Solid cosmetic

Abstract

To provide a solid cosmetic which is excellent in all of gloss durability, color durability, resistance to breakage of a cosmetic and easy taking up after repeated using.SOLUTION: There is provided a solid composition which contains (A) a partially crosslinked organopolysiloxane polymer, (B) a crosslinked organosilicon resin which is an addition reaction product of the following component (X) and component (Y) and is obtained by addition reaction of the component (Y) in an amount so that the amount of hydrosilyl group is 0.5 to 1.2 moles based on 1 mol of the amount of alkenyl group in the component (X) in which the amount of a hydrogen gas per mass generated from the resin is 1.5 mL / g or less in a standard state, (C) an oil solution which is liquid at 25°C and (D) a powder, wherein the content mass ratio(C) / (D) of the component (C) to the component (D) is 0.60 to 1.60. (X) an alkenyl group-containing organosilicon resin represented by the following formula (1). (Y) an organohydrogenpolysiloxane having two or more hydrosilyl groups in one molecule represented by the following formula (2).SELECTED DRAWING: None

Description

Technical Field

[0001] The present invention relates to solid cosmetics.

Background Art

[0002] Solid cosmetics are in a form that is used in a wide range of products such as base makeup products like foundation and point makeup products like eyeshadow due to their portability and ease of use. Generally, solid cosmetics include water-based solids, oil-based solids, emulsion solids, etc. in which water or oil forms a continuous layer and the liquid is solidified with a solidifying agent, and solid powder dosage forms in which powder forms a continuous layer and the powder is solidified with an excipient, and various studies have been conducted. Among them, cosmetics in the intermediate region between oil-based solids and solid powders where both powder and oil can form continuous layers are a dosage form that attracts attention because they can combine the glossiness and emollient effect of the oil-based dosage form with the light spread and powdery finish of the powder dosage form.

[0003] Technologies that combine the advantages of each dosage form have been developed so far. For example, by containing a specific amount of silicone elastomer, isododecane, film-forming resin, brightening powder, and liquid fatty acid ester oil, a solid cosmetic is disclosed that has good spreadability and elongation during application, is non-greasy, is excellent in makeup persistence and uniformity, and further forms a cosmetic film with excellent visual effects (see, for example, Patent Document 1). In addition, a cosmetic is disclosed that has good usability, good makeup retention, good elongation and finish, and excellent abrasion resistance by containing a specific crosslinked organic silicon resin (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] For example, in the technology of Patent Document 1, the cosmetic film formed after applying the cosmetic to the skin is hard, and although the cosmetic film is less likely to break against external impacts such as hair touching it, it is inferior in flexibility and brittle. For this reason, the cosmetic film may crack due to reasons such as shrinking during film formation or being unable to follow the movement of the skin after film formation. Further, for example, in the technology of Patent Document 2, it is described that the flexibility of a specific crosslinked organosilicon resin film is high, but when applied particularly to solid cosmetics, the expected effects may not be exhibited. Further, Patent Document 2 did not examine the gloss persistence, color persistence, and further, whether an appropriate amount can be taken (ease of taking) when taking the cosmetic from the container with an applicator or finger after repeatedly using the cosmetic.

[0006] Therefore, an object of the present invention is to provide a solid cosmetic having high gloss persistence and color persistence, and in which the cosmetic film formed by the cosmetic is less likely to crack. Another object of the present invention is to provide a solid cosmetic excellent in ease of taking after repeated use.

Means for Solving the Problems

[0007] As a result of intensive studies, the present inventors have found that by containing a silicone elastomer, a specific crosslinked organosilicon resin, an oil agent that is liquid at 25°C, and a powder, and containing the oil agent and the powder in a specific ratio, a solid cosmetic excellent in gloss persistence, color persistence, resistance to cracking of the cosmetic, and ease of taking after repeated use can be obtained, and the present invention has been completed.

[0008] That is, the present invention includes the following forms. [1] The following components (A) to (D); (A) A partially crosslinked organopolysiloxane polymer (excluding component (B)) (B) A crosslinked organosilicon resin which is an addition reaction product of the following components (X) and (Y), wherein the amount of hydrogen gas generated per mass from said crosslinked organosilicon resin is 1.5 mL / g or less under standard conditions, and said component (Y) is added in an amount such that the amount of hydrosilyl groups is 0.5 to 1.2 moles per mole of alkenyl groups in said component (X). (C) Oil that is liquid at 25℃ (D) Powder wherein the mass ratio (C) / (D) of component (C) to component (D) is 0.60 to 1.60. (X) An alkenyl-containing organosilicon resin represented by the following formula (1) and having one or more alkenyl groups in each molecule:

[0009] [ka]

[0010] [In the formula, R 1 is 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)下記式(2)で表され、1分子中にヒドロシリル基を2個以上有するオルガノハイドロジェンポリシロキサン

[0011] [ka]

[0012] [In the formula, 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.] [2] The solid cosmetic according to [1], wherein the component (C) contains an oil agent having a refractive index of 1.48 or more. [3] The solid cosmetic according to [2], wherein the oil agent having a refractive index of 1.48 or more in the component (C) is a phenyl-modified silicone. [4] The solid cosmetic according to any one of [1] to [3], wherein the component (D) contains plate-shaped powder. [5] The solid cosmetic according to [4], wherein the content mass ratio of the plate-shaped powder to the component (D) is 0.5 or more. [6] Furthermore, the solid cosmetic according to any one of [1] to [3], which contains an oil-soluble polyurethane as the component (E). [7] Furthermore, the solid cosmetic according to any one of [1] to [3], which contains inulin fatty acid ester as the component (F).

Advantages of the Invention

[0013] According to the present invention, it is possible to provide a solid cosmetic excellent in gloss persistence, color persistence, crack resistance of the cosmetic, and ease of removal after repeated use.

Modes for Carrying Out the Invention

[0014] The 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 modified within the scope of the present invention. In this specification, "~" means a range including the numerical values before and after it. Further, the "average particle diameter" in the present invention is the value of the median diameter (D50) obtained by measurement using 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 taken as the average particle diameter. In the present invention, component names may be described using cosmetic display names or the International Nomenclature of Cosmetic Ingredient (INCI). When the cosmetic display name and INCI correspond, the English description may be omitted. In this specification, when simply described as "%", it means mass%. Further, when describing the content of each of the following components, when two or more kinds of the components are present, the content refers to the total amount.

[0015] The solid cosmetic of the present invention is excellent in gloss persistence, color persistence, and resistance to cracking of the cosmetic. The gloss formed by the cosmetic is, for example, the luster formed by plate-shaped powder, pearl agent, or oil agent. However, after applying the cosmetic on the skin, for example, due to sebum secretion over time, the optical properties become different from the optical properties originally exhibited by the cosmetic film. For this reason, the gloss decreases over time. Also, in makeup cosmetics, color is mainly imparted by coloring pigments. However, if the coloring pigments cannot continue to adhere to the skin over time, the color persistence decreases. Further, as described above, the cosmetic film may not be maintained by daily movements, leading to cracking of the cosmetic. Since the solid cosmetic is a system in which oils and powders with different properties are intricately intertwined, it is difficult to grasp the behavior of each component. In the present invention, in a solid cosmetic in which component (A) and component (B) and component (C) and component (D) are in a specific ratio, by acting synergistically, the gloss persistence and color persistence in the solid powder cosmetic are achieved, and the resistance to cracking of the cosmetic is also improved. Furthermore, the ease of taking off after repeated use is also improved.

[0016] Hereinafter, each component constituting the present invention will be described.

[0017] [Component (A)] Component (A) in the present invention is a partially crosslinked organopolysiloxane polymer. The partially crosslinked organopolysiloxane polymer is a polymer obtained by crosslinking organopolysiloxane and has a three-dimensional crosslinked structure in part. Component (A) can be obtained, for example, by addition polymerization of (a) an organohydrogenpolysiloxane containing on average 1.5 or more hydrogen atoms bonded to silicon atoms in the molecule and (b) a compound having on average 1.5 or more vinylic reactive sites in the molecule.

[0018] (a) is SiO2 unit, HSiO 1.5 unit, RSiO 1.5 unit, RHSiO unit, R2SiO unit, R3SiO 0.5 unit and R2HSiO 0.5 unit (wherein R is a substituted or unsubstituted monovalent hydrocarbon group having 1 to 30 carbon atoms excluding aliphatic unsaturated groups. The monovalent hydrocarbon group is an alkyl group such as methyl group, ethyl group, propyl group, an aryl group such as phenyl group, tolyl group, an aliphatic unsaturated group such as vinyl group, an aralkyl group in which a hydrogen atom of methyl group, ethyl group, propyl group, etc. is substituted with an aryl group such as phenyl group, tolyl group, a cycloalkyl group such as cyclohexyl group, a halogenated hydrocarbon group containing a fluoro group, a hydrocarbon group containing an ethylene oxide group, a glyceryl group, etc.). It is an organohydrogenpolysiloxane composed of at least one structural unit selected from the group consisting of and containing on average 1.5 or more hydrogen atoms bonded to silicon atoms in the molecule.

