CN101652320A - Granulated silica particle, composite powder, their production methods, and cosmetic preparation containing them - Google Patents

Granulated silica particle, composite powder, their production methods, and cosmetic preparation containing them Download PDF

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CN101652320A
CN101652320A CN200880011022A CN200880011022A CN101652320A CN 101652320 A CN101652320 A CN 101652320A CN 200880011022 A CN200880011022 A CN 200880011022A CN 200880011022 A CN200880011022 A CN 200880011022A CN 101652320 A CN101652320 A CN 101652320A
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dioxide
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CN101652320B (en
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增渕祐二
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Kose Corp
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • A—HUMAN NECESSITIES
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/12—Face or body powders for grooming, adorning or absorbing
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/413—Nanosized, i.e. having sizes below 100 nm

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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 [mu]m and a silanol group (SiOH) per unit specific surface area of 20-70 [mu]mol/m<2>. This granulated silica particle has anaverage particle diameter of 1-50 [mu]m, and a compressive strength of 1-4 MPa.

Description

Granulated silica particle, composite powder and their preparation method and the makeup that contain them
Technical field
The present invention relates to granulated silica particle and in this granulated silica particle in the composite particles that forms of packetize effective constituent, more particularly, relate to and use the granulated silica particle utilize flakey silicon-dioxide and the firm laminated film that forms by the bonding between the silanol group of this silicon dioxide granule, be surrounded by the composite powder of imitating composition in stably with ad hoc structure.
Background technology
In the past, reported the use spray-drier, with granulation between the various powder particles, the synthetic particle (patent documentation 1) that is suitable for cosmetic use.
The slaking of among the preparation method with above-mentioned patent documentation 1 particle that granulation between the powder particle is formed that is representative, utilize usually, hydrous water soluble macromolecular or hydrophobic polymer being adjusted particle is not easy disintegration with particle when the particle preparation.
But if use macromolecular compound to carry out granulation, then owing to high molecular stringiness, the shape of the granulation particle after the spraying drying forms the shape of distortion, and when the particle with granulation was engaged in the makeup, to the poor ductility of skin, usability might be poor.In addition, because high molecular cooperation, the usability of the granulation particle that obtains produces rough sense or the sense of being clamminess, can not be satisfactory.
In addition, contain various organic compositions in the powder particle and carried out various trials making.The for example known water swellable clays mineral that utilize make the interlayer of this clay mineral contain the technology (patent documentation 3～6) of effective constituent.Further, there is report to point out to use spray-drier,, obtains containing the composite powder of effective constituent the tackiness agent as powder or powder such as water-soluble polymer, hydrophobic polymer or resin.
But, imitate the interior bag thing that composition forms by the composite powder that these technology obtain in the interlayer of clay mineral, being surrounded by, but have the few problem of maintenance dose of effective constituent.
Therefore, in order to improve the stability or the interior bag rate of composite powder, consider to increase the use level of above-mentioned tackiness agent, the mobile variation when but exist spraying this moment, can not stably spray by nozzle, or because high molecular stringiness, the shape of the composite powder that forms after the spraying drying forms the problem of the shape of distortion.
Therefore, when containing formed composite powder in the makeup, to the poor ductility of skin, usability might be poor.In addition, there is the trend of the usability reduction that makes resulting composite powder in the cooperation of tackiness agent itself, exists in and produces rough sense when makeup use or the problem of the sense of being clamminess, can not be satisfactory.
Patent documentation 1: Japanese kokai publication hei 05-201830 communique
Patent documentation 2: TOHKEMY 2001-163613 communique
Patent documentation 3: Japanese kokai publication sho 63-30313 communique
Patent documentation 4: Japanese kokai publication sho 63-50311 communique
Patent documentation 5: Japanese kokai publication hei 1-47706 communique
Patent documentation 6: Japanese kokai publication hei 1-47711 communique
Summary of the invention
Therefore, requirement the technical scheme of the granulation particle that does not use macromolecular compound to prepare particularly to give excellent usability when being used for skin is provided and can stablize and in large quantities in be surrounded by the composite powder of imitating composition, the object of the present invention is to provide this technology.
In view of the above problems, the inventor furthers investigate in order to address the above problem, found that, by selecting specific particle diameter, the flakey silicon-dioxide of silanol group density is as raw material, after being dispersed in it in aqueous solvent, carry out spraying drying, thus need not hydrous water soluble macromolecular or hydrophobic polymer, keep roughly spheric shape in the time of just can forming preparation, show the granulated silica particle of easy disintegrating during use, and if the granulated silica particle that obtains is engaged in the makeup, then good to the ductility of skin, the film of being made up uniformly.Further, if be surrounded by the effect composition in this granulated silica particle, then mismatch tackiness agent and also can form stable and the high composite powder of interior bag rate, if will be engaged in the makeup with the composite powder of water soluble component as effective constituent, then obtain the ductility of skin good, adaptation, the makeup of moisture retention excellence, in addition, if will be engaged in the makeup with the composite powder of water insoluble active ingredient as effective constituent, then obtain the ductility in the skin good, adaptation, the skin moisten sense, the makeup of agglomeration resistance effect excellence, thus the present invention finished.
That is, the present invention is a granulated silica particle, and this particle is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide form as integrant, median size is that 1～50 μ m, compressive strength are 1～4MPa.
The present invention is the preparation method of granulated silica particle, the method is characterized in that, and be that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide be dispersed in the aqueous solvent form slurries after, these slurries are carried out spraying drying with spray-drier.
The present invention is makeup, and it contains above-mentioned granulated silica particle.
The present invention is a composite powder, it is characterized in that, and be that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m at thickness with primary particle 2The granulated silica particle that forms as integrant of flakey silicon-dioxide in be surrounded by water soluble component.
The present invention is the preparation method of composite powder, the method is characterized in that, and be that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide be dispersed in the aqueous solvent that contains water soluble component form slurries after, these slurries are carried out spraying drying with spray-drier.
The present invention is a composite powder, it is characterized in that, and be that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m at thickness with primary particle 2The granulated silica particle that forms as integrant of flakey silicon-dioxide in be surrounded by water insoluble active ingredient.
The present invention is the preparation method of composite powder, the method is characterized in that, and be that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide join form slurries in the aqueous solvent of disperse water insoluble composition after, these slurries are carried out spraying drying with spray-drier.
The present invention is the preparation method of composite powder, it is characterized in that, and be that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide join form slurries in the aqueous solvent of water insoluble active ingredient of dispersion and emulsion composition forms after, these slurries are carried out spraying drying with spray-drier.
The present invention is makeup, and it contains above-mentioned composite powder.
Granulated silica particle of the present invention, even when not using macromolecular compound to prepare, its shape is also stable.In addition, it is coupled in the makeup etc., when being coated on the skin, slowly disintegration is good to the ductility of skin by the friction of physical property, the film of can being made up uniformly.In addition, composite powder of the present invention does not utilize binder constituents just to wrap in the granulated silica particle with stable effective ingredients and in large quantities.And, this composite powder is coupled in the makeup, when being coated on the skin, the slowly disintegration by the friction of physical property discharges effective constituent, therefore can expect high cosmetic result.Further, this composite powder itself is engaged in the makeup, ductility when being coated on the skin is good, interior bag water soluble component is as adaptation, the moisture retention excellence of the composite powder of effective constituent, and interior bag water insoluble active ingredient is as adaptation, skin moisten sense, the agglomeration resistance effect excellence of the composite powder of effective constituent.
Embodiment
The flakey silicon-dioxide that uses as raw material when preparing the granulated silica particle of first embodiment of the present invention (hereinafter referred to as " first invention "), the thickness of its primary particle is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m 2The amount of the silanol group of this unit specific surface area is equivalent to the several times of silica gel～tens of times.Further, the average aggregate particle size of this flakey silicon-dioxide is 0.05～5 μ m, and thickness is more than 10 with the aspect ratio of long particle diameter, is preferably more than 30.This flakey silicon-dioxide for example obtains by patent documentation 2 disclosed methods, usually provide this flakey silicon-dioxide is dispersed in the colloid that forms in the water with the concentration of 13～15 quality % (following brief note for " % ") disperses thing, therefore can utilize it as flakey silicon-dioxide.As the example of this colloidal dispersion, can enumerate AGCSi-Tech Co., the commercially available products such as SUNLOVELY LFS that Ltd produces.
In addition, (measure under following condition by Model 990 TGA-analyzers (production of TA Instruments Japan company) by thermogravimetry for the silanol group density of above-mentioned flakey silicon-dioxide.That is, silica-filled in little quartz crucible with 20～100mg put in the TGA-analyzer.Make on one side drying nitrogen with 50ml/ minute flow velocity by heating chamber, on one side with 10 ℃/minute ratio sample is heated to 120 ℃, with the water of absorption from the silica sphere physical property remove.Sample is maintained 120 ℃ until no longer observing weight loss.Then, temperature is increased to 300 ℃, keep this temperature until reaching constant weight with previous identical rate of heating.Repeat identical operations down at 500 ℃, 700 ℃, 900 ℃, 1050 ℃ and 1200 ℃.At each temperature, each sample is observed distinctive weight loss.Total silanol group concentration of titanium dioxide silicon face is calculated by the loss of the gross weight % till 1200 ℃ after 120 ℃ drying stage.The calculating of silanol group concentration is undertaken by the supposition that adds thermal bonding form 1 mole water (it loses) in heat treated from sample based on 2 moles of silanol groups.Total silanol group concentration (μ mol/m of titanium dioxide silicon face 2) calculate according to following formula.
Silanol group concentration=W * 1111.1/SA
Wherein, W is that the weight % loss under the balance till the heating of playing during from 120 ℃ constant under 1200 ℃ is poor, and SA is the BET nitrogen specific surface area m of silicon-dioxide 2/ g.
As the aqueous solvent that uses in order to disperse above-mentioned flakey silicon-dioxide, can use purify waste water, the mixed solvent of mineral water, deep water or water and lower alcohol etc.As operable lower alcohol, for example can enumerate ethanol, Virahol etc.Among the present invention, most preferably use in these solvents and purify waste water.And, when flakey silicon-dioxide provides with the form of colloidal dispersion, its further use solvent cut can be used for later granulation step.
The granulated silica particle of first invention can form slurries by flakey silicon-dioxide is dispersed in as required in the aqueous solvent, then this slurries liquid is prepared by granulation step desolventizings such as spraying dryings.As the formation method of slurries, can enumerate and disperse thing to mix flakey silicon-dioxide or its colloid with aqueous solvent, form the method for slurries etc. continuously.At this moment, can also add other composition.
Flakey silica concentration in the above-mentioned slurries is considered to be preferably 7～15% especially from having stability and sense of touch aspect concurrently preferably less than 20%.If more than 20%, the bad dispersibility of the flakey silicon-dioxide in the slurries then, for example, and when adopting the method desolventizing that uses spray-drier, might can not be stably by nozzle spray.
As the method for desolventizing from slurries, can utilize the whole bag of tricks, use spray-drier etc. to carry out spray-dired method but be preferably.As the spray-drier that uses in this spraying drying, the preferred use has disc atomizer or the two-fluid spray nozzle spray-drier as the form of spraying plant.As the spray condition of spray-drier, under the situation of disc atomizer, preferred rotating speed is that 25000～30000rpm, flow are 30～70ml/min.In addition, as drying conditions, can enumerate 90～350 ℃ temperature range.As this spray drying unit, can enumerate the L-8 type of great river former chemical industry machine society production etc.
The median size of the granulated silica particle that as above obtains can be used laser class dry type particle size distribution device (for example, SEISHIN ENTERPRISE Co., the PRO7000S that LTD produces etc.), with volume average particle size (D 50) form measure.Median size to granulated silica particle of the present invention does not limit especially, considers from the sense of touch aspect, is preferably 1～50 μ m, more preferably 1～30 μ m.In addition, particle diameter also can be judged by electron microscope image.And the shape of the granulated silica particle that obtains can be forms such as spherical, special-shaped shape (oval spherical, flats etc.), indefinite shape, but is preferably spherical.In addition, the particle that also has hollow shape in the granulated silica particle.
In addition, the compressive strength of the granulated silica particle of first invention can use slight compression trier MCT-W500 (production of society of Shimadzu Seisakusho Ltd.) to measure.And this compressive strength is that Φ 50 μ m plane pressure heads (Buddha's warrior attendant is made of stones), load speed are that 0.892mN/sec, test power are when measuring under the condition of 9.81mN at the pressurization pressure head, is the scope of 1～4MPa, if then have easy disintegrating at least in this scope.
Second embodiment of the present invention (hereinafter referred to as " second invention ") is surrounded by the composite powder of water soluble component as effective constituent in the granulated silica particle, the flakey silicon-dioxide that uses as raw material is identical with above-mentioned first invention.
In second invention, as the interior water soluble component that wraps in the composite powder, because the drying temperature of the spray-drier that uses in solvable in water, the common desolventizing is more than 100 ℃, therefore be preferably the normally used composition in makeup that boiling point surpasses 100 ℃, for stable and a large amount of hydrous water dissolubility beauty treatment compositions, be preferably polyvalent alcohol.As concrete polyvalent alcohol, can enumerate glycerine, Glycerol dimer, Sorbitol Powder, ethylene glycol, dipropylene glycol, Diethylene Glycol, triethylene glycol, 1,3 butylene glycol etc., can use to be selected from them one or more.
In addition, as water soluble component, except above-mentioned polyvalent alcohol, can also enumerate and to be dissolved in wherein each kind of physiologically active ingredient.The physiologically active ingredient that uses among the present invention can be enumerated the material of when being coated on the skin skin being given certain physiologically active.For example can enumerate whitening composition, anti-inflammatory agent, antiaging agent, anoretic, the agent of compacting, antioxidant, wetting Agent for Printing Inks, blood circulation accelerant, antiseptic-germicide, sterilant, siccative, creeping chill agent, heat sensitizer, vitamins, amino acid, wound healing promotor, stimulation negative catalyst, analgesic agent, cell activator, pigmenting of skin agent, enzyme component etc.Wherein, plant extraction liquid, the marine alga that is preferably natural class especially extracted composition, crude drug composition.Among the present invention, can use one or more these physiologically active ingredients.
Further, as other water soluble component, water colo(u)r such as can also enumerate red No. 106, red No. 227, blue No. 202, blue No. 205, yellow No. 5, yellow No. 203, green No. 201, green No. 202, orange No. 205.
After making above-mentioned water soluble component be included in the aqueous solvent, disperse thing to mix, form slurries with the colloid of flakey silicon-dioxide.Use therein aqueous solvent refers to and purifies waste water, the mixed solvent of mineral water, deep water or these water and lower alcohol.As lower alcohol, can enumerate for example ethanol, Virahol etc.Among the present invention, most preferably use in these aqueous solvents and purify waste water.
