KR20090125203A - Granulated silica particle, composite powder, their production methods, and cosmetic preparation containing them - Google Patents

Abstract

Disclosed is a granulated silica particle which provides excellent feeling of use especially when applied to the skin. This granulated silica particle is formed by using, as a constitutional element, a scale-like silica having a thickness of a primary particle of 0.001-0.1 μm and a silanol group (SiOH) per unit specific surface area of 20-70 μmol/m. This granulated silica particle has an average particle diameter of 1-50 μm, and a compressive strength of 1-4 MPa.

Description

Granulated silica particles, composite powders, and preparation methods thereof and cosmetics containing them {GRANULATED SILICA PARTICLE, COMPOSITE POWDER, THEIR PRODUCTION METHODS, AND COSMETIC PREPARATION CONTAINING THEM}

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to granulated silica particles and composite particles containing an active ingredient in granulated silica particles. TECHNICAL FIELD This invention relates to the composite powder which stably contained an active ingredient using the granulated silica particle which has a specific structure using silica, and the strong laminated film formed by the bonding of the silanol groups of this silica particle.

BACKGROUND ART Conventionally, various powder particles are granulated using a spray dryer to synthesize particles to be applied to cosmetic applications (Patent Document 1).

In the manufacturing method of the particle | grains which granulated powder particles together, including the said patent document 1, it mix | blends using water-soluble polymer or a hydrophobic polymer so that particle | grains may not be easily collapsed at the time of manufacture, and adjusts the disintegration property of particle | grains. It was common.

However, when granulation is carried out using a high molecular compound, the shape of the granulated particles after spray drying is distorted due to the sharpness of the polymer, and the malleability to the skin when the granulated particles are incorporated into the cosmetics. The exhibition was bad and the usability was inferior. In addition, the feeling of use of the granulated particles obtained by the blending of the polymers caused nogginess and stickiness and was not satisfactory.

In addition, various attempts have been made to include various active ingredients in powder particles. For example, the technique of containing an active ingredient between layers of this clay mineral using water swellable clay mineral is known (patent documents 3-6). In addition, it has been reported that a composite powder containing an active ingredient is obtained by using a spray dryer as a powder or powder binder using a water-soluble polymer, a hydrophobic polymer or a resin.

However, the composite powder obtained by these techniques is a inclusion containing an active ingredient between layers of clay minerals, but there is a problem that the amount of the active ingredient is small.

For this reason, although the compounding quantity of the said binder can be considered to increase in order to stabilize the composite powder and to raise the containment rate, in that case, the fluidity | liquidity at the time of spraying will worsen, it can not spray stably from a nozzle, or it is an ordinary example of a polymer. There existed a problem that the shape of the composite powder formed after spray drying by shape became a distorted shape.

For this reason, when the formed composite powder was contained in cosmetics, the malleability to skin was bad and usability was inferior. In addition, the compounding of the binder itself tends to lower the usability of the obtained composite powder, and there is a problem that it causes noddiness and stickiness during use of the cosmetics, which was not satisfactory.

[Patent Document 1]: Japanese Patent Application Laid-Open No. 05-201830

[Patent Document 2]: Japanese Patent Application Laid-Open No. 2001-163613

[Patent Document 3]: Japanese Patent Application Laid-Open No. 63-30313

[Patent Document 4]: Japanese Patent Application Laid-open No. 63-50311

[Patent Document 5] Japanese Unexamined Patent Publication No. Hei 1-47706

[Patent Document 6]: JP-A-47711.

Disclosure of Invention

Problems to be Solved by the Invention

Therefore, there is a need to provide a composite powder that can stably and in large quantities contain a means for producing granulated particles giving excellent usability especially when applied to the skin without using a high molecular compound, and an active ingredient, It is a problem of the present invention to provide such a technique.

Means to solve the problem

In view of such a situation, the present inventors have made a thorough review to solve the above problems, and as a raw material, the present inventors have selected, as raw materials, scaly shaped silica having a specific particle diameter and silanol group density, dispersing it in an aqueous solvent, and then spray-drying Without blending a water-soluble polymer or a hydrophobic polymer, forming a granulated silica particle that maintains a nearly spherical shape at the time of manufacture and exhibits ease of disintegration during use, and when the granulated silica particle obtained is added to a cosmetic, it is malleable to the skin. It was found that it was good and a uniform makeup film was obtained. In addition, when the active ingredient is contained in the granulated silica particles, it is possible to form a composite powder having a stable and high inclusion rate without blending a binder, and when the composite powder containing the water-soluble ingredient as an active ingredient is added to the cosmetic, Has excellent malleability, and has excellent adhesion and moisturizing cosmetics, and when the composite powder containing water-insoluble ingredients as an active ingredient is blended with the cosmetic, it has good malleability to the skin and has a feeling of adhesion and emollient. It discovered that the cosmetics excellent in the feel and caking prevention effect were obtained, and completed this invention.

That is, the present invention has an average particle diameter of 1 to 50, wherein the primary particles have a thickness of 0.001 to 0.1 µm and a silanol group (SiOH) of 20 to 70 µmol / m 2 per specific surface area as a component. And granulated silica particles having a compressive strength of 1 to 4 MPa.

According to the present invention, the particle size of the silica particles having a thickness of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of 20 to 70 µmol / m 2 is dispersed in an aqueous solvent and slurried. Spray drying is a method for producing granulated silica particles.

The present invention is a cosmetic containing the granulated silica particles.

In the present invention, a water-soluble component is contained in granulated silica particles formed by using scaly silica having a thickness of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of 20 to 70 mol / m 2. It is a composite powder characterized by the above-mentioned.

The present invention is a slurry in which the flaky silica having a thickness of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of the primary particles is dispersed in an aqueous solvent containing a water-soluble component and slurried. This is a method for producing a composite powder, which is then spray dried with a spray dryer.

The present invention provides a water-insoluble component in the granulated silica particles formed by using the scaly shaped silica particles having a thickness of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of 20 to 70 mol / m 2. It is a composite powder characterized by nesting.

The present invention is prepared by slurrying a flaky silica having a thickness of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of primary particles in an aqueous solvent in which a water-insoluble component is dispersed. This is a method for producing a composite powder, which is then spray dried with a spray dryer.

The present invention adds a scale-like silica having a thickness of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of primary particles in an aqueous solvent in which a water-insoluble component is dispersed as an emulsion composition. After slurrying, this is a method for producing a composite powder, which is spray dried with a spray dryer.

This invention is a cosmetics containing the said composite powder.

Effects of the Invention

The granulated silica particles of the present invention have a stable shape when manufactured without using a high molecular compound. Moreover, when mix | blending this with cosmetics etc. and apply | coating on skin, it disintegrates gradually by physical friction, the malleability to skin is favorable, and it is possible to obtain a uniform cosmetic film. In addition, the composite powder of this invention contains the active ingredient stably and in large quantities in the granulated silica particle, without using a binder component. Therefore, since it disintegrates gradually by physical friction when it mix | blends with a cosmetics and apply | coats on skin, and releases an active ingredient, high cosmetic effect can be expected. In addition, the composite powder itself is blended with a cosmetic, and has good malleability when applied to the skin, and the composite powder containing a water-soluble component as an active ingredient is excellent in adhesion and moisture retention properties, and contains a water-insoluble component as an active ingredient. The composite powder is excellent in adhesion, emollient feeling, and anti-caking effect.

Implement the invention  Best form for

The scale-like silica used as a raw material for producing granulated silica particles of the first embodiment (hereinafter referred to as "first invention") in the present invention has a thickness of the primary particles of 0.001 to 0.1 µm. And silanol groups (SiOH) per specific surface area are from 20 to 70 mol / m 2. The amount of silanol groups per specific surface area corresponds to several to several tens of silica gels. Moreover, the average secondary particle diameter of this flaky silica is 0.05-5 micrometers, and the aspect ratio of thickness and longest particle diameter is 10 or more, Preferably it is 30 or more. Such scaly flaky silica is obtained by the method disclosed by patent document 2, for example, and generally this scaly flaky silica is the density | concentration of 13-15 mass% (henceforth only referred to as "%"). Since it is provided as a colloidal dispersion dispersed in water, it can be used as scaly silica. Examples of such colloidal dispersions include commercially available products such as SUNLOVELY LFS manufactured by Asahi Glass Co., Ltd. (AGC Si-Tech Co., Ltd.).

In addition, the silanol group density of the said flaky silica was measured on the following conditions by the thermogravimetric analysis (model 990 TGA-analyzer (made by TA Instruments Japan)). That is, 20-100 mg of silica was charged into a small quartz crucible and placed in a TGA-analyzer. The sample was heated to 120 ° C. at a rate of 10 ° C./min while dry nitrogen gas was passed through the heating chamber at a flow rate of 50 ml / min to physically remove the adsorbed water from the silica surface. The sample was kept at 120 ° C. until no weight loss could now be observed. Next, the temperature was raised to 300 ° C. at the heating rate as described above, and maintained at this temperature until a constant weight was reached. The same operation was repeated at 500 degreeC, 700 degreeC, 900 degreeC, 1050 degreeC, and 1200 degreeC. At each temperature, characteristic weight loss was observed for each sample. The total silanol group concentration of the silica side was calculated from the total weight% loss up to 1200 ° C. followed by the drying step of 120 ° C. The calculation of the silanol group concentration was performed based on the assumption that 2 moles of silanol groups were bonded by heating to 1 mole of water (which is lost from the sample during the heat treatment). The total silanol group concentration (μmol / m 2) of the silica side was calculated according to the following formula:

Silanol group concentration = W × 1111.1 / SA

Here, W is a weight-% loss difference in equilibrium from 120 ° C constant time to heating at 1200 ° C, and SA is silica BET nitrogen surface area m 2 / g.

As the aqueous solvent used to disperse the scaly silica, purified water, mineral water, deep water, a mixed solvent of water and a lower alcohol, and the like can be used. As lower alcohol which can be used, ethyl alcohol, an isopropyl alcohol, etc. are mentioned, for example. In this invention, it is most preferable to use purified water among these. In addition, when the scaly silica is provided as a colloidal dispersion, it may be further diluted with an aqueous solvent and used in a subsequent granulation step.

The granulated silica particles of the first invention can be prepared by dispersing the scaly silica in an aqueous solvent as necessary to form a slurry, and desolvating it in a granulation step such as spray drying. As a method of forming a slurry, the method of mixing a scale-like silica or its colloidal dispersion, and an aqueous solvent, and forming a slurry continuously is mentioned. At this time, it is also possible to add other components.

It is preferable that the scaly silica concentration in the said slurry exists in the range of less than 20%, and especially 7-15% is preferable because stability and a touch are compatible. If it is 20% or more, the dispersibility of the flaky silica in a slurry is bad, for example, when employing the method of using a spray dryer as a desolvent, it may not be possible to spray stably from a nozzle.

As a desolvent method from a slurry, various methods are available, but the method of spray-drying using a spray dryer etc. is preferable. As a spray dryer used for this spray drying, the thing of the type which has a disc atomizer and a double nozzle as a spraying apparatus can be used preferably. As the spraying conditions of the spray dryer, in the case of a disc type atomizer, the rotation speed is preferably 25000 to 30000 rpm and the flow rate is 30 to 70 ml / min. Moreover, as dry conditions, the temperature range of 90-350 degreeC is mentioned. As such a spray dryer apparatus, L-8 type etc. which are manufactured by Ohkawara Kakohki Co., Ltd. are mentioned.

The average particle diameter of the granulated silica particles obtained as described above is a volume average particle using a laser type dry particle size distribution measuring device (for example, PRO7000S manufactured by SEISHIN ENTERPRISE Co., LTD.). It can be measured as diameter (D ₅₀ ). Although the average particle diameter of the granulated silica particle of this invention does not have a restriction | limiting in particular, It is preferable that it is the range of 1-50 micrometers on a feel, More preferably, it is the range of 1-30 micrometers. In addition, the particle diameter can also be determined from the electron microscope image. In addition, although the shape of the granulated silica particle obtained may be spherical shape, another shape (elliptic spherical shape, flat shape, etc.), an irregular shape, etc., it is preferable that it is spherical. In addition, in the granulated silica particles, there are also hollow particles.

Moreover, the compressive strength of the granulated silica particle of 1st invention can be measured using the micro compression tester MCT-W500 (made by Shimadzu Corporation). The compressive strength is a compressive strength in the range of 1 to 4 MPa when the pressure indenter is a Φ 50 µm plane indenter (made of diamond) and the load speed is measured under the conditions of 0.892 mN / sec and a test force of 9.81 mN. If it is at least this range, it will become easy to collapse.

A second aspect of the present invention (hereinafter referred to as "second invention") is a composite powder containing a water-soluble component as an active ingredient in granulated silica particles, and the scale-like silica that can be used as a raw material is the first invention. Same thing with.

In the second invention, the water-soluble component contained in the composite powder is soluble in water, and since the drying temperature of the spray dryer used for the desolvent is generally 100 ° C or higher, it is usually used for cosmetics having a boiling point exceeding 100 ° C. It is preferable that it is a component used, and in order to mix | blend a water-soluble beauty component stably and a large amount, polyhydric alcohol is preferable. Specific polyhydric alcohols include glycerine, diglyserine, sorbitol, ethylene glycol, dipropylene glycol, diethylene glycol, triethylene glycol, 1,3-butylene glycol, and the like. It is illustrated and can use 1 type, or 2 or more types selected from these.

Moreover, as a water-soluble component, various bioactive components which can be dissolved in it besides the said polyhydric alcohol can also be illustrated. Examples of the physiologically active component used in the present invention include substances which impart some physiological activity to the skin when applied to the skin. For example, whitening ingredients, anti-inflammatory agents, anti-aging agents, slimming agents, resilient agents, antioxidants, moisturizers, blood stimulators, antibacterial agents, fungicides, desiccants, cold agents, warmers, vitamins, amino acids, wound healing accelerators , Irritant, analgesic, cell activator, skin colorant, enzyme component and the like. Among them, natural plant extracts, seaweed extract components, and herbal components are particularly preferred. In the present invention, one or two or more of these bioactive components can be used.

Moreover, water-soluble pigment | dyes, such as red 106, red 227, blue 202, blue 205, yellow 5, yellow 203, green 201, green 202, and orange 205, are mentioned as another water-soluble component. .

The above-mentioned water-soluble component is mixed with the colloidal dispersion of the flaky silica in the state contained in the aqueous solvent, and it slurrys. The aqueous solvent used here means purified water, mineral water, deep water, or a mixed solvent of these water and lower alcohol. As lower alcohol, ethanol, isopropyl alcohol, etc. are mentioned, for example. In this invention, it is most preferable to use purified water among these.

Although the manufacturing method of the composite powder of this invention is not limited to this, It is preferable to mix each said component into a slurry form, and to prepare this by desolventing it by granulation processes, such as spray drying. As a method of forming a slurry, a method of continuously forming a slurry by mixing a water-soluble component with a colloidal dispersion of scaly silica and an aqueous solvent by a dispermill, and the like can be given.

It is preferable that the scaly silica concentration in the said slurry exists in the range of less than 20%, and especially 7-15% is preferable because stability and a touch are compatible. If it is 20% or more, the dispersibility of the flaky silica in a slurry is bad, for example, when employing the method of using a spray dryer as a desolvent, it may not be possible to spray stably from a nozzle.

