Solid powder cosmetic

Abstract

To develop a solid powder cosmetic showing superiority in all of uniformity of coating film, non-occurrence of smudging, and absence of white film look.SOLUTION: A solid powder cosmetic comprises the following components (A) to (C): (A) a specific crosslinked organosilicon resin, (B) a silicone oil that is liquid at 25°C, and (C) a lustrous powder. The solid powder cosmetic is prepared by the following process in which: a cosmetic base, in which the content mass ratio of oil agents including the component (B) to the total amount of powders including the component (C) (total of oil agents / total of powders) is 0.05 to 1.5, is mixed with a solvent to form a slurry; and the slurry is charged into a container, followed by removing the solvent.SELECTED DRAWING: None

Description

Technical Field

[0001] The present invention relates to solid powder cosmetics.

Background Art

[0002] Solid powder cosmetics are a dosage form that is widely used in foundations, eyeshadows, etc. because they are easy to use and highly portable. Among them, solid powder cosmetics mainly composed of powder are preferred for their good spreading and non-greasy finish during use.

[0003] In recent years, studies have been made to improve the usability of solid powder cosmetics, and solid powder cosmetics excellent in impact resistance and uniformity of the coating film during use have been proposed using oil-absorbing powder and a specific oil agent (see, for example, Patent Document 1). In addition, cosmetics having a good feel in use, good elongation and finish, and excellent abrasion resistance have been disclosed by containing a specific crosslinked organosilicon resin in solid powder cosmetics (see, for example, Patent Document 2).

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Patent Document 2

Summary of the Invention

Problems to be Solved by the Invention

[0005] However, in the conventional technology, it was likely to form a thick makeup film at the start, and there was a problem in uniformly forming a thin makeup film. In addition, when using oil-absorbed powder, streaks were likely to occur, and it was difficult to develop a solid powder cosmetic that had a uniform makeup film and was excellent in streak-free property. Therefore, an object of the present invention is to provide a solid powder cosmetic that forms a coating film excellent in uniformity without a white film feeling and is excellent in streak-free property.

Means for Solving the Problem

[0006] In view of such circumstances, as a result of intensive studies by the present inventors, by combining a specific crosslinked organosilicon resin, a silicone oil that is liquid at 25°C, and a bright powder, a uniform cosmetic film is formed without a white film feeling from the time of application with an appropriate adhesive force and is difficult to have thickness, and furthermore, a solid powder cosmetic excellent in spreadability is obtained, leading to the completion of the present invention.

[0007] That is, the present invention includes the following aspects. [1] The following components (A) to (C); (A) A crosslinked organosilicon resin that is an addition reaction product of the following component (X) and component (Y), wherein the amount of hydrogen gas generated per mass of this crosslinked organosilicon resin is 1.5 mL / g or less under standard conditions. (B) A silicone oil that is liquid at 25°C (C) A bright powder Containing, the content mass ratio (total amount of all oil agents / total amount of all powders) of the total amount of the oil agent containing the component (B) to the total amount of the powder containing the component (C) is 0.05 to 1.5, a cosmetic base, and a solvent are mixed to form a slurry, filled into a container, and then a solid powder cosmetic obtained by removing the solvent. (X) An alkenyl group-containing organosilicon resin represented by the following formula (1) and having one or more alkenyl groups in one molecule

Chemical formula

[0008] According to the present invention, a solid powder cosmetic excellent in the uniformity of the coating film, the absence of streaks, and the absence of a white film feeling can be provided.

Best Mode for Carrying Out the Invention

[0009] Preferred embodiments of the present invention will be described in detail. However, the present invention is not limited to the following preferred embodiments and can be freely changed within the scope of the present invention. In this specification, "~" means a range including the numerical values before and after it. Also, the "average particle diameter" in the present invention is the value of the median diameter (D50) obtained by measurement with an image analyzer (Lucerex AP, manufactured by Nireco Corporation). In the case of an asymmetric shape, in the present invention, the value of the median diameter (D50) obtained from the distribution of the largest particle diameter is used as the average particle diameter. Further, in the present invention, component names may be described by cosmetic display names or International Nomenclature of Cosmetic Ingredient (INCI). When the cosmetic display name and INCI correspond, the English description may be omitted.

[0010] [Component (A)] Hereinafter, component (A) in the present invention will be described in detail. Component (A) is a crosslinked organosilicon resin which is an addition reaction product of the following component (X) and component (Y), and is a crosslinked organosilicon resin in which the amount of hydrogen gas per mass generated from this crosslinked organosilicon resin is 1.5 mL / g or less under standard conditions.

[0011] [Component (X)] Component (X) is an alkenyl group-containing organosilicon resin represented by the following average compositional formula (1) and having one or more alkenyl groups in one molecule, and can be used alone or in combination of two or more. [Chemical formula] [In the formula, R 1 are each independently an alkenyl group having 2 to 8 carbon atoms, and R 2 are each independently a group selected from an alkyl group having 1 to 30 carbon atoms, an aryl group having 6 to 30 carbon atoms, and an aralkyl group having 7 to 30 carbon atoms. R 3are, independently of each other, an organopolysiloxane-containing group, and said R 2 selected from the group consisting of, each R 3 3SiO 1 / 2 in the unit, one or more of the R 3 are organopolysiloxane-containing groups. a1, a2, a3, b, c, and d are numbers such that 0 < a1 ≤ 5, 0 < a2 ≤ 400, 0 ≤ a3 ≤ 400, 0 ≤ b ≤ 320, 0 ≤ c ≤ 320, 0 < d ≤ 1,000, and satisfy 0.5 ≤ (a1 + a2 + a3) / d ≤ 1.5.]

[0012] [Component (Y)] (Component (Y)) is an organohydrogenpolysiloxane represented by the following average compositional formula (2) and having two or more hydrosilyl groups in one molecule, and can be used alone or in combination of two or more. The addition reaction amount is such that the amount of hydrosilyl groups is 0.5 to 1.2 moles with respect to 1 mole of the amount of alkenyl groups in the above (X) component, preferably 0.5 to 1.2 moles, more preferably 0.8 to 1.2, and even more preferably 0.9 to 1.1. [Chemical formula] [In the formula, R 2 is the same as above, R 4 are, independently of each other, a hydrogen atom or a group represented by the above R 2 , and two or more of all the R 4 are hydrogen atoms, e, f, g, h are 0 or positive numbers, provided that 2 ≤ e + f + g + h < 32 is satisfied.]

[0013] In the above formula, R 1 are, independently of each other, alkenyl groups having 2 to 8 carbon atoms. More specifically, vinyl group, allyl group, isopropenyl group, butenyl group, pentenyl group, hexenyl group, cyclohexenyl group, octenyl group, etc. can be mentioned. In particular, vinyl group and allyl group are preferable.

[0014] In the above formula, R 2is, independently of each other, a group selected from an alkyl group having 1 to 30 carbon atoms, an aryl group having 6 to 30 carbon atoms, or an aralkyl group having 7 to 30 carbon atoms. Among them, an alkyl group, aryl group, aralkyl group, or fluorine-substituted alkyl group having 1 to 10 carbon atoms is preferable. More specifically, a methyl group, ethyl group, propyl group, butyl group, pentyl group, cyclopentyl group, cyclohexyl group, phenyl group, tolyl group, etc., a trifluoropropyl group, etc. can be mentioned. In particular, an alkyl group having 1 to 5 carbon atoms, a phenyl group, or a trifluoropropyl group is preferable. Also, optionally R 2 a part of may contain one or more groups selected from a hydroxyl group or an alkoxy group having 1 to 8 carbon atoms.

[0015] In the alkenyl group-containing organosilicon resin represented by the above formula (1), a1, a2, a3, b, c, and d satisfy 0 < a1 ≤ 5, preferably 0 < a1 ≤ 4.5, more preferably 1 ≤ a1 ≤ 4, and still more preferably 1 ≤ a1 ≤ 3. When a1 is greater than 5, the possibility of gelation increases and film-forming properties are also lacking. 0 ≤ a2 ≤ 400, preferably 0 ≤ a2 ≤ 100, more preferably 0 ≤ a2 ≤ 50. 0 ≤ a3 ≤ 400, preferably 0 ≤ a3 ≤ 100, more preferably 0 ≤ a3 ≤ 50. When a3 is greater than 400, the melting point of the resin becomes low and film-forming properties are lacking. 0 ≤ b ≤ 320, 0 ≤ c ≤ 320, and b = 0 and c = 0 are preferable. 0 < d ≤ 1,000, and it is a number that satisfies 0.5 ≤ (a1 + a2 + a3) / d ≤ 1.5, preferably a number that satisfies 0.7 ≤ (a1 + a2 + a3) / d ≤ 1.2. When the value of (a1 + a2 + a3) / d is less than the above lower limit, the degree of crosslinking increases and the molecular weight becomes large, resulting in a gel state. When it exceeds the above upper limit, the molecular weight becomes small and film-forming properties are lacking.