The preparation method of composite powder of the present invention is not limited thereto, but preferred by above-mentioned each composition is mixed the formation pulpous state, and these slurries are prepared by granulation step desolventizings such as spraying dryings.As the formation method of slurries, can enumerate by dispersion mill (デ ス パ one ミ Le) and disperse mixing water soluble components in thing and the aqueous solvent at the colloid of flakey silicon-dioxide, form the method for slurries etc. continuously.
Flakey silica concentration in the above-mentioned slurries is considered to be preferably 7～15% especially from having stability and sense of touch aspect concurrently preferably less than 20%.If more than 20%, the bad dispersibility of the flakey silicon-dioxide in the slurries then, for example, and when adopting the method desolventizing that uses spray-drier, might can not be stably by nozzle spray.
As the method for desolventizing from slurries, can utilize the whole bag of tricks, preferred but be not limited to utilize and use spray-drier etc. to carry out spray-dired method.As the spray-drier that uses in this spraying drying, the preferred use has disc atomizer or the two-fluid spray nozzle spray-drier as the form of spraying plant.As the spray condition of spray-drier, under the situation of disc atomizer, preferred rotating speed is that 25000～30000rpm, flow are 30～70ml/min.In addition,, can enumerate 90～350 ℃ temperature range, but, be preferably 90～120 ℃ especially for fear of the sex change of the water soluble component of interior bag as drying conditions.As this spray drying unit, can enumerate the L-8 type that great river former chemical industry machine society produces.
By above-mentioned preparation condition, obtain the composite powder of the water soluble component of preferred interior bag 2～25%.For example, will be prepared into pulpous state as the glycerine and flakey silica 1 5% colloid aqueous solution of water soluble component, the interior bag rate of carrying out the composite powder that spraying drying obtains by spray-drier is 25%.Desire surpasses when bag rate is carried out interior the bag in this, can not wrap in glycerine in the particle that forms by flakey silicon-dioxide fully, glycerine might inboard wall of tube body face attached to drying installation on, the glycerine cohesion that the composite powder of formation and this adhere to can not be reclaimed composite powder effectively.In this specification sheets, interior bag rate by the composite particles that will obtain from room temperature be warming up to 500 ℃ so that when under this temperature, keeping 5 hours the quality (calcination loss) of loss try to achieve.
The particle diameter of the composite powder that as above obtains can use laser class dry type particle size distribution device (for example, SEISHIN ENTERPRISE Co., the PRO7000S that LTD produces etc.), with volume average particle size (D 50) form measure.Particle diameter to second composite powder of inventing does not limit especially, but considers from the sense of touch aspect, is preferably 1～50 μ m, more preferably 1～30 μ m.In addition, particle diameter also can be judged by electron microscope image.The shape of resulting composite powder can be forms such as spherical, special-shaped shape, indefinite shape, but is preferably spherical.
In addition, the compressive strength of the composite powder of second invention can use slight compression trier MCT-W500 (production of society of Shimadzu Seisakusho Ltd.) to measure.And, this compressive strength is that Φ 50 μ m plane pressure heads (Buddha's warrior attendant is made of stones), load speed are that 0.892mN/sec, test power are when measuring under the condition of 9.81mN at the pressurization pressure head, be preferably 0.1～4MPa, be preferably 0.2～3MPa especially, as can be known if in this scope easy disintegrating excellence then.
The composite powder of second invention can also obtain this granulated silica powder absorption, interior bag water soluble component by at first forming the granulated silica powder with the slurries that contain flakey silicon-dioxide and aqueous medium except aforesaid method.
The 3rd embodiment of the present invention (hereinafter referred to as " the 3rd invention ") is surrounded by the composite powder of water insoluble active ingredient as effective constituent in the granulated silica particle, the flakey silicon-dioxide that uses as raw material is identical with above-mentioned first invention.
As the water insoluble active ingredient of interior bag, can enumerate the oiliness composition or contain the emulsifying composition of oiliness composition.Because the drying conditions of the spray-drier that uses in the desolventizing is more than 100 ℃ usually, so these water insoluble active ingredients are preferably the normally used composition in makeup that boiling point surpasses 100 ℃.
As the oiliness composition; can enumerate for example paraffin; ceresin (ceresin wax); ceresine; Microcrystalline Wax; montanin wax; f-t synthetic wax (Fischer-Tropsch wax); polyethylene wax; whiteruss; squalane; Vaseline; polyisobutene; hydrocarbon system classes such as polybutene; carnauba wax; beeswax; lanolin wax; natural waxes such as gama wax; three (docosoic acid) glyceryl ester; pentaerythritol abietate; Jojoba oil; the isocaprylic acid cetyl; Isopropyl myristate; caprylin; the Unimac 5680 double glyceride; ester classes such as Dipentaerythritol fatty acid ester; stearic acid; fatty acids such as docosoic acid; hexadecanol; stearyl alcohol; senior alcohols such as V-1326; sweet oil; Viscotrol C; ermine oil; lipid such as wild lacquer fruit wax; the lanolin fatty acid isopropyl ester; lanolin derivative classes such as Wool wax alcohol; amino acid derivative classes such as N-lauroyl-L-L-glutamic acid two (cholesteryl-docosyl-octyl group dodecyl) ester; polydimethylsiloxane; type siloxane finish classes such as methyl phenyl silicone; PFPE; perfluoro decane; fluorine class finish classes such as PFO; red No. 226; green No. 223; purple waits oil-soluble pigment etc. No. 201, can select to use one or more from them.
In addition, as the interior water insoluble active ingredient that wraps in the 3rd composite powder of inventing, except above-mentioned oiliness composition, can also enumerate phosphatide, UV light absorber, tensio-active agent etc.
As UV light absorber, for example,, can enumerate 2-hydroxyl-4-methoxy benzophenone, 2,2 '-dihydroxyl-4,4 '-dimethoxy-benzophenone, 2,4 dihydroxyl benzophenone, 2,2 ', 4,4 '-tetrahydroxybenzophenone etc. as benzophenone; As the PABA class, can enumerate parathesin, para-amino benzoic acid glyceryl ester, ESCAROL 507 pentyl ester, ESCAROL 507-2-ethylhexyl, to dihydroxypropyl ethyl benzoate etc.; As cinnamic acid, can enumerate p-methoxycinnamic acid-2-ethylhexyl, 4-methoxy cinnamic acid-2-ethoxy ethyl ester etc.; As salicylic acid, can enumerate Whitfield's ointment-2-ethylhexyl, salol, Uniderm Homsal (homomenthyl salicylate) etc.; In addition, can also enumerate 2-(2-hydroxy-5-methyl base phenyl) benzotriazole, the 4-tertiary butyl-4 '-methoxy dibenzoyl methylmethane, oxybenzone (oxybenzone) etc.
And, when being difficult to be dispersed in the aqueous solvent, preferably the form of this composition with emulsifying composition cooperated on the preparation method as the oiliness composition of water insoluble active ingredient.The emulsifying composition of this moment is so long as the composition that is formed by water composition, oiliness composition and tensio-active agent, then can be in O/W type, w/o type, W/O/W type, the O/W/O type any one, can still be preferably O/W type, W/O/W type also with multiple in addition.
When wrapping in the composite powder of the 3rd invention in the water insoluble active ingredient, the method that direct disperse water insoluble composition cooperates is arranged in aqueous solvent and in advance water insoluble active ingredient is made the method for disperseing, cooperating behind the emulsifying composition as mentioned above.
All essential in either event aqueous medium, as aqueous solvent used herein, refer to purify waste water, the mixed solvent of mineral water, deep water or these water and lower alcohol.As lower alcohol, can enumerate for example ethanol, Virahol etc.In the 3rd invention, most preferably use in these aqueous solvents and purify waste water.
Further, as the tensio-active agent that is used for water insoluble active ingredient is made emulsifying composition, so long as the tensio-active agent that uses in makeup then can especially not use with limiting usually.Specifically; can enumerate glycerol fatty acid ester and alkylene glycol affixture thereof; polyglycerol fatty acid ester and alkylene glycol affixture thereof; propylene glycol fatty acid ester and alkylene glycol affixture thereof; sorbitan fatty acid esters and alkylene glycol affixture thereof; Sorbitol Powder fatty acid ester and alkylene glycol affixture thereof; polyalkylene glycol fatty acid; the polyoxyalkylene modified siloxane; nonionic surfactant classes such as the alkyl co-modified siloxanes of polyoxyalkylene; alkyl sulfate; alkylsulfonate; sulfonated; dialkyl sulfosuccinates; α-alpha-sulfonated fatty hydrochlorate; alkyl methyl taurine salt; N-methyl-N-alkyl tauride; polyoxyethylene alkyl ether sulfate salt; polyoxyethylene alkylphenyl ether sulfate salt; alkylphosphonic; Voranol EP 2001 phosphoric acid salt; polyoxyethylene alkyl phenyl ether phosphoric acid salt; N-acyl group-anionic surfactant's classes such as N-alkylaminoacid salts; alkylamine salt; polyamine and alkane acid amides derivative of fatty acid; alkylammonium salt; cationic surfactant classes such as alicyclic ammonium salt; Yelkin TTS; N; N-dimethyl-N-alkyl-amphoterics classes such as N-carboxymethyl ammonium trimethyl-glycine etc. can be used they one or more.
In the above-mentioned water insoluble active ingredient, can further cooperate to be dissolved in wherein each kind of physiologically active ingredient.This physiologically active ingredient can be enumerated the material of when being coated on the skin skin being given certain physiologically active.For example can enumerate whitening composition, anti-inflammatory agent, antiaging agent, anoretic, the agent of compacting, antioxidant, wetting Agent for Printing Inks, blood circulation accelerant, antiseptic-germicide, sterilant, siccative, creeping chill agent, heat sensitizer, vitamins, amino acid, wound healing promotor, stimulation negative catalyst, analgesic agent, cell activator, pigmenting of skin agent, enzyme component etc.Wherein, plant extraction liquid, the marine alga that is preferably natural class especially extracted composition, crude drug composition.These physiologically active ingredients can use one or more.
In addition, can also in above-mentioned aqueous solvent, further add water composition in advance.As this water composition, so long as the water composition that uses in makeup does not then limit especially usually, specifically, can enumerate propylene glycol, 1, polyalcohols such as 3-butyleneglycol, dipropylene glycol, glycerols such as glycerine, Glycerol dimer, Polyglycerine, the wet distillation water of Aloe Barbadensis Miller, witch hazel, cucumber, lemon, lavandula angustifolia, rose etc. etc. can use they one or more.In addition further, in this aqueous solvent, can cooperate to be dissolved in wherein each kind of physiologically active ingredient.This physiologically active ingredient can be enumerated the material of when being coated on the skin skin being given certain physiologically active.For example can enumerate whitening composition, anti-inflammatory agent, antiaging agent, anoretic, the agent of compacting, antioxidant, wetting Agent for Printing Inks, blood circulation accelerant, antiseptic-germicide, sterilant, siccative, creeping chill agent, heat sensitizer, vitamins, amino acid, wound healing promotor, stimulation negative catalyst, analgesic agent, cell activator, pigmenting of skin agent, enzyme component etc.Wherein, plant extraction liquid, the marine alga that is preferably natural class especially extracted composition, crude drug composition.Among the present invention, can use one or more these physiologically active ingredients.
The composite powder of the 3rd invention is by after being dispersed in above-mentioned water insoluble active ingredient in the aqueous solvent, and any composition and the flakey silicon-dioxide that mix other simultaneously form pulpous state, and this slurries desolventizing is prepared.As the formation method of slurries, can enumerate by dispersion mill and disperse mixing water insoluble composition in thing and the aqueous solvent or contain the emulsification of water insoluble active ingredient at the colloid of flakey silicon-dioxide, form the method for slurries etc. continuously.Utilize the high wax time-like of fusing point, preferably it is heated with liquid finish down in room temperature (25 ℃) and mix, add after being prepared into pasty state,, be preferably 60～100 ℃ as this Heating temperature.
Flakey silica concentration in the above-mentioned slurries is considered to be preferably 7～15% especially from having stability and sense of touch aspect concurrently preferably less than 20%.If more than 20%, the bad dispersibility of the flakey silicon-dioxide in the slurries then, for example, and when adopting the method desolventizing that uses spray-drier, might can not be stably by nozzle spray.
As the method for desolventizing from slurries, can utilize the whole bag of tricks, preferred but be not limited to use spray-drier etc. to carry out spray-dired method.As the spray-drier that uses in this spraying drying, the preferred use has disc atomizer or the two-fluid spray nozzle spray-drier as the form of spraying plant.As the spray condition of spray-drier, under the situation of disc atomizer, preferred rotating speed is that 25000～30000rpm, flow are 30～70ml/min.In addition, as drying conditions, can enumerate 90～350 ℃ temperature range, the sex change for fear of the water-based effective constituent of interior bag is preferably 90～120 ℃ especially.As this spraying drying machine, can enumerate great river former chemical industry machine L-8 type.
By above-mentioned preparation condition, obtain the composite powder of the water insoluble active ingredient of preferred interior bag 5～75%.For example, will be prepared into pulpous state as the squalane and flakey silica 1 5% colloid aqueous solution of oiliness composition, the interior bag rate of carrying out the composite powder that spraying drying obtains by spray-drier is about 71%.In addition, the emulsifying composition and flakey silica 1 5% colloid aqueous solution that will contain squalane are prepared into pulpous state, and the interior bag rate of carrying out the composite powder that spraying drying obtains by spray-drier is about 68%.Under any one situation, when the bag rate is bigger in desiring to make, all can not wrap in squalane or emulsifying composition in the flakey silicon-dioxide fully, and on the inboard wall of tube body face attached to drying installation, the composite powder that forms and this squalane that adheres to or emulsifying composition cohesion can not be reclaimed composite powder effectively.
And interior bag rate is to use 1100 ℃ of box-type furnace KBF794 (Koyo Lindberg Co., Ltd. produce) etc., the composite particles that obtains is warming up to the quality (calcination loss) of 500 ℃ and then loss when keeping 5 hours down for 500 ℃ from room temperature.
The particle diameter of the composite powder of the 3rd invention that as above obtains can use laser class dry type particle size distribution device (for example, SEISHIN ENTERPRISE Co., the PRO7000S that LTD produces etc.), with volume average particle size (D 50) form measure.Particle diameter to the 3rd composite powder of inventing does not limit especially, but considers from the sense of touch aspect, is preferably 1～50 μ m, more preferably 1～30 μ m.In addition, particle diameter can be judged by electron microscope image.And the shape of the composite powder that obtains can be forms such as spherical, different form, indefinite shape, but is preferably spherical.
In addition, the compressive strength of the composite powder of the 3rd invention can use slight compression trier MCT-W500 (society of Shimadzu Seisakusho Ltd. system) to measure.And, this compressive strength is that Φ 50 μ m plane pressure heads (Buddha's warrior attendant is made of stones), load speed are that 0.892mN/sec, test power are when measuring under the condition of 9.81mN at the pressurization pressure head, be preferably 0.1～4MPa, be preferably the compressive strength of 0.1～3MPa especially, as can be known if in this scope easy disintegrating excellence then.