Various methods are available as a desolvent method from a slurry, It is preferable to use the method of spray-drying using a spray dryer etc., although it is not limited to this. As a spray dryer used for this spray drying, the thing of the type which has a disk type atomizer and an airflow nozzle as a spraying apparatus can be used preferably. As the spraying conditions of the spray dryer, in the case of the disc type atomizer, the rotation speed is preferably 25000 to 30000 rpm and the flow rate is 30 to 70 ml / min. In addition, as drying conditions, although the temperature range of 90-350 degreeC is mentioned, 90-120 degreeC is especially preferable in order to avoid denaturation of the water-soluble component contained. As such a spray dryer apparatus, L-8 type which is a product made from Okawara Co., Ltd. is mentioned.

By the said manufacturing conditions, the composite powder which contains 2-25% of water-soluble components preferably is obtained. For example, the containment rate of the composite powder obtained by preparing the glycerine which is a water-soluble component and the 15% colloidal aqueous solution of the scale-like silica in the form of a slurry, and spray-drying with a spray dryer was 25%. In the case where it is intended to contain more than this, it is not possible to completely contain glycerine in the particles formed from the scaly silica, and the glycerine may adhere to the inner wall surface of the tubular body of the drying apparatus. The composite powder may aggregate with this attached glycerine, and the composite powder may not be recovered efficiently. In addition, in this specification, an inclusion rate was calculated | required from the mass (loss of ignition loss) at the time of heating up the obtained composite particle from room temperature to 500 degreeC, and holding at this temperature for 5 hours.

Particle size of the composite powder obtained as mentioned above is, by using a dry type laser particle size distribution analyzer (for example, by Seishin Enterprise Co. PRO7000S the like), it is possible measure the volume average particle diameter (D _50). Although there is no restriction | limiting in particular in the particle diameter of the composite powder of 2nd invention, It is preferable that it is the range of 1-50 micrometers, and it is more preferable that it is the range of 1-30 micrometers on the touch. In addition, the particle diameter can also be determined from the electron microscope image. In addition, although the shape of the obtained composite powder may be spherical shape, another shape, irregular shape, etc., it is preferable that it is spherical.

Moreover, the compressive strength of the composite powder of 2nd invention can be measured using the micro compression tester MCT-W500 (made by Shimadzu Corporation). The compressive strength is preferably from 0.1 to 4 MPa when the pressure indenter is a Φ 50 µm plane indenter (made of diamond), and the load speed is measured under conditions of 0.892 mN / sec and a test force of 9.81 mN. It is preferable that it is the compressive strength of the range of 0.2-3 Mpa, and when it was this range, it turned out that it was excellent in easy collapse.

The composite powder of the second invention can be obtained by forming granulated silica powder with a slurry composed of scaly silica and an aqueous medium in addition to the above-described method, absorbing the water-soluble component therein, and including the same.

A third aspect of the present invention (hereinafter referred to as "third invention") is a composite powder containing a water-insoluble component as an active ingredient in granulated silica particles, and the scale-like silica used as a raw material is the first invention. Same thing with.

As a water-insoluble component contained, an oily component and the emulsion composition containing this are mentioned. Since these water-insoluble components generally have a drying condition of 100 degreeC or more of the spray dryer used for a desolvent, it is preferable that it is a component normally used for cosmetics whose boiling point exceeds 100 degreeC.

As the oily component, for example, paraffin wax, ceresin wax, ozokerite, microcrystalline wax, montan wax, Fischer-Tropsch wax, polyethylene Hydrocarbons such as wax, liquid paraffin, squalane, petrolatum, polyisobutylene and polybutene; Natural waxes such as carnauba wax, beeswax, lanolin wax, and candellia; Tribehenic acid glyceryl, rosin acid pentaerythrityl rosinate, jojoba oil, isococtanoate cetyl, myristic acid isopropyl, trioctanoic acid glyceryl, isostearic acid diglycerol, dipenta Esters such as erythritol fatty acid ester; Fatty acids such as stearic acid and behenic acid; Higher alcohols such as cetanol, stearyl alcohol and behenyl alcohol; Fats and oils such as olive oil, castor oil, mink oil, and rhus succedanea fruit wax; Lanolin derivatives such as lanolin fatty acid isopropyl and lanolin alcohols; Amino acid derivatives such as N-lauroyl-L-glutamic acid di (cholesteryl behenyl octyldodecyl); Silicone emulsions such as dimethyl polysiloxane and methylphenyl polysiloxane; Fluorinated emulsions such as perfluoropolyether, perfluorodecane and perfluorooctane; Oil-soluble pigment | dyes, such as red 226, green 223, and purple 201, etc. are mentioned, 1 type, or 2 or more types can be selected and used from these.

Moreover, as a water-insoluble component contained in the composite powder of 3rd invention, a phospholipid, a ultraviolet absorber, surfactant, etc. are mentioned besides the said oily component.

As a ultraviolet absorber, For example, as a benzophenone system, 2-hydroxy-4-methoxy benzophenone, 2,2'- dihydroxy-4,4'- dimethoxy benzophenone, 2, 4- di Hydroxybenzophenone, 2,2 ', 4,4'-tetrahydroxybenzophenone, and the like, and examples of PABA system include ethyl paraaminobenzoate, paraaminobenzoic acid glyceryl, paradimethylaminobenzoic acid amyl and paradimethyl. Aminobenzoic acid 2-ethylhexyl, a paradihydroxy propyl benzoate, ethyl etc. are mentioned, As a cinnamic-acid system, paramethoxy cinnamic acid 2-ethylhexyl, 4-methoxy cinnamic acid 2-ethoxyethyl, etc. are mentioned. As salicylic acid system, 2-ethylhexyl salicylate, phenyl salicylate, homomentyl salicylate, etc. are mentioned, In addition, 2- (2-hydroxy-5- methylphenyl) benzotriazole, 4-tert- butyl-4 '-Methoxydibenzoylmethane, oxybenzone and the like.

In addition, when the oil component which is a water insoluble component is hard to disperse in an aqueous solvent, it is preferable to mix | blend this as an emulsion composition on the manufacturing method. The emulsion composition in this case may be any of O / W type, W / O type, W / O / W type and O / W / O type as long as it is formed of an aqueous component, an oily component and a surfactant. Although a plurality of combinations may be used, O / W and W / O / W types are preferable.

In order to contain a water-insoluble component in the composite powder of 3rd invention, the method of directly disperse | distributing a water-insoluble component in an aqueous solvent, and mix | blending and mixing and mixing a water-insoluble component beforehand as an emulsion composition as mentioned above There is this.

In either case, an aqueous medium is required, but the aqueous solvent used herein means purified water, mineral water, deep water, or a mixed solvent of these waters and lower alcohols. As lower alcohol, ethyl alcohol, isopropyl alcohol, etc. are mentioned, for example. In 3rd invention, it is most preferable to use purified water among these.

Moreover, as surfactant used in order to make a water-insoluble component into an emulsion composition, as long as it is normally used for cosmetics, it can use without particular limitation. Specifically, glycerin fatty acid esters and alkylene glycol adducts thereof, polyglycerine fatty acid esters and alkylene glycol adducts thereof, propylene glycol fatty acid esters and alkylene glycol adducts thereof , Sorbitan fatty acid esters and alkylene glycol adducts thereof, sorbitol fatty acid esters and alkylene glycol adducts thereof, polyalkylene glycol fatty acid esters, polyoxyalkylene modified silicones, polyoxyalkylene alkyl comodified Nonionic surfactants such as silicone; Alkylbenzene sulfates, alkylsulfonates, α-olefinsulfonates, dialkylsulfosuccinate salts, α-sulfonated fatty acid salts, alkylmethyltaurine salts, N-methyl-N-alkyltaurine salts, polyoxyethylene alkylether sulfates, Anionic surfactants such as polyoxyethylene alkyl phenyl ether sulfate, alkyl phosphate, polyoxyethylene alkyl ether phosphate, polyoxyethylene alkyl phenyl ether phosphate and N-acyl-N-alkylamino acid salt; Cationic surfactants such as alkylamine salts, polyamines and alkanoylamine fatty acid derivatives, alkylammonium salts and alicyclic ammonium salts; Amphoteric surfactants such as lecithin, N, N-dimethyl-N-alkyl-N-carboxymethylammonium betaine, and the like, and one or two or more thereof can be used.

In the said water-insoluble component, the various bioactive components which can be melt | dissolved further can be mix | blended. Examples of such a bioactive component include substances which impart some biological activity to the skin when applied to the skin. For example, whitening ingredients, anti-inflammatory agents, anti-aging agents, slimming agents, emollients, antioxidants, moisturizers, blood circulation accelerators, antibacterial agents, fungicides, desiccants, cooling agents, warming agents, vitamins, amino acids, wound healing accelerators, irritants, Analgesics, cell activators, skin colorants, enzyme components and the like. Among them, natural plant extracts, seaweed extracts, and herbal ingredients are particularly preferred. These bioactive components can use 1 type (s) or 2 or more types.

Moreover, you may add an aqueous component further to the said aqueous solvent. Such an aqueous component is not particularly limited as long as it is usually used in cosmetics, and specifically, polyhydric alcohols such as propylene glycol, 1,3-butylene glycol and dipropylene glycol, glycerine And distilled water such as glycerols such as diglyserine and polyglycerine, Aloe barbadensis, hamamelis, cucumber, lemon, lavender, and rose, and the like. Species or two or more kinds can be used. In addition, in this aqueous solvent, various physiologically active ingredients which can be dissolved therein can be blended. Examples of such a bioactive component include substances which impart some biological activity to the skin when applied to the skin. For example, whitening ingredients, anti-inflammatory agents, anti-aging agents, slimming agents, emollients, antioxidants, moisturizers, blood circulation accelerators, antibacterial agents, fungicides, desiccants, cooling agents, warming agents, vitamins, amino acids, wound healing accelerators, irritants, Analgesics, cell activators, skin colorants, enzyme components and the like. Among them, natural plant extracts, seaweed extracts, and herbal ingredients are particularly preferred. In this invention, 1 type (s) or 2 or more types can be used for these bioactive components.

The composite powder of the third invention is prepared by mixing the above-mentioned water-insoluble component in an aqueous solvent with a scale-like silica together with other optional components to form a slurry and desolventing it. As a method of forming a slurry, the colloidal dispersion of flaky silica and an aqueous solvent, a water-insoluble component or the emulsion containing this, are mixed with a dispermill, and the method of forming a slurry continuously is mentioned. In the case of using waxes having a high melting point, it is preferable to heat-mix this with a liquid oil agent at room temperature (25 ° C.), adjust it to a paste shape, and then add the wax. desirable.

It is preferable that the scaly silica concentration in the said slurry exists in the range of less than 20%, and especially 7-15% is preferable because stability and a touch are compatible. If it is 20% or more, the dispersibility of the flaky silica in a slurry is bad, for example, when employing the method of using a spray dryer as a desolvent, it may not be possible to spray stably from a nozzle.

As the desolvent method from a slurry, since various methods are available, it is not limited to this, The method of spray-drying using a spray dryer etc. is preferable. As a spray dryer used for this spray drying, the thing of the type which has a disk type atomizer and an airflow nozzle as a spraying apparatus can be used preferably. As the spraying conditions of the spray dryer, in the case of the disc type atomizer, the rotation speed is preferably 25000 to 30000 rpm and the flow rate is 30 to 70 ml / min. In addition, as a drying condition, although the temperature range of 90-350 degreeC is mentioned, 90-120 degreeC is especially preferable in order to avoid the modification of the contained aqueous active ingredient. As such a spray dryer apparatus, L-8 type which is a product made from Okawara Co., Ltd. is mentioned.

According to the above production conditions, a composite powder containing preferably 5 to 75% of a water insoluble component can be obtained. For example, the content rate of the composite powder obtained by preparing the squalane which is an oil component and 15% colloidal aqueous solution of the scale-like silica in the form of slurry, and spray-drying with a spray dryer was about 71%. Incidentally, the inclusion rate of the composite powder obtained by preparing an emulsion composition containing squalane and a 15% colloidal aqueous silica gel solution in the form of a slurry and spray drying with a spray dryer was about 68%. In any case, the squalane and the emulsified composition may not be completely contained in the scaly silica in the case where it is intended to be contained further, and the formed composite powder adheres to the inner wall surface of the tubular body of the drying apparatus, It may not be possible to recover the composite powder efficiently by coagulating with the emulsion composition.

Incidentally, the inclusion rate is increased by heating the obtained composite powder from room temperature to 500 ° C using KBF794 (manufactured by Koyo Lindberg Co., Ltd.) and the like at 1100 ° C box furnace. It was set as the mass lost (ignition loss) when hold | maintained at 5 hours.

The particle diameter of the composite powder of the third invention obtained as described above is measured as a volume average particle diameter (D ₅₀ ) using a laser type dry particle size distribution measuring apparatus (for example, PRO7000S manufactured by Seishin Corporation). It is possible. Although there is no restriction | limiting in particular in the particle diameter of the composite powder of 3rd invention, It is preferable that it is the range of 1-50 micrometers, and it is more preferable that it is the range of 1-30 micrometers on the touch. The particle diameter can also be determined from the electron microscope image. In addition, although the shape of the obtained composite powder may be spherical shape, another shape, irregular shape, etc., it is preferable that it is spherical.

Moreover, the compressive strength of the composite powder of 3rd invention can be measured using the micro compression tester MCT-W500 (made by Shimadzu Corporation). The compressive strength is preferably in the range of 0.1 to 4 MPa when the pressure indenter is a Φ 50 µm plane indenter (made by diamond), and the load speed is measured under conditions of 0.892 mN / sec and a test force of 9.81 mN. It is preferable that it is the compressive strength of the range of 0.1-3 Mpa especially, and it turned out that it is excellent in easy collapse if it is this range.

Although the granulated silica particle of the 1st invention and the composite powder of 2nd and 3rd invention of this invention (henceforth these may only be called "composite powder") can be used for various uses, Especially, It is preferable to mix | blend cosmetics, external pharmaceuticals, etc. For example, although the compounding quantity at the time of using the granulated silica particle or composite powder of this invention for cosmetics depends on the formulation, 0.5-100% is preferable and 5-100% is more preferable. When the blending amount of the granulated silica particles or the composite powder is 100%, that is, when all of the cosmetics are granulated silica particles or the composite powder, a binderless prescription powder, that is, a face powder or the like can be obtained. Can be.

In the cosmetics of the present invention, in addition to the granulated silica particles and the composite powder, components normally used in cosmetics, for example, powders excluding the granulated silica particles and the composite powder (hereinafter referred to as "powder"), fats and oils, Oily components such as waxes, hydrocarbons, higher fatty acids, higher alcohols, esters, metal soaps, silicone oils, alcohols, nonionic surfactants, anionic surfactants, cationic surfactants, zwitterionic surfactants, silicone surfactants, and the like. Pigments such as surfactants, dyes, natural pigments, fragrances, vitamins, hormones, preservatives, ultraviolet absorbers, antioxidants, fungicides, plant extracts, special ingredients such as enzymes, acids, alkalis, salts, water, polyhydric alcohols, A polymeric substance, a thickener, a chelating agent, etc. can be suitably selected and used in the range which does not impair the effect of this invention.

