Oily particle dispersion composition and method for producing the same

Abstract

To provide a novel oil-based particle dispersion composition, and to provide a method for producing the same.SOLUTION: Provided is an oil-based particle dispersion composition characterized by containing (A) two or more solid oils, (B) an amphiphilic substance, and (C) water, the total amount of components (A) to (C) in the oil-based particle dispersion composition being 90 mass% or more, and component (B) being at least one selected from the group consisting of the following (B1) to (B4): (B1) a divalent carboxylic acid ester; (B2) an alkylene oxide derivative; (B3) at least one selected from the group consisting of a dihydric alcohol and a polyethylene glycol; and (B4) a nonionic surfactant having an HLB of 3.5 or more.SELECTED DRAWING: None

Description

Technical Field

[0001] The present invention relates to an oil-based particle dispersion composition and a method for producing the same.

Background Art

[0002] Conventionally, a composition containing oil-based particles has been known, and such a composition has been used in preparations such as cosmetics.

[0003] As a composition in which oil-based particles are dispersed in an aqueous phase, for example, Patent Document 1 reports a capsule-containing composition in which an oil-based component is dispersed in an aqueous solvent as oil-based capsules having an average particle diameter of 100 μm or more. The film of the oil-based capsules in the capsule-containing composition is composed of one or more components selected from the group consisting of higher alcohols having 16 or more carbon atoms and glycerin fatty acid ester eicosanedioic acid condensates, and the component necessarily contains behenyl alcohol and is contained in the capsule composition at 5 to 40% by mass, and it is essential that the aqueous solvent contains a water-soluble polymer. According to Patent Document 1, the capsule-containing composition does not cause a foreign body sensation even when applied to the skin, and since the average particle diameter of the capsule particles is as large as 100 μm and visible to the naked eye, it has an appearance that can be said to be an emulsion in which emulsion particles can be seen, and it has been reported that it is possible to make it visually novel and beautiful.

[0004] Thus, a composition in which oil-based particles prepared according to the purpose are dispersed has been conventionally reported.

Prior Art Documents

Patent Documents

[0005]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0006] The objective is to provide a novel oily particle dispersion composition and a method for producing the same. In particular, the objective is to provide a novel oily particle dispersion composition with dispersion stability in a simple manner. [Means for solving the problem]

[0007] As a result of diligent research, the inventors have found that a new oily particle dispersion composition with dispersion stability can be easily produced by combining (A) two or more solid oils, (B) an amphiphilic substance, and (C) water, such that the total amount of components (A) to (C) is 90% by mass or more of the composition, and by using at least one selected from the group consisting of (B1) to (B4) as component (B). Furthermore, they have found that compositions containing dispersed oily particles that easily disintegrate when force is applied, and compositions containing dispersed oily particles that do not easily disintegrate when force is applied and have a granular texture, can be easily obtained. The present invention was completed by further research based on the above findings, and this disclosure includes, for example, the inventions represented below. Item 1. Oily particle dispersion composition having the following characteristics: (A) Contains two or more solid oils, (B) an amphiphilic substance, and (C) water. In the oily particle dispersion composition, the total amount of components (A) to (C) is 90% by mass or more. Component (B) is at least one selected from the group consisting of (B1) to (B4) below. (B1) Divalent carboxylic acid ester, (B2) Alkylene oxide derivatives, (B3) At least one selected from the group consisting of dihydric alcohols and polyethylene glycols, (B4) Nonionic surfactant with an HLB of 3.5 or higher. Item 2. The oily particle dispersion composition according to Item 1, wherein the content of component (A) in the composition is 0.1 to 50% by mass. Item 3. The oily particle dispersion composition according to item 1 or 2, wherein the amount of component (B) is 0.02 to 90 parts by mass per 100 parts by mass of component (A). Item 4. An oily particle dispersion composition according to any one of items 1 to 3, wherein the total amount of component (A) and component (B) in the composition is 0.2 to 60% by mass. Item 5. Oily particles that are removed from the dispersion medium of an oily particle dispersion composition described in any one of items 1 to 4. Item 6. An oily particle formulation comprising an oily particle dispersion composition described in any one of items 1 to 4 or an oily particle described in item 5. Item 7. A method for producing an oily particle dispersion composition, comprising the following steps: Step (1) A step of mixing (A) two or more solid oils and (B) an amphiphilic substance to obtain a mixed liquid at a temperature above the melting point of component (A), and Step (2) A step of granulating oily particles by adding the mixture and water (C) at a temperature above the melting point of component (A), and stirring the resulting mixture to a temperature below the melting point of component (A). Here, the oily particle dispersion composition is It contains ingredients (A) to (C), In the composition, the total amount of components (A) to (C) is 90% by mass or more. Component (B) is at least one selected from the group consisting of (B1) to (B4) below. (B1) Divalent carboxylic acid ester, (B2) Alkylene oxide derivatives, (B3) At least one selected from the group consisting of dihydric alcohols and polyethylene glycols, (B4) Nonionic surfactant with an HLB of 3.5 or higher. [Effects of the Invention]

[0008] This disclosure provides novel oily particle dispersion compositions and methods for producing the same. In particular, this disclosure provides a simple way to provide novel oily particle dispersion compositions with dispersion stability. [Modes for carrying out the invention]

[0009] Hereinafter, embodiments included in the present disclosure will be described in more detail. In the present disclosure, "containing" also includes the meanings of "substantially consisting of" and "consisting of".

[0010] The present disclosure includes an oil-based particle dispersion composition having the following characteristics: containing (A) two or more solid oils, (B) an amphiphilic substance, and (C) water, in the oil-based particle dispersion composition, the total amount of components (A) to (C) is 90% by mass or more, component (B) is at least one selected from the group consisting of the following (B1) to (B4), (B1) a divalent carboxylic acid ester, (B2) an alkylene oxide derivative, (B3) at least one selected from the group consisting of a dihydric alcohol and polyethylene glycol, (B4) a nonionic surfactant having an HLB of 3.5 or more.

[0011] (A) Two or more types of solid oil The oil-based particle dispersion composition of the present disclosure contains two or more solid oils. The solid oil is not limited as long as it is solid at 25°C. Examples of such solid oils include higher alcohols, polyglycerol fatty acid esters, fatty acid glycerides, animal and plant waxes, hydrocarbon waxes, etc. Preferred examples of the solid oil include higher alcohols, polyglycerol fatty acid esters, fatty acid glycerides, animal and plant waxes.

[0012] Preferred examples of the melting point of the solid oil include a melting point of 55°C or higher, more preferably a melting point of 60 to 90°C, still more preferably a melting point of 65 to 85°C, and even more preferably 65 to 82°C.

[0013] Examples of the higher alcohol include higher alcohols having 12 to 22 carbon atoms such as behenyl alcohol, arachidyl alcohol, myristyl alcohol, cetanol, stearyl alcohol, arachidyl alcohol, etc. Preferred examples of the higher alcohol include behenyl alcohol and arachidyl alcohol.

[0014] In the present disclosure, the polyglyceryl fatty acid ester is a polyglyceryl fatty acid ester that is not usually used as a surfactant. As an example, octadeca (behenic acid / hydroxystearic acid) polyglyceryl-20, which is known as an oil thickener, polyglyceryl-6 octastearate, etc. are exemplified. Preferably, octadeca (behenic acid / hydroxystearic acid) polyglyceryl-20 is exemplified as the polyglyceryl fatty acid ester.

[0015] As an example of the fatty acid glyceride, fatty acid monoglyceride etc. are exemplified. Preferably, glyceryl stearate, glyceryl behenate, glyceryl (behenic acid / eicosandioic acid), glyceryl tri (behenic acid / isostearic acid / eicosandioic acid), glyceryl caprylate, glyceryl capric acid, glyceryl laurate, glyceryl myristate, etc. are exemplified as the fatty acid glyceride, and more preferably, glyceryl stearate, glyceryl behenate, glyceryl (behenic acid / eicosandioic acid) are exemplified.

[0016] As an example of the animal and plant waxes, sunflower seed wax, carnauba wax, rice bran wax, candelilla wax, beeswax, etc. are exemplified. Preferably, sunflower seed wax, carnauba wax, rice bran wax, candelilla wax are exemplified as the animal and plant waxes.

[0017] As an example of the hydrocarbon waxes, polyethylene wax, paraffin wax, ceresin, microcrystalline wax, etc. are exemplified.

