  • step (2) of the above production method it is preferable to use a kneading mixer or a wet mixer for dispersion in step (2) of the above production method.
  • One embodiment of the method for producing an oil dispersion of the present invention is a method for producing an oil dispersion, which includes step (1) of adding inorganic oxide powder while heating ester oil of fatty acid having 8 to 22 carbon atoms at a temperature of 70°C to 120°C, and step (2) of further mixing the dispersion to which the entire amount of inorganic oxide powder has been added at a temperature of 70°C to 120°C, and then cooling the oil dispersion and further dispersing it using a wet mixer/disperser.
  • step (2) of the above production method it is preferable to cool the mixture to room temperature (20°C to 30°C) and further disperse the mixture using a wet mixer.
  • the solids concentration of the inorganic oxide powder during production of the oil dispersion is 25% by mass or more.
  • the cosmetic of the present invention is characterized by containing an oil dispersion produced by the production method of the present invention.
  • the method for producing an oil-based dispersion of the present invention is characterized by including a step (1) of adding inorganic oxide powder to an ester oil of an ester oil of a fatty acid having 8 to 22 carbon atoms while heating the ester oil at a temperature of 70°C to 120°C, and a step (2) of further mixing the dispersion to which the entire amount of inorganic oxide powder has been added at a temperature of 70°C to 120°C.
  • the present invention by gradually adding inorganic oxide powder to an ester oil of a fatty acid having 8 to 22 carbon atoms while heating it at a temperature of 70°C to 120°C, it is possible to obtain an oil dispersion with high pigment dispersibility, an oil dispersion that can maintain high powder dispersibility even without the use of a dispersant, and a cosmetic product containing the same.
  • the ester oil of fatty acids having 8 to 22 carbon atoms (hereinafter, simply referred to as ester oil) used as a dispersion medium is an ester oil in which the carbon number of the fatty acid-derived portion is 8 to 22.
  • ester oil in which the carbon number of the fatty acid-derived portion is 8 to 22.
  • at least one of the fatty acids has a carbon number of 8 to 22, and preferably all of the fatty acids have a carbon number of 8 to 22.
  • tri(caprylic/capric)glyceryl is an ester of caprylic acid (C8)/capric acid (C10) and glycerin, so the fatty acid portion has 8 carbon atoms and 10 carbon atoms.
  • ester oil of fatty acids having 8 to 22 carbon atoms is non-volatile and has fluidity such as liquid or paste at 25°C.
  • non-volatile means that it does not volatilize at 25°C, but for example, it is a component whose boiling point at normal pressure exceeds 250°C.
  • Ester oil of fatty acids having less than 8 carbon atoms is not preferable because it is not possible to obtain an oil-based dispersion with good dispersibility of inorganic oxide powder.
  • a hydrocarbon oil or silicone oil other than the above ester oil is used, an oil-based dispersion with good dispersibility of the inorganic oxide powder cannot be obtained.
  • the ester oil of a fatty acid having 8 to 22 carbon atoms is an ester of a fatty acid having 8 to 18 carbon atoms.
  • the fatty acid may be a saturated fatty acid or an unsaturated fatty acid, but it is preferable that it is a saturated fatty acid, and the saturated fatty acid may be a straight chain or a branched chain.
  • ester oils include, for example, isononyl isononanoate, isodecyl isononanoate, isotridecyl isononanoate, tricyclodecane methyl isononanoate, (caprylic acid/capric acid) coconut alkyl, hexyl laurate, methylheptyl laurate, caprylyl laurate, decyl laurate, isopropyl myristate, methylheptyl myristate, 2-hexyldecyl myristate, octyldodecyl myristate, isopropyl palmitate, methylheptyl palmitate, palmitic acid, methylheptyl palmitate ...
  • monoester oils such as 2-ethylhexyl ester, 2-ethylhexyl stearate, ethyl isostearate, isopropyl isostearate, isobutyl isostearate, decyl isostearate, methylheptyl isostearate, 2-hexyldecyl isostearate, 2-ethylhexyl hydroxystearate, octyldodecyl oleate, oleyl oleate, octyldodecyl ricinoleate, octyl p-methoxycinnamate, alkyl benzoate, and glyceryl isostearate; diisostearate, polyglyceryl diisostearate, propanediol diisostearate, di(phytosteryl/octyldodecyl) lauroyl glutamate, di(cholesteryl/behen
  • Triester oils such as trimethylolpropane triisostearate, diglyceryl triisostearate, diglyceryl triisostearate, tri(caprylic/capric)glyceryl, glyceryl trioctanoate, macadamia nut oil, olive oil, castor oil, jojoba oil, avocado oil, and sunflower oil; pentaerythrityl tetraoctanoate, diglyceryl tetraisostearate, dipentaerythrityl tetraisostearate, and pentaerythritol tetraisostearate.
  • the ester oil is at least one selected from the group consisting of coconut alkyl (caprylic/capric acid), isopropyl myristate, 2-ethylhexyl palmitate, 2-ethylhexyl stearate, decyl isostearate, methylheptyl isostearate, diglyceryl triisostearate, tri(caprylic/capric acid)glyceryl, jojoba oil, diglyceryl tetraisostearate, and dipentaerythrityl tetraisostearate.
  • the fatty acid ester oil contains tri(caprylic/capric acid)glyceryl.
  • examples of inorganic oxide powder include inorganic oxides such as silicic anhydride (silicon oxide), aluminum oxide, iron oxide (red iron oxide, yellow iron oxide, black iron oxide, etc.), titanium oxide, zinc oxide, cerium oxide, and bismuth oxide that are generally used in cosmetics.
  • examples of inorganic oxides include fine particles of titanium oxide, zinc oxide, cerium oxide, bismuth oxide, and composites thereof.
  • the inorganic oxide powder is preferably titanium oxide and/or iron oxide.
  • the inorganic oxide is an inorganic oxide powder that has not been treated with a fatty acid. In another preferred embodiment, the inorganic oxide powder has not been hydrophobized.
  • hydrophobization refers to treatment with a known hydrophobizing surface treatment agent such as silicone treatment or fatty acid treatment.
  • a known hydrophobizing surface treatment agent such as silicone treatment or fatty acid treatment.
  • an inorganic oxide that has not been hydrophobized in this way dispersibility is maintained over time.
  • the inorganic oxide powder is an untreated powder.
  • An untreated powder refers to a powder that has not been surface-treated with a surface treatment agent.
  • the particle size of the inorganic oxide is, for example, 0.001 to 50 ⁇ m, and may be 0.01 to 30 ⁇ m.
  • the particle size is based on volume and can be measured using a laser diffraction particle size distribution analyzer.
  • the solids concentration of the inorganic oxide powder in the oil dispersion is preferably 25% by mass or more, more preferably 25 to 80% by mass, even more preferably 30 to 80% by mass, even more preferably 40 to 80% by mass, and particularly preferably 40 to 70% by mass. If the solids concentration of the inorganic oxide powder is 25% by mass or more, the dispersibility of the inorganic oxide powder over time will be good, and if it is 80% by mass or less, the aggregation of the powder will be easily suppressed.
  • the method for producing the oil dispersion of the present invention is a production method that is carried out in the following order: step (1) and step (2).
  • Step (1) the inorganic oxide powder is added to the ester oil of an ester oil of a fatty acid having 8 to 22 carbon atoms while heating the ester oil at a temperature of 70° C. to 120° C., until the entire target amount is added. It is also preferable to gradually add the inorganic oxide powder to the ester oil.
  • the temperature of the ester oil is preferably 70°C to 100°C.
  • the temperature of the ester oil is preferably maintained within the above temperature range while the inorganic oxide powder is being added. It is preferable to heat the ester oil using an appropriate heating means so that the temperature is maintained within the above temperature range.
  • the time for adding the inorganic oxide powder to the ester oil is, for example, 1 to 100 minutes.
  • a dispersion method for obtaining an oil dispersion can be used in which the inorganic oxide powder is added while stirring the ester oil using a stirrer such as a homomixer or disperser.
  • the rotation speed during stirring is not particularly limited as long as the dispersion proceeds well, but is, for example, 1000 rpm to 5000 rpm.
  • dispersant in step (1).
  • examples of dispersants include those listed below.
  • Step (2) The oil dispersion obtained in the step (1) is further mixed at a temperature of 70° C. to 120° C. to obtain an oil-based dispersion.
  • the dispersion time in the step (2) is preferably 2 hours or more from the viewpoint of dispersibility of the inorganic oxide powder in the ester oil, and more preferably 2 hours to 10 hours, and even more preferably 2 hours to 5 hours, from the viewpoint of saturation of the effect.
  • dispersion may continue using a homomixer, disperser, etc., but it is preferable to use a kneading mixer capable of applying a higher shear force, such as a kneader mixer, Henschel mixer, roll mixer, or extruder mixer, or a wet mixer and disperser, such as a propeller mixer, high-speed mixer, dissolver, ultemizer, wet jet mill, colloid mill, mass colloider, (wet) bead mill, sand mill, basket mill, or AD mill.
  • a kneading mixer capable of applying a higher shear force
  • a kneader mixer Henschel mixer, roll mixer, or extruder mixer
  • a wet mixer and disperser such as a propeller mixer, high-speed mixer, dissolver, ultemizer, wet jet mill, colloid mill, mass colloider, (wet) bead mill, sand mill, basket mill, or AD mill.
  • a dispersant may be used.
  • dispersants include polyhydroxystearic acid, glyceryl hydroxystearate, polyglyceryl-2 diisostearate, polyglyceryl-2 triisostearate, polyglyceryl-2 tetraisostearate, erythrityl triethylhexanoate, and sorbitan sesquiisostearate. One or more of these may be used. Of these dispersants, it is most preferable to use polyhydroxystearic acid. From the viewpoint of dispersibility, the amount of dispersant used is, for example, 1 to 10 parts by mass per 100 parts by mass of the inorganic oxide.
  • the temperature conditions during production are preferably such that the ester oil and oil dispersion are heated to a temperature of 70°C to 120°C. Temperatures below 70°C are not preferred because the inorganic oxide powder cannot be uniformly dispersed in the ester oil. Temperatures above 120°C are also not preferred because the ester oil decomposes and the yellow iron oxide and black iron oxide in the inorganic oxide powder discolor.
  • the mixing temperature of the oil dispersion is preferably 70°C to 100°C in terms of the effects of the present invention. It is preferable that the temperature is within the above range during mixing, and that the temperature range is maintained while heating using an appropriate heating means.
  • steps (1) and (2) it is preferable to cool the oil dispersion and then perform an additional dispersion step, since this will further atomize the inorganic oxide powder and make it more uniformly dispersed in the oil. Cooling is preferably performed until the temperature drops to 40°C or lower, and preferably to room temperature (20°C to 30°C). Examples of cooling methods include a method in which the mixture is left to stand while continuing to stir; and a method in which the mixture is cooled using a cooling means while continuing to stir.
  • the dispersing machine used for dispersion after cooling is preferably a wet mixer dispersing machine from the viewpoint of improving the dispersibility of the inorganic oxide powder in the oil dispersion, and among these, a wet bead mill is preferable. Specific examples of wet mixer dispersing machines are as described above.
