JPH10279826A - Treated powder and cosmetic containing the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a treated powder excellent in water repellency and dispersibility and a powdery cosmetic material contg. no oil by coating the surface of a powder with a silicone compd. having SiH groups and adding an SiH-reactive compd. to the parts of unreacted SiH groups of the silicone compd. in a specified density. SOLUTION: At least one powder having a particle size of 10 μm or lower and selected from among org. and inorg. pigments, metal oxides and hydroxides, mica, pearlescent materials, metals, etc., is used. It may be in the form of agglomerates or moldings. A superfine powder having a particle size of 0.02 μm or lower can be modified, too. Among silicone oils, silicone resins, silicon waxes, etc., a compd. represented by the formula (R<1> to R<3> are each H or a hydrocarbon group optionally halogenated; R<4> to R<6> are each H, etc.; a is 1 or higher; b is 0, 1, or higher; c is O or 2 provided 3<=a+b+c<=10,000; and there is at least one SiH group) is suitable as the silicone compd. An SiH- reactive compd. in an amt. of 100 μmol (based on 1 g of the powder) is added to the silicone compd.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a treated powder and a cosmetic containing the same. More specifically, a functional powder, particularly an alkyl group, is added to a silicone-coated powder at a high density to provide a highly water-repellent, highly dispersible treated powder, and an oil using the same. Free cosmetics.

[0002]

2. Description of the Related Art A technique of modifying a powder by coating the surface of the powder with a silicone compound having Si--H and adding an unsaturated compound to unreacted Si--H groups has been reported. (Japanese Patent Publication No. 1-54380, etc.), but the amount of addition is generally less than about 100 μmol / g per powder, and only an amount necessary for changing the hydrophobicity and the preference for dispersion is added. . When powder cosmetics and the like are produced using such a treated powder, it is difficult to obtain sufficient dispersibility in fats and oils. Therefore, it is necessary to add oil to enhance dispersibility in the system.

[0003] On the other hand, powder cosmetics, especially solid powder cosmetics, tend to solidify with the use of oils and fats with the use thereof. The realization of a solid powder cosmetic containing no oil has been desired. However, in the production of solid powder cosmetics, an oil-free cosmetic containing no oil has not been obtained.

[0004]

DISCLOSURE OF THE INVENTION The present invention has been made in view of the above circumstances, and provides a treated powder having high water repellency and excellent dispersibility, and containing substantially no oil component. The purpose is to provide safe and convenient powder cosmetics.

[0005]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies to achieve the above object, and as a result, the surface of the powder is uniformly coated with a silicone compound, and the surface is further coated with a high density higher than a predetermined value. By introducing a functional group, it is possible to obtain a treated powder having high water repellency and excellent dispersibility,
In addition, they have found that a powder cosmetic containing substantially no oil can be obtained safely and easily using the treated powder, and the present invention has been completed.

That is, the present invention relates to a method of coating a powder surface with a silicone compound having a Si-H group and reacting the unreacted Si-H group portion of the silicone compound with the Si-H group. The present invention relates to a treated powder obtained by adding a compound that can be obtained at a density of 100 μmol / g or more.

[0007] The present invention also relates to a cosmetic containing the above-mentioned treated powder, particularly a solid powder cosmetic containing substantially no oil.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.

Although the powder used in the present invention is not particularly limited, it generally means any object having a particle size of 10 mm or less (sometimes larger than 10 mm). , Organic pigments, inorganic pigments, metal oxides and hydroxides, mica, pearlescent materials, metals, carbon, magnetic powders, silicate minerals, porous materials and the like. These powders may be used alone or in combination of two or more, or may be an aggregate, a molded body, a molded body, or the like. Also on or in the powder other substances (eg colorants, UV absorbers, pharmaceuticals,
(Various additives) may be contained. According to the present invention, any powder including ultrafine powder having a particle size of 0.02 μm or less can be modified (treated).

As organic pigments, for example, Red No. 201,
Red No. 202, Red No. 204, Red No. 205, Red No. 22
No. 0, Red No. 226, Red No. 228, Red No. 305, Orange No. 203, Orange No. 204, Yellow No. 205, Yellow 401
No. and Blue No. 404, and Red No. 3 and Red No. 104
No. 106, Red No. 227, Red No. 230, Red No. 401, Red No. 505, Orange No. 205, Yellow No. 4, Yellow No. 5, Yellow No. 202, Yellow No. 203, Green No. 3, Blue No. 1, etc. And these organic pigments may be zirconium lake, barium lake or aluminum lake.

Examples of the inorganic pigment include navy blue, ultramarine blue, manganese violet, mica coated with (oxide) titanium, bismuth oxychloride, and the like.