The powder is not particularly limited as long as it is a powder normally used in cosmetics, such as plate-like, spherical or needle-like shapes, aerosol forms, particle diameters such as fine particles and pigment grades, porous and nonporous particle structures, and the like. And inorganic powders, organic powders, pigment powders, composite powders, and the like. Specifically, titanium oxide, black titanium oxide, iron blue, ultramarine, bengal (i.e. iron oxides), iron sulfate, black iron oxide, zinc oxide, aluminum oxide, silicic anhydride, magnesium oxide, zirconium oxide Inorganic powders such as magnesium carbonate, calcium carbonate, chromium oxide, chromium hydroxide, carbon black, aluminum silicate, magnesium silicate, magnesium aluminum silicate, mica, synthetic mica, sericite, talc, kaolin, silicon carbide, barium sulfate, and boron nitride visit; Bright powders such as bismuth oxychloride, titanium oxide coated mica, iron oxide coated mica, iron oxide coated mica titanium, organic pigment coated mica titanium and aluminum powder; Nylon, polymethyl methacrylate, alkyl polyacrylate, organopolysiloxane elastomer, polymethyl sesquioxane, crosslinked silicone reticulated silicone block copolymer, polystyrene, acrylonitrile-methacrylic acid copolymer, vinylidene chloride Organic powders such as methacrylic acid copolymers, polyethylene, urethanes, wool powders, silk powders, crystalline cellulose powders, and N-acylazine powders; Pigment powders such as organic tar pigments and lake pigments of organic pigments; Composite powders such as fine particle titanium oxide coated mica titanium, fine particle zinc oxide coated mica titanium, barium sulfate coated mica titanium, titanium oxide-containing silicic anhydride and zinc oxide-containing silicic anhydride, and the like. It is available. In addition, you may use these powders by surface-treating with normal well-known processing agents, such as a fluorine compound, a silicone compound, and surfactant.

As an oil agent, if it is an oil agent normally used for cosmetics, it will not specifically limit. Moreover, when using the composite powder of 3rd invention, it may be same or different from what was contained in the composite powder. Specifically, hydrocarbons such as paraffin wax, ceresin wax, ozokerite, microcrystalline wax, montan wax, Fischer-Tropsch wax, polyethylene wax, liquid paraffin, squalane, petrolatum, polyisobutylene and polybutene ; Natural waxes such as carnauba wax, beeswax, lanolin wax, and candelia; Tribehenic acid glyceryl, rosin acid pentaerythritol ester, jojoba oil, cetylisooctanate, myristic acid isopropyl, trioctanoic acid glyceryl, triisostearic acid glyceryl, dipentaerythritol Esters such as fatty acid esters and macadamiate oil fatty acid phytosteryl macadamiate; Fatty acids such as stearic acid, behenic acid, and 12-hydroxystearic acid; Higher alcohols such as cetanol, stearyl alcohol and behenyl alcohol; Fats and oils, such as olive oil, castor oil, mink oil, and a fuchsia lacquer wax; Lanolin derivatives such as lanolin fatty acid isopropyl and lanolin alcohols; Amino acid derivatives such as N-lauroyl-L-glutamic acid di (cholesteryl behenyl octyldodecyl); Dimethyl polysiloxane, methylphenyl polysiloxane, alkyl-modified organopolysiloxane, alkoxy-modified organopolysiloxane, higher fatty acid-modified organopolysiloxane, silicones such as fluorine-modified silicone, perfluoropolyether, perfluorode Fluorine-based emulsions such as kane and perfluorooctane; and one or two or more thereof can be used.

As surfactant, if it is an oil agent normally used for cosmetics, it will not specifically limit. Moreover, when using the composite powder of 3rd invention, it may be same or different from what was used by the emulsified composition contained in the composite powder. Specifically, glycerin fatty acid esters and alkylene glycol adducts thereof, polyglycerine fatty acid esters and alkylene glycol adducts thereof, propylene glycol fatty acid esters and alkylene glycol adducts thereof Sorbitan fatty acid esters and alkylene glycol adducts thereof, sorbitol fatty acid esters and alkylene glycol adducts thereof, polyalkylene glycol fatty acid esters, polyoxyalkylene modified silicones, polyoxyalkylenealkyl comodified Nonionic surfactants such as silicone; Alkylbenzene sulfates, alkylsulfonates, α-olefin sulfonates, dialkylsulfosuccinate salts, α-sulfonated fatty acid salts, alkylmethyltaurine salts, N-methyl-N-alkyltaurine salts, polyoxyethylene alkylether sulfates, Anionic surfactants such as polyoxyethylene alkyl phenyl ether sulfate, alkyl phosphate, polyoxyethylene alkyl ether phosphate, polyoxyethylene alkyl phenyl ether phosphate and N-acyl-N-alkylamino acid salt; Cationic surfactants such as alkylamine salts, polyamines and alkanoyl amine fatty acid derivatives, alkylammonium salts and alicyclic ammonium salts; Amphoteric surfactants such as lecithin, N, N-dimethyl-N-alkyl-N-carboxymethylammonium betaine, and the like, and one or two or more thereof can be used.

The oil gelling agent is not particularly limited as long as it is usually used for cosmetics. Specifically, dextrin fatty acid ester, sucrose fatty acid ester, starch fatty acid ester, hydroxystearic acid, calcium stearate, and the like can be used, and one or two or more thereof can be used.

The aqueous component is not particularly limited as long as it is usually used in cosmetics. When using the composite powder of 2nd invention, this may be the same as or different from what was contained in the composite powder. Similarly, when using the composite powder of 3rd invention, it may be same or different from what was used by the emulsion composition enclosed in the composite powder. Specifically, Polyhydric alcohols, such as water and a propylene glycol, 1, 3- butylene glycol, dipropylene glycol; Glycerols such as glycerine, diglyserine and polyglycerine; And plant extracts such as aloe vera, hamamelis, cucumbers, lemons, lavenders, and roses, and the like, and one or two or more thereof can be used.

It will not specifically limit, if it is a thing used normally for cosmetics as a ultraviolet absorber. Specifically, 2-hydroxy-4-methoxybenzophenone, 2,4,6-trianilino-p- (carbo-2'-ethylhexyl-1'-oxy) -1,3,5-tri Benzophenones such as azine; PABA systems, such as salicylic acid system, such as 2-ethylhexyl salicylate, and ethyl paradihydroxypropyl benzoate; Dibenzoyl methane type, such as 4-tert-4'-methoxydibenzoyl methane, etc. are mentioned, These 1 type, or 2 or more types can be used.

The water-soluble polymer is not particularly limited as long as it is usually used in cosmetics. Specific examples include cellulose derivatives such as methyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose and carboxymethyl cellulose; Natural polymers such as sodium alginate, carrageenan, quince seed gum, agar, gelatin, xanthan gum, locust bean gum, pectin, gellan gum; Synthetic polymers such as polyvinyl alcohol, carboxyvinyl polymer, alkyl moiety carboxyvinyl polymer, sodium methacrylate, polyacrylic acid glycerine ester, polyvinylpyrrolidone, etc .; Can be used.

The cosmetics of the present invention include those in the form of powder, solid (hereinafter, simply referred to as "solid"), solid powder, stick, liquid, cream, multilayer, sheet, and the like. In addition, the formulation of the cosmetic of the present invention may include a powder cosmetic, an oil cosmetic, an oil-in-water (O / W) emulsion cosmetic, a water-in-oil (W / O) emulsion cosmetic, an aqueous cosmetic, a solvent cosmetic, a sheet cosmetic, and the like. have. On the other hand, the form and formulation in which the effect of the present invention is remarkably exhibited are cosmetics in the form of a solid powder.

The cosmetics of the present invention include, for example, makeup cosmetics such as foundation, face powder, cheek paste, eye shadow, eyebrow, concealer, lipstick, mascara and eyeliner; Skin care cosmetics such as lotion, milky lotion, cream, pack, sunscreen (for example, sun cream), face wash, cleansing agent; Hair cosmetics such as shampoo, rinse, and hair dressing; Moreover, although it can use as a body powder, a bath agent, etc., a makeup cosmetics is especially preferable.

Although the granulated silica particle whose shape is stable is obtained by the 1st invention in this invention, the action mechanism is considered as follows.

In other words, the primary particles of the flaky silica have a thickness of 0.1 µm or less, and the silanol groups (SiOH) per specific surface area are very large, ranging from several times to several tens of silica gel, from 20 to 70 µmol / m 2.

Therefore, since flaky silica is laminated | stacked by normal temperature drying or heat drying, and the silanol groups of a surface are bonded by hydrogen bonding, it is interpreted that it becomes a strong laminated film and forms the granulated silica particle whose shape is stable.

Moreover, although the 2nd invention and 3rd invention in this invention can obtain the composite powder which contains a water-soluble component or a water-insoluble component in large quantity stably, the action mechanism is considered as follows.

That is, as mentioned above, since laminated | stacked flaky silica couple | bonds the silanol groups of a surface by hydrogen bonding, it forms a strong laminated film, and the specific outer surface area of this flaky silica is 50-400 m <2> / g. It is large and has a gap of about 0.05 to 1 ml / g, so that water-insoluble components such as water-soluble components, oil-based components or emulsions containing the same in the gap is captured, and spray-dried, if the water-soluble component, For example, if it is about 5 to 25% and a water insoluble component, it can contain a large amount about 5 to 75%, for example.

1 is an electron micrograph (magnification 2000 times) of granulated silica particles obtained in Example 1;

2 is an optical micrograph (400x magnification) of a 10% colloidal dispersion (slurry) of granulated silica particles of Example 1;

3 is an electron micrograph (2000 times magnification) of the composite powder obtained in Example 12;

4 is an electron micrograph (2000 times magnification) of the comparative composite powder obtained in Comparative Example 4;

5 is an electron micrograph (2000 times magnification) of the composite powder obtained in Example 26;

6 is an electron micrograph (magnification 2000 times) of the composite powder obtained in Example 34;

Fig. 7 is an electron micrograph (2000 times magnification) showing a state in which the composite powder is broken, from which it becomes clear that some of the composite powder has a hollow structure.

Hereinafter, the present invention will be described in detail by Examples and Comparative Examples. Moreover, the various evaluation methods of the cosmetics used by the Example and the comparative example are shown below. In addition, these do not limit this invention at all.

Example  One

Preparation of Granulated Silica Particles

A 15% concentration aqueous solvent colloidal suspension (Sun Lovely-LFS-C; manufactured by Asahigarasu S-ITECH Co., Ltd.) of scale flaky silica having a silanol group density of 60 μmol / m 2 was used as a raw material slurry. This was sprayed using a spray dryer (L-8 type; manufactured by Okawara Kakoki Co., Ltd.) having a disc type atomizer as the atomizer, and the atomizer rotation speed 30000 rpm, flow rate 50 ml / min, inlet temperature setting 200 ° C, outlet temperature Spray drying was carried out at conditions of setting 130 to 140 ° C.

It was 15 micrometers when the average particle diameter of the obtained granulated silica particle was measured with the laser type dry particle size distribution analyzer (PRO7000S by Seishin Corporation). Moreover, it was 2.6 Mpa when the compressive strength of the obtained granulated silica particle was measured by the microcompression tester. In addition, when the obtained granulated silica particle was observed by SEM, it was confirmed that it is spherical particle | grains by which scale-like silica was laminated | stacked (FIG. 1). In addition, when a 10% colloidal dispersion (slurry) in which granulated silica particles were dispersed in purified water was observed under an optical microscope, it was confirmed that the dispersion was uniformly carried out in an aqueous continuous phase without using a surfactant (FIG. 2).

Comparative example  One

The same conditions as in Example 1 were carried out using a spray dryer having a disk-type atomizer as a spraying apparatus, using a slurry having a concentration of 15% in which spherical silica having a silanol group density of 8.0 µmol / m 2 and an average particle diameter of 12 µm was dispersed in purified water. Spray dried. As a result of observing the dried matter with a scanning electron microscope, the spherical particles having a thickness of 12 µm existed as aggregates in which some were aggregated, and no granulated particles were obtained.

Comparative example  2

Example 1 using a spray dryer having a disk-type atomizer as a spraying apparatus, a slurry having a concentration of 15% having a silanol group density of 7.0 μmol / m 2 and an average particle diameter of 25 μm dispersed in purified water silica in purified water. Spray drying was carried out under the same conditions as the above. As a result of observing the dry matter with a scanning electron microscope, the scale-like silica only existed as an aggregate in which a part was aggregated, and no granulated particles were obtained.

Example  2

Foundation in solid powder form (for dry use only):

Using the granulated silica obtained in Example 1 and the dried products obtained in Comparative Examples 1 to 2, a foundation in the form of a solid powder was prepared by the composition shown in Table 1 and the following method.

About the foundation of the obtained solid powder form, "smooth spreadability" and "formation of a uniform cosmetic film" were evaluated by the evaluation method and judgment criteria shown below. This result was combined with Table 1 and shown.

(%)  ingredient invention Comparative product One One 2 3 One Siliconized Titanium Oxide 15.0 15.0 15.0 15.0 2 Siliconized Bengala 1.0 1.0 1.0 1.0 3 Siliconated Iron Sulfate 3.0 3.0 3.0 3.0 4 Silicon-treated black iron oxide 0.5 0.5 0.5 0.5 5 Granulated Silica of Example 1 10.0 - - - 6 Granulated Silica of Comparative Example 1 - - 10.0 - 7 Granulated Silica of Comparative Example 2 - - - 10.0 8 Silicon-treated synthetic mica 20.0 20.0 20.0 20.0 9 Silicon-treated Talc Remaining amount Remaining amount Remaining amount Remaining amount 10 Nylon powder 3.0 3.0 3.0 3.0 11 Crosslinked Silicone / Reticulated Silicone Copolymer 5.0 5.0 5.0 5.0 12 Methyl Paraoxybenzoate 0.2 0.2 0.2 0.2 13 Floating paraffin 2.0 2.0 2.0 2.0 14 Dimethylpolysiloxane 2.0 2.0 2.0 2.0 15 Methoxycinnamic acid octyl 6.0 6.0 6.0 6.0 16 Spices 0.1 0.1 0.1 0.1 <Evaluation Item> Seamless spreadability ◎ × △ △ Formation of uniform makeup film ◎ × × ×

(Production method)

A. Components 1 to 12 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike Co., Ltd.).

B. Mix components 13 to 16 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and subjected to compression molding to obtain a foundation (only for dry use) in the form of a solid powder.

(Assessment Methods)

Twenty cosmetic evaluation panels were made to use foundations in the form of solid powders, and each sample was evaluated in seven steps according to the following evaluation criteria for the items of "smooth spreadability" and "formation of a uniform makeup film". . About the rating given to every sample, the average score of the rating of all the panels was calculated | required, and it judged according to the following criteria.

 Evaluation standard: (evaluation) (Contents) 6 Very good 5  Good 4 Somewhat good 3 usually 2 Somewhat poor One Bad 0 Very bad

Criteria:  (Average score of the rating) (evaluation)  5.0 or more ◎ (very good)  3.5 or more and less than 5.0 ○ (good) 1.0 or more and less than 3.5 △ (normal)  Less than 1.0 X (bad)

As is apparent from the results of Table 1, the solid powder form (invention) prepared using the granulated silica of Example 1 was excellent in both the items of "smooth spreadability" and "formation of uniform makeup film". On the other hand, powder foundation (Comparative article 1) which did not mix granulated silica particle was inferior in both a smooth spreadability and a uniform cosmetic film. Moreover, the powder foundation (comparative product 2) which mix | blended the dry matter of the comparative example 1 was inferior in the smooth spreadability and the uniform cosmetic film. Moreover, also in the powder foundation (comparative example 3) which mix | blended the dry matter of the comparative example 2, it was inferior in a smooth spreadability and a uniform cosmetic film. This is presumed that the granulated silica particles of Comparative Example 2 have a lower silanol group density than the granulated silica particles of Example 1, so that the granulation is not effective.

