JP2006160616A - Method for forming composition and powdery cosmetic - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for forming a composition, capable of increasing the filling rate of the composition containing powder, and a powdery cosmetic obtained by the method for forming the composition. <P>SOLUTION: This method for forming the composition comprises a process of surface-treating the powder, a process of producing slurry containing the surface treated powder, and a process of filling the slurry into a container and sucking with compressing for forming. The powdery cosmetic is formed by using the above method for forming the composition. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a method for molding a composition and a powder cosmetic.

  Powder cosmetics are mainly composed of powder and oil, and as a molding method, dry molding in which a raw material composition is filled in a container such as an inner dish and then pressed has been generally used. On the other hand, when a large amount of spherical powder is blended for the purpose of improving the usability, sufficient hardness cannot be obtained by the above molding method, and there is a tendency that the amount of training by an applicator such as a sponge increases. There is also a problem that the strength against impact such as dropping or vibration is inferior.

  On the other hand, suction press molding is known in which a slurry obtained by dispersing a raw material composition in a solvent is filled in a container, and then the solvent is removed by vacuum suction and then pressed (see Patent Document 1). According to this method, since the filling property of the cosmetic is improved, sufficient hardness and strength can be imparted to the molded product even when a large amount of spherical powder is blended. However, the cosmetic containing sericite has a problem that the filling rate is lowered. Since sericite has smoothness and fineness, development of a molding method that can increase the filling rate of cosmetics containing sericite is required.

On the other hand, a cosmetic containing a powder and an oil component obtained by coating the surface of a powder with a silicone compound having a silicon-hydrogen bond and adding a compound capable of reacting with the silicon-hydrogen bond to the silicone compound has makeup, It is known that the secondary adhesion preventing effect is excellent (see Patent Document 2).
Japanese Patent No. 1556592 Japanese Patent Laid-Open No. 11-060439

  The present invention provides a method for molding a composition capable of increasing the filling rate of a composition containing powder, and a powder cosmetic obtained by the method for molding the composition, in view of the above-described problems of the prior art. For the purpose.

  The invention according to claim 1 is a method of molding a composition containing a powder exhibiting a dilatant behavior, the step of surface-treating the powder, the step of producing a slurry containing the surface-treated powder, and the slurry. It has the process of filling a container and carrying out suction press molding.

  According to the first aspect of the present invention, the method includes a step of surface-treating the powder, a step of manufacturing a slurry containing the surface-treated powder, and a step of filling the slurry into a container and performing suction press molding. Further, it is possible to provide a molding method capable of increasing the filling rate of the composition containing the powder.

  According to a second aspect of the present invention, in the method for molding a composition according to the first aspect, the powder is sericite.

  According to the invention described in claim 2, since the powder is sericite, a molded product having smoothness and fineness can be obtained.

  According to a third aspect of the present invention, in the molding method of the composition according to the first or second aspect, the surface treatment step includes the step of coating the powder with a silicone compound having a silicon-hydrogen bond and the silicone compound. It has the process of making this react with an unsaturated compound.

  According to the invention of claim 3, the surface treatment step includes a step of coating the powder with a silicone compound having a silicon-hydrogen bond and a step of reacting the silicone compound with an unsaturated compound. The dilatant behavior can be suppressed.

  The invention according to claim 4 is the method for molding the composition according to claim 3, wherein the ratio of the weight of the silicone compound to the weight of the powder is 0.01 or more and 0.2 or less. To do.

  According to the invention described in claim 4, since the ratio of the weight of the silicone compound to the weight of the powder is 0.01 or more and 0.2 or less, the powder can be coated without excess or deficiency.

  The invention according to claim 5 is the molding method of the composition according to claim 3 or 4, wherein the ratio of the equivalent of the unsaturated compound to the equivalent of the silicon-hydrogen bond is 0.5 or more and 5 or less. It is characterized by that.

  According to the invention of claim 5, since the ratio of the equivalent of the unsaturated compound to the equivalent of the silicon-hydrogen bond is 0.5 or more and 5 or less, the silicon-hydrogen bond is allowed to react quantitatively. Can do.

  The invention according to claim 6 is the method for molding a composition according to claim 1 or 2, wherein the surface treatment step coats the powder with a cationic surfactant.

  According to the invention described in claim 6, since the surface treatment step coats the powder with the cationic surfactant, the dilatant behavior of the powder can be suppressed.

  The invention according to claim 7 is the molding method of the composition according to claim 6, wherein the ratio of the weight of the cationic surfactant to the weight of the powder is 0.005 or more and 0.05 or less. It is characterized by.

  According to the invention described in claim 7, since the ratio of the weight of the cationic surfactant to the weight of the powder is 0.005 or more and 0.05 or less, the surface of the powder is made of a cationic surfactant. Can be coated.

  The invention described in claim 8 is characterized in that the powder cosmetic is molded by the molding method of the composition according to any one of claims 1 to 7.

  According to invention of Claim 8, since it shape | molds with the shaping | molding method of the composition as described in any one of Claims 1 thru | or 7, powder cosmetics with a high filling rate can be provided.

  ADVANTAGE OF THE INVENTION According to this invention, the powder cosmetics obtained by the molding method of the composition which can raise the filling rate of the composition containing powder, and the molding method of this composition can be provided.

