JP2003081771A - Method of producing solid powder cosmetic - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a solid powder cosmetic that gives good application sensation with powder cracking reduced. SOLUTION: Fine particles, a polymer giving a coated layer with the elastic modulus of 1-200 kg/cm<2> and a volatile solvent are mixed, then the solvent is vaporized off to form solid particle powder that has the hardness of 10-75 according to the Asker rubber hardness meter C1L type, a porosity of 0.4-0.7 and impact strength of >=5.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a solid powder cosmetic having a smooth and moist feel, an excellent feeling in use, and less cracking due to external force.

[0002]

[Prior Art] Foundation, Face Powder,
Solid powder cosmetics such as eye shadows are generally manufactured by a press molding method in which a raw material composition is filled in a container and then compressed and solidified. However, a general solid powder cosmetic has a relatively small amount of an oil formulation and thus has a weak binding force between powders, and a high press pressure is required in the above press molding method. The resulting moldings are generally hard and have a powdery feel. When the hardness of the solid powder cosmetic is lowered, the bonding force between the powders is usually lowered accordingly, so that the molded product is easily broken by an external force.

On the other hand, as another molding method, there is a solvent method in which a cosmetic base material is mixed with a low-boiling point organic solvent or the like to form a slurry, which is filled in a container, and then the solvent is removed to solidify the mixture. (Kaisho 56-108703). The solvent method is advantageous in that the content can be uniformly filled, but shrinkage and cracking occur as a large amount of solvent in the slurry evaporates during drying, and the content after molding is easily cracked by external force. However, there was a drawback that it was easy to cake.

[0004]

SUMMARY OF THE INVENTION It is an object of the present invention to provide a method for producing a solid powder cosmetic having a smooth and moist feel, an excellent feeling of use such as powder removal, and a crack which hardly occurs. It is in.

[0005]

Means for Solving the Problems The present inventor has found that if a powder, a specific film-forming polymer are contained, and hardness, porosity and impact resistance are set to specific values, the solid content of the above object is obtained. It has been found that a powder cosmetic can be obtained.

That is, according to the present invention, a powder having an elastic modulus of 1 to 2 is used.
The hardness is characterized by mixing the film-forming polymer (00 kg / cm ²⁾ and the volatile solvent and then volatilizing the volatile solvent to solidify the mixture. The hardness is 10-75 with Asker rubber hardness tester C1L type.
The present invention provides a method for producing a solid powder cosmetic having a porosity of 0.4 to 0.7 and an impact resistance value of 5 or more.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION The solid powder cosmetic material of the present invention has a hardness of 10 to 75 on an Asker rubber hardness meter C1L type,
It is preferable that the porosity is 0.4 to 0.7, particularly 0.45 to 0.7, and the impact resistance value is 5 or more, particularly 7 or more, because it is excellent in use feeling and cracking. When the solid powder cosmetic is a foundation, the hardness is 10
Is more preferably 70 to 70, particularly 10 to 65, and in the case of eye shadow, the hardness is 30 to 75, especially 50 to 7.
More preferably, it is 5.

Here, the hardness is obtained by directly measuring the hardness of a molded product with an Asker rubber hardness meter C1L type. In the following production examples, the measurement was performed by filling, molding and drying the sample in an aluminum inner plate having a diameter of 54 mm and a depth of 4 mm. The porosity was obtained by measuring the weight and volume of the molded product and the true specific gravity of the powder bulk, and using the following equation.

[0009]

[Equation 1]

Here, the term "molded product" refers to a cosmetic material after molding and drying. The powder bulk is a dry powder mixture before molding, and the true specific gravity thereof was measured using an Accupic 1330 type manufactured by Shimadzu Corporation.

The impact resistance is evaluated by repeatedly dropping the molded product from a height of 50 cm onto a 25 mm thick lauan veneer plate until abnormalities such as cracking and cracking occur.