Example  3

Face color in solid powder form

By the following components and the preparation method, a face color in the form of a solid powder was prepared.

(ingredient) (%) 1. Mica 2. Talc 3. Granulated silica particles of Example 1 4. Titanium oxide coated mica 5. Red 226 6. Ultramarine blue 7. Synthetic hydrocarbon wax powder 8. Methyl paraoxybenzoate 9. Squalane 10. Fragrance 20.0 remaining 10.0 10.0 0.5 0.2 5.0 0.2 1.0 proper amount

(Production method)

A. Components 1 to 8 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 9 and 10 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and subjected to compression molding to obtain a face color in the form of a solid powder.

The face color of the obtained solid powder form was excellent in both the items of "smooth spreadability" and "formation of uniform makeup film".

Example  4

Eyeshadow in solid powder form

By the following ingredients and preparation methods, eyeshadows in the form of a solid powder were prepared.

(ingredient) (%) 1. Dimethyl polysiloxane treated synthetic mica 2. Dimethyl polysiloxane treated talc 3. Titanium oxide coated mica 4. Boron nitride 5. Polyethylene terephthalate, aluminum, epoxy laminate 6. Granulated silica particles of Example 1 7 Ultramarine yellow No. 401 9. Crosslinked silicone and reticulated silicone copolymer 10. Methyl paraoxybenzoate 11. Liquid paraffin 12. Vaseline 13. Dimethyl polysiloxane 14. Fragrance 10.0 remaining 30.0 5.0 5.0 20.0 2.0 0.5 1.0 0.2 2.0 1.0 3.0 appropriate amount

(Production method)

A. The components 1 to 10 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Components 11-14 are heated and uniformly dispersed.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. D was filled into a metal container and compression molded to obtain an eye shadow in the form of a solid powder.

The obtained solid powder eyeshadow was excellent in both items of "smooth spreadability" and "formation of uniform makeup film".

Example  5

Foundation in solid powder form (for water use only)

By the following ingredients and preparation methods, eyeshadows in the form of a solid powder were prepared.

(ingredient) (%) 1. Talc 2. Mica 3. Titanium oxide coated mica 4. Titanium oxide 5. Boron nitride 6. Bengala 7. Iron sulfate 8. Iron black oxide 9. Granulated silica particles of Example 1 10. Methyl paraoxybenzoate 11. Purple Luoropolyether 12. Dimethyl polysiloxane 13. Oxybenzone 14. Polyoxyethylene (20 mol) sorbitan monooleate 15. Fragrance  Remaining amount 20.0 2.0 15.0 5.0 0.8 2. 5 0.3 15.0 0.2 2.0 5.0 3.0 0.5 Suitable amount

(Production method)

A. The components 1 to 10 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 11-15 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and compression molded to obtain a foundation (only for water use) in the form of a solid powder.

The obtained solid powder form foundation (for water use only) was excellent in both items of "smooth spreadability" and "formation of uniform makeup film".

Example  6

Oil cleansing

Oil cleansing was prepared by the following ingredients and production method.

(ingredient) (%) 1. Rice bran oil 2. Liquid paraffin 3. Tri-2-ethylhexanoic acid glyceryl 4. Methylphenylpolysiloxane 5. Tetraoleic acid POE (30) sorbet 6. Phenoxyethanol 7. Yulmu oil 8. Safflower oil 9. Natural Vitamin E 10. Fragrances 11. Granulated silica particles of Example 1 35.0 remaining 10.0 5.0 9.0 0.8 0.1 0.1 0.1 appropriate amount 1.0

(Production method)

A. Mix components 1 to 10 uniformly.

B. Oil cleansing was obtained by gradually adding component 11 to A and mixing uniformly.

The obtained oil cleansing was excellent in "smooth spreading property".

Example  7

Oil-in-water sunscreen

Water-in-oil sun cream was prepared by the following ingredients and production method.

(ingredient) (%) 1. Methyl trimethicone 2. Acrylic-silicone treated fine particle titanium oxide (Note 1) 3. PEG-9 polydimethylsiloxyethyl dimethicone (Note 2) 4. Dimethyl polysiloxane (Note 3) 5. 5. Trimethylsiloxysilicate / decamethylcyclopentasiloxane solution (Note 4) 6. Stearic acid inulin (Note 5) 7. Paramethoxy cinnamic acid octyl 8. Diethyl aminohydroxybenzoylhexyl benzoate 9. 2 -Ethylhexanoic acid cetyl 10. PEG-9 polydimethylsiloxyethyl dimethicone (Note 2) 11.ethanol 12. glycerine 13. sodium chloride 14. preservative 15. granulated silica particles of Example 1 16. fragrance 17. Purified Water  5.0 5.0 0.5 2.0 9.0 2.0 3.0 0.5 5.0 2.5 10.0 2.0 1.0 Moderate 2.0 Moderate Note 1: KF-549 (manufactured by Shin-Etsu Chemical Co., Ltd.) Treated particulate titanium oxide (average particle diameter 0.02 μm) Note 2: KF-6028 (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 3: KF96A-2cs (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 4: KF-7312J (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 5: Leopard ISK (product manufactured by Chiba)

(quite)

A: The components 1 to 3 are bead milled and uniformly dispersed.

B: The components 4-10 are heated and melt | dissolved at 70 degreeC, and the said A is added and mixed and dissolved uniformly.

C: The components 11-14 and 17 were mixed-dissolved.

D: It cools after emulsifying adding said C to said B.

E: The components 15 and 16 were added and mixed uniformly in said D, and the water-in-water sun cream was obtained.

The obtained water-in-oil type sun cream had no stickiness and was excellent in smooth spreadability.

Example  8

2nd floor lotion

The two-layer lotion was prepared by the following component and production method.

(ingredient) (%) 1. POE alkyl ether (8 moles) phosphoric acid 2. Purified water 3. Zinc oxide 4. Granulated silica of Example 1 5. Aluminum chloride 6. Purified water 7. Ethanol 8. Isostearic acid polyoxyethylene hydrogenated castor oil 9. Isopropylmethylphenol 10. Preservative 11. Ethanol 12. Sodium citrate 13. Purified water  0.1 2.5 0.1 0.5 0.4 Remaining 2.0 0.1 0.1 Suitable 18.0 0.5 10.0

(Production method)

A. Mix components 5 to 7 uniformly.

B. Components 1 to 4 are mixed and uniformly dispersed in A.

C. After mixing components 8-13, it mixed uniformly with B and the two-layer lotion was obtained.

The obtained two-layer lotion had a smooth texture and was excellent in smooth spreadability.

Example  9

Liquid cleaning agent

The liquid detergent was prepared by the following components and the production method.

(ingredient) (%) 1. Palm oil fatty acid triethanolamine 2. Palm oil fatty acid potassium 3. Palm oil fatty acid amidopropylbetaine 4. 2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazolinium betaine 5. Palm oil fatty acid diethanolamide 6. Monostearate Ethylene Glycol 7. Squalane 8. Xanthan Gum 9. Hydroxyethylcellulose 10. Cationic Cellulose 11. Granulated Silica of Example 1 12. Purified Water 13. Preservative 10.0 5.0 5.0 3.0 3.0 3.0 0.5 0.1 0.1 0.1 0.5 Remaining balance

(Production method)

A. After mixing components 6-8 uniformly at 70 degreeC, a part of component 12 is added and emulsified. Then, it cools to room temperature.

B. The balance of components 1 to 5 and 12 are mixed uniformly.

C. Add A to B and mix uniformly.

D. The components 9 and 10 are added to said C, and it mixes uniformly.

E. The components 11 and 13 were added to said D, it mixed uniformly, and the liquid face wash was obtained.

The obtained liquid face wash was a smooth texture, and was excellent in the smooth spreadability.

Example  10

Underwater Type Oil Painting Foundation

Underwater type emulsion foundation was prepared by the following component and preparation method.

(ingredient)  (%) 1. Stearic acid 2. Cetanol 3. Monooleic acid polyoxyethylene (20 moles) sorbitan 4. Sesquioleic acid sorbitan 5. 2-ethylhexanoate cetyl 6. Fluid paraffin 7. Granulated silica of Example 1 8 Glycerine 9. 1,3-butylene glycol 10. Alkyl-modified carboxyvinyl polymer 11. Alkyl acrylate copolymer 12. Triethanolamine 13. Preservative 14. Purified water 15. Fluorine compound treatment Titanium oxide 16. Fluorine compound Treatment Talc 17. Fluoride Compound Bengala 18. Fluoride Compound Iron Sulfate 19. Fluoride Compound Black Iron Oxide  0.5 1.0 0.8 0.4 5.0 5.0 3.0 3.0 5.0 0.1 1.0 0.5 Appropriate amount remaining 4.0 1.0 0.5 1.5 0.1

(Production method)

A: The components 1-3, components 5, 6 are added, and it heat-mixes uniformly at 75 degreeC.

B: The components 15-19 are mixed with components 4, 8, and 9, and it is disperse | distributed uniformly with three rollers.

C: The components 10-14 are added to said B, and it heat-mixes uniformly at 75 degreeC.

D: The said A is added to said C and emulsified.

E: After cooling said D, component 7 was added and the water type emulsion foundation was obtained.

The obtained oil-in-water emulsion foundation was excellent in the smooth spreadability and the uniformity of a makeup film with a soft touch.

Example  11

Non-aqueous mascara

A non-aqueous mascara was prepared by the following component and production method.

(ingredient) (%) 1. Rosin acid pentaerythritol 2. Candilia wax resin 3. Palmitate dextrin 4. Ceresin 5. Beeswax 6. Soybean phospholipid 7. Hard isoparaffin 8. Trimethylsiloxysilicate 9. Dimethyldiarylammonium Hectorite 10. Propylene carbonate 11. Light flowing isoparaffin 12. Fluorine-treated black iron oxide 13. Fluorine-treated talc 14. Granulated silica of Example 1 10.0 2.0 3.0 4.0 3.0 0.5 Remaining 2.0 3.0 1.0 30.0 5.0 10.0 2.0

(Production method)

A: The components 1-8 were melt | dissolved uniformly at 110 degreeC by heat.

B: Components 9 to 11 are uniformly dispersed to obtain an oily gel.

C: The said B is added to the said A, and it mixes uniformly.

D: The components 12 and 13 are added to said C, and it mixes uniformly.

E: The above D is treated with three rollers.

F: Component 14 is added to E and it mixes uniformly.

G: The said F was filled in the container, and the non-aqueous mascara was obtained.

The obtained non-aqueous mascara was excellent in quick-drying and uniformity of a makeup film.

Example  12

Preparation of glycerine-containing composite powder:

Dissolve 5.0 parts by mass of glycerine in 95 parts by mass of a 15% strength aqueous solvent colloidal suspension (Sun Lovely-LFS-C; manufactured by Asahigaras Co., Ltd.) of scaly silica having a silanol group density of 60 μmol / m 2. It was made to disperse | distribute uniformly in a permill and it was set as the slurry. The atomizer rotation speed was 30000 rpm, flow rate 50 ml / min, inlet temperature setting 200 degreeC, outlet temperature setting using the spray dryer (L-8 type | mold; product made by Okawara-Kakoki Co., Ltd.) which has a disk type atomizer as a spraying apparatus. It was spray dried at the conditions of 130-140 degreeC.

It was 14% when the glycerin content rate of the obtained composite powder was measured from the loss on ignition. Moreover, it was 1.0 Mpa when the compressive strength of the obtained composite powder was measured by the microcompression tester. Moreover, it was 18 micrometers when the average particle diameter of the composite powder was measured with the laser type dry particle size distribution analyzer. In addition, ignition loss was performed according to the ignition loss test method described in the quasi quasi-drug raw material standard.

Example  13

Preparation of 1,3-butylene glycol-containing composite powder:

5.4 parts by mass of 1,3-butylene glycol and 0.1 ascorbic acid dissolved therein in 94.5 parts by mass of a colloidal dispersion having a concentration of 60% mol / m 2 and having a scaly silica having a density of 60 μmol / m 2 in purified water. Mass parts were uniformly dispersed in a dispermill. This was spray-dried on the conditions of Example 12 using the spray dryer which has a disk type atomizer as a spraying apparatus.

The inclusion rate of the melt | dissolution of 1, 3- butylene glycol and ascorbic acid of the composite powder calculated | required from the loss of ignition of the obtained composite powder was 9.5%. Moreover, it was 18 micrometers when the average particle diameter of the composite powder was measured with the laser type dry particle size distribution analyzer (PRO7000S by Seishin Corporation).

Example  14

Preparation of glycerine-containing composite powder:

9.9 parts by mass of glycerine and phenylbenzimidazole sulfonic acid, which is a water-soluble absorbent dissolved in 90 parts by mass of a colloidal dispersion having a concentration of 60 μmol / m 2, and having a scaly silica of 60 μmol / m 2 dispersed in purified water. 0.1 parts by mass was uniformly dispersed in a disper mill. This was spray-dried on the conditions of Example 12 using the spray dryer which has a disk type atomizer as a spraying machine, and the composite powder was obtained.

The inclusion rate of the melt | dissolution of glycerine and phenyl benzimidazole sulfonic acid of the composite grain | particle calculated | required from the loss of ignition of the obtained composite powder was 22%. Moreover, it was 16 micrometers when the average particle diameter of the composite powder was measured with the laser type dry particle size distribution measuring apparatus (PRO7000S by Seishin Corporation).

Example  15

Preparation of Diglycerin Containing Composite Powder:

9.9 parts by mass of diglyserine and dipotassium diglyceride (dipotassium) dissolved in 90 parts by mass of a colloidal dispersion having a concentration of 60 μmol / m 2 and having a scaly silica having a density of 60 μmol / m 2 in purified water. 0.1 part by mass of glycyrrhizinate was uniformly dispersed in a dispermill. This was spray-dried on the conditions of Example 12 using the spray dryer which has a disk type atomizer as a spraying machine, and the composite powder was obtained.

The content rate of the melt | dissolution of the diglyserine and the dipotassium glycitrate dihydrate of the composite grain | particle calculated | required from the weight loss of the obtained composite powder was 20%. Moreover, it was 15 micrometers when the average particle diameter of the composite powder was measured with the laser type dry particle size distribution analyzer (PRO7000S by Seishin Corporation).

Comparative example  3

Preparation of Comparative Composite Powder:

5.0 parts by mass of glycerine were uniformly dispersed in a dispermill in 95 parts by mass of a 15% concentration of a colloidal dispersion in which spherical silica having a silanol group density of 8.0 μmol / m 2 and a particle diameter of 12 μm was dispersed in purified water. This was spray-dried on the conditions of Example 12 using the spray dryer which has a disk type atomizer as a spraying machine, and obtained composite powder.

The inclusion rate of glycerine of the composite powder obtained from the loss in ignition of the obtained composite powder was 6.0%. As a result of observing this comparative composite powder with a scanning electron microscope, it was found that only a part of 12 µm spherical particles existed as aggregated aggregates, and granulated particles were not formed as in the example.