  Next, the best mode for carrying out the present invention will be described with reference to the drawings.

  In the molding method of the composition of the present invention, a powder exhibiting a dilatant behavior is surface-treated. This is because, as a result of investigation, it has been clarified that the composition containing a powder exhibiting a dilatant behavior has a reduced filling rate when performing suction press molding. Therefore, when the powder is surface-treated, the dilatant behavior is not exhibited and the filling rate can be increased. This is presumably because the surface treatment of the powder reduces the interaction between the powders and suppresses the formation of the structure that is considered to be the cause of the dilatant behavior. From such consideration, the powder to be surface-treated is a powder exhibiting dilatant behavior, and specifically, sericite can be mentioned.

  Examples of the surface treatment in the present invention include treatment with a silicone compound and an unsaturated compound and treatment with a cationic surfactant.

  In the surface treatment with a silicone compound and an unsaturated compound, it is preferable to coat the powder with a silicone compound having a silicon-hydrogen bond. At this time, a crosslinking reaction of the silicone compound occurs on the surface of the powder, and a network structure is formed.

  The coating with the silicone compound can be performed by a known method. Dissolve the silicone compound in an organic solvent such as chloroform, hexane, benzene, toluene, acetone, etc., disperse the powder in this to prepare a dispersion, and heat the dispersion to evaporate the solvent. The surface can be coated. Moreover, the surface of a powder can be coat | covered by the method of pouring the said dispersion liquid in the poor solvent of a silicone compound, and the method of pouring the poor solvent of a silicone compound in said dispersion liquid. Furthermore, the surface of the powder can be coated by polymerizing the silicone compound in the presence of a catalyst. Moreover, it can also coat | cover by making the active point distributed on the surface of a powder and a silicone compound react. The silicone compound may be applied to a powder, and the silicone compound to be applied may be diluted with a solvent. Furthermore, the silicone compound can be coated in an aqueous solvent containing about 80% by weight or more of water. Examples of components other than water include alcohols such as ethanol, methanol, and isopropanol, sodium hydroxide, potassium hydroxide, calcium hydroxide, hydrochloric acid, sulfuric acid, and mixtures thereof. In addition, the crosslinking reaction of the silicone compound in the aqueous solvent can be controlled by adjusting the pH. That is, when the pH is increased, crosslinking can be promoted, and when the pH is decreased, crosslinking can be suppressed.

  The ratio of the weight of water to the weight of the silicone compound is preferably from 0.1 to 100, and more preferably from 5 to 50. In addition, mixing in an aqueous solvent can be performed using a commonly used mixer. In addition, when the powder and the silicone compound are wet-mixed, the amount of water used is slightly increased, and when dry-mixed, the amount of water is slightly decreased.

  The ratio of the weight of the silicone compound to the weight of the powder is preferably 0.01 or more and 0.2 or less, and more preferably 0.03 or more and 0.1 or less. If this ratio is less than 0.01, the silicone compound cannot be introduced to such an extent that the effect of the present invention can be obtained, and if it exceeds 0.2, it is not preferable because it is not in the form of powder.

  The silicone compound having a silicon-hydrogen bond used in the present invention has a general formula

で示される化合物である。ここで、Ｒ_１、Ｒ_２及びＲ_３は、それぞれハロゲン原子で置換されうる炭素数1以上１０以下の炭化水素基であり、ａ及びｃはそれぞれ０以上の整数であり、ｂは１以上の整数であり、ａ、ｂ及びｃの和は、３以上１００００以下である。なお、Ｒ_１、Ｒ_２及びＲ_３は、それぞれハロゲン原子で置換されうる炭素数1以上４以下の炭化水素基又はアリール基であることが好ましく、ハロゲン原子としては、フッ素原子が好ましい。また、ａ、ｂ及びｃの和は、１０以上１０００以下であることが好ましく、２０以上５００以下が特に好ましい。

It is a compound shown by these. Here, R ₁ , R ₂ and R ₃ are each a hydrocarbon group having 1 to 10 carbon atoms that can be substituted with a halogen atom, a and c are each an integer of 0 or more, and b is 1 or more. It is an integer, and the sum of a, b and c is 3 or more and 10,000 or less. R ₁ , R _2, and R ₃ are each preferably a hydrocarbon group or aryl group having 1 to 4 carbon atoms that can be substituted with a halogen atom, and the halogen atom is preferably a fluorine atom. The sum of a, b and c is preferably 10 or more and 1000 or less, and particularly preferably 20 or more and 500 or less.

  The silicone compound used in the present invention may be either a chain silicone compound or a cyclic silicone compound. Examples of the chain silicone compound include methyl hydrogen polysiloxane, phenyl hydrogen polysiloxane, 1,1,1,3,5,7,7,7-octamethyltetrasiloxane, 1,1,1,3,5, 7,9,9,9-nonamethylpentasiloxane, 1,1,1,3,5,7,9,11,11,11-decamethylhexasiloxane, 1,3,5,7-tetramethylcyclotetra Examples thereof include siloxane. Examples of the cyclic silicone compound include cyclic methyl hydrogen polysiloxane.