As the metal oxide and the metal hydroxide,
For example, magnesium oxide, magnesium hydroxide, calcium oxide, calcium hydroxide, aluminum oxide, aluminum hydroxide, silica, iron oxide (α-Fe ₂ O ₃ , γ-
Fe ₂ O ₃ , Fe ₃ O ₄ , FeO, etc.), yellow iron oxide (especially rod-shaped), red iron oxide, black iron oxide, iron hydroxide, titanium oxide (particularly having a particle size of 0.001 to 0.1 μm). Titanium oxide), lower titanium oxide, zirconium oxide, chromium oxide, chromium hydroxide, manganese oxide, cobalt oxide, nickel oxide and composite oxides and hydroxides of combinations of two or more of these, for example, silica alumina, Examples include iron titanate, cobalt titanate, lithium cobalt titanate, cobalt aluminate and the like.

Examples of the mica include muscovite, phlogopite, biotite, sericite, iron mica, phlogopite, lithia mica, chinwald mica, soda mica, artificial mica or KAl ₂ (A
1, Si ₃ ) O ₁₀ F ₂ , KMg ₃ (Al, Si ₃ ) O
_And mica represented by ₁₀ F ₂ , K (Mg, Fe ₃ ) (Al, Si ₃ ) O ₁₀ F ₂ .

As the pearl luster material, for example, a mica titanium-based composite material, a mica iron oxide-based composite material, bismuth oxychloride, guanine, and a titanium compound containing titanium oxynitride and / or lower titanium oxide are used. Mica and the like. The titanium of the mica-titanium-based composite material may be any of titanium dioxide, low-order titanium oxide, and titanium oxynitride. Further, mica titanium-based composite material or bismuth oxychloride, for example, iron oxide,
It may be a mixture of navy blue, chromium oxide, carbon black, carmine, ultramarine, or the like.

As the metal, for example, aluminum, iron,
Nickel, cobalt, chromium, gold, silver, copper, platinum,
Zinc, indium, tin, antimony, tungsten,
Zirconium, molybdenum, silicon, titanium and the like can be mentioned.

Examples of the magnetic powder include γ-Fe ₂ O ₃ ,
Magnetite (Fe ₃ O ₄ ), Beltrite iron oxide (F
eO _x ; 1.33 <x <1.5) or those modified with cobalt, manganese, nickel, zinc, chromium, etc., or acicular iron or Al, B, Co, Cr, Cu,
Examples thereof include iron powder containing Mo, Mn, Ni, P, Si, Sn, and Zn, CrO _2, and Ba ferrite.

The powder may be iron, nickel, cobalt or an oxide thereof coated on mica,
It is not limited to this.

The silicate minerals include phyllosilicate minerals (for example, kaolin, montmorillonite, clay mica, chlorite, serpentine) and tectosilicate minerals (for example, zeolite), and pyrophyllite. , Talc, chlorite, chrysotile, antigolite, lizadite, kaolinite, deckite, nacrite, halloysite, montmorillonite, nontronite, saponite, sauconite, bentonite, soda zeolite, medium zeolite, scoless zeolite, Thomson zeolite Examples include the albite group such as a sodalite group, a pyroxene, a bouillite, and an exfoliate, and a zeolite such as a mesolite, a heavy zeolitic stone, an acrolite, a chabazite, and a gmelinite.

In the present invention, the treatment of a porous material can be performed well. Examples of the porous material include porous glass beads, hollow silica or zeolite, or metal oxides, metal nitrides, silicates. Minerals, carbonate minerals, sulfate minerals or phosphate minerals, granulated or molded, or granulated or molded and fired after the above minerals, metals, celluloses, fibers or synthetic resins Can be.

As the silicone compound having a Si-H group used in the present invention, any compound can be used as long as it is a silicone compound having a Si-H group. For example, silicone oil, silicone resin, silicone wax and the like can be mentioned. Among them, the following general formula (I)

[0021]

Embedded image (R ¹ HSiO) _a (R ² R ³ SiO) _b (R ⁴ R ⁵ R ⁶ SiO _1/2 ) _c (I) wherein R ¹ , R ² and R ³ are each independently A hydrogen atom or a hydrocarbon group having 1 to 10 carbon atoms that can be substituted with at least one halogen atom (provided that
R ¹ , R ² and R ³ are not simultaneously hydrogen atoms);
R ⁴ , R ⁵ and R ⁶ are each independently a hydrogen atom or a hydrocarbon group having 1 to 10 carbon atoms which can be substituted with at least one halogen atom; a is an integer of 1 or more; b is 0 or an integer of 1 or more; c is 0 or 2 (provided that 3 ≦ a + b + c ≦ 10000); and the compound contains at least one Si—H group moiety. Silicone compounds are preferably used.