[0016] The alkenyl group-containing organosilicon resin represented by the above formula (1) has Q units (SiO 4 / 2 ), M units (R 2 3SiO 1 / 2 and R 1 R 2 2SiO 1 / 2 ) as essential structures, and D units (R 2 2SiO 2 / 2)、T unit (R 2 SiO 3 / 2 ) is composed of a structure with an arbitrary structure. It may be solid or liquid at 25°C, but a solid state is preferred from the viewpoint of film-forming properties. For example, MQ resin, MTQ resin, MDQ resin, MDTQ resin can be mentioned. Its weight average molecular weight preferably ranges from 1,000 to 30,000, and more preferably ranges from 3,000 to 15,000 in terms of performance and workability such as filtration. The weight average molecular weight can be determined as the weight average molecular weight in terms of polystyrene in gel permeation chromatography (GPC) analysis.

[0017] In the organohydrogenpolysiloxane having two or more hydrosilyl groups in one molecule represented by the above formula (2), R 4 is, independently of each other, a monovalent hydrocarbon group having no aliphatic unsaturated bond with 1 to 30 carbon atoms, and two or more of all R 4 are hydrogen atoms.

[0018] In the above formula (2), e, f, g, h are 0 or positive numbers, and may be selected so as to satisfy 2 ≤ e + f + g + h < 32. Preferably g = 0 and h = 0, more preferably e = 2, 0 ≤ f < 30, g = 0, h = 0, and even more preferably e = 2, 0 ≤ f ≤ 20, g = 0, h = 0. If the number of silicon atoms contained in the (Y) component is 32 or more, the crosslinked organosilicon resin is likely to gel due to entraining the solvent, so that it is likely to form a sticky film after the solvent volatilizes. If the number of silicon atoms contained in the (Y) component is less than 32, the crosslinked organosilicon resin is likely to dissolve in the solvent, so that a non-sticky film is likely to be obtained after the solvent volatilizes.

[0019] The above R 3 is, independently of each other, an organopolysiloxane-containing group, or a group selected from the above R 2 . Examples of the organopolysiloxane-containing group include groups represented by the following general formulas (3) to (6). R 3 3SiO 1 / 2In each of the units, there is one or more R 3 is an organopolysiloxane-containing group. Optionally, a part of R 3 may be a hydroxyl group. [Chemical formula] (In the formula, R 2 is the same as above, n and i are integers satisfying 0 ≤ n ≤ 5 and 0 ≤ i ≤ 500, and j1 to j3 are each an integer of 0 or more and 2 or less.)

[0020] m is an integer of 0 ≤ m ≤ 5, preferably 0 ≤ m ≤ 2, i is an integer of 0 ≤ i ≤ 500, preferably 1 ≤ i ≤ 100, and more preferably 1 ≤ i ≤ 50. When i is greater than 500, the melting point of the resin becomes low, resulting in a lack of film-forming property. j1 to j3 are each an integer of 0 or more and 2 or less.

[0021] In the above formula (1), it is preferable that b = 0 and c = 0. When b and c are 0, the alkenyl group-containing organosilicon resin does not contain a flexible skeleton such as a D unit or a T unit, and is composed only of an M unit and a Q unit. By using an alkenyl group-containing organosilicon resin that does not contain a D unit or a T unit as a raw material, the crosslinked organosilicon resin, which is an addition reaction product, can form a strong film.

[0022] In the above formula (2), it is preferable that g = 0 and h = 0. When g and h are 0, the organohydrogenpolysiloxane does not contain branched components such as a T unit and a Q unit, and becomes a linear molecule composed only of an M unit and a D unit. By using a linear organohydrogenpolysiloxane as a raw material, the crosslinked organosilicon resin, which is an addition reaction product, can form a flexible film.

[0023] Also, two or more groups represented by the formula (2) may be included. The group represented by the formula (2) has an effect of imparting flexibility to the organosilicon resin as the chain length becomes longer. Therefore, for example, by including two types of groups represented by the formula (2) having different chain lengths, the film physical properties can be controlled.

[0024] [Physical properties of the crosslinked organosilicon resin] The weight average molecular weight of the crosslinked organosilicon resin of component (A) is preferably from 5,000 to 1,000,000, more preferably from 8,000 to 500,000, and even more preferably from 10,000 to 500,000. Being within such a range is more preferable in terms of performance and workability such as filtration. The weight average molecular weight can be determined as the weight average molecular weight in terms of polystyrene in gel permeation chromatography (GPC) analysis (hereinafter the same).

[0025] The crosslinked organosilicon resin of component (A) may be in a solid state, a gel state, or a liquid state at 25°C. For example, it can be dissolved in a liquid oil agent and volatilized to easily form a film. This film is a strong and brittle film before crosslinking, but after crosslinking, its brittleness is improved and a non-sticky and flexible film can be obtained. From the viewpoint of film-forming property, a solid state or a gel state is preferable, and a solid state is more preferable. The film-forming ability can be determined by dropping 1.5 g of a solution diluted to 30% by mass with isododecane or decamethylcyclopentasiloxane onto PTFE (fluororesin) and drying it at 105°C for 3 hours to see if a self-supporting film is formed. If a film is not formed, oil will seep out due to cracks in the film and the oil resistance will be significantly reduced, and the followability with the skin will be low, resulting in an unnatural finish.

[0026] The crosslinked organosilicon resin of component (A) can be more suitably used as a film-forming agent. The organosilicon resin before crosslinking forms a strong and brittle film, while the crosslinked organosilicon resin after crosslinking has improved brittleness and forms a non-sticky and flexible film. This is because the organosilicon resin before crosslinking forms a strong film, but by crosslinking with flexible chains, flexibility is imparted to the film. Generally, a hard film has low flexibility, and a film with high flexibility tends to be soft, so the strength and flexibility of the film have been considered to be in an antinomic relationship. However, the crosslinked organosilicon resin has the characteristic of excellent followability due to its high flexibility despite forming a strong film.

[0027] In addition, the film formed of the crosslinked organic silicon resin of component (A) has significantly improved oil resistance to oily agents such as sebum as compared with the film formed of the organic silicon resin before crosslinking. Although the oil resistance of the organic silicon resin tends to improve as the molecular weight increases, since there is a limit to increasing the molecular weight of the organic silicon resin, the oil resistance also has a limit point. Crosslinking of the organic silicon resin with a crosslinking agent leads to a pseudo-increase in the molecular weight of the organic silicon resin, and thus has the effect of raising that limit point. Therefore, the crosslinked organic silicon resin has oil resistance that cannot be achieved with conventional organic silicon resins.

[0028] The crosslinked organic silicon resin in which f in the above formula (2) is an integer satisfying 0 < f < 30 is solid at 25°C, and a crosslinked organic silicon resin with particularly excellent film-forming properties can be obtained.

[0029] In addition, for the crosslinked organic silicon resin in which f in the above formula (2) satisfies 0 ≤ f < 30 and two of R 4 are hydrogen atoms, it is solid at 25°C, and a crosslinked organic silicon resin with particularly excellent film-forming properties can be obtained. When f is 30 or more, or when three or more of R 4 are hydrogen atoms, there is a high possibility of becoming gel-like when the diluting solvent is removed. In this case, although there is film-forming property, it has the feel derived from the gel.

[0030] In the above formula (1), when a1 satisfies 0 < a1 ≤ 3, f in the above formula (2) satisfies 0 ≤ f < 20, and two of R 4 are hydrogen atoms, the crosslinked organic silicon resin is solid at 25°C, and a crosslinked organic silicon resin with particularly excellent film-forming properties can be obtained. The obtained film exhibits particularly excellent flex resistance and oil resistance.

[0031] The amount of hydrogen gas generated per unit mass from the crosslinked organosilicon resin of component (A) is 1.5 mL or less under standard conditions. If it exceeds 1.5 mL / g, the generation of hydrogen gas over time, or the reaction between the remaining hydroxy groups or alkoxy groups and hydrosilyl groups, may increase the likelihood of thickening over time and deteriorate the stability over time. The amount of hydrogen gas generated is preferably 0.01 to 1.2 mL / g, more preferably 0.02 to 1.0 mL / g.

[0032] The amount of hydrogen gas per unit mass can be calculated from the volume of hydrogen gas generated by the reaction of a hydrosilyl group with a base. For example, the following method can be used, but the calculation method is not limited to this. <Measurement method of hydrogen gas amount> To a mixed solution of 50 g of a crosslinked organosilicon resin diluted to 50% by mass with decamethylcyclopentasiloxane and 10 g of 1-butanol, 10 g of a 20% by mass aqueous sodium hydroxide solution is added dropwise. The amount of hydrogen gas per unit mass is obtained by dividing the volume of the generated hydrogen gas by the pure content of the crosslinked organosilicon resin.