  In the surface treatment with the silicone compound and the unsaturated compound, the silicone compound is preferably reacted with the unsaturated compound. On the powder surface coated with the silicone compound, unreacted silicon-hydrogen bonds remain due to steric hindrance or the like. By adding this residual silicon-hydrogen bond to the unsaturated compound, a hydrocarbon group is introduced into the silicone compound. This reduces the interaction between the powders and does not exhibit dilatant behavior. In addition, if reactive silicon-hydrogen bonds remain, the powder surface becomes unstable, which is not preferable.

  Both the coating of the silicone compound and the addition reaction to the unsaturated compound can be performed in an aqueous solvent. As such a method, after mixing a silicone compound, an unsaturated compound, and water with a mixer, this mixed solution is added to a powder, heated and mixed, and a catalyst is added. Further, it is possible to add a catalyst after adding an aqueous solvent to a kneader containing powder, stirring and mixing, adding a silicone compound and an unsaturated compound, heating and mixing. When these methods are used, the crosslinking reaction and the addition reaction can be performed simultaneously. The addition reaction is preferably performed while heating because the reaction time is shortened. Here, it is preferable that heating temperature is 50 degreeC or more and 120 degrees C or less. Further, the ratio of the equivalent of the unsaturated compound to the equivalent of silicon-hydrogen bond of the silicone compound is preferably 0.5 or more and 5 or less, and more preferably 1 or more and 2 or less. Thereby, a silicon-hydrogen bond can be made to react quantitatively. Here, the equivalent of silicon-hydrogen bond means the equivalent of silicon-hydrogen bond of the silicone compound before use.

  The silicone compound and the unsaturated compound may be supplied as a gas, or may be stirred and mixed together with the powder by a ball mill or the like. In addition, when supplying with gas, a thing with a low boiling point is desirable.

  The unsaturated compound used in the present invention has the general formula

又は一般式

Or general formula

で示される。ここで、Ｒ_４、Ｒ_５、Ｒ_６及びＲ_７としては、それぞれ水素原子、ハロゲン原子、水酸基、メルカプト基、アシルオキシ基、アルコキシ基、アミノ基、ニトロ基、カルボキシル基、スルホ基又は炭素数１以上３０以下の置換及び無置換の炭化水素基等が挙げられる。

Indicated by Here, R ₄ , R ₅ , R ₆ and R ₇ are each a hydrogen atom, a halogen atom, a hydroxyl group, a mercapto group, an acyloxy group, an alkoxy group, an amino group, a nitro group, a carboxyl group, a sulfo group, or a carbon number of 1 Examples thereof include substituted and unsubstituted hydrocarbon groups of 30 or less.

  Examples of the substituted or unsubstituted hydrocarbon group having 1 to 30 carbon atoms include aliphatic groups (alkyl groups, alkenyl groups, alkynyl groups, etc.), aromatic groups (phenyl groups, naphthyl groups, etc.), heterocyclic groups ( Those containing at least one nitrogen atom, oxygen atom or sulfur atom as a hetero atom), alicyclic groups (cycloalkyl groups, cycloalkenyl groups, cycloalkynyl groups, etc.), spiro compound residues, terpene compound residues, etc. Can be mentioned.

R ₄ , R ₅ , R ₆ and R ₇ may be substituted with an unsaturated hydrocarbon group or a functional group as long as they do not adversely affect the unsaturated bond addition reaction. Here, functional groups include halogen atoms, amino groups, carboxyl groups, sulfo groups, mercapto groups, epoxy groups, cyano groups, nitro groups, hydroxyl groups, alkoxy groups, alkoxycarbonyl groups, acyl groups, acyloxy groups, and quaternary ammonium groups. Group, polyalkylene ether group and the like.

  Specific examples of the unsaturated compound used in the present invention include acetylene, ethylene, propylene, butene, octene, decene, octadecene and the like. Moreover, butadiene, isoprene, etc. which have two or more double bonds can also be used.

In the present invention, a compound in which R ₄ , R _5, and R ₆ are hydrogen atoms, R ₇ is an alkyl group having 1 to 30 carbon atoms, and R ₇ is 8 or more carbon atoms is generally used. 18 or less is preferably used. When such an alkyl group is used, the interaction between the powder particles is suppressed.

  As the catalyst for the addition reaction used in the present invention, platinum group catalysts, that is, ruthenium, rhodium, palladium, osmium, iridium and platinum compounds are suitable, and palladium and platinum compounds are particularly suitable. In the palladium system, palladium (II) chloride, ammonium tetraaminepalladium (II) chloride, palladium (II) oxide, palladium (II) hydroxide and the like can be mentioned. Platinum-based platinum (II) chloride, tetrachloroplatinic acid (II), platinum chloride (IV), hexachloroplatinic acid (IV), ammonium hexachloroplatinate (IV), platinum (II) oxide, platinum (II) hydroxide Platinum (IV) dioxide, platinum (IV) oxide, platinum (IV) disulfide, platinum (IV) sulfide, potassium hexachloroplatinate (IV), and the like. Furthermore, an amine catalyst such as tributylamine or a polymerization initiator can be used.

  In the surface treatment with the cationic surfactant, the powder is preferably coated with the cationic surfactant. At this time, the powder is coated with the hydrophobic group of the surfactant by the interaction between the powder surface and the cation. Thereby, the interaction between the powder particles is reduced and the dilatant behavior is not exhibited.

