CN102333514A - Titanium dioxide composite powders and makeup composition containing the same - Google Patents
Titanium dioxide composite powders and makeup composition containing the same Download PDFInfo
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- CN102333514A CN102333514A CN2010800091320A CN201080009132A CN102333514A CN 102333514 A CN102333514 A CN 102333514A CN 2010800091320 A CN2010800091320 A CN 2010800091320A CN 201080009132 A CN201080009132 A CN 201080009132A CN 102333514 A CN102333514 A CN 102333514A
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- titanium dioxide
- composite powder
- dioxide composite
- powder
- silicone elastomer
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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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
- A61K8/893—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone modified by an alkoxy or aryloxy group, e.g. behenoxy dimethicone or stearoxy dimethicone
-
- 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
- A61K8/29—Titanium; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
-
- 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
-
- 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
-
- 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
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
- A61Q1/10—Preparations containing skin colorants, e.g. pigments for eyes, e.g. eyeliner, mascara
-
- 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
-
- 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
- A61K2800/412—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
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
- A61K2800/62—Coated
- A61K2800/624—Coated by macromolecular compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
Abstract
The present invention relates to titanium dioxide composite powders and a base makeup composition containing the same, more specifically to: titanium dioxide composite powders which are produced by mixing titanium dioxide with elastomers, coating the mixture with polymethylsilsesquioxane, and applying the coated mixture to formulations, thereby covering the skin naturally and providing a soft feeling while avoiding aggregation thereof; and a base makeup composition containing the same.
Description
Technical field
The present invention relates to a kind of titanium dioxide composite powder and contain the cosmetic composition of this composite powder; More particularly; Relate to titanium dioxide composite powder and contain the basic cosmetics compositions of this composite powder, wherein, said titanium dioxide composite powder is through mixing titanium dioxide with silicone elastomer; And with poly methyl silsesquioxane said mixture is coated and to make; Thereby the preparation that contains titanium dioxide composite powder can cover skin surface naturally, and can be applied to skin smoothly and can not condense.
Background technology
The various powder that are usually used in cosmetics have inherent character, and demonstrate various functions according to himself characteristic.Usually, in order to overcome its shortcoming, according to the characteristic of the cosmetics that comprise the inorganic pigment powder, the inorganic pigment powder will pass through various operations, comprises the blend step and the finishing step that are used to make composite powder.In these operations, the blend step that is used to prepare composite powder is commonly used to modify the overall characteristic of powder, so that make its accord with expectation purpose.
Simultaneously, according to its function, can powder roughly be divided into color pigment, Chinese white, extender pigment and functional pigment.
Color pigment is used to regulate the tone of product, and its example comprises ferrum oxide, iron oxide yellow, iron oxide black, chromium oxide and white carbon black.Except that tone, Chinese white can be regulated spreadability, and its example comprises titanium dioxide and zinc oxide.Extender pigment is the diluent that is used to regulate tone, simultaneously, regulates the sense of touch (ductility or adhesiveness) or the gloss of product, and is used to keep product forms.The example of extender pigment comprises Talcum, Muscovitum, sericite and boron nitride.
Being used for these powder of cosmetics, will do more detailed description to Chinese white.In described Chinese white, titanium dioxide (TiO
2) be generally used for hiding skin blemishes, comprise out-of-flatness and wrinkle, thereby make skin neatly smooth.Yet, titanium dioxide (TiO
2) have various defectives, comprise harder sense of touch, caking and not sense naturally, and for these reasons, often use and improve above-mentioned defective such as steps such as mixing and finishinges.For the situation of titanium dioxide, use titanium dioxide and extender pigment (for example Talcum, Muscovitum, sericite or boron nitride) are carried out blended technology, improve the defective of titanium dioxide or give the attribute of titanium dioxide.Yet this composite powder is defectiveness still, because they show harder sense of touch and can not use smoothly, causes caking.