[0033] [Manufacturing method] The crosslinked organosilicon resin can be synthesized by various formulations known in the art. For example, crosslinking can be achieved by reacting an organopolysiloxane having hydroxyl groups at both ends with the surface silanol groups of the organosilicon resin. However, since it is difficult to completely control the amount of silanol groups on the surface of the organosilicon resin, there is a problem that it is difficult to accurately control the amount of the organopolysiloxane to be crosslinked. In addition, synthesis can be achieved by an addition reaction between an organosilicon resin having a hydrosilyl group and an organopolysiloxane having alkenyl groups at both ends. However, the hydrosilyl groups in the organosilicon resin have low reactivity, and there is a problem that the remaining hydrosilyl groups react over time, causing an increase in viscosity and the generation of hydrogen gas. Therefore, as a method for producing a crosslinked organosilicon resin crosslinked with silicone, a synthesis method by an addition reaction between an organosilicon resin having an alkenyl group and an organopolysiloxane having hydrosilyl groups at both ends is preferred.

[0034] The method for producing a crosslinked organosilicon resin by the above hydrosilylation reaction will be described in more detail below. In the hydrosilylation reaction step of the alkenyl group-containing organosilicon resin represented by the above average composition formula (1) and the organohydrogenpolysiloxane represented by the above formula (2), the molar ratio of the terminal hydrosilyl group / unsaturated group can be selected from the range of 0.5 to 2.0, preferably 0.5 to 1.2 moles, more preferably 0.8 to 1.2, and even more preferably 0.9 to 1.1. If the above ratio is too large, the residual amount of the hydrosilyl group will increase, and the stability over time may deteriorate.

[0035] This hydrosilylation reaction is preferably carried out in the presence of a platinum catalyst or a rhodium catalyst. For example, chloroplatinic acid, alcohol-modified chloroplatinic acid, chloroplatinic acid-vinylsiloxane complex, etc. are preferred. Also, since the sample will be colored if the amount of the catalyst used is excessive, the amount of platinum or rhodium is preferably 50 ppm or less, and more preferably 20 ppm or less.

[0036] Furthermore, the addition reaction may be carried out in the presence of an organic solvent as needed. Examples of the organic solvent include cyclic organopolysiloxanes such as octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, and dodecamethylcyclohexasiloxane; short-chain silicone oils such as methyltrimethicone and short-chain dimethicone; aromatic hydrocarbons such as toluene and xylene; ketone-based organic solvents such as acetone, methyl ethyl ketone, diethyl ketone, and methyl isobutyl ketone; aliphatic hydrocarbons such as hexane, heptane, octane, decane, isododecane, and cyclohexane; and aliphatic alcohols such as methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-methyl-1-propanol, 2-butanol, 2-methyl-2-propanol, 1-pentanol, 2-methylbutanol, 2-pentanol, 1-hexanol, 2-methylpentanol, 1-heptanol, 1-octanol, 1-nonanol, 1-decanol, phenol, benzyl alcohol, ethylene glycol, and 1,2-propylene glycol. Ethanol, 1-propanol, and 2-propanol are particularly preferred from the viewpoint of reactivity.

[0037] The amount of the solvent used is preferably 1 to 80% by mass, more preferably 5 to 50% by mass, of the entire reaction solution (system). When within the above range, the reaction system is uniformly maintained and the reaction proceeds efficiently.

[0038] The crosslinked organic silicon resin of component (A) used in the present invention can be dissolved in an organic solvent and used as a pre-dissolved product. The organic solvent used during the addition reaction may be used as it is, or may be replaced after the addition reaction, and an organic solvent for replacement can be selected according to the application. The replacement solvent is not particularly limited and can be selected from the aforementioned organic solvents.

[0039] The addition reaction conditions are not particularly limited, but it is preferable to heat at a temperature of 50 to 150°C, more preferably 80 to 120°C, for about 1 to 10 hours under reflux.

[0040] After the addition reaction, it is also possible to include a step of removing the rhodium catalyst or platinum catalyst used with activated carbon. The amount of activated carbon used is preferably 0.001 to 5.0% by mass of the whole system, and more preferably 0.01 to 1.0% by mass. When within the above range, coloring of the sample can be more suppressed.

[0041] After the addition reaction, it is possible to include a step of removing the remaining hydrosilyl groups as necessary. Particularly when used in applications such as cosmetics, the hydrosilyl groups may be deactivated by dehydrogenation over time. Since hydrogen gas is generated, there is no problem from the viewpoint of safety, so it is preferable to include a step of removing the hydrosilyl groups.

[0042] Examples of the step of removing the hydrosilyl groups include a formulation in which a basic catalyst is added to hydrolyze the unreacted hydrosilyl groups, and then an acidic catalyst equivalent to the molar equivalent of the basic catalyst is added for neutralization. Examples of the basic catalyst include strong basic catalysts and weak basic catalysts. Examples of strong basic catalysts include alkali metal hydroxides such as lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide, and barium hydroxide. Examples of weak basic catalysts include alkali metal carbonates such as sodium carbonate and calcium carbonate, and alkali metal hydrogen carbonates such as sodium hydrogen carbonate and potassium hydrogen carbonate. In terms of promoting the dehydrogenation reaction, it is particularly preferable to use a strong basic catalyst, and specifically sodium hydroxide is preferable. Examples of the acidic catalyst include inorganic acids such as hydrochloric acid, sulfuric acid, sulfurous acid, fuming sulfuric acid, and phosphoric acid, sulfonic acids such as p-toluenesulfonic acid, methanesulfonic acid, and trifluoromethanesulfonic acid, and carboxylic acids such as oxalic acid, formic acid, acetic acid, propionic acid, benzoic acid, citric acid, and trifluoroacetic acid.

[0043] Generally, it is preferable to use an acid or a base in combination with water and heat at a temperature below the boiling point of water rather than using them alone. By this step, a hydrosilyl group (SiH group) becomes a hydroxysilyl group (SiOH group). However, when a crosslinked organosilicon resin is treated with a base catalyst, the physical properties change due to the reaction of silanol groups and alkoxy groups in the organosilicon resin. Therefore, it is not preferable to remove the hydrosilyl group by this method.

[0044] The content of the component (A) in the present invention is not particularly limited, and is preferably 0.01% by mass (hereinafter simply abbreviated as %) or more, more preferably 0.1% or more, and even more preferably 0.5% or more, based on the total amount of the solid powdered cosmetic. Also, it is preferably 10% or less, more preferably 8% or less, and even more preferably 6% or less. Further, 0.01 to 10% is preferable, 0.1 to 8% is more preferable, and 0.5 to 6% is even more preferable. Within this range, it is more preferable because the uniformity of the coating film is excellent.

[0045] [Component (B)] The component (B) in the present invention is a silicone oil that is liquid at 25°C. Here, being liquid means having fluidity at 25°C. The silicone oil that is liquid at 25°C is not particularly limited in terms of properties such as volatility and non-volatility as long as it is normally used in cosmetics, and any of them can be used. Examples of non-volatile silicone oils include linear silicone oils such as dimethylpolysiloxane (kinematic viscosity at 25°C of 6 CS or more), phenyl-modified silicones such as diphenylsiloxyphenyltrimethicone, phenyltrimethicone, diphenyldimethylsilicone, trimethylpentaphenyltrisiloxane, and fluorine-modified silicones such as trifluoropropylcyclopolysiloxane. Examples of volatile silicone oils include dimethylpolysiloxane (kinematic viscosity at 25°C of 5 CS or less), methyltrimethicone, decamethylcyclopentasiloxane, octamethylcyclotetrasiloxane, etc. The silicone oil that is liquid at 25°C is not particularly limited, and one or a combination of two or more of these can be used.

[0046] In the present invention, component (B) is preferably a non-volatile silicone oil from the viewpoints of the uniformity of the coating film and the absence of a white film feeling, more preferably a linear silicone oil or a phenyl-modified silicone, and even more preferably dimethylpolysiloxane. Further, the kinematic viscosity of dimethylpolysiloxane at 25°C is preferably 1,000 CS or less, more preferably 500 CS or less, and even more preferably 100 CS or less. If it is within this range, it is more preferable because it is more excellent in the absence of streaks. In the present invention, the kinematic viscosity at 25°C is measured by a single-cylinder rotational viscometer Visometron model VS-A1 (manufactured by Shibaura System Co., Ltd.).