Here, when c = 0, the following general formula (I
II)

[0023]

Embedded image (R ¹ HSiO) _a (R ² R ³ SiO) _b (III) wherein R ¹ , R ² , R ³ , a and b are as defined in the above formula (I). However, preferably, R ¹ , R ² and R ³ are each independently a lower alkyl group having 1 to 4 carbon atoms or an aryl group (for example, a phenyl group) which can be substituted with at least one halogen atom (particularly a fluorine atom). Yes; a +
b is 3 or more, preferably 10 to 1,000, particularly preferably 20 to 500]. Preferably, two or more hydrogen atoms are present in one molecule. Specific examples of the compound of the general formula (III) include a cyclic methyl hydrogen polysiloxane.

When c = 2, the following general formula (I)
V)

[0025]

Embedded image (R ¹ HSiO) _a (R ² R ³ SiO) _b (R ⁴ R ⁵ R ⁶ SiO _1/2 ) ₂ (IV) wherein R ^{1 to} R ⁶ , a and b are the same as defined above. As defined in formula (I). However, preferably, R ^{1 to} R ⁶ are each independently a lower alkyl group or an aryl group having 1 to 4 carbon atoms (for example, a phenyl group) which can be substituted with at least one halogen atom (particularly, a fluorine atom); Is 10 to 100
0, especially 20 to 500]. Specific examples of the general formula (IV) 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, -tetramethylcyclotetrasiloxane and the like can be mentioned.

The compound capable of reacting with the Si—H group (Si—H group reactive compound) used in the present invention is a compound capable of reacting with the unreacted Si—H group of the silicone compound. Any compound can optionally be used.

The Si—H group-reactive compound is for adding to the unreacted Si—H portion of the silicone compound to introduce a desired pendant group into the silicone compound. Therefore, various functions can be imparted to the powder by appropriately selecting the Si-H reactive compound and introducing a desired pendant group. Here, the “pendant group” is a residue of a compound capable of reacting with a Si—H group portion, and means a group introduced into a silicone compound by an addition reaction of the compound.
The pendant groups impart various properties and functions to the powder. The hydrophobicity can be further enhanced by adjusting the type or length of the hydrocarbon group of the unsaturated compound to be added.

The pendant group can be arbitrarily selected. For example, an alkyl group has a high water repellency and is well dispersed in fats and oils, and the addition of an ultraviolet absorber makes it possible to obtain an ultraviolet absorbing powder without percutaneous absorption. If a group having an antibacterial action is added, an antibacterial powder without percutaneous absorption can be obtained. Those having an epoxy group added thereto can react with the resin, form a strong resin-powder composite, and become a hard composite that does not expand due to heat.

As such a Si—H group reactive compound,
For example, a compound having an OH group or SH group, for example, an amino acid (such as cysteine) can be used. Further, an unsaturated compound (vinyl compound) having at least one carbon-carbon double bond or triple bond and capable of reacting with the Si-H group portion can be used.

Suitable unsaturated compounds include those represented by the following general formula (II):

[0031]

Embedded image

(Wherein R ⁷ , R ⁸ , R ⁹ and R ¹⁰ are each independently 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 1 carbon atom
Whether it is 30 substituted or unsubstituted hydrocarbon group; or the R ⁷ and R ⁹ carbon - form a carbon bond, -C = C-and together carbon - to form carbon triple bond Or R ⁸ and R ¹⁰ form a carbon-carbon bond;
Which can form an alicyclic group together with C = C-).

In the above, the substituted or unsubstituted hydrocarbon group having 1 to 30 carbon atoms includes, for example, an aliphatic group (eg, an alkyl group, an alkenyl group, an alkynyl group,
Etc.), aromatic groups (for example, phenyl group, naphthyl group,
Etc.), a heterocyclic group (for example, a nitrogen atom as a hetero atom,
Containing one or more oxygen or sulfur atoms, etc.),
Examples include an alicyclic group (eg, a cycloalkyl group, a cycloalkenyl group, a cycloalkynyl group, etc.), a spiro compound residue, a terpene compound residue, and the like.

The hydrocarbon groups R ^{7 to} R ¹⁰ have the general formula (I)
One or more unsaturated hydrocarbon groups (e.g. those exemplified in the definition of general formula (II) above) and / or as long as they do not adversely affect the addition reaction of the compounds of I) due to double or triple bonds. It can be substituted with one or more functional groups. Representative examples of the functional group include a halogen atom, an amino group, a carboxyl group, a sulfo group, a mercapto group, an epoxy group, a cyano group, a nitro group, a hydroxyl group, an alkoxy group, an alkoxycarbonyl group, an acyl group, an acyloxy group, and a quaternary ammonium. And polyalkylene ether groups.