  • the dispersion time for dispersion after cooling is, for example, 15 minutes to 5 hours, and may be 30 minutes to 3 hours.
  • a dispersant when the oil dispersion is blended with a cosmetic, a dispersant can be used in the manufacturing process of the oil dispersion to the extent that it does not affect the storage stability or cosmetic durability of the cosmetic.
  • the dispersant include polyhydroxystearic acid, glyceryl hydroxystearate, polyglyceryl-2 diisostearate, polyglyceryl-2 triisostearate, polyglyceryl-2 tetraisostearate, erythrityl triethylhexanoate, sorbitan sesquiisostearate, etc., and one or more of these can be used.
  • polyhydroxystearic acid glyceryl hydroxystearate
  • polyglyceryl-2 diisostearate polyglyceryl-2 triisostearate
  • polyglyceryl-2 tetraisostearate polyerythrityl triethylhexanoate
  • sorbitan sesquiisostearate etc.
  • the cosmetic of the present invention uses a highly safe ester oil by blending the oil dispersion prepared by the above-mentioned manufacturing method, and therefore has good compatibility with other cosmetic ingredients, and has good stability over time and a good feel despite its high solids concentration, and can also be used to create cosmetics such as sunscreens with high SPF values and transparency.
  • Specific examples of cosmetics that can be used include makeup cosmetics such as foundations, eye shadows, and blushes, as well as basic cosmetics such as sunscreen cosmetics, hair cosmetics, emulsions, and creams.
  • the amount of oil dispersion blended is not particularly limited, but is preferably 0.1 to 90% by mass in the cosmetic.
  • the cosmetic of the present invention may contain ingredients that are normally used in cosmetics, such as powders, surfactants, oils, gelling agents, polymers, beauty ingredients, moisturizers, pigments, preservatives, fragrances, etc., to the extent that the effects of the present invention are not impaired.
  • the cosmetic composition of the present invention may be in any form, including powder, emulsion, cream, stick, solid, spray, and multi-layered separation.
  • Example 1 40 g of 2-ethylhexyl palmitate was heated to 90°C. After confirming that the temperature had reached 90°C, 60 g of titanium oxide (particle diameter: 0.2 ⁇ m) was gradually added over 10 minutes while stirring the 2-ethylhexyl palmitate with a disper at 2000 rpm. After the entire amount of titanium oxide was added, the mixture was further stirred at 90°C with a disper at 2000 rpm for 3 hours to obtain an oil-based dispersion of titanium oxide with a solid content concentration of 60% by mass.
  • titanium oxide particle diameter: 0.2 ⁇ m
  • Example 2 An oil dispersion of red iron oxide having a solid content concentration of 60 mass % was obtained in the same manner as in Example 1, except that red iron oxide (particle diameter: 0.5 ⁇ m) was used instead of titanium oxide.
  • Example 3 An oil dispersion of yellow iron oxide having a solid content concentration of 60 mass % was obtained in the same manner as in Example 1, except that yellow iron oxide (particle diameter: 0.7 ⁇ m) was used instead of titanium oxide.
  • Example 4 An oil dispersion of black iron oxide having a solid content concentration of 60 mass % was obtained in the same manner as in Example 1, except that black iron oxide (particle diameter: 0.2 ⁇ m) was used instead of titanium oxide.
  • Example 5 The oil dispersion obtained in Example 1 was allowed to stand while continuing to stir and cooled to room temperature (25°C), and was then dispersed and mixed for 1 hour using a wet bead mill (DYNO-MILL, Shinmaru Enterprises) under conditions of a peripheral speed of 10 m/s, ⁇ 0.5 mm zirconia beads, and a packing rate of 70%, to obtain an oil dispersion of titanium oxide with a solid content concentration of 60 mass%.
  • DYNO-MILL Shinmaru Enterprises
  • Example 6 47 g of tri(caprylic/capric)glyceryl is heated to 90°C. After confirming that the temperature has reached 90°C, 50 g of fine titanium dioxide particles (MT-05, manufactured by Teika Co., Ltd.) are gradually added over 9 minutes while stirring the tri(caprylic/capric)glyceryl with a disperser at 2000 rpm. The entire amount of fine titanium dioxide particles is charged, and 3 g of polyhydroxystearic acid (Salacos HS-6C, manufactured by Nisshin Oillio Group Co., Ltd.) is added as a dispersant.
  • MT-05 fine titanium dioxide particles
  • disperser 2000 rpm
  • the mixture is then dispersed for 2 hours using a wet bead mill (DYNO-MILL, manufactured by Shinmaru Enterprises Co., Ltd.) under conditions of a peripheral speed of 10 m/s, ⁇ 0.5 mm zirconia beads, a filling rate of 70%, and a temperature of 90°C, to obtain an oil-based dispersion having a solid concentration of fine titanium dioxide particles of 50% by mass.
  • a wet bead mill DYNO-MILL, manufactured by Shinmaru Enterprises Co., Ltd.
  • Example 7 An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that coconut alkyl caprylate/caprate was used instead of 2-ethylhexyl palmitate.
  • Example 8 An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that isopropyl myristate was used instead of 2-ethylhexyl palmitate.
  • Example 9 60 g of 2-ethylhexyl stearate was heated to 80° C. After confirming that the temperature had reached 80° C., 40 g of zinc oxide fine particles (MZ-500, manufactured by Teica Corporation) was gradually added over 8 minutes while stirring the 2-ethylhexyl stearate with a disper at 2000 rpm. After the entire amount of zinc oxide was added, the mixture was further stirred at 80° C. and 2000 rpm with a disper for 3 hours to obtain an oil-based dispersion of zinc oxide fine particles having a solid content concentration of 40% by mass.
  • MZ-500 zinc oxide fine particles
  • Example 10 50 g of decyl isostearate was heated to 70° C. After confirming that the temperature had reached 70° C., 50 g of titanium oxide was gradually added over 9 minutes while stirring the decyl isostearate with a disper at 2000 rpm. After the entire amount of titanium oxide was added, the mixture was further stirred at 70° C. and 2000 rpm with a disper for 3 hours to obtain an oil dispersion of titanium oxide with a solid content concentration of 50% by mass.
  • Example 11 30 g of methylheptyl isostearate was heated to 100° C. After confirming that the temperature had reached 100° C., 70 g of titanium oxide was gradually added over 11 minutes while stirring the methylheptyl isostearate with a disper at 2000 rpm. After the entire amount of titanium oxide was added, the mixture was further stirred at 100° C. and 2000 rpm with a disper for 3 hours to obtain an oil dispersion of titanium oxide with a solid content concentration of 70% by mass.
  • Example 12 An oil dispersion of titanium oxide having a solids concentration of 50 mass % was obtained in the same manner as in Example 10, except that diglyceryl triisostearate was used instead of decyl isostearate.
  • Example 13 An oil dispersion of titanium oxide having a solids concentration of 70 mass % was obtained in the same manner as in Example 11, except that jojoba oil was used instead of methylheptyl isostearate.
  • Example 14 An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that diglyceryl tetraisostearate was used instead of 2-ethylhexyl palmitate.
  • Example 15 An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that dipentaerythrityl tetraisostearate was used instead of 2-ethylhexyl palmitate.
  • Example 16 40 g of 2-ethylhexyl palmitate was heated to 90°C. After confirming that the temperature had reached 90°C, 60 g of titanium oxide (particle diameter: 0.2 ⁇ m) was gradually added over 10 minutes while stirring the 2-ethylhexyl palmitate with a disper at 2000 rpm.
  • titanium oxide After the entire amount of titanium oxide was added, it was dispersed for 2 hours using a wet bead mill (DYNO-MILL, Shinmaru Enterprises) under conditions of a peripheral speed of 10 m/s, ⁇ 0.5 mm zirconia beads, a filling rate of 70%, and a temperature of 90°C, to obtain an oil-based dispersion of titanium oxide with a solid content concentration of 60% by mass.
  • DYNO-MILL Shinmaru Enterprises
  • Example 17 70 g of 2-ethylhexyl palmitate was heated to 90° C. After confirming that the temperature had reached 90° C., 30 g of titanium oxide was gradually added over 5 minutes while stirring the 2-ethylhexyl palmitate with a disper at 2000 rpm. After the entire amount of titanium oxide was added, the mixture was further stirred at a temperature of 90° C. for 3 hours to obtain an oil-based dispersion of titanium oxide with a solid content concentration of 30% by mass.
  • the products of the present invention had good dispersibility one day after production and after storage at 40°C for one month. It was also found that the products of the present invention have superior dispersibility, especially dispersibility over time, compared to Comparative Examples 1 to 6. It was also found that the oil dispersions of the products of the present invention have superior dispersibility over time compared to the case of using inorganic oxide powder that has been surface-treated in advance with a fatty acid.
  • Example 18 Oil-based foundation
  • An oil-based foundation was obtained by dispersing and mixing the blended composition shown in Table 2 with a homomixer.
  • the dispersion stability of Example 18 was good (no powder aggregation or settling occurred over time).
  • Example 19 Sunscreen cream A sunscreen cream was obtained using the formulation shown in Table 3 and the method described below. The dispersion stability of Example 19 was good.
  • Examples 18 and 19 were cosmetics with good pigment dispersion stability (no powder aggregation or settling occurred over time).
  • the oil dispersion produced by the manufacturing method of the present invention is characterized in that inorganic oxide powder, which tends to aggregate, is highly dispersible in oil agents. Furthermore, this oil dispersion can provide cosmetics with good dispersion stability, and has great industrial applicability.
  • the present invention includes the following aspects:
  • a method for producing an oil dispersion containing an inorganic oxide powder and an ester oil of a fatty acid having 8 to 22 carbon atoms comprising the steps of: (1) adding an inorganic oxide powder to the ester oil while heating the ester oil at a temperature of 70° C. to 120° C.; and (2) further mixing the dispersion to which the entire amount of the inorganic oxide powder has been added at a temperature of 70°C to 120°C.
  • step (2) A method for producing an oil-based dispersion according to (1) or (2) above, in which a kneading mixer or a wet mixer/disperser is used for mixing in step (2).
  • step (2) A method for producing an oil dispersion according to any one of (1) to (3) above, in which after step (2), the oil dispersion is cooled and further dispersed using a wet mixer/disperser.
  • a method for producing an oil-based dispersion in which after all steps of the production method described in (3) above, the oil-based dispersion is cooled and further dispersed using a wet mixer disperser.
  • oil dispersion is an oil dispersion consisting of only two components: inorganic oxide powder and an ester oil of a fatty acid having 8 to 22 carbon atoms.

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Abstract

The present invention addresses the problem of providing: a method for producing an oily dispersion having excellent dispersibility of an inorganic oxide powder without treating the surface of the inorganic oxide powder in advance to increase the dispersibility in an oil agent; and a cosmetic material having said oily dispersion blended therein. The inorganic oxide powder, which easily aggregates, is characterized in having high dispersibility in an oil agent. Also, the oily dispersion provides the cosmetic material with good dispersion stability.　The method for producing an oily dispersion produces an oily dispersion containing an inorganic oxide powder and an ester oil of a C8-22 fatty acid, the method comprising: a step (1) for adding the inorganic oxide power to the ester oil while heating the ester oil at a temperature of 70-120°C; and a step (2) for further mixing, at a temperature of 70-120°C, the dispersed product to which the entire amount of the inorganic oxide powder has been added.