  Examples of cationic surfactants include alkyltrimethylammonium salts such as stearyltrimethylammonium chloride, dialkyldimethylammonium salts such as distearyldimethylammonium chloride, alkylpyridinium salts such as cetylpyridinium chloride, alkyl quaternary ammonium salts, and alkyldimethyl. Examples include benzylammonium salt, alkylisoquinolinium salt, dialkyl morpholinium salt, POE alkylamine, alkylamine salt, polyamine fatty acid derivative, amyl alcohol fatty acid derivative, benzalkonium chloride, and benzethonium chloride.

  Surface treatment with a cationic surfactant can be performed by dispersing a powder and a cationic surfactant in water or an aqueous solvent to prepare a dispersion, and heating the dispersion to evaporate the solvent. it can. The ratio of the weight of the cationic surfactant to the weight of the powder is preferably 0.005 or more and 0.05 or less. Thereby, the surface of the powder can be coated with the cationic surfactant.

  In the molding method of the composition of the present invention, a slurry containing the surface-treated powder is produced. For the production of the slurry, it is preferable to use a wet disperser that performs pulverization by applying an impact force to the powder in a solvent. Examples of wet dispersers include sand grinder mills, bead mills, ball mills and other medium agitation mills, homomixers, clear mixes, roller mills, TK mills, etc., but disperse the powder to a state close to primary particles. As long as it can be used, it can be used without particular limitation. Among them, a medium stirring mill such as a batch type bead mill such as a basket mill having a relatively strong dispersion force, a horizontal type, a vertical type or an annular type bead mill is particularly preferably used.

  Glass, alumina, zirconia, titanium, steel, and the like are used as the material of the medium such as beads, sand, and balls used in the medium stirring mill, and zirconia is particularly preferable. In the case of a bead mill, a diameter of about 1 mm to 10 mm is preferable, and a diameter of 3 mm to 5 mm is more preferable. Further, it is preferable that the powder is firstly pulverized to some extent by dispersing it with a disperser such as a homomixer or a homogenizer before dispersing the powder with a medium stirring mill. This is because by crushing the particles in an agglomerated state by the primary treatment, the load required for dispersion in the medium stirring mill, which is the secondary treatment, can be reduced, and the powder can be dispersed efficiently.

  Examples of the solvent used in the slurry include one or a mixture of two or more selected from lower alcohols such as methanol, ethanol and isopropyl alcohol, and low-boiling organic solvents such as acetone, ethyl acetate, hexane and chlorofluorocarbon. Ethanol is preferred. A small amount of water or a surfactant may be added for the purpose of controlling dispersibility in these solvents. The blending amount of these solvents is usually 10% by weight or more and 100% by weight or less of the raw material composition.

  In the molding method of the composition of the present invention, the slurry is filled in a container and suction press molded. As suction press molding, the filled slurry is pressed with a filter that also serves as a press mold, and the filter press method in which the solvent is leached and removed by suction. The suction press that removes the solvent by pressing the filled slurry while suctioning is performed. Law.

  The powder cosmetic of the present invention can be obtained by using the molding method of the above composition. In order to obtain a powder cosmetic, it is preferable to add untreated powder, polymer spherical powder, oil, surfactant, etc. in addition to the surface-treated powder when producing a slurry.

  Untreated powders include talc, kaolin, mica, muscovite, phlogopite, synthetic mica, sauroite, biotite, lithia mica, vermiculite, magnesium carbonate, calcium carbonate, aluminum silicate, barium silicate, calcium silicate. , Magnesium silicate, strontium silicate, metal tungstate, magnesium, silica, zeolite, barium sulfate, calcined calcium sulfate (baked gypsum), calcium phosphate, fluorapatite, hydroxyapatite, ceramic powder, metal soap (zinc myristate, palmitic acid) Calcium carbonate, aluminum stearate, etc.), extender pigments such as boron nitride; inorganic white pigments such as titanium dioxide and zinc oxide; inorganic red pigments such as iron oxide (Bengara) and iron titanate; γ-iron oxide, etc. Inorganic brown pigment; yellow iron oxide Inorganic yellow pigments such as ocher; Inorganic black pigments such as black iron oxide, carbon black, low-order titanium oxide; Inorganic purple pigments such as mango violet and Baltic violet; Chrome oxide, chromium hydroxide, cobalt titanate, etc. Inorganic green pigments; inorganic blue pigments such as ultramarine and bitumen; inorganic pearl pigments such as titanium oxide-coated mica, titanium oxide-coated bismuth oxychloride, titanium oxide-coated talc, colored titanium oxide-coated mica, bismuth oxychloride, and fish scale foil; Metal powder pigments such as aluminum powder and copper powder; red 201, red 202, red 204, red 205, red 220, red 226, red 228, red 405, orange 203, orange 204 , Organic pigments such as yellow 205, yellow 401, blue 404; red 3; red 104; red 1 Zircon lakes such as 06, Red 227, Red 230, Red 401, Red 505, Orange 205, Yellow 4, Yellow 5, Yellow 202, Yellow 203, Green 3 and Blue 1 , Organic lake pigments such as barium lake and aluminum lake; natural pigments such as chlorophyll and β-carotene.