[0018] Although not limiting the present disclosure, as the solid oil, preferably, glyceryl (behenic acid / eicosandioic acid), behenyl alcohol, glyceryl tri (behenic acid / isostearic acid / eicosandioic acid), octadeca (behenic acid / hydroxystearic acid) polyglyceryl-20, rice bran wax, carnauba wax, sunflower seed wax, candelilla wax, beeswax, glyceryl stearate, glyceryl behenate, etc. are exemplified.

[0019] Solid oils are commercially available, for example, (behenate / eicosanedioic acid) glyceryl under the trade name NOMUCOAT HK-G (manufactured by Nisshin Oillio Group, melting point 65°C), tri(behenate / isostearate / eicosanedioic acid) glyceryl under the trade name NOMUCOAT SG (manufactured by Nisshin Oillio Group, melting point 40-65°C), behenyl alcohol under the trade name Behenyl Alcohol 65 (manufactured by Higher Alcohol Industry Co., Ltd., melting point 65-73°C), and octadeca (behenate / hydroxystearic acid) polyglyceryl-20 under the trade name TAISET. Products such as OG-C (manufactured by Taiyo Kagaku Co., Ltd., melting point 67°C), refined rice wax R-100 (manufactured by Yokozeki Oil & Fat Co., Ltd., melting point 73-80°C) as rice bran wax, refined carnauba wax No. 1 (manufactured by Cerarica NODA Co., Ltd., melting point 80-86°C) as carnauba wax, refined TOWAX-6F2 (manufactured by Toa Kasei Co., Ltd., melting point 73.5-79.5°C) as sunflower seed wax, Sunsoft No. 8004-C (manufactured by Taiyo Kagaku Co., Ltd., melting point 67-70°C) as glyceryl stearate, and Sunsoft No. 8100-C (manufactured by Taiyo Kagaku Co., Ltd., melting point 75-85°C) as glyceryl behenate are sold.

[0020] In the oily particle dispersion composition of this disclosure, two or more solid oils are used in combination.

[0021] In the oily particle dispersion composition, the total amount of two or more solid oils is not limited as long as the total amount of components (A) to (C) is 90% by mass or more, but preferably 0.1 to 50% by mass is exemplified, more preferably 1 to 40% by mass, even more preferably 5 to 35% by mass, and particularly preferably 10 to 30% by mass is exemplified.

[0022] Furthermore, without limiting this disclosure, from the viewpoint of easily obtaining a composition in which oily particles that easily disintegrate when force is applied are dispersed, it is exemplified that component (A) may more preferably include at least one selected from the group consisting of glyceryl stearate and glyceryl behenate (hereinafter sometimes referred to as component (A2)). Also, from a similar viewpoint, it is exemplified that component (A) may more preferably include at least one selected from the group consisting of (behenate / eicosanedioic acid) glyceryl, behenyl alcohol, tri(behenate / isostearate / eicosanedioic acid) glyceryl, octadeca(behenate / hydroxystearate) polyglyceryl-20, rice bran wax, carnauba wax, sunflower seed wax, candelilla wax, and beeswax (hereinafter sometimes referred to as component (A1)) and component (A2) in combination. Without limiting this disclosure, in these cases, the content of component (A2) is more preferably 1.5% by mass or more in the oily particle dispersion composition, more preferably 2 to 20% by mass, and particularly preferably 2 to 15% by mass. Also without limiting this disclosure, the content of component (A2) is preferably 3 to 70 parts by mass, 4 to 65 parts by mass, more preferably 5 to 25 parts by mass, etc., per 100 parts by mass of component (A1).

[0023] Furthermore, although not limiting to this disclosure, from the viewpoint of obtaining a composition in which oily particles are dispersed that do not easily break down even when force is applied and have a granular texture, it is preferably exemplified that the composition does not contain component (A2) or that its content is less than 1.5% by mass in the oily particle dispersion composition, and more preferably exemplified that it is 0 to 1% by mass or 0 to 0.5% by mass. In this case, although not limiting to this disclosure, it is more preferable that the composition of this disclosure contains component (A1), and that component (A2) is preferably less than 3 parts by mass, more preferably 0 to 2 parts by mass, per 100 parts by mass of component (A1).

[0024] (B) Amphiphilic substances The oily particle dispersion composition of this disclosure comprises (B) an amphiphilic substance, the amphiphilic substance being at least one selected from the group consisting of (B1) to (B4). (B1) Divalent carboxylic acid ester, (B2) Alkylene oxide derivatives, (B3) At least one selected from the group consisting of dihydric alcohols and polyethylene glycols, (B4) Nonionic surfactant with an HLB of 3.5 or higher.

[0025] (B1) The divalent carboxylic acid ester is not particularly limited, but examples of component (C1) include esters of a divalent carboxylic acid and polyglycerin such as (eicosanedioic acid / tetradecanedioic acid) polyglyceryl-10, cyclohexane-1,4-dicarboxylic acid bisethoxydiglycol, diethoxyethyl succinate, and diethylhexyl succinate.

[0026] These are commercially available, and examples include (eicosanedioic acid / tetradecanediic acid) polyglyceryl-10, trade names Neosolue-Aqua and Neosolue-AquaS; cyclohexane-1,4-dicarboxylic acid bisethoxydiglycol, trade name Neosolue-Aqulio; diethoxyethyl succinate, trade name CRODAMOL DES; and diethylhexyl succinate, trade name CRODAMOL OSU (all manufactured by Croda Japan Co., Ltd.).

[0027] Component (B1) may be used alone or in combination of two or more components.

[0028] (B2) The alkylene oxide derivative is not particularly limited, but examples include PEG / PPG / polybutylene glycol-8 / 5 / 3 glycerin, PPG-16 glyceryl ether, glycereth-26, PPG-10 methyl glucose, PPG-20 methyl glucose, methyl gluceth-10, methyl gluceth-20, PPG-14 polyglyceryl-2 ether, PPG-9 diglyceryl, PPG-10 buteth-9, PPG-17 buteth-17, PPG-25 sorbitol, PPG-10 sorbitol, PPG-7, PPG-34, PEG / PPG-150 / 35 copolymer, PEG / PPG-160 / 30 copolymer, etc. Examples of component (B2) include preferably PEG / PPG / polybutylene glycol-8 / 5 / 3 glycerin, PPG-10 methyl glucose, PPG-20 methyl glucose, methyl gluceth-10, methyl gluceth-20, PPG-9 diglyceryl, glycereth-26, PPG-14 polyglyceryl-2 ether, etc.

[0029] These are commercially available and are sold under various names, such as Wilbride S-753 (manufactured by NOF Corporation) as PEG / PPG / polybutylene glycol-8 / 5 / 3 glycerin, Macbiobride MG-10P (manufactured by NOF Corporation) as PPG-10 methyl glucose, Macbiobride MG-20P (manufactured by NOF Corporation) as PPG-20 methyl glucose, Macbiobride MG-10E (manufactured by NOF Corporation) as methyl gluceth-10, Macbiobride MG-20E (manufactured by NOF Corporation) as methyl gluceth-20, SY-DP9 (manufactured by Sakamoto Pharmaceutical Co., Ltd.) as PPG-9 diglyceryl, Brownon GL-026 (manufactured by Aoki Oil & Fat Co., Ltd.) as glycereth-26, and SY-DP14 (manufactured by Sakamoto Pharmaceutical Co., Ltd.) as PPG-14 polyglyceryl-2 ether.

[0030] Component (B2) may be used alone or in combination of two or more types.

[0031] (B3) At least one selected from the group consisting of dihydric alcohols and polyethylene glycol (PEG) is not particularly limited, but examples of component (B3) include 1,3-butylene glycol (BG), pentylene glycol, isopentyl diol, propylene glycol, dipropylene glycol (DPG), PEG-6, PEG-8, etc.

[0032] Examples of component (B3) include preferably 1,3-butylene glycol, pentylene glycol, isopentyl diol, dipropylene glycol, PEG-6, and the like.

[0033] These are commercially available, and are sold under various trade names such as 1,3-butylene glycol (trade name 1,3-butylene glycol P, manufactured by KH Neochem), pentylene glycol (trade name PUROLAN PD-LO N, manufactured by LANXESS), isopentyl diol (trade name isoprene glycol, manufactured by Kuraray), dipropylene glycol (trade name dipropylene glycol LO+, manufactured by Dow Chemical), and PEG-6 (trade name PEG-300, manufactured by Sanyo Chemical Industries).

[0034] Component (B3) may be used alone or in combination of two or more components.

[0035] (B4) Nonionic surfactants with an HLB of 3.5 or higher are not particularly limited, but examples of components (B4) include polyoxyethylene (POE) alkyl ethers, sorbitan fatty acid esters, POE-sorbitan fatty acid esters, POE-glycerin fatty acid esters, POE-hydrogenated castor oil, POE-hydrogenated castor oil fatty acid esters, POE fatty acid esters, POE sterols / hydrogenated sterols, sucrose fatty acid esters, polyglycerin fatty acid esters, etc.