Description

油性分散体の製造方法およびこの油性分散体を配合した化粧料Method for producing oil dispersion and cosmetic preparation containing said oil dispersion
　本発明は、油性分散体の製造方法および油性分散体を配合した化粧料に関する。さらに詳しくは、本発明は無機酸化物粉体を脂肪酸のエステル油に特定の温度において添加することで、高固形分であっても油剤に分散できる油性分散体の製造方法及びこの製造方法によって製造された油性分散体を配合した化粧料に関するものである。 The present invention relates to a method for producing an oil dispersion and a cosmetic containing the oil dispersion. More specifically, the present invention relates to a method for producing an oil dispersion that can be dispersed in an oil even if it has a high solid content by adding inorganic oxide powder to a fatty acid ester oil at a specific temperature, and to a cosmetic containing the oil dispersion produced by this production method.
　一般に、化粧料用の油性分散体は、ファンデーション、アイシャドウ、チークなどのメイクアップ化粧料や、サンスクリーン化粧料、頭髪化粧料、乳液、クリームなどの基礎化粧品に配合される顔料を予め油性媒体に高度に分散させている。このため、化粧料用の油性分散体は、化粧料の調製の際に顔料の飛散汚染が少ないことや、すでに顔料が高度に分散してあるために特殊な混合設備を必要としない等のハンドリング性の良さから、広く利用されている。 　In general, oil dispersions for cosmetics are made by pre-dispersing pigments in an oily medium, which are blended into makeup cosmetics such as foundation, eye shadow, and blush, as well as basic cosmetics such as sunscreen cosmetics, hair cosmetics, milky lotions, and creams. For this reason, oil dispersions for cosmetics are widely used due to their good handling properties, such as less scattering and contamination of pigments during the preparation of cosmetics, and no need for special mixing equipment because the pigments are already highly dispersed.
　また、無機酸化物粉体は粉体同士の凝集力が強いためそのままでは、油剤に分散させることが困難である。従って油性分散体に用いられる顔料には、無機酸化物粉体の油剤への分散を容易にする目的で疎水化処理を施すことが広く行われており、例えば、高級脂肪酸、高級アルコール、炭化水素、シリコーンオイル、シリコーン樹脂等のシリコーン類を用いて、顔料表面を被覆して、疎水性を付与する方法が知られている。中でも、シリコーン類を表面処理剤として用いた顔料の疎水化処理は現在までに多くの方法が確立されており（例えば、特許文献１、２参照）、それらを用いた油性分散体も広く知られている（例えば、特許文献３、４、５参照）。 In addition, inorganic oxide powders have strong cohesive forces between the powders, making them difficult to disperse in oil as is. Therefore, pigments used in oil dispersions are widely subjected to hydrophobic treatment in order to make it easier to disperse the inorganic oxide powder in oil. For example, a method is known in which the pigment surface is coated with silicones such as higher fatty acids, higher alcohols, hydrocarbons, silicone oils, and silicone resins to impart hydrophobicity. Among these, many methods have been established to date for hydrophobizing pigments using silicones as surface treatment agents (see, for example, Patent Documents 1 and 2), and oil dispersions using these methods are also widely known (see, for example, Patent Documents 3, 4, and 5).
　更に、無機酸化物粉体は、粉体同士の凝集力が強いことから、分散後の再凝集を抑制して分散安定性を維持するために、ポリエーテル変性シリコーンなどのシリコーン系分散剤や界面活性剤等を添加して無機酸化物粉体を分散させることが一般的に行われている（例えば、特許文献６、７参照）。 Furthermore, since inorganic oxide powders have strong cohesive forces between the powder particles, it is common to disperse the inorganic oxide powder by adding silicone-based dispersants such as polyether-modified silicone or surfactants in order to suppress re-agglomeration after dispersion and maintain dispersion stability (see, for example, Patent Documents 6 and 7).
特開昭６０－１６３９７３号公報Japanese Patent Application Laid-Open No. 60-163973 特開昭６２－１７７０７０号公報Japanese Patent Application Laid-Open No. 62-177070 特開２００２－８０７４８号公報JP 2002-80748 A 特開２００５－１７１１４５号公報JP 2005-171145 A 再表２０１１／００７６６８号公報Republished 2011/007668 特開２００７－２９１３７９号公報JP 2007-291379 A 特開２０１２－１８４１７８号公報JP 2012-184178 A
　しかしながら、無機酸化物粉体を疎水化処理する方法では、一旦、無機酸化物粉体を表面処理剤で表面処理する工程を経た後でないと油性分散体を作製することができず、煩雑さの点が問題である。 However, the method of hydrophobizing inorganic oxide powder requires a step of first treating the inorganic oxide powder with a surface treatment agent before an oil-based dispersion can be produced, which is problematic in terms of its complexity.
　また、分散剤や界面活性剤等を使用して得られた油性分散体を化粧料に配合した場合、化粧料の保存安定性や化粧持続性を悪化させるなど悪影響を及ぼす恐れがある。 In addition, when oil-based dispersions obtained using dispersants, surfactants, etc. are blended into cosmetics, there is a risk of adverse effects such as impairing the storage stability and cosmetic durability of the cosmetics.
　本発明は、前述のような問題点に鑑みてなされたものであり、無機酸化物粉体に油剤への分散性を高めるために予め表面処理を施すことを要さず、また分散剤を添加しなくても、無機酸化物粉体の分散性の優れた油性分散体を得るための油性分散体の製造法及びこの製造方法で製造された油性分散体を含有する化粧料を提供することを目的とするものである。 The present invention was made in consideration of the problems described above, and aims to provide a method for producing an oil dispersion that does not require prior surface treatment of the inorganic oxide powder to enhance its dispersibility in oil agents, and that can obtain an oil dispersion with excellent dispersibility of inorganic oxide powder without the addition of a dispersant, and a cosmetic that contains the oil dispersion produced by this production method.
　本発明者らは上記目的を達成すべく鋭意研究した結果、炭素数８～２２の脂肪酸のエステル油を７０℃～１２０℃の温度で加熱しながら、無機酸化物粉体を添加することで高い粉体分散性を有する油性分散体が得られること、更に分散剤を用いなくても高い顔料分散性が維持できる油性分散体が得られることを見出し、本発明を完成させるに至った。 As a result of intensive research conducted by the inventors to achieve the above object, they discovered that an oil-based dispersion with high powder dispersibility can be obtained by heating an ester oil of a fatty acid having 8 to 22 carbon atoms at a temperature of 70°C to 120°C while adding an inorganic oxide powder, and further, that an oil-based dispersion capable of maintaining high pigment dispersibility can be obtained without using a dispersant, thus completing the present invention.
　本発明の一形態にかかる油性分散体の製造方法は、炭素数８～２２の脂肪酸のエステル油を７０℃～１２０℃の温度で加熱しながら、無機酸化物粉体をエステル油に徐々に添加する工程（１）と前記無機酸化物粉体を全量加えた分散物を７０℃～１２０℃の温度で更に混合する工程（２）とを包含することを特徴とするものである。 The method for producing an oil-based dispersion according to one embodiment of the present invention is characterized by including a step (1) of gradually adding inorganic oxide powder to an ester oil of an ester oil of a fatty acid having 8 to 22 carbon atoms while heating the ester oil at a temperature of 70°C to 120°C, and a step (2) of further mixing the dispersion to which the entire amount of inorganic oxide powder has been added at a temperature of 70°C to 120°C.
　本発明の油性分散体の製造方法は、上記製造方法の工程（２）において分散に混練混合機または湿式混合分散機を用いることが好ましい。 In the method for producing the oil dispersion of the present invention, it is preferable to use a kneading mixer or a wet mixer for dispersion in step (2) of the above production method.
　本発明の油性分散体の製造方法の一態様は、炭素数８～２２の脂肪酸のエステル油を７０℃～１２０℃の温度で加熱しながら、無機酸化物粉体を添加する工程（１）と前記無機酸化物粉体を全量加えた分散物を７０℃～１２０℃の温度で更に混合する工程（２）とを包含する製造方法の全工程後に、油性分散体を冷却し、更に湿式混合分散機を用いて分散する、油性分散体の製造方法である。 One embodiment of the method for producing an oil dispersion of the present invention is a method for producing an oil dispersion, which includes step (1) of adding inorganic oxide powder while heating ester oil of fatty acid having 8 to 22 carbon atoms at a temperature of 70°C to 120°C, and step (2) of further mixing the dispersion to which the entire amount of inorganic oxide powder has been added at a temperature of 70°C to 120°C, and then cooling the oil dispersion and further dispersing it using a wet mixer/disperser.
　本発明の油性分散体の製造方法は、上記製造方法の工程（２）の後に、好ましくは室温（２０℃～３０℃）まで冷却し、更に追加で湿式混合分散機を用いて分散させて製造することが好ましい。 In the method for producing the oil-based dispersion of the present invention, after step (2) of the above production method, it is preferable to cool the mixture to room temperature (20°C to 30°C) and further disperse the mixture using a wet mixer.
　上記態様において、油性分散体製造時における前記無機酸化物粉体の固形分濃度が２５質量％以上であることが好ましい。 In the above embodiment, it is preferable that the solids concentration of the inorganic oxide powder during production of the oil dispersion is 25% by mass or more.
　更に、本発明の化粧料は、本発明の製造方法で製造された油性分散体を配合したことを特徴とする化粧料である。 Furthermore, the cosmetic of the present invention is characterized by containing an oil dispersion produced by the production method of the present invention.
　次に、本発明による油性分散体の製造方法と、この製造方法によって製造される油性分散体を含有する化粧料の具体的な実施の形態について説明する。なお、本明細書において、範囲を示す「Ｘ～Ｙ」は「Ｘ以上、Ｙ以下」を意味する。また、特記しない限り、操作は室温（２０℃～３０℃）／相対湿度４５～５５％ＲＨの条件下で行う。さらに全ての実施形態の組み合わせが本願では開示されていると理解されなければならない。 Next, we will explain the method for producing an oil dispersion according to the present invention and specific embodiments of a cosmetic containing an oil dispersion produced by this production method. In this specification, the range "X to Y" means "X or more, Y or less." Furthermore, unless otherwise specified, operations are carried out under conditions of room temperature (20°C to 30°C) and relative humidity of 45 to 55% RH. Furthermore, it should be understood that all combinations of embodiments are disclosed in this application.
　本発明の油性分散体の製造方法は、炭素数８～２２の脂肪酸のエステル油を７０℃～１２０℃の温度で加熱しながら、無機酸化物粉体をエステル油に添加する工程（１）と前記無機酸化物粉体を全量加えた分散物を７０℃～１２０℃の温度で更に混合する工程（２）とを包含することを特徴とするものである。 The method for producing an oil-based dispersion of the present invention is characterized by including a step (1) of adding inorganic oxide powder to an ester oil of an ester oil of a fatty acid having 8 to 22 carbon atoms while heating the ester oil at a temperature of 70°C to 120°C, and a step (2) of further mixing the dispersion to which the entire amount of inorganic oxide powder has been added at a temperature of 70°C to 120°C.