Summary of the invention
Therefore, the present invention has carried out when keeping the high covering power of titanium dioxide to skin surface, improves the coarse research with defective such as caking of the sense of touch of titanium dioxide.The result; The inventor finds through titanium dioxide being mixed with silicone elastomer and using poly methyl silsesquioxane said mixture to be coated the titanium dioxide composite powder for preparing; Can prepare a kind of basic cosmetics compositions; It can cover skin surface naturally, and can be applied to skin surface smoothly, thereby has accomplished the present invention.
Therefore, the object of the invention just provides a kind of cosmetic composition, and it contains titanium dioxide composite powder, and can cover skin surface naturally thus and have slick sense of touch and do not lump.
The invention provides a kind of through titanium dioxide being mixed with silicone elastomer and using poly methyl silsesquioxane (PMSQ) the gained mixture to be coated the composite powder that obtains.
Titanium dioxide (the TiO that uses among the present invention
2) preferably have the particle mean size of 0.1-10 μ m.Along with granularity diminishes, powder covers the ability grow of skin surface.Yet, if granularity greater than 10 μ m, the ability that powder covers skin surface will reduce, and the sense of touch that contains the powder-type cosmetics of composite powder will become coarse.Owing to this reason, particle mean size is not suitable in the cosmetics greater than the titanium dioxide composite powder of 10 μ m.
The silicone elastomer that uses among the present invention is preferably the cross-linked copolymer (crosspolymer) of dimethicone and vinyl-dimethyl polysiloxanes (vinyl dimethicone).In with titanium dioxide and the blended step of silicone elastomer, based on the gross weight of titanium dioxide composite powder, the consumption of silicone elastomer is 30.0-50.0 weight %.If the content of silicone elastomer is higher than 50.0 weight % in the composite powder; The ability that titanium dioxide covers skin surface will descend, and, if the content of silicone elastomer is lower than 30.0 weight %; Composite powder will demonstrate the coarse sense of touch of titanium dioxide, and can not be coated with uniformly.
The poly methyl silsesquioxane that uses among the present invention (PMSQ) is a kind of with the resin of silicon as substrate, relates to a kind of T-resin that contains three Si-O keys, shown in structure formula 1.It is commonly called and is connected with Si-CH
3" organopolysiloxane ", and it has-the OH active group, the surface that allows titanium dioxide is by the coating of silicone elastomer (cross-linked copolymer of dimethicone and vinyl-dimethyl polysiloxanes) chemistry, and is used to give resistance to water and oil resistivity.
Based on the gross weight of titanium dioxide composite powder, the consumption of poly methyl silsesquioxane is 2-5 weight %, coats with the mix powder to titanium dioxide and silicone elastomer.If the poly methyl silsesquioxane content that in composite powder, coats is lower than 2 weight %, powder will descend to the adhesiveness of skin, and if the amount that coats be higher than 5 weight %, powder can not be coated on the surface uniformly.
Hereinafter, will be to the blend step of titanium dioxide and silicone elastomer (dimethicone and vinyl-dimethyl polysiloxanes cross-linked copolymer), and use the poly methyl silsesquioxane resin that the step that mixture coats is further described in detail.
(1) step 1: preparation titanium dioxide
With the titanium dioxide of preparing to coat in exsiccator in 105 ℃ of dryings 4 hours or more than.
(2) step 2: form complex with silicone elastomer
The titanium dioxide of preparation in the step 1 is put into the Hensel agitator, in agitator, mixed by high-speed stirred, make titanium dioxide composite powder thus with silicone elastomer.Here, in the titanium dioxide composite powder weight ratio of titanium dioxide and silicone elastomer in 5: 5 to 7: 3 scopes.If weight ratio is higher than 5: 5; The sense of touch of powder will be very level and smooth, will significantly descend but powder covers the ability of skin surface, and if weight ratio less than 7: 3; The ability of powder covering skin surface will be quite excellent, but can demonstrate the coarse sense of touch of titanium dioxide.Because this factor, above-mentioned specified weight ratio is highly preferred.
(3) step 3: use poly methyl silsesquioxane to coat
With consumption based on composite powder gross weight 2-5 weight %, poly methyl silsesquioxane is sprayed on the composite powder that step 2 obtains, mix afterwards and disperses 15-600 second, preferably 30-300 second.