[0036] In this disclosure, the HLB (Hydrophile Lypophile Balance) value is a known indicator of the balance between hydrophilicity and lipophilicity, and within the range of HLB values ​​from 0 to 20, a smaller HLB value indicates stronger lipophilicity, and a larger HLB value indicates stronger hydrophilicity. In this disclosure, HLB usually follows the Griffin formula. Component (B4) may be used as one or more components, or as two or more components.

[0037] Without limiting this disclosure, examples of components (B4) include: POE-alkyl ethers such as polyoxyethylene oleyl ether and polyoxyethylene cetyl ether; sorbitan fatty acid esters such as sorbitan stearate, sorbitan sesquioleate, sorbitan sesquistearate, sorbitan tristearate, and sorbitan oleate; POE-sorbitan fatty acid esters such as polyethylene glycol (PEG)-20 sorbitan isostearate, PEG-20 sorbitan oleate, PEG-20 sorbitan stearate, and PEG-20 sorbitan coconut oil fatty acid esters; POE-glycerin fatty acid esters such as PEG-15 glyceryl stearate and PEG-20 glyceryl trioleate; POE-hydrogenated castor oil such as PEG-60 hydrogenated castor oil and PEG-40 hydrogenated castor oil; and PE isostearate. Examples include POE-hydrogenated castor oil fatty acid esters such as G-20 hydrogenated castor oil; POE fatty acid esters such as PEG-40 stearate and PEG-150 stearate; POE sterols and hydrogenated sterols such as PEG-20 phytosterol; sucrose fatty acid esters such as sucrose palmitate, sucrose stearate, and sucrose oleate; and polyglycerin fatty acid esters such as polyglyceryl-2 stearate, polyglyceryl-2 isostearate, polyglyceryl-10 stearate, polyglyceryl-10 oleate, polyglyceryl-10 tristearate, polyglyceryl-4 stearate, polyglyceryl-10 distearate, polyglyceryl-10 pentastearate, polyglyceryl-10 stearate, polyglyceryl-10 myristate, and polyglyceryl-10 laurate.

[0038] More preferably, component (B4) includes polyglycerin fatty acid esters, POE fatty acid esters, sucrose stearate esters, and the like. More preferably, component (B4) includes polyglyceryl-10 tristearate, polyglyceryl-4 stearate, polyglyceryl-10 pentastearate, polyglyceryl-10 stearate, polyglyceryl-10 distearate, polyglyceryl-10 myristate, polyglyceryl-10 laurate, PEG-25 stearate, PEG-40 stearate, and PEG-150 stearate.

[0039] These are commercially available, for example, polyglyceryl-10 tristearate under the trade name Decaglyn 3-SV (HLB 7.5) (manufactured by Nikko Chemicals Co., Ltd.), polyglyceryl-4 stearate under the trade name Tetraglyn 1-SV (HLB 6.0) (manufactured by Nikko Chemicals Co., Ltd.), polyglyceryl-10 pentastearate under the trade name Decaglyn 5-SV (HLB 3.5) (manufactured by Nikko Chemicals Co., Ltd.), polyglyceryl-10 stearate under the trade name Decaglyn 1-SV (HLB 12.0) (manufactured by Nikko Chemicals Co., Ltd.), polyglyceryl-10 myristate under the trade name Decaglyn 1-M (HLB 15) (manufactured by Nikko Chemicals Co., Ltd.), and PEG-25 stearate under the trade name NIKKOL Products such as MYS-25V (HLB15) (manufactured by Nikko Chemicals Co., Ltd.), PEG-40 stearate (product name NIKKOL MYS-40V (HLB17.5) (manufactured by Nikko Chemicals Co., Ltd.)), PEG-150 stearate (product name Emanone 3199VB (HLB19.4) (manufactured by Kao Corporation)), and polyglyceryl-10 distearate (product name Decaglyn 2-SV (HLB9.5) (manufactured by Nikko Chemicals Co., Ltd.) are sold.

[0040] Component (B4) may be used alone or in combination of two or more components.

[0041] Although a portion of component (B) may correspond to the component that can be called solid oil, in this case, component (B) is not included in the solid oil in this disclosure. For this reason, the content of component (B) is not included in the content of the solid oil.

[0042] The content of component (B) in the oily particle dispersion composition of this disclosure (the total amount of at least one selected from the group consisting of components (B1) to (B4)) is not limited to satisfying the condition that the total amount of components (A) to (C) described above is 90% by mass or more, but preferably the total amount of component (A) (i.e., two or more solid oils) and component (B) is exemplified as 0.2 to 60% by mass, more preferably 5 to 51% by mass, and even more preferably 8 to 40% by mass.

[0043] Furthermore, the content of component (B) in the oily particle dispersion composition of this disclosure is not limited to satisfying the condition that the total amount of components (A) to (C) described above is 90% by mass or more, but preferably 0.01 to 30% by mass is exemplified. From the viewpoint of producing oily particles more efficiently, more preferably 0.02 to 25% by mass, and even more preferably 0.02 to 20% by mass is exemplified.

[0044] Furthermore, the content of component (B) in the oily particle dispersion composition of this disclosure is not limited to the extent that the total amount of components (A) to (C) described above is 90% by mass or more. However, from the viewpoint of producing good oily particles more efficiently while further suppressing aggregation due to contact between particles during the production of the oily particle dispersion composition, preferably, component (B) is 0.02 to 90 parts by mass per 100 parts by mass of component (A), and more preferably, component ( B ) is 0.1 to 70 parts by mass, more preferably component ( B Examples include amounts of 0.2 to 65 parts by mass.

[0045] Furthermore, without limiting the present disclosure, when component (B1) is used, for example, at least one selected from the group consisting of cyclohexane-1,4-dicarboxylic acid bisethoxydiglycol, diethoxyethyl succinate, and diethylhexyl succinate (referred to as component (B-1)), the content of component (B1-1) in the composition is preferably 0.05 to 20% by mass, more preferably 2 to 18% by mass, and even more preferably 3 to 17% by mass.

[0046] Furthermore, without limiting the present disclosure, when an ester of a divalent carboxylic acid such as (eicosanedioic acid / tetradecanedioic acid) polyglyceryl-10 and polyglycerin (referred to as component (B1-2)) is used as component (B1), the content of component (B1-2) in the composition is preferably 0.01 to 2% by mass, more preferably 0.01 to 1% by mass, and even more preferably 0.01 to 0.7% by mass.

[0047] Without limiting this disclosure, when component (B2) is used as component (B), the content of component (B2) in the composition is preferably 0.05 to 15% by mass, more preferably 0.1 to 13% by mass, and even more preferably 0.5 to 12% by mass.

[0048] Without limiting this disclosure, when component (B3) is used as component (B), the content of component (B3) in the composition is preferably 0.05 to 15% by mass, more preferably 1 to 13% by mass, and even more preferably 3 to 12% by mass.

[0049] Without limiting this disclosure, when component (B4) is used as component (B), the content of component (B4) in the composition is preferably 0.001 to 3% by mass, more preferably 0.005 to 1.5% by mass. Furthermore, when a nonionic surfactant with an HLB of 3.5 or more and less than 10 is used as component (B4), the content of the nonionic surfactant with an HLB of 3.5 or more and less than 10 in the composition is preferably 0.01 to 3% by mass, more preferably 0.05 to 2% by mass, and even more preferably 0.08 to 1.2% by mass. Furthermore, when a nonionic surfactant with an HLB of 10 or more and 20 or less is used as component (B4), the content of the nonionic surfactant with an HLB of 10 or more and 20 or less in the composition is preferably 0.001 to 2% by mass, more preferably 0.005 to 1% by mass, and even more preferably 0.01 to 0.8% by mass.

[0050] (C)Water (C) Water may be tap water, purified water, deionized water, etc. These may be used individually or in combination of two or more. The content of component (C) in the oily particle dispersion composition is not limited to satisfying the requirement that the total amount of components (A) to (C) described above is 90% by mass or more, but preferably 40 to 99% by mass is exemplified, more preferably 50 to 95% by mass, and even more preferably 55 to 90% is exemplified.

[0051] Furthermore, in the oily particle dispersion composition of this disclosure, the ratio of the total amount of solid oil of component (A) and amphiphilic substance of component (B) to water of component (C) (total amount:water) is preferably 1:99 to 60:40. From the viewpoint of producing oily particles more efficiently, the ratio is more preferably 10:90 to 30:70, and even more preferably 20:80 to 30:70.

