JP2003261418A - Method for producing solid powder cosmetic - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a solid powder cosmetic moldable at low pressures, having high impact resistance with no disintegration of soft organic powder, in the form of uniform molding with little powder stickiness. <P>SOLUTION: A method for producing the solid powder cosmetic is provided, which comprises packing a mold with a composition containing the organic powder 0.05-1 kg/mm<SP>2</SP>in mean collapse strength and subjecting the organic powder to pressure molding at a pressure of ≤20 kg/cm<SP>2</SP>, wherein the packing and/or pressure molding are (is) carried out while applying vibration to the organic powder. <P>COPYRIGHT: (C)2003,JPO

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, which is capable of obtaining a uniform compact having excellent impact resistance and good powder removal without breaking soft organic powder.

[0002]

2. Description of the Related Art Solid powder cosmetics such as foundations and eye shadows are generally manufactured by a press molding method in which a raw material composition is filled in a container and then compressed to solidify.
A general solid powder cosmetic has a relatively small amount of an oil agent and therefore has a weak binding force between powders, and a high pressing pressure is required in the above press molding method. However, in the case of a solid powder cosmetic containing low-strength organic powder, the filling property of the raw material composition is poor even when attempting to fill and mold it in an intermediate dish.
The organic powder was broken by the molding pressure, and a uniform solid powder cosmetic could not be obtained.

[0003]

SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing a solid powder cosmetic, which is capable of obtaining a uniform compact having excellent impact resistance and good powder removal without breaking soft organic powder. To provide.

[0004]

Means for Solving the Problems When producing solid powder cosmetics containing a soft organic powder, the inventors of the present invention can perform filling and / or pressure molding while applying vibration to obtain a soft organic powder. It has been found that a uniform molded article having excellent impact resistance and good powder removal can be obtained without breaking the powder.

The present invention has an average crushing strength of 0.05 to 1 kg /
A method for producing a solid powder cosmetic by filling a composition containing mm ² of organic powder into a container, and then press-molding at a pressure not exceeding 20 kg / cm ² , which comprises filling and / or pressing. The present invention provides a method for producing a solid powder cosmetic, which is performed while applying vibration.

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION The organic powder used in the present invention has an average crushing strength of 0.05 to 1 kg / mm ² , preferably 0.05 to
It is of 0.6 kg / mm ² . Here, the average crushing strength is obtained from the load when one powder particle is loaded by the upper indenter and the particle is broken, and the particle size of the particle. This is the average value when repeated.

In the present invention, the average crush strength is measured by
Shimadzu micro compression tester model; MCTM-200 (manufactured by Shimadzu Corporation) was used according to the instruction manual, and the value was calculated by the following formula (1). Here, d represents the particle size of the powder.

St (crush strength) = 2.8P (breaking load) / πd ² (1)

Examples of such organic powders include aliphatic amide sulfonic acid polyvalent metal salts, acylated amino acid polyvalent metal salts, acylated phosphoric acid polyvalent metal salts, aliphatic ester sulfonic acid polyvalent metal salts, Examples thereof include polyvalent metal salts such as alkylaminomethyl sulfuric acid ester polyvalent metal salts and basic amino acids such as lauroyl lysine. Of these, those having an alkyl group and an amide group in the molecule are preferable,
Aliphatic amide sulfonic acid polyvalent metal salt, acylated amino acid polyvalent metal salt, and acylated phosphoric acid polyvalent metal salt are preferable, and acylated taurine polyvalent metal salt is particularly preferable. The alkyl group in the molecule preferably has 7 to 21 carbon atoms, particularly 9 to 17 carbon atoms. Examples of the polyvalent metal atom include calcium, magnesium, barium, aluminum, zinc,
Examples include iron, titanium, zirconium, calcium,
Alkaline earth metals such as magnesium and barium are preferable, and calcium is particularly preferable.

These organic powders can be used as they are or after the surface is subjected to a hydrophobic treatment. The hydrophobic treatment is
For example, silicone oil, fatty acid metal salt, alkyl phosphoric acid,
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, a conventional method Can be done.
As the hydrophobic treatment agent, a fluorine compound is particularly preferable.
The treatment amount of the hydrophobic treatment agent with respect to the powder is 0.05 to 20.
%, Especially 2 to 10% by weight is preferred.

The organic powder may be used in one kind or more, and is 1 to 90% by weight, especially 5 to 70% by weight in the solid powder cosmetic.
It is preferable that the content is 10% by weight, further 10 to 60% by weight.

In the present invention, in the solid powder cosmetic,
It is preferable to include a film-forming polymer having an elastic modulus of 200 kg / cm ² or less together with the above-mentioned organic powder.

