Oily solids

Abstract

The present invention provides an oily solid composition containing a high concentration of at least one active ingredient selected from the group consisting of ascorbic acid, a salt of ascorbic acid, or a water-soluble derivative, which exhibits excellent inhibitory effect on precipitation of the active ingredient in the oil phase and uniform dispersibility, and is easy to apply to the skin, as it breaks down moderately and spreads easily while maintaining stability as a formulation. [Solution] The following components (A) to (D); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass An oily solid composition containing [the specified ingredient].

Description

Technical Field

[0001] The present invention relates to an oily solid composition.

Background Art

[0002] The skin develops wrinkles, sagging, pigmentation such as spots and freckles due to internal factors such as aging and stress, and external factors such as ultraviolet rays and air dryness. Among these, morphological changes such as wrinkles and sagging, and visual changes such as pigmentation greatly affect the impression of appearance. Therefore, many people hope for improvement, and various products are provided.

[0003] Ascorbic acid and its water-soluble derivatives are used as active ingredients for preventing and improving wrinkles, sagging, and pigmentation. Ascorbic acid and its water-soluble derivatives (for example, ascorbic acid glucoside, etc.) have an inhibitory effect on melanin production, a promoting effect on collagen production, and an antioxidant effect. Therefore, they have been used in cosmetics as whitening ingredients, anti-wrinkle ingredients, and anti-aging ingredients. However, since ascorbic acid is easily oxidized and decomposed, various techniques for stably formulating it into cosmetics have been studied. Since these active ingredients are powdery and water-soluble and are usually dissolved and formulated in a solvent such as water, it is difficult to formulate them into an oily composition mainly composed of an oil phase or an oil phase. Therefore, at present, there are still few techniques for uniformly and stably formulating ascorbic acid and its water-soluble derivatives into the oil phase in an oily composition.

[0004] Regarding these problems, for example, in an anhydrous oily solid skin external preparation containing one or more fine particles selected from ascorbic acid, ascorbate, and its water-soluble derivatives, and containing sucrose fatty acid ester and not containing polyhydric alcohol, a technique excellent in formulation stability and usability is disclosed (for example, see Patent Document 1). Also, in an oily cosmetic containing retinol, at least one compound selected from the group consisting of ascorbic acid and salts of ascorbic acid, spherical powder having a refractive index of 1.6 or less in a specific amount, and an oil agent, a technique excellent in the effect of hiding wrinkles is disclosed (for example, see Patent Document 2). [Prior art documents] [Patent Documents]

[0005] [Patent Document 1] Japanese Patent Publication No. 2006-213738 [Patent Document 2] Japanese Patent Publication No. 2021-001154 [Overview of the Initiative] [Problems that the invention aims to solve]

[0006] As mentioned earlier, there are still few technologies for uniformly and stably incorporating ascorbic acid and its water-soluble derivatives into the oil phase. However, in contrast to this situation, the market demands oily compositions (oily cosmetics or topical skin preparations) with various functionalities and textures. In particular, there is growing demand for oily solid compositions that can be developed into balm or stick formulations due to their portability and ease of use. Therefore, to meet these needs, there is a need for the development of new technologies for oily solid compositions that maintain uniform dispersion of the active ingredient in the oil phase while achieving formulation stability, functionality, and a good texture. In the technology disclosed in Patent Document 1, while the stability (residual rate) of the ascorbic acid derivative is excellent, the case where the ascorbic acid derivative is included in a high concentration was not investigated. Furthermore, the dispersion state of the ascorbic acid derivative in the oily solid composition was not mentioned, and the ease of application to the skin, such as being able to break down appropriately and spread while maintaining a solid shape, was sometimes insufficient. Furthermore, the technology disclosed in Patent Document 2 did not consider the case where ascorbic acid derivatives were included in high concentrations, and there were cases where the stability, dispersibility, and ease of application to the skin of ascorbic acid and its water-soluble derivatives were insufficient.

[0007] Therefore, the present invention aims to develop an oily solid composition that contains a high concentration of at least one active ingredient selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, which exhibits excellent precipitation suppression effect and uniform dispersibility of the active ingredient in the oil phase, maintains the stability of the formulation as a solid, yet crumbles moderately and spreads easily, resulting in excellent ease of application to the skin. [Means for solving the problem]

[0008] In view of the above circumstances, the inventors, after diligent study, have found that the above problems can be solved with an oily solid composition containing at least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, wax, a liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which a branched fatty acid and a polyhydric alcohol having a trivalent or higher hydroxyl group are esterified, and anhydrous silicic acid, with each component present in a specific amount, and have completed the present invention.

[0009] In other words, the present invention provides the following: [1] The following components (A) to (D); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass It is an oily solid composition containing [the specified ingredient]. [2] The oily solid composition is as described in [1], wherein component (A) is ascorbic acid. [3] The oily solid composition according to [1] or [2] is wherein component (C) is a liquid oil obtained by esterifying a branched-chain fatty acid having 14 to 22 carbon atoms with a polyhydric alcohol having three or more hydroxyl groups selected from the group consisting of glycerin, polyglycerin, and pentaerythritol. [4] The oily solid composition is as described in [1] or [2], wherein the mass ratio (C) / (A) of component (C) to component (A) is 0.8 to 1.7. [5] Furthermore, the oily solid composition according to [1] or [2] contains component (E) a non-volatile diester oil (excluding component (C)). [6] The oily solid composition according to [5], wherein component (E) is one or more selected from diethylhexyl succinate, diisostearyl malate, and propylene glycol dicaprate. [7] It is an oily solid composition described in [1] or [2], which is a cosmetic or a topical skin preparation. [8] The following components (A) to (D); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass A method for producing an oily solid composition containing, (Step 1) A step of preparing a mixture of an oily component containing part or all of component (A) and component (C) such that component (A) accounts for 20 to 80% by mass of the total amount of the mixture. (Step 2) Step of kneading the mixture from Step 1. (Step 3) A step in which the mixture from Step 2 and the remaining ingredients are heated and mixed. This is a method for producing an oily solid composition containing [a specific ingredient]. [Effects of the Invention]

[0010] The present invention relates to an oily solid composition highly containing at least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives as an active ingredient, which is excellent in the effect of suppressing precipitation of the active ingredient in the oil phase and has uniform dispersibility, and is excellent in the ease of application to the skin while maintaining the stability as a preparation, and can be appropriately spread while crumbling.

Embodiments for Carrying Out the Invention

[0011] Hereinafter, preferred embodiments for carrying out the present invention will be described. The embodiments described below show an example of a typical embodiment of the present invention, and the scope of the present invention is not construed narrowly thereby. In the present specification, percentages are shown by mass unless otherwise specified. Also, the upper limit value (hereinafter) and the lower limit value (above) of each numerical range (~) can be arbitrarily combined as desired. In the present specification, "X~Y" indicating a range includes X and Y and means "X or more and Y or less".

[0012] (Component (A): At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives)

[0013] Component (A) used in the present invention is at least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives. Among them, in the present invention, it is more preferable to use ascorbic acid.