[0047] The content of component (B) in the present invention is not particularly limited, and is preferably 1% or more, more preferably 2% or more, and even more preferably 3% or more based on the total amount of the solid powder cosmetic. Further, it is preferably 20% or less, more preferably 18% or less, and even more preferably 15% or less. Also, 1 to 20% is preferable, 2 to 18% is more preferable, and 3 to 15% is even more preferable. If it is within this range, it is more preferable because the coating film is more excellent in uniformity.

[0048] [Component (C)] Component (C) in the present invention is a bright powder. The bright powder is a powder having a high-luminance appearance such as a pearl agent or a lame agent. The average particle diameter of component (C) is not particularly limited. For example, it is preferably 10 μm or more, more preferably 30 μm or more, and even more preferably 50 μm or more. Further, it is preferably 250 μm or less, more preferably 230 μm or less, and even more preferably 200 μm or less. Also, 10 to 250 μm is preferable, 30 to 230 μm is more preferable, and 50 to 200 μm is even more preferable. If it is within this range, it is more preferable because it is more excellent in the absence of a white film feeling.

[0049] Component (C) is not particularly limited as long as it is commonly used in cosmetics. For example, mica titanium, titanium oxide-coated synthetic phlogopite, iron oxide-coated mica, iron oxide-coated mica titanium, iron oxide / black iron oxide-coated mica titanium, congo-coated mica titanium, carmine-coated mica titanium, carmine / congo-coated mica titanium, iron oxide / carmine-coated mica titanium, iron oxide / congo-coated mica titanium, organic pigment-coated mica titanium, metal powder-coated mica titanium, metal powder-coated synthetic phlogopite, glass powder, titanium oxide-coated glass powder, metal powder-coated glass powder, aluminum powder, titanium oxide-coated alumina powder, titanium oxide-coated silica powder, iron oxide / silica-coated aluminum powder, polyethylene terephthalate / aluminum / epoxy laminated powder, polyethylene terephthalate / polyolefin laminated film powder, polyethylene terephthalate / polymethyl methacrylate laminated film powder, goniochromatic gloss pigment, fish scale foil, gold powder, silver powder, etc. can be mentioned, and one or more of these can be used in combination.

[0050] Among these, from the viewpoint of the absence of a white film feeling, component (C) is preferably one or more selected from the group consisting of titanium oxide-coated glass powder, titanium oxide-coated mica, and titanium oxide-coated synthetic phlogopite, more preferably one or two selected from the group consisting of titanium oxide-coated glass powder and titanium oxide-coated synthetic phlogopite, and even more preferably titanium oxide-coated glass powder.

[0051] The content of component (C) in the present invention is not particularly limited. With respect to the total amount of the solid powder cosmetic, 20% or more is preferable, 25% or more is more preferable, and 30% or more is even more preferable. Also, 60% or less is preferable, 55% or less is more preferable, and 50% or less is even more preferable. Further, 20 to 60% is preferable, 25 to 55% is more preferable, and 30 to 50% is even more preferable. Within this range, it is more preferable because of the better absence of a white film feeling.

[0052] [Component (D)] The present invention can further contain an oily agent in the form of a paste at 25°C as component (D). Here, the paste form means a state that does not have fluidity at 25°C and deforms when a force equal to its own weight is applied. The melting point of component (D) in the present invention is not particularly limited. For example, 30°C or higher is preferable, and 35°C or higher is more preferable. Also, 68°C or lower is preferable, and 65°C or lower is more preferable. Further, 30 to 68°C is preferable, and 35 to 65°C is more preferable. The melting point can be measured by the first method of the melting point test method in the General Test Methods of the Raw Material Standards for Quasi-Drugs 2006.

[0053] Component (D) is not particularly limited as long as it is usually used in cosmetics. For example, petrolatum (melting point 38 - 60°C), paraffin (melting point 55 - 61°C), stearyldimethicone (melting point 38 - 53°C), dimer dilinoleic acid (phytosteryl / isostearyl / cetyl / stearyl / behenyl (melting point 40°C)), (caprylic / capric / myristic / stearic acid) triglyceride (melting point 40°C), hexakis (hydroxystearic acid / stearic acid / rosin acid) dipentaerythrityl (melting point 37°C), hydrogenated castor oil stearate, cocoa butter, shea butter, phytosteryl macadamia nut oil fatty acid, di(octyldodecyl / phytosteryl / behenyl) lauroyl glutamate, etc. can be mentioned.

[0054] Among these, from the viewpoint of the uniformity of the coating film, petrolatum is preferable as component (D).

[0055] The content of component (D) in the present invention is not particularly limited. With respect to the total amount of the solid powder cosmetic, 1% or more is preferable, 2% or more is more preferable, and 3% or more is even more preferable. Also, 10% or less is preferable, 8% or less is more preferable, and 6% or less is even more preferable. Further, 1 - 10% is preferable, 2 - 8% is more preferable, and 3 - 6% is even more preferable. Within this range, it is more preferable because the uniformity of the coating film is more excellent.

[0056] [Component (E)] The present invention can further contain an oil agent (excluding the above components (B) and (D)) with a refractive index of 1.48 or more for component (E). As long as the refractive index of component (E) is 1.48 or more, the chemical species is not particularly limited, and any of them can be used. For example, polybutene (refractive index 1.48 - 1.51), heavy liquid isoparaffin (refractive index 1.49 - 1.50), tritridecyl trimellitate (refractive index 1.48), di(phytosteryl·2-octyldodecyl) N-lauroyl-L-glutamate (refractive index 1.48), ethylhexyl methoxycinnamate (refractive index 1.50), macadamia nut oil (refractive index 1.47), castor oil (refractive index 1.48), rice bran oil (refractive index 1.47), safflower oil (refractive index 1.47), sunflower oil (refractive index 1.47), olive oil (refractive index 1.47), rapeseed oil (refractive index 1.47), jojoba oil (refractive index 1.47), meadowfoam oil (refractive index 1.47), etc. can be mentioned. In addition, the refractive index in the present invention is measured by a hand-held refractometer R-5000 (manufactured by Atago Co., Ltd.).

[0057] From the viewpoints of the uniformity of the coating film and the absence of a white film feeling, tritridecyl trimellitate (refractive index 1.48) is preferable for component (E).

[0058] The content of component (E) in the present invention is not particularly limited, and is preferably 2% or more, more preferably 5% or more, and even more preferably 10% or more, based on the total amount of the solid powder cosmetic. Also, it is preferably 35% or less, more preferably 32% or less, and even more preferably 30% or less. Further, 2 - 35% is preferable, 5 - 32% is more preferable, and 10 - 30% is even more preferable. If it is within this range, it is more preferable because the uniformity of the coating film is more excellent.

[0059] [Component (F)] The present invention can further contain component (F), a surfactant. As long as it is a surfactant usually used in cosmetics, it is not particularly limited, and any of them can be used regardless of being nonionic or ionic. For example, nonionic surfactants, anionic surfactants, cationic surfactants, ionic surfactants such as amphoteric surfactants, etc. can be mentioned.

[0060] Examples of nonionic surfactants include glycerin fatty acid esters or their alkylene glycol adducts, polyglycerin fatty acid esters or their alkylene glycol adducts, propylene glycol fatty acid esters or their alkylene glycol adducts, sorbitan fatty acid esters or their alkylene glycol adducts, sorbitol fatty acid esters or their alkylene glycol adducts, polyalkylene glycol fatty acid esters, sucrose fatty acid esters, polyoxyalkylene alkyl ethers, polyoxyethylene alkyl ether phosphates, glycerin alkyl ethers, polyoxyethylene alkyl phenyl ethers, polyoxyethylene hydrogenated castor oil, alkylene glycol adducts of lanolin, polyoxyalkylene alkyl co-modified silicones, polyether-modified silicones, and the like.

[0061] Examples of anionic surfactants include inorganic and organic salts of fatty acids such as stearic acid and lauric acid, alkylbenzene sulfates, alkyl sulfonates, α-olefin sulfonates, dialkyl sulfosuccinates, α-sulfonated fatty acid salts, acylmethyl taurine salts, N-methyl-N-alkyl taurine salts, polyoxyethylene alkyl ether sulfates, polyoxyethylene alkyl phenyl ether sulfates, alkyl phosphates, polyoxyethylene alkyl ether phosphates, polyoxyethylene alkyl phenyl ether phosphates, N-acyl amino acid salts, N-acyl-N-alkyl amino acid salts, ο-alkyl-substituted malates, alkyl sulfosuccinates, and the like.

[0062] Examples of cationic surfactants include alkylamine salts, polyamines and alkanolamine fatty acid derivatives, alkyl quaternary ammonium salts, cyclic quaternary ammonium salts, and the like.