The film-forming polymer used in the present invention has an elastic modulus of 1 to 200 kg / cm ² , and particularly 1 to 100 kg / cm ^2.
Are preferred. When a material having an elastic modulus of more than 200 kg / cm ² is used, the product is inferior in softness and smoothness and the usability is deteriorated. In the present invention, the elastic modulus was measured as follows. That is, first, 10 g of a solution or dispersion of each film-forming polymer was weighed in an amount of 10 g on a petri dish made of Teflon (registered trademark) having a diameter of 5 cm, and naturally dried for 5 to 10 days to obtain a film (thickness 0 .3 ~
0.5 mm) was cut into a strip having a length of 15 mm and a width of 5 mm to obtain a measurement sample. After leaving this sample at 25 ° C. and 30% relative humidity for 24 hours or more, a dynamic viscoelasticity measuring device (UBM
It was fixed to a jig for tensile test of Rheospectler DVE-V4) manufactured by Co., Ltd., and the measurement was carried out under the conditions of vibration frequency 10 Hz and amplitude 10 μm.

As such a film-forming polymer, those having a molecular weight of about 10,000 to 1,000,000 are preferable, and for example, one or more kinds of monomers having a polymerizable double bond are polymerized. The resulting polymer and poly (N-acylalkyleneimine) -modified silicone (JP-A-5-112)
No. 423, JP-A-7-133352, and JP-A-10-9.
5705), vinyl-silicone block polymers (JP-A No. 11-100307) and the like. Examples of the monomer having a polymerizable double bond include ethylenically unsaturated carboxylic acids such as acrylic acid, methacrylic acid, maleic acid and fumaric acid; hydroxyethyl (meth) acrylate, polyethylene glycol mono (meth) acrylate and the like. Unsaturated carboxylic acid ester; unsaturated carboxylic acid amide such as (meth) acrylamide, N-diacetone acrylamide; aminoethyl (meth) acrylate, N, N-dimethylaminoethyl (meth) acrylate, N, N-diethylaminoethyl ( Hydrophilic monomers such as amino group-containing unsaturated carboxylic acid esters such as (meth) acrylate and N, N, N-trimethylaminoethyl (meth) acrylate or salts thereof; styrene, α-methylstyrene, chlorostyrene, alkylstyrene Aromatic vinyl compounds such as Acrylic acid esters such as ethyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, t-butyl (meth) acrylate, cyclohexyl (meth) acrylate And methacrylic acid ester; vinyl cyanide compounds such as acrylonitrile and methacrylonitrile; vinyl esters such as vinyl acetate; halogenated vinyl such as vinyl chloride and vinylidene chloride; trifluoroethyl methacrylate, 2,2,3,3-tetrafluoro Fluorine-based monomers such as propyl methacrylate, 2,2,3,3,4,4-hexafluorobutyl methacrylate, perfluorooctyl methacrylate, and perfluorooctyl acrylate; the following general formulas (1) to (5) Hydrophobic monomers such as silicone macromonomers represented by

[0014]

[Chemical 1]

[In the above formula, R ¹ represents a hydrogen atom or a methyl group, R ^{2 to} R ¹⁰ each represent an alkyl group having 1 to 6 carbon atoms, an alkoxy group having 1 to 6 carbon atoms, or a phenyl group; Indicates a number from 1 to 500]

The poly (N-acylalkyleneimine) -modified silicone has the formula (6) in the molecule.

[0017]

[Chemical 2]

(In the formula, R ¹¹ is a hydrogen atom and has 1 to 22 carbon atoms.
Is an alkyl group, a cycloalkyl group, an aralkyl group or an aryl group, and m is 2 or 3. ) Has a segment of poly (N-acylalkyleneimine) consisting of a repeating unit represented by the formula (1) and a segment of organopolysiloxane, and an alkylene group containing a hetero atom at the terminal of the segment of organopolysiloxane or as a side chain. The poly (N-acylalkyleneimine) segment consisting of the repeating unit represented by the above formula (6) is bound via, and the poly (N-acylalkyleneimine) segment and the organopolysiloxane segment are linked. With a weight ratio of 1/50 to 20/1 and a molecular weight of 1
50,000 to 500,000, especially 50,000 to 30
Those of 10,000 are preferable.