[0014] The ascorbic acid of component (A) used in the present invention may be any of D-form, L-form, and DL-form, but it is preferably L-form (L-ascorbic acid). As ascorbic acid, commercially available products can be used. Examples of commercially available products of ascorbic acid include ascorbic acid ultrafine powder (component name: L-ascorbic acid: manufactured by DSM) and the like.

[0015] Specific examples of water-soluble derivatives of ascorbic acid, component (A) used in the present invention, include, for example, L-ascorbic acid phosphate salts such as L-ascorbic acid phosphate ester, L-ascorbic acid phosphate sodium salt, L-ascorbic acid phosphate potassium salt, L-ascorbic acid phosphate calcium salt, L-ascorbic acid phosphate magnesium salt, and L-ascorbic acid phosphate triethanolamine salt, as well as water-soluble ascorbic acid active derivatives such as L-ascorbic acid sulfate, L-ascorbic acid sulfate salt, and L-ascorbic acid-2-glucoside. Among these, L-ascorbic acid-2-glucoside, which has a high whitening effect, is more preferred as a water-soluble derivative of ascorbic acid.

[0016] In the present invention, it is preferable to atomize component (A). Specifically, the average particle size of component (A) is preferably 300 μm or less as an upper limit, more preferably 250 μm or less, and even more preferably 200 μm or less, from the viewpoint of suppressing precipitation of component (A) and dispersibility. There is no particular lower limit, but for example, 0.1 μm or more is preferred, 1 μm or more is more preferred, and 5 μm or more is even more preferred.

[0017] In this invention, the average particle size of component (A) can be measured using an optical microscope. Specifically, an appropriate amount of the sample is placed on a slide glass at room temperature, the sample is sandwiched between cover slips and observed, the major axis of any 20 samples is measured, and the average value is calculated to determine the average particle size. In this invention, the shape of component (A) includes not only spherical and nearly spherical shapes, but also flattened, spindle-shaped, polyhedral, fibrous shapes, and irregular shapes.

[0018] While either a wet or dry method can be used to atomize component (A), it is preferable to use a wet method to avoid deterioration of component (A). Specifically, methods for kneading (grinding) component (A) include, for example, a roll mill (3-roller), a pressure kneader, an extruder, a ball mill, and a bead mill.

[0019] In the present invention, when micronizing component (A), from the viewpoint of suppressing the precipitation of component (A) and dispersibility, it is preferable to knead (grind) a mixture containing component (A) and some or all of the components other than component (A), and more preferably to knead (grind) a mixture containing component (A) and some of the components other than component (A). In particular, the components other than component (A) are preferably a part of component (C), more preferably a part of component (C) and a part of component (B) or a part of component (E), and even more preferably three components: a part of component (C), a part of component (B), and a part of component (E). Component (D) may be contained in the mixture. From the viewpoint of suppressing the precipitation of component (A) and dispersibility, the content of component (A) in the mixture is preferably 20 to 80% by mass (hereinafter, "mass%" will be simply abbreviated as "%"), more preferably 30 to 70%, and even more preferably 35 to 65% of the total amount of the mixture.

[0020] The content of component (A) in this invention is preferably 27% or more, and more preferably 30% or more, from the viewpoint of inhibiting the precipitation of component (A) and ease of application to the skin. The upper limit is preferably 40% or less, preferably 38% or less, and more preferably 35% or less, from the viewpoint of inhibiting the precipitation of component (A), dispersibility, and formulation stability. This range is preferable because it provides excellent precipitation inhibition and dispersibility of component (A), allows component (A) to exert its various skin effects, and provides superior formulation stability and ease of application.

[0021] In this invention, the content of component (A) is 25-40%, preferably 27-40%, more preferably 30-40%, even more preferably 27-38%, and even more preferably 30-35%. This range is preferable because it provides excellent precipitation inhibition and dispersibility of component (A), allows component (A) to exert its various skin effects, and also provides superior formulation stability and ease of application.

[0022] (Ingredient (B) Wax)

[0023] The component (B) wax used in the present invention is not particularly limited as long as it is used in cosmetics or topical skin preparations, and can be hydrocarbon-based, ester-based, natural, or synthetic. Specifically, examples include hydrocarbon waxes such as paraffin wax, ceresin wax, ozokerite wax, microcrystalline wax, ethylene-propylene copolymer, Fischer-Tropsch wax, and polyethylene wax, and polar waxes such as candelilla wax, carnauba wax, rice wax, beeswax, Japanese wax, and gay wax. One or more of these can be used.

[0024] In the present invention, component (B) is preferably a hydrocarbon wax, and among these, paraffin wax, microcrystalline wax, ethylene-propylene copolymer, and polyethylene wax are more preferred. Furthermore, in the present invention, it is preferable to use microcrystalline wax and / or polyethylene wax, and from the viewpoint of formulation stability and ease of application to the skin, it is more preferable to use microcrystalline wax and polyethylene wax.

[0025] The lower limit of the content of component (B) in the present invention is 5% or more, preferably 6% or more, more preferably 8% or more, and even more preferably 10% or more, from the viewpoint of inhibiting the precipitation of component (A), dispersibility, and formulation stability. The upper limit is 20% or less, preferably 18% or less, more preferably 16% or less, and even more preferably 15% or less, from the viewpoint of inhibiting the precipitation of component (A), dispersibility, and ease of application to the skin. This range is preferable because it provides excellent precipitation inhibition and dispersibility of component (A), allows component (A) to exert its various skin effects, and further improves formulation stability and ease of application.

[0026] In the present invention, the content of component (B) is 5 to 20%, preferably 6 to 18%, more preferably 8 to 16%, and even more preferably 10 to 15%. This range is preferable because it provides excellent dispersibility of component (A), allowing the active ingredient to exert various skin effects, while also providing excellent inhibition of precipitation and dispersibility of component (A), allowing the various skin effects of component (A) to be exerted, as well as superior formulation stability and ease of application.

[0027] (Component (C): A liquid oil in which branched-chain fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, with a viscosity of 200 mPa·s or higher at 25°C.)

[0028] Component (C) used in the present invention is an oil obtained by esterifying a branched-chain fatty acid with a polyhydric alcohol having three or more hydroxyl groups, and is a liquid oil with a viscosity of 200 mPa·s or higher at 25°C. Here, a liquid oil is defined as one that has fluidity at 25°C.

[0029] In the present invention, component (C) is a liquid oil with a viscosity of 200 mPa·s or more at 25°C. While there are no particular upper limits on viscosity, it is preferably 7,000 mPa·s or less, more preferably 6,000 mPa·s or less, even more preferably 5,000 mPa·s or less, even more preferably 4,000 mPa·s or less, even more preferably 3,000 mPa·s or less, and particularly preferably 2,000 mPa·s or less. Viscosity measurement is not particularly limited and can be performed using known methods.