More preferably, the unsaturated compound has one unsaturated bond (double bond, triple bond) at the terminal or at any position.
Alkene or alkyne having, for example, acetylene, ethylene, propylene, butene, octene,
Decene, octadecene and the like can be mentioned. Alkenes etc.
If it has an unsaturated bond, it undergoes an addition reaction with the Si-H group at that position, so cyclohexane,
A cyclic structure such as benzene and naphthalene may be present.

Also, butadiene, isoprene, etc. having two or more double bonds can be used.

In the present invention, in the general formula (II), R ⁸ , R ⁹ and R ¹⁰ in the above general formula (II) are hydrogen atoms;
R ⁷ has 1 to 30 carbon atoms, preferably 8 to carbon atoms.
Those having 18 alkyl groups are preferably used. When an alkyl group is used as the pendant group, a treated powder having particularly high water repellency and high dispersibility can be obtained.

In the present invention, the surface of the powder is uniformly coated with a silicone compound having a Si—H group, and a compound having a pendant group is added to the unreacted Si—H group of the silicone compound in an amount of 100 μmol / powder. / G or more at a high density. By introducing a functional group into the powder at such a high density, not only the functionality can be sufficiently exhibited, but also the performance different from the conventional one can be exhibited. The functional powder of the present invention can be applied to various fields such as cosmetics, paints, and composite materials. In particular, in the case of cosmetics, it is possible to provide a powdery cosmetic which does not contain any conventionally required oil.

The method of coating the silicone compound having a Si—H group with a powder and the method of adding a functional group can be performed by conventional means.

With respect to the method of coating the silicone compound having a Si—H group with a powder, for example, the above silicone compound is dissolved in an organic solvent (chloroform, hexane, benzene, toluene, acetone, etc.), and the powder is added thereto. The powder can be coated with the silicone compound film by dispersing to prepare a dispersion, heating the dispersion to evaporate the solvent, and forming a film on the powder surface. Alternatively, the powder is poured by pouring the dispersion into the poor solvent of the silicone compound, or by pouring the poor solvent into the dispersion and adhering the insolubilized silicone compound onto the powder surface to form a film thereof. The body may be covered.
Further, as in the in-situ polymerization method, the powder may be encapsulated with a coating of the silicone compound by subjecting the silicone compound to monomer polymerization in the presence of a catalyst on the surface of the powder. Alternatively, coating can be carried out by utilizing active sites widely distributed on substantially the entire surface of the powder.

The silicone compound may be sprayed on the powder as it is, or the silicone compound may be sprayed after the powder is dissolved in a solvent.

Alternatively, the powder is preferably coated with the silicone compound in water or an aqueous solvent. The aqueous solvent means a solution containing water as a main component and containing about 80% by weight or more of water. Other 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, examples of water contained in the aqueous solution include ion-exchanged water and distilled water, and inorganic water may be present in the water. As inorganic ions, L
i ⁺ , Na ⁺ , K ⁺ , Rb ⁺ , Cs ⁺ , Mg ⁺⁺ , Ca ⁺ , HS
O4 ^-, Cl ^-, and the like. By changing the content of these ions, the pH of the aqueous system can be controlled, and as a result, the addition reaction of the pendant group in the aqueous system can be controlled. That is, when the pH value is increased by increasing the amount of the inorganic ions, the crosslinking of the Si—H group can be promoted. On the other hand, when the pH value is decreased by decreasing the amount of the inorganic ions, the degree of crosslinking can be suppressed. . Therefore, if the pH value is decreased to make the crosslinking of the Si-H groups less likely to occur and the remaining Si-H groups are increased, the additional density of the pendant groups by the hydrosilylation reaction described later can be increased. In the present invention, the pH is preferably controlled to about 5 to 8 in order to add the compound having a pendant group at a high density of 100 μmol / g or more per powder.

The ratio between the silicone compound and the aqueous solution varies depending on the method of mixing the powder, but it is preferable to carry out the reaction in the range of 0.1 to 100 (weight ratio) of water with respect to 1 silicone.
More preferably, it is 5 to 50. The mixing method can be performed by a conventional method using a commonly used mixer. In the case of wet mixing, the amount of water used is slightly larger, and in the case of dry mixing, the amount of water is slightly smaller.

The amount of the silicone compound relative to the powder is 2-2.
It is preferably 0% by weight, more preferably 3 to 10% by weight. When the amount of the silicone is less than 2% by weight, a pendant group cannot be introduced to the extent that the effects of the present invention can be obtained. Further, the Si—H group-reactive compound is used in the range of 0.5 to 3 of the Si—H group of the silicone compound of the entire system.
Equivalents are preferred, more preferably 1-2 equivalents. Water is mixed with the above amount of silicone compound at the above-mentioned ratio and used as a reaction liquid.