In this way, when spherical silica having a silanol group density of 8.0 µmol / m 2 was used, the inclusion rate of glycerine could not be 6.0% or more. In the case where spherical silica having a particle diameter of 12 µm is used, granulated particles are not formed, and glycerin is adhered to the inner wall surface of the tubular body of the drying apparatus without inclusion, and thus the formed composite powder adheres to the glyce. This is because it was not able to recover the composite powder efficiently by coagulating with serine. Therefore, when the silanol group density was low, it turned out that a water-soluble component is not contained regardless of the shape of a silica.

Comparative example  4

Preparation of Comparative Composite Powder:

5.0 parts by mass of glycerine were uniformly dispersed in a dispermill in 95 parts by mass of 15% colloidal dispersion in which scaly-shaped silica having a silanol group density of 7.0 μmol / m 2 and a particle diameter of 25 μm was dispersed in purified water. This was spray-dried on the conditions of Example 12 using the spray dryer which has a disk type atomizer as a spraying machine, and obtained composite powder.

The glycerin content rate of the composite powder obtained from the loss in ignition of the obtained composite powder was 5.0%. As a result of observing this comparative composite powder with a scanning electron microscope, it was found that only a part of the scaly silica was present as an aggregated aggregate, and granulated particles were not formed as in the example.

As described above, when the scale-like silica having a silanol group density of 7.0 µmol / m 2 was used, the inclusion rate of glycerine could not be made 5.0% or more. This is because the glycerine is not contained in the scaly silica having a particle diameter of 25 µm and adheres to the inner wall surface of the tubular body of the drying apparatus, so that the formed composite powder aggregates with the attached glycerine. Therefore, when the silanol group density was low, it turned out that even if it is scaly-shaped, it is not nested.

Example  16

Foundation in solid powder form (dry use only):

By the composition shown in Table 2 and the following manufacturing method, the foundation (dry use only) of the solid powder form was prepared. About this solid powder foundation,

The "smooth spreadability", "adhesion to skin", and "moisture retention to skin" were evaluated by the evaluation method and judgment criteria shown below. These results are shown in Table 2 together.

(Furtherance)

(%)  ingredient invention Comparative product 2 3 4 5 4 5 6 One Siliconized Titanium Oxide 15.0 15.0 15.0 15.0 15.0 15.0 15.0 2 Siliconized Bengala 1.0 1.0 1.0 1.0 1.0 1.0 1.0 3 Siliconated Iron Sulfate 3.0 3.0 3.0 3.0 3.0 3.0 3.0 4 Silicon-treated black iron oxide 0.5 0.5 0.5 0.5 0.5 0.5 0.5 5 Composite powder of Example 12 10.0 - - - - - - 6 Composite powder of Example 13 - 10.0 - - - - - 7 Composite powder of Example 14 - - 10.0 - - - - 8 Composite powder of Example 15 - - - 10.0 - - - 9 Composite Powder of Comparative Example 3 - - - - - 10.0 - 10 Composite Powder of Comparative Example 4 - - - - - - 10.0 11 Silicon-treated synthetic mica 20.0 20.0 20.0 20.0 20.0 20.0 20.0 12 Silicon-treated Talc Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount 13 Nylon powder 3.0 3.0 3.0 3.0 3.0 3.0 3.0 14 Crosslinked Silicone / Reticulated Silicone Copolymer 5.0 5.0 5.0 5.0 5.0 5.0 5.0 15 Methyl Paraoxybenzoate 0.2 0.2 0.2 0.2 0.2 0.2 0.2 16 Floating paraffin 2.0 2.0 2.0 2.0 2.0 2.0 2.0 17 Dimethylpolysiloxane 2.0 2.0 2.0 2.0 2.0 2.0 2.0 18 Methoxycinnamic acid octyl 6.0 6.0 6.0 6.0 6.0 6.0 6.0 19 Spices 0.1 0.1 0.1 0.1 0.1 0.1 0.1 <Evaluation Item> Seamless spreadability ◎ ◎ ◎ ◎ × ○ ○ Adhesion to skin ◎ ◎ ◎ ◎ × × × Moisturizing to the skin ◎ ◎ ◎ ◎ × × ×

(Production method)

A. Components 1 to 14 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 15-19 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and subjected to compression molding to obtain a foundation (only for dry use) in the form of a solid powder.

(Assessment Methods)

20 panelists specialized in cosmetic evaluation were used in the form of solid powder of the present invention and the comparative product (for dry use only), and each of them had a feeling of "smooth spreading", "adhesion to skin" and "moisture to skin". According to the following evaluation criteria, 7 levels of evaluation were performed for every sample and the grade was given. Moreover, the average point of the rating of all the panels was calculated | required, and it judged according to the following criteria. In addition, about the "moisturizing feeling to skin", it was set as the comprehensive evaluation of the moisturizing feeling immediately after application | coating of each specialty panel, and the moisturizing feeling after performing general life for 3 hours after application | coating.

 Evaluation standard: (evaluation) (Contents) 6 Very good 5  Good 4 Somewhat good 3 usually 2 Somewhat poor One Bad 0 Very bad

Criteria:  (Average score of the rating) (evaluation)  5.0 or more ◎ (very good)  3.5 or more and less than 5.0 ○ (good) 1.0 or more and less than 3.5 △ (normal)  Less than 1.0 X (bad)

As is apparent from the results in Table 2, the foundation in the form of a solid powder of the inventions 2 to 5 was excellent in all items of "smooth spreadability", "adhesion to skin" and "moisture to skin".

On the other hand, the powder foundation of the comparative product 4 which does not mix | blend complex powder was inferior in both smooth spreadability, adhesiveness to skin, and the moisture retention to skin. Moreover, although the powder foundation of the comparative product 5 which mix | blended the composite powder of the comparative example 3 was excellent in the smooth spreadability, it was inferior in adhesiveness and moisture retention. Moreover, although the powder foundation of the comparative product 6 which mix | blended the composite powder of the comparative example 4 was excellent in the smooth spreadability, it was inferior in the adhesiveness to skin and the moisturizing feeling to skin.

Example  17

Face color in solid powder form:

By the following components and the preparation method, a face color in the form of a solid powder was prepared.

(ingredient) (%) 1. Mica 2. Talc 3. Composite powder of Example 13 4. Titanium oxide-coated mica 5. Red 226 6. Ultramarine blue 7. Synthetic hydrocarbon wax powder 8. Methyl paraoxybenzoate 9. Squalane 10. Fragrance 20.0 remaining 10.0 10.0 0.5 0.2 5.0 0.2 1.0 proper amount

(Production method)

A. Components 1 to 8 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 9 and 10 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and subjected to compression molding to obtain a face color in the form of a solid powder.

The face color of the obtained solid powder form was excellent in all items of "smooth spreadability", "adhesion to skin", and "moisture to skin".

Example  18

Eyeshadow in solid powder form:

By the following ingredients and preparation methods, eyeshadows in the form of a solid powder were prepared.

(ingredient) (%) 1. Dimethyl polysiloxane treated synthetic mica 2. Dimethyl polysiloxane treated talc 3. Titanium oxide coated mica 4. Boron nitride 5. Polyethylene terephthalate, aluminum, epoxy laminated powder 6. Composite powder of Example 14 7. Ultramarine blue 8. Yellow No. 401 9. Crosslinked silicone and reticulated silicone copolymer 10. Methyl paraoxybenzoic acid 11. Liquid paraffin 12. Vaseline 13. Dimethyl polysiloxane 14. Fragrance 10.0 remaining 30.0 5.0 5.0 20.0 2.0 0.5 1.0 0.2 2.0 1.0 3.0 appropriate amount

(Production method)

A. The components 1 to 10 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Components 11-14 are heated and uniformly dispersed.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. D was filled into a metal container and compression molded to obtain an eye shadow in the form of a solid powder.

The obtained solid powder eyeshadow was excellent in all items of "smooth spreadability", "adhesion to skin", and "moisture to skin".

Example  19

Foundation in solid powder form (for water use only):

The foundation (solid water only) was prepared in the form of a solid powder by the following ingredients and preparation method.

(ingredient) (%) 1. Talc 2. Mica 3. Titanium oxide coated mica 4. Titanium oxide 5. Boron nitride 6. Bengala 7. Iron sulfate 8. Iron black oxide 9. Composite powder of Example 15 10. Methyl paraoxybenzoate 11. Perfluoro Polyether 12. Dimethyl polysiloxane 13. Oxybenzone 14. Polyoxyethylene (20 moles) sorbitan monooleate 15. Fragrance  Remaining amount 20.0 2.0 15.0 5.0 0.8 2. 5 0.3 15.0 0.2 2.0 5.0 3.0 0.5 Suitable amount

(Production method)

A. The components 1 to 10 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 11-15 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and compression molded to obtain a foundation (only for water use) in the form of a solid powder.

The obtained solid powder form foundation (for water use only) was excellent in all items of "smooth spreadability", "adhesion to skin" and "moisture to skin".

Example  20

Oil cleansing

Oil cleansing was prepared by the following ingredients and production method.

(ingredient) (%) 1. Rice bran oil 2. Liquid paraffin 3. Tri-2-ethylhexanoic acid glyceryl 4. Methylphenylpolysiloxane 5. Tetraoleic acid POE (30) sorbet 6. Phenoxyethanol 7. Yulmu oil 8. Safflower oil 9. Natural Vitamin E 10. Fragrances 11. Composite powder of Example 12 35.0 remaining 10.0 5.0 9.0 0.8 0.1 0.1 0.1 appropriate amount 1.0

(Production method)

A. Mix components 1 to 10 uniformly.

B. Oil cleansing was obtained by gradually adding component 11 to A and mixing uniformly.

The obtained oil cleansing was excellent in "smooth spreading property", "mixability with contamination", and "moisture retention to skin". Moreover, when oil cleansing was prepared for the composite powder of Example 12 instead of the composite powder of Example 13 or 15, it was similarly excellent in "smooth spreadability", "mixability with contamination", and "moisture to skin".

Example  21

Oil-in-water sunscreen

Water-in-oil sun cream was prepared by the following ingredients and production method.

(ingredient) (%) 1. Methyl trimethicone 2. Acrylic-silicone treated fine particle titanium oxide (Note 1) 3. PEG-9 polydimethylsiloxyethyl dimethicone (Note 2) 4. Dimethyl polysiloxane (Note 3) 5. Tri Methyl siloxy silicic acid / decamethylcyclopentasiloxane solution (Note 4) 6. Stearic acid inulin (Note 5) 7. Paramethoxy cinnamic acid octyl 8. Diethyl aminohydroxybenzoylhexyl benzoate 9. 2-ethylhexanoic acid Cetyl 10. PEG-9 polydimethylsiloxyethyl dimethicone (Note 2) 11.ethanol 12. glycerine 13. sodium chloride 14. preservative 15. composite powder of Example 12 16. flavor 17. purified water  5.0 5.0 0.5 2.0 9.0 2.0 3.0 0.5 5.0 2.5 10.0 2.0 1.0 Moderate 2.0 Moderate Note 1: KF-549 (manufactured by Shin-Etsu Chemical Co., Ltd.) Treated particulate titanium oxide (average particle diameter 0.02 μm) Note 2: KF-6028 (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 3: KF96A-2cs (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 4: KF-7312J (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 5: Leopard ISK (product manufactured by Chiba)

(quite)

A: The components 1 to 3 are bead milled and uniformly dispersed.

B: The components 4-10 are heated and melt | dissolved at 70 degreeC, and the said A is added and mixed and dissolved uniformly.

C: The components 11-14 and 17 were mixed-dissolved.

D: It cools after emulsifying adding said C to said B.

E: The components 15 and 16 were added and mixed uniformly in said D, and the water-in-water sun cream was obtained.

The obtained water-in-oil type sun cream was excellent in "smooth spreadability", "adhesion to skin", and "moisture to skin". In addition, the water-in-oil type sun cream was prepared using the composite powder of Example 13 or 15 instead of the composite powder of Example 12, and was similarly excellent in "smooth spreadability", "adhesion to skin" and "moisture to skin". Was.

Example  22

2nd floor lotion

The two-layer lotion was prepared by the following component and production method.

(ingredient) (%) 1. POE alkyl ether (8 moles) phosphoric acid 2. Purified water 3. Zinc oxide 4. Composite powder of Example 12 5. Aluminum chloride 6. Purified water 7. Ethanol 8. Isostearic acid polyoxyethylene hydrogenated castor oil 9. Iso Propylmethylphenol 10. Preservatives 11. Ethanol 12. Sodium citrate 13. Purified water  0.1 2.5 0.1 0.5 0.4 Remaining 2.0 0.1 0.1 Suitable 18.0 0.5 10.0

(Production method)

A. Mix components 5 to 7 uniformly.

B. Components 1 to 4 are mixed and uniformly dispersed in A.

C. After mixing components 8-13, it mixed uniformly with B and the two-layer lotion was obtained.

The obtained two-layer lotion was excellent in "smooth spreadability", "adhesion to skin", and "moisture to skin". In addition, instead of the composite powder of Example 12, a two-layer lotion was prepared using the composite powder of Example 13 or 15, and was similarly excellent in "smooth spreadability", "adhesion to skin" and "moisture to skin". Was.

Example  23

Liquid cleaning agent

The liquid detergent was prepared by the following components and the production method.

(ingredient) (%) 1. Palm oil fatty acid triethanolamine 2. Palm oil fatty acid potassium 3. Palm oil fatty acid amidopropylbetaine 4. 2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazolinium betaine 5. Palm oil fatty acid diethanolamide 6. Monostearic acid ethylene glycol 7. Squalane 8. Xanthan gum 9. Hydroxyethylcellulose 10. Cationic cellulose 11. Composite powder of Example 12 12. Purified water 13. Preservative 10.0 5.0 5.0 3.0 3.0 3.0 0.5 0.1 0.1 0.1 0.5 Remaining balance

(Production method)

A. After mixing components 6-8 uniformly at 70 degreeC, a part of component 12 is added and emulsified. Then, it cools to room temperature.

B. The balance of components 1 to 5 and 12 are mixed uniformly.

C. Add A to B and mix uniformly.

D. The components 9 and 10 are added to said C, and it mixes uniformly.

E. The components 11 and 13 were added to said D, it mixed uniformly, and the liquid face wash was obtained.

The obtained liquid face wash was excellent in "smooth spreadability", "familiarity with contamination", and "moisture to skin". In addition, instead of the composite powder of Example 12, a liquid face wash was prepared using the composite powder of Example 13 or 15, and as a result, "smooth spreadability", "mixability with contamination", and "moisture to skin" It was excellent.

Example  24

Underwater Type Oil Painting Foundation

Underwater type emulsion foundation was prepared by the following component and preparation method.

(ingredient) (%) 1. Stearic acid 2. Cetanol 3. Monooleic acid polyoxyethylene (20 mol) sorbitan 4. Sesquioleic acid sorbitan 5. 2-ethylhexanoic acid cetyl 6. Fluid paraffin 7. Composite powder of Example 12 8. Glycerine 9. 1,3-butylene glycol 10. Alkyl-modified carboxyvinyl polymer 11. Alkyl acrylate copolymer 12. Triethanolamine 13. Preservative 14. Purified water 15. Fluorine compound treatment Titanium oxide 16. Fluorine compound treatment Talc 17. Fluorine treatment Bengala 18. Fluorine treatment Iron sulphate 19. Fluorine treatment Black iron oxide  0.5 1.0 0.8 0.4 5.0 5.0 3.0 3.0 5.0 0.1 1.0 0.5 Appropriate amount remaining 4.0 1.0 0.5 1.5 0.1

(Production method)

A: The components 1-3, components 5, 6 are added, and it heat-mixes uniformly at 75 degreeC.