The vinyl / silicone block polymer has the following general formula (7):

[0020]

[Chemical 3]

(Where R¹², R¹³, R¹⁴And R¹⁵Are the same
Or, differently, a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, or
Represents a nitrile group, R¹⁶, R¹⁷, R¹⁸And R¹⁹Are the same
Or, differently, a hydrogen atom or a halogen atom is substituted
Is an alkyl group or an aryl group, Y is halogen
A straight-chain or branched chain having 1 to 10 carbon atoms which may be substituted with an atom
A branched chain saturated or unsaturated hydrocarbon group is shown, and A is -CON
H-group or -COO- group is shown, and B is -NHCO- group or
Represents an —OCO— group. Here, A is a -CONH- group
When B is a -NHCO- group and A is a -COO- group
B is a -OCO- group. q represents a number from 0 to 200,
p shows the number of 0-6, and a shows the number of 2-300. )
Having a silicone polymer unit represented by and a fluorine atom
Vinyl vinyl having a vinyl monomer unit as a constituent unit
A recone block copolymer having the general formula (7)
Silicone monomer that constitutes the silicone polymer unit
5-10 ⁶And the total amount of vinyl monomer units
Number is 10-10⁶And the total number of silicone monomers
And the total number of vinyl monomers is 10²-10⁶And
And the total number of the silicone monomers / the vinyl monomer
Block copo whose ratio of the total number of users is 1/99 to 99/1
A limmer can be mentioned as an example.

As the film-forming polymer, one or more kinds can be used, and 0.1 to 15% by weight, particularly 0.5 to 15% by weight based on the total composition.
It is preferable to add 10 to 10% by weight, more preferably 1 to 8% by weight.

The powder is not particularly limited as long as it is an extender pigment or a coloring pigment usually used in cosmetics. For example, silicic acid, silicic acid anhydride, magnesium silicate, talc, sericite, mica, kaolin, Red iron oxide, clay, bentonite, titanium-coated mica, bismuth oxychloride, zirconium oxide, magnesium oxide, zinc oxide,
Aluminum oxide, calcium sulfate, barium sulfate, magnesium sulfate, calcium carbonate, magnesium carbonate,
Inorganic powders of iron oxide, ultramarine blue, chromium oxide, chromium hydroxide, calamine and carbon black, and composites thereof; polyamide, polyester, polypropylene, polystyrene, polyurethane, vinyl resin, urea resin, phenol resin, fluororesin, silicon Organic powder consisting of resin, acrylic resin, melamine resin, epoxy resin, polycarbonate resin, divinylbenzene-styrene copolymer, silk powder, cellulose, long-chain alkylphosphoric acid metal salt, N-mono long-chain alkylacyl basic amino acid, etc. Examples thereof include a body, an organic powder such as a complex thereof, or a composite powder of the above inorganic powder and an organic powder.

These powders are preferably used because the powders whose surface is originally hydrophobic or those whose surface is hydrophobized can be used and are excellent in the feeling of use. The hydrophobic treatment is
For example, silicone oil, fatty acid metal salt, alkyl phosphoric acid,
It is carried out using a hydrophobizing agent such as an alkali metal salt or amine salt of alkylphosphoric acid, an N-mono long-chain (C8 to C22) aliphatic acyl basic amino acid, or a fluorine compound having a perfluoroalkyl group.

The method of hydrophobizing the powder is not particularly limited, and may be carried out in accordance with a conventional method, and the treatment amount of the hydrophobizing agent with respect to the powder is preferably 0.05 to 20% by weight,
It is more preferably 2 to 10% by weight.