[0063] Examples of amphoteric surfactants include carbobetaine-type amphoteric surfactants such as coconut oil fatty acid amide propyl betaine, octyldimethylaminoacetic acid betaine, lauryldimethylaminoacetic acid betaine, lauric acid amide propyl betaine, coconut oil fatty acid alkyldimethylaminoacetic acid betaine, myristyldimethylaminoacetic acid betaine, cetyl dimethylaminoacetic acid betaine, coconut oil fatty acid amide propyl dimethylaminoacetic acid betaine, lauric acid amide propyl dimethylaminoacetic acid betaine, lauryldihydroxyethylaminoacetic acid betaine, cetyl dihydroxyethylaminoacetic acid betaine; sulfobetaine-type amphoteric surfactants such as coconut oil alkyl sulfobetaine, lauryl sulfobetaine; ampho(di)acetic acid-type amphoteric surfactants such as 2-alkyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, N-coconut oil fatty acid acyl-N-carboxymethoxyethyl-N-carboxymethylethylenediamine disodium; alkyliminodicarboxylate-type amphoteric surfactants such as sodium laurylaminodiacetate, sodium coconut oil alkylaminodiacetate, sodium laurylaminodipropionate; amino acid-based amphoteric surfactants such as N-[3-alkyl(12,14)oxy-2-hydroxypropyl]-L-arginine hydrochloride, etc.

[0064] From the viewpoint of the absence of a white film feeling, it is preferable to use a nonionic surfactant for component (F), and one or more selected from the group consisting of polyglycerol fatty acid esters, sorbitan fatty acid esters, and sucrose fatty acid esters are more preferable, one or more selected from the group consisting of polyglycerol fatty acid esters and sorbitan fatty acid esters are even more preferable, and sorbitan fatty acid esters are particularly preferable.

[0065] Among sorbitan fatty acid esters, from the viewpoint of the absence of a white film feeling, one or more selected from the group consisting of sorbitan monooleate, sorbitan sesquioleate, sorbitan monostearate, sorbitan monoisostearate, sorbitan sesquistearate, and sorbitan sesquisoisostearate are preferable, one or more selected from the group consisting of sorbitan monostearate, sorbitan monoisostearate, sorbitan sesquistearate, and sorbitan sesquisoisostearate are more preferable, sorbitan sesquistearate and sorbitan sesquisoisostearate are even more preferable, and sorbitan sesquisoisostearate is particularly preferable.

[0066] The content of the component (F) in the present invention is not particularly limited, and is preferably 0.1% or more, more preferably 0.5% or more, and even more preferably 1% or more with respect to the total amount of the solid powder cosmetic. Also, it is preferably 4% or less, more preferably 3% or less, and even more preferably 2.5% or less. Further, 0.1 to 4% is preferable, 0.5 to 3% is more preferable, and 1 to 2.5% is even more preferable. Within this range, it is more preferable because it is more excellent in the absence of a white film feeling.

[0067] In the solid powder cosmetic of the present invention, the content mass ratio (total amount of oil agents / total amount of powders) of the total amount of oil agents containing the component (B) to the total amount of powders containing the component (C) is 0.05 to 1.5. The total amount of powders is the sum of the component (C) and powders other than the component (C). The total amount of oil agents is the sum of the component (B) and oil agents other than the component (B). Examples of the oil agents other than the component (B) include the component (D), (E), and the solvent of the component (A) when used as a solution, and further include oil agents other than the components (B), (D) to (E). (Total amount of oil agents / total amount of powders) is not particularly limited as long as it is within the above range, and from the viewpoint of the absence of a white film feeling, 0.08 or more is preferable, 0.1 or more is more preferable, and 0.15 or more is even more preferable. Also, from the viewpoints of the uniformity of the coating film and the absence of sagging, 1.3 or less is preferable, 1.2 or less is more preferable, and 1 or less is even more preferable. Also, 0.08 to 1.3 is preferable, 0.1 to 1.2 is more preferable, and 0.15 to 1 is even more preferable.

[0068] The powdery substances other than the component (C) used in the present invention are not particularly limited as long as they are commonly used in cosmetics, and any of them can be used. Specifically, white inorganic pigments such as titanium oxide, zinc oxide, cerium oxide, and barium sulfate; colored inorganic pigments such as iron oxide, carbon black, titanium-titanium oxide sintered product, chromium oxide, chromium hydroxide, navy blue, and ultramarine blue; talc, muscovite, phlogopite, biotite, synthetic mica, sericite (sericite), synthetic sericite, kaolin, silicon carbide, bentonite, smectite, aluminum oxide, magnesium oxide, zirconium oxide, antimony oxide, diatomaceous earth, aluminum silicate, magnesium aluminum metasilicate, calcium silicate, barium silicate, magnesium silicate, calcium carbonate, magnesium carbonate, zinc stearate, hydroxyapatite, boron nitride, anhydrous silicic acid, etc. white extender powders; copolymer resins such as polyamide resins, polyethylene resins, polyacrylic resins, polyester resins, fluorine resins, cellulose resins, polystyrene resins, styrene-acrylic copolymer resins; organic polymer resin powders such as polypropylene resins, urethane resins; organic low-molecular powders such as N-acyl lysine; natural organic powders such as silk powder, cellulose powder, dextrin powder; organic pigment powders such as zirconium, barium or aluminum lakes of Red No. 201, Red No. 202, Red No. 205, Red No. 226, Red No. 228, Orange No. 203, Orange No. 204, Blue No. 404, Yellow No. 401, etc., and Red No. 3, Red No. 104, Red No. 106, Orange No. 205, Yellow No. 4, Yellow No. 5, Green No. 3, Blue No. 1, etc.; composite powders such as titanium oxide-containing silicon dioxide, zinc oxide-containing silicon dioxide; fibers such as nylon, polyester, rayon, cellulose, etc. These can be used alone or in combination of two or more. Further, these may be surface-treated with a fluorine compound, silicone oil, powder, oil agent, gelling agent, emulsion polymer, surfactant, etc.

[0069] As the oil agents other than the components (B), (D) to (E) used in the present invention, those usually used in cosmetics are not particularly limited, and any of them can be used. For example, hydrocarbon oils, ester oils, fatty acids, higher alcohols, fluorine-based oils, etc. can be mentioned, and one or more of these can be used. For example, waxes such as beeswax, carnauba wax, candelilla wax, cotton wax, shellac wax, Japan wax, hardened oil, etc.; mineral waxes such as ozokerite, ceresin, paraffin wax, microcrystalline wax, etc.; synthetic waxes such as polyethylene wax, Fischer-Tropsch wax, ethylene-propylene copolymer, etc.; hydrocarbon oils such as petrolatum, liquid paraffin, heavy liquid isoparaffin, squalane, polyisobutylene, polybutene, decane, dodecane, isododecane, isohexadecane, etc.;Diisobutyl adipate, 2-hexyldecyl adipate, di-2-heptylundecyl adipate, cetyl 2-ethylhexanoate, stearyl 2-ethylhexanoate, isostearyl 2-ethylhexanoate, glyceryl tri(caprylate / caprate), neopentyl glycol dicaprate, propylene glycol dicaprate, glyceryl tri-2-ethylhexanoate, pentaerythrityl tetra-2-ethylhexanoate, polyglyceryl-10 deca-2-ethylhexanoate, isotridecyl isononanoate, isononyl isononanoate, diisopropyl sebacate, di-2-ethylhexyl sebacate, isopropyl myristate, octyldodecyl myristate, isostearyl myristate, myristyl myristate, isopropyl palmitate, cetyl palmitate, 2-ethylhexyl palmitate, 2-ethylhexyl stearate, octyldodecyl isostearate, isostearyl isostearate, 2-ethylhexyl isostearate, isopropyl isostearate, octyldodecyl stearoyl stearate, polyglyceryl-2 isostearate, polyglyceryl-2 diisostearate, polyglyceryl-2 triisostearate, polyglyceryl-2 tetraisostearate, dipentaerythrityl tetraisostearate, polyglyceryl-10 decaisostearate, oleyl oleate, octyldodecyl oleate, decyl oleate, triethyl citrate, di-2-ethylhexyl succinate, diisostearyl malate, etc. ester oils; fatty acids such as palmitic acid, stearic acid, behenic acid, isostearic acid, oleic acid, linoleic acid, linolenic acid; higher alcohols such as behenyl alcohol, cetyl alcohol, stearyl alcohol, oleyl alcohol, isostearyl alcohol, octyldodecanol, decyltetradecanol; fluorine-based oils such as perfluorodecane, perfluorooctane, perfluoropolyether; etc. are mentioned, and one or more of these can be used.;

[0070] In addition to the above components, the solid powder cosmetic of the present invention can contain components used in ordinary cosmetics as necessary within a range that does not impair the effects of the present invention. For example, it can contain oil agents other than components (B), (D), and (E), powders other than component (C), water-soluble polymers, film-forming agents other than component (A), ultraviolet absorbers, antioxidants, pH adjusters, chelating agents, beauty components, preservatives, fragrances, cooling agents, etc.