The composite powder (following sometimes they are abbreviated as " composite powder ") of the granulated silica particle of the invention of first among the present invention and second invention and the 3rd invention can be used for various uses, but especially preferably is engaged in makeup, the externally applied medicine etc.For example, the use level when granulated silica particle of the present invention or composite powder are used for makeup is different and different according to its formulation, but is preferably 0.5～100%, and more preferably 5～100%.The use level of granulated silica particle or composite powder is 100% o'clock, when promptly makeup all are granulated silica particle or composite powder, obtains the powder of adhesive-free prescription etc.
In the makeup of the present invention, except above-mentioned granulated silica particle and composite powder, in the scope of not damaging effect of the present invention, can also suitably select to use the composition that in makeup, uses usually, for example, powder except above-mentioned granulated silica particle and composite powder (hereinafter referred to as " powder "), grease, the wax class, hydrocarbon, higher fatty acid, higher alcohols, the ester class, metallic soap, oiliness compositions such as silicone oil, alcohols, nonionogenic tenside, anion surfactant, cats product, zwitterionics, siloxane type surfactants etc. are surfactant-based, dyestuff, pigments such as natural pigment, spices, VITAMIN, hormone, sanitas, UV light absorber, antioxidant, sterilant, plant milk extract, enzyme, acid, alkali, special composition classes such as salt, water, polyvalent alcohol, polymer substance, thickening material, sequestrant etc.
As powder, if the common powder that in makeup, uses, then need not be tabular, spherical, shape such as needle-like, particle diameters such as smoke-like, particulate, pigment-level, particle structures such as porous matter, atresia matter wait and limit especially, can enumerate inorganic powder class, organic dust class, pigment powdery type, composite powder class etc.Specifically; can enumerate titanium oxide; black oxidation titanium; Prussian blue; ultramarine; red iron oxide; iron oxide yellow; iron oxide black; zinc oxide; aluminum oxide; silicic anhydride; magnesium oxide; zirconium white; magnesiumcarbonate; lime carbonate; chromic oxide; chromium hydroxide; carbon black; pure aluminium silicate; Magnesium Silicate q-agent; magnesium aluminum silicate; mica; synthetic mica; sericite; talcum; kaolin; silicon carbide; barium sulfate; inorganic powder classes such as boron nitride; pearl white; titanium oxide lining mica; ferric oxide lining mica; ferric oxide lining mica titanium; pigment dyestuff lining mica titanium; luminous powdery type such as aluminium powder form; nylon; polymethylmethacrylate; polyalkyl acrylate; the organopolysiloxane elastomerics; poly methyl silsesquioxane (polymethyl sesquioxane); cross-linking type siloxanes-netted silicone block copolymer; polystyrene; vinyl cyanide-Sipacril 2739OF; vinylidene chloride-Sipacril 2739OF; polyethylene; urethane; the wool powder; the silk powder; the crystalline cellulose powder; organic dust classes such as N-acyl-lysine powder; organic tar class pigment; pigment powdery type such as the pigment lake of organic pigment; the titanium coated mica titanium of particulate oxide; particulate oxide zinc lining mica titanium; barium sulfate lining mica titanium; the anhydrous silicic acid that contains titanium oxide; contain the composite powders such as anhydrous silicic acid of zinc oxide etc., can use in them one or more.And these powder can also be implemented to use after the surface treatment by generally well-known treatment agent such as fluorine cpd, silicone compounds, tensio-active agent.
As finish, so long as the finish that uses in makeup does not then limit especially usually.In addition, the composition that wraps in the composite powder in the time of can be with the composite powder that uses the 3rd invention is identical or different.Specifically; can enumerate paraffin; ceresin; ceresine; Microcrystalline Wax; montanin wax; f-t synthetic wax; polyethylene wax; whiteruss; squalane; Vaseline; polyisobutene; hydro carbons such as polybutene; carnauba wax; beeswax; lanolin wax; natural waxes such as gama wax; three (docosoic acid) glyceryl ester; pentaerythritol abietate; Jojoba oil; the isocaprylic acid cetyl; Isopropyl myristate; caprylin; three Unimac 5680 double glycerides; the Dipentaerythritol fatty acid ester; ester classes such as plant sterol Queensland nut oleic acid ester; stearic acid; docosoic acid; fatty acids such as 12-oxystearic acid; hexadecanol; stearyl alcohol; senior alcohols such as V-1326; sweet oil; Viscotrol C; ermine oil; lipid such as wild lacquer fruit wax; the lanolin fatty acid isopropyl ester; lanolin derivative classes such as Wool wax alcohol; amino acid derivative classes such as N-lauroyl-L-L-glutamic acid two (cholesteryl-docosyl-octyl group dodecyl) ester; polydimethylsiloxane; methyl phenyl silicone; alkyl-modified organopolysiloxane; alkoxy-modified organopolysiloxane; higher fatty acid modification organopolysiloxane; type siloxanes such as fluorine modified siloxane; PFPE; perfluoro decane; fluorine class finish classes such as PFO etc. can be used in them one or more.
As tensio-active agent, so long as the finish that uses in makeup does not then limit especially usually.In addition, it is identical or different to wrap in the composition that uses in the emulsifying composition in the composite powder in the time of can be with the composite powder that uses the 3rd invention.Specifically; can enumerate glycerol fatty acid ester and alkylene glycol affixture thereof; polyglycerol fatty acid ester and alkylene glycol affixture thereof; propylene glycol fatty acid ester and alkylene glycol affixture thereof; sorbitan fatty acid esters and alkylene glycol affixture thereof; Sorbitol Powder fatty acid ester and alkylene glycol affixture thereof; polyalkylene glycol fatty acid; the polyoxyalkylene modified siloxane; nonionic surfactant classes such as the alkyl co-modified siloxanes of polyoxyalkylene; alkyl sulfate; alkylsulfonate; sulfonated; dialkyl sulfosuccinates; α-alpha-sulfonated fatty hydrochlorate; alkyl methyl taurine salt; N-methyl-N-alkyl tauride; polyoxyethylene alkyl ether sulfate salt; polyoxyethylene alkylphenyl ether sulfate salt; alkylphosphonic; Voranol EP 2001 phosphoric acid salt; polyoxyethylene alkyl phenyl ether phosphoric acid salt; N-acyl group-anionic surfactant's classes such as N-alkylaminoacid salts; alkylamine salt; polyamine and alkane acid amides derivative of fatty acid; alkylammonium salt; cationic surfactant classes such as alicyclic ammonium salt; Yelkin TTS; N; N-dimethyl-N-alkyl-amphoterics classes such as N-carboxymethyl ammonium trimethyl-glycine etc. can be used they one or more.
As oily jelling agent, so long as the composition that uses in makeup does not then limit especially usually.Specifically, dextrin fatty acid ester, sucrose fatty ester, starch fatty acid ester, oxystearic acid, calcium stearate etc. can be enumerated, they one or more can be used.
As water composition, so long as the water composition that uses in makeup does not then limit especially usually.This water composition can with when using the composite powder of second invention in the water composition that wraps in the composite powder identical or different.Similarly, can with when using the composite powder of the 3rd invention in to wrap in the water composition that uses in the emulsifying composition in the composite powder identical or different.Specifically, can enumerate water, propylene glycol, 1, polyalcohols such as 3-butyleneglycol, dipropylene glycol, glycerols such as glycerine, Glycerol dimer, Polyglycerine, plant extraction liquids such as Aloe Barbadensis Miller, witch hazel, cucumber, lemon, lavandula angustifolia, rose etc. can use they one or more.
As UV light absorber, so long as the UV light absorber of using in makeup does not then limit especially usually.Specifically; can enumerate 2-hydroxyl-4-methoxy benzophenone, 2; 4; 6-triphen amido-right-(carbonyl-2-ethylhexyl-1 '-oxygen base)-benzophenones such as 1,3,5-triazines; Whitfield's ointment-salicylic acids such as 2-ethylhexyl; to PABA classes such as dihydroxypropyl ethyl benzoates, phenyl phenacyl ketone classes such as uncle 4--4 '-methoxy dibenzoyl methylmethane etc. can be used they one or more.
As water-soluble polymer, so long as the water-soluble polymer that uses in makeup does not then limit especially usually.Specifically, can enumerate derivatived cellulose classes such as methyl fiber, Walocel MT 20.000PV, Natvosol, hydroxypropylcellulose, carboxymethyl cellulose, sodiun alginate, carrageenin, Quinces Quince seed glue, agar, gelatin, xanthan gum, Viscogum BE, pectin, gelling gum natural polymers such as (gellangum), synthetic macromolecule classes such as polyvinyl alcohol, carboxyvinyl polymer, alkyl addition carboxyvinyl polymer, sodium methacrylate, polyacrylic acid glycerol ester, polyvinylpyrrolidone etc. can be used they one or more.
The makeup of forms such as that makeup of the present invention can be enumerated is Powdered, solid state, solid powdery, bar-shaped, aqueous, emulsifiable paste shape, multilayer shape, sheet.In addition, the formulation of makeup of the present invention can be enumerated powdery cosmetic, oil-based cosmetic preparation, oil-in-water emulsion type cosmetic preparation, water-in-oil emulsified cosmetic, water system makeup, solvent-borne type makeup, sheet cosmetics etc.And form and the formulation of significantly bringing into play effect of the present invention are the makeup of solid powdery.
Makeup of the present invention, for example can be used as color make-up makeup such as foundation cream, powder, rouge, eye shadow, eyebrow cosmetics, screening flaw product, lipstick, Mascara, eyeliner etc., skin protection cosmeticss such as astringent, emulsion, emulsifiable paste, facial mask, sunscreen products, clean product, makeup removing product, cosmetic hairs such as shampoo, hair conditioner, hair mousse, and toilet powder shui, bath shampoo etc., but wherein be preferably the color make-up makeup.
Invent the granulated silica particle that obtains dimensionally stable by first among the present invention, think that its mechanism of action is as described below.
That is, the primary particle of flakey silicon-dioxide is 20～70 μ mol/m of the thickness several times that are that 0.1 μ m is following, the silanol group (SiOH) of unit specific surface area is very many, are equivalent to silica gel～tens of times 2Primary particle.
Therefore,, by hydrogen bonding, therefore form firm laminated film between the silanol group on flakey silicon-dioxide lamination, surface, form the granulated silica particle of dimensionally stable by carrying out Air drying or heat drying.
In addition,, obtain in a large number and the stably interior composite powder that wraps water soluble component or water insoluble active ingredient, think that its mechanism of action is as described below by second invention of the present invention and the 3rd invention.
That is, as mentioned above, laminated flakey silicon-dioxide since the surface silanol group between form firm laminated film by hydrogen bonding, in addition the ratio outer surface area of this flakey silicon-dioxide big, be 50～400m 2/ g, and has the gap about 0.05～1ml/g, in this gap, catch water soluble component, oiliness composition or contain water soluble component or the water insoluble active ingredient of the emulsification of oiliness composition etc., when carrying out spraying drying, if water soluble component, then can interiorly in large quantities wrap for example 5～25 left and right sides %, if water insoluble active ingredient, then can interior in large quantities bag about 5～75%.
Embodiment
With comparative example the present invention is carried out specific description by the following examples.In addition, the various evaluation methods of the makeup that use in embodiment and the comparative example are as follows.These embodiment do not carry out any qualification to the present invention.
Embodiment 1
The preparation of granulated silica particle
With silanol group density is 60 μ mol/m 215% concentration aqueous solvent colloidal suspended substance (SUNLOVELY-LFS-C of flakey silicon-dioxide; AGC Si-Tech Co., Ltd. produces) as raw slurry.This raw slurry use had spray-drier (the L-8 type of disc atomizer; Great river former chemical industry machine society system), be that 30000rpm, flow are that 50ml/min, temperature in are set under the condition that 200 ℃, temperature out are set at 130～140 ℃ and carry out spraying drying at the atomizer rotating speed as spraying plant.
The median size of the granulated silica particle that obtains is measured by laser class dry type particle size distribution device (SEISHIN ENTERPRISE Co., the PRO7000S that LTD produces), and the result is 15 μ m.In addition, the compressive strength of the granulated silica particle that obtains is measured by the slight compression trier, and the result is 2.6MPa.Further, during with the observable granulated silica particle of SEM, confirm that flakey silicon-dioxide is laminated spherical particle (Fig. 1).Further, when in purifying waste water, being dispersed with the 10% colloid dispersion thing (slurries) of granulated silica particle, do not use tensio-active agent to be evenly dispersed in (Fig. 2) in the water system external phase even confirm with observation by light microscope yet.
Comparative example 1
With silanol group density is 8.0 μ mol/m 2, median size is the slurries that the spherical silicon dioxide of 12 μ m is dispersed in 15% concentration that obtains in purifying waste water, and uses the spray-drier with disc atomizer as spraying plant, carries out spraying drying under condition similarly to Example 1.With the scanning electron microscope thing that sees drying, the result as can be known, the spherical particle of 12 μ m only exists with the form of the aggregate of part cohesion, can not get the granulation particle.
Comparative example 2
With silanol group density is 7.0 μ mol/m 2, median size is the slurries that the flakey silicon-dioxide of 25 μ m is dispersed in 15% concentration that obtains in purifying waste water, and uses the spray-drier with disc atomizer as spraying plant, carries out spraying drying under condition similarly to Example 1.With the scanning electron microscope thing that sees drying, the result as can be known, above-mentioned flakey silicon-dioxide only exists with the form of the aggregate of part cohesion, can not get the granulation particle.
Embodiment 2
Solid powdery foundation cream (do and use special use):
The dry thing that obtains in granulated silica that obtains among the use embodiment 1 and the comparative example 1～2 prepares the solid powdery foundation cream with composition shown in the table 1 and following preparation method.
For the solid powdery foundation cream that obtains,, " along sliding putting on the skin open property (sliding ら か な stretches び Wide Ga り) " and " formation of the film of making up uniformly " are estimated according to evaluation method shown below and judgment standard.Its result is as shown in table 1.
[table 1]
(％)
Figure G2008800110220D00171
(preparation method)
A: use Henschel mixer (Mitsui three Chi She systems) with composition 1～12 homodisperse.
B: with composition 13～16 uniform mixing.
C: stir A with Henschel mixer (Henschel mixer) on one side, Yi Bian add B, and homodisperse.
D: pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains solid powdery foundation cream (do and use special use).
(evaluation method)
The member of cosmetic evaluation professional group 20 people use each solid powdery foundation cream, for the project of " along sliding putting on the skin open property " and " formation of the film of making up uniformly ", according to following metewand each sample are carried out the evaluation of 7 grades separately.For the scoring that each sample is given, try to achieve the average mark of whole group members' scoring, judge according to following judging criterion.