(4) step 4: heat treatment
After dispersion steps in the step 3 is finished, the product powder in 120-150 ℃ of drying 4 hours or longer time, is accomplished the step that coats with polymer thus.
According to make-up cosmetic composition of the present invention, contain the titanium dioxide composite powder of 0.1-10.0 weight % based on composition total weight according to method for preparing.If the consumption of composite powder is lower than 0.1 weight % in cosmetic composition, compositions can not be smoothly and is coated on skin equably, and the skin surface spreadability that causes thus will be not enough.On the other hand, if the consumption of powder is greater than 10 weight % in the compositions, the preparation stability of compositions will reduce.
When the cosmetic composition that contains titanium dioxide composite powder was used as preparation, can be level and smooth be applied to skin surface and can not lump can show very naturally, and had the effect of extremely excellent covering skin blemishes.
Said composition can be formulated as various forms, comprises cosmetic substrate, foundation cream, the preceding bottoming of woman's persona frost, dual-purpose muffin, muffin, loose powder and eye shadow.
In addition, the present invention provides a kind of make-up cosmetic composition that contains said titanium dioxide composite powder.
Titanium dioxide composite powder of the present invention prepares through titanium dioxide and silicone elastomer being mixed and using poly methyl silsesquioxane that mixture is coated.The basic cosmetics compositions that contains titanium dioxide composite powder can be applied to skin smoothly and not lump, and can recover natural skin texture and demonstrate the effect that covers skin surface.
The specific embodiment
Hereinafter, the present invention does further detailed description with control Example and Test Example.But these embodiment are used for understanding better the present invention, and are not used in qualification the present invention.
Embodiment 1: the preparation titanium dioxide composite powder
70g titanium dioxide in 105 ℃ of dryings 4 hours or longer time, is added it in Hensel agitator then, mix with the 30g silicone elastomer cross-linked copolymer of vinyl-dimethyl polysiloxanes (dimethicone with).Next, spray and mix with mixture with the PMSQ of 2.1g, with mixture in 120-150 ℃ of heat treated 4 hours, thereby acquisition 100.3g titanium dioxide compound.In this embodiment; The titanium dioxide that uses is C47-056 (Sunchemical Crop; The U.S.); Employed silicone elastomer is DC 9506C (Dow Coming Corp., the U.S.), and employed PMSQ is the PMSQ through polymerization MTES (GE Toshiba Corp.) preparation.
Comparative Examples 1: the titania powder that the preparation alkylsiloxane coats
With 100g titanium dioxide (CR50; Ishibara Co., Ltd., Japan) in 105 ℃ of dryings 4 hours or longer time, afterwards it is added the Hensel agitator, in agitator, use the spraying of 2.1g triethoxy octyl group silane to spray, and stir with mixture.Afterwards, 120-150 ℃ with the mixture process that obtains 4 hours, thereby obtain the titanium dioxide that the 102.1g alkylsiloxane coats.
Test Example 1: skin texture adjustment (skin texture correction) contrast
In order to detect the skin texture adjustment effect of the cosmetic composition that contains titanium dioxide composite powder of the present invention,, use following table 1 listed component preparation to contain the muffin of titanium dioxide composite powder prepared among the embodiment 1 according to conventional method.In order to contrast, also prepared the Comparative formulation 1 that contains the cladding titanium dioxide powder of preparation in the Comparative Examples 1.