  The polymer spherical powder is preferably an organopolysiloxane elastomer spherical powder, a composite spherical powder using this as a mother powder, a polyurethane spherical powder, a composite spherical powder using this as a mother powder, etc., and commercially available products such as Trefil E-505C, Trefill E-506C, Trefill E-506S (Toray Dow Corning Silicone), Silicone Powder KSP-100 (Shin-Etsu Chemical Co., Ltd.), Plastic Powder D-400, Plastic Powder D-800 (Toyo Pigment) ) And the like.

  Oils include solid fats such as cacao butter, hardened coconut oil, hardened oil, molasses, hardened castor oil, waxes such as beeswax, candelilla wax, carnauba wax, lanolin, polyethylene wax, paraffin wax, ceresin, petrolatum, microcrystalline. Hydrocarbon waxes such as wax, higher alcohols such as cetyl alcohol, cetostearyl alcohol, behenyl alcohol, monostearyl glycerin ether (batyl alcohol), evening primrose oil, camellia oil, macadamia nut oil, olive oil, castor oil, safflower oil, cottonseed oil, Liquid fats such as jojoba oil, 2-ethylhexyl palmitate, cetyl lactate, 2-hexyldecyl adipate, di-2-ethylhexyl sebacate, neopentyl glycol dioctanoate, tri-2-ethylhexa Acid glycerin, triisooctanoic acid glycerin, tri-2-ethylhexanoic acid trimethylolpropane, tetra-2-ethylhexanoic acid pentane erythritol and other ester oils, liquid paraffin, squalane, polybutene and other hydrocarbon oils, dimethylpolysiloxane, methyl Chain polysiloxane such as phenyl polysiloxane, diphenyl polysiloxane, cyclic polysiloxane such as octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexanesiloxane, amino-modified polysiloxane, alkyl-modified polysiloxane, fluorine-modified polysiloxane And silicone oils such as various modified polysiloxanes. These oil components are blended in one kind or a mixture of two or more kinds. The blending amount of the oil is preferably 2% by weight or more and 30% by weight or less of the powder cosmetic, and more preferably 10% by weight or more and 20% by weight or less.

  Examples of surfactants include soap bases, fatty acid soaps such as sodium laurate, higher alkyl sulfates such as sodium lauryl sulfate, and alkyl ether sulfates such as polyoxyethylene (hereinafter abbreviated as POE) lauryl sulfate triethanolamine. Ester salts, N-acyl sarcosine acids such as sodium lauroyl sarcosine, higher fatty acid amide sulfonates such as coconut oil fatty acid methyl tauride sodium, phosphate ester salts such as POE stearyl ether phosphate, di-2-ethylhexyl Sulfosuccinates such as sodium sulfosuccinate, alkylbenzene sulfonates such as sodium dodecylbenzene sulfonate, N-acyl glutamates such as disodium N-stearoyl glutamate, hydrogenated coconut oil fatty acid glycerol sulfate sodium Higher fatty acid ester sulfate such as um, sulfated salt such as funnel oil, POE alkyl ether carboxylate, POE alkyl allyl ether carboxylate, α-olefin sulfonate, higher fatty acid ester sulfonate, secondary alcohol Anionic surfactants such as sulfates, higher fatty acid alkylolamide sulfates, sodium louroyl monoethanolamide succinate, ditriethanolamine N-palmitoyl aspartate, sodium caseinate; alkyltrimethylammonium such as stearyltrimethylammonium chloride Salts, dialkyldimethylammonium salts such as distearyldimethylammonium chloride, alkylpyridinium salts such as cetylpyridinium chloride, alkyl quaternary ammonium salts, Cationic surfactants such as benzyl ammonium salt, alkyl isoquinolinium salt, dialkyl morpholinium salt, POE alkyl amine, alkyl amine salt, polyamine fatty acid derivative, amyl alcohol fatty acid derivative, benzalkonium chloride, benzethonium chloride; Amphoteric surfactants such as 2-undecyl-N, N, N- (hydroxyethylcarboxymethyl) -2-imidazoline sodium and other imidazoline-based amphoteric surfactants and betaine-based amphoteric surfactants such as lauryldimethylaminoacetic acid betaine Sorbitan fatty acid esters such as sorbitan monoisostearate and sorbitan sesquioleate, glycerin polyglycerin fatty acids such as glyceryl monostearate, and propylene glycol fatty acid esters such as propylene glycol monostearate Hydrophobic, non-ionic surfactants such as hardened castor oil derivatives, glycerin alkyl ethers; POE sorbitan fatty acid esters such as POE sorbitan monostearate, POE sorbite fatty acid esters such as POE sorbit monooleate, POE glycerin monoiso POE glycerin fatty acid esters such as stearate, POE stearyl ether, POE alkyl ethers such as POE cholestanol ether, POE alkyl phenyl ethers such as POE nonyl phenyl ether, pluronic types such as Pluronic, POE / polyoxypropylene (hereinafter referred to as POE / polyoxypropylene) POP / POP alkyl ethers such as cetyl ether, tetra-POE / tetra-POP ethylenediamine condensates such as tetronic, POE castor oil, POE POE castor oil hardened castor oil derivatives such as hydrogenated castor oil, POE beeswax lanolin derivative, alkanolamide, POE propylene glycol fatty acid ester, POE alkylamine, POE aliphatic amide, sucrose fatty acid ester, POE nonylphenyl formaldehyde condensate, alkyl Examples include hydrophilic nonionic surfactants such as ethoxydimethylamine oxide and trioleyl phosphate. In addition, 1 type, or 2 or more types can be selected and these surfactants can be mix | blended.