Metewand:
(evaluation) (content)
6: very good
5: good
4: good slightly
3: common
2 is poor slightly
1: poor
0: non-constant
Judgment standard:
(average mark of scoring) (evaluation)
5.0 more than: ◎ (very good)
3.5 it is above and less than 5.0: zero (well)
1.0 it is above and: △ (common) less than 3.5
Less than 1.0: * (bad)
As shown in Table 1, the solid powdery foundation cream (contrivance) of the granulated silica preparation of use embodiment 1 is all excellent in " along sliding putting on the skin open property " and " formation of the film of making up uniformly " two projects.On the other hand, the powder foundation cream (relatively thing 1) that does not cooperate granulated silica particle along sliding putting on the skin open property, uniformly make up all poor aspect the film.In addition, the powder foundation cream (relatively thing 2) that is combined with the dry thing of comparative example 1 along sliding putting on the skin open property, uniformly make up all poor aspect the film.Further, the powder foundation cream (relatively thing 3) that is combined with the dry thing of comparative example 2 along sliding putting on the skin open property, uniformly make up all poor aspect the film.Infer that this is that silanol group density is low, can not carry out granulation effectively because the granulated silica of comparative example 2 is compared with the granulated silica particle of embodiment 1.
Embodiment 3
The solid powdery rouge
By following compositions and preparation method, preparation solid powdery rouge.
(composition) (%)
1. mica 20.0
2. talcum surplus
3. the granulated silica particle 10.0 of embodiment 1
4. titanium oxide lining mica 10.0
5. red No. 226 0.5
6. ultramarine 0.2
7. synthetic chloroflo powder 5.0
8. methyl p-hydroxybenzoate 0.2
9. squalane 1.0
10. spices is an amount of
(preparation method)
A: composition 1～8 is disperseed equably with Henschel mixer (Mitsui three Chi She systems).
B: composition 9,10 is mixed equably.
C: add B on one side stir A with Henschel mixer on one side, and homodisperse.
D: pulverize C with pulverizer.
E: D is filled in the metal ware, and compressed moulding obtains the solid powdery rouge.
The solid powdery rouge that obtains is all excellent in " along sliding putting on the skin open property " and " formation of the film of making up uniformly " two projects.
Embodiment 4
The solid powdery eye shadow
By following compositions and preparation method, preparation solid powdery eye shadow.
(composition) (%)
1. polydimethylsiloxane is handled synthetic phlogopite 10.0
2. polydimethylsiloxane is handled the talcum surplus
3. titanium oxide lining mica 30.0
4. boron nitride 5.0
5. polyethylene terephthalate-aluminium-epoxy (epoxy) lamination powder 5.0
6. the granulated silica particle 20.0 of embodiment 1
7. ultramarine 2.0
8. yellow No. 401 0.5
9. cross-linking type siloxanes-web-like silicon siloxane copolymers 1.0
10. methyl p-hydroxybenzoate 0.2
11. whiteruss 2.0
12. Vaseline 1.0
13. polydimethylsiloxane 3.0
14. spices is an amount of
(preparation method)
A: composition 1～10 is disperseed equably with Henschel mixer (Mitsui three Chi She systems).
B: with composition 11～14 heating and dispersion equably.
C: add B on one side stir A with Henschel mixer on one side, and homodisperse.
D: pulverize C with pulverizer.
E: D is filled in the metal ware, and compressed moulding obtains the solid powdery eye shadow.
The solid powdery eye shadow that obtains is all excellent in " along sliding putting on the skin open property " and " formation of the film of making up uniformly " two projects.
Embodiment 5
Solid powdery foundation cream (water uses special-purpose (water uses Graduate to use))
By following compositions and preparation method, preparation solid powdery eye shadow.
(composition) (%)
1. talcum surplus
2. mica 20.0
3. titanium oxide lining mica 2.0
4. titanium oxide 15.0
5. boron nitride 5.0
6. red iron oxide 0.8
7. iron oxide yellow 2.5
8. iron oxide black 0.3
9. the granulated silica particle 15.0 of embodiment 1
10. methyl p-hydroxybenzoate 0.2
11. PFPE 2.0
12. polydimethylsiloxane 5.0
13. oxybenzone 3.0
14. polyoxyethylene (20 moles) dehydrated sorbitol mono-fatty acid ester 0.5
15. spices is an amount of
(preparation method)
A: composition 1～10 is disperseed equably with Henschel mixer (Mitsui three Chi She systems).
B: composition 11～15 is mixed equably.
C: add B on one side stir A with Henschel mixer on one side, and homodisperse.
D: pulverize C with pulverizer.
E: D is filled in the metal ware, and compressed moulding obtains solid powdery foundation cream (water uses special-purpose).
The solid powdery foundation cream that obtains (water uses special-purpose) is all excellent in " along sliding putting on the skin open property " and " formation of the film of making up uniformly " two projects.
Embodiment 6
Makeup removing oil
By following compositions and preparation method, preparation makeup removing oil.
(composition) (%)
1. Rice pollard oil 35.0
2. whiteruss surplus
3. three-2 ethyl hexanoic acid glyceryl ester 10.0
4. methyl phenyl silicone 5.0
5. four oleic acid POE (30) sorbitol esters 9.0
6. phenoxyethyl alcohol 0.8
7. Semen Coicis oil (coix seed oil) 0.1
8. Thistle oil 0.1
9. natural VE 0.1
10. spices is an amount of
11. the granulated silica particle 1.0 of embodiment 1
(preparation method)
A: composition 1～10 is mixed equably.
B: in A, add composition 11 lentamente, mix equably, obtain makeup removing oil thus.
The makeup removing oil that obtains is excellence aspect " along sliding putting on the skin open property ".
Embodiment 7
The water-in-oil type sunscreen emulsifiable paste
By following compositions and preparation method, preparation water-in-oil type sunscreen emulsifiable paste.
(composition) (%)
1. methyl trimethoxy polysiloxane (methyl trimethicone) 5.0
2. vinylformic acid-siloxane treated particulate titanium dioxide (annotate 1) 5.0
3.PEG-9 polydimethyl siloxy-ethyl dimethicone (annotating 2) 0.5
4. polydimethylsiloxane (annotate 3) 2.0
5. trimethylsiloxy silicic acid/decamethylcyclopentasiloxane solution (annotate 4) 9.0
6. stearic acid inulin (annotate 5) 2.0
7. the p-methoxycinnamic acid monooctyl ester 3.0
8. diethylamino hydroxy benzoyl hexyl benzene manthanoate 0.5
9.2-thylhexoic acid cetyl 5.0
10.PEG-9 polydimethyl siloxy-ethyl dimethicone (annotating 2) 2.5
11. ethanol 10.0
12. glycerine 2.0
13. sodium-chlor 1.0
14. sanitas is an amount of
15. the granulated silica particle 2.0 of embodiment 1
16. spices is an amount of
The surplus 17. purify waste water
Annotate 1:KF-549 (chemical industry society of SHIN-ETSU HANTOTAI system) and handle particulate titanium dioxide (median size 0.02 μ m)
Annotate 2:KF-6028 (chemical industry society of SHIN-ETSU HANTOTAI system)
Annotate 3:KF96A-2cs (chemical industry society of SHIN-ETSU HANTOTAI system)
Annotate 4:KF-7312J (chemical industry society of SHIN-ETSU HANTOTAI system)
Annotate 5:RHEOPEARL ISK (Chiba powder process society system)
(preparation method)
A: handle composition 1～3 with ball mill, they are disperseed equably.
With composition 4～10 heating for dissolving, add A and mixed dissolution equably under 70 ℃ of the B:D.
C: with composition 11～14 and composition 17 mixed dissolutions.
D: carry out emulsification on one side in B, add C on one side, cool off then.
E: added ingredients 15,16 in D, and carry out uniform mixing, obtain the water-in-oil type sunscreen emulsifiable paste.
The acomia viscosity of water-in-oil type sunscreen emulsifiable paste that obtains is along sliding putting on the skin open property excellence.
Embodiment 8
Double zone lotion (lotion)
By following compositions and preparation method, the preparation double zone lotion.
(composition) (%)
1.POE alkyl oxide (8 moles) phosphoric acid 0.1
2. purify waste water 2.5
3. zinc oxide 0.1
4. the granulated silica 0.5 of embodiment 1
5. aluminum chloride 0.4
6. the surplus of purifying waste water
7. ethanol 2.0
8. the Unimac 5680 polyoxyethylene hydrogenated castor oil 0.1
9. isopropyl methyl phenol 0.1
10. sanitas is an amount of
11. ethanol 18.0
12. Trisodium Citrate 0.5
13. purify waste water 10.0
(preparation method)
A. with composition 5～7 uniform mixing.
B. composition 1～4 is mixed, be dispersed among the A.
C. after composition 8～13 being mixed, uniform mixing obtains double zone lotion in B.
The double zone lotion sense of touch that obtains is dry and comfortable, along sliding putting on the skin open property excellence.
Embodiment 9
Liquid detergent
By following compositions and preparation method, the preparation liquid detergent.
(composition) (%)
1. the fatty acid distribution of coconut oil trolamine 10.0
2. fatty acid distribution of coconut oil potassium 5.0
3. the fatty acid distribution of coconut oil amido propyl betaine 5.0
4.2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazole trimethyl-glycine 3.0
5. the fatty acid distribution of coconut oil diglycollic amide 3.0
6. ethylene glycol monostearate 3.0
7. squalane 0.5
8. xanthan gum 0.1
9. Natvosol 0.1
10. Poise C-80M 0.1
11. the granulated silica 0.5 of embodiment 1
The surplus 12. purify waste water
13. sanitas is an amount of
(preparation method)
A. after under 70 ℃ composition 6～8 being mixed equably, the part of added ingredients 12 is carried out emulsification.Then, be cooled to room temperature.
B. the remainder with composition 1～5 and 12 mixes equably.
C. in B, add A, mix equably.
D. in C, add composition 9,10, mix equably.
E. in D, add 11,13, mix equably, obtain liquid clean agent.
Liquid clean the agent sense of touch that obtains is dry and comfortable, along sliding putting on the skin open property excellence.
Embodiment 10
The oil-in-water type emulsion foundation cream
By following compositions and preparation method, preparation oil-in-water type emulsion foundation cream.
(composition) (%)
1. stearic acid 0.5
2. hexadecanol 1.0
3. polyoxyethylene (20 moles) dehydrated sorbitol mono-fatty acid ester 0.8
4. NOFABLE SO-992 0.4
5.2-thylhexoic acid cetyl 5.0
6. whiteruss 5.0
7. the granulated silica 3.0 of embodiment 1
8. glycerine 3.0
9.1,3-butyleneglycol 5.0
10. the alkyl-modified carboxyl group vinyl polymer 0.1
11. alkyl acrylate copolymer 1.0
12. trolamine 0.5
13. sanitas is an amount of
The surplus 14. purify waste water
15. fluorine cpd are handled titanium oxide 4.0
16. fluorine cpd are handled talcum 1.0
17. fluorine cpd are handled red iron oxide 0.5
18. fluorine cpd are handled iron oxide yellow 1.5
19. fluorine cpd are handled iron oxide black 0.1
(preparation method)
A: add composition 1～3 and composition 5,6, heating mixes under 75 ℃.
B: mixing element 15～19 in composition 4,8,9, use the triple-roller mill homodisperse.
C: in B, add composition 10～14, heat down at 75 ℃ and mix.
D: in C, add A, carry out emulsification.
E: after the D cooling, added ingredients 7 obtains the oil-in-water type emulsion foundation cream.
The oil-in-water type emulsion foundation cream sense of touch that obtains is dry and comfortable, along sliding putting on the skin open property, the excellent in uniformity of cosmetic film.
Embodiment 11
Non-water system Mascara
By following compositions and preparation method, prepare non-water system Mascara.
(composition) (%)
1. pentaerythritol abietate 10.0
2. the gama wax resin 2.0
3. the Palmiticacid dextrin 3.0
4. ceresin 4.0
5. beeswax 3.0
6. soybean phospholipid 0.5
7. light isoparaffins surplus
8. trimethylsiloxy silicic acid 2.0
9. dimethyl distearyl ammonium hectorite 3.0
10. propylene glycol carbonate 1.0
11. light liquid isoparaffin 30.0
12. fluorine cpd are handled iron oxide black 5.0
13. fluorine cpd handle sliding 10.0
14. the granulated silica 2.0 of embodiment 1
(preparation method)
A: under 110 ℃ with composition 1～8 heating for dissolving equably.
B:, obtain oil-base gel with composition 9～11 homodisperse.
C: in A, add B, mix equably.
D: in C, add composition 12,13, mix equably.
E: D is handled with triple-roller mill.
F: in E, add composition 14, mix equably.
G: F is filled in the container, obtains non-water system Mascara.
The rapid-drying properties of the non-water system Mascara that obtains, the excellent in uniformity of cosmetic film.
Embodiment 12
The preparation that powder is closed in cladding in the glycerine:
In silanol group density is 60 μ mol/m 215% concentration aqueous solvent colloidal suspended substance (SUNLOVELY-LFS-C of flakey silicon-dioxide; AGC Si-Tech Co., Ltd. produces) disperse glycerine 5.0 mass parts equably with dispersion mill in 95 mass parts, form slurries.This slurries use had spray-drier (the L-8 type of disc atomizer; Great river former chemical industry machine society system), be that 30000rpm, flow are that 50ml/min, temperature in are set at spraying drying under the condition that 200 ℃, temperature out are set at 130～140 ℃ at the atomizer rotating speed as spraying plant.
The bag rate is measured by calcination loss in the glycerine of the composite powder that obtains, and the result is 14%.In addition, the compressive strength of the composite powder that obtains is measured by the slight compression trier, and the result is 1.0MPa.Further, by the median size of laser class dry type particle size distribution device mensuration composite powder, the result is 18 μ m.Calcination loss carries out according to the calcination loss test method(s) of quasi drug (medicine part outer article) raw material standard record.
Embodiment 13
The preparation that powder is closed in cladding in the 1,3 butylene glycol:
With silanol group density 60 μ mol/m 2The flakey silicon-dioxide colloid that is dispersed in 15% concentration that obtains in purifying waste water disperse in thing 94.5 mass parts, disperse 1,3 butylene glycol 5.4 mass parts equably and be dissolved in wherein xitix 0.1 mass parts with dispersion mill.The spray-drier that its use is had disc atomizer is as spraying plant, spraying drying under the condition of embodiment 12.
The interior bag rate of the 1,3 butylene glycol of the composite powder of being tried to achieve by the calcination loss of the composite powder that obtains and the solute of xitix is 9.5%.In addition, the median size of the composite powder that records by laser class dry type particle size distribution device (PRO7000S that SEISHIN ENTERPRISE Co., LTD produce) is 18 μ m.
Embodiment 14
The preparation that powder is closed in cladding in the glycerine:
With silanol group density 60 μ mol/m 2The flakey silicon-dioxide colloid that is dispersed in 15% concentration that obtains in purifying waste water disperse in thing 90 mass parts, disperse glycerine 9.9 mass parts equably and be dissolved in wherein water-soluble absorption agent Phenylbenzimidazolesulfonic acid 0.1 mass parts with dispersion mill.The spray-drier that its use is had disc atomizer is as spraying plant, and spraying drying under the condition of embodiment 12 obtains composite powder.