[0071] The solid powder cosmetic of the present invention is produced by mixing a cosmetic base and a solvent to form a slurry, filling this into a container, and then removing the solvent. Here, the cosmetic base refers to a mixture obtained by mixing the above components (A) to (C), components (D) to (F) as necessary, and other components. The method for obtaining the cosmetic base and the like is not particularly limited and can be produced by a generally known method. Specifically, a cosmetic base in which components (A) to (C), and components (D) to (F) as necessary, and other optional components are uniformly dispersed can be obtained. After mixing the cosmetic base and the solvent to form a slurry, filling this into a container, and then removing part or all of the solvent while performing compression molding, a solid powder cosmetic can be obtained. The solvent is not particularly limited, and for example, water, ethanol, aqueous solvents such as ethanol-water, volatile oil agents such as isododecane, non-volatile oil agents such as cetyl 2-ethylhexanoate, etc. can be used. In the present invention, isododecane is preferably used as the solvent. Also, if necessary, drying may be performed after compression molding. The drying temperature and drying time are not particularly limited and can be appropriately changed according to the solvent used.

[0072] The solid powder cosmetic of the present invention can be used as cosmetics for various purposes. For example, there are listed makeup cosmetics such as eyeshadow, eyebrow, foundation, base, concealer, face powder, blusher, lipstick, etc. Among these, from the viewpoint of smear resistance, eyeshadow and eyebrow are preferred.

[0073] In addition, the present invention can also take the following configuration. [1] The following components (A) to (C); (A) A crosslinked organosilicon resin which is an addition reaction product of the following components (X) and (Y), and which generates hydrogen gas per unit mass of the crosslinked organosilicon resin at standard conditions in an amount of 1.5 mL / g or less. (B) Silicone oil that is liquid at 25°C (C) Glitter powder A solid powder cosmetic is obtained by mixing a cosmetic base containing the above-mentioned component (C) and a solvent to form a slurry, in which the mass ratio of the total amount of oils including component (B) to the total amount of powder including component (C) (total amount of all oils / total amount of all powders) is 0.05 to 1.5, filling this into a container, and then removing the solvent. (X) An alkenyl-containing organosilicon resin represented by the following formula (1) and having one or more alkenyl groups in each molecule: [ka] [In the formula, R 1 are each independently an alkenyl group having 2 to 8 carbon atoms; R 2 are each independently a group selected from an alkyl group having 1 to 30 carbon atoms, an aryl group having 6 to 30 carbon atoms, and an aralkyl group having 7 to 30 carbon atoms. 3 are each independently an organopolysiloxane-containing group, and the R 2 Each R 3 3SiO 1 / 2 R in units 3 At least one of a1, a2, a3, b, c, and d is an organopolysiloxane-containing group. <a1≦5、0<a2≦400、0≦a3≦400、0≦b≦320、0≦c≦320、0<d≦1,000であり、かつ、0.5≦(a1+a2+a3) / d≦1.5を満たす数である。] (Y) an organohydrogenpolysiloxane having two or more hydrosilyl groups per molecule, represented by the following formula (2): an amount of hydrosilyl groups of 0.5 to 1.2 moles per mole of alkenyl groups in the above component (X) [ka] [In the formula, R 2 is the same as above, and R4 are, independently of each other, a hydrogen atom or a group represented by the above R 2 wherein two or more of all R's 4 are hydrogen atoms, and e, f, g, and h are 0 or positive numbers, provided that 2 ≦ e + f + g + h < 32 is satisfied.] [2] The solid powder cosmetic according to [1], wherein the kinematic viscosity of the component (B) at 25°C is 1,000 CS or less. [3] The solid powder cosmetic according to [1] or [2], wherein the average particle diameter of the component (C) is 10 to 250 μm. [4] The solid powder cosmetic according to any one of [1] to [3], further containing an oily agent in a paste form at 25°C as the component (D). [5] The solid powder cosmetic according to any one of [1] to [4], further containing an oily agent (excluding the components (B) and (D)) having a refractive index of 1.48 or more as the component (E). [6] The solid powder cosmetic according to any one of [1] to [5], further containing a surfactant as the component (F).

Examples

[0074] Hereinafter, the present invention will be described in more detail by way of examples and comparative examples, but the present invention is not limited to the following examples.

[0075] In addition, in the following, the alkenyl group-containing organosilicon resin as a raw material is synthesized according to a known production method. In the following production examples and comparative examples, the reaction rate of the alkenyl group is 1 determined by calculation based on the remaining amount of the alkenyl group after the reaction by H-NMR spectrum analysis.

[0076] [Production Example 1] Method for producing a crosslinked organosilicon resin / 30% solution of decamethylcyclopentasiloxane 1,000 g of a 50% solution of a powdery alkenyl group-containing organosilicon resin (weight average molecular weight: 7,430, vinyl value: 0.229 mmol / g) represented by the following average compositional formula (E1) in decamethylcyclopentasiloxane, 700 g of decamethylcyclopentasiloxane, 126.9 g of an organopolysiloxane having hydrosilyl groups at both ends represented by the following formula (E2) (hydrogen gas generation amount: 20.3 mL / g, hydrosilyl group / vinyl group = 1.0), and 0.6 g of a 0.5% solution of chloroplatinic acid in 2-propanol were charged into a reactor and reacted by heating at 120°C for 8 hours. Thereafter, the solvent was distilled off by heating under reduced pressure. After adjusting by adding decamethylcyclopentasiloxane so that the concentration became 30%, filtration was performed to obtain a decamethylcyclopentasiloxane solution of a crosslinked organosilicon resin.

[0077] Further, the product obtained by heating the decamethylcyclopentasiloxane solution of the crosslinked organosilicon resin obtained under reduced pressure to 120 to 130°C to remove decamethylcyclopentasiloxane was a solid powder (weight average molecular weight 221,000). The reaction rate of the alkenyl group was 92%, and the amount of hydrogen gas generated from the remaining hydrosilyl groups was 0.8 mL / g. Formula (E1): [Chemical formula] Formula (E2): [Chemical formula]

[0078] [Production Example 2] Method for producing a 30% solution of a crosslinked organosilicon resin in decamethylcyclopentasiloxane 1,000 g of a 50% solution of a powdery alkenyl group-containing organosilicon resin (weight average molecular weight: 8,050, vinyl value: 0.224 mmol / g) represented by the following average compositional formula (E3) in decamethylcyclopentasiloxane, 700 g of decamethylcyclopentasiloxane, 53.8 g of an organopolysiloxane having hydrosilyl groups at both ends represented by the following formula (E4) (hydrogen gas generation amount: 51.3 mL / g, hydrosilyl group / vinyl group = 1.1), and 0.6 g of a 0.5% solution of chloroplatinic acid in 2-propanol were charged into a reactor and reacted by heating at 110°C for 5 hours. Thereafter, the solvent was distilled off by heating under reduced pressure. After adjusting by adding decamethylcyclopentasiloxane so that the concentration became 30%, filtration was performed to obtain a solution of a crosslinked organosilicon resin in decamethylcyclopentasiloxane.

[0079] Further, the product obtained by heating the obtained solution of the crosslinked organosilicon resin in decamethylcyclopentasiloxane to 120 to 130°C under reduced pressure to remove decamethylcyclopentasiloxane was a solid powder (weight average molecular weight: 154,000). The reaction rate of the alkenyl group was 93%, and the amount of hydrogen gas generated from the remaining hydrosilyl groups was 1.0 mL / g. Formula (E3): [Chemical formula] Formula (E4): [Chemical formula]

[0080] [Production Example 3] Method for producing a 30% solution of a crosslinked organosilicon resin / decamethylcyclopentasiloxane 1,000 g of a 50% solution of a powdery alkenyl group-containing organosilicon resin (weight average molecular weight 14,860, vinyl value: 0.323 mmol / g) represented by the following average compositional formula (E5) in decamethylcyclopentasiloxane, 700 g of decamethylcyclopentasiloxane, 160.0 g of an organopolysiloxane having hydrosilyl groups at both ends represented by the following formula (E6) (hydrogen gas generation amount: 22.6 mL / g, hydrosilyl group / vinyl group = 1.0), and 0.6 g of a 0.5% solution of chloroplatinic acid in 2-propanol were charged into a reactor and reacted by heating at 110 °C for 3 hours. Thereafter, the solvent was distilled off by heating under reduced pressure. After adjusting by adding decamethylcyclopentasiloxane so that the concentration became 30%, filtration was performed to obtain a solution of a crosslinked organosilicon resin in decamethylcyclopentasiloxane.