  Examples of the form of the powder cosmetic of the present invention include makeup cosmetics such as foundation, white powder, lipstick, eye shadow, teak, mascara and eyeliner, and basic cosmetics such as cleansing, pack and sunscreen agent.

  EXAMPLES Hereinafter, the present invention will be specifically described with reference to examples. However, the technical scope of the present invention is not limited to these examples. In addition, the compounding quantity in a table | surface shows weight%.

  With the formulation shown in Table 1, surface treated sericites 1 to 4 were produced. After the surface treatment sericite 1 and 2 are treated with silicone, the remaining silicon-hydrogen bond is reacted with tetradecene. The surface treatment sericite 1 is a thin film, and the surface treatment sericite 2 is a thick film. ing. The surface-treated sericite 3 is treated with an alkyl cation, and the surface-treated sericite 4 is treated with silicone.

以下に、表面処理セリサイト１〜４の製造方法を示す。
（表面処理セリサイト１の製造）
セリサイト９７ｇとテトラヒドロテトラメチルシクロテトラシロキサン１．５ｇを混合し、約５０℃に加温し、気相で疎水化処理を行った。次に、アルコール０．５Ｌ中に移し、テトラデセン１．５ｇを塩化白金存在下で、攪拌しながらアルキル付加を行い、ろ過、乾燥、粉砕し、表面処理セリサイト１を得た。
（表面処理セリサイト２の製造）
セリサイト９３ｇとメチルハイドロジェンポリシロキサン２．５ｇをイオン交換水０．５Ｌ中で混合し、約１２０℃まで加熱して疎水化処理を行った。次に、テトラデセン４．５ｇとイオン交換水０．５Ｌを添加し、約９０℃まで加熱し、塩化白金存在下でアルキル付加を行い、乾燥、粉砕し、表面処理セリサイト２を得た。
（表面処理セリサイト３の製造）
７０〜８０℃に加熱したイオン交換水１Ｌに、塩化ジステアリルジメチルアンモニウム１ｇを溶解させ、セリサイト９９ｇを添加し、約２時間攪拌した。次に、ろ過、洗浄し、７０℃で約２４時間乾燥させた後、粉砕し、表面処理セリサイト３を得た。
（表面処理セリサイト４の製造）
セリサイト９７ｇとメチルハイドロジェンポリシロキサン３ｇを混合し、２５０〜４００℃に加熱し、冷却、粉砕し、表面処理セリサイト４を得た。

Below, the manufacturing method of the surface treatment sericite 1-4 is shown.
(Manufacture of surface-treated sericite 1)
97 g of sericite and 1.5 g of tetrahydrotetramethylcyclotetrasiloxane were mixed, heated to about 50 ° C., and hydrophobized in the gas phase. Next, the mixture was transferred into 0.5 L of alcohol, and 1.5 g of tetradecene was added with stirring in the presence of platinum chloride, followed by filtration, drying and pulverization to obtain surface-treated sericite 1.
(Manufacture of surface-treated sericite 2)
93 g of sericite and 2.5 g of methylhydrogenpolysiloxane were mixed in 0.5 L of ion-exchanged water, and heated to about 120 ° C. for hydrophobic treatment. Next, 4.5 g of tetradecene and 0.5 L of ion-exchanged water were added, and the mixture was heated to about 90 ° C., subjected to alkyl addition in the presence of platinum chloride, dried and pulverized to obtain surface-treated sericite 2.
(Manufacture of surface-treated sericite 3)
1 g of distearyldimethylammonium chloride was dissolved in 1 L of ion-exchanged water heated to 70 to 80 ° C., 99 g of sericite was added, and the mixture was stirred for about 2 hours. Next, it was filtered, washed, dried at 70 ° C. for about 24 hours, and then pulverized to obtain surface-treated sericite 3.
(Manufacture of surface-treated sericite 4)
97 g of sericite and 3 g of methyl hydrogen polysiloxane were mixed, heated to 250 to 400 ° C., cooled and pulverized to obtain surface-treated sericite 4.

  Next, with the formulation shown in Table 2, the slurry (solid content 35-80%) was dispersed in ethanol for 15 minutes using a sand grinder mill containing zirconia beads, and the resulting slurry (solid content 35-80%) Powder foundations (Examples 1 to 3 and Comparative Examples 1 and 2) were prepared by filling in a dish) and performing suction press molding.

上記のパウダリーファンデーションの成型性、耐衝撃性の評価結果を表３に示す。

Table 3 shows the evaluation results of the moldability and impact resistance of the powdery foundation.

成型性は、吸引プレス成型時のパクト表面に発生するクラックを評価し、クラックが発生しないものを○、クラックの混入率が５％未満であるものを△、クラックの混入率が５％以上であるものを×として判定した。

Formability is evaluated by evaluating cracks generated on the surface of the pact during suction press molding. The case where cracks do not occur is ○, the case where cracks are mixed is less than 5%, the case where cracks are mixed is 5% or more. Some were judged as x.