[0052] The oily particle dispersion composition of this disclosure may further contain any other components as needed, to the extent that it does not impair the effects of this disclosure. Examples of such other components include preservatives, surfactants (cationic surfactants, anionic surfactants, amphoteric surfactants, nonionic surfactants with an HLB of less than 3.5, etc.), inorganic salts, liquid oils, thickeners, colorants, fragrances, vitamins, repellents, etc. These may be used individually or in combination of two or more, and their amounts may be set as appropriate. It can be said that the solid oil of component (A) and the amphiphilic substance of component (B) may have the effects of these other components, but the solid oil and amphiphilic substance are not included in the other components.

[0053] To illustrate with an example of other components, examples of colorants include natural pigments such as iron oxide, tar-based dyes, β-carotene, and carrot root extract, as well as synthetic pigments and mixtures thereof. Although not limiting to this disclosure, oily particles can be colored by simply incorporating (e.g., dissolving or dispersing) a colorant into the oil phase described later.

[0054] Examples of fragrances include various essential oils and blended fragrances such as herbal essential oils like lavender oil, rosemary oil, clary sage oil, thyme oil, bergamot oil, and eucalyptus oil; mint essential oils like peppermint oil, spearmint oil, and peppermint oil; and citrus essential oils like orange oil, lemon oil, and grapefruit oil (whether natural, synthetic, or a mixture thereof). Although not limiting to this disclosure, a simple way to flavor oily particles is to blend a fragrance into the oil phase described later.

[0055] Examples of vitamins include tocopherol, tocopherol succinate, tocopherol nicotinate, tocopherol acetate, ascorbyl tetrahexyldecanoate, retinyl acetate, retinyl palmitate, and retinyl propionate. Since vitamins are mainly oil-soluble, this disclosure is not limited, but for convenience, it is preferable to incorporate vitamins into the oil phase described later.

[0056] Examples of inorganic salts include inorganic salts of alkali metals such as sodium and potassium; and inorganic salts of alkaline earth metals such as magnesium and calcium. Examples of inorganic salts of alkali metals include chlorides such as sodium chloride and potassium chloride. Examples of inorganic salts of alkaline earth metals include chlorides such as calcium chloride and magnesium sulfate. When inorganic salts are included, the content is not limited, but an example of 2% by mass or less in the composition is given, and preferably 0.001 to 2% by mass, 0.01 to 1.5% by mass, 0.05 to 1% by mass, etc. Note that the oily particle dispersion composition of this disclosure may not contain inorganic salts.

[0057] Liquid oils are liquid at 25°C, and examples of liquid oils include ester oils, hydrocarbon oils, vegetable oils, animal oils, silicone oils, higher fatty acids, and higher alcohols. These may be used individually or in combination of two or more types.

[0058] Ester oils include ester oils of linear fatty acids and lower alcohols such as diethyl sebacate, diisopropyl sebacate, isopropyl myristate, isopropyl palmitate, and ethyl stearate; ester oils of linear fatty acids and linear higher alcohols such as cetyl caprate, hexyl laurate, decyl oleate, and oleyl oleate; isostearyl laurate, isotridecyl myristate, isocetyl myristate, isostearyl myristate, octyldodecyl myristate, ethylhexyl palmitate, and iso Ester oils of straight-chain fatty acids such as cetyl, isostearyl palmitate, 2-ethylhexyl stearate, isocetyl stearate, isodecyl oleate, octyldodecyl oleate, and octyldodecyl ricinoleate with branched-chain alcohols; ester oils of branched-chain fatty acids such as ethyl isostearate and isopropyl isostearate with lower alcohols; branched-chain fatty acids such as cetyl ethylhexanoate, cetearyl ethylhexanoate, stearyl ethylhexanoate, hexyl isostearate, and hexyldecyl isostearate Ester oils of fatty acids and linear higher alcohols; ester oils of branched fatty acids and polyhydric alcohols such as neopentyl glycol diethylhexanoate; ethylene glycol dioctanoate, ethylene glycol dioleate, propylene glycol caprylate, propylene glycol dicaprylate, di(caprylic / capric acid)propylene glycol, propylene glycol dicaprate, dipropylene glycol dioleate, neopentyl glycol dicaprate, neopentyl glycol dioctanoate, glyceryl tricaprylate, Ester oils of fatty acids and polyhydric alcohols such as triethylhexanoin, caprylic / capric triglyceride, glyceryl triisopalmitate, triisostearin, glyceryl diisostearate, caprylic / capric / myristic / stearic triglyceride, glyceryl ethylhexanoate / stearic / adipate, trimethylolpropane triethylhexanoate, trimethylolpropane triisostearate, pentaerythrityl tetraethylhexanoate, and pentaerythrityl tetraisostearate;Ester oils of branched-chain fatty acids and branched-chain alcohols such as octyldodecyl neopentanoate, isodecyl neopentanoate, isocetyl octanoate, isostearyl octanoate, ethylhexyl isoperargonate, hexyldecyl dimethyloctanoate, octyldodecyl dimethyloctanoate, ethylhexyl isopalmitate, isocetyl isostearate, isostearyl isostearate, octyldodecyl isostearate; lauryl lactate, myristyl lactate, octyldodecyl lactate, trioctyl citrate, triisocetyl citrate, trioctyldodecyl citrate Examples include ester oils containing hydroxyl groups such as syl, diisostearyl malate, and trimethyl trimellitate; ester oils of fatty acids and dibasic acids with polyhydric alcohols such as (caprylic / capric / succinic acid) triglyceride; ester oils of benzoic acid and fatty alcohols such as alkyl benzoate (C12-15) and alkyl benzoate (C16,17); ester oils of fatty acids and polyglycerin such as polyglyceryl-6 octacaprylate; and dimer dilinoleate ester oils such as dimer dilinoleyl dimer dilinoleate and di(isostearyl / phytosteryl) dimer dilinoleate.

[0059] Examples of hydrocarbon oils include liquid paraffin, light liquid isoparaffin, heavy liquid isoparaffin, liquid isoparaffin, polybutene, polyisobutene, hydrogenated polyisobutene, squalane (including sugar-squalane), squalene, α-olefin oligomers, isohexadecane, isododecane, and other linear or branched hydrocarbon oils.

[0060] Examples of vegetable oils include rapeseed oil, avocado oil, almond oil, olive oil, kukui nut oil, sesame oil, wheat germ oil, rice germ oil, rice bran oil, rice oil, safflower oil, sunflower oil, soybean oil, evening primrose oil, corn oil, rapeseed oil, peach kernel oil, palm oil, palm kernel oil, castor oil, jojoba oil, grapeseed oil, macadamia nut oil, meadowfoam oil, barnyard grass oil, coconut oil, and rosehip oil.

[0061] Examples of animal oils include liquid horse oil, mink oil, and liquid lanolin. Examples of silicone oils include cyclopentasiloxane, methylpolysiloxane, dimethylpolysiloxane, dimethylcyclopolysiloxane, decamethylcyclopentasiloxane, methylphenylpolysiloxane, methylhydrogenpolysiloxane, and higher alcohol-modified silicone oils. Examples of higher fatty acids include oleic acid and isostearic acid. Examples of higher alcohols include isostearyl alcohol, octyldodecanol, and hexyldecanol.

[0062] As described above, the oily particle dispersion composition of this disclosure may contain liquid oil, and its content is not limited. For example, the liquid oil content in the composition is exemplified as 10% by mass or less, preferably 0-5% by mass, more preferably 0-2% by mass, 0-0.5% by mass, etc. Thus, the composition may or may not contain liquid oil. Conventional oily particle dispersion compositions often use liquid oil as an essential component. According to this disclosure, a desired oily particle dispersion composition can be obtained without using such liquid oil as an essential component. In particular, according to this disclosure, the hardness and disintegration of the oily particle dispersion composition, more specifically the hardness and disintegration of the oily particles contained in the composition, can be adjusted as shown in the examples described below, even without using liquid oil as an essential component.