[0019] (b) is one or more selected from the following (b-1) to (b-3).

[0020] (b-1) is SiO2 unit, (CH=CH)SiO 1.5 unit, RSiO 1.5units, R(CH2=CH)SiO units, R2SiO units, R3SiO 0.5 units and R2(CH2=CH)SiO 0.5 units (wherein R is a substituted or unsubstituted monovalent hydrocarbon group having 1 to 30 carbon atoms excluding an aliphatic unsaturated group. Examples of the monovalent hydrocarbon group include alkyl groups such as methyl group, ethyl group, and propyl group, aryl groups such as phenyl group and tolyl group, aliphatic unsaturated groups such as vinyl group, aralkyl groups in which a hydrogen atom of methyl group, ethyl group, propyl group, etc. is substituted with an aryl group such as phenyl group and tolyl group, cyclohexyl group, halogenated hydrocarbon groups containing a fluoro group, hydrocarbon groups containing an ethylene oxide group, glyceryl group, etc.). It is an organopolysiloxane composed of at least one kind of structural unit selected from the group consisting of, and containing an average of 1.5 or more vinyl groups bonded to silicon atoms in the molecule.)

[0021] (b-2) is polyoxyalkylene represented by the following general formula (a). C m H 2m-1 O(C2H4O) h (C3H6O) i C m H 2m-1 ···(a) (In the formula, h is an integer of 2 to 200, i is an integer of 0 to 200, h + i is an integer of 3 to 200, and m each represents 2 to 6) (b-3) is an unsaturated hydrocarbon represented by the following general formula (b). C n H 2n-1 (CH2) j C n H 2n-1 ···(b) (However, n is 2 to 6 and j is an integer of 1 or more.).

[0022] Specific examples of component (A) can be appropriately selected and contained one or more of these when represented by INCI names (International Nomenclature Cosmetic Ingredient labeling names). For example, partially crosslinked methylpolysiloxanes such as (dimethicone / vinyl dimethicone) copolymer, and partially crosslinked methylphenylpolysiloxanes such as (dimethicone / phenyldimethylsilicone) copolymer can be mentioned. In addition, examples of polymers containing a polyoxyalkylene group in the molecule include partially crosslinked polyether-modified silicones such as dimethicone / (PEG-10 / 15)) copolymer. Examples of polymers containing a long-chain alkyl group in the molecule include partially crosslinked alkyl-modified silicones such as (vinyldimethylsilicone / lauryldimethylsilicone) copolymer. Examples of polymers containing a polyoxyalkylene group and a long-chain alkyl group in the molecule include partially crosslinked alkyl·polyether copoly-modified silicones such as PEG-15 lauryldimethylsilicone copolymer. Examples of polymers containing a halogenated hydrocarbon group in the molecule include partially crosslinked fluorine-modified silicones such as (trifluoropropyldimethylsilicone / trifluoropropyldivinyldimethylsilicone) copolymer. Examples of polymers containing a glyceryl group in the molecule include partially crosslinked polyglycerol-modified silicones such as (dimethicone / polyglycerin-3) copolymer. These can be used alone or in combination of two or more. In one aspect, component (A) is a partially crosslinked methylpolysiloxane and / or a partially crosslinked alkyl-modified silicone.

[0023] The partially crosslinked organopolysiloxane polymer of component (A) may be contained alone, but is often commercially available as a mixture with an oil agent, and in the present invention, the commercially available product in this state can also be used. For example, KSG-15 (solid content 5%) as a mixture of a partially crosslinked methylpolysiloxane and a cyclic silicone, KSG-16 (solid content 20 - 30%) as a mixture of a partially crosslinked methylpolysiloxane and a dimethylpolysiloxane, KSG-18 (solid content 10 - 20%) as a mixture of a partially crosslinked methylphenylpolysiloxane and a phenyltrimethicone, KSG-210 (solid content 20 - 30%) as a mixture of a partially crosslinked polyether-modified silicone and a dimethylpolysiloxane, KSG-41 (solid content 25 - 35%), KSG-42 (solid content 20 - 30%), KSG-43 (solid content 25 - 35%) and KSG-44 (solid content 25 - 35%) as mixtures of a partially crosslinked alkyl-modified silicone and an oil agent, KSG-310 (solid content 25 - 35%), KSG-320 (solid content 20 - 30%), KSG-330 (solid content 15 - 25%), KSG-340 (solid content 25 - 35%) and KSG-340 (solid content 25 - 35%) as mixtures of a partially crosslinked alkyl-polyether co-modified silicone and an oil agent, the partially crosslinked fluorine-modified silicone is KSG-51 (solid content 15 - 25%) as a mixture with a cyclic fluorine-containing silicone such as a cyclic organopolysiloxane containing a fluoroalkyl group, and KSG-710 (solid content 20 - 25%) as a mixture of a partially crosslinked polyglycerin-modified silicone and a dimethylpolysiloxane (the above are all manufactured by Shin-Etsu Chemical Co., Ltd.), etc. can be mentioned.

[0024] The partially crosslinked organopolysiloxane polymer of component (A) in the present invention does not necessarily have to be swollen with an oil agent that is liquid at 25°C of component (C), but it is more preferable to be present in the cosmetic in a state swollen with an oil agent that is liquid at 25°C of component (C) in terms of more excellent elasticity, dropping strength, etc.

[0025] The content of component (A) in the present invention is not particularly limited, but it is preferably 1% or more, more preferably 2% or more, still more preferably 3% or more, and even more preferably 5% or more based on the total amount of the solid cosmetic. Also, from the viewpoint of good removability after repeated use, the content of component (A) is preferably 15% or less, more preferably 12% or less, and still more preferably 10% or less. Further, the content of component (A) is preferably 1 to 15%, more preferably 3 to 12%, and still more preferably 5 to 10% based on the total amount of the solid cosmetic. Within this range, it is more preferable because the solid cosmetic is less likely to crack and has better removability after repeated use.

[0026] [Component (B)] Hereinafter, component (B) in the present invention will be described in detail.

[0027] Component (B) 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 generated per mass from this crosslinked organosilicon resin is 1.5 mL / g or less under standard conditions. Hereinafter, this crosslinked organosilicon resin will also be simply referred to as "crosslinked organosilicon resin" or "crosslinked organosilicon resin of the present invention".

[0028] [(X) component] The component (X) of the present invention is an alkenyl group-containing organosilicon resin represented by the following average composition formula (1) and having one or more alkenyl groups in one molecule, and can be used alone or in combination of two or more.

[0029] [Chemical formula]

[0030] [In the formula, R 1 is 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 the above R 2 selected from the groups, and 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.] [Component (Y)] Component (Y) of the present invention is represented by the following average composition formula (2), and is preferably an organohydrogenpolysiloxane 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 an amount such that the amount of hydrosilyl groups is 0.5 to 1.2 moles, more preferably 0.8 to 1.2 moles, and even more preferably 0.9 to 1.1 moles, per mole of the alkenyl group amount in the above component (X).

[0031] [Chemical formula]

[0032] [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, and e, f, g, h are 0 or positive numbers, provided that 2 ≤ e + f + g + h < 32 is satisfied.] In the above formula, R 1 is an alkenyl group having 2 to 8 carbon atoms. More specifically, R 1 can include a vinyl group, an allyl group, an isopropenyl group, a butenyl group, a pentenyl group, a hexenyl group, a cyclohexenyl group, an octenyl group, etc. In particular, R 1 is preferably a vinyl group or an allyl group, and more preferably a vinyl group.

[0033] In the above formula, R 2is, independently of one another, 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, R 2 is preferably an alkyl group, aryl group, aralkyl group, or fluorine-substituted alkyl group having 1 to 10 carbon atoms. More specifically, R 2 can be a methyl group, ethyl group, propyl group, butyl group, pentyl group, cyclopentyl group, cyclohexyl group, phenyl group, tolyl group, etc., a trifluoropropyl group, etc. In particular, R 2 is preferably an alkyl group having 1 to 5 carbon atoms, a phenyl group, or a trifluoropropyl group, and R 2 is more preferably an alkyl group having 1 to 5 carbon atoms. Further, optionally, a part of R 2 may contain one or more groups selected from a hydroxyl group or an alkoxy group having 1 to 8 carbon atoms.

[0034] The above R 3 is, independently of one another, an organopolysiloxane-containing group, or a group selected from the above R 2 The organopolysiloxane-containing group includes, for example, groups represented by the following general formulas (3) to (6). R 3 3SiO 1 / 2 In each of the units, one or more R 3 is an organopolysiloxane-containing group. Further, optionally, a part of R 3 may be a hydroxyl group.