B: The components 15-19 are mixed with components 4, 8, and 9, and it is disperse | distributed uniformly with three rollers.

C: The components 10-14 are added to component B, and it heat-mixes uniformly at 75 degreeC.

D: The said A is added to said C and emulsified.

E: After cooling said D, component 7 was added and the water type emulsion foundation was obtained.

The obtained underwater type emulsion foundation was excellent in "smooth spreadability", "adhesion to skin", and "moisture to skin". Moreover, when the composite powder of Example 12 prepared the water type emulsion foundation instead of the composite powder of Example 13 or 15, it was similarly excellent in "smooth spreadability", "adhesion to skin", and "moisture to skin". .

Example  25

Non-aqueous mascara

A non-aqueous mascara was prepared by the following component and production method.

(ingredient) (%) 1. Rosin acid pentaerythritol 2. Candilia wax resin 3. Palmitate dextrin 4. Ceresin 5. Beeswax 6. Soy phospholipid 7. Hard isoparaffin 8. Trimethylsiloxysilicate 9. Dimethyldiarylammonium Hectorite 10. Propylene carbonate 11. Light flow isoparaffin 12. Fluorine compound black iron oxide 13. Fluorine compound talc 14. Composite powder of Example 12 10.0 2.0 3.0 4.0 3.0 0.5 Remaining 2.0 3.0 1.0 30.0 5.0 10.0 2.0

(Production method)

A: The components 1-8 were melt | dissolved uniformly at 110 degreeC by heat.

B: Components 9 to 11 are uniformly dispersed to obtain an oily gel.

C: The said B is added to the said A, and it mixes uniformly.

D: The components 12 and 13 are added to said C, and it mixes uniformly.

E: The above D is treated with three rollers.

F: Component 14 is added to E and it mixes uniformly.

G: The said F was filled in the container, and the non-aqueous mascara was obtained.

The obtained non-aqueous mascara was excellent in "smooth spreadability", "adhesion to eyelashes", and "flexibility of eyelashes". In addition, instead of the composite powder of Example 12, a non-aqueous mascara was prepared using the composite powder of Example 13 or 15. Similarly, "smooth spreading", "adhesion to eyelashes" and "flexibility of eyelashes" were excellent. .

Example  26

Preparation of squalane-containing composite powder:

30 parts by mass of squalane in 70 parts by mass of a 15% concentration aqueous solvent colloidal suspension (sun Lovely-LFS-C; manufactured by Asahigarasu I-Tec Co., Ltd.) of scaly silica having a silanol group density of 60 μmol / m 2 in a dispermill It disperse | distributed and it was set as the slurry. This was used as a spray device using a spray dryer (L-8 type; manufactured by Okawara Kakoki Co., Ltd.) having a disc type atomizer, at which the atomizer rotation speed was 30000 rpm, the flow rate was 50 ml / min, the inlet temperature was set at 200 ° C, and the outlet temperature was set. It was spray dried at the conditions of 135-140 degreeC.

It was 62% when the squalane content of the obtained composite powder was measured from the loss on ignition. Moreover, it was 0.36 Mpa when the compressive strength of the obtained composite powder was measured by the microcompression tester. Moreover, it was 22 micrometers when the average particle diameter of the composite powder was measured with the laser type dry particle size distribution analyzer (PRO7000S by Seishin Corporation).

Example  27

Preparation of 2-ethylhexanoic acid glyceryl-containing composite powder:

29.8 parts by mass of 2-ethylhexanoic acid glyceryl and 70 parts by mass of 70% by mass of a colloidal dispersion having a concentration of 60 μmol / m 2 and having a scaly silica having a density of 60 μmol / m 2 in purified water. 0.1 parts by weight of vitamin E and 0.1 parts by weight of stearyl glycyric acid were dispersed in a dispermill. This was spray-dried on the conditions described in Example 26 using the spray drier which has a disk type atomizer as a spraying apparatus.

The 2-ethylhexanoic acid glyceryl inclusion rate of the composite powder obtained from the loss on ignition of the obtained composite powder was 71%. Moreover, it was 20 micrometers when the average particle diameter of the composite powder was measured with the laser type dry particle size distribution analyzer (PRO7000S by Seishin Corporation).

Example  28

Preparation of N-lauroyl-L-glutamic acid di (phytosteryl 2-octyldodecyl) inclusion composite powder:

N-lauroyl-L-glutamic acid di (phytosteryl 2-octyldode), which is a moisturizing agent, in 80 parts by mass of a colloidal dispersion having a concentration of 60 μmol / m 2 and having a scaly silica of 60 μmol / m 2 dispersed in purified water. 20 mass parts of yarns were dispersed in a disper mill. This was spray-dried on the conditions of Example 25 using the spray dryer which has a disk type atomizer as a spraying machine, and the composite powder was obtained.

The inclusion rate of N-lauroyl-L-glutamic acid di (phytosteryl 2-octyldodecyl) of the composite powder obtained from the loss in ignition of the obtained composite powder was 64%. Moreover, it was 27 micrometers when the average particle diameter of the composite powder was measured with the laser type dry particle size distribution analyzer (PRO7000S by Seishin Corporation).

Example  29

Preparation of paramethoxycinnamic acid 2-ethylhexyl inclusion composite powder:

10 parts by mass of 2-methoxyhexyl paramethoxycinnamic acid, an oil-soluble ultraviolet absorber, was dispersed in a dispermill in 90 parts by mass of a colloidal dispersion having a concentration of 60 μmol / m 2 and having a scaly silica of 60 μmol / m 2 dispersed in purified water. I was. This was spray-dried on the conditions of Example 26 using the spray dryer which has a disk type atomizer as a spraying machine, and the composite powder was obtained.

The inclusion rate of 2-ethylhexyl paramethoxycinnamate in the composite powder obtained from the loss in ignition of the obtained composite powder was 41%. Moreover, it was 19 micrometers when the average particle diameter of the composite powder was measured with the laser type dry particle size distribution analyzer (PRO7000S by Seishin Corporation).

Comparative example  5

Preparation of Comparative Composite Powder:

5.0 parts by mass of squalane was uniformly dispersed in a dispermill in 95 parts by mass of a 15% concentration colloidal dispersion in which spherical silica having a silanol group density of 8.0 μmol / m 2 and a particle diameter of 12 μm was dispersed in purified water. This was spray-dried on the conditions of Example 26 using the spray dryer which has a disk type atomizer as a spraying apparatus, and the composite powder was obtained.

The inclusion rate of squalane of the composite powder obtained from the loss in ignition of the obtained composite powder was 16%. As a result of observing this comparative composite powder with a scanning electron microscope, it was found that only a part of spherical particles existed as agglomerated aggregates, and granulated particles were not formed as in the example.

As described above, when spherical silica having a silanol group density of 8.0 μmol / m 2 was used, the inclusion rate of squalane could not be made 16% or more. When spherical silica having a particle diameter of 12 µm is used, granulated particles are not formed, and squalane adheres to the inner wall surface of the tubular body of the drying apparatus without inclusion, and the formed composite powder aggregates with the squalane to which the spherical silica is attached. This is because the composite powder could not be recovered efficiently. Therefore, when the silanol group density was low, it turned out that the inclusion rate of a water-insoluble component is low regardless of the shape of a silica.

Comparative example  6

Preparation of Comparative Composite Powder:

5.0 parts by mass of squalane were uniformly dispersed in a dispermill in 95 parts by mass of 15% colloidal dispersion in which scaly-shaped silica having a silanol group density of 7.0 μmol / m 2 and a particle diameter of 25 μm was dispersed in purified water. This was spray-dried on the conditions described in Example 26 using the spray drier which has a disk type atomizer as a spraying apparatus.

The squalane content of the composite powder obtained from the loss in ignition of the obtained composite powder was 14%. As a result of observing this comparative composite powder with a scanning electron microscope, it was found that only a part of the scaly silica was present as an aggregated aggregate, and granulated particles were not formed as in the example. Specifically, when the silanol group density was 7.0 µmol / m 2, the squalene content could not be 14% or more. This is because squalane is not completely contained in scaly silica having a particle diameter of 25 µm, but adheres to the inner wall surface of the tubular body of the drying apparatus, and the formed composite powder aggregates with the squalane to which it is attached, thereby efficiently recovering the composite powder. Because I could not. Therefore, when the silanol group density was low, it was found that the inclusion rate was low even in the shape of scales.

Example  30

Foundation in solid powder form (dry use only):

By the composition shown in Table 3 and the following manufacturing method, the foundation (dry use only) of the solid powder form was prepared. About the foundation of this solid powder form, about the "smooth spreading property", "adhesion to skin", "emollient feeling to skin", and "caking prevention effect" to the evaluation method and judgment criteria shown below Evaluated. These results are shown in Table 3 together.

(%)  ingredient invention Comparative product 6 7 8 9 7 8 9 10 One Siliconized Titanium Oxide 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 2 Siliconized Bengala 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 3 Siliconated Iron Sulfate 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 4 Silicon-treated black iron oxide 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 5 Composite Powder of Example 26 10.0 - - - - - - - 6 Composite Powder of Example 27 - 10.0 - - - - - - 7 Composite powder of Example 28 - - 10.0 - - - - - 8 Composite Powder of Example 29 - - - 10.0 - - - - 9 Composite powder of Comparative Example 5 - - - - - 10.0 - - 10 Composite Powder of Comparative Example 6 - - - - - - 10.0 10.0 11 Silicon-treated synthetic mica 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 12 Silicon-treated Talc Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount 13 Nylon powder 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 14 Crosslinked Silicone / Reticulated Silicone Copolymer 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 15 Methyl Paraoxybenzoate 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 16 Floating paraffin 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 17 Squalane 2.0 2.0 2.0 2.0 2.0 2.0 2.0 6.8 18 Methoxycinnamic acid octyl 6.0 6.0 6.0 6.0 6.0 6.0 6.0 6.0 19 Spices 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 <Evaluation Item> Seamless spreadability ◎ ◎ ◎ ◎ × ○ ○ △ Adhesion to skin ◎ ◎ ◎ ◎ × △ △ ○ A feeling of emollient to skin ◎ ◎ ◎ ◎ × × × △ Caking prevention effect ◎ ◎ ◎ ◎ ○ ○ ○ ×

(Production method)

A. Components 1 to 15 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 16-19 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and subjected to compression molding to obtain a foundation (only for dry use) in the form of a solid powder.

(Assessment Methods)

 For "smooth spreading", "adhesion to skin" and "emollient to skin", we use foundation (for dry use) of solid powder form of the above-mentioned this invention and comparative product for 20 cosmetic evaluation expert panels Each item was evaluated by seven steps for each sample according to the following evaluation criteria, and the rating was given. Moreover, the average point of the rating of all the panels was calculated | required, and it judged according to the following criteria. In addition, about the "emollient feeling to skin", it was set as the comprehensive evaluation of the emollient feeling immediately after application | coating of each specialty panel, and the emollient feeling after carrying out general life for 3 hours after application | coating.

 Evaluation standard: (evaluation) (Contents) 6 Very good 5  Good 4 Somewhat good 3 usually 2 Somewhat poor One Bad 0 Very bad

Criteria:  (Average score of the rating) (evaluation)  5.0 or more ◎ (very good)  3.5 or more and less than 5.0 ○ (good) 1.0 or more and less than 3.5 △ (normal)  Less than 1.0 X (bad)

"The anti-caking effect" prepares five powder foundations of the said Example and the comparative example, and is made into the metal container, and the surface is examined 80 times continuously using the powder foundation mat (material NBR). The surface state after (iii) was observed, the grade was given by the following evaluation criteria for every foundation, the average point of the grade for every sample was computed, and it judged by the following four steps of criteria.

 Evaluation standard: (evaluation) (Contents) 3 No change 2 Surface is shiny but no problem in usability One Significant surface shine and usability problems

Criteria:  (Average score of the rating) (evaluation)  2.5 or more ◎  2.0 or more and less than 2.5 ○ 1.5 or more and less than 2.0 △  Less than 1.5 ×

As is apparent from the results of Table 3, the solid powder form of the present inventions 6 to 9 has a "smooth spreadability", "adhesion to the skin", "emollient to the skin" and "caking prevention effect" It was excellent in all of the items.

On the other hand, the powder foundation of the comparative product 7 which does not mix | blend composite powder was inferior in the smooth spreadability, adhesiveness to skin, and the feeling of emollient to skin. Moreover, although the powder foundation of the comparative product 8 which mix | blended the composite powder of the comparative example 5 was excellent in the smooth spreadability, it was inferior in the adhesiveness to skin and the feeling of emollient to skin. Moreover, although the powder foundation of the comparative product 9 which mix | blended the composite powder of the comparative example 6 was excellent in the smooth spreadability, it was inferior in the adhesiveness to skin and the feeling of emollient to skin. This suggests that the inclusion rate of the water-insoluble component of the composite powders of Comparative Products 8 and 9 is small. Moreover, the caking produced the composite powder of the comparative example 6, and the comparative product 10 which mix | blended the water-insoluble substance so that it may be equivalent to this invention 6.

Example  31

Face color in solid powder form:

By the following components and the preparation method, a face color in the form of a solid powder was prepared.

(ingredient) (%) 1. Mica 2. Talc 3. Composite powder of Example 27 4. Titanium oxide coated mica 5. Red No. 226 6. Ultramarine blue 7. Synthetic hydrocarbon wax powder 8. Methyl paraoxybenzoate 9. Squalane 10. Fragrance 20.0 remaining 10.0 10.0 0.5 0.2 5.0 0.2 1.0 proper amount

(Production method)

A. Components 1 to 8 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 9 and 10 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and subjected to compression molding to obtain a face color in the form of a solid powder.

The obtained solid powder face color was excellent in all items of smooth spreadability, adhesion to skin, emollient feeling to the skin, and anti-caking effect.

Example  32

Eyeshadow in solid powder form:

By the following ingredients and preparation methods, eyeshadows in the form of a solid powder were prepared.

(ingredient) (%) 1. Dimethyl polysiloxane treated synthetic mica 2. Dimethyl polysiloxane treated talc 3. Titanium oxide coated mica 4. Boron nitride 5. Polyethylene terephthalate, aluminum, epoxy laminated powder 6. Composite powder of Example 28 7. Ultramarine blue 8. Yellow No. 401 9. Crosslinked silicone and reticulated silicone copolymer 10. Methyl paraoxybenzoic acid 11. Liquid paraffin 12. Vaseline 13. Dimethyl polysiloxane 14. Fragrance 10.0 remaining 30.0 5.0 5.0 20.0 2.0 0.5 1.0 0.2 2.0 1.0 3.0 appropriate amount

(Production method)

A. The components 1 to 10 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Components 11-14 are heated and uniformly dispersed.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. D was filled into a metal container and compression molded to obtain an eye shadow in the form of a solid powder.

The obtained solid powder eyeshadow was excellent in all items of smooth spreadability, adhesion to skin, emollient feeling to the skin, and anti-caking effect.

Example  33

Foundation in solid powder form (for water use only):

The foundation (solid water only) was prepared in the form of a solid powder by the following ingredients and preparation method.