The thus-obtained silicone-coated powder has an unreacted Si-H group, and becomes slightly unstable under severe conditions such as alkali and acid.

Next, a compound capable of reacting with the Si—H group is added to the unreacted Si—H group of the silicone compound coated with the powder. Thereby, the Si—H reactive compound is added to the unreacted Si—H portion of the silicone compound, and a pendant group derived from the Si—H reactive compound is introduced into the silicone compound. By appropriately selecting the Si—H reactive compound and introducing a desired pendant group, various functions can be imparted to the powder.

This will be further described below.
In the step of the coating process, cross-linking between Si-H groups occurs on the powder surface to form a network structure, and the powder surface is coated with a coating of a silicone compound. Not done. For this reason, residual Si-H groups are present and tend to be slightly unstable under severe conditions such as alkalis and acids. This remaining Si-H group is replaced with Si-H
By adding a reactive compound (for example, an unsaturated compound such as an alkene or an alkylene, etc.) by a hydrosilylation reaction to generate a Si—C bond, a powder more stable to an alkali or an acid can be obtained. it can.

Accordingly, various functions can be imparted to the powder by appropriately selecting a Si—H reactive compound (unsaturated compound, etc.) and introducing a desired pendant group. Here, the “pendant group” refers to Si—H
A residue of a compound capable of reacting with a base moiety,
It means a group introduced into the silicone compound by the addition reaction of the compound. The pendant groups impart various properties and functions to the powder. The hydrophobicity can be further enhanced by adjusting the type or length of the hydrocarbon group of the unsaturated compound to be added.

In the present invention, the pendant S
i-H reactive compound was added to 100 g
1 / g or more, preferably 150 μmol / g or more.

Incidentally, both the coating of the silicone compound and the addition reaction of the pendant group may be carried out in an aqueous solution.
For example, a predetermined amount of a silicone compound having a Si-H group, a compound capable of reacting with the Si-H group, and water are charged into a mixer, and after mixing, the mixed solution is sprayed on powder as a mist, A method in which the mixture is heated and mixed, and a catalyst is further added thereto. Further, an aqueous solvent is put into a kneader containing powder, and after stirring and mixing well, a silicone compound having a Si-H group and a compound capable of reacting with the Si-H group are added, and the mixture is heated and mixed to form a catalyst. Addition allows simultaneous coating and addition. The reaction by this contact is preferably carried out while heating, since this shortens the reaction time.

Further, it may be supplied in the form of a gas, or may be stirred and mixed together with the powder by a ball mill or the like. When supplied in gaseous form, those having a low boiling point are desirable.

The heating temperature can be in the range of 50 to 120 ° C., but the higher the temperature, the higher the reaction rate and the shorter the reaction time.

Next, a catalyst is added to promote the hydrosilylation reaction between the Si—H group and the pendant group of the silicone compound.

As a catalyst for accelerating the hydrosilation reaction, a platinum group catalyst, that is, a compound of ruthenium, rhodium, palladium, osmium, iridium, and platinum is suitable, and a compound of palladium and platinum is particularly preferable. Examples of the palladium-based compound include palladium (II) chloride, ammonium tetraamine palladium (II) chloride, palladium (II) oxide, and palladium (II) hydroxide. In the platinum system, platinum (II) chloride, tetrachloroplatinic acid (II), platinum chloride (IV), hexachloroplatinic acid (IV), ammonium hexachloroplatinate (IV),
Platinum (II) oxide, platinum (II) hydroxide, platinum dioxide (IV), platinum (IV) oxide, platinum (IV) disulfide, platinum (IV) sulfide, potassium hexachloroplatinate (IV), and the like. Further, an amine catalyst such as tributylamine or a polymerization initiator can be used.

A solid powder cosmetic containing no oil can be prepared by mixing only the high-addition-density powder thus obtained or other powders.