[0035]

Chemical formula

[0036] (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.)

[0037] m is an integer satisfying 0 ≦ m ≦ 5, preferably 0 ≦ m ≦ 2, i is an integer satisfying 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.

[0038] In the alkenyl group-containing organosilicon resin represented by the above formula (1), a1 satisfies 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 the film-forming property is also lacking. a2 satisfies 0 ≦ a2 ≦ 400, preferably 0 ≦ a2 ≦ 100, and more preferably 0 ≦ a2 ≦ 50. a3 satisfies 0 ≦ a3 ≦ 400, preferably 0 ≦ a3 ≦ 100, and more preferably 0 ≦ a3 ≦ 50. When a3 is greater than 400, the melting point of the resin becomes low, resulting in a lack of film-forming property. b satisfies 0 ≦ b ≦ 320, c satisfies 0 ≦ c ≦ 320, and 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. d is a number satisfying 0 < d ≦ 1,000 and 0.5 ≦ (a1 + a2 + a3) / d ≦ 1.5, preferably a number satisfying 0.7 ≦ (a1 + a2 + a3) / d ≦ 1.2. When the value of (a1 + a2 + a3) / d is less than the above lower limit, the crosslinking degree increases and the molecular weight becomes large, resulting in a gel state. When it exceeds the above upper limit, the molecular weight becomes small, resulting in a lack of film-forming property.

[0039] The alkenyl group-containing organosilicon resin represented by the above formula (1) has a Q unit (SiO 4 / 2 ), an M unit (R 2 3SiO 1 / 2 and R 1 R 2 2SiO 1 / 2 ) as an essential structure, and a D unit (R 2 2SiO 2 / 2 ), a T unit (R 2 SiO 3 / 2) has a structure of arbitrary configuration. It may be in a solid state or a liquid state at 25°C, but a solid state is preferred from the viewpoint of film-forming property. 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.

[0040] In the organohydrogenpolysiloxane having two or more hydrosilyl groups in one molecule represented by the above formula (2), 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 R 4 are hydrogen atoms. Examples of R 2 in the formula (2), and preferred embodiments and the like are as described above.

[0041] 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, 0 < e or 0 < f. Preferably, g = 0 and h = 0, more preferably e = 2, 0 ≤ f < 30, g = 0, h = 0, and still more preferably e = 2, 0 ≤ f ≤ 20, g = 0, h = 0.

[0042] If the number of silicon atoms contained in the (Y) component is 32 or more, the crosslinked organosilicon resin tends to trap the solvent and the properties tend to become gel-like. Therefore, it tends 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 dissolves in the solvent and the properties tend to become liquid. Therefore, it is easier to obtain a non-sticky film after the solvent volatilizes.

[0043] 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 T units and Q units, and becomes a linear molecule composed only of M units and D units. By using a linear organohydrogenpolysiloxane as a raw material, the crosslinked organosilicon resin as an addition reactant can form a flexible film.

[0044] Also, two or more kinds of 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 kinds of groups represented by the formula (2) having different chain lengths, the film physical properties can be controlled.

[0045] [Physical properties of crosslinked organosilicon resin] The weight average molecular weight of the crosslinked organosilicon resin of the component (B) is preferably 5,000 to 1,000,000, more preferably 8,000 to 500,000, and even more preferably 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 (the same shall apply hereinafter).

[0046] The crosslinked organosilicon resin 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 brittle and strong 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 dissolved product diluted to 30% by mass with isododecane or decamethylcyclopentasiloxane on PTFE (fluororesin) and drying it at 105°C for 3 hours to form a self-supporting film. If a film is not formed, oil will seep out due to cracks in the film, etc., and the oil resistance will be significantly reduced, and the followability with the skin will be low, resulting in an unnatural finish.

[0047] The crosslinked organosilicon resin of component (B) forms a brittle and strong film before crosslinking, while the crosslinked organosilicon resin after crosslinking has improved brittleness and forms a flexible film without stickiness. 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.

[0048] In addition, the film formed from the crosslinked organosilicon resin has significantly improved oil resistance against oil agents such as sebum compared to the film formed from the organosilicon resin before crosslinking. The oil resistance of the organosilicon resin tends to improve as the molecular weight increases, but since there is a limit to increasing the molecular weight of the organosilicon resin, the oil resistance also has a limit. Crosslinking of the organosilicon resin with a crosslinking agent leads to a pseudo-increase in the molecular weight of the organosilicon resin, so it has the effect of raising that limit point. Therefore, the crosslinked organosilicon resin has oil resistance that cannot be achieved with conventional organosilicon resins.

[0049] The crosslinked organosilicon resin in which f in the above formula (2) is an integer satisfying 0 < f < 30 is solid at 25°C, and a crosslinked organosilicon resin with particularly excellent film-forming properties can be obtained.

[0050] In addition, when f in the above formula (2) satisfies 0 ≤ f < 30 and two of R 4 are hydrogen atoms, the crosslinked organosilicon resin is solid at 25°C, and a crosslinked organosilicon 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.

[0051] In the above formula (1), a1 satisfies 0 < a1 ≤ 3, f in the above formula (2) satisfies 0 ≤ f < 20, and R 4 Among them, a crosslinked organosilicon resin in which two of them are hydrogen atoms is in a solid state at 25°C, and a crosslinked organosilicon resin with particularly excellent film-forming properties can be obtained. The obtained film exhibits particularly excellent flex resistance and oil resistance.

[0052] The amount of hydrogen gas generated per mass of the above crosslinked organosilicon resin 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 of remaining hydroxy groups, alkoxy groups with hydrosilyl groups, may increase the likelihood of thickening over time and deteriorate the stability over time. The generation amount of hydrogen gas is preferably 0.01 - 1.2 mL / g, more preferably 0.02 - 1.0 mL / g. The standard state of the gas is the condition (SATP: Standard Ambient Temperature and Pressure) where the reference temperature is 25°C and the standard pressure is 100 kPa.

[0053] The amount of hydrogen gas per mass can be calculated from the volume of hydrogen gas generated by the reaction of hydrosilyl groups and a base. For example, the following method can be mentioned, but the calculation method is not limited to this.

[0054] <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 (25 g of decamethylcyclopentasiloxane and 25 g of crosslinked organosilicon resin) and 10 g of 1-butanol, 10 g of a 20% by mass aqueous sodium hydroxide solution is added dropwise. By dividing the volume of the generated hydrogen gas by the pure content of the crosslinked organosilicon resin, the amount of hydrogen gas per mass can be obtained.

[0055] [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 of 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, resulting in 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 of an organosilicon resin having an alkenyl group and an organopolysiloxane having hydrosilyl groups at both ends is preferred.

[0056] The method for producing the 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 / alkenyl group can be selected from the range of 0.5 to 1.2, preferably 0.8 to 1.2, and more preferably 0.9 to 1.1. If the above ratio is too large, the remaining amount of hydrosilyl groups will increase, and the stability over time may deteriorate.

[0057] 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. In addition, if the amount of the catalyst used is excessive, the sample will be colored, so the amount of platinum or rhodium is preferably 50 ppm or less, and more preferably 20 ppm or less.

[0058] 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.

[0059] 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 kept uniform and the reaction proceeds efficiently.

[0060] The crosslinked organic silicon resin of component (B) 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.

[0061] 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.

[0062] 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.

[0063] After the addition reaction, it is possible to include a step of removing residual hydrosilyl groups as necessary. Especially when used in applications such as cosmetics, the hydrosilyl groups may be deactivated by dehydrogenation reaction over time. Since hydrogen gas is generated, it is a problem from the viewpoint of safety, so it is preferable to include a step of removing the hydrosilyl groups.

[0064] Examples of the step of removing the hydrosilyl group include a formulation in which a basic catalyst is added to hydrolyze 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 hydrogencarbonates such as sodium hydrogencarbonate and potassium hydrogencarbonate. 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.

[0065] 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 or alkoxy groups in the organosilicon resin, so it is not preferable to remove the hydrosilyl group by this method.

[0066] The content of component (B) in the present invention is not particularly limited, and is preferably 0.1% or more, may be 0.5% or more, more preferably 1% or more, further preferably 2% or more, and even more preferably 3% or more, based on the total amount of the solid cosmetic. Also, it is preferably 10% or less, more preferably 9% or less, and even more preferably 8% or less. Also, 1 to 10% is preferable, 2 to 9% is more preferable, and 3 to 8% is even more preferable. Within this range, it is more preferable because it is more excellent in terms of the crack resistance of the cosmetic and the ease of removal after repeated use.

