TW200521159A - Surface coated powder and a cosmetic composition containing said powder - Google Patents

Surface coated powder and a cosmetic composition containing said powder Download PDF

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Publication number
TW200521159A
TW200521159A TW093138104A TW93138104A TW200521159A TW 200521159 A TW200521159 A TW 200521159A TW 093138104 A TW093138104 A TW 093138104A TW 93138104 A TW93138104 A TW 93138104A TW 200521159 A TW200521159 A TW 200521159A
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powder
coated
group
mixture
metal oxide
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TW093138104A
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Chinese (zh)
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TWI359164B (en
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Toshihiro Ishimori
Masato Nakade
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Kose Corp
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11Encapsulated compositions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89Polysiloxanes
    • A61K8/891Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/48Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
    • C08G77/58Metal-containing linkages
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/14Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Chemical & Material Sciences (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Dermatology (AREA)
  • Cosmetics (AREA)
  • Silicon Polymers (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

A surface-coated powder which comprises a powder coated with a metal oxide-organopolysiloxane hybrid wherein an organopolysiloxane and a metal oxide form a composite at a molecular level. The surface-coated powder is prepared by coating a powder with a metal oxide-organopolysiloxane hybrid sol, to thereby form a thin film of the above hybrid on the surface of the powder. The metal oxide of the above metal oxide-organopolysiloxane hybrid is preferably one or more of metal oxides selected from among a titanium oxide, a zirconium oxide and silicon dioxide. The above metal oxide-organopolysiloxane hybrid can have a controlled water repellency by the adjustment of the proportion of the metal oxide to the organopolysiloxane, and thus the water repellency of the powder can be controlled with ease by the adjustment of the above proportion. A cosmetic containing the above surface-coated powder is excellent in natural appearance and in the feeling during the practice of application.