　本発明によれば、炭素数８～２２の脂肪酸のエステル油に、７０℃～１２０℃の温度で加熱しながら、無機酸化物粉体を徐々に添加することで高い顔料分散性を有する油性分散体、更に分散剤を用いなくても高い粉体分散性が維持できる油性分散体が得られ、さらにそれを含有する化粧料を得ることができる。 According to the present invention, by gradually adding inorganic oxide powder to an ester oil of a fatty acid having 8 to 22 carbon atoms while heating it at a temperature of 70°C to 120°C, it is possible to obtain an oil dispersion with high pigment dispersibility, an oil dispersion that can maintain high powder dispersibility even without the use of a dispersant, and a cosmetic product containing the same.
　分散媒体として使用される炭素数８～２２の脂肪酸のエステル油（以下、単にエステル油とも称する）は、脂肪酸由来の部分の炭素数が８～２２であるエステル油である。ジエステルやトリエステルなど、脂肪酸由来の部分が複数存在する場合には、少なくとも一の脂肪酸の炭素数が８～２２であることを指し、好ましくはすべての脂肪酸の炭素数が８～２２である。例えば、トリ（カプリル／カプリン酸）グリセリルは、カプリル酸（Ｃ８）／カプリン酸（Ｃ１０）と、グリセリンとのエステルであるので、脂肪酸部分の炭素数８および炭素数１０となる。炭素数８～２２の脂肪酸のエステル油は、不揮発性でかつ２５℃で液状又はペースト状の、流動性を有するものが好ましい。ここで、不揮発性とは、２５℃で揮発しないことであるが、例えば常圧での沸点が２５０℃を超える成分である。炭素数８未満の脂肪酸のエステル油では、無機酸化物粉体の分散性が良好な油性分散体が得られないため好ましくない。また、上記エステル油以外の炭化水素油やシリコーン油でも無機酸化物粉体の分散性が良好な油性分散体が得られない。また、炭素数８～２２の脂肪酸のエステル油は、炭素数８～１８の脂肪酸のエステルであることがより好ましい。また、脂肪酸は飽和脂肪酸であっても不飽和脂肪酸であってもよいが、飽和脂肪酸であることが好ましく、また飽和脂肪酸は直鎖であっても分岐鎖であってもよい。 The ester oil of fatty acids having 8 to 22 carbon atoms (hereinafter, simply referred to as ester oil) used as a dispersion medium is an ester oil in which the carbon number of the fatty acid-derived portion is 8 to 22. In the case where there are multiple fatty acid-derived portions, such as diesters and triesters, at least one of the fatty acids has a carbon number of 8 to 22, and preferably all of the fatty acids have a carbon number of 8 to 22. For example, tri(caprylic/capric)glyceryl is an ester of caprylic acid (C8)/capric acid (C10) and glycerin, so the fatty acid portion has 8 carbon atoms and 10 carbon atoms. It is preferable that the ester oil of fatty acids having 8 to 22 carbon atoms is non-volatile and has fluidity such as liquid or paste at 25°C. Here, non-volatile means that it does not volatilize at 25°C, but for example, it is a component whose boiling point at normal pressure exceeds 250°C. Ester oil of fatty acids having less than 8 carbon atoms is not preferable because it is not possible to obtain an oil-based dispersion with good dispersibility of inorganic oxide powder. Furthermore, if a hydrocarbon oil or silicone oil other than the above ester oil is used, an oil-based dispersion with good dispersibility of the inorganic oxide powder cannot be obtained. Furthermore, it is more preferable that the ester oil of a fatty acid having 8 to 22 carbon atoms is an ester of a fatty acid having 8 to 18 carbon atoms. Furthermore, the fatty acid may be a saturated fatty acid or an unsaturated fatty acid, but it is preferable that it is a saturated fatty acid, and the saturated fatty acid may be a straight chain or a branched chain.
　かかるエステル油としては、例えば、イソノナン酸イソノニル、イソノナン酸イソデシル、イソノナン酸イソトリデシル、イソノナン酸トリシクロデカンメチル、（カプリル酸／カプリン酸）ヤシアルキル、ラウリン酸ヘキシル、ラウリン酸メチルヘプチル、ラウリン酸カプリリル、ラウリン酸デシル、ミリスチン酸イソプロピル、ミリスチン酸メチルヘプチル、ミリスチン酸２－ヘキシルデシル、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、パルミチン酸メチルヘプチル、パルミチン酸２－エチルヘキシル、ステアリン酸２－エチルヘキシル、イソステアリン酸エチル、イソステアリン酸イソプロピル、イソステアリン酸イソブチル、イソステアリン酸デシル、イソステアリン酸メチルヘプチル、イソステアリン酸２－ヘキシルデシル、ヒドロキシステアリン酸２－エチルヘキシル、オレイン酸オクチルドデシル、オレイン酸オレイル、リシノレイン酸オクチルドデシル、パラメトキシケイ皮酸オクチル、安息香酸アルキル、イソステアリン酸グリセリル等のモノエステル油；ジ（カプリル酸／カプリン酸）プロパンジオール、ジイソノナン酸ネオペンチルグリコール、ジカプリン酸ネオペンチルグリコール、ジイソステアリン酸グリセリル、ジイソステアリン酸ポリグリセリル、ジイソステアリン酸プロパンジオール、ラウロイルグルタミン酸ジ（フィトステリル／オクチルドデシル）、ラウロイルグルタミン酸ジ（コレステリル／ベヘニル／オクチルドデシル）、ラウロイルグルタミン酸ジ（オクチルドデシル／フィトステリル／ベヘニル）、ジオクタン酸ネオペンチルグリコール等のジエステル油；トリイソステアリン酸トリメチロールプロパン、トリイソステアリン酸ジグリセリル、トリイソステアリン酸ジグリセリル、トリ（カプリル／カプリン酸）グリセリル、トリオクタン酸グリセリル、マカデミアナッツ油、オリーブ油、ヒマシ油、ホホバ油、アボガド油、ヒマワリ油等のトリエステル油；テトラオクタン酸ペンタエリスリチル、テトライソステアリン酸ジグリセリル、テトライソステアリン酸ジペンタエリスリチル、テトライソステアリン酸ペンタエリトリット等が挙げられる。 Such ester oils include, for example, isononyl isononanoate, isodecyl isononanoate, isotridecyl isononanoate, tricyclodecane methyl isononanoate, (caprylic acid/capric acid) coconut alkyl, hexyl laurate, methylheptyl laurate, caprylyl laurate, decyl laurate, isopropyl myristate, methylheptyl myristate, 2-hexyldecyl myristate, octyldodecyl myristate, isopropyl palmitate, methylheptyl palmitate, palmitic acid, methylheptyl palmitate ... monoester oils such as 2-ethylhexyl ester, 2-ethylhexyl stearate, ethyl isostearate, isopropyl isostearate, isobutyl isostearate, decyl isostearate, methylheptyl isostearate, 2-hexyldecyl isostearate, 2-ethylhexyl hydroxystearate, octyldodecyl oleate, oleyl oleate, octyldodecyl ricinoleate, octyl p-methoxycinnamate, alkyl benzoate, and glyceryl isostearate; diisostearate, polyglyceryl diisostearate, propanediol diisostearate, di(phytosteryl/octyldodecyl) lauroyl glutamate, di(cholesteryl/behenyl/octyldodecyl) lauroyl glutamate, di(octyldodecyl/phytosteryl/behenyl) lauroyl glutamate, di(octyldodecyl/phytosteryl/behenyl) dioctanoate, neopentyl glycol dioctanoate, etc. Triester oils such as trimethylolpropane triisostearate, diglyceryl triisostearate, diglyceryl triisostearate, tri(caprylic/capric)glyceryl, glyceryl trioctanoate, macadamia nut oil, olive oil, castor oil, jojoba oil, avocado oil, and sunflower oil; pentaerythrityl tetraoctanoate, diglyceryl tetraisostearate, dipentaerythrityl tetraisostearate, and pentaerythritol tetraisostearate.
　これらのうち、低粘度で使用感が良く、また本発明の効果の点から、エステル油としては、（カプリル酸／カプリン酸）ヤシアルキル、ミリスチン酸イソプロピル、パルミチン酸２－エチルヘキシル、ステアリン酸２－エチルヘキシル、イソステアリン酸デシル、イソステアリン酸メチルヘプチル、トリイソステアリン酸ジグリセリル、トリ（カプリル／カプリン酸）グリセリル、ホホバ油、テトライソステアリン酸ジグリセリル、およびテトライソステアリン酸ジペンタエリスリチルからなる群から選択される少なくとも１種であることが好ましい。また、保存安定性の観点から、脂肪酸のエステル油が、トリ（カプリル／カプリン酸）グリセリルを含むことが好ましい。 Among these, in terms of low viscosity, good usability, and the effects of the present invention, it is preferable that the ester oil is at least one selected from the group consisting of coconut alkyl (caprylic/capric acid), isopropyl myristate, 2-ethylhexyl palmitate, 2-ethylhexyl stearate, decyl isostearate, methylheptyl isostearate, diglyceryl triisostearate, tri(caprylic/capric acid)glyceryl, jojoba oil, diglyceryl tetraisostearate, and dipentaerythrityl tetraisostearate. Also, in terms of storage stability, it is preferable that the fatty acid ester oil contains tri(caprylic/capric acid)glyceryl.
　本発明において、無機酸化物粉体は、一般的に化粧品に用いられる無水ケイ酸（ケイ素酸化物）、酸化アルミニウム、酸化鉄（赤酸化鉄、黄酸化鉄、黒酸化鉄など）、酸化チタン、酸化亜鉛、酸化セリウム、酸化ビスマスなどの無機酸化物が挙げられ、特に紫外線遮蔽効果を目的とした場合は、微粒子の酸化チタン、酸化亜鉛、酸化セリウム、酸化ビスマスなどの無機酸化物及びこれらの複合体などが挙げられる。中でも、無機酸化物粉体は、酸化チタンおよび／または酸化鉄であることが好ましい。好適な一態様として、無機酸化物は、脂肪酸処理されていない無機酸化物粉体である。また、他の好適な一態様は、無機酸化物粉体が疎水化処理されていない。ここで、疎水化処理とは、シリコーン処理、脂肪酸処理など公知の疎水化表面処理剤で処理することを指す。このように疎水化処理されていない無機酸化物を用いることで、経時でも分散性が維持される。また、無機酸化物粉体は、未処理粉体であることが好ましい。未処理粉体とは表面処理剤により表面処理されていない粉体を指す。 In the present invention, examples of inorganic oxide powder include inorganic oxides such as silicic anhydride (silicon oxide), aluminum oxide, iron oxide (red iron oxide, yellow iron oxide, black iron oxide, etc.), titanium oxide, zinc oxide, cerium oxide, and bismuth oxide that are generally used in cosmetics. In particular, when the objective is to achieve an ultraviolet ray shielding effect, examples of inorganic oxides include fine particles of titanium oxide, zinc oxide, cerium oxide, bismuth oxide, and composites thereof. Among these, the inorganic oxide powder is preferably titanium oxide and/or iron oxide. In one preferred embodiment, the inorganic oxide is an inorganic oxide powder that has not been treated with a fatty acid. In another preferred embodiment, the inorganic oxide powder has not been hydrophobized. Here, hydrophobization refers to treatment with a known hydrophobizing surface treatment agent such as silicone treatment or fatty acid treatment. By using an inorganic oxide that has not been hydrophobized in this way, dispersibility is maintained over time. In addition, it is preferable that the inorganic oxide powder is an untreated powder. An untreated powder refers to a powder that has not been surface-treated with a surface treatment agent.