[0063] As an example of a thickening agent, a water-soluble thickening agent is given. The water-soluble thickening agent is not limited as long as it can impart viscosity to the aqueous phase described later at room temperature (25°C). Examples of water-soluble thickening agents include plant-derived polymers such as agar, xanthan gum, gum arabic, galactan, carob gum, guar gum, carrageenan, tragacanth gum, karaya gum, pectin, quince seed (quince), and algae colloid (brown algae extract); microbial polymers such as dextran, succinoglucan, and pullulan; animal-derived polymers such as collagen, casein, albumin, and gelatin; alginate-based polymers such as sodium alginate and propylene glycol alginate; vinyl-based polymers such as polyvinyl alcohol, polyvinyl ethyl ether, polyvinylpyrrolidone, carboxyvinyl polymer, and alkali-modified carboxyvinyl polymer; methylcellulose, ethylcellulose, etc. Examples include cellulosic polymers such as hydroxypropylcellulose, methylhydroxypropylcellulose, hydroxyethylcellulose, nitrocellulose, sodium carboxymethylcellulose, crystalline cellulose, sodium cellulose sulfate, and cellulose powder; acrylic polymers such as sodium polyacrylate, polyethyl acrylate, polyacrylamide, and (acrylic acid / alkyl acrylate (C10-30) copolymer); polyoxyethylene polymers; polyoxyethylene polyoxypropylene copolymer polymers; polyethyleneimine; cationic polymers; bentonite; magnesium aluminum silicate; laponite; hectorite; and anhydrous silicic acid.

[0064] By incorporating a water-soluble thickener into the aqueous phase, viscosity is imparted to the aqueous phase, which is the dispersion medium. This makes it more difficult for oily particles to come into contact with each other, thus suppressing aggregation, coalescence, and damage caused by shaking of the oily particles. In this respect, incorporating a water-soluble thickener into the aqueous phase is preferable.

[0065] However, since a desired oily particle dispersion composition can be easily manufactured even without using a water-soluble thickener in this disclosure, the oily particle dispersion composition of this disclosure preferably does not contain a water-soluble thickener. From this viewpoint, examples of the water-soluble thickener content in the aqueous phase include preferably 0 to 1% by mass, more preferably 0 to 0.5% by mass, 0 to 0.1% by mass, 0 to 0.01% by mass, 0 to 0.008% by mass, 0 to 0.005% by mass, etc. When a water-soluble thickener is incorporated, problems tend to arise such as the oily particle dispersion composition taking a long time to dry due to its water retention properties, or the oily particles being difficult to separate due to aggregation even after drying. In this disclosure, since a good oily particle dispersion composition can be manufactured even without incorporating a water-soluble thickener or by reducing its amount, the advantage of being able to easily manufacture a good oily particle dispersion composition while mitigating such problems can be appropriately demonstrated. Furthermore, while this disclosure includes manufacturing an oily particle dispersion composition without a water-soluble thickener or by reducing the amount of water-soluble thickener used, this does not prevent the use of a water-soluble thickener in combination with the composition or with the oily particles which are the dispersion medium removal product after the composition has been manufactured.

[0066] While not limited to the foregoing, examples of the viscosity of the aqueous phase, which is the dispersion medium in this disclosure, include preferably 100 mPa·s or less at 25°C, more preferably 50 mPa·s or less, even more preferably 30 mPa·s or less, and particularly preferably 15 mPa·s or less. The lower limit of viscosity is theoretically 0 mPa·s. Examples of the viscosity of the aqueous phase include preferably a range of 0 to 100 mPa·s, more preferably 0 to 30 mPa·s. As can be understood from the examples described later, the oily particle dispersion composition of this disclosure is usually manufactured by mixing an oil phase containing a solid oil of component (A) and an amphiphilic substance of component (B) with an aqueous phase containing water of component (C), and the viscosity of the aqueous phase is determined according to the procedure of the examples described later. The viscosity of the aqueous phase in this disclosure refers to the viscosity of the aqueous phase (dispersion medium) obtained by filtering the oily particle dispersion composition, as shown in the examples described later.

[0067] Such viscosity ranges are preferably exemplified from the standpoint of suppressing adhesion of oily components to the container wall during the manufacture of the composition of this disclosure, particularly when manufacturing using large-capacity containers such as tanks in factories, as well as preventing adhesion of the oil phase and oily particles to the container wall and poor dispersion due to coalescence of particles, and from the standpoint of obtaining spherical particles more easily.

[0068] In the oily particle dispersion composition of this disclosure, oily particles containing component (A) are present in a dispersion medium containing component (C). Furthermore, in the oily particle dispersion composition of this disclosure, component (B) is present in both the oily particles and the dispersion medium. Thus, the oily particle dispersion composition of this disclosure is a composition in which oily particles are dispersed, and the composition as a whole is liquid at room temperature (25°C).

[0069] In this disclosure, the size of the oily particles in the composition is not limited, but examples of average particle size (diameter) are typically 0.01 to 3 mm, preferably 0.05 to 3 mm, and more preferably 0.1 to 2.5 mm. The particle size may be appropriately determined within these ranges depending on the intended use. The particle size refers to the particle size of the primary particles. The particle size is determined according to the procedure in the examples described below. If necessary, the magnification of the lens may be appropriately changed according to the particle size during measurement.

[0070] In this disclosure, the form of the oily particles in the composition is not limited, but it is preferably exemplified that the value calculated according to the following formula is in the range of 0 or more and less than 0.3, and more preferably in the range of 0 or more and less than 0.1. This value is determined by observation and measurement using a digital microscope according to the procedure of the examples described below. Oblateness F=(ab) / a In the formula, a is the major axis of the oily particle (in mm), and b is the minor axis of the oily particle (in mm). In the case of a spherical shape, a and b are equivalent, so the flattening ratio F is 0.

[0071] The oily particle dispersion composition of this disclosure can be produced by mixing components (A) to (C), and, if necessary, other components. The other components may be mixed in the oil phase, in the aqueous phase, or in a mixture obtained after mixing the oil phase and the aqueous phase, and the choice of the other components may be determined as appropriate depending on their properties (solubility, etc.) and intended use.

[0072] The following procedure exemplifies a preferred method for producing the oily particle dispersion composition of this disclosure, although this method is not limited to the foregoing.

[0073] [Step (1)] A step of mixing (A) two or more solid oils and (B) an amphiphilic substance to obtain a mixed liquid at a temperature above the melting point of component (A), and [Step (2)] A step of granulating oily particles by adding the above mixture and water (C) at a temperature above the melting point of component (A), and stirring the resulting mixture to a temperature below the melting point of component (A). A method for producing an oily particle dispersion composition containing [the specified element].

[0074] By mixing components (A) to (C) in this manner, and by further mixing other components as needed, to the extent that they do not interfere with the effects of this disclosure, and by lowering the temperature to below the melting point of component (A) while stirring, oily particles are formed in a dispersed state in the dispersion medium, and an oily particle dispersion composition can be produced.

[0075] The temperature above the melting point of component (A) can be appropriately determined depending on the component (A) used and is not particularly limited, but preferably it is above the melting point of component (A) and less than 100°C, more preferably it is above the melting point of component (A) and 90°C or less, even more preferably it is above the melting point of component (A) and 88°C or less, and particularly preferably it is above the melting point of component (A) and 85°C or less. The means of raising the temperature above the melting point of component (A) are not limited and the temperature can be adjusted by any means such as water bath heating using a water bath as needed. In the manufacturing method of this disclosure, above the melting point of component (A) means above the melting point of the solid oil with the highest melting point among the solid oils of component (A) used.

[0076] The temperature below the melting point of component (A) can be appropriately determined depending on the component (A) used and is not particularly limited, but preferably below the melting point of component (A) at 5°C or higher is an example, more preferably below the melting point of component (A) at 10°C or higher, 15 to 40°C is an example, and from the viewpoint of simplicity and low cost, temperatures around room temperature (25°C), such as 20 to 38°C or 20 to 35°C, are also examples. In this case as well, the means of adjusting the temperature are not limited and any means may be used as needed. In the manufacturing method of this disclosure, below the melting point of component (A) means below the melting point of the solid oil with the lowest melting point among the solid oils of component (A) used. These temperatures may be appropriately changed depending on the other components.

[0077] As described above, after mixing the oil phase and the aqueous phase, the resulting mixture is stirred to a temperature below the melting point of component (A) to granulate oily particles. The stirring should be sufficient to ensure that the mixture obtained by mixing the liquid phase and the aqueous phase is stirred to the extent that the resulting oily particles do not remain in the mixture. Furthermore, shearing treatment is not required in this stirring. For this reason, in this disclosure, low-speed stirring using a stirring device such as a propeller, pulsator, or anchor-type paddle is preferable. In the case of propeller stirring, although it depends on the manufacturing scale and the size of the propeller, a rotational speed of 50 to 400 rpm, more preferably 50 to 250 rpm, is preferably exemplified. In the case of stirring using a pulsator or the like, it is sufficient to stir to the same extent as propeller stirring. Thus, the stirring should be sufficient to the extent that it does not violently disturb the surface of the mixture or entrain a large amount of air bubbles. When the mixing tank (container for mixing the liquid phase and aqueous phase) is deep or the manufacturing scale is large, stirring efficiency may be improved by promoting vertical convection by installing stirring devices at multiple locations as needed, such as by installing propellers at two locations (top and bottom). In such cases, however, strong stirring that generates localized shear force through high-speed stirring with a single propeller is undesirable.