Table 1
Component | Preparation 1 (weight %) | Comparative formulation 1 (weight %) |
Talcum | ?44.7 | ?44.7 |
Sericite | ?20.0 | ?20.0 |
Silicon dioxide | ?10.0 | ?10.0 |
Titanium dioxide | ?8.0 | ?8.0 |
Zinc oxide | ?3.0 | ?3.0 |
The titanium dioxide composite powder of embodiment 1 | ?5.0 | |
The cladding titanium dioxide powder of Comparative Examples 1 | ?- | ?5.0 |
Ferrum oxide | ?2.0 | ?2.0 |
Mineral oil | ?7.0 | ?7.0 |
Antiseptic | ?0.3 | ?0.3 |
To be applied to wrist respectively with Comparative formulation 1 according to the preparation 1 of method for preparing, and use imaging analysis instrument (Primos handheld device, GFM GmbH) to measure the wrinkle degree of skin surface then, estimate the skin texture adjustment effect of each preparation thus.For reaching this purpose, every kind of preparation on the Ms's of two Mies of more than 20 year old and two one's late 30s wrist, is used twice with powder puff by vertical respectively, measure the wrinkle degree of skin surface then.Following table 2 has shown the wrinkle depth measurement result before and after using.
Table 2
Preparation 1 | Comparative formulation 1 | |
The skin texture adjustment | ?37% | ?20% |
Result from last table 2 can know; Use Comparative formulation 1 to show skin texture adjustment effect equally; But the preparation 1 that contains titanium dioxide composite powder according to the invention can be used to recover natural skin texture smoothly; This shows with Comparative formulation 1 compares, and preparation 1 has outstanding skin texture adjustment effect.
Test Example 2: flatness test
The powder for preparing in embodiment 1 and the Comparative Examples 1 is respectively got 0.015g and is applied to respectively on the dermatine, flow graph is placed on the dermatine of having used said powder respectively, estimates the smoothness of each powder thus.Table 3 has shown evaluation result.
Table 3
Smoothness | |
Embodiment 1 | 104 |
Comparative Examples 1 | 150 |
As above shown in the table 3, Comparative Examples 1 shown and has been higher than 140 value, and this value makes skin feel coarse, and this shows that the cosmetic composition sense of touch that contains Comparative Examples 1 powder is bad.Yet embodiment 1 has shown and has been lower than 110 value, feels usually smoothly that at this value skin this shows that the cosmetic composition that contains titanium dioxide composite powder of the present invention can show level and smooth sense of touch.
Test Example 3: respondent's sense of touch is estimated
Through every kind of preparation directly being applied to 20 faces, estimate preparation 1 and Comparative formulation 1 covering power, flatness, thickness sense and application properties separately to 20 female consumer respondents of one's late 30s.Particularly, preparation 1 and Comparative formulation 1 are applied to respectively on each respondent's the skin, and before and after every kind of preparation is used, carry out sensory evaluation.Following table 4 has shown evaluation result.
Table 4
Covering power | Flatness | The thickness sense | Application properties | |
Preparation 1 | Zero (outstanding) | ◎ (very outstanding) | ◎ (approaching) | ◎ (very outstanding) |
Comparative formulation 1 | ◎ (very outstanding) | △ (slightly) | △ (thick) | △ (slightly) |
◎: very outstanding, zero: outstanding, △: slight, *: do not have
Can find out that from the result of last table 4 preparation 1 that contains titanium dioxide composite powder of the present invention with use is compared, use the Comparative formulation 1 that contains the cladding titanium dioxide powder to demonstrate outstanding skin covering power.But preparation 1 shows aspect flatness, thickness sense and application properties better, and this shows that the integral body sensation of using preparation 1 is obviously better.
Claims (8)
1. a titanium dioxide composite powder is characterized in that, this composite powder makes through titania powder being mixed with silicone elastomer and using poly methyl silsesquioxane to coat the gained mixture.
2. titanium dioxide composite powder according to claim 1, wherein, the particle mean size of said titanium dioxide is 0.1-10 μ m.
3. titanium dioxide composite powder according to claim 1, wherein, said silicone elastomer is the cross-linked copolymer of dimethicone and vinyl-dimethyl polysiloxanes.
4. titanium dioxide composite powder according to claim 1, wherein, based on the gross weight of titanium dioxide composite powder, with the consumption of the blended silicone elastomer of titanium dioxide be 30.0-50.0 weight %.
5. titanium dioxide composite powder according to claim 1 wherein, based on the gross weight of titanium dioxide composite powder, is 2-5 weight % in order to the consumption of poly methyl silsesquioxane that the mixture of titanium dioxide and silicone elastomer is coated.