The interior bag rate of the glycerine of the composite particles of being tried to achieve by the calcination loss of the composite powder that obtains and the solute of Phenylbenzimidazolesulfonic acid is 22%.In addition, the median size of the composite powder that records by laser class dry type particle size distribution device (PRO7000S that SEISHIN ENTERPRISE Co., LTD produce) is 16 μ m.
Embodiment 15
The preparation that powder is closed in cladding in the Glycerol dimer:
With silanol group density 60 μ mol/m 2The flakey silicon-dioxide colloid that is dispersed in 15% concentration that obtains in purifying waste water disperse in thing 90 mass parts, disperse Glycerol dimer 9.9 mass parts equably and be dissolved in wherein Rizinsan K2 A2 0.1 mass parts with dispersion mill.The spray-drier that its use is had disc atomizer is as spraying plant, and spraying drying under the condition of embodiment 12 obtains composite powder.
The interior bag rate of the Glycerol dimer of the composite particles of being tried to achieve by the calcination loss of the composite powder that obtains and the solute of Rizinsan K2 A2 is 20%.In addition, the median size of the composite powder that records by laser class dry type particle size distribution device (PRO7000S that SEISHIN ENTERPRISE Co., LTD produce) is 15 μ m.
Comparative example 3
The relatively preparation of composite powder:
With silanol group density 8.0 μ mol/m 2, particle diameter is that the colloid that the spherical silicon dioxide of 12 μ m is dispersed in 15% concentration that obtains in purifying waste water disperses to disperse glycerine 5.0 mass parts equably with dispersion mill in thing 95 mass parts.The spray-drier that its use is had disc atomizer is as spraying plant, and spraying drying under the condition of embodiment 12 obtains composite powder.
Try to achieve by the calcination loss of the composite powder that obtains that the bag rate is 6.0% in the glycerine of composite powder.In addition, observe this comparison composite powder with scanning electron microscope, the result as can be known, only the form with the aggregate of the part cohesion of the spherical particle of 12 μ m exists, and can not form the granulation particle as embodiment.
So using silanol group density is 8.0 μ mol/m 2Spherical silicon dioxide the time, the interior bag rate of glycerine can not be for more than 6.0%.This be because, when utilizing particle diameter to be the spherical silicon dioxide of 12 μ m, do not form the granulation particle, glycerine is not by Nei Bao and on the inboard wall of tube body face attached to drying installation, the glycerine that the composite powder of formation and this adhere to condenses, and can not reclaim composite powder effectively.Hence one can see that, when silanol group density is hanged down, no matter the shape of silicon-dioxide is how, in the bag water soluble component.
Comparative example 4
The relatively preparation of composite powder:
With silanol group density 7.0 μ mol/m 2, particle diameter is that the colloid that the flakey silicon-dioxide of 25 μ m is dispersed in 15% concentration that obtains in purifying waste water disperses to disperse glycerine 5.0 mass parts equably with dispersion mill in thing 95 mass parts.The spray-drier that its use is had disc atomizer is as spraying plant, and spraying drying under the condition of embodiment 12 obtains composite powder.
Try to achieve by the calcination loss of the composite powder that obtains that the bag rate is 5.0% in the glycerine of composite powder.In addition, observe this comparison composite powder with scanning electron microscope, the result as can be known, only the form with the aggregate of the part of above-mentioned flakey silicon-dioxide cohesion exists, and can not form the granulation particle as embodiment.
And using silanol group density as mentioned above is 7.0 μ mol/m 2Flakey silicon-dioxide the time, the interior bag rate of glycerine can not reach more than 5.0%.This be because, glycerine wraps in the flakey silicon-dioxide that particle diameter is 25 μ m in not, and on the inboard wall of tube body face attached to drying installation, the glycerine that the composite powder of formation and this adhere to condenses.Hence one can see that, when silanol group density is hanged down, even be that flakey is not also by interior bag.
Embodiment 16
Solid powdery foundation cream (do and use special use):
Prepare solid powdery foundation cream (do and use special use) by composition shown in the table 2 and following preparation method.For this solid powdery foundation cream,, its " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the sense of preserving moisture of skin " are estimated according to evaluation method shown below and judgment standard.Its result is as shown in table 2.
(composition)
[table 2]
(％)
Figure G2008800110220D00301
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～14 is disperseed equably.
B. composition 15～19 is mixed equably.
C. stir A with Henschel mixer on one side and add B, homodisperse on one side.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains solid powdery foundation cream (do and use special use).
(evaluation method)
The member of cosmetic evaluation professional group 20 people use above-mentioned thing of the present invention and compare the solid powdery foundation cream of thing (do and use special use), for " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the sense of preserving moisture of skin ", according to following metewand each sample is carried out the evaluation of 7 grades separately, and mark.Further try to achieve the average mark of whole group members' scoring, judge according to following judgment standard.About " to the sense of preserving moisture of skin ", be the comprehensive evaluation of the preserve moisture sense of each member of professional group after carrying out common life in 3 hours after preserve moisture sense and the coating after the coating just.
Metewand:
(evaluation) (content)
6: very good
5: good
4: good slightly
3: common
2: poor slightly
1: poor
0: non-constant
Judgment standard:
(average mark of scoring) (evaluation)
5.0 more than: ◎ (very good)
3.5 it is above and less than 5.0: zero (well)
1.0 it is above and: △ (common) less than 3.5
Less than 1.0: * (bad)
As shown in Table 2, use the solid powdery foundation cream of thing 2～5 of the present invention all excellent in " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the sense of preserving moisture of skin " whole projects.
On the other hand, do not cooperate composite powder comparison thing 4 the powder foundation cream along sliding putting on the skin open property, with the adaptation of skin, the sense of preserving moisture to skin in all poor.In addition, be combined with the powder foundation cream of comparison thing 5 of the composite powder of comparative example 3, along sliding putting on the skin open property excellence, but adaptation, the sense of preserving moisture are poor.In addition, be combined with the powder foundation cream of comparison thing 6 of the composite powder of comparative example 4, along sliding putting on the skin open property excellence, but with the adaptation of skin, poor to the sense of preserving moisture of skin.
Embodiment 17
The solid powdery rouge
By following compositions and preparation method, preparation solid powdery rouge.
(composition) (%)
1. mica 20.0
2. talcum surplus
3. the composite powder 10.0 of embodiment 13
4. titanium oxide lining mica 10.0
5. red No. 226 0.5
6. ultramarine 0.2
7. synthetic chloroflo powder 5.0
8. methyl p-hydroxybenzoate 0.2
9. squalane 1.0
10. spices is an amount of
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～8 is disperseed equably.
B. composition 9,10 is mixed equably.
C. stir A with Henschel mixer on one side and add B, homodisperse on one side.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains the solid powdery rouge.
The solid powdery rouge that obtains is all excellent in " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the sense of preserving moisture of skin " whole projects.
Embodiment 18
The solid powdery eye shadow:
By following compositions and preparation method, preparation solid powdery eye shadow.
(composition) (%)
1. polydimethylsiloxane is handled synthetic phlogopite 10.0
2. polydimethylsiloxane is handled the talcum surplus
3. titanium oxide lining mica 30.0
4. boron nitride 5.0
5. polyethylene terephthalate-aluminium-epoxy laminate powder 5.0
6. the composite powder 20.0 of embodiment 14
7. ultramarine 2.0
8. yellow No. 401 0.5
9. cross-linking type siloxanes-web-like silicon siloxane copolymers 1.0
10. methyl p-hydroxybenzoate 0.2
11. whiteruss 2.0
12. Vaseline 1.0
13. polydimethylsiloxane 3.0
14. spices is an amount of
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～10 is disperseed equably.
B. with composition 11～14 heating, dispersion equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains the solid powdery eye shadow.
The solid powdery eye shadow that obtains is all excellent in " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the sense of preserving moisture of skin " whole projects.
Embodiment 19
Solid powdery foundation cream (water uses special-purpose):
By following compositions and preparation method, preparation solid powdery foundation cream (water uses special-purpose).
(composition) (%)
1. talcum surplus
2. mica 20.0
3. titanium oxide lining mica 2.0
4. titanium oxide 15.0
5. boron nitride 5.0
6. red iron oxide 0.8
7. iron oxide yellow 2.5
8. iron oxide black 0.3
9. the composite powder 15.0 of embodiment 15
10. methyl p-hydroxybenzoate 0.2
11. PFPE 2.0
12. polydimethylsiloxane 5.0
13. oxybenzone 3.0
14. polyoxyethylene (20 moles) dehydrated sorbitol mono-fatty acid ester 0.5
15. spices is an amount of
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～10 is disperseed equably.
B. composition 11～15 is mixed equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains solid powdery foundation cream (water uses special-purpose).
The solid powdery foundation cream that obtains (water uses special-purpose) is all excellent in " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the sense of preserving moisture of skin " whole projects.
Embodiment 20
Makeup removing oil
By following compositions and preparation method, preparation makeup removing oil.
(composition) (%)
1. Rice pollard oil 35.0
2. whiteruss surplus
3. three-2 ethyl hexanoic acid glyceryl ester 10.0
4. methyl phenyl silicone 5.0
5. four oleic acid POE (30) sorbitol esters 9.0
6. phenoxyethyl alcohol 0.8
7. Semen Coicis oil 0.1
8. Thistle oil 0.1
9. natural VE 0.1
10. spices is an amount of
11. the composite powder 1.0 of embodiment 12
(preparation method)
A. composition 1～10 is mixed equably.
B. in A, add composition 11 lentamente, mix equably, obtain makeup removing oil thus.
The makeup removing oil that obtains " along sliding putting on the skin open property ", " with the affinity (な じ body) of dirt " and " to the sense " excellence of preserving moisture of skin.In addition, the composite powder that the composite powder of embodiment 12 is replaced by embodiment 13 or 15 prepares makeup removing oil, the result similarly, " along sliding putting on the skin open property ", " with the affinity of dirt " and " to the sense " excellence of preserving moisture of skin.
Embodiment 21
The water-in-oil type sunscreen emulsifiable paste
By following compositions and preparation method, preparation water-in-oil type sunscreen emulsifiable paste.
(composition) (%)
1. the methyl trimethoxy polysiloxane 5.0
2. vinylformic acid-siloxane treated particulate titanium dioxide (annotate 1) 5.0
3.PEG-9 polydimethyl siloxy-ethyl dimethicone (annotating 2) 0.5
4. polydimethylsiloxane (annotate 3) 2.0
5. trimethylsiloxy silicic acid/decamethylcyclopentasiloxane solution (annotate 4) 9.0
6. stearic acid inulin (annotate 5) 2.0
7. the p-methoxycinnamic acid monooctyl ester 3.0
8. diethylamino hydroxy benzoyl hexyl benzene manthanoate 0.5
9.2-thylhexoic acid cetyl 5.0
10.PEG-9 polydimethyl siloxy-ethyl dimethicone (annotating 2) 2.5
11. ethanol 10.0
12. glycerine 2.0
13. sodium-chlor 1.0
14. sanitas is an amount of
15. the composite powder 2.0 of embodiment 12
16. spices is an amount of
The surplus 17. purify waste water
Annotate 1:KF-549 (chemical industry society of SHIN-ETSU HANTOTAI system) and handle particulate titanium dioxide (median size 0.02 μ m)
Annotate 2:KF-6028 (chemical industry society of SHIN-ETSU HANTOTAI system)
Annotate 3:KF96A-2cs (chemical industry society of SHIN-ETSU HANTOTAI system)
Annotate 4:KF-7312J (chemical industry society of SHIN-ETSU HANTOTAI system)
Annotate 5:RHEOPEARL ISK (Chiba powder process society system)
(preparation method)
A: handle composition 1～3 with ball mill, disperse equably.
B: under 70 ℃,, add A then with composition 4～10 heating for dissolving, and mixed dissolution equably.
C: with composition 11～14 and composition 17 mixed dissolutions.
D: carry out emulsification on one side in B, add C on one side, cool off then.
E: added ingredients 15,16 in D, and mix equably, obtain the water-in-oil type sunscreen emulsifiable paste.
" along sliding putting on the skin the open property " of the water-in-oil type sunscreen emulsifiable paste that obtains, " with the adaptation of skin " and " to the sense of preserving moisture of skin " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 12 of embodiment 13 or 15 to prepare the water-in-oil type sunscreen emulsifiable paste, similarly " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the sense of preserving moisture of skin " excellence.
Embodiment 22
Double zone lotion
By following compositions and preparation method, the preparation double zone lotion.
(composition) (%)
1.POE alkyl oxide (8 moles) phosphoric acid 0.1
2. purify waste water 2.5
3. zinc oxide 0.1
4. the composite powder 0.5 of embodiment 12
5. aluminum chloride 0.4
6. the surplus of purifying waste water
7. ethanol 2.0
8. the Unimac 5680 polyoxyethylene hydrogenated castor oil 0.1
9. isopropyl methyl phenol 0.1
10. sanitas is an amount of
11. ethanol 18.0
12. Trisodium Citrate 0.5
13. purify waste water 10.0
(preparation method)
A. composition 5～7 is mixed equably.
B. composition 1～4 is mixed, be dispersed among the A.
C. after composition 8～13 being mixed, uniform mixing obtains double zone lotion in B.
" along sliding putting on the skin the open property " of the double zone lotion that obtains, " with the adaptation of skin " and " to the sense of preserving moisture of skin " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 12 of embodiment 13 or 15 to prepare double zone lotion, similarly " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the sense of preserving moisture of skin " excellence.
Embodiment 23
Liquid detergent
By following compositions and preparation method, the preparation liquid detergent.
(composition) (%)
1. the fatty acid distribution of coconut oil trolamine 10.0
2. fatty acid distribution of coconut oil potassium 5.0
3. the fatty acid distribution of coconut oil amido propyl betaine 5.0
4.2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazole trimethyl-glycine 3.0
5. the fatty acid distribution of coconut oil diglycollic amide 3.0
6. ethylene glycol monostearate 3.0
7. squalane 0.5
8. xanthan gum 0.1
9. Natvosol 0.1
10. Poise C-80M 0.1
11. the composite powder 0.5 of embodiment 12
The surplus 12. purify waste water
13. sanitas is an amount of
(preparation method)
A. after under 70 ℃ composition 6～8 being mixed equably, the part of added ingredients 12 is carried out emulsification.Then, be cooled to room temperature.
B. the remainder with composition 1～5 and composition 12 mixes equably.
C. in B, add A, mix equably.
D. in C, add composition 9,10, mix equably.
E. added ingredients 11,13 in D mixes equably, obtains liquid clean agent.
" along sliding putting on the skin the open property " of liquid clean the agent that obtains, " with the affinity of dirt " and " to the sense of preserving moisture of skin " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 12 of embodiment 13 or 15 to prepare liquid clean agent, similarly " along sliding putting on the skin open property ", " with the affinity of dirt " and " to the sense of preserving moisture of skin " excellence.
Embodiment 24
The oil-in-water type emulsion foundation cream
By following compositions and preparation method, preparation oil-in-water type emulsion foundation cream.