[0067] [Component (C)] Component (C) in the present invention is an oil agent that is liquid at 25°C. Being liquid at 25°C means having no specific shape and having fluidity at 25°C. The oil agent that is liquid at 25°C is not particularly limited as long as it is usually used in cosmetics, and any of them can be used. For example, hydrocarbon oils, ester oils, fatty acids, higher alcohols, silicone oils, fluorine-based oils, etc. can be mentioned, and one or more of these can be used.

[0068] More specifically, hydrocarbon oils such as liquid paraffin, squalane, polybutene, polyisobutylene, α-olefin oligomer, isododecane, and light isoparaffin; esters such as 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, trimethylolpropane triisostearate, ethylhexyl methoxycinnamate, 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, tritridecyl trimellitate, coconut oil, olive oil, palm oil, macadamia nut oil, meadowfoam oil, jojoba oil, rapeseed oil, rice bran oil, castor oil, mink oil, dimer dilinoleyl bisisostearate, dimer dilinoleyl diisostearate, di(isostearyl / phytosteryl) dimer dilinoleate, dihydrogenated rosin dimer dilinoleyl, N-lauroyl-L-glutamic acid di(phytosteryl·2-octyldodecyl), dimer dilinoleyl hydrogenated rosin condensate, etc.;Fatty acids such as isostearic acid and oleic acid; higher alcohols such as oleyl alcohol, isostearyl alcohol, octyldodecanol, and decyltetradecanol; silicone oils such as dimethylpolysiloxane (kinematic viscosity 1 to 1000 CS), cyclomethicone, caprylyl methicone, dimethiconol, methylphenylpolysiloxane, diphenylpolysiloxane, and decamethylcyclopentasiloxane; fluorine-based oils such as perfluorodecane, perfluorooctane, and perfluoropolyether; etc. may be mentioned, and one or more of these can be used. Component (C) may be in a form containing dimethylpolysiloxane, tritridecyl trimellitate, heavy liquid isoparaffin, methylphenylpolysiloxane, dimer dilinoleyl hydrogenated rosin condensate, diglyceryl triisostearate, or a combination thereof.;

[0069] In addition, for the liquid oil agent of component (C) at 25°C, when using a commercial product of a mixture of component (A) and a liquid oil agent at 25°C, the oil agent in the commercial product is also included in component (C). When component (B) is produced as a mixture of liquid oil agents at 25°C as in the production examples described later, the liquid oil agents at 25°C in the mixture are also included in component (C). Also, when a liquid oil agent at 25°C is used as a surface treatment agent for powder, the oil agent does not correspond to component (C).

[0070] Component (C) preferably contains an oil agent having a refractive index of 1.48 or more because it improves the crack resistance of the cosmetic and the ease of removal after repeated use. In the present invention, the refractive index can be measured using a commercially available refractometer. Examples of commercially available refractometers include the hand-held refractometer R-5000 (manufactured by Atago Co., Ltd.). The measurement method may be carried out according to the description in the instruction manual of the hand-held refractometer R-5000. That is, the measurement sample is filled into a glass bottle with an outer diameter of 45 mm, an inner diameter of 38 mm, and a height of 82 mm so that no air space is generated, capped, and left in a 25 °C constant temperature bath for one day and night. The next day, the measured value can be read with a refractometer to obtain the refractive index. Examples of oil agents having a refractive index of 1.48 or more include ester oils such as tritridecyl trimellitate (refractive index 1.48), 2-ethylhexyl paramethoxycinnamate (refractive index 1.508), and phytosteryl macadamia nut fatty acid (refractive index 1.501), hydrocarbon oils such as polybutene (refractive index 1.503) and heavy liquid isoparaffin (refractive index 1.502), and phenyl-modified silicone oils such as trimethylpentaphenyl polysiloxane (refractive index 1.58), diphenyldimethylsilicone (refractive index 1.505), and methylphenyl polysiloxane (refractive index 1.502). Among these, component (C) preferably contains a phenyl-modified silicone, and more preferably contains methylphenyl polysiloxane. Examples of commercially available phenyl-modified silicones include KF-54 and KF-56 (both manufactured by Shin-Etsu Chemical Co., Ltd.).

[0071] The content of component (C) in the present invention is not particularly limited, and is preferably 30% or more, more preferably 32% or more, and even more preferably 35% or more, based on the total amount of the solid cosmetic. Also, the content of component (C) is preferably 60% or less, more preferably 55% or less, even more preferably 50% or less, even more preferably 48% or less, and even more preferably 45% or less, based on the total amount of the solid cosmetic. Further, the content of component (C) is preferably 30 to 50%, more preferably 32 to 48%, and even more preferably 35 to 45%, based on the total amount of the solid cosmetic. Within this range, it is more preferable because the crack resistance of the cosmetic and the ease of removal after repeated use are more excellent.

[0072] [Component (D)] Component (D) in the present invention is a powder. Component (D) is not particularly limited as long as it is usually 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, ultramarine blue, and ultramarine, white extender powders such as talc, muscovite, phlogopite, biotite, synthetic mica, 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, hydroxyapatite, boron nitride, and silicic anhydride, titanium oxide-coated mica, titanium oxide-coated glass powder, titanium oxide-coated bismuth oxychloride, iron oxide mica titanium, ultramarine-treated mica titanium, carmine-treated mica titanium, bismuth oxychloride, fish scale foil, polyethylene terephthalate-aluminum-epoxy laminate powder, polyethylene terephthalate-polyolefin laminate film powder, polyethylene terephthalate-polymethyl methacrylate laminate film powder, etc. of brightening powders, copolymer resins such as polyamide-based resins, polyethylene-based resins, polyacrylic-based resins, polyester-based resins, fluorine-based resins, cellulose-based resins, polystyrene-based resins, and styrene-acrylic copolymer resins, organic polymer resin powders such as polypropylene-based resins and urethane resins, organic low-molecular-weight powders such as zinc stearate and N-acyl lysine, natural organic powders such as silk powder, cellulose powder, and dextrin powder, organic pigment powders such as Pigment Red 201, Pigment Red 202, Pigment Red 205, Pigment Red 226, Pigment Red 228, Pigment Orange 203, Pigment Orange 204, Pigment Blue 404, Pigment Yellow 401, etc., or Pigment Red 3, Pigment Red 104, Pigment Red 106, Pigment Orange 205, Pigment Yellow 4, Pigment Yellow 5, Pigment Green 3, Pigment Blue 1, etc. of zirconium, barium, or aluminum lake, or further metal powders such as aluminum powder, gold powder, and silver powder, composite powders such as fine particle titanium oxide-coated mica titanium, fine particle zinc oxide-coated mica titanium, barium sulfate-coated mica titanium, titanium oxide-containing silicon dioxide, and zinc oxide-containing silicon dioxide, fibers such as nylon, polyester, rayon, and cellulose, etc. can be mentioned, and one or more of these can be used in combination.In addition, these may be surface-treated with a fluorine compound, silicone oil, powder, oil agent, gelling agent, emulsion polymer, surfactant, or the like.

[0073] Among these, from the viewpoint of the crack resistance of the cosmetic, component (D) preferably contains plate-like powder. The plate-like powder means a powder having an aspect ratio of 3 or more. The aspect ratio of the plate-like powder may be 100 or less, or 50 or less. In the present invention, the aspect ratio can be calculated by dividing the average particle diameter by the average thickness. Further, the average thickness of the powder can be calculated by measuring the thickness of 10 particles in an arbitrary field of view using a scanning electron microscope and obtaining the average value. Such plate-like powders include inorganic powders such as muscovite, phlogopite, biotite, synthetic phlogopite (synthetic fluorophlogopite), sericite, synthetic sericite, kaolin, bismuth oxychloride, boron nitride, barium sulfate, glass powder, anhydrous silicic acid, plate-like zinc oxide, etc., organic powders such as N-acyl lysine, aluminum powder, silica-coated aluminum powder, titanium oxide-coated mica (mica titanium), titanium oxide-coated bismuth oxychloride, titanium oxide-coated glass powder (glass pearl), iron oxide·titanium oxide-coated glass powder, iron oxide mica titanium, ultramarine-treated mica titanium, carmine-treated mica titanium, fish scale foil, polyethylene terephthalate·aluminum·epoxy laminated powder, polyethylene terephthalate·polyolefin laminated film powder, polyethylene terephthalate·polymethyl methacrylate laminated film, etc., and shiny powders. Among these, the plate-like powder is preferably an inorganic powder or a shiny powder, and more preferably a powder containing mica. Further, the plate-like powder preferably contains one or more selected from the group consisting of muscovite, phlogopite, biotite, synthetic phlogopite (synthetic fluorophlogopite), sericite, synthetic sericite, mica titanium, iron oxide mica titanium, ultramarine-treated mica titanium, and carmine-treated mica titanium.