One or more kinds of powders can be used, and it is preferable to add 55 to 99.9% by weight, particularly 65 to 99.9% by weight, and further 75 to 99.9% by weight in the total composition. .

An oil agent can be further added to the solid powder cosmetic of the present invention, and the moist feeling and the contact with the skin are improved, which is preferable. As the oil agent, for example, solid / semisolid oil components such as petrolatum, lanolin, ceresin, microcrystalline wax, carnauba wax, candelilla wax, higher fatty acid, higher alcohol; squalane, liquid paraffin, ester oil, diglyceride, triglyceride, silicone oil, etc. Fluid oil components; examples include fluorine-based oil agents such as perfluoropolyether, perfluorodecalin, and perfluorooctane.

One or more kinds of these oil agents may be used, and it is preferable to add up to about 30% by weight, particularly 20% by weight or less, further 15% by weight or less in the total composition.

The solid powder cosmetic of the present invention further comprises a surfactant, a preservative, an antioxidant, a pigment, a thickener, a pH adjuster,
Perfumes, ultraviolet absorbers, humectants, blood circulation promoters, cooling agents, antiperspirants, bactericides, skin activators and the like can be appropriately added within a range that does not impair the effects of the present invention.

The solid powder cosmetic of the present invention is obtained by mixing powder, a film-forming polymer having an elastic modulus of 1 to 200 kg / cm ² and a volatile solvent, and then volatilizing the volatile solvent to solidify. Manufactured by. Examples of the volatile solvent used here include water; low-boiling alcohols such as ethanol and isopropyl alcohol; hexane, isoparaffin, acetone, ethyl acetate, and volatile silicone oil. Water or an aqueous alcohol solution is particularly preferable. powder,
When the film-forming polymer and the volatile solvent are mixed, the powder is 40 to 94.9% by weight, particularly 50 to 94.9% by weight, the film-forming polymer is 0.1 to 14% by weight, Especially 0.
It is preferable to mix 5 to 10% by weight and 5 to 40% by weight of a volatile solvent. When the volatile solvent is used in an amount of 5 to 40% by weight, the mixture is a slightly moist powder. However, when the amount of the volatile solvent is more than 40% by weight, the mixture of JP-A No. 56-1.
As described in No. 08703, it becomes "slurry", and the solid content shrinks as a large amount of the solvent in the slurry volatilizes during drying, so that the void ratio becomes small, the molded product becomes hard, and cracks etc. occur. Problems can occur,
Not preferable. A mixture of powder, film-forming polymer and volatile solvent is filled in a container, compression molded, and the solvent is volatilized under appropriate conditions (temperature, pressure, time) to give a solidified powder cosmetic. can get. Here, the conditions of compression molding and solvent volatilization can be appropriately determined according to the type, size, and shape of the intended solid powder cosmetic.

[0031]

EFFECTS OF THE INVENTION According to the present invention, a solid powder cosmetic having a smooth and moist feel, good powder removal and an excellent feeling of use, and free from cracks and less cracks by external force can be obtained. The solid powder cosmetics of the present invention are suitable as makeup cosmetics such as foundations, face powders, blushers and eye shadows.

[0032]

EXAMPLES Next, the present invention will be further described with reference to examples.

Preparation Example 1 150 parts of water, 3 parts of sodium lauryl sulfate,
0.5 parts of potassium persulfate was charged, and nitrogen gas was passed to remove dissolved oxygen. Meanwhile, add 17 parts of styrene to the dropping funnel,
33 parts of 2-ethylhexyl acrylate and 2.0 parts of n-dodecyl mercaptan were charged. The temperature of the reaction vessel was raised to 70 ° C. with stirring, and the above monomer was dropped from the dropping funnel over 3 hours. After the completion of dropping, the mixture was aged for 3 hours to remove some aggregates to obtain an alkyl acrylate copolymer emulsion having a solid content of 45% by weight. Further, it was diluted with water to obtain a 12% by weight emulsion.