　無機酸化物の粒子径は、例えば、０．００１～５０μｍであり、０．０１～３０μｍであってもよい。粒子径は、体積基準であり、レーザー回折式粒度分布計を用いて測定することができる。 The particle size of the inorganic oxide is, for example, 0.001 to 50 μm, and may be 0.01 to 30 μm. The particle size is based on volume and can be measured using a laser diffraction particle size distribution analyzer.
　油性分散体の無機酸化物粉体の固形分濃度は、２５質量％以上であることが好ましく、２５～８０質量％であることがより好ましく、３０～８０質量％であることがさらにより好ましく、さらに４０～８０質量％であることがより好ましく、４０～７０質量％であることが特に好ましい。無機酸化物粉体の固形分濃度が２５質量％以上であると経時における無機酸化物粉体の分散性が良好となり、８０質量％以下であることで粉体の凝集が抑制されやすくなる。 The solids concentration of the inorganic oxide powder in the oil dispersion is preferably 25% by mass or more, more preferably 25 to 80% by mass, even more preferably 30 to 80% by mass, even more preferably 40 to 80% by mass, and particularly preferably 40 to 70% by mass. If the solids concentration of the inorganic oxide powder is 25% by mass or more, the dispersibility of the inorganic oxide powder over time will be good, and if it is 80% by mass or less, the aggregation of the powder will be easily suppressed.
　本発明の油性分散体の製造方法は、下記工程（１）及び工程（２）の順に実施する製造方法である。 The method for producing the oil dispersion of the present invention is a production method that is carried out in the following order: step (1) and step (2).
　工程（１）；
　工程（１）では、炭素数８～２２の脂肪酸のエステル油を７０℃～１２０℃の温度で加熱しながら、エステル油に無機酸化物粉体を添加し、目的の投入量をすべて添加する。また、エステル油には無機酸化物粉体を徐々に添加することが好ましい。 Step (1);
In step (1), the inorganic oxide powder is added to the ester oil of an ester oil of a fatty acid having 8 to 22 carbon atoms while heating the ester oil at a temperature of 70° C. to 120° C., until the entire target amount is added. It is also preferable to gradually add the inorganic oxide powder to the ester oil.
　エステル油の温度としては、本発明の効果の点から、７０℃～１００℃であることが好ましい。当該エステル油の温度は、無機酸化物粉体を添加している間、上記温度範囲内で維持されることが好ましい。上記温度範囲内で温度が維持されるように、適宜加熱手段を用いて加熱することが好ましい。 In terms of the effects of the present invention, the temperature of the ester oil is preferably 70°C to 100°C. The temperature of the ester oil is preferably maintained within the above temperature range while the inorganic oxide powder is being added. It is preferable to heat the ester oil using an appropriate heating means so that the temperature is maintained within the above temperature range.
　無機酸化物粉体のエステル油への添加時間は、例えば、１分～１００分である。 The time for adding the inorganic oxide powder to the ester oil is, for example, 1 to 100 minutes.
　工程（１）において油分散物を得る分散方法としては、ホモミキサーまたはディスパーなどの撹拌機を用いてエステル油を撹拌しながら無機酸化物粉体を投入する方法が挙げられる。攪拌の際の回転数としては、分散が良好に進めば特に限定されるものではないが、例えば、１０００ｒｐｍ～５０００ｒｐｍである。 In step (1), a dispersion method for obtaining an oil dispersion can be used in which the inorganic oxide powder is added while stirring the ester oil using a stirrer such as a homomixer or disperser. The rotation speed during stirring is not particularly limited as long as the dispersion proceeds well, but is, for example, 1000 rpm to 5000 rpm.
　また、エステル油と、無機酸化物粉体との混合質量比は、本発明の効果の観点から、エステル油：無機酸化物粉体＝７５：２５～２０：８０であることが好ましく、７０：３０～２０：８０であることがより好ましく、６０：４０～２０：８０であることがさらに好ましく、６０：４０～３０：７０であることが特に好ましい。 In addition, from the viewpoint of the effects of the present invention, the mixed mass ratio of ester oil to inorganic oxide powder is preferably ester oil:inorganic oxide powder = 75:25 to 20:80, more preferably 70:30 to 20:80, even more preferably 60:40 to 20:80, and particularly preferably 60:40 to 30:70.
　本発明の効果の点から、工程（１）においては、分散剤を使用しないほうが好ましい。ここで、分散剤としては下記に列挙したものが挙げられる。 In terms of the effectiveness of the present invention, it is preferable not to use a dispersant in step (1). Examples of dispersants include those listed below.
　工程（２）；
　前記工程（１）で得られた油分散物を、７０℃～１２０℃の温度で更に混合し、油性分散体を得る。工程（２）における分散時間は、無機酸化物粉体のエステル油への分散性の観点から２時間以上が好ましく、効果の飽和の観点から、２時間～１０時間であることがより好ましく、２～５時間であることがさらに好ましい。 Step (2);
The oil dispersion obtained in the step (1) is further mixed at a temperature of 70° C. to 120° C. to obtain an oil-based dispersion. The dispersion time in the step (2) is preferably 2 hours or more from the viewpoint of dispersibility of the inorganic oxide powder in the ester oil, and more preferably 2 hours to 10 hours, and even more preferably 2 hours to 5 hours, from the viewpoint of saturation of the effect.
　分散工程においても引き続きホモミキサー、ディスパーなどを用いて分散を行ってもよいが、より高い剪断力を加えることのできる、例えば、ニーダー混練、ヘンシェル混練、ロール混練、エクストルーダー混練等の混練混合機、プロペラミキサー、ハイスピードミキサー、ディゾルバー、アルテマイザー、湿式ジェットミル、コロイドミル、マスコロイダー、（湿式）ビーズミル、サンドミル、バスケットミル、ＡＤミル等の湿式混合分散機を用いるほうが好ましい。 In the dispersion step, dispersion may continue using a homomixer, disperser, etc., but it is preferable to use a kneading mixer capable of applying a higher shear force, such as a kneader mixer, Henschel mixer, roll mixer, or extruder mixer, or a wet mixer and disperser, such as a propeller mixer, high-speed mixer, dissolver, ultemizer, wet jet mill, colloid mill, mass colloider, (wet) bead mill, sand mill, basket mill, or AD mill.
　工程（２）においては、分散剤を使用してもよい。分散剤としては、例えば、ポリヒドロキシステアリン酸、ヒドロキシステアリン酸グリセリル、ジイソステアリン酸ポリグリセリル－２、トリイソステアリン酸ポリグリセリル－２、テトライソステアリン酸ポリグリセリル－２、トリエチルヘキサン酸エリスリチル、セスキイソステアリン酸ソルビタン等が挙げられ、これらを１種又は２種以上使用できる。これら分散剤のうちポリヒドロキシステアリン酸を使用することが最も好ましい。分散剤の使用量は、分散性の観点から、例えば、無機酸化物１００質量部に対して１質量部～１０質量部である。 In step (2), a dispersant may be used. Examples of dispersants include polyhydroxystearic acid, glyceryl hydroxystearate, polyglyceryl-2 diisostearate, polyglyceryl-2 triisostearate, polyglyceryl-2 tetraisostearate, erythrityl triethylhexanoate, and sorbitan sesquiisostearate. One or more of these may be used. Of these dispersants, it is most preferable to use polyhydroxystearic acid. From the viewpoint of dispersibility, the amount of dispersant used is, for example, 1 to 10 parts by mass per 100 parts by mass of the inorganic oxide.
　前記工程（１）及び（２）において製造時の温度条件はエステル油及び油分散物の温度が７０℃～１２０℃になるよう加熱するのが好ましい。７０℃未満では無機酸化物粉体がエステル油に均一に分散できず好ましくない。なお、温度が１２０℃を超えるとエステル油が分解したり、無機酸化物粉体の中で黄酸化鉄や黒酸化鉄は変色したりするので好ましくない。 In the above steps (1) and (2), the temperature conditions during production are preferably such that the ester oil and oil dispersion are heated to a temperature of 70°C to 120°C. Temperatures below 70°C are not preferred because the inorganic oxide powder cannot be uniformly dispersed in the ester oil. Temperatures above 120°C are also not preferred because the ester oil decomposes and the yellow iron oxide and black iron oxide in the inorganic oxide powder discolor.
　油分散物の混合温度としては、本発明の効果の点から、７０℃～１００℃であることが好ましい。混合の間上記温度範囲であることが好ましく、適宜加熱手段を用いて加熱しながら温度範囲を維持することが好ましい。 The mixing temperature of the oil dispersion is preferably 70°C to 100°C in terms of the effects of the present invention. It is preferable that the temperature is within the above range during mixing, and that the temperature range is maintained while heating using an appropriate heating means.
　前記工程（１）及び（２）の後に、油性分散体を冷却し更に分散工程を追加して行うと無機酸化物粉体が更に微粒子化され、油剤中により均一に分散した状態となるので好ましい。冷却は、４０℃以下となるまで行うことが好ましく、室温（２０℃～３０℃）まで冷却することが好ましい。冷却は、攪拌状態を継続して静置する方法；攪拌状態を継続したまま、冷却手段を用いて油性分散体を冷却する方法などが挙げられる。 After steps (1) and (2), it is preferable to cool the oil dispersion and then perform an additional dispersion step, since this will further atomize the inorganic oxide powder and make it more uniformly dispersed in the oil. Cooling is preferably performed until the temperature drops to 40°C or lower, and preferably to room temperature (20°C to 30°C). Examples of cooling methods include a method in which the mixture is left to stand while continuing to stir; and a method in which the mixture is cooled using a cooling means while continuing to stir.
　冷却後の分散の際に使用する分散機は油性分散体中の無機酸化物粉体の分散性を向上させるという観点から湿式混合分散機が好ましく、中でも湿式ビーズミルが好ましい。湿式混合分散機の具体例は上記のとおりである。冷却後の分散における分散時間は、例えば、１５分～５時間であり、３０分～３時間であってもよい。 The dispersing machine used for dispersion after cooling is preferably a wet mixer dispersing machine from the viewpoint of improving the dispersibility of the inorganic oxide powder in the oil dispersion, and among these, a wet bead mill is preferable. Specific examples of wet mixer dispersing machines are as described above. The dispersion time for dispersion after cooling is, for example, 15 minutes to 5 hours, and may be 30 minutes to 3 hours.