[0030] In the present invention, the fatty acid of component (C) is a branched-chain fatty acid, preferably a branched-chain fatty acid having 14 to 22 carbon atoms, more preferably a branched-chain fatty acid having 16 to 20 carbon atoms, and even more preferably a branched-chain fatty acid having 16 to 18 carbon atoms, and isostearic acid is particularly preferred. Furthermore, the polyhydric alcohol of component (C) is a polyhydric alcohol having three or more hydroxyl groups, preferably a polyhydric alcohol having three or more hydroxyl groups selected from the group consisting of glycerin, polyglycerin, and pentaerythritol, more preferably a polyhydric alcohol having three or more hydroxyl groups selected from the group consisting of polyglycerin and pentaerythritol, and isostearic acid is particularly preferred. Examples of polyglycerins include polyglycerin-2 (also called diglycerin), polyglycerin-3 (also called triglycerin), polyglycerin-4 (also called tetraglycerin), and polyglycerin-5 (also called pentaglycerin). One or more of these can be selected and used, with one or more selected from polyglycerin-2 and polyglycerin-3 being preferred, and polyglycerin-2 being more preferred.Specifically, polyglyceryl-10 decaethylhexanoate (S-Face KEH-1010, manufactured by Sakamoto Pharmaceutical Co., Ltd., viscosity: 500 mPa·s), pentaerythrityl tetraisostearate (Saracos 5418, manufactured by Nisshin Oillio Group, viscosity: 420 mPa·s), polyglyceryl-2 monoisostearate (Cosmol 41V, manufactured by Nisshin Oillio Group, viscosity: 6540 mPa·s), polyglyceryl-2 diisostearate (Cosmol 42V, manufactured by Nisshin Oillio Group, viscosity: 750 mPa·s), polyglyceryl-2 triisostearate (Cosmol 41V, manufactured by Nisshin Oillio Group, viscosity: 350 mPa·s), polyglyceryl- Examples include 2 (Cossmall 44V, manufactured by Nisshin Oillio Group, viscosity: 275 mPa·s), and it is preferable to select one or more from pentaerythrityl tetraisostearate, polyglyceryl-2 diisostearate, polyglyceryl-2 triisostearate and polyglyceryl-2 tetraisostearate, more preferably one or more from polyglyceryl-2 diisostearate, polyglyceryl-2 triisostearate and polyglyceryl-2 tetraisostearate, and from the viewpoint of the dispersibility of component (A), polyglyceryl-2 triisostearate is even more preferred.

[0031] The content of component (C) in the present invention is preferably 50% or less, more preferably 45% or less, and more preferably 40% or less, from the viewpoint of inhibiting the precipitation of component (A), dispersibility, and formulation stability. There is no particular lower limit, but it is preferably 10% or more, more preferably 15% or more, even more preferably 20% or more, and particularly preferably 25% or more, from the viewpoint of inhibiting the precipitation of component (A), dispersibility, and ease of application to the skin. This range is preferable because it provides excellent precipitation inhibition and dispersibility of component (A), allows component (A) to exert various skin effects, and provides superior formulation stability and ease of application.

[0032] The content of component (C) in the present invention is 50% or less, preferably 10-50%, more preferably 15-50%, even more preferably 20-50%, even more preferably 25-50%, particularly preferably 25-45%, and most preferably 25-40%. This range is preferable because it provides excellent precipitation inhibition and dispersibility of component (A), allows component (A) to exert its various skin effects, and also provides superior formulation stability and ease of application.

[0033] In the present invention, the mass ratio (C) / (A) of component (C) to component (A) is not particularly limited, but as a lower limit, it is preferably 0.8 or higher, more preferably 0.85 or higher, and even more preferably 0.9 or higher, and even more preferably 1.0 or higher, from the viewpoint of the dispersibility of component (A) and ease of application to the skin. Furthermore, as an upper limit, from the viewpoint of the precipitation inhibition effect of component (A), dispersibility, and formulation stability, it is preferably 1.7 or lower, more preferably 1.6 or lower, even more preferably 1.5 or lower, and even more preferably 1.4 or lower. This range is preferable because it provides excellent precipitation inhibition and dispersibility of component (A), allows component (A) to exhibit various skin effects, and provides superior formulation stability and ease of application.

[0034] In the present invention, the mass ratio (C) / (A) of component (C) to component (A) is not particularly limited, but is preferably 0.8 to 1.7, more preferably 0.85 to 1.6, even more preferably 0.9 to 1.5, and particularly preferably 1.0 to 1.4. This range is preferable because it provides excellent precipitation suppression and dispersibility of component (A), allows component (A) to exhibit various skin effects, and provides superior formulation stability and ease of application.

[0035] (Component (D) Anhydrous silicic acid)

[0036] The component (D) anhydrous silicic acid used in the present invention is not particularly limited as long as it is commonly used in cosmetics or topical skin preparations. However, from the viewpoint of having excellent dispersibility of component (A) and excellent formulation stability, a specific surface area of ​​80 m² is preferred. 2Preferably 100m / g or more 2 It is more preferable that the amount is 1 / g or more, and it is particularly preferable that it is in a fuzzy, non-porous, anhydrous form of silicic acid.

[0037] In the present invention, it is preferable that component (D) is hydrophobized anhydrous silicic acid. While not particularly limited, examples of hydrophobization treatments include dimethyldichlorosilane (dimethylsilyl) treatment, hexamethyldisilazane (trimethylsilyl) treatment, octylsilane treatment, dimethylsilylation treatment, coating and baking treatment using methylhydrogenpolysiloxane, and coating with metal soap. Dimethylsilylated anhydrous silicic acid is more preferable, and in the present invention, fuming dimethylsilylated anhydrous silicic acid is even more preferable. Examples of commercially available products include AEROSIL R972 (dimethylsilylated, fuming, specific surface area: 110 m²). 2 / g), AEROSIL RX300 (trimethylsilylated, fume, specific surface area 210±20m²) 2 / g, hexamethyldisilazane treated) (manufactured by Nippon Aerosil Co., Ltd.) AEROSIL RX200 (trimethylsilylated, fume, specific surface area 140±25m²) 2 Examples include / g) (manufactured by Nippon Aerosil Co., Ltd.).

[0038] The content of component (D) in the present invention is preferably 0.5% or more, with a lower limit of 0.1% or more, from the viewpoint of formulation stability and ease of application to the skin. The upper limit is preferably 3% or less, with a lower limit of 2.5% or less, and a higher limit of 2% or less, from the viewpoint of the precipitation inhibition effect of component (A), dispersibility, and ease of application to the skin. This range is preferable because it provides excellent precipitation inhibition and dispersibility of component (A), allows component (A) to exert its various skin effects, and further improves formulation stability and ease of application.

[0039] The content of component (D) in the present invention is 0.1 to 3%, preferably 0.5 to 2.5%, and more preferably 0.5 to 2%. This range is preferable because it provides excellent precipitation inhibition and dispersibility of component (A), allows component (A) to exert its various skin effects, and also provides superior formulation stability and ease of application.