[0078] Conventionally, when mixing an oil phase and an aqueous phase to form oily particles in a mixed liquid, shearing treatment was sometimes essential. When shearing treatment is performed, shearing equipment such as homomixers, disperser mixers, ultramixers, colloid mills, and homogenizers is usually required, which added extra effort and cost to their manufacture. In this disclosure, an oily particle dispersion composition can be easily manufactured without such shearing treatment. Furthermore, in the stirring process of this disclosure, baffles that generate turbulence to improve stirring efficiency are not essential. Rather, in this disclosure, the use of baffles that generate turbulence is undesirable because it suppresses deformation of the oily particles and efficiently produces spherical oily particles.

[0079] Furthermore, according to this disclosure, it is not essential to inject the oil phase from below the aqueous phase when mixing the oil phase and the aqueous phase. From this perspective as well, this disclosure makes it possible to easily produce an oily particle dispersion composition without performing such complicated procedures.

[0080] In the manufacturing method of this disclosure, when preparing the oil phase and aqueous phase, stirring is optional as long as the components in each phase are uniformly mixed, but it is preferable to stir to ensure uniform mixing. Also, for example, the aqueous phase may be added to the oil phase, or the oil phase to the aqueous phase, and the mixing order is not limited.

[0081] Furthermore, as long as the oily particle dispersion composition of this disclosure is obtained, the amount of oil phase and aqueous phase mixed is not limited. Examples of the amount of oil phase and aqueous phase mixed include, preferably, 1:0.8 to 30, more preferably 1:0.8 to 15, even more preferably 1:0.8 to 10, particularly preferably 1:0.8 to 5, particularly more preferably 1:0.8 to 3, and most still preferably 1:0.8 to 2.5 as the oil phase:aqueous phase (mass ratio).

[0082] The oily particle dispersion compositions of this disclosure have good dispersion stability in liquid. In this disclosure, good dispersion stability in liquid means that aggregation of oily particles is suppressed at room temperature (25°C). Dispersion stability in liquid is evaluated according to the dispersion stability in liquid (25°C) shown in the examples below.

[0083] The oily particle dispersion composition of this disclosure may be used as is, or may be used after being incorporated into a pharmaceutical raw material. Furthermore, the oily particles (dispersion medium removed) obtained by removing the dispersion medium from the oily particle dispersion composition may be used as is, or the oily particles (dispersion medium removed) may be incorporated into a pharmaceutical raw material. The oily particles of this disclosure may also be used as capsules (also referred to as capsule coating materials, etc.). As described above, in the oily particle dispersion composition of this disclosure, oily particles are formed in a mixed liquid containing an oil phase and an aqueous phase, so the oily particles can be called the dispersed phase and the rest can be called the dispersion medium. When obtaining oily particles by removing the dispersion medium, there is no limit to the degree of dispersion medium removal, and only a part of the dispersion medium (total dispersion medium) constituting the oily particle dispersion composition (for example, 1 / 2 mass% of the total dispersion medium) may be removed, or the entire dispersion medium may be removed by sieving with a sieve or similar device. Thus, when oily particles are incorporated into a formulation raw material, they may be incorporated in the presence of a dispersion medium, or the oily particles may be incorporated after the dispersion medium has been removed by sieving the oily particle dispersion composition. Furthermore, if substantially all of the dispersion medium is removed by sieving, for example, the resulting oily particles may be washed with water, or they may be dried in an environment with a temperature and humidity that does not affect the quality of the oily particles. In this disclosure, "formulation raw material" means the raw material of the final formulation, and refers to raw materials (components) other than the oily particle dispersion composition (or the dispersion medium removed material if only the dispersion medium removed material is used) contained in the formulation. The formulation raw material (component) is not limited as long as it can be used in combination with the oily particle dispersion composition or the dispersion medium removed material. Although this does not limit this disclosure, for example, as mentioned above, a water-soluble thickener is not essential in the manufacture of the oily particle dispersion composition in this disclosure, but if a viscous formulation is desired, a water-soluble thickener may be used as a formulation raw material.

[0084] From this perspective, without limiting the present disclosure, when using a dispersion medium-removed product (particularly when using a product with the entire dispersion medium removed), a more preferable example of the oily particle dispersion composition of this disclosure is a composition in which aggregation of oily particles obtained by removing the dispersion medium is suppressed. Whether aggregation of oily particles obtained by removing the dispersion medium is suppressed is evaluated according to the stability (25°C) of the oily particles obtained by removing the dispersion medium by sieving, as shown in the examples described later.

[0085] The form of the formulation is not limited and may be liquid at room temperature (liquid, emulsion, etc.), semi-solid, or solid (gel, cream, paste, mousse, stick, granules, etc.), preferably liquid or semi-solid. Therefore, the formulation may be any dosage form, such as a liquid, gel, or cream, such as a lotion, liniment, or emulsion. Preferred examples of formulations include cosmetics, quasi-drugs, pharmaceuticals, chemical products, and pesticides. Thus, the oily particle formulation of this disclosure is not limited to any particular use. Preferred examples of formulations include facial cleansers, lotions, emulsions, serums, gel formulations, creams, fragrances, insect repellents, and insecticides.

[0086] The amount of oily particle dispersion composition and the amount of oily particles to be incorporated into the formulation may be appropriately determined depending on the intended use and the form of the formulation. Furthermore, the other components (formulation raw materials) in the formulation, besides the oily particle dispersion composition and oily particles, may also be appropriately determined depending on the form and intended use. Such components may include any components, including the aforementioned other components, and their amounts may also be appropriately determined. While not limiting this disclosure, the formulations described above are examples, and preferably examples include external formulations (external compositions) such as scrubs (scrub facial cleansers, etc.), fragrances, and insect repellents for clothing.

[0087] Thus, according to this disclosure, new oily particle dispersion compositions can be easily manufactured. In particular, according to this disclosure, new oily particle dispersion compositions with dispersion stability as described above can be easily provided. Furthermore, according to this disclosure, compositions containing dispersed oily particles that easily disintegrate when force is applied, or compositions containing dispersed oily particles that do not easily disintegrate when force is applied and have a granular texture can be easily manufactured according to the purpose. Thus, according to this disclosure, the hardness and disintegrability of the granular texture can be appropriately changed, so for example, if hard and difficult-to-disintegrate oily particles are used, they can be preferably applied as scrubbing agents, fragrances, clothing insect repellents, etc. [Examples]

[0088] The embodiments of this disclosure will be described in more detail below with examples, but the embodiments of this disclosure are not limited to the examples below.

[0089] Test example 1. Preparation of an oily particle dispersion composition Each composition was prepared according to the components and content shown in Tables 1-3 (Examples 1-33, Comparative Examples 1-8).

[0090] For example, the manufacturing procedure for the oily particle dispersion composition of Example 1 shown in Table 1 is as follows: (A) two types of solid oils and (B) an amphiphilic substance were added in their entirety to a dissolution tank. The resulting mixture was heated in a water bath to a temperature above the melting point of component (A) (85°C), and stirred to obtain mixture 1 (oil phase). Separately, (C) water and phenoxyethanol were added in their entirety to a mixing tank. The resulting mixture was heated in a water bath to a temperature above the melting point of component (A), and stirred to obtain mixture 2 (aqueous phase). Next, the obtained mixture 1 was added in its entirety to the mixing tank (mixture 2), and stirred (propeller stirring at 200 rpm). While stirring and dispersing the resulting oil droplets, the mixing tank was cooled with water (25°C) using a water bath. During the stirring and cooling process, the dispersed oil droplets hardened at approximately 50-65°C (mixture temperature) (formation of oily particles). The mixture was then stirred and cooled to approximately 30°C (mixture temperature) to prepare the oily particle dispersion composition of Example 1. The oily particle dispersion compositions of Examples 2 to 33, shown in Tables 1 to 3, were prepared in the same manner as in Example 1.

[0091] Comparative Examples 1 to 8 were prepared in the same manner as in Example 1, except that only one type of solid oil of component (A) was used, no solid oil of component (A) was used at all, and / or component (B) was not used. The oil phase and aqueous phase were obtained in the same manner as in Example 1, the entire amount of the obtained mixture was put into a mixing tank, stirred in the same manner as described above, and the mixing tank was cooled and stirred in the same manner using a water bath with water (25°C) to prepare each of the comparative examples.