Powders that can be compounded in addition to this powder include talc, kaolin, mica, sericite, muscovite,
Phlogopite, synthetic mica, biotite, rhombite, lithia mica, permiculite, 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, calcium palmitate, aluminum stearate), inorganic powder such as boron nitride, polyamide resin powder (nylon powder), polyethylene powder, polymethyl methacrylate powder , Polystyrene powder, styrene-acrylic acid copolymer resin powder, benzoguanamine resin powder, silicone powder, polytetrafluoroethylene powder, cellulose powder and other organic powder components; inorganic white pigments such as titanium dioxide and zinc oxide, iron oxide (Red iron), inorganic red pigments such as iron titanate, inorganic brown pigments such as γ-iron oxide, inorganic yellow pigments such as yellow iron oxide and loess, black iron oxide, carbon black, and inorganics such as lower titanium oxide Black pigment, mango violet, cobalt bar Inorganic purple pigments such as olet, inorganic green pigments such as chromium oxide, chromium hydroxide, and cobalt titanate; inorganic blue pigments such as ultramarine and navy blue; titanium oxide coated mica; titanium oxide coated bismuth oxychloride; titanium oxide coated Talc, colored titanium oxide coated mica, bismuth oxychloride, pearl pigments such as fish scale foil, metal powder pigments such as aluminum powder and copper powder, red 201, red 202, red 2
04, Red 205, Red 220, Red 226,
Red No. 228, Red No. 305, Orange No. 203, Orange No. 20
No. 4, Yellow No. 205, Yellow No. 401 and Blue No. 404, and Red No. 3, Red No. 104, Red No. 106, Red No. 227, Red No. 230, Red No. 401, Red No. 505
No. Orange No. 205, Yellow No. 4, Yellow No. 5, Yellow No. 202
And organic pigments such as zirconium, barium or aluminum lake such as No. 203, Yellow No. 203, Green No. 3 and Blue No. 1.

In addition to these powders, antioxidants, preservatives and the like can be added.

These powders can be mixed using an ordinary mixer, but it is preferable to use those having a high shearing force.

By using the above-mentioned treated powder to which a pendant group is added at a high density according to the present invention, or by mixing other powders, a solid powder cosmetic containing substantially no oil is obtained. Can be. Here, the term "oil" refers to a liquid state at normal temperature, specifically, avocado oil, camellia oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk Oil, sesame oil, persic oil, wheat germ oil, sasanqua oil, castor oil, linseed oil, safflower oil, cottonseed oil, eno oil, soybean oil, peanut oil, teaseed oil, kaya oil, rice bran oil, sinagiri oil, Japanese kiri Oil, jojoba oil, germ oil,
Liquid fats and oils such as glycerin trioctanoate and glycerin triisopalmitate; hydrocarbons such as liquid paraffin, squalene, squalane, and pristane; fatty acids such as oleic acid, tall oil and isostearic acid; lauryl alcohol, oleyl alcohol, isostearyl alcohol,
Liquid higher alcohols such as octyldodecanol; liquid silicones such as methylpolysiloxane, methylphenylpolysiloxane, methylhydrogenpolysiloxane and decamethylpolysiloxane; isopropyl myristate, isopropyl palmitate, hexyl laurate;
Esters such as oleyl oleate, decyl oleate, octyldodecyl myristate, hexyldecyl dimethyloctanoate, diethyl phthalate and dibutyl phthalate are exemplified. Therefore, a cosmetic that does not substantially contain oil means a cosmetic that does not substantially contain any of these liquid oils.

[0060]

The present invention will be described in more detail with reference to the following examples. However, it goes without saying that the scope of the present invention is not limited by these examples.

Example 1-1 Treatment of Sericite 291 g of sericite and 190 g of ion-exchanged water were subjected to an internal volume of 1
The mixture was placed in an L kneader, and sufficiently stirred and mixed at room temperature. Thereafter, 12 g of “Silicone KF-99” (a product of Shin-Etsu Chemical Co., Ltd.), which is a silicone compound having a Si—H group, was added, and the temperature was increased while stirring and mixing, and the water was evaporated at 100 ° C. for 5 hours. Reacted. Next, the remaining water was removed by a reduced-pressure drier to obtain silicone-treated sericite.

Thereafter, 250 g of ion-exchanged water was added to the silicone-treated sericite, and the mixture was stirred and mixed well. Then, 50 g of tetradecene and 15 mg of chloroplatinic acid were added, and the mixture was heated while stirring and mixing, and the water was evaporated at 100 ° C. The reaction was carried out for 5 hours. Next, after removing the remaining water and unreacted tetradecene with a vacuum dryer,
The coated powder was taken out. The resulting treated powder exhibited remarkable hydrophobicity. The addition amount of tetradecene per powder was measured by elemental analysis, and was 382 μmol / g.

Example 1-2 The same treatment was carried out except that the sericite of Example 1-1 was replaced with titanium dioxide to obtain a treated powder. The addition amount of tetradecene was 330 μmol / g.

Example 1-3 The same treatment was carried out except that the sericite of Example 1-1 was changed to silica gel to obtain a treated powder. The addition amount of tetradecene was 318 μmol / g.

Example 1-4 The same treatment was carried out except that sericite in Example 1-1 was replaced with talc to obtain a treated powder. The addition amount of tetradecene is 35
It was 5 μmol / g.