[0040] (Component (E): Non-volatile diester oil)

[0041] Furthermore, it is preferable to further include a non-volatile diester oil, component (E), from the viewpoint of having excellent precipitation suppression and dispersibility effects of component (A), as well as increasing strength and improving the formulation stability of the oily solid composition. Here, a diester is a substance having two ester bonds in its structure, and examples include diesters of fatty acids and polyhydric alcohols, diesters of organic acids and alcohols, and diesters of dicarboxylic acids and alcohols. Non-volatility means that it does not volatilize at 25°C, and for example, refers to substances with a boiling point of 260°C or higher at atmospheric pressure. In the present invention, component (E) is the same as component (C), and specifically includes ethylene glycol di2-ethylhexanoate, ethylene glycol dioleate, propylene glycol dicaprylate, di(caprylic / capric acid)propylene glycol, propylene glycol dicaprate, propylene glycol dioleate, diethylhexyl succinate, diisostearyl malate, diethylhexyl succinate, di2-ethylhexyl adipate, diisopropyl sebacate, di2-ethylhexyl sebacate, and dibutyloctyl sebacate. Among these, branched diester oils are preferred in the present invention, with one or more selected from diethylhexyl succinate, diisostearyl malate, and propylene glycol dicaprate being more preferred, and diisostearyl malate being even more preferred. For example, commercially available products such as Kurodamol OSU (ingredient: diethylhexyl succinate, manufactured by Croda Japan Co., Ltd.), Cosmol 222 (ingredient: diisostearyl malate, manufactured by Nisshin Oillio Co., Ltd.), and Nikkol PDD (ingredient: propylene glycol dicaprate, manufactured by Nippon Surfactant Industry Co., Ltd.) are preferably used.

[0042] The content of component (E) in the present invention is not particularly limited, but preferably at a lower limit of 1% or more, more preferably at 3% or more, even more preferably at 5% or more, even more preferably at 7% or more, and particularly preferably at 10% or more. Furthermore, preferably at an upper limit of 40% or less, more preferably at 35% or less, and even more preferably at 30% or less. This range is preferable because it provides excellent precipitation suppression and dispersibility of component (A), allows component (A) to exert its various skin effects, and provides superior ease of application.

[0043] The content of component (E) in the present invention is preferably 1 to 40%, more preferably 3 to 35%, even more preferably 5 to 30%, even more preferably 7 to 30%, and particularly preferably 10 to 30%. This range is preferable because it provides excellent precipitation inhibition and dispersibility of component (A), allows component (A) to exert its various skin effects, and also provides superior formulation stability and ease of application.

[0044] In the present invention, the mass ratio of component (A) to component (E), (A) / (E), is not particularly limited, but is preferably 0.8 or higher as a lower limit, more preferably 0.9 or higher, and even more preferably 1.0 or higher from the viewpoint of formulation stability, etc. Furthermore, is preferably 5.0 or lower as an upper limit, more preferably 4.3 or lower, even more preferably 4.0 or lower, even more preferably 3.5 or lower, and particularly preferably 3.0 or lower. This range is preferable because it provides excellent precipitation suppression and dispersibility of component (A), allows component (A) to exhibit various skin effects, and provides superior formulation stability and ease of application.

[0045] In the present invention, the mass ratio (A) / (E) of component (A) to component (E) is not particularly limited, but is preferably 0.8 to 5.0, more preferably 0.9 to 4.3, even more preferably 0.9 to 4.0, even more preferably 0.9 to 3.5, and particularly preferably 1.0 to 3.0. This range is preferable because it provides excellent precipitation suppression and dispersibility of component (A), allows component (A) to exhibit various skin effects, and provides superior formulation stability and ease of application.

[0046] In the oily solid composition of the present invention, it is preferable that the composition is substantially free of polyhydric alcohols from the viewpoint of the dispersibility of component (A) in the oil phase. The presence of polyhydric alcohols causes differences in specific gravity in the oily solid composition, resulting in uneven dispersion of component (A) and raising concerns about concentration gradients in the composition. In the present invention, "substantially free of polyhydric alcohols" means that the amount of polyhydric alcohols does not affect the dispersibility of component (A) due to their presence, and specifically, the content is 1% or less. Here, the polyhydric alcohols are not particularly limited as long as they are commonly used in cosmetics or topical skin preparations, but examples include propylene glycol, 1,3-butylene glycol, dipropylene glycol, glycerin, diglycerin, polyglycerin, sorbitol, maltitol, polyethylene glycol, and the like.

[0047] In the present invention, in addition to the above components (A) to (E), any other components commonly found in cosmetics or topical skin preparations, such as water, surfactants, oils, UV absorbers, antioxidants, inorganic salts, organic salts, metal chelating agents, preservatives, powders, dyes, fragrances, and various other agents, may be included as long as they do not impair the effects of the present invention. Examples of such components include the following.

[0048] Examples of surfactants include nonionic surfactants, anionic surfactants, cationic surfactants, and amphoteric surfactants. For example, these include glycerin fatty acid esters and their alkylene glycol adducts, polyglycerin fatty acid esters and their alkylene glycol adducts, sorbitan fatty acid esters and their alkylene glycol adducts, sucrose fatty acid esters, polyoxyethylene hydrogenated castor oil, polyoxyalkylene alkyl copolymerized organopolysiloxanes, polyether-modified organopolysiloxanes, phospholipids, etc., and one or more of these can be used.

[0049] Examples of UV absorbers include benzophenone-based, para-aminobenzoic acid-based, cinnamic acid-based, salicylic acid-based, 4-tert-butyl-4'-methoxydibenzoylmethane, and oxybenzone.

[0050] As for the oily component, any oily component other than components (B), (C), and (E) can be used, such as higher alcohols, hydrocarbon oils, ester oils, fats and oils, and silicone oils. Specifically, examples include higher alcohols such as oleyl alcohol and octyldodecanol; fatty acids such as isostearic acid and oleic acid; hydrocarbon oils such as polybutene, hydrogenated polydecene, hydrogenated polyisobutene, α-olefin oligomers, mineral oil, and squalane; ester oils such as propylene glycol dicaprate, isotridecyl isononanoate, cetyl 2-ethylhexanoate, alkyl (C12-15) benzoate, glyceryl tri-2-ethylhexanoate, trimethylolpropane triethylhexanoate, and tri(caprylic / capric acid) glyceryl; vegetable oils such as palm oil, palm kernel oil, olive oil, safflower oil, soybean oil, and cottonseed oil; animal oils such as liver oil and egg yolk oil; and silicone oils such as methylpolysiloxane, methylphenylpolysiloxane, and decamethylcyclopentasiloxane.

[0051] Examples of antioxidants include α-tocopherol, dibutylhydroxytoluene, and butylhydroxyanisole.

[0052] Examples of preservatives include benzoic acid, salicylic acid, carbolic acid, sorbic acid, parahydroxybenzoic acid esters, benzalkonium chloride, chlorhexidine chloride, trichlorocarbanilide, photosensitizer, and phenoxyethanol.