　本発明において油性分散体を化粧料に配合した際に、化粧料の保存安定性や化粧持続性に影響しない範囲で油性分散体の製造工程において分散剤を使用できる。前記分散剤としては、例えば、ポリヒドロキシステアリン酸、ヒドロキシステアリン酸グリセリル、ジイソステアリン酸ポリグリセリル－２、トリイソステアリン酸ポリグリセリル－２、テトライソステアリン酸ポリグリセリル－２、トリエチルヘキサン酸エリスリチル、セスキイソステアリン酸ソルビタン等が挙げられ、これらを１種又は２種以上使用できる。これら分散剤のうちポリヒドロキシステアリン酸を使用することが最も好ましい。 In the present invention, when the oil dispersion is blended with a cosmetic, a dispersant can be used in the manufacturing process of the oil dispersion to the extent that it does not affect the storage stability or cosmetic durability of the cosmetic. Examples of the dispersant include polyhydroxystearic acid, glyceryl hydroxystearate, polyglyceryl-2 diisostearate, polyglyceryl-2 triisostearate, polyglyceryl-2 tetraisostearate, erythrityl triethylhexanoate, sorbitan sesquiisostearate, etc., and one or more of these can be used. Of these dispersants, it is most preferable to use polyhydroxystearic acid.
　次に、本発明に係る化粧料について説明する。本発明の化粧料は、上述した製造方法によって調製された油性分散体を配合することによって、安全性の高いエステル油を使用していることから、他の化粧料成分との相性が良く、しかも高固形分濃度でありながら、経時安定性が良く、感触が良い化粧料となり、さらにはＳＰＦ値や透明性の高い日焼け止めなどの化粧料を作成することができる。化粧料の具体例としては、ファンデーション、アイシャドウ、チークなどのメイクアップ化粧料や、サンスクリーン化粧料、頭髪化粧料、乳液、クリームなどの基礎化粧品等に用いることができる。油性分散体の配合量は特に限定されないが、好ましくは化粧料中、０．１～９０質量％である。 Next, the cosmetic of the present invention will be described. The cosmetic of the present invention uses a highly safe ester oil by blending the oil dispersion prepared by the above-mentioned manufacturing method, and therefore has good compatibility with other cosmetic ingredients, and has good stability over time and a good feel despite its high solids concentration, and can also be used to create cosmetics such as sunscreens with high SPF values and transparency. Specific examples of cosmetics that can be used include makeup cosmetics such as foundations, eye shadows, and blushes, as well as basic cosmetics such as sunscreen cosmetics, hair cosmetics, emulsions, and creams. The amount of oil dispersion blended is not particularly limited, but is preferably 0.1 to 90% by mass in the cosmetic.
　さらに、本発明の化粧料には通常化粧料に用いられる成分、例えば、粉体、界面活性剤、油剤、ゲル化剤、高分子、美容成分、保湿剤、色素、防腐剤、香料等を本発明の効果を損なわない範囲で使用することができる。 Furthermore, the cosmetic of the present invention may contain ingredients that are normally used in cosmetics, such as powders, surfactants, oils, gelling agents, polymers, beauty ingredients, moisturizers, pigments, preservatives, fragrances, etc., to the extent that the effects of the present invention are not impaired.
　本発明の化粧料の形態としては、パウダー状、乳液状、クリーム状、スティック状、固型状、スプレー、多層分離型などいずれの剤型を用いても構わない。 The cosmetic composition of the present invention may be in any form, including powder, emulsion, cream, stick, solid, spray, and multi-layered separation.
　次に、本発明の製造方法によって製造された油性分散体と、この油性分散体を含有する化粧料の実施例および比較例に基づいて本発明をより具体的に説明するが、本発明は以下の実施例に限定されるものではない。 Next, the present invention will be explained in more detail based on examples and comparative examples of an oil dispersion produced by the production method of the present invention and a cosmetic composition containing this oil dispersion, but the present invention is not limited to the following examples.
　（実施例１）
　パルミチン酸２－エチルヘキシル４０ｇを９０℃に加熱した。温度が９０℃になったことを確認した後、ディスパー２０００ｒｐｍでパルミチン酸２－エチルヘキシルを撹拌しながら酸化チタン（粒子径０．２μｍ）６０ｇを１０分かけて少しずつ添加した。酸化チタンを全量投入した後、更に３時間、温度９０℃で、ディスパー２０００ｒｐｍで撹拌し、固形分濃度６０質量％の酸化チタンの油性分散体を得た。 Example 1
40 g of 2-ethylhexyl palmitate was heated to 90°C. After confirming that the temperature had reached 90°C, 60 g of titanium oxide (particle diameter: 0.2 µm) was gradually added over 10 minutes while stirring the 2-ethylhexyl palmitate with a disper at 2000 rpm. After the entire amount of titanium oxide was added, the mixture was further stirred at 90°C with a disper at 2000 rpm for 3 hours to obtain an oil-based dispersion of titanium oxide with a solid content concentration of 60% by mass.
　（実施例２）
　実施例１において酸化チタンの代わりに赤酸化鉄（粒子径０．５μｍ）を用いる他は同様にして固形分濃度６０質量％の赤酸化鉄の油性分散体を得た。 Example 2
An oil dispersion of red iron oxide having a solid content concentration of 60 mass % was obtained in the same manner as in Example 1, except that red iron oxide (particle diameter: 0.5 μm) was used instead of titanium oxide.
　（実施例３）
　実施例１において酸化チタンの代わりに黄酸化鉄（粒子径０．７μｍ）を用いる他は同様にして固形分濃度６０質量％の黄酸化鉄の油性分散体を得た。 Example 3
An oil dispersion of yellow iron oxide having a solid content concentration of 60 mass % was obtained in the same manner as in Example 1, except that yellow iron oxide (particle diameter: 0.7 μm) was used instead of titanium oxide.
　（実施例４）
　実施例１において酸化チタンの代わりに黒酸化鉄（粒子径０．２μｍ）を用いる他は同様にして固形分濃度６０質量％の黒酸化鉄の油性分散体を得た。 Example 4
An oil dispersion of black iron oxide having a solid content concentration of 60 mass % was obtained in the same manner as in Example 1, except that black iron oxide (particle diameter: 0.2 μm) was used instead of titanium oxide.
　（実施例５）
　実施例１で得られた油性分散体を室温（２５℃）まで攪拌を維持したまま静置して冷却し、更に湿式ビーズミル（シンマルエンタープライゼス社ＤＹＮＯ－ＭＩＬＬ）を用いて、周速１０ｍ／ｓ、φ０．５ｍｍのジルコニアビーズ、充填率７０％の条件で１時間分散混合して、固形分濃度６０質量％の酸化チタンの油性分散体を得た。 Example 5
The oil dispersion obtained in Example 1 was allowed to stand while continuing to stir and cooled to room temperature (25°C), and was then dispersed and mixed for 1 hour using a wet bead mill (DYNO-MILL, Shinmaru Enterprises) under conditions of a peripheral speed of 10 m/s, φ0.5 mm zirconia beads, and a packing rate of 70%, to obtain an oil dispersion of titanium oxide with a solid content concentration of 60 mass%.
　（実施例６）
　トリ（カプリル／カプリン酸）グリセリル４７ｇを９０℃に加熱する。温度が９０℃になったことを確認した後、ディスパー２０００ｒｐｍでトリ（カプリル／カプリン酸）グリセリルを撹拌しながら微粒子酸化チタン（ＭＴ－０５、テイカ社製）５０ｇを９分かけて少しずつ添加する。微粒子酸化チタンを全量投入し、更に分散剤としてポリヒドロキシステアリン酸（サラコス　ＨＳ－６Ｃ、日清オイリオグループ社製）を３ｇ添加した後、湿式ビーズミル（シンマルエンタープライゼス社ＤＹＮＯ－ＭＩＬＬ）を用いて、周速１０ｍ／ｓ、φ０．５ｍｍのジルコニアビーズ、充填率７０％、温度９０℃の条件で２時間分散し、微粒子酸化チタンの固形分濃度５０質量％の油性分散体を得た。 Example 6
47 g of tri(caprylic/capric)glyceryl is heated to 90°C. After confirming that the temperature has reached 90°C, 50 g of fine titanium dioxide particles (MT-05, manufactured by Teika Co., Ltd.) are gradually added over 9 minutes while stirring the tri(caprylic/capric)glyceryl with a disperser at 2000 rpm. The entire amount of fine titanium dioxide particles is charged, and 3 g of polyhydroxystearic acid (Salacos HS-6C, manufactured by Nisshin Oillio Group Co., Ltd.) is added as a dispersant. The mixture is then dispersed for 2 hours using a wet bead mill (DYNO-MILL, manufactured by Shinmaru Enterprises Co., Ltd.) under conditions of a peripheral speed of 10 m/s, φ0.5 mm zirconia beads, a filling rate of 70%, and a temperature of 90°C, to obtain an oil-based dispersion having a solid concentration of fine titanium dioxide particles of 50% by mass.
　（実施例７）
　実施例１においてパルミチン酸２－エチルヘキシルの代わりに（カプリル酸／カプリン酸）ヤシアルキルを用いる他は同様にして固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Example 7)
An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that coconut alkyl caprylate/caprate was used instead of 2-ethylhexyl palmitate.
　（実施例８）
　実施例１においてパルミチン酸２－エチルヘキシルの代わりにミリスチン酸イソプロピルを用いる他は同様にして固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Example 8)
An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that isopropyl myristate was used instead of 2-ethylhexyl palmitate.
　（実施例９）
　ステアリン酸２－エチルヘキシル６０ｇを８０℃に加熱した。温度が８０℃になったことを確認した後、ディスパー２０００ｒｐｍでステアリン酸２－エチルヘキシルを撹拌しながら微粒子酸化亜鉛（ＭＺ－５００、テイカ社製）４０ｇを８分かけて少しずつ添加した。酸化亜鉛を全量投入した後、更に３時間、温度８０℃で、ディスパー２０００ｒｐｍで撹拌し、固形分濃度４０質量％の微粒子酸化亜鉛の油性分散体を得た。 Example 9
60 g of 2-ethylhexyl stearate was heated to 80° C. After confirming that the temperature had reached 80° C., 40 g of zinc oxide fine particles (MZ-500, manufactured by Teica Corporation) was gradually added over 8 minutes while stirring the 2-ethylhexyl stearate with a disper at 2000 rpm. After the entire amount of zinc oxide was added, the mixture was further stirred at 80° C. and 2000 rpm with a disper for 3 hours to obtain an oil-based dispersion of zinc oxide fine particles having a solid content concentration of 40% by mass.
　（実施例１０）
　イソステアリン酸デシル５０ｇを７０℃に加熱した。温度が７０℃になったことを確認した後、ディスパー２０００ｒｐｍでイソステアリン酸デシルを撹拌しながら酸化チタン５０ｇを９分かけて少しずつ添加した。酸化チタンを全量投入した後、更に３時間、温度７０℃で、ディスパー２０００ｒｐｍで撹拌し、固形分濃度５０質量％の酸化チタンの油性分散体を得た。 (Example 10)
50 g of decyl isostearate was heated to 70° C. After confirming that the temperature had reached 70° C., 50 g of titanium oxide was gradually added over 9 minutes while stirring the decyl isostearate with a disper at 2000 rpm. After the entire amount of titanium oxide was added, the mixture was further stirred at 70° C. and 2000 rpm with a disper for 3 hours to obtain an oil dispersion of titanium oxide with a solid content concentration of 50% by mass.