Example 1-5 The same treatment was performed as in Example 1-1 except that sericite was replaced with zinc white to obtain a treated powder. The added amount of tetradecene is 34
It was 8 μmol / g.

Example 1-6 The same treatment as in Example 1-1 was performed, except that the sericite was changed to titanium mica, to obtain a treated powder. The addition amount of tetradecene was 311 μmol / g.

Example 1-7 The same treatment as in Example 1-1 was carried out except that the sericite was replaced with red iron oxide to obtain a treated powder. The addition amount of tetradecene is 2
It was 87 μmol / g.

Example 1-8 The same treatment as in Example 1-1 was performed, except that the sericite was changed to iron oxide yellow, to obtain a treated powder. The addition amount of tetradecene is 3
It was 64 μmol / g.

Example 1-9 The same treatment was performed as in Example 1-1 except that the sericite was changed to black iron oxide to obtain a treated powder. The addition amount of tetradecene is 3
03 μmol / g.

Example 2 50 kg of sericite, 20 kg of mica powder, titanium dioxide 1
0 kg, 15 kg of talc, 1 kg of red iron oxide, 3.2 kg of yellow iron oxide, 0.2 kg of black iron oxide, 0.6 kg of fine titanium dioxide, and 60 kg of ion-exchanged water were thoroughly mixed in a 200 L kneader. Similarly, while adding 3.5 kg of “Silicone KF-99” (manufactured by Shin-Etsu Chemical Co., Ltd.), the temperature was raised and the reaction was carried out at 100 ° C. for 8 hours. next,
The remaining water was removed with a vacuum dryer to obtain a silicone-treated composite powder.

Thereafter, 100 kg of ion-exchanged water was added to the silicone-treated composite powder, and the mixture was stirred and mixed well. Then, 8 kg of tetradecene and 3.5 g of chloroplatinic acid were added, and the mixture was heated while stirring and mixing. The reaction was performed for 2 hours while evaporating water. Next, after removing the remaining water and unreacted tetradecene with a vacuum dryer,
The coated powder was taken out. The resulting treated powder exhibited remarkable hydrophobicity. The addition amount of tetradecene was measured by elemental analysis and found to be 402 μmol / g.

Example 3 150 g of sericite, 100 g of mica powder, titanium dioxide 3
0 g, talc 45 g, red iron oxide 3 g, yellow iron oxide 10
g, 0.6 g of black iron oxide, 1.8 g of finely divided titanium dioxide and 180 g of ion-exchanged water in a 1 L kneader and mixed well. As in Example 1, "Silicone KF-99" (manufactured by Shin-Etsu Chemical Co., Ltd.) ) The temperature was raised while gradually adding 7.5 g, and the reaction was carried out at 100 ° C for 8 hours. Next, remaining water was removed by drying under reduced pressure to obtain a silicone-treated composite powder.

Thereafter, 300 g of ion-exchanged water was added to the silicone-treated composite powder, and the mixture was thoroughly stirred and mixed. After 15 g of tetradecene and 10 mg of chloroplatinic acid were added, the mixture was stirred.
The temperature was raised while mixing was continued, and the reaction was performed at 100 ° C. for 2 hours while evaporating water. Next, after the remaining water and unreacted tetradecene were removed by a vacuum dryer, the coated powder was taken out. The resulting treated powder exhibited remarkable hydrophobicity. The amount of tetradecene added was measured by elemental analysis and found to be 210 μmol / g.

Comparative Example 1 A treated powder composite was obtained in the same manner as in Example 3 except that the amount of “Silicone KF-99” (manufactured by Shin-Etsu Chemical Co., Ltd.) was changed to 3.0 g. . The resulting treated composite powder is hydrophobic, and the added amount of tetradecene is 85μ.
mol / g.

Example 4: Foundation Component Weight% (1) Treated Powder of Example 1-1 40.0 (2) Treated Powder of Example 1-2 13.0 (3) Example 1-4 (4) Treated powder of Example 1-7 1.0 (5) Treated powder of Example 1-8 2.5 (6) Treated powder of Example 1-9 0 1.1 (7) Spherical silica 3.0 (8) Spherical silicone powder 2.0 (9) Spherical polyethylene powder 3.5 (10) Ethylparaben 0.2 Production method Mixing the above components (1) to (9) The mixture was pulverized to a mean particle size of 1 to 5 μm through a pulverizer, passed through a sieve to adjust the particle size, and then compression-molded to obtain a cake-type foundation. Although the obtained foundation did not contain any oil, it could be molded, had good spreadability, had a smooth usability, and had good makeup.