[0053] The powder components are powders other than component (D), and are not particularly limited in terms of shape (plate-like, spindle-like, needle-like, etc.), particle size, particle structure (porous, non-porous, etc.), etc. Examples include inorganic powders, lustrous powders, organic powders, and composite powders. Specifically, these include inorganic powders such as titanium dioxide, zinc oxide, aluminum oxide, cerium oxide, magnesium oxide, zirconium oxide, magnesium carbonate, calcium carbonate, chromium oxide, chromium hydroxide, aluminum silicate, magnesium silicate, aluminum magnesium silicate, mica, synthetic mica, synthetic sericite, sericite, talc, kaolin, silicon carbide, barium sulfate, and boron nitride, as well as bismuth oxychloride, titanium mica, anhydrous silica-coated titanium mica, titanium dioxide-coated glass powder, titanium dioxide / iron oxide-coated glass powder, and titanium dioxide / anhydrous silica-coated glass powder. Examples include glittering powders such as coated glass powder and aluminum powder, organic powders such as N-acyllysine and nylon, composite powders such as fine-particle titanium oxide-coated titanium mica, fine-particle zinc oxide-coated titanium mica, barium sulfate-coated titanium mica, titanium oxide-containing silicon dioxide, and zinc oxide-containing silicon dioxide, as well as polyethylene terephthalate-aluminum-epoxy laminated powder, polyethylene terephthalate-polyolefin laminated film powder, and polyethylene terephthalate-polymethyl methacrylate laminated film powder, and one or more of these can be used. Furthermore, these powders may be composites of one or more of these, and may be surface-treated by known methods using fluorine compounds, silicone-based oils, metal soaps, waxes, surfactants, oils and fats, hydrocarbons, etc.

[0054] The oily solid composition of the present invention possesses sufficient hardness to maintain the stability (solid shape) of the formulation, yet it crumbles moderately and spreads easily, making it excellent for application to the skin. For example, when used on areas of concern such as wrinkles and blemishes around the mouth and eyes, it can be used to visually conceal wrinkles and blemishes while also providing an excellent improvement effect on these skin concerns through the active ingredients. In the present invention, while exhibiting various skin effects of the active ingredients, the strength (cutter load) is preferably 50 to 100 g, and more preferably 60 to 95 g, from the viewpoint of formulation stability and ease of application to the skin. Here, the strength (cutter load) can be calculated by leaving three samples of each type at 35°C for one hour, measuring the maximum cutter load under the following conditions, and calculating the average cutter load of the three samples. Measuring instrument: FUDOH RHEOMETER RT-2002D·D (manufactured by Rheotech) Speed: 6cm / m Adapter: Piano wire Measurement section: Extend the device to its maximum length from the container and measure 12 mm from the base of the container.

[0055] (Manufacturing method) The oily solid composition of the present invention can be manufactured by conventional methods, and any general dispersion equipment such as a dispersion device can be used as the manufacturing equipment. For example, it can be obtained by heating and mixing components (A) to (E), uniformly mixing them with a dispersion device, and then heating and filling as necessary. In the present invention, for example, dispersion equipment such as a paddle mixer or a dispersion device can be used as the mixing method.

[0056] In the present invention, it is preferable to heat and mix components (A) to (E) and then further knead them. As for the kneading method, for example, a roll mill (3-roller), a pressure kneader, an extruder, a ball mill, or a bead mill can be used.

[0057] In the present invention, from the viewpoint of inhibiting the precipitation of component (A) and dispersibility, the following manufacturing method (I) or (II) is more preferable. Manufacturing method (I) involves the following ingredients (A) to (D); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass A method for producing an oily solid composition containing, (Step 1) A step of preparing a mixture of an oily component containing part or all of component (A) and component (C) such that component (A) accounts for 20 to 80% by mass of the total amount of the mixture. (Step 2) Step of kneading the mixture from Step 1. (Step 3) A step in which the mixture from Step 2 and the remaining ingredients are heated and mixed. This is a method for producing an oily solid composition containing [a specific ingredient]. Furthermore, the manufacturing method (II) is as follows: (A)~(E); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass (E) Non-volatile diester oil A method for producing an oily solid composition containing, (Step 1) A step of preparing a mixture of an oily component containing part or all of component (A), component (C), and component (E), such that component (A) accounts for 20 to 80% by mass of the total amount of the mixture. (Step 2) Step of kneading the mixture from Step 1. (Step 3) A step in which the mixture from Step 2 and the remaining ingredients are heated and mixed. This is a method for producing an oily solid composition containing [a specific ingredient].

[0058] The oily solid composition of the present invention is preferably in the form of a balm or stick, and more preferably in the form of a stick, due to its portability and ease of use.

[0059] The oily solid composition of the present invention may be used as is as the final formulation, or it may be used as part of a final formulation mixed with other components. Examples of the final formulation include topical skin preparations such as pharmaceuticals and cosmetics, such as topical solid preparations, topical liquid preparations, sprays, ointments, creams, gels, patches, lotions, cosmetic oils, serums, face packs, massage cosmetics, makeup bases, body cosmetics, and hair cosmetics. In the present invention, the final formulation is preferably a cosmetic or a topical skin preparation.

[0060] The content of the oily solid composition of the present invention contained in the aforementioned cosmetic or topical skin preparation is not particularly limited, but is preferably 20 to 100%.

[0061] The aforementioned cosmetic or topical skin preparation is preferably in the form of a balm or stick, and more preferably in the form of a stick, due to its portability and ease of use.