　（実施例１１）
　イソステアリン酸メチルヘプチル３０ｇを１００℃に加熱した。温度が１００℃になったことを確認した後、ディスパー２０００ｒｐｍでイソステアリン酸メチルヘプチルを撹拌しながら酸化チタン７０ｇを１１分かけて少しずつ添加した。酸化チタンを全量投入した後、更に３時間、温度１００℃で、ディスパー２０００ｒｐｍで撹拌し、固形分濃度７０質量％の酸化チタンの油性分散体を得た。 (Example 11)
30 g of methylheptyl isostearate was heated to 100° C. After confirming that the temperature had reached 100° C., 70 g of titanium oxide was gradually added over 11 minutes while stirring the methylheptyl isostearate with a disper at 2000 rpm. After the entire amount of titanium oxide was added, the mixture was further stirred at 100° C. and 2000 rpm with a disper for 3 hours to obtain an oil dispersion of titanium oxide with a solid content concentration of 70% by mass.
　（実施例１２）
　実施例１０においてイソステアリン酸デシルの代わりにトリイソステアリン酸ジグリセリルを用いる他は同様にして固形分濃度５０質量％の酸化チタンの油性分散体を得た。 Example 12
An oil dispersion of titanium oxide having a solids concentration of 50 mass % was obtained in the same manner as in Example 10, except that diglyceryl triisostearate was used instead of decyl isostearate.
　（実施例１３）
　実施例１１においてイソステアリン酸メチルヘプチルの代わりにホホバ油を用いる他は同様にして固形分濃度７０質量％の酸化チタンの油性分散体を得た。 (Example 13)
An oil dispersion of titanium oxide having a solids concentration of 70 mass % was obtained in the same manner as in Example 11, except that jojoba oil was used instead of methylheptyl isostearate.
　（実施例１４）
　実施例１においてパルミチン酸２－エチルヘキシルの代わりにテトライソステアリン酸ジグリセリルを用いる他は同様にして固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Example 14)
An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that diglyceryl tetraisostearate was used instead of 2-ethylhexyl palmitate.
　（実施例１５）
　実施例１においてパルミチン酸２－エチルヘキシルの代わりにテトライソステアリン酸ジペンタエリスリチルを用いる他は同様にして固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Example 15)
An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that dipentaerythrityl tetraisostearate was used instead of 2-ethylhexyl palmitate.
　（実施例１６）
　パルミチン酸２－エチルヘキシル４０ｇを９０℃に加熱した。温度が９０℃になったことを確認した後、ディスパー２０００ｒｐｍでパルミチン酸２－エチルヘキシルを撹拌しながら酸化チタン（粒子径０．２μｍ）６０ｇを１０分かけて少しずつ添加した。酸化チタンを全量投入した後、湿式ビーズミル（シンマルエンタープライゼス社ＤＹＮＯ－ＭＩＬＬ）を用いて、周速１０ｍ／ｓ、φ０．５ｍｍのジルコニアビーズ、充填率７０％、温度９０℃の条件で２時間分散し、固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Example 16)
40 g of 2-ethylhexyl palmitate was heated to 90°C. After confirming that the temperature had reached 90°C, 60 g of titanium oxide (particle diameter: 0.2 μm) was gradually added over 10 minutes while stirring the 2-ethylhexyl palmitate with a disper at 2000 rpm. After the entire amount of titanium oxide was added, it was dispersed for 2 hours using a wet bead mill (DYNO-MILL, Shinmaru Enterprises) under conditions of a peripheral speed of 10 m/s, φ0.5 mm zirconia beads, a filling rate of 70%, and a temperature of 90°C, to obtain an oil-based dispersion of titanium oxide with a solid content concentration of 60% by mass.
　（実施例１７）
　パルミチン酸２－エチルヘキシル７０ｇを９０℃に加熱した。温度が９０℃になったことを確認した後、ディスパー２０００ｒｐｍでパルミチン酸２－エチルヘキシルを撹拌しながら酸化チタン３０ｇを５分かけて少しずつ添加した。酸化チタンを全量投入した後、更に３時間、温度９０℃で撹拌し、固形分濃度３０質量％の酸化チタンの油性分散体を得た。 (Example 17)
70 g of 2-ethylhexyl palmitate was heated to 90° C. After confirming that the temperature had reached 90° C., 30 g of titanium oxide was gradually added over 5 minutes while stirring the 2-ethylhexyl palmitate with a disper at 2000 rpm. After the entire amount of titanium oxide was added, the mixture was further stirred at a temperature of 90° C. for 3 hours to obtain an oil-based dispersion of titanium oxide with a solid content concentration of 30% by mass.
　（比較例１）
　パルミチン酸２－エチルヘキシル４０ｇを６０℃に加熱した。温度が６０℃になったことを確認した後、ディスパー２０００ｒｐｍでパルミチン酸２－エチルヘキシルを撹拌しながら酸化チタン６０ｇを１０分かけて少しずつ添加し、酸化チタンを全量投入して固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Comparative Example 1)
40 g of 2-ethylhexyl palmitate was heated to 60° C. After confirming that the temperature had reached 60° C., 60 g of titanium oxide was gradually added over 10 minutes while stirring the 2-ethylhexyl palmitate with a disper at 2000 rpm, and the entire amount of titanium oxide was added to obtain an oil dispersion of titanium oxide with a solid content concentration of 60 mass %.
　（比較例２）
　パルミチン酸２－エチルヘキシル４０ｇを９０℃に加熱した。温度が９０℃になったことを確認した後、ディスパー２０００ｒｐｍでパルミチン酸２－エチルヘキシルを撹拌しながらステアリン酸（酸化チタンに対して２質量％）で表面処理された疎水化処理酸化チタン６０ｇを１０分かけて少しずつ添加した。疎水化処理酸化チタンを全量投入した後、更に３時間、温度９０℃で撹拌し、固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Comparative Example 2)
40 g of 2-ethylhexyl palmitate was heated to 90° C. After confirming that the temperature had reached 90° C., 60 g of hydrophobized titanium oxide that had been surface-treated with stearic acid (2% by mass relative to titanium oxide) was gradually added over 10 minutes while stirring the 2-ethylhexyl palmitate with a disper at 2000 rpm. After the entire amount of hydrophobized titanium oxide was added, the mixture was further stirred at a temperature of 90° C. for 3 hours to obtain an oil-based dispersion of titanium oxide with a solid content concentration of 60% by mass.
　（比較例３）
　実施例１においてパルミチン酸２－エチルヘキシルの代わりにヘキサン酸ヘキシルを用いる他は同様にして固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Comparative Example 3)
An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that hexyl hexanoate was used instead of 2-ethylhexyl palmitate.
　（比較例４）
　実施例１においてパルミチン酸２－エチルヘキシルの代わりにスクワランを用いる他は同様にして固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Comparative Example 4)
An oil dispersion of titanium oxide having a solid content concentration of 60% by mass was obtained in the same manner as in Example 1, except that squalane was used instead of 2-ethylhexyl palmitate.
　（比較例５）
　実施例１においてパルミチン酸２－エチルヘキシルの代わりにジメチルポリシロキサン（６ｃｓ）を用いる他は同様にして固形分濃度６０質量％の酸化チタンの油性分散体を得た。 (Comparative Example 5)
An oil dispersion of titanium oxide having a solids concentration of 60% by mass was obtained in the same manner as in Example 1, except that dimethylpolysiloxane (6cs) was used instead of 2-ethylhexyl palmitate.
　次に、分散安定性の評価法について説明する。 Next, we will explain how to evaluate dispersion stability.
　試料作製後１日経過した試料及び４０℃で１ヶ月保存した試料の再分散性（粒子が沈降している場合は、良く振とうする）を目視で観察した。 The redispersibility of samples was visually observed one day after preparation and samples stored at 40°C for one month (if particles have settled, shake well).
　１日後の評価基準
○：分散粒子は均一で、凝集を認めなかった。
△：分散粒子はほぼ均一であるが、わずかな凝集を認めた。
×：分散粒子が均一でなく、著しい凝集を認めた。 Evaluation criteria after one day: ◯: Dispersed particles were uniform, and no aggregation was observed.
Δ: The dispersed particles are almost uniform, but slight aggregation is observed.
×: Dispersed particles were not uniform and significant aggregation was observed.
　１ヶ月保存後の評価基準
○：分散粒子は均一で、凝集を認めなかった。
△：分散粒子はほぼ均一であるが、わずかな凝集を認めた。
×：粒子が再分散せず、沈降若しくは著しい凝集を認めた。 Evaluation criteria after storage for one month: ◯: Dispersed particles were uniform, and no aggregation was observed.
Δ: The dispersed particles are almost uniform, but slight aggregation is observed.
×: The particles were not redispersed, and sedimentation or significant aggregation was observed.
　実施例１～１５及び比較例１～６を上記評価法で評価した結果を表１に記載する。 The results of evaluating Examples 1 to 15 and Comparative Examples 1 to 6 using the above evaluation methods are shown in Table 1.
　本発明品である実施例１～１５は製造１日後及び４０℃、１ヶ月保存後の分散性が良好なものであった。また、本発明品は、比較例１～６に比べて分散性、特に経時の分散性に優れていることがわかった。また、予め脂肪酸で表面処理した無機酸化物粉体を用いる場合より経時の分散性においても本発明品の油性分散体は優れていることもわかった。 The products of the present invention, Examples 1 to 15, had good dispersibility one day after production and after storage at 40°C for one month. It was also found that the products of the present invention have superior dispersibility, especially dispersibility over time, compared to Comparative Examples 1 to 6. It was also found that the oil dispersions of the products of the present invention have superior dispersibility over time compared to the case of using inorganic oxide powder that has been surface-treated in advance with a fatty acid.
　（実施例１８：油性ファンデーション）
　表２に記載した配合組成を、ホモミキサーで分散混合して油性ファンデーションを得た。実施例１８の分散安定性は良好であった（経時においても紛体の凝集や沈降が生じなかった）。 (Example 18: Oil-based foundation)
An oil-based foundation was obtained by dispersing and mixing the blended composition shown in Table 2 with a homomixer. The dispersion stability of Example 18 was good (no powder aggregation or settling occurred over time).

 
 
　（実施例１９：日焼け止めクリーム）
　表３に記載した配合組成を、下記製法で日焼け止めクリームを得た。実施例１９の分散安定性は良好であった。 Example 19: Sunscreen cream
A sunscreen cream was obtained using the formulation shown in Table 3 and the method described below. The dispersion stability of Example 19 was good.
　（製法）
　成分（１）～（４）を混合する。これにあらかじめ混合溶解しておいた成分（５）～（８）の水溶液をホモミキサーで撹拌しながら添加して目的の油中水型の日焼け止めクリームを得た。 (Production method)
Components (1) to (4) were mixed together, and an aqueous solution of components (5) to (8) that had been mixed and dissolved in advance was added to the mixture while stirring with a homomixer to obtain the desired water-in-oil sunscreen cream.