[0074] In addition, since the solid cosmetic of the present invention is excellent in color sustainability, it contains colored inorganic pigments such as iron oxide (red iron oxide, yellow iron oxide, black iron oxide, etc.), carbon black, titanium - titanium oxide sintered product, chromium oxide, chromium hydroxide, ultramarine blue, and ultramarine; Pigment Red 201, Pigment Red 202, Pigment Red 205, Pigment Red 226, Pigment Red 228, Pigment Orange 203, Pigment Orange 204, Pigment Blue 404, Pigment Yellow 401, etc., and colored organic pigments such as Pigment Red 3, Pigment Red 104, Pigment Red 106, Pigment Orange 205, Pigment Yellow 4, Pigment Yellow 5, Pigment Green 3, Pigment Blue 1, etc., which are zirconium, barium or aluminum lakes. The content of the colored pigment is, for example, 0.1 to 10% by mass based on the solid cosmetic.

[0075] The content of component (D) in the present invention is not particularly limited, and may be 30% or more, or 32% or more, preferably 35% or more, more preferably 37% or more, and even more preferably 40% or more, based on the total amount of the solid cosmetic. Also, the content of component (D) is preferably 58% or less, more preferably 55% or less, still more preferably 53% or less, and even more preferably 50% or less, based on the total amount of the solid cosmetic. Further, the content of component (D) is preferably 35 to 55%, more preferably 37 to 53%, and even more preferably 40 to 50%, based on the total amount of the solid cosmetic. Within this range, it is more preferable because the solidity of the cosmetic is more excellent. In addition, when the powder is surface - treated, the amount of the entire powder including the surface - treating agent is included in the calculation of the content of the said component (D).

[0076] In the present invention, the content mass ratio of the plate - shaped powder to the component (D) [(plate - shaped powder) / component (D)] is not particularly limited, and is preferably 0.5 or more (upper limit 1.0), more preferably 0.6 or more, still more preferably 0.65 or more, and even more preferably 0.8 or more. Within this range, it is more preferable because the solidity of the cosmetic is more excellent.

[0077] The content mass ratio (C) / (D) of the component (C) to the component (D) (hereinafter also simply referred to as (C) / (D)) is 0.60 to 1.60. When (C) / (D) is less than 0.60, the cosmetic is likely to crack, and the gloss persistence is not sufficient. Also, when (C) / (D) exceeds 1.60, the color persistence significantly decreases, and the gloss persistence and the ease of removal after repeated use are not sufficient. (C) / (D) is preferably, for example, 0.65 or more, more preferably 0.70 or more, and even more preferably 0.75 or more. Also, (C) / (D) may be 1.55 or less, or 1.50 or less, preferably 1.40 or less, more preferably 1.20 or less, and even more preferably 1.00 or less. Also, (C) / (D) is preferably 0.65 to 1.40, more preferably 0.70 to 1.20, and even more preferably 0.75 to 1.00. Within this range, it is more preferable because the cosmetic is less likely to crack and the ease of removal after repeated use is more excellent.

[0078] [Component (E)] The present invention can further contain a component (E), an oil-soluble polyurethane. In the system of the present invention described above, when the component (E) is further contained, the color persistence is further improved. The component (E) in the present invention is not particularly limited as long as it is a polyurethane that shows solubility in an oily component and can be used, but those that can be dissolved in cetyl 2-ethylhexanoate at least 1% or more at 30 °C are preferable. The structure of the oil-soluble polyurethane is not particularly limited, but those having a (e1) hydrophobic part and a (e2) hydrophilic part are preferable from the viewpoints of elasticity and load stability.

[0079] (e1) The hydrophobic part preferably contains a structural unit derived from an isocyanate compound from the viewpoints of elasticity and the like. Examples of the isocyanate compound include 1,6-hexamethylene diisocyanate, 1,3-bis(isocyanatomethyl)benzene, 1,3-bis(isocyanatomethyl)cyclohexane, 2,4-toluene diisocyanate, 2,6-toluene diisocyanate, etc. Among these, 1,6-hexamethylene diisocyanate is preferable.

[0080] Also, from the viewpoint of elasticity and the like, the hydrophobic part (e1) preferably further contains a structural unit derived from a hydrogenated polyolefin polyol. Examples of the hydrogenated polyolefin polyol include hydrogenated polybutadiene polyol, hydrogenated polyisoprene polyol, etc., and among them, hydrogenated polybutadiene diol is preferable.

[0081] From the viewpoint of elasticity and the like, it is preferable that the hydrophobic part (e1) further contains a structural unit derived from dimer diol. Examples of the dimer diol include dimer dilinoleyl alcohol, dimer dioleyl alcohol, etc., dimer dilinoleyl alcohol is preferable, and particularly hydrogenated dimer dilinoleyl alcohol is preferable.

[0082] From the viewpoint of elasticity and the like, it is preferable that the hydrophilic part (e2) contains a structural unit derived from a low molecular weight diol. Examples of the low molecular weight diol include ethylene glycol, propylene glycol, 1,3 - butylene glycol, 1,4 - butylene glycol, diethylene glycol, etc., and ethylene glycol and 1,4 - butylene glycol are preferable.

[0083] Preferable embodiments of the component (E) oil - soluble polyurethane include the following (I) and (II). In this specification, "terminal" means "both terminals". (I) (i) A hydrogenated polybutadiene having an isocyanate group at the terminal and (ii) HO - R 3 -OH (wherein R 3 represents a linear or branched C2 - C6 alkylene group which may have an ether bond) and a polyurethane obtained by the reaction with a glycol represented thereby (II) (iii) A hydrogenated polybutadiene having a hydroxyl group at the terminal, (iV) a diisocyanate compound, and (ii) HO - R 3 -OH (wherein R 3 represents a linear or branched C2 - C6 alkylene group which may have an ether bond) and a polyurethane obtained by the reaction with a glycol represented thereby (i) is not particularly limited as long as it is a hydrogenated polybutadiene having an isocyanate group at the terminal. For example, a compound represented by the following general formula (7) is shown.

[0084]

Chemical formula

[0085] (In the formula, R 1 , R 2 each independently represents a C1-C6 alkylene group, n represents an integer of 10-100, and n1 and n2 each independently represent 0 or 1) R 1 , R 2 each independently represents the same or different C1-C6 alkylene group, and the alkylene may be linear or branched. Examples of the C1-C6 alkylene group include methylene, ethylene, n-propylene, n-butylene, n-pentylene, n-hexylene, etc. The alkylene group of R 1 is preferably a C1-C2 alkylene group. The alkylene group of R 2 is preferably a C5-C6 alkylene group. The alkylene group is preferably linear.

[0086] n represents an integer of 10-100, and a more preferable range of n is 15-55.

[0087] n1 and n2 each independently represent the same or different 0 or 1.

[0088] In the repeating unit "C4H8" of the hydrogenated polybutadiene moiety of the general formula (7) (the following general formula (8)), there are various types as shown in the following general formulas (9a)-(9d), for example.

[0089]

Chemical formula

[0090]

Chemical formula

[0091] In the hydrogenated polybutadiene having an isocyanate group at the terminal, the hydrogenated polybutadiene moiety may consist of only one kind of repeating unit as exemplified above, or may contain two or more kinds of repeating units regularly or randomly.

[0092] The repeating unit "C4H8" constituting the hydrogenated polybutadiene moiety of the general formula (7) (the above general formula (8)) may have the same or different three-dimensional structures, and all structures in which the hydrogenated polybutadiene moiety is represented by the general formula (8) are included in the present invention.

[0093] Examples of the hydrogenated polybutadiene having an isocyanate group at the terminal represented by the general formula (7) include, for example, a compound represented by the following general formula (10).

[0094]

Chemical formula

[0095] (Here, in the formula (10), n represents an integer of 10 to 100) The compound of the general formula (10) is a hydrogenated polybutadiene having an isocyanate group at the terminal of the general formula (1), where R 1 is an ethylene group, R 2 is a hexamethylene group, and it corresponds to the case where n1 = n2 = 1.

[0096] (ii) HO-R 3 -OH (wherein R 3(which may have an ether bond and represents a linear or branched C2-C6 alkylene group), examples of glycols represented by, for example, ethylene glycol (HOCH2CH2OH), propylene glycol (HOCH2CH(OH)CH3), 1,3-butylene glycol (HOCH2CH2CH(OH)CH3), 1,4-butylene glycol (HOCH2CH2CH2CH2OH), and diethylene glycol (HOCH2CH2OCH2CH2OH, the following general formula (11)), etc. can be mentioned.

[0097] [Chemical formula]

[0098] (iii) The hydrogenated polybutadiene having a hydroxyl group at the terminal is not particularly limited, and for example, compounds represented by the following general formula (12) are exemplified.

[0099] [Chemical formula]

[0100] (In the formula, n represents an integer of 10 to 100) In general formula (12), the hydrogenated polybutadiene moiety (general formula (8)) has the same meaning as described above.