[0062] Furthermore, the present invention may also employ the following configuration. <1> The following components (A) to (D); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass It is an oily solid composition containing [the specified ingredient]. <2> The oily solid composition is as described in <1>, wherein component (A) is ascorbic acid. <3> The oily solid composition according to <1> or <2> is an oily solid composition according to <1> or <2>, wherein component (C) is a liquid oil obtained by esterifying a branched-chain fatty acid having 14 to 22 carbon atoms with a polyhydric alcohol having three or more hydroxyl groups selected from the group consisting of glycerin, polyglycerin, and pentaerythritol. <4> The oily solid composition is one of the following (1) to (3), wherein the mass ratio (C) / (A) of component (C) to component (A) is 0.8 to 1.7. <5> The oily solid composition is as described in any one of (1) to (4), wherein component (C) is at least one selected from the group consisting of pentaerythrityl tetraisostearate, polyglyceryl-2 diisostearate, polyglyceryl-2 triisostearate, and polyglyceryl-2 tetraisostearate. <6> Furthermore, the oily solid composition is one of the following: (E) a non-volatile diester oil (excluding component (C)). <7> The oily solid composition according to <6> is wherein component (E) is one or more selected from diethylhexyl succinate, diisostearyl malate, and propylene glycol dicaprate. <8> The oily solid composition according to <6> or <7>, wherein the mass ratio (A) / (E) of component (A) to component (E) is 0.8 to 5.0. <9> The oily solid composition is one of the following (1) to (9), wherein the average particle size of component (A) is 200 μm or less. <10> It is an oily solid composition described in any one of (1) to (9), which is a cosmetic or a topical skin preparation. <11> The following components (A) to (D); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass A method for producing an oily solid composition containing, (Step 1) A step of preparing a mixture of an oily component containing part or all of component (A) and component (C) such that component (A) accounts for 20 to 80% by mass of the total amount of the mixture. (Step 2) Step of kneading the mixture from Step 1. (Step 3) A step in which the mixture from Step 2 and the remaining ingredients are heated and mixed. This is a method for producing an oily solid composition containing [a specific ingredient]. <12> The following components (A) to (D); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass A method for producing an oily solid composition containing, (Step 1) A step of preparing a mixture of an oily component containing component (A) and a portion of component (C) such that component (A) accounts for 20 to 80% by mass of the total amount of the mixture. (Step 2) Step of kneading the mixture from Step 1. (Step 3) A step in which the mixture from Step 2 and the remaining ingredients are heated and mixed. This is a method for producing an oily solid composition containing [a specific ingredient]. <13> The following components (A) to (E); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass (E) Non-volatile diester oil A method for producing an oily solid composition containing, (Step 1) A step of preparing a mixture of an oily component containing part or all of component (A), component (C), and component (E), such that component (A) accounts for 20 to 80% by mass of the total amount of the mixture. (Step 2) Step of kneading the mixture from Step 1. (Step 3) A step in which the mixture from Step 2 and the remaining ingredients are heated and mixed. This is a method for producing an oily solid composition containing [a specific ingredient]. <14> The following components (A) to (E); (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25-40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or greater hydroxyl groups are esterified, comprising 50% or less by mass. (D) Anhydrous silicic acid 0.1-3% by mass (E) Non-volatile diester oil A method for producing an oily solid composition containing, (Step 1) A step of preparing a mixture of an oily component containing a portion of component (A), component (C), and component (E), such that component (A) accounts for 20 to 80% by mass of the total amount of the mixture. (Step 2) Step of kneading the mixture from Step 1. (Step 3) A step in which the mixture from Step 2 and the remaining ingredients are heated and mixed. This is a method for producing an oily solid composition containing [a specific ingredient]. [Examples]

[0063] The present invention will now be further explained with reference to examples. These examples are not intended to limit the present invention in any way.

[0064] <Examples 1-17 and Comparative Examples 1-11: Oil-based solid sticks> Oily solid sticks with the compositions shown in Tables 1 and 2 below were prepared by the manufacturing method described below. The precipitation inhibitory effect of component (A), the dispersibility of component (A), the formulation stability, and the ease of application to the skin were evaluated using the evaluation method and criteria described below, and the results are also shown in Tables 1 and 2.

[0065] [Table 1]

[0066] [Table 2] Note 1: Ascorbic acid (fine powder) (manufactured by DSM) Note 2: MULTIWAX W445 (manufactured by SONNEBORN, LLC) Note 3: PERFORMA SW-87 (manufactured by Japan Surfactant Industry Co., Ltd.) Note 4: BENTONE 27V (manufactured by Elementis) Note 5: Cosmoll 43V (manufactured by Nisshin Oillio Group Co., Ltd.) Note 6: Cosmoll 42V (manufactured by Nisshin Oillio Group Co., Ltd.) Note 7: Cosmoll 44V (manufactured by Nisshin Oillio Group Co., Ltd.) Note 8: KF-96A-350CS (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 9: AEROSIL R972 (smoky, non-porous, specific surface area: 110m 2 (Specific surface area per gram, manufactured by Nippon Aerosol Co., Ltd.)

[0067] (Manufacturing method) A: By uniformly mixing component (1) and some of components (2) to (11) at 100°C The mixture is prepared and then kneaded using a three-roller system. B: Mix component (12) and the remaining components (2) to (11) uniformly at 100°C. C: After mixing A and B, the mixture was heated to 90°C, filled into a stick container (12φ diameter), and allowed to cool at room temperature to obtain an oily solid stick. Here, the content of component (A) in the mixture of step A was set to 50%.

[0068] <Evaluation Method 1: Effect of inhibiting precipitation of component (A)> The precipitation-inhibiting effect of ingredient (A) was evaluated through a usage test conducted by a panel of 10 cosmetic evaluation specialists. Each panel member evaluated whether they felt any roughness (grittiness) due to precipitation when applying each sample to their skin, using the absolute evaluation scale described below on a 4-point scale. The average score was calculated from the sum of all panel members' scores and evaluated according to the 4-point evaluation criteria described below. [Absolute evaluation criteria] (Rating): (Evaluation Criteria) 4: I don't feel any roughness (crunchiness) at all. 3: You may feel a slight roughness (crunchiness), but it is very minor. 2: Slightly rough (crunchy) texture. 1: It feels very rough (crunchy). [4-level evaluation criteria] (Judgment) :(Judgment criteria) A (excellent): 3.5 points or more B (Good): 3.0 points or higher, less than 3.5 points C (Somewhat unacceptable): 2.0 points or higher, less than 3.0 points D (Not acceptable): Less than 2.0 points

[0069] <Evaluation Method 2: Dispersibility of Component (A)> Regarding the dispersibility of component (A), immediately after molding into a stick shape, the concentration of component (A) in each part of the stick (top, middle, bottom, center, and outer edge) was measured. The concentration of component (A) in the compositions shown in Tables 1 and 2 was set as 100%, and the concentration of component (A) in each part was compared with this value and judged according to the following four-stage evaluation criteria. [4-level evaluation criteria] (Judgment) :(Judgment criteria) A (Excellent): The concentration of component (A) in all parts is It is in the range of 98% to 100%. B (Good): The concentration of component (A) in any of the parts is It is in the range of 96% to less than 98%. C (Somewhat unacceptable): The concentration of component (A) in any of the parts is It is in the range of 90% to less than 96%. D (Not acceptable): Crystals of component (A) can be visually confirmed, The concentration of component (A) in any of the sites is less than 90%.

[0070] <Evaluation Method 3: Formulation Stability> Regarding formulation stability, when each sample was applied immediately after manufacturing, the degree to which the sample crumbled and the bulk remained on the skin as a clump was observed and judged according to the following four-level evaluation criteria. [4-level evaluation criteria] (Evaluation) : (Evaluation Criteria) A (Excellent): No bulk clumps remain on the skin during application. B (Good): A small amount of bulk may remain on the skin when applied, It is very minor. C (Somewhat unacceptable): It crumbles upon application, and the bulk remains on the skin in clumps. D (Not suitable): It crumbles easily during application, and the bulk remains on the skin in clumps. (Larger chunks than a C rating are observed, or the stick breaks)

[0071] <Evaluation Method 4: Ease of application to the skin> Regarding ease of application to the skin, each sample was tested by a panel of 10 cosmetic evaluation specialists. When each sample was applied to the skin, each panel member evaluated on a four-point scale using the absolute evaluation method below, assessing whether it spread easily, crumbled appropriately, and provided a smooth feel. The average score was calculated from the sum of all panel members' scores and judged according to the four-point evaluation criteria below. [Absolute evaluation criteria] (Rating) : (Evaluation Criteria) 4: Very good 3: Fairly good 2: Slightly bad 1: Very bad [4-level evaluation criteria] (Judgment) :(Judgment criteria) A (excellent): 3.5 points or more B (Good): 3.0 points or higher, less than 3.5 points C (Somewhat unacceptable): 2.0 points or higher, less than 3.0 points D (Not acceptable): Less than 2.0 points

[0072] As is clear from the results in Tables 1 and 2, the oily solid sticks (oily solid compositions) of Examples 1 to 17 of the present invention were superior to Comparative Examples 1 to 12 in terms of the inhibitory effect on precipitation of component (A), the dispersibility of component (A), formulation stability, and ease of application to the skin. Furthermore, the average particle size of component (A) in Examples 1 to 17 was 200 μm or less in all cases.