(composition) (%)
1. stearic acid 0.5
2. hexadecanol 1.0
3. polyoxyethylene (20 moles) dehydrated sorbitol mono-fatty acid ester 0.8
4. NOFABLE SO-992 0.4
5.2-thylhexoic acid cetyl 5.0
6. whiteruss 5.0
7. the composite powder 3.0 of embodiment 12
8. glycerine 3.0
9.1,3-butyleneglycol 5.0
10. the alkyl-modified carboxyl group vinyl polymer 0.1
11. alkyl acrylate copolymer 1.0
12. trolamine 0.5
13. sanitas is an amount of
The surplus 14. purify waste water
15. fluorine cpd are handled titanium oxide 4.0
16. fluorine cpd handle sliding 1.0
17. fluorine cpd are handled red iron oxide 0.5
18. fluorine cpd are handled iron oxide yellow 1.5
19. fluorine cpd are handled iron oxide black 0.1
(preparation method)
A: add composition 1～3 and composition 5,6, heating mixes equably under 75 ℃.
B: mixing element 15～19 in composition 4,8,9, use the triple-roller mill homodisperse.
C: add composition 10～14 in B, heating mixes equably under 75 ℃.
D: in C, add A, carry out emulsification.
E: after the D cooling, added ingredients 7 obtains the oil-in-water type emulsion foundation cream.
" along sliding putting on the skin the open property " of the oil-in-water type emulsion foundation cream that obtains, " with the adaptation of skin " and " to the sense of preserving moisture of skin " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 12 of embodiment 13 or 15 to prepare the oil-in-water type emulsion foundation cream, similarly " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the sense of preserving moisture of skin " excellence.
Embodiment 25
Non-water system Mascara
By following compositions and preparation method, prepare non-water system Mascara.
(composition) (%)
1. pentaerythritol abietate 10.0
2. the gama wax resin 2.0
3. the Palmiticacid dextrin ester 3.0
4. ceresin 4.0
5. beeswax 3.0
6. soybean phospholipid 0.5
7. light isoparaffins surplus
8. trimethylsiloxy silicic acid 2.0
9. dimethyl distearyl ammonium hectorite 3.0
10. propylene glycol carbonate 1.0
11. light liquid isoparaffin 30.0
12. fluorine cpd are handled iron oxide black 5.0
13. fluorine cpd handle sliding 10.0
14. the composite powder 2.0 of embodiment 12
(preparation method)
A: under 110 ℃ with composition 1～8 heating for dissolving equably.
B:, obtain oil-base gel with composition 9～11 homodisperse.
C: in A, add B, mix equably.
D: in C, add composition 12,13, mix equably.
E: D is handled with triple-roller mill.
F: in E, add composition 14, mix equably.
G: F is filled in the container, obtains non-water system Mascara.
The non-water system Mascara that obtains " along sliding putting on the skin open property ", " with the adaptation of eyelashes " and " flexibilities of eyelashes " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 12 of embodiment 13 or 15 to prepare non-water system Mascara, similarly " along sliding putting on the skin open property ", " with the adaptation of eyelashes " and " flexibilities of eyelashes " excellence.
Embodiment 26
The preparation that powder is closed in cladding in the squalane:
In silanol group density is 60 μ mol/m 215% concentration aqueous solvent colloidal suspended substance (SUNLOVELY-LFS-C of flakey silicon-dioxide; AGC Si-Tech Co., Ltd. produces) in 70 mass parts, disperse squalane 30 mass parts with dispersion mill, form slurries.This slurries use had spray-drier (the L-8 type of disc atomizer; Great river former chemical industry machine society system), be that 30000rpm, flow are that 50ml/min, temperature in are set under the condition that 200 ℃, temperature out are set at 135～140 ℃ and carry out spraying drying at the atomizer rotating speed as spraying plant.
The bag rate is measured by calcination loss in the squalane of the composite powder that obtains, and the result is 62%.In addition, the compressive strength of the composite powder that obtains is measured by the slight compression trier, and the result is 0.36MPa.Further, the median size that records composite powder by laser class dry type particle size distribution device (PRO7000S that SEISHIN ENTERPRISE Co., LTD produce) is 22 μ m.
Embodiment 27
The preparation that powder is closed in cladding in the 2 ethyl hexanoic acid glyceryl ester:
With silanol group density 60 μ mol/m 2The flakey silicon-dioxide colloid that is dispersed in 15% concentration that obtains in purifying waste water disperse in thing 70 mass parts, disperse 2 ethyl hexanoic acid glyceryl ester 29.8 mass parts and be dissolved in wherein natural VE 0.1 mass parts and Potenlini stearyl ester 0.1 weight part with dispersion mill.The spray-drier that its use is had disc atomizer carries out spraying drying as spraying plant under the condition of embodiment 26 records.
Try to achieve by the calcination loss of the composite powder that obtains that the bag rate is 71% in the 2 ethyl hexanoic acid glyceryl ester of composite powder.In addition, the median size that records composite powder by laser class dry type particle size distribution device (PRO7000S that SEISHINENTERPRISE Co., LTD produce) is 20 μ m.
Embodiment 28
The preparation that powder is closed in cladding in N-lauroyl-L-L-glutamic acid two (plant steroid base (phytosteryl) the 2-octyl group dodecyl) ester:
With silanol group density 60 μ mol/m 2The flakey silicon-dioxide colloid that is dispersed in 15% concentration that obtains in purifying waste water disperse in thing 80 mass parts, disperse N-lauroyl-L-L-glutamic acid two (plant steroid base 2-octyl group dodecyl) ester 20 mass parts with dispersion mill as wetting Agent for Printing Inks.The spray-drier that its use is had disc atomizer carries out spraying drying as spraying plant under the condition of embodiment 25 records, obtain composite powder.
The interior bag rate of being tried to achieve N-lauroyl-L-L-glutamic acid two (plant steroid base 2-octyl group dodecyl) ester of composite powder by the calcination loss of the composite powder that obtains is 64%.In addition, the median size that records composite powder by laser class dry type particle size distribution device (PRO7000S that SEISHIN ENTERPRISE Co., LTD produce) is 27 μ m.
Embodiment 29
The preparation that powder is closed in cladding in the p-methoxycinnamic acid 2-ethylhexyl:
With silanol group density 60 μ mol/m 2The flakey silicon-dioxide colloid that is dispersed in 15% concentration that obtains in purifying waste water disperse to disperse oil-soluble UV light absorber p-methoxycinnamic acid 2-ethylhexyl 10 mass parts with dispersion mill in thing 90 mass parts.The spray-drier that its use is had disc atomizer is as spraying plant, and spraying drying under the condition of embodiment 26 records obtains composite powder.
Try to achieve by the calcination loss of the composite powder that obtains that the bag rate is 41% in the p-methoxycinnamic acid 2-ethylhexyl of composite powder.In addition, the median size that records composite powder by laser class dry type particle size distribution device (PRO7000S that SEISHIN ENTERPRISE Co., LTD produce) is 19 μ m.
Comparative example 5
The relatively preparation of composite powder:
With silanol group density 8.0 μ mol/m 2, particle diameter is that the colloid that the spherical silicon dioxide of 12 μ m is dispersed in 15% concentration that obtains in purifying waste water disperses to disperse squalane 5.0 mass parts equably with dispersion mill in thing 95 mass parts.The spray-drier that its use is had disc atomizer carries out spraying drying as spraying plant under the condition of embodiment 26 records, obtain composite powder.
Try to achieve by the calcination loss of the composite powder that obtains that the bag rate is 16% in the squalane of composite powder.In addition, observe this comparison composite powder with scanning electron microscope, the result as can be known, only the form with the aggregate of the part of spherical particle cohesion exists, and can not form the granulation particle as embodiment.
So using silanol group density is 8.0 μ mol/m 2Spherical silicon dioxide the time, the interior bag rate of squalane can not reach more than 16%.This be because, when utilizing particle diameter to be the spherical silicon dioxide of 12 μ m, do not form the granulation particle, squalane is not by Nei Bao and on the inboard wall of tube body face attached to drying installation, composite powder that forms and the cohesion of this squalane that adheres to can not be reclaimed composite powder effectively.Hence one can see that, and when silanol group density was hanged down, no matter the shape of silicon-dioxide how, the interior bag rate of water insoluble active ingredient was all low.
Comparative example 6
The relatively preparation of composite powder:
With silanol group density 7.0 μ mol/m 2, particle diameter is that the flakey silicon-dioxide of 25 μ m is dispersed in 15% colloid that obtains in purifying waste water and disperses to disperse squalane 5.0 mass parts equably with dispersion mill in thing 95 mass parts.The spray-drier that its use is had disc atomizer is as spraying plant, spraying drying under the condition of embodiment 26 records.
Try to achieve by the calcination loss of the composite powder that obtains that the bag rate is 14% in the squalane of composite powder.In addition, observe this comparison composite powder with scanning electron microscope, the result as can be known, only the form with the aggregate of the part of above-mentioned flakey silicon-dioxide cohesion exists, and can not form the granulation particle as embodiment.Specifically, be 7.0 μ mol/m in above-mentioned silanol group density 2Situation under, the interior bag rate of squalane can not reach more than 14%.This be because, squalane does not wrap in the flakey silicon-dioxide that particle diameter is 25 μ m in fully, and on the inboard wall of tube body face attached to drying installation, the squalane that the composite powder of formation and this adhere to condenses, and can not reclaim composite powder effectively.Hence one can see that, when silanol group density is hanged down, even be that flakey, interior bag rate are also low.
Embodiment 30
Solid powdery foundation cream (do and use special use):
Prepare solid powdery foundation cream (do and use special use) by composition shown in the table 3 and following preparation method.For this solid powdery foundation cream,, its " along sliding putting on the skin open property ", " with the adaptation of skin ", " to the skin moisten sense of skin " and " agglomeration resistance effect " are estimated according to evaluation method shown below and judgment standard.Its result is as shown in table 3.
[table 3]
(％)
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～15 is disperseed equably.
B. composition 16～19 is mixed equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains solid powdery foundation cream (do and use special use).
(evaluation method)
For " along sliding putting on the skin open property ", " with the adaptation of skin ", " to the skin moisten sense of skin ", the member of cosmetic evaluation professional group 20 people use above-mentioned thing of the present invention and compare the solid powdery foundation cream of thing (do and use special use), according to following metewand each sample is carried out the evaluation of 7 grades separately for projects, and scoring.Further try to achieve the average mark of whole group members' scoring, judge according to following judgment standard.And " to the skin moisten sense of skin " is each member of professional group carries out the skin moisten sense after the common life in 3 hours after skin moisten sense after the coating just and coating comprehensive evaluation.
Metewand:
(evaluation) (content)
6: very good
5: good
4: good slightly
3: common
2: poor slightly
1: poor
0: non-constant
Judgment standard:
(average mark of scoring) (evaluation)
5.0 more than: ◎ (very good)
3.5 it is above and less than 5.0: zero (well)
1.0 it is above and: △ (common) less than 3.5
Less than 1.0: * (bad)
For " agglomeration resistance effect ", prepare 5 of the powder foundation creams of the foregoing description and comparative example respectively, under the state in being filled into the metal ware, use the powder foundation cream with filling up (material N BR), observe the condition of surface of embrocating continuously after its surperficial 80 times, each foundation cream according to following metewand scoring, is calculated the average mark of the scoring of each sample, judge according to the judgment standard of following 4 grades.
Metewand:
(evaluation) (content)
3: no change
2: have the rough of surface, but usability is no problem.
1: have the rough of significant surface, the usability existing problems.
Judgment standard:
(average mark of scoring) (evaluation)
2.5 more than: ◎
2.0 above～less than 2.5: zero
1.5 above～less than 2.0: △
Less than 1.5: *
As shown in Table 3, the solid powdery foundation cream of thing 6～9 of the present invention is all excellent in " along sliding putting on the skin open property ", " with the adaptation of skin ", " to the skin moisten sense of skin " and " agglomeration resistance effect " whole projects.
On the other hand, do not cooperate the powder foundation cream of the comparison thing 7 of composite powder, along sliding putting on the skin open property, with the adaptation of skin, skin moisten sense to skin in all poor.In addition, be combined with the powder foundation cream of comparison thing 8 of the composite powder of comparative example 5, along sliding putting on the skin open property excellence, but with the adaptation of skin, poor to the skin moisten sense of skin.In addition, be combined with the powder foundation cream of comparison thing 9 of the composite powder of comparative example 6, along sliding putting on the skin open property excellence, but with the adaptation of skin, poor to the skin moisten sense of skin.Hinted that this is because the interior bag rate of the water insoluble active ingredient of the composite powder of comparative example 8 and 9 is few.Further, be combined with the composite powder of comparative example 6 and produce caking with the comparison thing 10 of the water-insoluble substance of thing 6 equivalent of the present invention.
Embodiment 31
The solid powdery rouge
By following compositions and preparation method, preparation solid powdery rouge.
(composition) (%)
1. mica 20.0
2. talcum surplus
3. the composite powder 10.0 of embodiment 27
4. titanium oxide lining mica 10.0
5. red No. 226 0.5
6. ultramarine 0.2
7. synthetic chloroflo powder 5.0
8. methyl p-hydroxybenzoate 0.2
9. squalane 1.0
10. spices is an amount of
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～8 is disperseed equably.
B. composition 9,10 is mixed equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains the solid powdery rouge.
The solid powdery rouge that obtains along sliding putting on the skin open property, with the adaptation of skin, whole projects to the skin moisten sense of skin and agglomeration resistance effect in all excellent.
Embodiment 32
The solid powdery eye shadow:
By following compositions and preparation method, preparation solid powdery eye shadow.
(composition) (%)
1. polydimethylsiloxane is handled synthetic phlogopite 10.0
2. polydimethylsiloxane is handled the talcum surplus
3. titanium oxide lining mica 30.0
4. boron nitride 5.0
5. polyethylene terephthalate-aluminium-epoxy laminate powder 5.0
6. the composite powder 20.0 of embodiment 28
7. ultramarine 2.0
8. yellow No. 401 0.5
9. cross-linking type siloxanes-web-like silicon siloxane copolymers 1.0
10. methyl p-hydroxybenzoate 0.2
11. whiteruss 2.0
12. Vaseline 1.0
13. polydimethylsiloxane 3.0
14. spices is an amount of
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～10 is disperseed equably.
B. composition 11～14 is disperseed equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains the solid powdery eye shadow.
The solid powdery eye shadow that obtains along sliding putting on the skin open property, with the adaptation of skin, whole projects to the skin moisten sense of skin and agglomeration resistance effect in all excellent.
Embodiment 33
Solid powdery foundation cream (water uses special-purpose):
By following compositions and preparation method, preparation solid powdery eye shadow (water uses special-purpose).