(ingredient) (%) 1. Talc 2. Mica 3. Titanium oxide coated mica 4. Titanium oxide 5. Boron nitride 6. Bengala 7. Iron sulfate 8. Iron black oxide 9. Composite powder of Example 29 10. Methyl paraoxybenzoate 11. Perfluoro Polyether 12. Dimethyl polysiloxane 13. Oxybenzone 14. Polyoxyethylene (20 moles) sorbitan monooleate 15. Fragrance  Remaining amount 20.0 2.0 15.0 5.0 0.8 2. 5 0.3 15.0 0.2 2.0 5.0 3.0 0.5 Suitable amount

(Production method)

A. The components 1 to 10 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 11-15 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and compression molded to obtain a foundation (only for water use) in the form of a solid powder.

The obtained solid powder form foundation (for water use only) was excellent in all items of smooth spreadability, adhesion to skin, emollient feeling to the skin, and anti-caking effect.

Reference Example  One

Preparation of Emulsifying Compositions:

The emulsion composition was prepared by the following components and production method.

(ingredient) (%) 1. Phospholipid-cholesterol mixture ^{* 1} 2. 1,3-butylene glycol 3. Glycerin 4. Squalane 5. Purified water  2.0 10.0 10.0 10.0 68.0  * 1: COM POSITE-PC (manufactured by Japan Seika Co., Ltd.)

(Production method)

A. Components 1 to 3 are uniformly dispersed with a disper at 70 ° C.

B. Component 4 is added to A at 70 degreeC, and it mixes uniformly.

C. The component 5 was gradually added to B at 75 degreeC, and it emulsified in the disper, and obtained the emulsion composition.

Reference Example  2

Preparation of Emulsifying Compositions:

The emulsion composition was prepared by the following components and production method.

(ingredient) (%) 1. N-Stearoyl-N-methyltaurine Sodium 2. Glycerin 3. Purified water 4. 1,3-butylene glycol 5. Liquid paraffin 6. Vaseline 7. Cetostearyl alcohol 8. Monooleic acid poly Oxyethylene Sorbitan (20E.O.)  1.0 5.0 45.5 15.0 20.0 10.0 3.0 0.5

(Production method)

A. Components 1 to 3 are uniformly dispersed with a disper at 70 ° C.

B. Components 4 to 8 are uniformly dispersed at 70 ° C.

C. The said B was gradually added to said A at 75 degreeC, and it emulsified in the disper, and the emulsion composition was obtained.

Reference Example  3

Preparation of Emulsifying Compositions:

The emulsion composition was prepared by the following components and production method.

(ingredient) (%) 1. Stearic acid 2. Behenyl alcohol 3. Cetostearyl alcohol 4. 2-ethylhexyl paramethoxycinnamic acid 5. Tri-2-ethylhexanoic acid glyceryl 6. Purified water 7. Triethanolamine 8. 1,3 Butylene glycol 9.Dipropylene glycol  2.5 0.5 0.5 20.0 10.0 55.5 1.0 5.0 5.0

(Production method)

A. Components 1 to 5 are uniformly dispersed at 70 ° C.

B. Components 6-9 are uniformly dispersed at 70 ° C.

C. The said B was gradually added to said A at 75 degreeC, and it emulsified in the disper, and the emulsion composition was obtained.

Example  34

Preparation of Composite Powders:

60 mass parts of the emulsion composition obtained by the reference example 1 was added to 40 mass parts of 15% colloidal dispersions which disperse | distributed the scaly-shaped silica of 60 micromol / m <2> in silanol-group density in purified water, and it disperse | distributed uniformly in the dispermill. This was spray-dried on the conditions described in Example 26 using the spray drier which has a disk type atomizer as a spraying apparatus.

From the weight loss of the obtained composite powder, the inclusion rate of the emulsion composition of Reference Example 1 contained in this particle was 59%. Moreover, the average particle diameter of the composite powder was 20 micrometers by the laser type dry particle size distribution measuring apparatus (PRO7000S by Seishin Corporation). In addition, in the following example and a comparative example, a containment rate means the containment rate regarding the component except the aqueous component of 100 degrees C or less among the components which comprise an emulsion composition.

Example  35

Preparation of Composite Powders:

50 mass parts of the emulsion composition obtained by the reference example 2 was disperse | distributed in the dispermill to 50 mass parts of 15% colloidal dispersion which disperse | distributed the scale fragment silica of 60 micromol / m <2> in purified water. This was spray-dried on the conditions described in Example 26 using the spray drier which has a disk type atomizer as a spraying apparatus.

From the weight loss of the obtained composite powder, the inclusion rate of the emulsion composition of Reference Example 2 contained in this particle was 50%. Moreover, it was 0.30 Mpa when the compressive strength of the obtained composite powder was measured by the microcompression tester. In addition, the average particle diameter of the composite powder was 18 micrometers by the laser type dry particle size distribution analyzer (PRO7000S by Seishin Corporation).

Example  36

Preparation of Composite Powders:

40 parts by mass of the emulsion composition obtained in Reference Example 3 was uniformly dispersed in a dispermill in 60 parts by mass of 15% colloidal dispersion in which the scaly-like silica having a silanol group density of 60 µmol / m 2 was dispersed in purified water. This was spray-dried on the conditions described in Example 26 using the spray drier which has a disk type atomizer as a spraying apparatus.

From the weight loss of the obtained composite powder, the inclusion rate of the emulsion composition of Reference Example 3 contained in this particle was 43%. In addition, the average particle diameter of the composite powder was 19 micrometers by the laser type dry particle size distribution measuring apparatus (PRO7000S by Seishin Corporation).

Comparative example  7

Preparation of Comparative Composite Powder:

10 parts by mass of the emulsion composition of Reference Example 1 was uniformly dispersed in a dispermill to 90 parts by mass of a 15% concentration of a colloidal dispersion in which spherical silica having a silanol group density of 8.0 μmol / m 2 and a particle diameter of 12 μm was dispersed in purified water. . This was spray-dried on the conditions described in Example 26 using the spray drier which has a disk type atomizer as a spraying apparatus.

From the loss of ignition of the obtained composite powder, the inclusion rate of the emulsion composition of Reference Example 1 contained in the spherical silica particles was 8.0%. In addition, it was found that only a part of 12 µm spherical particles were aggregated by the laser type dry particle size distribution measuring device, but granulated particles were not formed as in the example. Specifically, when the silanol group density was 8.0 μmol / m 2, the inclusion rate of the emulsion composition of Reference Example 1 could not be set to 8.0% or more. This is because the emulsified composition of Reference Example 1 is not completely contained in the spherical silica having a particle diameter of 12 μm, but adheres to the inner wall surface of the tubular body of the drying apparatus, and the formed composite powder aggregates with the emulsified composition of Reference Example 1 to which it is attached. This is because the composite powder could not be recovered efficiently. Therefore, when the silanol group density was low, it was found that the inclusion rate was low regardless of the shape of the silica.

Comparative example  8

Preparation of Comparative Composite Powder:

10 parts by mass of the emulsion composition of Reference Example 1 was uniformly dispersed in a dispermill in 90 parts by mass of 15% colloidal dispersion in which scaly-shaped silica having a silanol group density of 7.0 μmol / m 2 and a particle diameter of 25 μm was dispersed in purified water. . This was spray-dried on the conditions described in Example 26 using the spray drier which has a disk type atomizer as a spraying apparatus.

From the loss of ignition of the obtained composite powder, the inclusion rate of the emulsion composition of Reference Example 1 contained in the powder was 7.0%. Further, it was found that only a part of 25 µm flake silica was aggregated by the laser type dry particle size distribution analyzer, but granulated particles were not formed as in the example. Specifically, when the silanol group density was 7.0 μmol / m 2, the inclusion rate of the emulsion composition of Reference Example 1 could not be made 7.0% or more. This is because the emulsified composition of Reference Example 1 is not completely contained in scaly silica having a particle diameter of 25 μm, but adheres to the inner wall surface of the tubular body of the drying apparatus, and the formed composite powder adheres to the emulsified composition of Reference Example 1 attached thereto. It is because it was not able to collect | recover the composite powder efficiently by being aggregated. Therefore, when the silanol group density was low, it was found that the inclusion rate was low even in the shape of scales.

Example  37

Foundation in solid powder form (dry use only):

By the composition shown in Table 4 and the following manufacturing method, the foundation (dry use only) of the solid powder form was prepared. About the foundation of this solid powder form, about the "smooth spreading property", "adhesiveness to skin", "emollient feeling to skin", and "caking prevention effect" to the evaluation methods and judgment criteria shown below Evaluated. These results are shown in Table 4 together.

(%)  ingredient invention Comparative product 10 11 12 13 11 12 13 14 One Siliconized Titanium Oxide 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 2 Siliconized Bengala 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 3 Siliconated Iron Sulfate 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 4 Silicon-treated black iron oxide 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 5 Composite Powder of Example 34 10.0 - - - - - - - 6 Composite powder of Example 35 - 10.0 - - - - - - 7 Composite powder of Example 36 - - 10.0 - - - - - 8 Composite Powder of Example 37 - - - 10.0 - - - - 9 Composite Powder of Comparative Example 7 - - - - - 10.0 - - 10 Composite Powder of Comparative Example 8 - - - - - - 10.0 10.0 11 Silicon-treated synthetic mica 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 12 Silicon-treated Talc Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount 13 Nylon powder 3.0 3.0 3.0 3.0 3.0 3.0 3.0 3.0 14 Crosslinked Silicone / Reticulated Silicone Copolymer 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 15 Methyl Paraoxybenzoate 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 16 Floating paraffin 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 17 Dimethylpolysiloxane 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 18 Methoxycinnamic acid octyl 6.0 6.0 6.0 6.0 6.0 6.0 6.0 6.0 19 Phospholipids and Cholesterol Mixtures 0.325 20 1,3-butylene glycol 1.625 21 Squalane 1.625 22 Methoxycinnamic acid octyl 1.625 23 Spices 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 <Evaluation Item> Seamless spreadability ◎ ◎ ◎ ◎ × ○ ○ △ Adhesion to skin ◎ ◎ ◎ ◎ × △ △ ○ A feeling of emollient to skin ◎ ◎ ◎ ◎ × × × △ Caking prevention effect ◎ ◎ ◎ ◎ ○ ○ ○ ×

(Production method)

A. Components 1 to 15 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 16-23 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and subjected to compression molding to obtain a foundation (only for dry use) in the form of a solid powder.

(Assessment Methods)

In the same manner as in Example 30, the present invention and the comparative product were used in the form of a solid powder form (for dry use only), such as "smooth spreadability", "adhesion to skin", "feeling emollient to skin" and The "caking prevention effect" was evaluated.

As is apparent from the results of Table 4, the solid powder form foundations of the present inventions 10 to 13 were excellent in all items of smooth spreading, adhesion to skin, emollient to the skin, and anti-caking effect.

On the other hand, the powder foundation of the comparative product 11 which does not mix | blend complex powder was inferior in all of the smooth spreadability, adhesiveness to skin, and the feeling of emollient to skin. Moreover, although the powder foundation of the comparative product 12 which mix | blended the composite powder of the comparative example 7 was excellent in the smooth spreadability, it was inferior in the adhesiveness to skin and the feeling of emollient to skin. Moreover, although the powder foundation of the comparative product 13 which mix | blended the composite powder of the comparative example 8 was excellent in the smooth spreadability, it was inferior in adhesiveness and a feeling of emollient. This suggests that the inclusion rate of the water-insoluble component of the composite powder of Comparative Examples 7 and 8 is small. Moreover, the caking produced the composite powder of the comparative example 8, and the comparative product 14 which mix | blended the water-insoluble substance so that it may be equivalent to this invention 10.

Example  38

Face color in solid powder form:

By the following components and the preparation method, a face color in the form of a solid powder was prepared.

(ingredient) (%) 1. Mica 2. Talc 3. Composite powder of Example 35 4. Titanium oxide-coated mica 5. Red 226 6. Ultramarine blue 7. Synthetic hydrocarbon wax powder 8. Methyl paraoxybenzoate 9. Squalane 10. Fragrance 20.0 remaining 10.0 10.0 0.5 0.2 5.0 0.2 1.0 proper amount

(Production method)

A. Components 1 to 8 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 9 and 10 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and subjected to compression molding to obtain a face color in the form of a solid powder.

The obtained solid powder face color was excellent in all items of smooth spreadability, adhesion to skin, emollient feeling to the skin, and anti-caking effect.

Example  39

Eyeshadow in solid powder form:

By the following ingredients and preparation methods, eyeshadows in the form of a solid powder were prepared.

(ingredient) (%) 1. Dimethyl polysiloxane treated synthetic mica 2. Dimethyl polysiloxane treated talc 3. Titanium oxide coated mica 4. Boron nitride 5. Polyethylene terephthalate, aluminum, epoxy laminate 6. Composite powder of Example 36 7. Ultramarine blue 8. Yellow No. 401 9. Crosslinked silicone and reticulated silicone copolymer 10. Methyl paraoxybenzoic acid 11. Liquid paraffin 12. Vaseline 13. Dimethyl polysiloxane 14. Fragrance 10.0 remaining 30.0 5.0 5.0 20.0 2.0 0.5 1.0 0.2 2.0 1.0 3.0 appropriate amount

(Production method)

A. The components 1 to 10 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Components 11-14 are heated and uniformly dispersed.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. D was filled into a metal container and compression molded to obtain an eye shadow in the form of a solid powder.

The obtained solid powder eyeshadow was excellent in all items of smooth spreadability, adhesion to skin, emollient feeling to the skin, and anti-caking effect.

Example  40

Foundation in solid powder form (for water use only):

The foundation (solid water only) was prepared in the form of a solid powder by the following ingredients and preparation method.

(ingredient) (%) 1. Talc 2. Mica 3. Titanium oxide coated mica 4. Titanium oxide 5. Boron nitride 6. Bengala 7. Iron sulfate 8. Iron black oxide 9. Composite powder of Example 37 10. Methyl paraoxybenzoate 11. Perfluoro Polyether 12. Dimethyl polysiloxane 13. Oxybenzone 14. Polyoxyethylene (20 moles) sorbitan monooleate 15. Fragrance  Balance 20.0 2.0 15.0 5.0 0.8 2.5 0.3 15.0 0.2 2.0 5.0 3.0 0.5 Appropriate amount

(Production method)

A. The components 1 to 10 are uniformly dispersed in a Henschel mixer (manufactured by Mitsui Miike).

B. Mix components 11-15 uniformly.

C. While A is stirred in a Henschel mixer, B is added and dispersed uniformly.

D. C is ground in the mill.

E. The above D was filled into a metal container and compression molded to obtain a foundation (only for water use) in the form of a solid powder.

The obtained solid powder form foundation (for water use only) was excellent in all items of smooth spreadability, adhesion to skin, emollient feeling to the skin, and anti-caking effect.

Example  41

Oil cleansing

Oil cleansing was prepared by the following ingredients and production method.

(ingredient) (%) 1. Rice bran oil 2. Liquid paraffin 3. Tri-2-ethylhexanoic acid glyceryl 4. Methylphenylpolysiloxane 5. Tetraoleic acid POE (30) sorbet 6. Phenoxyethanol 7. Yulmu oil 8. Safflower oil 9. Natural Vitamin E 10. Fragrances 11. Composite powder of Example 26 35.0 remaining 10.0 5.0 9.0 0.8 0.1 0.1 0.1 appropriate amount 1.0

(Production method)

A. Mix components 1 to 10 uniformly.

B. Oil cleansing was obtained by gradually adding component 11 to A and mixing uniformly.

The obtained oil cleansing was excellent in "smooth spreadability", "mixability with contamination", and "feeling emollient to skin". Further, instead of the composite powder of Example 26, oil cleansing was prepared using the composite powder of Examples 27, 28, 34, 35, or 36. Similarly, "smooth spreadability", "mixability with contamination", and "skin A feeling of emollient to "was excellent.