As the film-forming polymer used here,
Modulus 200 kg / cm ² or less, are preferred in particular 1 to 100 kg / cm ^2. 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 10% by weight solution or dispersion of each film-forming polymer was weighed in a Teflon (registered trademark) Petri dish having a diameter of 5 cm, and 5 g to 5-1
A film obtained by air-drying for 0 days (thickness 0.3 to 0.5
mm) was cut into strips with a length of 15 mm and a width of 5 mm to obtain a measurement sample. After leaving this sample at 25 ° C. and a relative humidity of 30% for 24 hours or more, a dynamic viscoelasticity measuring device (manufactured by UBM,
It was fixed to a tensile test jig of Rheospectr DVE-V4) and measured under conditions of a vibration frequency of 10 Hz and an amplitude of 10 μm.

As such a film-forming polymer, one having a molecular weight of about 10,000 to 1,000,000 is 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.

As the monomer having a polymerizable double bond,
For example, ethylenically unsaturated carboxylic acids such as acrylic acid, methacrylic acid, maleic acid and fumaric acid; unsaturated carboxylic acid esters such as hydroxyethyl (meth) acrylate and polyethylene glycol mono (meth) acrylate;
Unsaturated carboxylic acid amides such as (meth) acrylamide and N-diacetone acrylamide; aminoethyl (meth) acrylate, N, N-dimethylaminoethyl (meth) acrylate, N, N-diethylaminoethyl (meth) acrylate, N, Hydrophilic monomers such as amino group-containing unsaturated carboxylic acid esters such as N, N-trimethylaminoethyl (meth) acrylate or salts thereof; aromatic vinyl compounds such as styrene, α-methylstyrene, chlorostyrene and alkylstyrene Methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, 2-
Acrylic ester and methacrylic acid ester such as ethylhexyl (meth) acrylate, t-butyl (meth) acrylate, cyclohexyl (meth) acrylate;
Vinyl cyanide compounds such as acrylonitrile and methacrylonitrile; vinyl esters such as vinyl acetate; vinyl halides such as vinyl chloride and vinylidene chloride; trifluoroethyl methacrylate, 2,2,3,3-tetrafluoropropyl methacrylate, 2, 2, 3, 3, 4, 4
-Fluorine-based monomers such as hexafluorobutyl methacrylate, perfluorooctyl methacrylate, and perfluorooctyl acrylate; the following general formulas (1) to
Hydrophobic monomers such as silicone macromonomers as represented by (5) are mentioned.

[0016]

[Chemical 1]

[Wherein R ¹ represents a hydrogen atom or a methyl group, R ^{2 to} R ¹⁰ are each an alkyl group having 1 to 6 carbon atoms,
N represents an alkoxy group having 1 to 6 carbon atoms or a phenyl group, n
Indicates a number from 1 to 500]

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

[0019]

[Chemical 2]

(In the formula, R ¹¹ is a hydrogen atom and has 1 to 22 carbon atoms.
Of an alkyl group, a cycloalkyl group, an aralkyl group, or an aryl group, wherein m is 2 or 3), and a poly (N-acylalkyleneimine) segment consisting of a repeating unit, and an organopolysiloxane. A poly (N-acylalkyleneimine consisting of the repeating unit represented by the above formula (6), which has a segment of ## STR3 ## at the end of the segment of the organopolysiloxane or as a side chain via an alkylene group containing a hetero atom. ), The poly (N-acylalkyleneimine) segment and the organopolysiloxane segment have a weight ratio of 1/50 to 20/1 and a molecular weight of 10,
000 to 500,000, especially 50,000 to 300,
000 is preferable.

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

[0022]

[Chemical 3]

(Where R¹²~ R¹⁵Is the hydrogen source
A child, an alkyl group having 1 to 6 carbon atoms or a nitrile group,
R¹⁶~ R¹⁹Are respectively replaced by hydrogen atom and halogen atom
Represents an optionally substituted alkyl group or aryl group, and Y is
Saturation of 1 to 10 carbon atoms which may be substituted by halogen atom
Represents a sum or unsaturated hydrocarbon group, A is a -CONH- group or
Represents a -COO- group, B represents an -NHCO- group or -OC.
An O-group is shown. Here, when A is a -CONH- group, B is-
NHCO- group, when A is -COO- group, B is -O
It is a CO-group. q represents a number from 0 to 200, and p represents 0 to
6 represents the number, and a represents the number from 2 to 300).
Vinyl without silicone polymer unit and fluorine atom
Vinyl-silicone vinyl containing monomer units as constituent units
Silicone of the general formula (7), which is a lock copolymer
The total number of silicone monomers that make up the polymer unit is 5
-10 ⁶And the total number of vinyl monomer units is 10
10⁶And the total number of the silicone monomers and the vinyl
Sum of total number of monomers is 10²-10⁶And the
Ratio of total number of silicone monomers / total number of vinyl monomers
Is a block copolymer having a ratio of 1/99 to 99/1,
Can be cited as an example.