(composition) (%)
1. talcum surplus
2. mica 20.0
3. titanium oxide lining mica 2.0
4. titanium oxide 15.0
5. boron nitride 5.0
6. red iron oxide 0.8
7. iron oxide yellow 2.5
8. iron oxide black 0.3
9. the composite powder 15.0 of embodiment 29
10. methyl p-hydroxybenzoate 0.2
11. PFPE 2.0
12. polydimethylsiloxane 5.0
13. oxybenzone 3.0
14. polyoxyethylene (20 moles) dehydrated sorbitol mono-fatty acid ester 0.5
15. spices is an amount of
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～10 is disperseed equably.
B. composition 11～15 is mixed equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains solid powdery foundation cream (water uses special-purpose).
The solid powdery foundation cream that obtains (water use special-purpose) along sliding putting on the skin open property, with the adaptation of skin, whole projects to the skin moisten sense of skin and agglomeration resistance effect in all excellent.
Reference example 1
The preparation of emulsifying composition:
By following compositions and preparation method, the preparation emulsifying composition.
(composition) (%)
1. phosphatide-cholesterol mixture * 12.0
2.1,3-butyleneglycol 10.0
3. glycerine 10.0
4. squalane 10.0
5. purify waste water 68.0
*1:COMPOSITE-PC (Japan refine society's system)
(preparation method)
A. under 70 ℃, composition 1～3 is disperseed equably with dispersion machine.
B. under 70 ℃, in A, add composition 4, mix equably.
C. under 75 ℃, in B, add composition 5 lentamente, use dispersion machine emulsification, obtain emulsifying composition.
Reference example 2
The preparation of emulsifying composition:
By following compositions and preparation method, the preparation emulsifying composition.
(composition) (%)
1.N-stearyl--N methyl taurine sodium 1.0
2. glycerine 5.0
3. purify waste water 45.5
4.1,3-butyleneglycol 15.0
5. whiteruss 20.0
6. Vaseline 10.0
7. blubber alcohol (cetostearyl alcohol) 3.0
8. polyoxyethylene sorbitan (20E.O.) monoleate 0.5
(preparation method)
A. under 70 ℃, composition 1～3 is disperseed equably with dispersion machine.
B. under 70 ℃, composition 4～8 is disperseed equably.
C. under 75 ℃, in A, add B lentamente, use dispersion machine emulsification, obtain emulsifying composition.
Reference example 3
The preparation of emulsifying composition:
By following compositions and preparation method, the preparation emulsifying composition.
(composition) (%)
1. stearic acid 2.5
2. V-1326 0.5
3. blubber alcohol 0.5
4. p-methoxycinnamic acid 2-ethylhexyl 20.0
5. three 2 ethyl hexanoic acid glyceryl ester 10.0
6. purify waste water 55.5
7. trolamine 1.0
8.1,3-butyleneglycol 5.0
9. dipropylene glycol 5.0
(preparation method)
A. under 70 ℃, composition 1～5 is disperseed equably.
B. under 70 ℃, composition 6～9 is disperseed equably.
C. under 75 ℃, in A, add B lentamente, use dispersion machine emulsification, obtain emulsifying composition.
Embodiment 34
The preparation of composite powder:
To being 60 μ mol/m with silanol group density 2Flakey silicon-dioxide be dispersed in 15% colloid that obtains in purifying waste water and disperse to add emulsifying composition 60 mass parts that obtain in the reference example 1 in thing 40 mass parts, disperse equably with dispersion mill.The spray-drier that its use is had disc atomizer carries out spraying drying as spraying plant under embodiment 26 record conditions.
The interior bag rate of the emulsifying composition of the reference example 1 that contains in this particle of being tried to achieve by the calcination loss of the composite powder that obtains is 59%.When in addition, recording the median size of composite powder by laser class dry type particle size distribution device (PRO7000S that SEISHIN ENTERPRISE Co., LTD produce) is 20 μ m.And in following embodiment, the comparative example, interior bag rate refers to the interior bag rate of removing the composition that the water system composition below 100 ℃ obtains in the composition that constitutes emulsifying composition.
Embodiment 35
The preparation of composite powder:
With silanol group density 60 μ mol/m 2Flakey silicon-dioxide be dispersed in 15% colloid that obtains in purifying waste water and disperse in thing 50 mass parts, disperse emulsifying composition 50 mass parts that obtain in the reference example 2 with dispersion mill.The spray-drier that its use is had disc atomizer is as spraying plant, spraying drying under the condition of embodiment 26 records.
The interior bag rate of being tried to achieve the emulsifying composition of the reference example 2 that contains in this particle by the calcination loss of the composite powder that obtains is 50%.In addition, the compressive strength of the composite powder of the gained that records by the slight compression trier is 0.30MPa.Further, the median size that records composite powder by laser class dry type particle size distribution device (PRO7000S that SEISHIN ENTERPRISE Co., LTD produce) is 18 μ m.
Embodiment 36
The preparation of composite powder:
With silanol group density 60 μ mol/m 2Flakey silicon-dioxide be dispersed in 15% colloid that obtains in purifying waste water and disperse in thing 60 mass parts, disperse emulsifying composition 40 mass parts that obtain in the reference example 3 equably with dispersion mill.The spray-drier that its use is had disc atomizer is as spraying plant, spraying drying under the condition of embodiment 26 records.
The interior bag rate of being tried to achieve the emulsifying composition of the reference example 3 that contains in this particle by the calcination loss of the composite powder that obtains is 43%.In addition, the median size that records composite powder by laser class dry type particle size distribution device (PRO7000S that SEISHIN ENTERPRISE Co., LTD produce) is 19 μ m.
Comparative example 7
The relatively preparation of composite powder:
With silanol group density 8.0 μ mol/m 2, particle diameter is that the spherical silicon dioxide of 12 μ m is dispersed in and obtains 15% concentration colloid in purifying waste water and disperse in thing 90 mass parts emulsifying composition 10 mass parts of disperseing reference example 1 with dispersion mill equably.The spray-drier that its use is had disc atomizer is as spraying plant, spraying drying under the condition of embodiment 26 records.
The interior bag rate of being tried to achieve the emulsifying composition of the reference example 1 that contains in the spherical silicon dioxide particle by the calcination loss of the composite powder that obtains is 8.0%.In addition, by laser class dry type particle size distribution device as can be known, only the form with the aggregate of the part cohesion of the spherical particle of 12 μ m exists, and can not form the granulation particle as embodiment.Specifically, above-mentioned silanol group density is 8.0 μ mol/m 2The time, the interior bag rate of the emulsifying composition of reference example 1 can not reach more than 8.0%.This be because, the emulsifying composition of reference example 1 does not wrap in the spherical silicon dioxide that particle diameter is 12 μ m in fully, and on the inboard wall of tube body face attached to drying installation, the cohesion of the emulsifying composition of the reference example 1 that the composite powder of formation and this adhere to can not be reclaimed composite powder effectively.Hence one can see that, and when silanol group density was hanged down, no matter the shape of silicon-dioxide how, interior bag rate was low.
Comparative example 8
The relatively preparation of composite powder:
With silanol group density 7.0 μ mol/m 2, particle diameter is that the flakey silicon-dioxide of 25 μ m is dispersed in 15% colloid that obtains in purifying waste water and disperses in thing 90 mass parts emulsifying composition 10 mass parts of disperseing reference example 1 with dispersion mill equably.The spray-drier that its use is had disc atomizer is as spraying plant, spraying drying under the condition of embodiment 26 records.
The interior bag rate of being tried to achieve the emulsifying composition of the reference example 1 that contains in this powder by the calcination loss of the composite powder that obtains is 7.0%.In addition, by laser class dry type particle size distribution device as can be known, only the form with the aggregate of the part cohesion of the laminar silicon-dioxide of 25 μ m exists, and can not form the granulation particle as embodiment.Specifically, above-mentioned silanol group density is 7.0 μ mol/m 2The time, the interior bag rate of the emulsifying composition of reference example 1 can not reach more than 7.0%.This be because, the emulsifying composition of reference example 1 does not wrap in the flakey silicon-dioxide that particle diameter is 25 μ m in fully, and on the inboard wall of tube body face attached to drying installation, the cohesion of the emulsifying composition of the reference example 1 that the composite powder of formation and this adhere to can not be reclaimed composite powder effectively.Hence one can see that, when silanol group density is hanged down, even be that flakey, interior bag rate are also low.
Embodiment 37
Solid powdery foundation cream (do and use special use):
Prepare solid powdery foundation cream (do and use special use) by composition shown in the table 4 and following preparation method.For this solid powdery foundation cream,, its " along sliding putting on the skin open property ", " with the adaptation of skin ", " to the skin moisten sense of skin " and " agglomeration resistance effect " are estimated according to evaluation method shown below and judgment standard.Its result is as shown in table 4.
[table 4]
(％)
Figure G2008800110220D00531
Figure G2008800110220D00541
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～15 is disperseed equably.
B. composition 16～23 is mixed equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains solid powdery foundation cream (do and use special use).
(evaluation method)
Similarly to Example 30, use thing of the present invention and the solid powdery foundation cream that compares thing (do and use special use), " suitable putting on the skin the open property of sliding ", " with the adaptation of skin ", " to the skin moisten sense of skin " and " agglomeration resistance effect " are estimated.
As shown in Table 4, the solid powdery foundation cream of thing 10～13 of the present invention is all excellent in along sliding putting on the skin open property, with the adaptation of skin, to the skin moisten sense of skin and the whole projects of agglomeration resistance effect.
On the other hand, do not cooperate the powder foundation cream of the comparison thing 11 of composite powder, along sliding putting on the skin open property, with the adaptation of skin, skin moisten sense to skin in all poor.In addition, be combined with the powder foundation cream of comparison thing 12 of the composite powder of comparative example 7, along sliding putting on the skin open property excellence, but with the adaptation of skin, poor to the skin moisten sense of skin.In addition, be combined with the powder foundation cream of comparison thing 13 of the composite powder of comparative example 8, along sliding putting on the skin open property excellence, but adaptation, skin moisten sense are poor.Hinted that this is owing to the interior bag rate of water insoluble active ingredient in the composite powder of comparative example 7 and 8 is few.Further, be combined with the composite powder of comparative example 8 and produce caking with the comparison thing 14 of the water-insoluble substance of thing 10 equivalent of the present invention.
Embodiment 38
The solid powdery rouge
By following compositions and preparation method, preparation solid powdery rouge.
(composition) (%)
1. mica 20.0
2. talcum surplus
3. the composite powder 10.0 of embodiment 35
4. titanium oxide lining mica 10.0
5. red No. 226 0.5
6. ultramarine 0.2
7. synthetic chloroflo powder 5.0
8. methyl p-hydroxybenzoate 0.2
9. squalane 1.0
10. spices is an amount of
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～8 is disperseed equably.
B. composition 9,10 is mixed equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains the solid powdery rouge.
The solid powdery rouge that obtains along sliding putting on the skin open property, with the adaptation of skin, whole projects to the skin moisten sense of skin and agglomeration resistance effect in all excellent.
Embodiment 39
The solid powdery eye shadow:
By following compositions and preparation method, preparation solid powdery eye shadow.
(composition) (%)
1. polydimethylsiloxane is handled synthetic phlogopite 10.0
2. polydimethylsiloxane is handled the talcum surplus
3. titanium oxide lining mica 30.0
4. boron nitride 5.0
5. polyethylene terephthalate-aluminium-epoxy laminate powder 5.0
6. the composite powder 20.0 of embodiment 36
7. ultramarine 2.0
8. yellow No. 401 0.5
9. cross-linking type siloxanes-web-like silicon siloxane copolymers 1.0
10. methyl p-hydroxybenzoate 0.2
11. whiteruss 2.0
12. Vaseline 1.0
13. polydimethylsiloxane 3.0
14. spices is an amount of
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～10 is disperseed equably.
B. with composition 11～14 heating and dispersion equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains the solid powdery eye shadow.
The solid powdery eye shadow that obtains along sliding putting on the skin open property, with the adaptation of skin, whole projects to the skin moisten sense of skin and agglomeration resistance effect in all excellent.
Embodiment 40
Solid powdery foundation cream (water uses special-purpose):
By following compositions and preparation method, preparation solid powdery eye shadow (water uses special-purpose).
(composition) (%)
1. talcum surplus
2. mica 20.0
3. titanium oxide lining mica 2.0
4. titanium oxide 15.0
5. boron nitride 5.0
6. red iron oxide 0.8
7. iron oxide yellow 2.5
8. iron oxide black 0.3
9. the composite powder 15.0 of embodiment 37
10. methyl p-hydroxybenzoate 0.2
11. PFPE 2.0
12. polydimethylsiloxane 5.0
13. oxybenzone 3.0
14. polyoxyethylene (20 moles) dehydrated sorbitol mono-fatty acid ester 0.5
15. spices is an amount of
(preparation method)
A. use Henschel mixer (Mitsui three Chi She systems) that composition 1～10 is disperseed equably.
B. composition 11～15 is mixed equably.
C. stir A with Henschel mixer on one side and add B on one side, and homodisperse.
D. pulverize C with pulverizer.
E. D is filled in the metal ware, compressed moulding obtains solid powdery foundation cream (water uses special-purpose).
The solid powdery foundation cream that obtains (water use special-purpose) along sliding putting on the skin open property, with the adaptation of skin, whole projects to the skin moisten sense of skin and agglomeration resistance effect in all excellent.
Embodiment 41
Makeup removing oil
By following compositions and preparation method, preparation makeup removing oil.
(composition) (%)
1. Rice pollard oil 35.0
2. whiteruss surplus
3. three-2 ethyl hexanoic acid glyceryl ester 10.0
4. methyl phenyl silicone 5.0
5. four oleic acid POE (30) sorbitol esters 9.0
6. phenoxyethyl alcohol 0.8
7. Semen Coicis oil 0.1
8. Thistle oil 0.1
9. natural VE 0.1
10. spices is an amount of
11. the composite powder 1.0 of embodiment 26
(preparation method)
A. composition 1～10 is mixed equably.
B. in A, add composition 11 lentamente, mix equably, obtain makeup removing oil thus.
" along sliding putting on the skin the open property " of the makeup removing oil that obtains, " with the affinity of dirt " and " to the skin moisten sense of skin " excellence.In addition, use the composite powder of the composite powder alternate embodiment 26 of embodiment 27,28,34,35 or 36 to prepare when removing ornaments and formal dress oil, similarly " along sliding putting on the skin open property ", " with the affinity of dirt " and " to the skin moisten sense of skin " excellence.
Embodiment 42
The water-in-oil type sunscreen emulsifiable paste
By following compositions and preparation method, preparation water-in-oil type sunscreen emulsifiable paste.