6. the application of any described titanium dioxide composite powder in the preparation cosmetic composition among the claim 1-5.
7. cosmetic composition that contains any described titanium dioxide composite powder among the claim 1-5.
8. cosmetic composition according to claim 7, wherein, based on the gross weight of said composition, the content of said titanium dioxide composite powder is 0.1-10.0 weight %.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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KR1020090015342A KR101081199B1 (en) | 2009-02-24 | 2009-02-24 | Titanium dioxide composite powder and the makeup cosmetic composition containing the same |
KR10-2009-0015342 | 2009-02-24 | ||
PCT/KR2010/001141 WO2010098575A2 (en) | 2009-02-24 | 2010-02-24 | Titanium dioxide composite powders and makeup composition containing the same |
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CN102333514A true CN102333514A (en) | 2012-01-25 |
CN102333514B CN102333514B (en) | 2013-04-17 |
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CN2010800091320A Active CN102333514B (en) | 2009-02-24 | 2010-02-24 | Titanium dioxide composite powders and makeup composition containing the same |
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KR (1) | KR101081199B1 (en) |
CN (1) | CN102333514B (en) |
WO (1) | WO2010098575A2 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106619194A (en) * | 2016-12-27 | 2017-05-10 | 广州市科能化妆品科研有限公司 | Sunscreen composition containing composite solid powder and polymer film-forming agent |
CN110934776A (en) * | 2019-12-17 | 2020-03-31 | 中南林业科技大学 | Titanium dioxide composite material coated with polytrifluoropropylmethylsiloxane and preparation method and application thereof |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
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KR101290339B1 (en) * | 2010-12-30 | 2013-08-07 | 주식회사 안느 | Cosmetic composition containing elastomer beads complexed powder coated with vegetable butter |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1533267A (en) * | 2000-07-10 | 2004-09-29 | Cosmetic compositions | |
CN101355923A (en) * | 2005-11-11 | 2009-01-28 | 株式会社太平洋 | Cosmetic composition for make up containing the interference color pigment and preparing method of the same |
Family Cites Families (3)
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KR100955353B1 (en) | 2003-03-19 | 2010-04-29 | 가오 가부시키가이샤 | A preparing method for cosmetics |
KR20070006088A (en) * | 2005-07-07 | 2007-01-11 | 주식회사 엘지생활건강 | A pressed type makeup composition with elasticity |
JP5083801B2 (en) | 2006-02-20 | 2012-11-28 | 株式会社 資生堂 | Water-in-oil emulsified sunscreen cosmetics |
-
2009
- 2009-02-24 KR KR1020090015342A patent/KR101081199B1/en active IP Right Grant
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2010
- 2010-02-24 CN CN2010800091320A patent/CN102333514B/en active Active
- 2010-02-24 WO PCT/KR2010/001141 patent/WO2010098575A2/en active Application Filing
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1533267A (en) * | 2000-07-10 | 2004-09-29 | Cosmetic compositions | |
CN101355923A (en) * | 2005-11-11 | 2009-01-28 | 株式会社太平洋 | Cosmetic composition for make up containing the interference color pigment and preparing method of the same |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106619194A (en) * | 2016-12-27 | 2017-05-10 | 广州市科能化妆品科研有限公司 | Sunscreen composition containing composite solid powder and polymer film-forming agent |
CN110934776A (en) * | 2019-12-17 | 2020-03-31 | 中南林业科技大学 | Titanium dioxide composite material coated with polytrifluoropropylmethylsiloxane and preparation method and application thereof |
CN110934776B (en) * | 2019-12-17 | 2022-09-13 | 中南林业科技大学 | Titanium dioxide composite material coated with polytrifluoropropylmethylsiloxane and preparation method and application thereof |
Also Published As
Publication number | Publication date |
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CN102333514B (en) | 2013-04-17 |
KR20100096454A (en) | 2010-09-02 |
WO2010098575A3 (en) | 2011-01-06 |
WO2010098575A2 (en) | 2010-09-02 |
KR101081199B1 (en) | 2011-11-07 |
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