[0101] (iV) Examples of the diisocyanate compound include 1,6-hexamethylene diisocyanate, 1,3-bis(isocyanatomethyl)benzene, 1,3-bis(isocyanatomethyl)cyclohexane, 2,4-toluene diisocyanate, and 2,6-toluene diisocyanate, etc. Among these, 1,6-hexamethylene diisocyanate represented by the following general formula (13) is preferred.

[0102] [Chemical formula]

[0103] (I): (i) A hydrogenated polybutadiene having an isocyanate group at the terminal and (ii) HO-R 3 -OH (wherein R 3 represents a linear or branched C2-C6 alkylene group which may have an ether bond), when producing a polyurethane by polyaddition, it is preferably carried out at a molar ratio of (i):(ii) = 1:4 to 4:1, more preferably at a molar ratio of (i):(ii) = 2:3 to 3:2, still more preferably 4:5 to 4:3, and even more preferably 9:10 to 10:9. In this case, the weight average molecular weight (Mw) of (i) is preferably 1,000 to 3,000.

[0104] (II): (iii) A hydrogenated polybutadiene having a hydroxyl group at the terminal, (iV) a diisocyanate compound, and (ii) HO-R 3 -OH (wherein R 3 represents a linear or branched C2-C6 alkylene group which may have an ether bond), when producing a polyurethane by reaction therewith, it is preferably carried out at a molar ratio of (iii):(ii) = 1:4 to 4:1, more preferably at a molar ratio of (iii):(ii) = 2:3 to 3:2, still more preferably 4:5 to 4:3, and even more preferably 9:10 to 10:9.

[0105] Also, the weight average molecular weight (Mw) of the polyurethane obtained in the above (I) or (II) is preferably 10,000 to 150,000, more preferably 15,000 to 130,000, still more preferably 20,000 to 110,000.

[0106] Examples of commercially available products (mixtures of component (E)) include Oilkemia 5S polymer (Rubrizol, INCI name: glyceryl tri (caprylate / caprate), polyurethane-79) (30% pure), Oilkemia 5S CC polymer (Rubrizol, INCI name: glyceryl tri (caprylate / caprate), hydrogenated poly (C6-20 olefin), (HDI / trimethylolhexyl lactone) cross-polymer) (30% pure), etc. Examples of component (E) include (HDI / trimethylolhexyl lactone) cross-polymer, polyurethane-79, etc.

[0107] The content of component (E) in the present invention is not particularly limited, and is preferably 0.1% or more, more preferably 0.3% or more, and even more preferably 0.5% or more, based on the total amount of the solid cosmetic. Also, the content of component (E) is preferably 15% or less, more preferably 13% or less, even more preferably 10% or less, and may be 8% or less, or 5% or less. Further, the content of component (E) is preferably 0.1 to 15%, more preferably 0.3 to 13%, and even more preferably 0.5 to 10%. This range is more preferable because of the better color persistence.

[0108] [Component (F)] The present invention can further contain component (F) inulin fatty acid ester. The inulin fatty acid ester as component (F) in the present invention is an ester of inulin and a straight-chain or branched-chain saturated or unsaturated fatty acid having 8 to 32 carbon atoms. The average molecular weight of inulin used for the inulin fatty acid ester is preferably in the range of 300 to 10,000. The inulin fatty acid ester is more preferably inulin stearate. Examples of commercially available products include Reopal ISK2 (manufactured by Chiba Flour Milling Co., Ltd.).

[0109] The content of component (F) in the present invention is not particularly limited. Preferably, it is 0.1% or more, more preferably 0.3% or more, and even more preferably 0.5% or more, based on the total amount of the solid cosmetic. Also, preferably, it is 15% or less, more preferably 13% or less, and even more preferably 10% or less. Further, preferably, it is 0.1 - 15%, more preferably 0.3 - 13%, and even more preferably 0.5 - 10%. Within this range, it is more preferable because the gloss persistence is more excellent.

[0110] Also, the form of using components (E) and (F) in combination is also a preferred embodiment. By using both in combination, the color and gloss persistence are further excellent. In this case, the blending mass ratio of the two is, for example, component (E): component (F) = 0.1:1 - 10:1, and 0.2:1 - 5:1.

[0111] In addition to the above essential components, the solid cosmetic of the present invention can contain, as necessary, components used in ordinary cosmetics, as long as the effects of the present invention are not impaired. For example, it can contain surfactants, oils other than component (C), water-soluble polymers, film-forming agents, antioxidants, anti-fading agents, defoaming agents, pH adjusters, chelating agents, beauty components, preservatives, fragrances, cooling agents, etc.

[0112] In this specification, the solid cosmetic is, for example, a cosmetic mainly composed of an oil and a powder. Here, the main components mean that the oil and the powder are contained in the cosmetic at 50% by mass or more, 60% by mass or more, 65% by mass or more, or 70% by mass or more. Also, the solid cosmetic is, for example, a cosmetic that has no fluidity. Having no fluidity means that after filling 30 g of the cosmetic into a container (Pharmaceutical Bottle PS - 6K manufactured by Daiichi Glass Co., Ltd.) with an inner diameter of 2.47 cm, a body diameter of 4.05 cm, and a total height of 7.4 cm, closing the lid, tilting it 90° in an environment of 25°C and 1 atm, and allowing it to stand for 1 minute, a part of the filled cosmetic does not adhere to the inside of the lid.

[0113] In addition, the solid cosmetic of the present invention preferably has a water content of 3% by mass or less, more preferably 1% by mass or less, and most preferably substantially no water content. Here, substantially no water content means that a content of impurities level is acceptable, for example, it refers to 0.1% by mass or less.

[0114] The production method of the solid cosmetic of the present invention is not particularly limited and can be produced by a generally known method. Examples of the production method are shown below, but it is not limited thereto. Specifically, after mixing components (A) to (D), and optionally components (E), (F) and other components, a method of dry compression molding (hereinafter abbreviated as "dry molding method"), or components (A) to (D), and optionally components (E), (F) and other components and a volatile oil are mixed to form a slurry, which is filled and molded, and then the volatile oil is removed for wet molding method and the like. The filling equipment used in the dry molding method is not particularly limited, and filling equipment used for filling an elastic composition, a clay-like composition having no fluidity, etc. is preferable. For example, a filling machine with a screw feeder, a box-type filling machine, etc. may be mentioned. Commercially available products such as a filling machine with a screw feeder, a box-type filling machine, etc. include Martian CN580 (manufactured by Leon Automatic Machine Co., Ltd.), TOA small dumpling filling machine (manufactured by Toa Industries, Ltd.), bean mincer BK-205N (manufactured by Bonny Co., Ltd.), Tsubuzoroi RC-1 (manufactured by Shinagawa Kogyo Co., Ltd.), etc.

[0115] The solid cosmetic of the present invention can be used as cosmetics for various applications. For example, makeup cosmetics such as eyeshadow, eyebrow, foundation, base, concealer, powder, blusher, lipstick, etc. may be mentioned. In particular, eyeshadow is preferable from the viewpoints of luster persistence and color persistence.

[0116] In addition, the present invention can also take the following configuration. [1] The following components (A) to (D); (A) A partially crosslinked organopolysiloxane polymer (excluding component (B)) (B) A crosslinked organosilicon resin which is an addition reaction product of the following components (X) and (Y), wherein the amount of hydrogen gas generated per mass from said crosslinked organosilicon resin is 1.5 mL / g or less under standard conditions, and said component (Y) is added in an amount such that the amount of hydrosilyl groups is 0.5 to 1.2 moles per mole of alkenyl groups in said component (X). (C) Oil that is liquid at 25℃ (D) Powder wherein the mass ratio (C) / (D) of component (C) to component (D) is 0.6 to 1.6. (X) An alkenyl-containing organosilicon resin represented by the following formula (1) and having one or more alkenyl groups in each molecule:

[0117] [ka]

[0118] [In the formula, R 1 is 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. 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)下記式(2)で表され、1分子中にヒドロシリル基を2個以上有するオルガノハイドロジェンポリシロキサン

[0119] [ka]

[0120] [In the formula, 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.] [2] The solid cosmetic according to [1], wherein the component (C) contains an oil agent having a refractive index of 1.48 or more. [3] The solid cosmetic according to [1] or [2], wherein the component (C) contains a phenyl-modified silicone. [4] The solid cosmetic according to any one of [1] to [3], wherein the component (D) contains plate-like powder. [5] The solid cosmetic according to [4], wherein the content mass ratio of the plate-like powder to the component (D) is 0.5 or more. [6] The solid cosmetic according to any one of [1] to [5], further containing a component (E) oil-soluble polyurethane. [7] The solid cosmetic according to any one of [1] to [6], further containing a component (F) inulin fatty acid ester.

Examples

[0121] Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples.

[0122] In addition, the alkenyl group-containing organosilicon resin as a raw material in the following is synthesized according to a known production method. In the following production 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 1H-NMR spectrum analysis.