[0073] In contrast, in Comparative Example 1, where the content of component (A) exceeded 40%, the inhibitory effect on precipitation of component (A), the dispersibility of component (A), and the formulation stability were insufficient. In Comparative Example 2, where clay minerals, which are oily thickeners, were used instead of component (B), component (A) was inferior in all aspects, including its precipitation inhibitory effect, dispersibility, formulation stability, and ease of application to the skin. In Comparative Example 3, where the content of component (B) exceeded 20%, the inhibitory effect on precipitation of component (A), the dispersibility of component (A), and the ease of application to the skin were inferior. In Comparative Example 4, where the content of component (B) was less than 5%, the precipitation inhibition effect of component (A), the dispersibility of component (A), and the formulation stability were inferior. In Comparative Example 5, where an ester oil with a viscosity of less than 200 mPa·s at 25°C was used instead of component (C), the precipitation inhibitory effect of component (A), the dispersibility of component (A), the formulation stability, and the ease of application to the skin were all inferior. Comparative Example 6, which used an ester oil of branched-chain fatty acids and monohydric alcohols with a viscosity of less than 200 mPa·s at 25°C instead of component (C), and Comparative Example 8, which did not contain component (C), exhibited insufficient formulation stability, and inferior precipitation inhibition effect of component (A), dispersibility of component (A), and ease of application to the skin. In Comparative Example 7, where a silicone oil with a viscosity of 200 mPa·s or higher at 25°C was used instead of component (C), the formulation stability was insufficient, and the precipitation inhibitory effect and dispersibility of component (A) were poor. In Comparative Example 9, where the content of component (C) exceeded 50%, the precipitation inhibitory effect of component (A) was insufficient, and the dispersibility and formulation stability of component (A) were poor. In Comparative Example 10, where the content of component (D) exceeded 3%, the inhibitory effect on precipitation of component (A), the dispersibility of component (A), and the ease of application to the skin were inferior. In Comparative Example 11, where the content of component (D) was less than 0.1%, the formulation stability was insufficient, and the ease of application to the skin was poor.

[0074] Example 18: Oil-based solid stick (component) (mass%) (1) Ascorbic acid 2-glucoside (component (A)) 30 (2) Microcrystalline wax (Component (B)) Note 2 5 (3) Polyethylene wax (component (B)) Note 3 7 (4) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (5) Diisostearyl malate (ingredient (E)) remaining amount (6) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0075] (Manufacturing method) A: Mix component (1), some of components (2) to (5), and component (6) uniformly at 100°C, and then knead using a three-roller system. B: Add the remaining ingredients (2) to (5) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0076] The oily solid stick of Example 18 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0077] Example 19: Oil-based solid stick (component) (mass%) (1) L-Ascorbic Acid Sulfate Disodium (Component (A)) 30 (2) Microcrystalline wax (Component (B)) Note 2 5 (3) Polyethylene wax (component (B)) Note 3 7 (4) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (5) Diisostearyl malate (ingredient (E)) remaining amount (6) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0078] (Manufacturing method) A: Mix component (1), some of components (2) to (5), and component (6) uniformly at 100°C, and then knead using a three-roller system. B: Add the remaining ingredients (2) to (5) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0079] The oily solid stick of Example 19 obtained as described above exhibited excellent performance in all aspects, including "suppression of precipitation of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0080] Example 20: Oil-based solid stick (component) (mass%) (1) Tetra-2-hexyldecanoate ascorbyl (component (A)) 30 (2) Microcrystalline wax (Component (B)) Note 2 5 (3) Polyethylene wax (component (B)) Note 3 7 (4) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (5) Diisostearyl malate (ingredient (E)) remaining amount (6) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0081] (Manufacturing method) A: Mix component (1), some of components (2) to (5), and component (6) uniformly at 100°C, and then knead using a three-roller system. B: Add the remaining ingredients (2) to (5) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0082] The oily solid stick of Example 20 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0083] Example 21: Oil-based solid stick (component) (mass%) (1) Magnesium L-ascorbyl phosphate (Component (A)) 30 (2) Microcrystalline wax (Component (B)) Note 2 5 (3) Polyethylene wax (component (B)) Note 3 7 (4) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (5) Diisostearyl malate (ingredient (E)) remaining amount (6) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0084] (Manufacturing method) A: Mix component (1), some of components (2) to (5), and component (6) uniformly at 100°C, and then knead using a three-roller system. B: Add the remaining components (2) to (5) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0085] The oily solid stick of Example 21 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0086] Example 22: Oil-based solid stick (component) (mass%) (1) Ascorbic acid (Component (A)) Note 1 30 (2) Tranexamic acid 3 (3) Microcrystalline wax (Component (B)) Note 2 5 (4) Polyethylene wax (component (B)) Note 3 7 (5) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (6) Diisostearyl malate (ingredient (E)) remaining amount (7) Diethylhexyl succinate (ingredient (E)) 5 (8) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0087] (Manufacturing method) A: Mix components (1) and (2) and a portion of components (5) to (7) uniformly at 100°C, and then knead using a three-roller system. B: Add ingredients (3), (4), (8) and the remaining ingredients (5) to (7) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0088] The oily solid stick of Example 22 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0089] Example 23: Oil-based solid stick (component) (mass%) (1) Ascorbic acid (Component (A)) Note 1 30 (2) Astaxanthin H3 (3) Microcrystalline wax (Component (B)) Note 2 5 (4) Polyethylene wax (component (B)) Note 3 7 (5) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (6) Diisostearyl malate (ingredient (E)) remaining amount (7) Propylene glycol dicaprate (Component (E)) 5 (8) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0090] (Manufacturing method) A: Mix a portion of ingredient (1) and ingredient (5) uniformly at 100°C, and then knead using a three-roller system. B: Add components (2) to (4), components (6) to (8), and the remainder of component (5) to A, and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0091] The oily solid stick of Example 23 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0092] Example 24: Oil-based solid stick (component) (mass%) (1) Ascorbic acid (Component (A)) Note 1 30 (2) Niacinamide 3 (3) Microcrystalline wax (Component (B)) Note 2 5 (4) Polyethylene wax (component (B)) Note 3 7 (5) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (6) Diisostearyl malate (ingredient (E)) remaining amount (7) Propylene glycol dicaprate (Component (E)) 5 (8) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0093] (Manufacturing method) A: Mix components (1) and (2), some of components (3) to (7), and component (8) uniformly at 100°C, and then knead using a three-roller system. B: Add the remaining ingredients (3) to (7) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0094] The oily solid stick of Example 24 obtained as described above exhibited excellent performance in all aspects, including "suppression of precipitation of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0095] Example 25: Oil-based solid stick (component) (mass%) (1) Ascorbic acid (Component (A)) Note 1 30 (2) Dipotassium glycyrrhizinate 3 (3) Microcrystalline wax (Component (B)) Note 2 5 (4) Polyethylene wax (component (B)) Note 3 7 (5) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (6) Diisostearyl malate (ingredient (E)) remaining amount (7) Diethylhexyl succinate (ingredient (E)) 5 (8) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0096] (Manufacturing method) A: Mix components (1) and (2), some of components (3) to (7), and component (8) uniformly at 100°C, and then knead using a three-roller system. B: Add the remaining ingredients (3) to (7) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0097] The oily solid stick of Example 25 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0098] Example 26: Oil-based solid stick (component) (mass%) (1) Ascorbic acid (Component (A)) Note 1 30 (2) Tocopherol 0.1 (3) Microcrystalline wax (Component (B)) Note 2 5 (4) Polyethylene wax (component (B)) Note 3 7 (5) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (6) Diisostearyl malate (ingredient (E)) remaining amount (7) Diethylhexyl succinate (ingredient (E)) 5 (8) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0099] (Manufacturing method) A: Mix components (1) and (2) and a portion of components (5) to (7) uniformly at 100°C, and then knead using a three-roller system. B: Add ingredients (3), (4), (8) and the remaining ingredients (5) to (7) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0100] The oily solid stick of Example 26 obtained as described above exhibited excellent performance in all aspects, including "suppression of precipitation of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0101] Example 27: Oil-based solid stick (component) (mass%) (1) Ascorbic acid (Component (A)) Note 1 30 (2) N-stearoyldihydrosphingosine 0.1 (3) Microcrystalline wax (Component (B)) Note 2 5 (4) Polyethylene wax (component (B)) Note 3 7 (5) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (6) Diisostearyl malate (ingredient (E)) remaining amount (7) Diethylhexyl succinate (ingredient (E)) 5 (8) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0102] (Manufacturing method) A: Mix components (1) and (2), some of components (3) to (7), and component (8) uniformly at 100°C, and then knead using a three-roller system. B: Add the remaining ingredients (3) to (7) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0103] The oily solid stick of Example 27 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0104] Example 28: Oil-based solid stick (component) (mass%) (1) Ascorbic acid (Component (A)) Note 1 30 (2) Hydrolyzed hyaluronic acid 0.1 (3) Microcrystalline wax (Component (B)) Note 2 5 (4) Polyethylene wax (component (B)) Note 3 7 (5) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (6) Diisostearyl malate (ingredient (E)) remaining amount (7) Diethylhexyl succinate (ingredient (E)) 5 (8) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0105] (Manufacturing method) A: Mix components (1) and (2), some of components (3) to (7), and component (8) uniformly at 100°C, and then knead using a three-roller system. B: Add the remaining ingredients (3) to (7) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0106] The oily solid stick of Example 28 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0107] Example 29: Oil-based solid stick (component) (mass%) (1) Ascorbic acid (Component (A)) Note 1 30 (2) 3-O-ethyl ascorbic acid (component (A)) 0.1 (3) Microcrystalline wax (Component (B)) Note 2 5 (4) Polyethylene wax (component (B)) Note 3 7 (5) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (6) Diisostearyl malate (ingredient (E)) remaining amount (7) Propylene glycol dicaprate (Component (E)) 5 (8) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0108] (Manufacturing method) A: Mix components (1) and (2), some of components (3) to (7), and component (8) uniformly at 100°C, and then knead using a three-roller system. B: Add the remaining ingredients (3) to (7) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0109] The oily solid stick of Example 29 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