(composition) (%)
1. the methyl trimethoxy polysiloxane 5.0
2. vinylformic acid-siloxane treated particulate titanium dioxide (annotate 1) 5.0
3.PEG-9 polydimethyl siloxy-ethyl dimethicone (annotating 2) 0.5
4. polydimethylsiloxane (annotate 3) 2.0
5. trimethylsiloxy silicic acid/decamethylcyclopentasiloxane solution (annotate 4) 9.0
6. stearic acid inulin (annotate 5) 2.0
7. the p-methoxycinnamic acid monooctyl ester 3.0
8. diethylamino hydroxy benzoyl hexyl benzene manthanoate 0.5
9.2-thylhexoic acid cetyl 5.0
10.PEG-9 polydimethyl siloxy-ethyl dimethicone (annotating 2) 2.5
11. ethanol 10.0
12. glycerine 2.0
13. sodium-chlor 1.0
14. sanitas is an amount of
15. the composite powder 2.0 of embodiment 26
16. spices is an amount of
The surplus 17. purify waste water
Annotate 1:KF-549 (chemical industry society of SHIN-ETSU HANTOTAI system) and handle particulate titanium dioxide (median size 0.02 μ m)
Annotate 2:KF-6028 (chemical industry society of SHIN-ETSU HANTOTAI system)
Annotate 3:KF96A-2cs (chemical industry society of SHIN-ETSU HANTOTAI system)
Annotate 4:KF-7312J (chemical industry society of SHIN-ETSU HANTOTAI system)
Annotate 5:RHEOPEARL ISK (Chiba powder process society system)
(preparation method)
A. handle composition 1～3 with ball mill, disperse equably.
B. at 70 ℃ of following heating for dissolving compositions 4～10, add A, and mixed dissolution equably.
C. with composition 11～14 and composition 17 mixed dissolutions.
Carry out emulsification when D. in B, adding C, cool off then.
E. added ingredients 15,16 in D, and mix equably, the water-in-oil type sunscreen emulsifiable paste obtained.
" along sliding putting on the skin the open property " of the water-in-oil type sunscreen emulsifiable paste that obtains, " with the adaptation of skin " and " to the skin moisten sense of skin " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 26 of embodiment 27,28,29,34,35 or 36 to prepare the water-in-oil type sunscreen emulsifiable paste, similarly, " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the skin moisten sense of skin " excellence.It is long particularly to use the sun-proof result of the water-in-oil type sunscreen emulsifiable paste that the composite powder of embodiment 29 and 36 obtains to continue, and it is few to be clamminess.
Embodiment 43
Double zone lotion
By following compositions and preparation method, the preparation double zone lotion.
(composition) (%)
1.POE alkyl oxide (8 moles) phosphoric acid 0.1
2. purify waste water 2.5
3. zinc oxide 0.1
4. the composite powder 0.5 of embodiment 26
5. aluminum chloride 0.4
6. the surplus of purifying waste water
7. ethanol 2.0
8. the Unimac 5680 polyoxyethylene hydrogenated castor oil 0.1
9. isopropyl methyl phenol 0.1
10. sanitas is an amount of
11. ethanol 18.0
12. Trisodium Citrate 0.5
13. purify waste water 10.0
(preparation method)
A. composition 5～7 is mixed equably.
B. composition 1～4 is mixed, be dispersed among the A.
C. after composition 8～13 being mixed, uniform mixing obtains double zone lotion in B.
" along sliding putting on the skin the open property " of the double zone lotion that obtains, " with the adaptation of skin " and " to the skin moisten sense of skin " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 26 of embodiment 27,28,29,34,35 or 36 to prepare double zone lotion, similarly " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the skin moisten sense of skin " excellence.
Embodiment 44
Liquid detergent
By following compositions and preparation method, the preparation liquid detergent.
(composition) (%)
1. the fatty acid distribution of coconut oil trolamine 10.0
2. fatty acid distribution of coconut oil potassium 5.0
3. the fatty acid distribution of coconut oil amido propyl betaine 5.0
4.2-alkyl-N-carboxymethyl-N-hydroxyethyl imidazole trimethyl-glycine 3.0
5. the fatty acid distribution of coconut oil diglycollic amide 3.0
6. ethylene glycol monostearate 3.0
7. squalane 0.5
8. xanthan gum 0.1
9. Natvosol 0.1
10. Poise C-80M 0.1
11. the composite powder 0.5 of embodiment 26
The surplus 12. purify waste water
13. sanitas is an amount of
(preparation method)
A. after under 70 ℃ composition 6～8 being mixed equably, the part of added ingredients 12 is carried out emulsification.Then, be cooled to room temperature.
B. the remainder with composition 1～5 and composition 12 mixes equably.
C. in B, add A, mix equably.
D. in C, add composition 9,10, mix equably.
E. added ingredients 11,13 in D mixes equably, obtains liquid clean agent.
" along sliding putting on the skin the open property " of liquid clean the agent that obtains, " with the affinity of dirt " and " to the skin moisten sense of skin " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 26 of embodiment 27,28,34,35 or 36 to prepare liquid clean agent, similarly " along sliding putting on the skin open property ", " with the affinity of dirt " and " to the skin moisten sense of skin " excellence.
Embodiment 45
The oil-in-water type emulsion foundation cream
By following compositions and preparation method, preparation oil-in-water type emulsion foundation cream.
(composition) (%)
1. stearic acid 0.5
2. hexadecanol 1.0
3. polyoxyethylene (20 moles) dehydrated sorbitol mono-fatty acid ester 0.8
4. NOFABLE SO-992 0.4
5.2-thylhexoic acid cetyl 5.0
6. whiteruss 5.0
7. the composite powder 3.0 of embodiment 26
8. glycerine 3.0
9.1,3-butyleneglycol 5.0
10. the alkyl-modified carboxyl group vinyl polymer 0.1
11. alkyl acrylate copolymer 1.0
12. trolamine 0.5
13. sanitas is an amount of
The surplus 14. purify waste water
15. fluorine cpd are handled titanium oxide 4.0
16. fluorine cpd are handled talcum 1.0
17. fluorine cpd are handled red iron oxide 0.5
18. fluorine cpd are handled iron oxide yellow 1.5
19. fluorine cpd are handled iron oxide black 0.1
(preparation method)
A: add composition 1～3 and composition 5,6, heating mixes equably under 75 ℃.
B: mixing element 15～19 in composition 4,8,9, use the triple-roller mill homodisperse.
C: add composition 10～14 in B, heating mixes equably under 75 ℃.
D: in C, add A, carry out emulsification.
E: after the D cooling, added ingredients 7 obtains the oil-in-water type emulsion foundation cream.
" along sliding putting on the skin the open property " of the oil-in-water type emulsion foundation cream that obtains, " with the adaptation of skin " and " to the skin moisten sense of skin " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 26 of embodiment 27,28,29,34,35 or 36 to prepare the oil-in-water type emulsion foundation cream, similarly " along sliding putting on the skin open property ", " with the adaptation of skin " and " to the skin moisten sense of skin " excellence.
Embodiment 46
Non-water system Mascara
By following compositions and preparation method, prepare non-water system Mascara.
(composition) (%)
1. pentaerythritol abietate 10.0
2. the gama wax resin 2.0
3. the Palmiticacid dextrin 3.0
4. ceresin 4.0
5. beeswax 3.0
6. soybean phospholipid 0.5
7. light isoparaffins surplus
8. trimethylsiloxy silicic acid 2.0
9. dimethyl distearyl ammonium hectorite 3.0
10. propylene glycol carbonate 1.0
11. light liquid isoparaffin 30.0
12. fluorine cpd are handled iron oxide black 5.0
13. fluorine cpd are handled talcum 10.0
14. the composite powder 2.0 of embodiment 26
(preparation method)
A: under 110 ℃ with composition 1～8 heating for dissolving equably.
B:, obtain oil-base gel with composition 9～11 homodisperse.
C: in A, add B, mix equably.
D: in C, add composition 12,13, mix equably.
E: D is handled with triple-roller mill.
F: in E, add composition 14, mix equably.
G: F is filled in the container, obtains non-water system Mascara.
" along sliding putting on the skin the open property " of the non-water system Mascara that obtains, " with the adaptation of eyelashes " and " flexibilities of eyelashes " excellence.In addition, when using the composite powder of the composite powder alternate embodiment 26 of embodiment 27,28,29,34,35 or 36 to prepare non-water system Mascara, similarly " along sliding putting on the skin open property ", " to the binding property of eyelashes " and " flexibilities of eyelashes " excellence.
Industrial applicibility
The granulated silica particle of first invention among the present invention is not even use macromolecular compound Its shape is also stable in the preparation, when being coated on the skin, slowly collapses by the friction of physical property Separate, ductility is good, so as the powder composition that is engaged in cosmetics or the external used medicine etc. be Suitable.
In addition, the composite powder of second invention does not utilize the adhesive ingredients just can be steady among the present invention Bag water soluble ingredient in fixed and a large amount of. And, if it is engaged in the cosmetics, then be coated on skin In the time of on the skin, slowly disintegration discharges a large amount of active ingredient by the friction of physical property, so Can expect high cosmetic result.
In addition, this composite powder itself is engaged in the cosmetics, the ductility when being coated on the skin Well, adaptation, moisture retention excellence form excellent cosmetics.
Further, the composite powder of the 3rd invention does not utilize adhesive ingredients just can among the present invention With stable and a large amount of interior bag water insoluble active ingredients. And, if it is engaged in the cosmetics, then be coated with Cloth is on skin the time, and slowly disintegration discharges a large amount of active ingredient by the friction of physical property, So can expect high cosmetic result.
In addition, this composite powder itself is engaged in the cosmetics, the ductility when being applied on the skin Well, adaptation, moisturizing sense, agglomeration resistance effect excellence form excellent cosmetics.
For example, in the situation of powder, usually in order to show the moisturizing sense, be necessary to cooperate big gauging Agent, but at this moment owing to the cohesion that produces the particle that causes because of the crosslinked power of liquid, can not be stably Cooperate. Therewith relatively, when utilizing composite powder of the present invention, can prevent the same of particle coacervation The time give high moisturizing sense.
In addition, in the situation that contains powder phase and water system double zone lotion mutually, goods in the past In, the bad dispersibility of powder might produce caking and (be deposited in the bottom, even vibration does not have dispersion yet Invertibity). In order to eliminate this problem, usually be necessary to cooperate activating agent. But, among the present invention, Mismatch activating agent and just can cooperate composite powder, and can stably keep, so can relax The irritating problem to skin that cooperates activating agent to cause.
Description of drawings
[Fig. 1] is the electron micrograph (multiplying power is 2000 times) of the granulated silica particle that obtains among the embodiment 1.
[Fig. 2] disperses the optical microscope photograph (multiplying power is 400 times) of thing (slurries) for 10% colloid of the granulated silica particle of embodiment 1.
[Fig. 3] is the electron micrograph (multiplying power is 2000 times) of the composite powder that obtains among the embodiment 12.
[Fig. 4] is the electron micrograph (multiplying power is 2000 times) of the comparison composite powder that obtains in the comparative example 4.
[Fig. 5] is the electron micrograph (multiplying power is 2000 times) of the composite powder that obtains among the embodiment 26.
[Fig. 6] is the electron micrograph (multiplying power is 2000 times) of the composite powder that obtains among the embodiment 34.
[Fig. 7] for representing the electron micrograph (multiplying power is 2000 times) of the state that composite powder splits, the composite powder of a part that hence one can see that is a hollow structure.

Claims (26)

1. granulated silica particle is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide form as integrant, median size is that 1～50 μ m, compressive strength are 1～4MPa.
2. granulated silica particle as claimed in claim 1, wherein, the average aggregate particle size of flakey silicon-dioxide is 0.05～5 μ m, its thickness is more than 10 with the aspect ratio of long particle diameter.
3. granulated silica particle as claimed in claim 1 or 2 is to be that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m by the thickness with primary particle 2Flakey silicon-dioxide be dispersed in the aqueous solvent form slurries after, these slurries are carried out with spray-drier spraying drying obtains.
4. the preparation method of granulated silica particle is characterized in that, is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide be dispersed in the aqueous solvent form slurries after, these slurries are carried out spraying drying with spray-drier.
5. makeup contain any described granulated silica particle in the claim 1～3.
6. composite powder is characterized in that, is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m at the thickness with primary particle 2The granulated silica particle that forms as integrant of flakey silicon-dioxide in be surrounded by water soluble component.
7. composite powder as claimed in claim 6, wherein, the average aggregate particle size of flakey silicon-dioxide is 0.05～5 μ m, its thickness is more than 10 with the aspect ratio of long particle diameter.
8. as claim 6 or 7 described composite powders, wherein, median size is 1～50 μ m.
9. as any described composite powder in the claim 6～8, wherein, compressive strength is 0.2～3MPa.
10. as any described composite powder in the claim 6～9, wherein, contain 5～25% water soluble component in the composite powder.
11. as any described composite powder in the claim 6～10, wherein, water soluble component is a polyvalent alcohol.
12., be to be that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m by thickness with primary particle as any described composite powder in the claim 6～11 2Flakey silicon-dioxide be dispersed in the aqueous solvent that contains water soluble component form slurries after, these slurries are carried out with spray-drier spraying drying obtains.
13. the preparation method of composite powder is characterized in that, is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide be dispersed in the aqueous solvent that contains water soluble component form slurries after, these slurries are carried out spraying drying with spray-drier.
14. makeup contain any described composite powder in the claim 6～12.
15. composite powder is characterized in that, is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m at the thickness with primary particle 2The granulated silica particle that forms as integrant of flakey silicon-dioxide in be surrounded by water insoluble active ingredient.
16. composite powder as claimed in claim 15, wherein, the average aggregate particle size of flakey silicon-dioxide is 0.05～5 μ m, and its thickness is more than 10 with the aspect ratio of long particle diameter.
17. as claim 15 or 16 described composite powders, wherein, median size is 1～50 μ m.
18. as any described composite powder in the claim 15～17, wherein, compressive strength is 0.1～3MPa.
19., wherein, contain 5～75% water insoluble active ingredient in the composite powder as any described composite powder in the claim 15～18.
20., be to be that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m by thickness with primary particle as any described composite powder in the claim 15～19 2Flakey silicon-dioxide join form slurries in the aqueous solvent of disperse water insoluble composition after, these slurries are carried out with spray-drier spraying drying obtains.
21. as any described composite powder in the claim 15～20, wherein, water insoluble active ingredient is the oiliness composition.
22., be that thickness with primary particle is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m as any described composite powder in the claim 15～21 2Flakey silicon-dioxide join with after forming slurries in the aqueous solvent of the form disperse water insoluble composition of emulsifying composition, these slurries are carried out with spray-drier spraying drying obtains.
23. the preparation method of composite powder is characterized in that, is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide join form slurries in the aqueous solvent of disperse water insoluble composition after, these slurries are carried out spraying drying with spray-drier.
24. the preparation method of composite powder as claimed in claim 23, wherein, water insoluble active ingredient is the oiliness composition.
25. the preparation method of composite powder is characterized in that, is that the silanol group (SiOH) of 0.001～0.1 μ m, unit specific surface area is 20～70 μ mol/m with the thickness of primary particle 2Flakey silicon-dioxide join with after forming slurries in the aqueous solvent of the form disperse water insoluble composition of emulsifying composition, these slurries are carried out spraying drying with spray-drier.
26. makeup contain any described composite powder in the claim 15～22.
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