[0092] 2. Evaluation Procedure For each prepared composition, the following were evaluated according to the procedure below: the state of oily particle formation after mixing the oil phase and the aqueous phase (Evaluation 1), particle size (Evaluation 2), particle shape (Evaluation 3), hardness and disintegration (Evaluation 4), and the dispersion stability of the oily particles in liquid (25°C) (Evaluation 5). The dispersion stability of the oily particles in liquid at 50°C and 0°C was also evaluated (Evaluation 6 and Evaluation 7, respectively). Furthermore, the stability of the oily particles obtained by removing the dispersion medium from each composition by sieving (25°C, 50°C) was also evaluated (Evaluation 8, 9).

[0093] 2-1) State of oily particle formation (Evaluation 1) The compositions of Examples 1-33 and Comparative Examples 1-8, obtained according to the procedure described above, were cooled to approximately 30°C (mixture temperature). The state of oily particle formation in the compositions was visually inspected and evaluated in three stages. Specifically, if the oily particles were dispersed without agglomeration in the obtained composition, it was evaluated as having good dispersibility (○). If agglomeration of oily particles was observed in the obtained composition, it was evaluated as having partial agglomeration (△). Furthermore, if more than one-third of the existing oily particles were agglomerated or no oily particles were formed, it was evaluated as agglomeration and no particle formation (×).

[0094] ○: Good dispersibility △: Partial aggregation ×: No agglomeration or particle formation

[0095] 2-2) Particle size (Evaluation 2) Using a digital microscope VHX-5000 (manufactured by Keyence Corporation), approximately 0.01 to 0.1 g of each of the oily particle dispersion compositions (Examples 1 to 33, Comparative Examples 5 to 8) was placed on a glass slide and observed at a magnification of 20 to 100 times. The diameter measured by scale measurement was defined as the particle size. When the particle size was small (evaluation A below), the sample amount was kept small for easier measurement, and the oily particles were diluted with water as appropriate to prevent overlapping. The number of oily particles measured was 30 per composition, and the average value (average particle size) was calculated. The observed oily particles were either spherical or elliptical. In the case of elliptical particles, the major and minor axes of the particle were measured, and the value calculated according to the following formula was defined as the diameter. The provisional diameter of an ellipse = (major axis + minor axis) / 2

[0096] <Average particle size (mm)> A: 0.05 or higher, less than 0.2 B: 0.2 or higher, less than 0.5 C: 0.5 or more, less than 1 D: 1 or more and less than 1.5 E: 1.5 or more and less than 2

[0097] 2-3) Shape of oily particles (Evaluation 3) The shape was observed using a digital microscope VHX-5000, following the same procedure as in Evaluation 2. If the particle was spherical, its diameter was measured. If it was not spherical, it was considered elliptical, and the flattening ratio (F), which indicates the degree of ellipsis, was used for shape evaluation. The flattening ratio was calculated from the major and minor axes of the measured oil particles using the following formula. Oblateness F=(ab) / a In the formula, a is the major axis (in mm) and b is the minor axis (in mm). In the case of a sphere, a and b are equivalent, so the flattening ratio F is 0.

[0098] ◎: Less than 0.1 ○: 0.1 or more and less than 0.3 ×: 0.3 or higher The number of oily particles measured was set at 30 per composition, and the average value was calculated. A value of flattening ratio F closer to 0 indicates that the particle is closer to a sphere.

[0099] 2-4) Hardness and disintegration properties (evaluation 4) 0.06g of each composition was placed on the backs of the hands of five expert panelists, and the distance was 16cm. 2 The product was applied to the area by drawing a circular motion (10 times) with the pad of a finger. The particle sensation felt on the skin during application and the disintegration of oily particles on the skin were evaluated according to the following criteria. The criteria were standardized by comparing them with the other panelists beforehand. The table shows the total values ​​from the five panelists.

[0100] 4 points: No grainy texture (the particles were soft), and it crumbled smoothly. 3 points: It gradually crumbled while you could feel the graininess. Points 2: It has a noticeable particle texture and is long-lasting. 1 point: The particles are hard and do not crumble.

[0101] 2-5) Dispersion stability of oily particles (25°C) (Rating 5) 45g of each composition was placed in a container (50ml glass screw-top tube), sealed, and stored at room temperature (25°C). The number of days on which particle aggregation was observed was recorded and evaluated as follows. Aggregation was defined as a state where the aggregated particles could not be broken up even by manually shaking the storage container.

[0102] ◎: No aggregation observed for 8 months or more. ○: No aggregation observed for more than one month. ×: Aggregation was observed in less than one month.

[0103] 2-6) Dispersion stability of oily particles (50°C) (Rating 6) Except for being stored at 50°C, the same procedure as in Evaluation 5 described above was used, and the number of days on which particle aggregation was observed was recorded and evaluated as follows. Aggregation was defined as a state where the aggregated particles could not be broken up even by manually shaking the storage container.

[0104] ◎: No aggregation observed for 4 months or more. ○: No aggregation observed for more than one month. ×: Aggregation was observed in less than one month.

[0105] 2-7) Dispersion stability of oily particles (0°C) (Rating 7) Except for being stored at 0°C, the same procedure as in Evaluation 5 described above was followed, and the number of days on which particle aggregation was observed was recorded and evaluated as follows. Aggregation was defined as a state where the aggregated particles could not be broken up even by manually shaking the storage container.

[0106] ◎: No aggregation observed for 4 months or more. ○: No aggregation observed for more than one month. ×: Aggregation was observed in less than one month.

[0107] 2-8) Stability of oily particles after sieving (25°C) (Rating 8) The dispersion medium was removed from each composition by sieving (nylon mesh N-No.305T, mesh opening 48 μm). The oily particles were washed by sprinkling purified water over them, and the resulting oily particles were left at room temperature (25°C) for 24 hours in a state where the particles were in contact with each other. After 24 hours, 10 g of oily particles was mixed with 50 g of water and stirred slowly with a stirring rod for 10 seconds, roughly by hand. The presence or absence of aggregation of oily particles in the resulting mixture was observed. At this time, the presence or absence of aggregation was confirmed visually or using an optical microscope depending on the particle size.

[0108] ◎: Dispersed quickly within 1 minute of stirring. ○: Although some oily particles showed aggregation, they quickly broke down and dispersed one by one within 5 minutes of stirring. △: Although the oily particles were broken down and dispersed one by one by stirring, it took more than 5 minutes of stirring (within 10 minutes) for all the oily particles to be broken down. ×: Aggregation remained even after 10 minutes of stirring.

[0109] 2-9) Stability of oily particles after sieving (0°C) (Rating 9) Except for being stored at 0°C, the same procedure as in Evaluation 8 described above was followed, and the number of days on which particle aggregation was observed was recorded and evaluated as follows.

[0110] Furthermore, the viscosity of the aqueous phase used in the preparation of each composition was measured. Specifically, the dispersion medium was removed from each composition prepared in the same manner as described above by sieving, and the viscosity of the dispersion medium obtained in this manner was measured and defined as the viscosity of the aqueous phase. The viscosity of the dispersion medium (aqueous phase) was measured at a dispersion medium temperature of 25°C using a B-type viscometer (VISCOMETER TVB-10M, manufactured by Toki Sangyo Co., Ltd., viscosity range 15~2,000,000 mPa·s), following the operating procedure, with a dispersion medium volume of 200 ml, rotor No. 1, and a rotation speed of 60 rpm, after 1 minute of rotation (the upper limit of viscosity measurement at rotor No. 1 and rotation speed of 60 rpm is 100 mPa·s). The lower limit of the viscosity that can be measured under these conditions (measurement limit) is 15 mPa·s, and as shown in Tables 1 to 3, the viscosity of the dispersion medium in all compositions was less than 15 mPa·s. Furthermore, the device used displays the measured viscosity even when it is below 15 mPa·s, and values ​​below 15 mPa·s are treated as reference values. The viscosity expressed in the dispersion medium for all of the compositions shown in Tables 1 to 3 was 3 mPa·s.

[0111] 3.Results The results are shown in Tables 1 to 3. Table 1 shows the results for Comparative Examples 1 to 8 and Examples 1 to 5 of the oily particle dispersion compositions, Table 2 shows the results for Examples 6 to 25 of the oily particle dispersion compositions, and Table 3 shows the results for Examples 26 to 33 of the oily particle dispersion compositions.