[0110] Example 30: Oil-based solid stick (component) (mass%) (1) Ascorbic acid (Component (A)) Note 1 30 (2) Ascorbyl tetrahexyldecanoate 0.1 (3) Microcrystalline wax (Component (B)) Note 2 5 (4) Polyethylene wax (component (B)) Note 3 7 (5) Polyglyceryl-2 triisostearate (Component (C)) Note 5 35 (6) Diisostearyl malate (ingredient (E)) remaining amount (7) Silylated anhydrous silicic acid (component (D)) Note 9 1

[0111] (Manufacturing method) A: Mix components (1) and (2) and a portion of components (3) to (6) uniformly at 100°C, and then knead using a three-roller system. B: Add ingredient (7) and the remaining ingredients (3) to (6) to A and mix uniformly at 90°C. C:B was heated to 100°C, filled into polypropylene stick containers, and cooled to room temperature to obtain oily solid sticks.

[0112] The oily solid stick of Example 30 obtained as described above exhibited excellent performance in all aspects, including "precipitation inhibition effect of component (A)," "dispersibility of component (A)," "formulation stability," and "ease of application to the skin." Furthermore, the average particle size of component (A) was 200 μm or less.

Claims

1. The following components (A) to (D): (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25 to 40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or higher hydroxyl groups are esterified, comprising 50% by mass or less. (D) Anhydrous silicic acid 0.1-3% by mass An oily solid composition containing [the specified ingredient].

2. The oily solid composition according to claim 1, wherein the component (A) is ascorbic acid.

3. The oily solid composition according to claim 1 or 2, wherein the component (C) is a liquid oil obtained by esterifying a branched-chain fatty acid having 14 to 22 carbon atoms with a polyhydric alcohol having three or more hydroxyl groups selected from the group consisting of glycerin, polyglycerin, and pentaerythritol.

4. The oily solid composition according to claim 1 or 2, wherein the mass ratio (C) / (A) of component (C) to component (A) is 0.8 to 1.

7.

5. Furthermore, the oily solid composition according to claim 1 or 2 contains component (E) a non-volatile diester oil (excluding component (C)).

6. The oily solid composition according to claim 5, wherein the component (E) is one or more selected from diethylhexyl succinate, diisostearyl malate, and propylene glycol dicaprate.

7. An oily solid composition according to claim 1 or 2, which is a cosmetic or a topical skin preparation.

8. The following components (A) to (D): (A) At least one selected from the group consisting of ascorbic acid, salts of ascorbic acid, or water-soluble derivatives, in an amount of 25 to 40% by mass. (B) Wax 5-20% by mass (C) A liquid oil having a viscosity of 200 mPa·s or more at 25°C, in which branched fatty acids and polyhydric alcohols having trivalent or higher hydroxyl groups are esterified, comprising 50% by mass or less. (D) Anhydrous silicic acid 0.1-3% by mass A method for producing an oily solid composition containing, (Step 1) A step of preparing a mixture of an oily component containing part or all of component (A) and component (C) such that component (A) accounts for 20 to 80% by mass of the total amount of the mixture. (Step 2) Step of kneading the mixture from Step 1. (Step 3) A step in which the mixture from Step 2 and the remaining ingredients are heated and mixed. A method for producing an oily solid composition containing [the specified ingredient].

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