[0123] [Production Example 1] Method for producing a crosslinked organosilicon resin / decamethylcyclopentasiloxane solution (solid content 30%) 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 (molar ratio)), 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. Then, 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. 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 221,000). The reaction rate of the alkenyl group was 92%, and the amount of hydrogen gas generated from the crosslinked organosilicon resin (remaining hydrosilyl groups) was 0.8 mL / g.

[0124]

Chemical formula

[0125]

Chemical formula

[0126] [Production Example 2] Method for producing a crosslinked organosilicon resin / decamethylcyclopentasiloxane solution (solid content 30%) 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 (molar ratio)), 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. Then, 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.

[0127] Further, the obtained decamethylcyclopentasiloxane solution of the crosslinked organosilicon resin 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 154,000). The reaction rate of the alkenyl group was 93%, and the amount of hydrogen gas generated from the crosslinked organosilicon resin (remaining hydrosilyl groups) was 1.0 mL / g.

[0128]

Chemical formula

[0129]

Chemical formula

[0130] [Production Example 3] Production method of crosslinked organosilicon resin / decamethylcyclopentasiloxane solution (solid content 30%) 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 (molar ratio)), 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. Then, 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.

[0131] 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 crosslinked organosilicon resin (remaining hydrosilyl groups) was 0.5 mL / g.

[0132] [Chemical formula]

[0133] [Chemical formula]

[0134] [Production Example 4] Method for producing a crosslinked organosilicon resin / decamethylcyclopentasiloxane solution (solid content 30%) 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 (molar ratio)), and 0.6 g of a 0.5% 2-propanol solution of chloroplatinic acid were charged into a reactor and reacted by heating at 120 °C for 5 hours. Then, 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.

[0135] Further, the decamethylcyclopentasiloxane solution of the obtained crosslinked organosilicon resin 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.

[0136]

Chemical formula

[0137]

Chemical formula

[0138] Examples 1 to 20 and Comparative Examples 1 to 8: Solid eye shadow Solid eye shadows having the compositions shown in Tables 1 to 3 were prepared by the following production method, and the gloss persistence (a), color persistence (b), resistance to cracking of the cosmetics (c), and ease of removal after repeated use (d) were evaluated and judged according to the following evaluation methods and criteria, and the results are also shown in Tables 1 to 3.

[0139]

Table 1

[0140]

Table 2

[0141]

Table 3

[0142] *2: KSG-43 (manufactured by Shin-Etsu Chemical Co., Ltd.) *3: Leo Pearl KL2 (manufactured by Chiba Flour Milling Co., Ltd.) *4: Solution obtained by dissolving the solid powder obtained in Production Example 1 in isododecane at 110°C and cooling to room temperature (solid content 50%) *5: SILFORM FLEXIBLE RESIN (manufactured by Momentive Performance Materials Japan, Inc.) *6: KF-54 (manufactured by Shin-Etsu Chemical Co., Ltd.) *7: Pearl Ream 18 (manufactured by NOF Corporation) *8: LIPONATE TDTM (manufactured by Lipo Chemicals) *9: KF-96-10CS (manufactured by Shin-Etsu Chemical Co., Ltd.) *10: COSMETICA SUPER WHITE N-8000S (manufactured by CQV) *11: OILKEMIA 5S CC POLYMER (manufactured by Lubrizol Japan Ltd.) *12: Leo Pearl ISK2 (manufactured by Chiba Flour Milling Co., Ltd).

[0143] (Manufacturing Method) A. Components (1) to (15), (20), and (21) were uniformly heated and mixed at 90°C. B. After cooling A to 25°C, components (16) to (19) were added to A and kneaded using a planetary mixer under reduced pressure. C. B was filled into a container using a filling machine equipped with a screw feeder, and press-molded into a dome shape with a lattice-patterned non-woven fabric sandwiched to obtain a solid eyeshadow.

[0144] [Evaluation Method 1] (Evaluation Items: Persistence of Gloss, Persistence of Color, Ease of Removal after Repeated Use) For each sample, 20 professional cosmetic evaluation panelists evaluated each item of "Persistence of Gloss", "Persistence of Color", and "Ease of Removal after Repeated Use" on a 7-point scale according to the following absolute evaluation criteria. Then, using the average score of all panelists, the determination was made according to the following determination criteria. For "Persistence of Gloss" and "Persistence of Color", after each panelist applied each sample, they were asked to spend 6 hours in daily life, and it was evaluated whether the gloss or color persisted. From the start until 10 minutes after application, observations were made every 1 minute. From 10 minutes to 1 hour after application, observations were made every 10 minutes. After 1 hour after application, observations were made every 1 hour, and it was compared with the state immediately after application. For "Ease of Removal after Repeated Use", the samples before use and after 30 uses were prepared, and the amount of removal when gently rubbed with a finger was evaluated.

[0145] (Evaluation Criteria for Persistence of Gloss and Persistence of Color) (Score): (Evaluation) 6 points: Very good (The gloss / color at the time of application is maintained almost until 6 hours compared to the time of application) 5 points: Good (The gloss / color at the time of application is maintained almost until 4 hours compared to the time of application) 4 points: Slightly good (The gloss / color at the time of application is maintained almost until 2 hours compared to the time of application) 3 points: Normal (The gloss / color at the time of application is maintained almost until 1 hour compared to the time of application) 2 points: Slightly poor (The gloss / color at the time of application is maintained almost until 30 minutes compared to the time of application) 1 point: Poor (The gloss / color at the time of application is maintained almost until 10 minutes compared to the time of application) 0 points: Very poor (The gloss / color at the time of application has almost disappeared 10 minutes after application compared to the time of application) (Evaluation Criteria for Ease of Removal after Repeated Use) (Score): (Evaluation) 6 points: The amount of removal is just right, very good 5 points: Slightly more or less, but good 4 points: Slightly more or less, but good 3 points: More or less, but within the acceptable range for use 2 points: Slightly too much or too little, defective 1 point: Too much or too little, defective 0 point: Extremely too much or too little, defective (Judgment criteria) (Judgment): (Average score) ◎: 5.0 or more ○: 3.5 or more and less than 5.0 △: 1.5 or more and less than 3.5 ×: Less than 1.5

[0146] [Evaluation method 2] (Evaluation item: Resistance to cracking of cosmetics) Each sample immediately after preparation was picked up with a finger and applied onto a thin aluminum plate. Immediately after application, the surface was leveled with a 20-μm doctor blade to create a 20-μm uniform coating film, and it was left to stand at 25 °C for 1 hour to obtain a dried coating film. After 1 hour, the aluminum plate coated with the sample was bent 90° along a 5-cm-diameter metal cylinder, and the cracking state of the coating film was observed. Regarding the resistance to cracking of each sample, compared with the state immediately after application, the degree was evaluated according to the following judgment criteria. [Judgment criteria] (Judgment): (State of cracking) ◎: No cracking at all 〇: Slight cracking △: Large degree of cracking ×: Extremely large degree of cracking As is clear from the results in Tables 1 to 3, the solid eye shadow of the examples was excellent in all items of "persistence of gloss", "persistence of color", "resistance to cracking of cosmetics", and "easiness of removal after repeated use". On the other hand, Comparative Example 1 that does not contain Component (A) did not obtain satisfactory quality in terms of persistence of gloss and persistence of color. Comparative Example 2 that contains dextrin palmitate instead of Component (A) did not obtain satisfactory quality in terms of persistence of gloss and resistance to cracking of cosmetics. Further, Comparative Example 3 that does not contain Component (B) did not obtain satisfactory quality in terms of persistence of gloss, persistence of color, and resistance to cracking of cosmetics. Comparative Example 4 that contains trimethylsiloxysilicate instead of Component (B) did not obtain satisfactory quality in terms of resistance to cracking of cosmetics. Comparative Example 5 that contains polymethylsilsesquioxane instead of Component (B) did not obtain satisfactory quality in terms of resistance to cracking of cosmetics. Furthermore, Comparative Example 6 that contains petrolatum instead of Component (C) did not obtain satisfactory quality in terms of persistence of gloss, resistance to cracking of cosmetics, and easiness of removal after repeated use. In addition, Comparative Example 7 in which the content mass ratio (C) / (D) of Component (C) and Component (D) exceeds 1.60 did not obtain satisfactory quality in terms of persistence of gloss, persistence of color, and easiness of removal after repeated use. Comparative Example 8 in which the ratio is less than 0.60 did not obtain satisfactory quality in terms of persistence of gloss and resistance to cracking of cosmetics.