[0112] [Table 1]

[0113] [Table 2]

[0114] [Table 3]

[0115] As shown in Table 1, compositions prepared by blending (A) two or more solid oils, (B1) a divalent carboxylic acid ester as component (B), and (C) water, with the total amount of components (A) to (C) being 99.5% by mass (Examples 1 to 5), all yielded good results in evaluations 1 to 8. Furthermore, in the compositions of Examples 3 to 5, which contained glyceryl stearate or glyceryl behenate as component (A), compositions were obtained in which oily particles that easily disintegrate when force is applied were dispersed.

[0116] In contrast, as shown in Table 1, in Comparative Examples 1-4, which contain (A) two or more types of solid oils and (C) water in a total amount of 99.5% by mass, but (B) no amphiphilic components, oily particles themselves were not formed, and the result of Evaluation 1 was ×. For this reason, Evaluations 2-9 were not performed for the compositions of Comparative Examples 1-4. Also, as shown in Table 1, in Comparative Examples 5-7, which contain (B) amphiphilic components and (C) water in a total amount of 99.5% by mass, but (A) no two or more types of solid oils, the formation of oily particles was observed in Evaluation 1 (○ in Comparative Example 5, △ in Comparative Examples 6 and 7), but the evaluation result for oily particles in Evaluation 3 was ×. Also, as shown in Table 1, in Comparative Example 8, which contains (B) amphiphilic components and (C) water in a total amount of 99.5% by mass, but (A) no two or more types of solid oils, oily particles themselves were not formed, and the result of Evaluation 1 was ×.

[0117] Table 2 shows the results when (B2), (B3), or (B4) were used instead of component (B1). Specifically, Examples 6 to 14 in Table 2 show the results of oily particle dispersion compositions in which an alkylene oxide derivative was blended with (B2) along with (A) two or more solid oils and (C) water, with the total amount of these components being 99.5% by mass. Examples 15 to 18 in Table 2 show the results of oily particle dispersion compositions in which a dihydric alcohol or polyethylene glycol was blended with (B3) along with (A) two or more solid oils and (C) water, with the total amount of these components being 99.5% by mass. Examples 19 to 25 in Table 2 show the results of oily particle dispersion compositions in which a nonionic surfactant with an HLB of 3.5 or higher was blended with (HLB of 3.5 or higher) along with (A) two or more solid oils and (C) water, with the total amount of these components being 99.5% by mass. Good results were also obtained in evaluations 1 to 8 for these compositions (Examples 6 to 25).

[0118] Table 3 shows the results (Examples 26-33) of using (A) two or more solid oils and (C) water in combination with two components selected from (B1), (B2), (B3), and (B4) as component (B). Good results were also obtained in evaluations 1-8 for the oily particle dispersion compositions of Examples 26-33.

[0119] Thus, it was found that by combining (A) two or more solid oils, (B) an amphiphilic substance (at least one selected from the group consisting of (B1) to (B4)), and (C) water, and by making the total amount of components (A) to (C) 90% by mass or more, an oily particle dispersion composition with excellent dispersion stability (25°C) can be obtained (Evaluations 1 and 5). Furthermore, as shown in Tables 1 to 3, it was found that the shape of the dispersed oily particles was close to spherical (Evaluation 3). In addition, among component (A), it was found that glyceryl stearate and glyceryl behenate in particular can be preferably used to obtain oily particles that easily disintegrate when force is applied (Examples 3 to 5, 7, 21, 26, 27, 30 and 32). Furthermore, as can be seen from Examples 1 to 33, it was found that compositions containing dispersed oily particles that easily disintegrate when force is applied, and compositions containing dispersed oily particles that do not easily disintegrate when force is applied and have a granular texture can be easily manufactured according to the purpose. Thus, according to this disclosure, the hardness and disintegration properties of the particles can be easily changed. For example, if hard, disintegration-resistant oily particles are used, they can be preferably applied to scrubbing agents, fragrances, insect repellents for clothing, and the like.

[0120] Furthermore, it has been found that, according to this disclosure, an oily particle dispersion composition can be easily obtained without requiring complicated processes such as shearing. It has also been found that the oily particles in the composition have good dispersion stability at least from 0 to 50°C (Evaluations 6 and 7). It has also been found that good dispersibility can be maintained even when the dispersion medium is removed (Evaluations 8 and 9). Therefore, the composition produced in this way may be used after removing the dispersion medium, and the obtained oily particles can also be used after being mixed with another liquid or the like.

Claims

1. An oily particle dispersion composition having the following characteristics: (A) At least two solid oils selected from the group consisting of (behenate / eicosanedioic acid) glyceryl, behenyl alcohol, tri(behenate / isostearate / eicosanedioic acid) glyceryl, octadeca(behenate / hydroxystearate) polyglyceryl-20, rice bran wax, glyceryl stearate, and glyceryl behenate. (B) Amphiphilic substances, and (C) Contains water, In the oily particle dispersion composition, The total amount of components (A) to (C) is 90% by mass or more. The total amount of component (A) is 5 to 40% by mass. The amount of component (B) is 0.1 to 80 parts by mass per 100 parts by mass of component (A). Component (B) is at least one selected from the group consisting of (B1) to (B4) below. (B1) At least one divalent carboxylic acid ester selected from the group consisting of cyclohexane-1,4-dicarboxylic acid bisethoxydiglycol and (eicosanedioic acid / tetradecanediic acid) decaglyceryl, (B2) At least one alkylene oxide derivative selected from the group consisting of PPG-10 methyl glucose, methyl gluceth-20, methyl gluceth-10, glycereth-26, PPG-9 diglyceryl, and PPG-14 polyglyceryl-2 ether. (B3) At least one selected from the group consisting of 1,3-butylene glycol, pentylene glycol, isopentyl diol, propylene glycol, dipropylene glycol, PEG-6 and PEG-8. (B4) At least one nonionic surfactant with an HLB of 3.5 or higher, selected from the group consisting of POE fatty acid esters, polyglyceryl-2 stearate, polyglyceryl-2 isostearate, polyglyceryl-4 stearate, polyglyceryl-10 stearate, polyglyceryl-10 distearate, polyglyceryl-10 tristearate, polyglyceryl-10 pentastearate, polyglyceryl-10 laurate, polyglyceryl-10 myristate, and polyglyceryl-10 oleate.

2. The oily particle dispersion composition according to claim 1, wherein the total amount of component (A) and component (B) in the composition is 8 to 60% by mass.

3. Oily particles that are removed from the dispersion medium of the oily particle dispersion composition described in claim 1.

4. An oily particle formulation comprising the oily particle dispersion composition described in claim 1 or the oily particles described in claim 3.

5. A method for producing an oily particle dispersion composition, comprising the following steps: Step (1) A step of mixing (A) at least two solid oils selected from the group consisting of (behenate / eicosanedioic acid) glyceryl, behenyl alcohol, tri(behenate / isostearate / eicosanedioic acid) glyceryl, octadeca(behenate / hydroxystearate) polyglyceryl-20, rice bran wax, glyceryl stearate and glyceryl behenate with (B) an amphiphilic substance to obtain a mixed solution at a temperature above the melting point of component (A), and Step (2) A step of granulating oily particles by adding the mixture and water (C) at a temperature above the melting point of component (A), while stirring the resulting mixture to a temperature below the melting point of component (A). Here, the oily particle dispersion composition is It contains ingredients (A) to (C), In the composition, the total amount of components (A) to (C) is 90% by mass or more. The total amount of component (A) is 5 to 40% by mass. The amount of component (B) is 0.1 to 80 parts by mass per 100 parts by mass of component (A). Component (B) is at least one selected from the group consisting of (B1) to (B4) below. (B1) At least one divalent carboxylic acid ester selected from the group consisting of cyclohexane-1,4-dicarboxylic acid bisethoxydiglycol and (eicosanedioic acid / tetradecanediic acid) decaglyceryl, (B2) At least one alkylene oxide derivative selected from the group consisting of PPG-10 methyl glucose, methyl gluceth-20, methyl gluceth-10, glycereth-26, PPG-9 diglyceryl, and PPG-14 polyglyceryl-2 ether. (B3) At least one selected from the group consisting of 1,3-butylene glycol, pentylene glycol, isopentyl diol, propylene glycol, dipropylene glycol, PEG-6 and PEG-8. (B4) At least one nonionic surfactant with an HLB of 3.5 or higher, selected from the group consisting of POE fatty acid esters, polyglyceryl-2 stearate, polyglyceryl-2 isostearate, polyglyceryl-4 stearate, polyglyceryl-10 stearate, polyglyceryl-10 distearate, polyglyceryl-10 tristearate, polyglyceryl-10 pentastearate, polyglyceryl-10 laurate, polyglyceryl-10 myristate, and polyglyceryl-10 oleate.

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