Example 5: Foundation Component Weight% (1) Processed powder of Example 2 85.0 (2) Spherical nylon powder 3.0 (3) Spherical silicone powder 2.0 (4) Spherical polyethylene Powder 9.8 (5) Ethyl paraben 0.2 Production method The above components (1) to (5) are mixed, pulverized through a pulverizer to an average particle size of 1 to 5 μm, and adjusted to a particle size through a sieve, followed by compression molding. Then, a cake-type foundation was obtained. Although the obtained foundation did not contain any oil, it could be molded, had good spreadability, had a smooth usability, and had good makeup.

Example 6: Foundation Component Weight% (1) Processed powder of Example 3 85.0 (2) Spherical nylon powder 3.0 (3) Spherical silicone powder 2.0 (4) Spherical polyethylene Powder 9.8 (5) Ethyl paraben 0.2 Production method The above components (1) to (5) are mixed, pulverized through a pulverizer to an average particle size of 1 to 5 μm, and adjusted to a particle size through a sieve, followed by compression molding. Then, a cake-type foundation was obtained. Although the obtained foundation did not contain any oil, it could be molded, had good spreadability, had a smooth usability, and had good makeup.

Comparative Example 2 A foundation was produced using exactly the same components as in Example 5, except that the treated powder of Comparative Example 1 was used instead of the treated powder of Example 2. did. The resulting foundation was quite powdery and could not be molded.

[0080]

As described in detail above, according to the present invention,
By adding a functional group, especially an alkyl group, to the silicone-coated powder at a higher density than in the past, it is possible to obtain a treated powder having a high water repellency and a function excellent in dispersibility, Further, using this treated powder, a solid powder cosmetic containing substantially no oil can be obtained.

 ──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Tetsuya Kanamaru 1050 Nippacho, Kohoku-ku, Yokohama, Kanagawa Prefecture Inside Shiseido Daiichi Research Center Co., Ltd. Inside Shiseido Daiichi Research Center Co., Ltd. (72) Inventor Kyoko Nagaya 1050 Nippa-cho, Kohoku-ku, Yokohama, Kanagawa Prefecture Inside Shiseido Daiichi Research Center Co., Ltd. 1050 Inside Shiseido Daiichi Research Center Co., Ltd.

Claims (10)

[Claims] Claims: 1. A compound capable of reacting with a Si-H group on an unreacted Si-H group portion of a silicone compound having a powder surface coated with a silicon compound having a Si-H group. A treated powder added at a density of 100 μmol / g or more. 2. The silicone compound having a Si—H group is represented by the following general formula (I): (R ¹ HSiO) _a (R ² R ³ SiO) _b (R ⁴ R ⁵ R ⁶ SiO _{1 / 2} ) _c (I) wherein R ¹ , R ² and R ³ are each independently a hydrogen atom or a hydrocarbon group having 1 to 10 carbon atoms which can be substituted by at least one halogen atom. Yes (However, R
¹ , R ² and R ³ are not simultaneously hydrogen atoms);
R ⁴ , R ⁵ and R ⁶ are each independently a hydrogen atom,
Or a hydrocarbon group having 1 to 10 carbon atoms which can be substituted with at least one halogen atom; a is an integer of 1 or more, b is 0 or an integer of 1 or more, and c is 0 or 2 Wherein the compound has at least one Si-H group portion. (3.ltoreq.a + b + c.ltoreq.10000). 3. The treated powder according to claim 1, wherein the silicone compound is methyl hydrogen polysiloxane. 4. The compound capable of reacting with the Si—H group is an unsaturated compound having at least one carbon-carbon double bond or triple bond and capable of reacting with the Si—H group. The processed powder according to claim 1. 5. The compound capable of reacting with the Si—H group is represented by the following general formula (II): (Wherein, R ⁷ , R ⁸ , R ⁹ and R ¹⁰ independently represent 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, A substituted or unsubstituted hydrocarbon group having 1 to 30 atoms; or R ⁷ and R ⁹
Form a carbon-carbon bond and together with -C = C- can form a carbon-carbon triple bond;
⁸ and R ¹⁰ form a carbon-carbon bond and can form an alicyclic group together with -C = C-). The treated powder according to claim 1. 6. In the above general formula (II), R ⁸ , R ⁹ , R ¹⁰
Is a hydrogen atom, and R ⁷ is a hydrocarbon group having 1 to 30 carbon atoms. 7. In the above general formula (II), R ⁸ , R ⁹ , R ¹⁰
Is a hydrogen atom, and R ⁷ is an alkyl group having 1 to 30 carbon atoms. 8. A cosmetic comprising the treated powder according to any one of claims 1 to 7. 9. The cosmetic according to claim 8, wherein the cosmetic is a solid powder cosmetic. 10. The cosmetic according to claim 8, which contains substantially no oil.