[0081] Further, the product obtained by heating the solution of the crosslinked organosilicon resin in decamethylcyclopentasiloxane under reduced pressure to 120 to 130 °C and removing decamethylcyclopentasiloxane was a solid powder (weight average molecular weight 168,500). The reaction rate of the alkenyl group was 92%, and the amount of hydrogen gas generated from the remaining hydrosilyl groups was 0.5 mL / g. Formula (E5): [Chemical formula] Formula (E6): [Chemical formula]

[0082] [Production Example 4] Production method of crosslinked organosilicon resin / 30% solution of decamethylcyclopentasiloxane 1,000 g of a 50% solution of a powdery alkenyl group-containing organosilicon resin (weight average molecular weight 11,730, vinyl value: 0.307 mmol / g) represented by the following average compositional formula (E7) in decamethylcyclopentasiloxane, 700 g of decamethylcyclopentasiloxane, 78.5 g of an organopolysiloxane having hydrosilyl groups at both ends represented by the following formula (E8) (hydrogen gas generation amount: 43.8 mL / g, hydrosilyl group / vinyl group = 1.0), and 0.6 g of a 0.5% solution of chloroplatinic acid in 2-propanol were charged into a reactor and reacted by heating at 120 °C for 5 hours. Thereafter, the solvent was distilled off by heating under reduced pressure. After adjusting by adding decamethylcyclopentasiloxane so that the concentration became 30%, filtration was performed to obtain a solution of a crosslinked organosilicon resin in decamethylcyclopentasiloxane.

[0083] Further, the solution of the obtained crosslinked organosilicon resin in decamethylcyclopentasiloxane was heated to 120 to 130 °C under reduced pressure to remove decamethylcyclopentasiloxane, and the resulting product was a solid powder (weight average molecular weight 96,500). The reaction rate of the alkenyl group was 97%, and the amount of hydrogen gas generated from the remaining hydrosilyl groups was 0.9 mL / g. Formula (E7): [Chemical formula] Formula (E8): [Chemical formula]

[0084] Examples 1 to 20 and Comparative Examples 1 to 7: Solid powder eyeshadow Solid powder eyeshadows having the compositions shown in Tables 1 to 3 were prepared by the following production method, and evaluated and judged for the uniformity of the coating film, freedom from bleeding, and freedom from a white film feeling by the following evaluation methods and criteria, and the results are shown in Tables 1 to 3 together.

[0085] [Table 1]

[0086]

Table 2

[0087]

Table 3

[0088] *1: The solid powder obtained in Production Example 1 was dissolved in isododecane at 110°C and cooled to room temperature to obtain a solution (solid content 50%) *2: SILFORM FLEXIBLE RESIN (manufactured by Momentive Performance Materials Japan) *3: KF-96-10CS (manufactured by Shin-Etsu Chemical Co., Ltd.) *4: KF-96-100CS (manufactured by Shin-Etsu Chemical Co., Ltd.) *5: KF-96-1000CS (manufactured by Shin-Etsu Chemical Co., Ltd.) *6: DC2503 (melting point 28-35°C) (manufactured by Dow Corning Toray Co., Ltd.) *7: Estol DISM (viscosity 5000 mPa·s / 25°C) (manufactured by National Maisu Co., Ltd.) *8: HELIOS R100G (manufactured by Topi Industries) *9: FLAMENCO GOLD220C (manufactured by BASF) *10: Micro Glass Metashine MT1200RY (manufactured by Nippon Sheet Glass Co., Ltd.) *11: Bengal: A mixture of yellow iron oxide:black iron oxide = 0.6:1:0.4

[0089] (Manufacturing method) A. Components (18) to (23) are uniformly mixed. B. Components (6) to (17) are heated and mixed at 80°C. C. B is added to A and uniformly mixed. D. Components (1) to (5) are added to C and mixed to obtain a cosmetic base. E. 15 parts by mass of isododecane is added to 85 parts by mass of D, mixed and kneaded to form a slurry, and filled into a gold dish container. Absorbent paper was placed on the surface of F.E., pressed to remove some or all of the solvent, and dried at 70 °C for 8 hours to obtain a solid powder eyeshadow.

[0090] [Evaluation Method 1] (Evaluation Items: Uniformity of the coating film, absence of white film feeling) For each sample, 20 professional cosmetics evaluation panelists evaluated the "uniformity of the coating film" and the "absence of white film feeling" when applying each sample on a scale of 7 according to the following absolute evaluation criteria. Furthermore, using the average score of all panelists, the determination was made according to the following determination criteria. Note that the "uniformity of the coating film" was evaluated from the perspective of whether it spreads uniformly when applying the sample, and the "absence of white film feeling" was evaluated from the perspective of whether a transparent cosmetic film with a uniform color and no blurring can be formed at the film thickness.

[0091] (Absolute Evaluation Criteria) (Score): (Evaluation) 6: Very good 5: Good 4: Slightly good 3: Ordinary 2: Slightly bad 1: Bad 0: Very bad

[0092] (Determination Criteria) (Determination): (Average score) ◎: Exceeding 5 points: Very good ○: Exceeding 3.5 points and below 5 points: Good △: Exceeding 2 points and below 3.5 points: Slightly bad ×: 2 points or less: Bad

[0093] [Evaluation Method 2] (Evaluation Item: Absence of sagging) Each sample is applied to 5 professional panels for cosmetic evaluation, and the same amount of each sample is applied to the panels. Images of the eyelids immediately after applying the sample and images of the eyelids after 100 blinks are obtained using VISIA-CR (manufactured by Canfield Scientific) as frontal face images. For the acquired images, a portion with a certain area (vertical 180 × horizontal 25 pixels) is cut out at three points: the outer corner of the eye, the center, and the inner corner of the eye. The difference in the L value between the initial image and the image after 100 blinks is detected by image analysis, and is plotted with the change amount of the L value on the vertical axis and the pixel on the horizontal axis. The area under the curve is calculated, and the sum is used as the change amount for evaluation.

[0094] (Judgment Criteria) (Judgment): (Analysis Results) ◎: The change amount is 999 or less ○: The change amount is 1000 - 1499 △: The change amount is 1500 - 1999 ×: The change amount is 2000 or more

[0095] As is clear from the results in Tables 1 to 3, the solid powder eyeshadow of the examples was excellent in all items of i. uniformity of the coating film, ii. lack of sagging, and iii. lack of white film feeling. On the other hand, in Comparative Example 1 using trimethylsiloxysilicic acid instead of component (A), the start was hard and lacked spreadability, and the uniformity of the coating film could not be achieved, and satisfactory results in terms of lack of sagging and lack of white film feeling could not be obtained. In Comparative Example 2 using polymethylsilsesquioxane instead of component (A), satisfactory results in terms of the uniformity of the coating film and lack of sagging could not be obtained. In Comparative Example 3 not containing component (B), satisfactory results in terms of lack of sagging and lack of white film feeling could not be obtained, and the uniformity of the coating film was inferior. Further, in Comparative Example 4 using stearyldimethylsilicone instead of component (B), the pick-up at the start was poor, and in addition to lack of sagging, the uniformity of the coating film was also inferior, and satisfactory results in terms of lack of white film feeling could not be obtained. In Comparative Example 5 not containing component (C), there was a tendency for the oil agent to not escape during molding and for caking to occur, and it was inferior in terms of the uniformity of the coating film and lack of white film feeling, and there was a tendency for lack of sagging to be less noticeable. In Comparative Example 6 where the content mass ratio of (total amount of all oil agents / total amount of all powder) was less than 0.05, aggregation of the powders was likely to occur, and it was inferior in terms of lack of white film feeling, and satisfactory results in terms of the uniformity of the coating film and lack of sagging could not be obtained. In Comparative Example 7 where the content mass ratio of (total amount of all oil agents / total amount of all powder) exceeded 1.5, the whole system became soft due to the oil agent, and it was inferior in terms of the uniformity of the coating film and lack of sagging, and satisfactory results in terms of lack of white film feeling could not be obtained.