　実施例１８及び実施例１９は顔料の分散安定性が良好な化粧料であった（経時においても紛体の凝集や沈降が生じなかった）。 Examples 18 and 19 were cosmetics with good pigment dispersion stability (no powder aggregation or settling occurred over time).
　本発明の製造方法で製造された油性分散体は、凝集しやすい無機酸化物粉体が油剤への分散性が高いという特徴を有するものである。また、この油性分散体は、分散安定性の良好な化粧料を提供することができ、産業上の利用可能性が大である。 The oil dispersion produced by the manufacturing method of the present invention is characterized in that inorganic oxide powder, which tends to aggregate, is highly dispersible in oil agents. Furthermore, this oil dispersion can provide cosmetics with good dispersion stability, and has great industrial applicability.
　本発明は以下の態様を包含する。 The present invention includes the following aspects:
　（１）無機酸化物粉体と炭素数８～２２の脂肪酸のエステル油とを含有する油性分散体を製造する方法であって、
　前記エステル油を７０℃～１２０℃の温度で加熱しながら、無機酸化物粉体を前記エステル油に添加する工程（１）と、
　前記無機酸化物粉体を全量加えた分散物を７０℃～１２０℃の温度で更に混合する工程（２）と、を有する、油性分散体の製造方法。 (1) A method for producing an oil dispersion containing an inorganic oxide powder and an ester oil of a fatty acid having 8 to 22 carbon atoms, comprising the steps of:
(1) adding an inorganic oxide powder to the ester oil while heating the ester oil at a temperature of 70° C. to 120° C.;
and (2) further mixing the dispersion to which the entire amount of the inorganic oxide powder has been added at a temperature of 70°C to 120°C.
　（２）油性分散体における前記無機酸化物粉体の固形分濃度が２５質量％以上である、上記（１）に記載の油性分散体の製造方法。 (2) The method for producing an oil dispersion described in (1) above, in which the solids concentration of the inorganic oxide powder in the oil dispersion is 25% by mass or more.
　（３）前記工程（２）において混合に混練混合機または湿式混合分散機を使用する、上記（１）または（２）に記載の油性分散体の製造方法。 (3) A method for producing an oil-based dispersion according to (1) or (2) above, in which a kneading mixer or a wet mixer/disperser is used for mixing in step (2).
　（４）前記工程（２）の後に、油性分散体を冷却し、更に湿式混合分散機を用いて分散する、上記（１）～（３）のいずれか一に記載の油性分散体の製造方法。 (4) A method for producing an oil dispersion according to any one of (1) to (3) above, in which after step (2), the oil dispersion is cooled and further dispersed using a wet mixer/disperser.
　（５）上記（３）記載の製造方法の全工程後に、油性分散体を冷却し、更に湿式混合分散機を用いて分散する、油性分散体の製造方法。 (5) A method for producing an oil-based dispersion, in which after all steps of the production method described in (3) above, the oil-based dispersion is cooled and further dispersed using a wet mixer disperser.
　（６）油性分散体が、無機酸化物粉体と炭素数８～２２の脂肪酸のエステル油との二成分のみからなる油性分散体である、上記（１）～（５）のいずれか一に記載の油性分散体の製造方法。 (6) A method for producing an oil dispersion according to any one of (1) to (5) above, in which the oil dispersion is an oil dispersion consisting of only two components: inorganic oxide powder and an ester oil of a fatty acid having 8 to 22 carbon atoms.
　（７）前記無機酸化物粉体が疎水化処理されていない、上記（１）～（６）のいずれか一に記載の油性分散体の製造方法。 (7) The method for producing an oil-based dispersion according to any one of (1) to (6) above, wherein the inorganic oxide powder has not been subjected to a hydrophobic treatment.
　（８）上記（１）～（７）のいずれか一に記載の製造方法で製造した油性分散体を配合した化粧料。 (8) A cosmetic preparation containing an oil-based dispersion produced by the method described in any one of (1) to (7) above.
　本出願は、２０２２年１１月２日に出願された日本特許出願番号２０２２－１７６４２６号に基づいており、その開示内容は、参照され、全体として、組み入れられている。 This application is based on Japanese Patent Application No. 2022-176426, filed on November 2, 2022, the disclosure of which is hereby incorporated by reference in its entirety.

Claims (14)

  1. 　無機酸化物粉体と炭素数８～２２の脂肪酸のエステル油とを含有する油性分散体を製造する方法であって、
    　前記エステル油を７０℃～１２０℃の温度で加熱しながら、無機酸化物粉体を前記エステル油に添加する工程（１）と、
    　前記無機酸化物粉体を全量加えた分散物を７０℃～１２０℃の温度で更に混合する工程（２）と、を有する、油性分散体の製造方法。     A method for producing an oil dispersion containing an inorganic oxide powder and an ester oil of a fatty acid having 8 to 22 carbon atoms, comprising the steps of:
    (1) adding an inorganic oxide powder to the ester oil while heating the ester oil at a temperature of 70° C. to 120° C.;
    and (2) further mixing the dispersion to which the entire amount of the inorganic oxide powder has been added at a temperature of 70°C to 120°C.
  2. 　油性分散体における前記無機酸化物粉体の固形分濃度が２５質量％以上である、請求項１に記載の油性分散体の製造方法。 The method for producing an oil-based dispersion according to claim 1, wherein the solids concentration of the inorganic oxide powder in the oil-based dispersion is 25% by mass or more.
  3. 　前記工程（２）において混合に混練混合機または湿式混合分散機を使用する、請求項１または２に記載の油性分散体の製造方法。 The method for producing an oil-based dispersion according to claim 1 or 2, wherein a kneading mixer or a wet mixer/disperser is used for mixing in step (2).
  4. 　前記工程（２）の後に、油性分散体を冷却し、更に湿式混合分散機を用いて分散する、請求項１または２に記載の油性分散体の製造方法。 The method for producing an oil dispersion according to claim 1 or 2, wherein after step (2), the oil dispersion is cooled and further dispersed using a wet mixer/disperser.
  5. 　請求項３記載の製造方法の全工程後に、油性分散体を冷却し、更に湿式混合分散機を用いて分散する、請求項３に記載の油性分散体の製造方法。 The method for producing the oil dispersion according to claim 3, wherein the oil dispersion is cooled after all steps of the method for producing the oil dispersion according to claim 3, and is further dispersed using a wet mixer/disperser.
  6. 　油性分散体が、無機酸化物粉体と炭素数８～２２の脂肪酸のエステル油との二成分のみからなる油性分散体である、請求項１または請求項２に記載の油性分散体の製造方法。 The method for producing an oil dispersion according to claim 1 or 2, wherein the oil dispersion is an oil dispersion consisting of only two components: inorganic oxide powder and an ester oil of a fatty acid having 8 to 22 carbon atoms.
  7. 　油性分散体が、無機酸化物粉体と炭素数８～２２の脂肪酸のエステル油との二成分のみからなる油性分散体である、請求項３に記載の油性分散体の製造方法。 The method for producing an oil dispersion according to claim 3, wherein the oil dispersion is an oil dispersion consisting of only two components: inorganic oxide powder and an ester oil of a fatty acid having 8 to 22 carbon atoms.
  8. 　油性分散体が、無機酸化物粉体と炭素数８～２２の脂肪酸のエステル油との二成分のみからなる油性分散体である、請求項４に記載の油性分散体の製造方法。 The method for producing an oil dispersion according to claim 4, wherein the oil dispersion is an oil dispersion consisting of only two components: inorganic oxide powder and an ester oil of a fatty acid having 8 to 22 carbon atoms.
  9. 　油性分散体が、無機酸化物粉体と炭素数８～２２の脂肪酸のエステル油との二成分のみからなる油性分散体である、請求項５に記載の油性分散体の製造方法。 The method for producing an oil dispersion according to claim 5, wherein the oil dispersion is an oil dispersion consisting of only two components: inorganic oxide powder and an ester oil of a fatty acid having 8 to 22 carbon atoms.
  10. 　前記無機酸化物粉体が疎水化処理されていない、請求項１または２に記載の油性分散体の製造方法。 The method for producing an oil-based dispersion according to claim 1 or 2, wherein the inorganic oxide powder has not been subjected to a hydrophobic treatment.
  11. 　請求項１または請求項２に記載の製造方法で製造した油性分散体を配合した化粧料。 A cosmetic preparation containing an oil dispersion produced by the method described in claim 1 or claim 2.
  12. 　請求項３に記載の製造方法で製造した油性分散体を配合した化粧料。 A cosmetic containing an oil dispersion produced by the method described in claim 3.
  13. 　請求項４に記載の製造方法で製造した油性分散体を配合した化粧料。 A cosmetic preparation containing an oil dispersion produced by the method described in claim 4.
  14. 　請求項５に記載の製造方法で製造した油性分散体を配合した化粧料。 A cosmetic containing an oil dispersion produced by the method of claim 5.
PCT/JP2023/032178 2022-11-02 2023-09-04 Method for producing oily dispersion, and cosmetic material having said oily dispersion blended therein WO2024095598A1 (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS647941A (en) * 1987-05-30 1989-01-11 Tioxide Group Plc Oil dispersion and its production
WO2011007668A1 (en) * 2009-07-13 2011-01-20 テイカ株式会社 Oily dispersion and cosmetic material incorporating this oily dispersion
JP2013121940A (en) * 2011-11-10 2013-06-20 Taiyo Kagaku Co Ltd Oil-based dispersant and oil-based cosmetic
CN105331200A (en) * 2015-11-13 2016-02-17 上海联锴日用化工有限公司 High-pigment-content pure oil non-emulsification cosmetic color paste and preparation method
JP2018016576A (en) * 2016-07-27 2018-02-01 株式会社トキワ Solid powder cosmetic and method for producing solid powder cosmetic
CN108272648A (en) * 2018-03-26 2018-07-13 上海蔻沣生物科技有限公司 Cosmetics powder, oil pastes and preparation method thereof
WO2019225491A1 (en) * 2018-05-23 2019-11-28 株式会社コーセー Novel titanium oxide powder and cosmetic formulated therewith

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS647941A (en) * 1987-05-30 1989-01-11 Tioxide Group Plc Oil dispersion and its production
WO2011007668A1 (en) * 2009-07-13 2011-01-20 テイカ株式会社 Oily dispersion and cosmetic material incorporating this oily dispersion
JP2013121940A (en) * 2011-11-10 2013-06-20 Taiyo Kagaku Co Ltd Oil-based dispersant and oil-based cosmetic
CN105331200A (en) * 2015-11-13 2016-02-17 上海联锴日用化工有限公司 High-pigment-content pure oil non-emulsification cosmetic color paste and preparation method
JP2018016576A (en) * 2016-07-27 2018-02-01 株式会社トキワ Solid powder cosmetic and method for producing solid powder cosmetic
CN108272648A (en) * 2018-03-26 2018-07-13 上海蔻沣生物科技有限公司 Cosmetics powder, oil pastes and preparation method thereof
WO2019225491A1 (en) * 2018-05-23 2019-11-28 株式会社コーセー Novel titanium oxide powder and cosmetic formulated therewith

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