The film-forming polymer may be used in one kind or more, and is contained in the solid powder cosmetic in an amount of 0.1 to 15% by weight, particularly 0.5 to 10% by weight, and further 1 to 8% by weight. Is preferred.

Further, the solid powder cosmetic may be blended with an extender pigment and a coloring pigment usually used in cosmetics. For example, silicic acid, anhydrous silicic acid, magnesium silicate, talc, sericite, mica, kaolin, red iron oxide, clay, bentonite, titanium-coated mica, bismuth oxychloride, zirconium oxide, magnesium oxide, zinc oxide, aluminum oxide, titanium oxide, Inorganic powder such as iron oxide, chromium oxide, calcium sulfate, barium sulfate, magnesium sulfate, calcium carbonate, magnesium carbonate, ultramarine blue, chromium hydroxide, calamine and carbon black, and their composites;
Polyamide, polyester, polypropylene, polystyrene, polyurethane, silicone resin, vinyl resin, urea resin, phenol resin, fluorine resin, silicon resin, acrylic resin, melamine resin, epoxy resin, polycarbonate resin, divinylbenzene / styrene copolymer, silk powder Examples thereof include resin powders made of cellulose, etc., resin powders such as composites thereof, or composite powders of the above inorganic powders and resin powders.

One or more kinds of these powders can be used, and they are 0 to 90% by weight, especially 10 to 10% by weight in the solid powder cosmetics.
It is preferable to contain 90% by weight.

An oil agent can be further added to the solid powder cosmetic,
It is preferable because the moist feeling and the contact with the skin are further improved.
As the oil agent, for example, petrolatum, lanolin, ceresin,
Solid / semi-solid oils such as microcrystalline wax, carnauba wax, candelilla wax, higher fatty acids, higher alcohols; squalane, liquid paraffin, ester oil,
Liquid oil components such as diglyceride, triglyceride, and silicone oil; and fluorine-based oil agents such as perfluoropolyether, perfluorodecalin, and perfluorooctane.

One or more of these oil agents may be used, and they may be used in solid powder cosmetics up to about 30% by weight, especially 20% by weight.
It is preferable to contain it in the range of not more than 15% by weight, more preferably not more than 15% by weight.

Solid powder cosmetics further include surfactants, preservatives, antioxidants, pigments, thickeners, pH adjusters, fragrances, ultraviolet absorbers, moisturizers, blood circulation promoters, cooling sensation agents, and antibacterial agents. A sweating agent, a bactericidal agent, a skin activating agent and the like can be appropriately added.

In the present invention, the solid powder cosmetic is prepared, for example, by mixing a powder component containing the above-mentioned organic powder with a film-forming polymer having an elastic modulus of 200 kg / cm ² or less, if necessary. The composition is manufactured by filling the composition in a container and then pressure-molding, and the filling and / or pressure-molding is performed while applying vibration and is 20 kg / cm ² or less, preferably 5-10 kg / cm. It is necessary to perform pressure molding at a pressure of ² . The vibration has a frequency of 40 Hz to 120 kHz, especially 20 to 40 kHz, and an amplitude of 1 in both cases of filling and pressure molding.
The thickness is preferably 0 to 500 μm, and particularly preferably 20 to 50 μm, and vibration and vibration may be applied to a die of a press machine by an amplitude controller to perform filling and pressure molding. In particular, applying vibration during both filling and pressure molding enhances the packing property in advance during filling, and further promotes particle rearrangement during molding, resulting in more uniform and excellent impact resistance. It is preferable because a molded body having the above-mentioned shape can be obtained.

The solid powder cosmetic thus obtained has a hardness of 75 or less, particularly 10 to 75, as measured by Asker rubber hardness tester C1L type, and a porosity of 0.36 or more, particularly 0.
It is 45 to 0.7, and the impact resistance value (the number of times until abnormalities occur when a molded product is repeatedly dropped from a height of 50 cm to a lauan veneer plate having a thickness of 25 mm) is 5 or more, especially 5
It is preferable that it is more than 7 and more than 7, since it is excellent in use feeling and cracking. When the solid powder cosmetic is a foundation, the hardness is 10 to 70, especially 10
It is more preferable that the hardness is from to 65, and in the case of the eye shadow, the hardness is from 30 to 75, and especially from 50 to 75.