  Impact resistance is evaluated by dropping a sample in a compact container for cosmetics from a height of 30 cm onto a steel plate with a thickness of 20 mm in a horizontal state after press-molding the sample in a plastic inner dish, The case where the number of drops until the sample was broken was judged as ◯, the case where it was 4-6 times as Δ, and the case where it was 1-3 times as x.

  From this, it was found that the powder cosmetic of the present invention is excellent in moldability and impact resistance, and therefore has a high filling rate.

  Furthermore, Table 4 shows the evaluation results of the usability (smoothness / goodness per skin, moistness, powderiness, uniformity of finish) of the powdery foundation of Example 2.

滑らかさ・肌あたりの良さは、２０名の女性パネラーにパウダリーファンデーションを塗布して評価し、滑らかで肌当たりが良いと回答した人数が１７名以上であるものを◎、１２〜１６名であるものを○、９〜１１名であるものを△、５〜８名であるものを×、４名以下であるものを××として判定した。

Smoothness / goodness per skin was evaluated by applying a powdery foundation to 20 female panelists, and the number of people who responded that they were smooth and had good skin contact was 17 or more. It was judged as ○, those having 9 to 11 people were Δ, those having 5 to 8 people were ×, and those having 4 or less people were xx.

  Moisture is evaluated by applying a powdery foundation to 20 female panelists, ◎ if the number of respondents who are moist is 17 or more, ◎, if it is 12-16, ○, 9-11 It was determined that the name was Δ, the number of 5 to 8 was ×, and the number of 4 or less was xx.

  The powderiness is evaluated by applying a powdery foundation to 20 female panelists, and the number of people who answered that there is no powderiness is 17 or more, and the number of 12-16 people is ○ , 9 to 11 persons were evaluated as Δ, 5 to 8 persons as ×, and 4 or less persons as xx.

  The uniformity of the finish is evaluated by applying a powdery foundation to 20 female panelists, ◎ if the number of people who answered that the finish is more than 17 is ◎, if it is 12-16, ○ Those having 9 to 11 persons were evaluated as Δ, those having 5 to 8 persons were evaluated as ×, and those having 4 or less persons were determined as xx.

  From this, it was found that the powder cosmetic of the present invention is excellent in usability as well as having a high filling rate. This is considered to be a result of the oil component being uniformly coated on the surface of the powder component.

  Next, in the formulation shown in Table 5, using a disper (manufactured by Tokushu Kika Kogyo Co., Ltd.), after dispersing in ethanol for 15 minutes, the obtained slurry was filled into a container (resin middle dish), Powder foundations (Examples 4 to 6, Comparative Examples 3 and 4) were prepared by suction press molding.

上記のパウダリーファンデーションの成型性、耐衝撃性、滑らかさ・肌あたりの良さ、しっとりさ、粉っぽさ、仕上がりの均一さの評価結果を表６に示す。

Table 6 shows the evaluation results of the moldability, impact resistance, smoothness and goodness per skin, moistness, powderiness and finish uniformity of the powdery foundation.

表２に示す処方よりは差が少ないものの、本発明の粉末化粧料は、成型性、耐衝撃性、さらには使用性に優れることがわかった。

Although the difference was smaller than the formulation shown in Table 2, it was found that the powder cosmetic of the present invention was excellent in moldability, impact resistance and usability.

  Hereinafter, various production methods of the powder cosmetic of the present invention will be described.

  Surface-treated sericite 2 (25% by weight), silicone-treated mica (10% by weight), silicone-treated synthetic mica (10% by weight), organopolysiloxane elastomer spherical powder (10% by weight), reticulated silicone resin-coated organopoly Siloxane elastomer spherical powder KSP-100 (Shin-Etsu Chemical Co., Ltd.) (5 wt%), boron nitride (3 wt%), zinc myristate (2 wt%), powdered hydrocarbon wax (3 wt%), silicone treatment Titanium oxide (10% by weight), silicone-treated iron oxide (4% by weight), silicone-treated zinc oxide (5% by weight), squalane (3% by weight), dimethylpolysiloxane (4% by weight), p-methoxycinnamic acid 2-ethylhexyl (3% by weight), polyoxyethylene / alkyl co-modified silicone (1% by weight), sesquiisostear After sorbitan acid sorbitan (1 wt%) preservative (appropriate amount), antioxidant (appropriate amount), and perfume (appropriate amount) were dispersed in ethanol for 15 minutes using a sand grinder mill containing zirconia beads. The obtained slurry was filled in a container (resin-made middle dish) and subjected to suction press molding to obtain a powdery foundation.

  Talc (10 wt%), mica (10 wt%), surface-treated sericite 3 (35 wt%), organopolysiloxane elastomer spherical powder (30 wt%), boron nitride (3 wt%), iron oxide (2 Wt%), ultramarine coated mica titanium (1 wt%), N-acylated lysine (2 wt%), powdered synthetic polyethylene wax (1 wt%), glycerin triisooctanoate (3 wt%), liquid paraffin (2 Weight%), sorbitan sesquiisostearate (0.5 wt%), preservative (appropriate amount), and perfume (appropriate amount) were dispersed in ethanol for 15 minutes using a sand grinder mill containing zirconia beads, The obtained slurry was filled into a container (resin-made middle dish) and subjected to suction press molding to obtain a white powder.