[0147] Example 21: Solid Eye Shadow (Component) (%) 1. (Dimethicone / Vinyldimethicone) Crosspolymer / Dimethylpolysiloxane (Solid content 60%) (Component (A) / Component (C)) 10 2. Crosslinked organosilicon resin / isododecane solution of Production Example 1 (solid content 50%) (Component (B) / Component (C)) *4 10 3. Methylphenylpolysiloxane (Component (C)) *6 35 4. Synthetic phlogopite (Component (D), plate-like powder) balance 5. Iron oxide red (Component (D)) 3 6. Glass pearl *13 (Component (D), plate-like powder) 10 7. Glyceryl tri(caprylate / caprate); Hydrogenated poly(C6-20 olefin); (HDI / trimethylolhexyl lactone) crosspolymer)(30%)(Component (C) / Component (E)) *11 3 8. Inulin stearate (Component (F)) *12 3 *13: Microglas Metashine MT1080RS (manufactured by Nippon Sheet Glass Co., Ltd.) (Manufacturing method) A: Components 1 to 3, 7, and 8 were uniformly mixed at 90 °C. B: After cooling A to 25 °C, Components 4 to 6 were added to A, and the mixture was kneaded while reducing the pressure using a planetary mixer. C: B was filled into a container using a filling machine with a screw feeder, and was press-molded into a dome shape with a lattice-patterned non-woven fabric sandwiched therein to obtain a solid eyeshadow.

[0148] The obtained solid eyeshadow was excellent in gloss persistence, color persistence, resistance to cracking of the cosmetic, and ease of removal after repeated use.

[0149] Example 22: Solid eyebrow (Components) (%) 1. (Dimethicone / vinyl dimethicone) crosspolymer / dimethylpolysiloxane (Solid content 60%)(Component (A) / Component (C)) 15 2. Crosslinked organosilicon resin / isododecane solution of Production Example 1 (solid content 50%)(Component (B) / Component (C)) *4 15 3. Methylphenylpolysiloxane (Component (C))*6 30 4. Synthetic phlogopite (Component (D), plate-like powder) balance 5. Iron black oxide (Component (D)) 10 6. Titanium dioxide (Component (D)) *14 3 7. Glyceryl tri(caprylate / caprate); Hydrogenated poly(C6-20 olefin); (HDI / trimethylolhexyl lactone) crosspolymer)(30%)(Component (C) / Component (E)) *11 5 *14: MP-1133 (manufactured by Teika Co., Ltd.) (Manufacturing method) A: Components 1 to 3 and 7 were uniformly mixed at 90 °C. B: After cooling A to 25 °C, components 4 to 6 were added to A and mixed with a three-roll mill. C: B was formed into a rod-shaped core and filled into a pencil-type dispensing container to obtain a solid eyebrow pencil.

[0150] The obtained solid eyebrow pencil was excellent in gloss persistence, color persistence, resistance to cracking of cosmetics, and ease of removal after repeated use.

[0151] Example 23: Solid lipstick (Components) (%) 1. (Vinyl dimethicone / lauryl dimethicone) Crosspolymer / Glyceryl tri-2-ethylhexanoate (solid content 30%) (Component (A) / Component (C)) *2 10 2. Crosslinked organosilicon resin / isododecane solution of Production Example 1 (solid content 50%) (Component (B) / Component (C)) *4 15 3. Dimer dilinoleyl hydrogenated rosin condensate (Component (C)) *15 30 4. Synthetic phlogopite (Component (D), plate-like powder) Balance 5. Iron oxide red (Component (D)) 3 6. Red 226 (Component (D)) *16 10 7. Fumed silica (Component (D)) *17 1 8. Glyceryl tri(caprylate / caprate); polyurethane-79) (30%) (Component (C) / Component (E))*18 1 *15: LUSPLAN DD-DHR (manufactured by Nippon Fine Chemical Co., Ltd.) *16: Red 226 No. (P): manufactured by Daito Kasei Kogyo Co., Ltd. *17: AEROSIL 300 (manufactured by Nippon Aerosil Co., Ltd.) *18: OILKEMIA 5S POLYMER (manufactured by Lubrizol Japan Ltd.) (Manufacturing method) A: Mix components 1 to 3 and 8 uniformly at 90 °C. B: After cooling A to 25°C, add components 4 to 7 to A and mix them with a three-roll mill. C: After filling B into a container using a filling machine equipped with a screw feeder at 25°C, press-mold it to obtain a solid lipstick.

[0152] The obtained solid lipstick was excellent in gloss persistence, color persistence, resistance to cracking of the cosmetic, and ease of removal after repeated use.

[0153] Example 24: Solid Cheek Blush (Components) (%) 1. (Vinyl Dimethicone / Lauryl Dimethicone) Crosspolymer / Glyceryl Tri-2-ethylhexanoate (solid content 30%) *2 (Component (A) / Component (C)) 7 2. Crosslinked organosilicon resin / isododecane solution of Production Example 1 (solid content 50%) (Component (B) / Component (C)) *4 10 3. Polybutene (refractive index 1.503) (Component (C)) *19 35 4. Synthetic phlogopite (Component (D), plate-like powder) balance 5. Red iron oxide (Component (D)) 1 6. Titanium dioxide (Component (D)) 5 7. Mica titanium (average particle size 27 μm, red interference color) (Component (D), plate-like powder) *20 10 8. Inulin stearate (Component (F)) *12 5 *19: Purified polybutene HV-100F (SB) (manufactured by Nippon Natural Products Co., Ltd.) *20: COSMETICA SUPER RED (manufactured by CQV Co., Ltd.) (Manufacturing method) A: Uniformly mix Components 1 to 3 and 8 at 90°C. B: After cooling A to 25°C, add components 4 to 7 to A and mix them with a three-roll mill. C: After filling B into a container using a filling machine equipped with a screw feeder at 25°C, press-mold it to obtain a solid cheek blush.

[0154] The obtained solid blusher was excellent in gloss persistence, color persistence, resistance to cracking of the cosmetic, and ease of removal after repeated use.

[0155] Example 25: Solid Concealer (Ingredients) (%) 1. (Vinyl dimethicone / lauryl dimethicone) Crosspolymer / Glyceryl tri-2-ethylhexanoate (30% solids)*2 (Component (A) / Component (C)) 10 2. Crosslinked organosilicon resin / isododecane solution of Production Example 1 (50% solids) (Component (B) / Component (C))*4 15 3. Diglyceryl triisostearate (refractive index less than 1.48) (Component (C)) *21 39 4. Synthetic phlogopite (Component (D), plate-like powder) balance 5. Yellow iron oxide (Component (D)) 1 6. n-Octylsilylated titanium oxide (Component (D)) *22 10 7. Zinc oxide (Component (D), plate-like powder) *23 3 8. Mica pearl (Component (D), plate-like powder) *24 10 9. Inulin stearate (Component (F)) *12 1 *21: Cosmol 43V (manufactured by Nisshin Oillio Group) *22: OTS-2 TiO2 MP-1133 (manufactured by Daito Kasei Kogyo Co., Ltd.) *23: Hexagonal plate-like zinc oxide XZ-300F (manufactured by Sakai Chemical Industry Co., Ltd.) *24: GEMTONE TAN OPAL G005 (manufactured by BASF) (Manufacturing method) A: Mix Components 1 to 3 and 9 uniformly at 90°C. B: After cooling A to 25°C, add Components 4 to 8 to A and mix with a three-roll mill. C: Heat B to 90°C, fill it into a mold, and rapidly cool it to -18°C using a freezer. D: Load C into a stick container, adjust the temperature to 25°C to obtain a solid concealer.

[0156] The obtained solid concealer was excellent in gloss persistence, color persistence, resistance to cracking of cosmetics, and ease of removal after repeated use.

Claims

Claim 1 The following components (A) to (D); (A) A partially crosslinked organopolysiloxane polymer (excluding component (B)) (B) 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 the crosslinked organosilicon resin is 1.5 mL / g or less under standard conditions, and the amount of the component (Y) is added in such an amount 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 component (X). A crosslinked organosilicon resin obtained by the addition reaction (C) An oil agent in a liquid state at 25 °C (D) Powder A solid cosmetic containing the above components, wherein the mass ratio (C) / (D) of the component (C) to the component (D) is 0.60 to 1.

60. (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 is 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 【Chemical Formula 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 cosmetic according to claim 1, wherein the component (C) contains an oil agent having a refractive index of 1.48 or more. Claim 3 The solid cosmetic according to claim 2, wherein the oil agent having a refractive index of 1.48 or more in the component (C) is a phenyl-modified silicone. Claim 4 The solid cosmetic according to any one of claims 1 to 3, wherein the component (D) contains plate-like powder. Claim 5 The solid cosmetic according to claim 4, wherein the mass ratio of the plate-like powder to the component (D) is 0.5 or more. Claim 6 The solid cosmetic according to any one of claims 1 to 3, further containing component (E) an oil-soluble polyurethane. Claim 7 The solid cosmetic according to any one of claims 1 to 3, further containing component (F) an inulin fatty acid ester.

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