[0032]

EFFECTS OF THE INVENTION According to the present invention, it is possible to obtain a solid powder cosmetic which can be molded at a low pressure, does not break the soft organic powder, has excellent impact resistance, and is a uniform molded product with good powder removal. To be Foundation, face powder,
It is suitable for producing makeup cosmetics such as cheek red and eye shadow.

[0033]

EXAMPLES Synthesis Example 1 125.2 g (1.0 mol) of taurine and 1 water in a flask.
000.8 g, 2-propanol 164.5 g, and 4
83.3 g of 8% sodium hydroxide aqueous solution (1.0 mol)
Was charged and dissolved. Then, the temperature was raised to 40 ° C., and 196.7 g (0.9 mol) of lauric acid chloride was adjusted to pH 11.0 with 74.5 g (0.9 mol) of 48% sodium hydroxide aqueous solution, while taking about 2 hours. Added. Further, the mixture was stirred at 40 ° C. for 1 hour to obtain 1645 g of an aqueous solution of sodium N-lauryl taurine salt. P with hydrochloric acid
The temperature was adjusted to H2.0, the temperature was raised to 40 ° C., and 277.5 g (0.5 mol) of a 20% calcium chloride aqueous solution was added dropwise over 10 minutes. The mixture was stirred at the same temperature for 1 hour and filtered under reduced pressure. Further, the solution was washed with 600 g of ion-exchanged water three times and with 600 g of 2-propanol three times. The cake obtained is dried under reduced pressure and the white N-lauryl taurine calcium salt is added to the cake.
Obtained 78 g (95%).

Example 1 A solid powder foundation having the composition shown in Table 1 was produced. That is, first, the powder components are mixed by using a Henschel mixer, and then a film-forming polymer is further added and mixed, and the mixture is filled in a medium plate (aluminum medium plate having a diameter of 54 mm and a depth of 4 mm) and press-molded. After that, it was dried to obtain a solid powder foundation. Filling and molding were performed according to the vibration conditions and the like shown in Table 1 using the apparatus shown in FIG. The obtained foundation was evaluated for hardness, porosity, impact resistance and powder removal according to the following criteria. The results are also shown in Table 1.

(Evaluation method) (1) Hardness: Measured with an Asker rubber hardness meter C1L type.

(2) Porosity: The weight and volume of the molded product and the true specific gravity of the powder bulk were measured and determined by the following equation (2).

[0037]

[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.

(3) Impact resistance: The obtained foundation was repeatedly dropped from a height of 50 cm onto a 25 mm thick lauan plywood board and evaluated by the number of times until abnormalities such as cracking and cracking occurred.

(4) Powder removal: Product (solid powder foundation) using a surface property tester 14DR manufactured by Shinto Kagaku Co., Ltd.
50 times back and forth with a sponge (load 5.88N, 4m
/ Min.), And the weight reduction of the product was taken as the amount of powder removed, and evaluated according to the following criteria. ◯: The amount of powder removed is 1.2 g or more and less than 1.7 g, Δ: The amount of powder removed is 0.7 g or more and less than 1.2 g, or 1.7 g
Or more and less than 2.0 g, x: less than 0.7 g or 2.0 g or more of powder removal amount

[0041]

[Table 1]

* 1: Tospearl 145A (manufactured by Toshiba Silicone Co., Ltd.) * 2: A 12% by weight aqueous dispersion prepared by dissolving the one described in Synthesis Example 7 of JP-A-10-95705 in ethanol and substituting the solvent.

[Brief description of drawings]

FIG. 1 is a view showing an apparatus used for filling a solid powder foundation and performing pressure molding in Examples.

Continued front page    F-term (reference) 4C083 AB212 AB242 AB432 AC662                       AC792 AC902 AD011 AD152                       AD162 BB21 BB24 DD17                       DD21 EE01 EE07 FF06

Claims (3)

[Claims] 1. A container is filled with a composition containing an organic powder having an average crushing strength of 0.05 to 1 kg / mm ² , and then 20 kg.
A method for producing a solid powder cosmetic by pressure molding at a pressure not exceeding / cm ² , wherein the filling and / or pressure molding is performed while applying vibration to the solid powder cosmetic. 2. A frequency of 40 Hz to 120 kHz and an amplitude of 10
The manufacturing method according to claim 1, wherein vibration of 500 μm is applied. 3. The method according to claim 1, wherein the composition contains a film-forming polymer having an elastic modulus of 200 kg / cm ² or less.