  Talc (8% by weight), surface-treated sericite 2 (45% by weight), mica (15% by weight), spherical nylon powder (5% by weight), organopolysiloxane elastomer spherical powder (15% by weight), iron oxide ( 1.5 wt%), alumina (5 wt%), squalane (2 wt%), dimethylpolysiloxane (2 wt%), sorbitan monooleate (0.5 wt%), preservative (appropriate amount), flavor ( (Suitable amount) was dispersed in ethanol for 15 minutes using a sand grinder mill with built-in zirconia beads, and the resulting slurry was filled into a container (resin medium dish), suction press molded, and eye shadow. Got.

  Surface-treated sericite 3 (30% by weight), silicone-treated mica (15% by weight), silicone-treated synthetic mica (10% by weight), silicone-treated mica titanium (red interference color) (5% by weight), organopolysiloxane elastomer spherical Powder (5 wt%), powdered hydrocarbon wax (3 wt%), silicone-treated titanium oxide (15 wt%), silicone-treated iron oxide (4 wt%), squalane (3 wt%), dimethylpolysiloxane ( 4% by weight), 2-ethylhexyl p-methoxycinnamate (3% by weight), polyoxyethylene / alkyl co-modified silicone (1% by weight), sorbitan sesquiisostearate (1% by weight), preservative (appropriate amount) ), Antioxidant (appropriate amount), and perfume (appropriate amount) were dispersed in ethanol using a disper for 15 minutes, and the resulting slurry It was filled in the container (in resin dish), and the suction press molded to obtain a powdery foundation.

  Talc (10 wt%), mica (10 wt%), surface-treated sericite 2 (45 wt%), spherical methylsiloxane network polymer powder (3 wt%), organopolysiloxane elastomer spherical powder (15 wt%), Aluminum oxide-coated mica titanium (green interference color) (4 wt%), iron oxide (2 wt%), boron nitride (1 wt%), N-acylated lysine (2 wt%), powdered synthetic polyethylene wax (1 Glycerin triisooctanoate (3% by weight), liquid paraffin (2% by weight), sorbitan sesquiisostearate (0.5% by weight), preservative (appropriate amount), and perfume (appropriate amount) using a disper After being dispersed in ethanol for 15 minutes, the obtained slurry was filled in a container (resin-made middle dish) and subjected to suction press molding to obtain a powdery foundation.

  Talc (8% by weight), surface-treated sericite 3 (45% by weight), mica (15% by weight), spherical PMMA powder (5% by weight), KSP-100 (5% by weight), bitumen-coated mica titanium (red interference) Color) (5 wt%), iron oxide (1.5 wt%), barium sulfate (5 wt%), squalane (2 wt%), dimethylpolysiloxane (2 wt%), sorbitan monooleate (0.5 wt%) Weight%), preservative (appropriate amount), and perfume (appropriate amount) were dispersed in ethanol for 15 minutes using a sand grinder mill with built-in zirconia beads, and the resulting slurry was put into a container (resin medium dish). The inside was filled and subjected to suction press molding to obtain an eye shadow.

  Surface-treated sericite 2 (38 wt%), synthetic mica (15 wt%), talc (8 wt%), bengara (0.8 wt%), yellow iron oxide (2 wt%), black iron oxide (0. 1 wt%), zinc white (2 wt%), silicone elastic powder (15 wt%), spherical polyethylene (4 wt%), dimethylpolysiloxane (3 wt%), liquid paraffin (5 wt%), petrolatum (5 % By weight), sorbitan sesquiisostearate (1% by weight), paraben (suitable amount), antioxidant (suitable amount), and fragrance (suitable amount) in ethanol using a sand grinder mill containing zirconia beads for 15 minutes. After the dispersion, the obtained slurry was filled in a container (resin middle dish) and subjected to suction press molding to obtain a powdery foundation.

Claims (8)

In a method for molding a composition containing a powder exhibiting dilatant behavior,
Surface treating the powder;
A method for molding a composition, comprising: a step of producing a slurry containing the surface-treated powder; and a step of filling the slurry into a container and performing suction press molding.   The method for molding a composition according to claim 1, wherein the powder is sericite. The surface treatment step includes
The method for molding a composition according to claim 1, comprising a step of coating the powder with a silicone compound having a silicon-hydrogen bond, and a step of reacting the silicone compound with an unsaturated compound.   The method of molding a composition according to claim 3, wherein the ratio of the weight of the silicone compound to the weight of the powder is 0.01 or more and 0.2 or less.   The method for molding a composition according to claim 3 or 4, wherein a ratio of an equivalent of the unsaturated compound to an equivalent of the silicon-hydrogen bond is 0.5 or more and 5 or less.   The method for molding a composition according to claim 1 or 2, wherein in the surface treatment, the powder is coated with a cationic surfactant.   The method for molding a composition according to claim 6, wherein a ratio of the weight of the cationic surfactant to the weight of the powder is 0.005 or more and 0.05 or less.   A powder cosmetic, which is molded by the method for molding a composition according to any one of claims 1 to 7.