Example  42

Oil-in-water sunscreen

Water-in-oil sun cream was prepared by the following ingredients and production method.

(ingredient) (%) 1. Methyl trimethicone 2. Acrylic-silicone treated fine particle titanium oxide (Note 1) 3. PEG-9 polydimethylsiloxyethyl dimethicone (Note 2) 4. Dimethyl polysiloxane (Note 3) 5. Tri Methyl siloxy silicic acid / decamethylcyclopentasiloxane solution (Note 4) 6. Stearic acid inulin (Note 5) 7. Paramethoxy cinnamic acid octyl 8. Diethyl aminohydroxybenzoylhexyl benzoate 9. 2-ethylhexanoic acid Cetyl 10. PEG-9 polydimethylsiloxyethyl dimethicone (Note 2) 11.ethanol 12. glycerine 13. sodium chloride 14. preservative 15. composite powder of Example 26 16. flavor 17. purified water  5.0 5.0 0.5 2.0 9.0 2.0 3.0 0.5 5.0 2.5 10.0 2.0 1.0 Moderate 2.0 Moderate Note 1: KF-549 (manufactured by Shin-Etsu Chemical Co., Ltd.) Treated particulate titanium oxide (average particle diameter 0.02 μm) Note 2: KF-6028 (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 3: KF96A-2cs (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 4: KF-7312J (manufactured by Shin-Etsu Chemical Co., Ltd.) Note 5: Leopard ISK (product manufactured by Chiba)

(quite)

A: The components 1 to 3 are bead milled and uniformly dispersed.

B: The components 4-10 are heated and melt | dissolved at 70 degreeC, and the said A is added and mixed and dissolved uniformly.

C: The components 11-14 and 17 were mixed-dissolved.

D: It cools after emulsifying adding said C to said B.

E: The components 15 and 16 were added and mixed uniformly in said D, and the water-in-water sun cream was obtained.

The obtained water-in-oil type sun cream was excellent in "smooth spreadability", "adhesion to skin" and "feeling emollient to skin". In addition, the water-in-oil type sun cream was prepared using the composite powder of Examples 27, 28, 29, 34, 35, or 36 instead of the composite powder of Example 26. Similarly, "smooth spreadability" and "adhesion to skin" were prepared. And "the feeling of emollient to skin" was excellent. In particular, using the composite powder of Examples 29 and 36 was a long lasting sunscreen effect, less stickiness.

Example  43

2nd floor lotion

The two-layer lotion was prepared by the following component and production method.

(ingredient) (%) 1. POE alkyl ether (8 moles) phosphoric acid 2. Purified water 3. Zinc oxide 4. Composite powder of Example 26 5. Aluminum chloride 6. Purified water 7. Ethanol 8. Isostearic acid polyoxyethylene hydrogenated castor oil 9. Iso Propylmethylphenol 10. Preservatives 11. Ethanol 12. Sodium citrate 13. Purified water  0.1 2.5 0.1 0.5 0.4 Remaining 2.0 0.1 0.1 Suitable 18.0 0.5 10.0

(Production method)

A. Mix components 5 to 7 uniformly.

B. Components 1 to 4 are mixed and uniformly dispersed in A.

C. After mixing components 8-13, it mixed uniformly with B and the two-layer lotion was obtained.

The obtained two-layer lotion was excellent in "smooth spreadability", "adhesion to skin", and "emollient feeling to skin". In addition, instead of the composite powder of Example 26, a two-layer lotion was prepared using the composite powder of Examples 27, 28, 29, 34, 35, or 36. Similarly, "smooth spreadability", "adhesion to skin", and "The feeling of emollient to skin" was superior.

Example  44

Liquid cleaning agent

The liquid detergent was prepared by the following components and the production method.

(ingredient) (%) 1. Palm oil fatty acid triethanolamine 2. Palm oil fatty acid potassium 3. Palm oil fatty acid amidopropylbetaine 4. 2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazolinium betaine 5. Palm oil fatty acid diethanolamide 6. Monostearic Acid Ethylene Glycol 7. Squalane 8. Xanthan Gum 9. Hydroxyethylcellulose 10. Cationic Cellulose 11. Composite Powder of Example 26 12. Purified Water 13. Preservative 10.0 5.0 5.0 3.0 3.0 3.0 0.5 0.1 0.1 0.1 0.5 Remaining balance

(Production method)

A. After mixing components 6-8 uniformly at 70 degreeC, a part of component 12 is added and emulsified. Then, it cools to room temperature.

B. The balance of components 1 to 5 and 12 are mixed uniformly.

C. Add A to B and mix uniformly.

D. The components 9 and 10 are added to said C, and it mixes uniformly.

E. The components 11 and 13 were added to said D, it mixed uniformly, and the liquid face wash was obtained.

The obtained liquid face wash was excellent in "smooth spreadability", "mixability with contamination", and "emollient feeling to skin". Further, instead of the composite powder of Example 26, liquid face wash was prepared using the composite powder of Examples 27, 28, 34, 35, or 36. Similarly, "smooth spreadability", "mixability with contamination", and " A feeling of emollient to skin "was superior.

Example  45

Underwater Type Oil Painting Foundation

Underwater type emulsion foundation was prepared by the following component and preparation method.

(ingredient) (%) 1. Stearic acid 2. Cetanol 3. Monooleic acid polyoxyethylene (20 moles) sorbitan 4. Sesquioleic acid sorbitan 5. 2-ethylhexanoate cetyl 6. Fluid paraffin 7. Composite powder of Example 26 8. Glycerine 9. 1,3-butylene glycol 10. Alkyl-modified carboxyvinyl polymer 11. Alkyl acrylate copolymer 12. Triethanolamine 13. Preservative 14. Purified water 15. Fluorine compound treatment Titanium oxide 16. Fluorine compound treatment Talc 17. Fluorine treatment Bengala 18. Fluorine treatment Iron sulphate 19. Fluorine treatment Black iron oxide  0.5 1.0 0.8 0.4 5.0 5.0 3.0 3.0 5.0 0.1 1.0 0.5 Appropriate amount remaining 4.0 1.0 0.5 1.5 0.1

(Production method)

A: The components 1-3, components 5, 6 are added, and it heat-mixes uniformly at 75 degreeC.

B: The components 15-19 are mixed with components 4, 8, and 9, and it is disperse | distributed uniformly with three rollers.

C: The components 10-14 are added to said B, and it heat-mixes uniformly at 75 degreeC.

D: The A is added to C and emulsified.

E: After cooling said D, component 7 was added and the water type emulsion foundation was obtained.

The obtained underwater type emulsion foundation was excellent in "smooth spreadability", "adhesion to skin", and "emollient feeling to skin". In addition, instead of the composite powder of Example 26, an underwater type emulsion foundation was prepared using the composite powder of Examples 27, 28, 29, 34, 35, or 36. Similarly, "smooth spreadability" and "adhesion to skin" were prepared. And "the feeling of emollient to skin" was excellent.

Example  46

Non-aqueous mascara

A non-aqueous mascara was prepared by the following component and production method.

(ingredient) (%) 1. Rosin acid pentaerythritol 2. Candilia wax resin 3. Palmitate dextrin 4. Ceresin 5. Beeswax 6. Soy phospholipid 7. Hard isoparaffin 8. Trimethylsiloxysilicate 9. Dimethyldiarylammonium Hectorite 10. Propylene carbonate 11. Light flow isoparaffin 12. Fluorine compound black iron oxide 13. Fluorine compound talc 14. Composite powder of Example 26 10.0 2.0 3.0 4.0 3.0 0.5 Remaining 2.0 3.0 1.0 30.0 5.0 10.0 2.0

(Production method)

A: The components 1-8 were melt | dissolved uniformly at 110 degreeC by heat.

B: Components 9 to 11 are uniformly dispersed to obtain an oily gel.

C: The said B is added to the said A, and it mixes uniformly.

D: The components 12 and 13 are added to said C, and it mixes uniformly.

E: The above D is treated with three rollers.

F: Component 14 is added to E and it mixes uniformly.

G: The said F was filled in the container, and the non-aqueous mascara was obtained.

The obtained non-aqueous mascara was excellent in "smooth spreadability", "adhesion to eyelashes", and "flexibility of eyelashes". Furthermore, instead of the composite powder of Example 26, a non-aqueous mascara was prepared using the composite powder of Examples 27, 28, 29, 34, 35, or 36. Similarly, "smooth spreadability", "adhesion to eyelashes", and "The flexibility of the eyelashes" was excellent.

The granulated silica particles of the first invention of the present invention have a stable shape when manufactured without using a high molecular compound. When applied onto the skin, the granulated silica particles gradually collapse due to physical friction and have good malleability. It is suitable as a powder component mix | blended with cosmetics, external preparations, etc.

Moreover, the composite powder of 2nd invention in this invention contains water-soluble component stably and in large quantities, without using a binder component. Therefore, when it is blended in cosmetics, when it is applied on the skin, it gradually disintegrates due to physical friction and releases a large amount of the active ingredient, so that a high cosmetic effect can be expected.

Moreover, this composite powder itself is mix | blended with cosmetics, the malleability at the time of apply | coating to skin is excellent, it is excellent in adhesiveness and moisture retention, and it becomes an excellent cosmetics.

Moreover, the composite powder of 3rd invention of this invention contains the water-insoluble component stably and in large quantities, without using a binder component. Therefore, when this is blended into the cosmetic, it is gradually disintegrated due to physical friction when applied on the skin, and a large amount of the active ingredient is released, so that a high cosmetic effect can be expected.

Moreover, this composite powder itself is mix | blended with cosmetics, the malleability at the time of apply | coating to skin is excellent, and it is excellent in adhesiveness, an emollient feeling, and an anti-caking effect, and becomes an excellent cosmetics.

For example, in the case of face powder, in order to express an emollient feeling, it is generally necessary to mix | blend a large amount of oils, but in that case, since aggregation of the particle by liquid crosslinking force occurs, stable compounding can be performed. There was no. On the other hand, when using the composite powder of this invention, it becomes possible to provide a high emollient feeling, preventing particle aggregation.

In addition, in the case of the two-layered lotion containing the powder phase and the aqueous phase, in the conventional products, the dispersibility of the powder is poor, and caking (no dispersion reversibility occurs even when deposited on the bottom and vibrates) may occur. In order to eliminate this, it is necessary to mix | blend an active agent normally. However, in the present invention, the composite powder can be blended without blending the active agent, and furthermore, it can be stably maintained, so that it is possible to alleviate the problem of irritation to the skin due to the active agent blend.

Claims (26)

The average particle diameter is 1-50 micrometers, Comprising: 1-50 micrometers of thickness of a primary particle, 0.001-0.1 micrometer, and the silanol group (SiOH) per specific surface area of 20-70 micromol / m <2> as a component. Granulated silica particles having a value of 1 to 4 MPa. The granulated silica particle of Claim 1 whose average secondary particle diameter of the said scale-shaped silica is 0.05-5 micrometers, and the aspect ratio of the thickness and the longest particle diameter is 10 or more. The scale-like silica according to claim 1 or 2, wherein the primary particles have a thickness of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of 20 to 70 µmol / m 2, which is dispersed in an aqueous solvent and slurried. And granulated silica particles obtained by spray drying this with a spray dryer. The flaky silica having a thickness of the primary particles of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of 20 to 70 mol / m 2 is dispersed in an aqueous solvent, slurryed, and then spray dried with a spray dryer. Method for producing granulated silica particles, characterized in that. Cosmetics containing the granulated silica particle of any one of Claims 1-3. The water-soluble component is contained in the granulated silica particles formed from the scaly silica having a thickness of 0.001 to 0.1 µm and primary silanol groups (SiOH) per specific surface area of 20 to 70 mol / m 2. Composite powder. The composite powder according to claim 6, wherein the average secondary particle diameter of the flaky silica is 0.05 to 5 µm, and the aspect ratio between the thickness and the longest particle diameter is 10 or more. The composite powder according to claim 6 or 7, wherein the average particle diameter is in the range of 1 to 50 µm. The composite powder according to any one of claims 6 to 8, wherein the compressive strength is in the range of 0.2 to 3 MPa. The composite powder according to any one of claims 6 to 9, wherein the composite powder contains 5 to 25% of water-soluble components. The composite powder according to any one of claims 6 to 10, wherein the water-soluble component is a polyhydric alcohol. The scale-shaped silica according to any one of claims 6 to 11, wherein the primary particles have a thickness of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of 20 to 70 µmol / m 2. The composite powder obtained by making it disperse | distribute in aqueous solvent to contain and slurry, and spray-drying this with a spray dryer. The particle size silica having a thickness of 0.001 to 0.1 µm of primary particles and a silanol group (SiOH) per specific surface area of 20 to 70 mol / m 2 is dispersed and slurryed in an aqueous solvent containing a water-soluble component, followed by spraying it. Spray drying with a dryer, The manufacturing method of the composite powder characterized by the above-mentioned. Cosmetics containing the composite powder of any one of Claims 6-12. The water-insoluble component is contained in the granulated silica particles formed from the flake silica having a thickness of 0.001 to 0.1 탆 and primary silanol groups (SiOH) per specific surface area of 20 to 70 mol / m 2. Composite powder. The composite powder according to claim 15, wherein the average secondary particle diameter of the flaky silica is 0.05 to 5 µm, and the aspect ratio between the thickness and the longest particle diameter is 10 or more. The composite powder according to claim 15 or 16, wherein the average particle diameter is in the range of 1 to 50 µm. The composite powder according to any one of claims 15 to 17, wherein the compressive strength is in the range of 0.1 to 3 MPa. The composite powder according to any one of claims 15 to 18, wherein the composite powder contains 5 to 75% of a water insoluble component. The water-insoluble component according to any one of claims 15 to 19, wherein the flaky silica having a thickness of the primary particles is 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area is 20 to 70 µmol / m 2. The composite powder obtained by adding in an aqueous solvent to disperse | distribute and making it slurry, and spray-drying this with a spray dryer. The composite powder according to any one of claims 15 to 20, wherein the water insoluble component is an oily component. The water-insoluble component according to any one of claims 15 to 21, wherein the flaky silica having a thickness of the primary particles is 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area is 20 to 70 mol / m 2. The composite powder obtained by adding in an aqueous solvent to disperse | distribute as an emulsion composition, making it slurry, and spray-drying this with a spray dryer. Scale-shaped silica having a thickness of the primary particles of 0.001 to 0.1 µm and a silanol group (SiOH) per specific surface area of 20 to 70 µmol / m 2 is added to an aqueous solvent in which a water-insoluble component is dispersed, and then slurryed. Spray drying with a dryer, The manufacturing method of the composite powder. The method for producing a composite powder according to claim 23, wherein the water insoluble component is an oily component. Slurky silica having a thickness of 0.001 to 0.1 탆 and primary silanol groups (SiOH) per specific surface area of 20 to 70 mol / m 2 was added to an aqueous solvent in which the water-insoluble component was dispersed as an emulsion composition, and then slurried. Then, this is spray-dried by a spray dryer, The manufacturing method of the composite powder characterized by the above-mentioned. Cosmetics containing the composite powder in any one of Claims 15-22.

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