Preparation Example 2 5 parts of methacrylic acid and 2 parts of methyl methacrylate were placed in a reaction vessel.
2 parts, n-butyl acrylate 33 parts, macroazo polymerization initiator having a polydimethylsiloxane structure in the molecule (VPS-0501, manufactured by Wako Pure Chemical Industries, average molecular weight 30,000 to 40,000)
40 parts and 200 parts of methyl ethyl ketone were charged, and nitrogen gas was flowed for about 1 hour with stirring at room temperature to remove dissolved oxygen. The temperature of the reaction vessel was raised to 80 ° C. with stirring, polymerization was carried out for 6 hours, and then aging was carried out at 85 ° C. for 2 hours to obtain a transparent viscous solution. The obtained solution was diluted with 100 parts of methyl ethyl ketone and then neutralized with 5 parts of 1N-NaOH, and then 600 parts of ion-exchanged water was added. Methyl ethyl ketone was distilled off under reduced pressure from the resulting solution and diluted with ion-exchanged water to obtain an emulsion having a solid content of 12% by weight.

Example 1 A solid powder foundation having the composition shown in Table 1 was produced,
The softness, smoothness, and powder removal were evaluated according to the following criteria. That is, first, the powder components were mixed using a Henschel mixer, then the oil component (dimethylpolysiloxane) was added, and then the film-forming polymer was added and mixed. This was filled in a medium plate, press-molded, and then dried to obtain a solid powder foundation. Regarding impact resistance,
Filling aluminum plate with diameter 54mm and depth 4mm, 3kg / cm
Press-molded at a pressure of ² , dried at 50 ° C and atmospheric pressure for 3 hours, and repeatedly dropped from a height of 50 cm on a 25 mm thick lauan veneer plate until abnormalities such as cracking and cracking occur. It was evaluated by the number of times. The results are also shown in Table 1. The product of the present invention had a softer feel than that of the comparative product, was excellent in feeling of use such as smoothness and powder removal, and had good impact resistance.

(Evaluation criteria) ◎: Excellent. ◯: Good. Δ: Slightly inferior X: Inferior

[0037]

[Table 1]

* 1: A 12 wt% aqueous dispersion prepared by dissolving the one described in Synthesis Example 7 of JP-A-10-95705 in ethanol and substituting the solvent. * 2: Iodozol GH-800 (Kanebo NSC)
Was diluted with water to give a 12% by weight emulsion.

Example 2 Using the same poly (N-acylalkyleneimine) -modified 12% by weight aqueous dispersion as in Example 1, an eye shadow having the composition shown in Table 2 was produced in the same manner as in Example 1.
The evaluation results are shown in Table 2. The product of the present invention had remarkable impact resistance as compared with the comparative product, and had a good feeling in use.

[0040]

[Table 2]

Continued front page    F-term (reference) 4C083 AA082 AB052 AB232 AB242                       AB432 AC022 AC242 AC342                       AC482 AC732 AC792 AC932                       AD011 AD072 AD092 AD152                       AD162 BB21 CC12 CC14                       DD17 DD21 EE06 EE07 EE11

Claims (2)

[Claims] 1. An asker rubber having a hardness characterized by mixing powder, a film-forming polymer having an elastic modulus of 1 to 200 kg / cm ² and a volatile solvent, and volatilizing the volatile solvent to solidify the mixture. Hardness meter C1L type is 10 to 75, porosity is 0.4 to 0.7, and impact resistance value (when a molded product is repeatedly dropped from a height of 50 cm to a lauan veneer plate having a thickness of 25 mm). The method for producing a solid powder cosmetic, wherein the number of occurrences of abnormality is 5 or more. 2. The mixed amount of the powder is 40 to 94.9% by weight, the film-forming polymer is 0.1 to 14% by weight, and the volatile solvent is 5 to 40% by weight. Manufacturing method.