[0096] Example 21: Eyebrow (Slurry) A powder foundation of the slurry method was produced according to the following formulation and production method. (Component) (%) 1. Crosslinked organosilicon resin / isododecane 50% solution of Production Example 1 5.0 2. Dimethylpolysiloxane (kinematic viscosity at 25°C 10 CS) 4.0 3. Tritridecyl trimellitate (refractive index 1.48) 15.0 4. Petrolatum (melting point 55°C) 5.0 5. Sorbitan sesquisoisostearate 1.0 6. Mica Titanium (average particle size 40 μm) *12 10.0 7. Iron Oxide-Coated Mica Titanium (average particle size 30 μm) *13 10.0 8. Titanium Oxide-Coated Glass Powder (average particle size 120 μm) *14 5.0 9. Titanium Dioxide (average particle size 250 nm) 1.5 10. Spherical Cellulose (average particle size 10 μm) 8.0 11. Spherical Silica (average particle size 9 μm) 1.5 12. Mica 20.0 13. Chlorphenesin 0.2 14. Kunzite 0.5 15. Red Ochre 3.0 16. Yellow Iron Oxide 3.0 17. Black Iron Oxide 2.0 18. Talc balance *12: COSMETICA SUPER WHITE N-8000S (manufactured by CQV) *13: GEMTONE TAN OPAL G005 (manufactured by BASF) *14: Micro Glass Metashine MT1120RY (manufactured by Nippon Sheet Glass Co., Ltd.)

[0097] (Manufacturing method) A. Mix components 6 to 18 uniformly with a super mixer. B. Add to A the mixture obtained by uniformly mixing components 1 to 5 at 60°C, add 10 parts of isododecane and mix to obtain a slurry-like mixture. C. Fill 1.8 g of the above mixture into a gold dish (diameter 2.5 cm), compress twice under the conditions of a pressing pressure of 2.0 kgf / cm 2 , a pressing time of 3 seconds, and 4 sheets of paper to remove part of the isododecane. Then, dry at 70°C for one day and night to remove the isododecane and obtain an eyebrow powder.

[0098] The obtained eyebrow powder (slurry) was excellent in all aspects such as the uniformity of the coating film, the absence of streaks, and the absence of a white film feeling.

[0099] Example 22: Powder Foundation (Slurry) A powder foundation by the slurry process was manufactured according to the following formulation and manufacturing method. (Ingredient) (%) 1. Crosslinked organosilicon resin of Production Example 1 / Decamethylcyclopentasiloxane 30% solution 4.0 2. Diphenylsiloxyphenyltrimethicone 8.0 3. Dimethylpolysiloxane (kinematic viscosity at 25°C: 2 cSt) 0.5 4. Dimethylpolysiloxane (kinematic viscosity at 25°C: 10 cSt) 2.0 5. Isotridecyl isononanoate (refractive index 1.44) 5.0 6. Petrolatum (melting point 55°C) 1.0 7. Silicone 3% - treated zinc oxide 5.0 8. Mica titanium *15 5.0 9. Titanium dioxide coated with iron oxide (average particle diameter 400 nm) 10.0 10. Boron nitride (average particle diameter 6 μm) 8.0 11. Spherical silica (average particle diameter 8 μm) 10.0 12. Lauroyl lysine 4.0 13. Mica (average particle diameter 20 μm) 10.0 14. Chlorphenesin 0.2 15. Bismuth oxychloride 5.0 16. Cinnabar 0.5 17. Yellow iron oxide 1.7 18. Black iron oxide 0.15 19. Talc balance *15: COSMETICA FINE WHITE N - 8000D (manufactured by CQV Co., Ltd.)

[0100] (Manufacturing method) A. Mix 7 to 19 uniformly with a super mixer. B. Add the mixture obtained by uniformly mixing components 1 to 6 at 60°C to A, disperse uniformly, pulverize, and obtain a cosmetic base. C. Add 50 parts of isododecane to 100 parts of the said cosmetic base, mix, and obtain a slurry - like mixture. D. Fill 11 g of the mixture into a round gold dish (diameter 5.5 cm), and compress it 4 times under the conditions of a pressing pressure of 2.0 kgf / cm 2 , a pressing time of 4 seconds, and 6 sheets of paper, and partially remove isododecane. E. Dry D at 70 °C for one day and night to remove isododecane and obtain a powder foundation (slurry).

[0101] The obtained powder foundation (slurry) was excellent in all aspects such as the uniformity of the coating film, the absence of streaks, and the absence of a white film feeling.

[0102] Example 23: Teak Color (Slurry) A teak color was produced according to the following formulation and production method. (Component) (%) 1. Glyceryl 2-ethylhexanoate (refractive index 1.44) 5.0 2. (Dimethicone / Vinyldimethicone) Crosspolymer 2.0 3. Dimethylpolysiloxane (kinematic viscosity at 25 °C 10 CS) 26.0 4. Hydrogenated polyisobutene (refractive index 1.49) 6.0 5. Vaseline (melting point 55 °C) 2.0 6. Crosslinked silicone-network silicone block copolymer *16 5.0 7. Titanium oxide-coated synthetic phlogopite (average particle diameter 10 μm) *17 3.0 8. Titanium oxide-coated synthetic phlogopite (average particle diameter 100 μm) *18 3.0 9. Mica titanium (average particle diameter 20 μm) *19 7.0 10. Spherical silica (average particle diameter 5 μm) 4.0 11. Titanium dioxide (average particle diameter 250 nm) 5.0 12. Red No. 226 0.5 13. Red iron oxide 0.5 14. Yellow iron oxide 0.3 15. Talc balance *16: KSP-100 (manufactured by Shin-Etsu Chemical Co., Ltd.) *17: HELIOS R10R (manufactured by Toppy Industries, Ltd.) *18: HELIOS R100R (manufactured by Topi Industries Co., Ltd.) *19: COSMETICA SUPER RED N-5401S (manufactured by CQV Co., Ltd.)

[0103] (Manufacturing method) A. Ingredients 6 - 15 are uniformly dispersed with a Henschel mixer (manufactured by Mitsui Miike Co., Ltd.). B. Ingredients 1 - 5 are uniformly mixed at 60°C. C. While stirring A with a Henschel mixer, add B and uniformly disperse them. D. Grind C with a pulverizer. E. Mix 30 parts by mass of isododecane with 100 parts by mass of D to obtain a slurry-like mixture. F. Fill E into a gold dish, compress it to remove isododecane, and dry it to obtain a solid powder-like cheek color (slurry).

[0104] The obtained cheek powder (slurry) was excellent in all aspects such as the uniformity of the coating film, lack of streaks, and lack of white film feeling.

Claims

Claim 1 The following components (A) to (C); (A) A crosslinked organosilicon resin which is an addition reaction product of the following component (X) and component (Y), wherein the amount of hydrogen gas generated per mass of this crosslinked organosilicon resin is 1.5 mL / g or less under standard conditions. Crosslinked organosilicon resin (B) A silicone oil that is liquid at 25°C (C) A pearlescent powder A solid powder cosmetic obtained by mixing a cosmetic base containing the above components and a solvent to form a slurry, filling this into a container, and then removing the solvent. The content mass ratio (total amount of oil agent / total amount of powder) of the total amount of the oil agent containing the component (B) to the total amount of the powder containing the component (C) is 0.05 to 1.5 (X) An alkenyl group-containing organosilicon resin represented by the following formula (1) and having one or more alkenyl groups in one molecule 【Chemical 1】 [In the formula, R １ are each independently an alkenyl group having 2 to 8 carbon atoms; R ２ are each independently a group selected from an alkyl group having 1 to 30 carbon atoms, an aryl group having 6 to 30 carbon atoms, and an aralkyl group having 7 to 30 carbon atoms. ３ are each independently an organopolysiloxane-containing group, and the R ２ Each R ３ ３ SiO １／２ R in units ３ At least one of the above is an organopolysiloxane-containing group. a1, a2, a3, b, c, and d are numbers that satisfy 0<a1≦5, 0<a2≦400, 0≦a3≦400, 0≦b≦320, 0≦c≦320, and 0<d≦1,000, and 0.5≦(a1+a2+a3) / d≦1.

5. (Y) An organohydrogenpolysiloxane represented by the following formula (2) and having two or more hydrosilyl groups in one molecule: an amount such that the amount of hydrosilyl groups is 0.5 to 1.2 moles with respect to 1 mole of the amount of alkenyl groups in the above component (X) 【Chemical 2】 [wherein, R ２ is the same as described above, and R ４ are each independently a hydrogen atom or a group represented by the above R ２ , and two or more of all R ４ are hydrogen atoms, and e, f, g, and h are 0 or positive numbers, provided that 2 ≦ e + f + g + h < 32 is satisfied.] Claim 2 The solid powder cosmetic according to Claim 1, wherein the kinematic viscosity of the component (B) at 25°C is 1,000 CS or less Claim 3 The solid powder cosmetic according to Claim 1 or 2, wherein the average particle diameter of the component (C) is 10 to 250 μm Claim 4 The solid powder cosmetic according to Claim 1 or 2, further containing a paste-like oil agent as component (D) at 25°C Claim 5 The solid powder cosmetic according to Claim 1 or 2, further containing, as component (E), an oil agent (excluding the components (B) and (D)) having a refractive index of 1.48 or more Claim 6 The solid powder cosmetic according to Claim 1 or 2, further containing a surfactant as component (F)

Images