Description

200521159 九、發明說明: 【發明所屬之技術領域】 本發明係關於表面經被覆之粉體。更詳細地說,係關 於以金屬氧化物•有機聚矽氧烷混成物被覆表面之粉體。 又’本發明亦關於由該粉體所構成之化粧品用粉體及含該 粉體之化粧料。 【先前技術】 化粧料所用之粉體,為提高化粧持久性或改善化粧塗 布時之觸感,-般而言,會以㈣、金屬4、以全氣烧基 磷酸酯為代表之含氟物質等撥水性表面處理劑進行表面被 覆。 而若經表面被覆處理後之粉體其撥水性低則化粧持久 性不能提升。反之,若撥水性太高則親膚性不佳,結果會 造成化粧持久性不佳、或者因脫粧而變髒。是以,撥水性 之调整疋重要的。該粉體撥水性之調整,可於對粉體進行 表面被覆處理時藉由改變撥水性表面處理劑之處理量來進 仃,但右處理量太少,則無法完全被覆粉體表面,會造成 品質不均-或凝集現象。又,增加處理量之場合,:量太 多’則會出ί見無法被覆於粉體表面之殘餘量,使得無法產 生因應處理量之撥水性。再者,處理量太少或太多都合 觸感不佳的問題。亦即,以改變撥水性表面處理二旦 以調整粉體撥水性的作法有其問題點。 里 一般最常使用的粉體夕4路UULi ^ 物體之撥水性表面處理劑,從構造之 200521159 夕樣化、取得容易度、機能性、安全性等方面來看,係矽 酮或其衍生物。本發明申請人先前曾開發了一種金屬氧化 物有機1碎乳烧複合粉體(日本專利特開2001 — 64395 號),其係將有機聚矽氧烷之矽原子中一部分透過氧與金屬 原子進行共價鍵結而均一複合化。該粉體可直接配合於化 粧料中。 【發明内容】 本發明人認為,要以表面處理控制粉體表面撥水性 時,並非利用控制撥水性表面處理劑對粉體表面之被覆量 來進行,而以控制撥水性表面處理劑其撥水性本身為較佳 的方法。 並且注意到,金屬氧化物•有機聚矽氧烷混成物係具 有親水性的金屬氧化物、與疏水性之有機聚矽氧烷之混成 物,即,藉由改變金屬氧化物與有機聚矽氧烷之比例,可 以調整混成物之撥水性,並考慮到將該混成物用於粉體表 面處理劑中以控制表面處理粉體之撥水性,以完成了本發 明。 即,本發明係以有機聚矽氧烷與金屬氧化物於分子層 次複合化之金屬氧化物•有機聚矽氧烷混成物進行表面被 覆之表面被覆粉體。上述金屬氧化物•有機聚矽氧烷混成 物中之金屬氧化物’較佳為擇自氧化鈦、氧化锆及二氧化 矽中1種或2種以上之金屬氧化物。又,上述金屬氧化物· 有機聚矽氧烧混成物中之有機聚矽氧烷,較佳為以下述通 200521159 式(1 )表示之殘基:200521159 IX. Description of the invention: [Technical field to which the invention belongs] The present invention relates to powder coated on the surface. In more detail, it is about powder coated with metal oxide / organic polysiloxane mixture on the surface. The present invention also relates to a cosmetic powder composed of the powder and a cosmetic containing the powder. [Previous technology] The powder used in cosmetics is used to improve the durability of the makeup or to improve the touch during makeup application. Generally speaking, it will be represented by fluorene, metal 4, and fluorinated phosphoric acid esters. The surface is coated with a water repellent surface treatment agent. If the surface-treated powder has low water repellency, the makeup durability cannot be improved. Conversely, if the water repellency is too high, the skin-friendly property is not good, and as a result, the durability of makeup may be poor, or the makeup may become dirty. Therefore, the adjustment of water repellency is important. The adjustment of the water repellency of the powder can be carried out by changing the treatment amount of the water repellent surface treatment agent when the powder is surface-coated, but the right treatment amount is too small, and the powder surface cannot be completely covered, which will cause Uneven quality-or agglutination. In the case of increasing the amount of treatment, if the amount is too large, a residual amount that cannot be covered on the surface of the powder will appear, making it impossible to generate water repellency corresponding to the amount of treatment. Furthermore, too little or too much processing is a problem of poor touch. That is, the method of adjusting the water repellency of the powder by changing the water repellent surface treatment has its problems. In general, the most commonly used powder is 4-way UULi ^ Water-repellent surface treatment agent for objects. From the perspective of 200521159 structure, easy access, performance, and safety, it is silicone or its derivative. . The applicant of the present invention has previously developed a metal oxide organic 1 crushed milk burned composite powder (Japanese Patent Laid-Open No. 2001-64395), which is a process in which a part of the silicon atoms of the organic polysiloxane is conducted through oxygen and metal atoms. Covalently bonded and uniformly complexed. This powder can be blended directly into makeup. [Summary of the invention] The present inventor believes that when surface treatment is used to control the water repellency of the powder surface, it is not performed by controlling the coating amount of the water repellent surface treatment agent on the powder surface, but to control the water repellency of the water repellent surface treatment agent. It is a better method in itself. It is also noted that the metal oxide-organic polysiloxane mixture is a mixture of a hydrophilic metal oxide and a hydrophobic organic polysiloxane, that is, by changing the metal oxide and the organic polysiloxane The proportion of the alkane can be adjusted by the water repellency of the mixture, and considering the use of the mixture in a powder surface treatment agent to control the water repellency of the surface-treated powder, the present invention has been completed. That is, the present invention is a surface-coated powder obtained by surface-coating a metal oxide-organic polysiloxane compound that is a composite of an organic polysiloxane and a metal oxide at a molecular level. The metal oxide 'in the metal oxide-organic polysiloxane mixture is preferably one or two or more metal oxides selected from titanium oxide, zirconia, and silicon dioxide. The organopolysiloxane in the metal oxide / organopolysiloxane fired mixture is preferably a residue represented by the following formula (1) in 200521159:

R I Y_S i I R -O-S iR I Y_S i I R -O-S i

y . R I I 0_S i-—O— S i _Yy. R I I 0_S i-—O— S i _Y

RR

[式中’ R為碳數1〜22之烧基、芳基或芳烧基,可為相 同或相異。Y為以一R、一〇—或—r1— Si( —〇 一)3表示之 基(惟,R1為碳數1〜5之烷撐基),可為相同或相異,但其中 至少有 1 個為一0 —或一R1— Si(~0 — )3。又,η=ι〜1〇〇、 m=〇〜5] 〇 又,本發明為由上述經表面被覆之粉體所構成之化粧 品用粉體,及包含該化粧品用粉體之化粧料。 又,本發明之表面被覆粉體之製造方法,其特徵為:以 金屬醇鹽之部分水解物、與末端或側鏈具有反應性官能基 之有機聚矽氧烷反應而得到之混成物,對粉體進行表面被 覆處理,之後進行乾燥而製得表面被覆粉體。該有機聚矽 氧烷以下述通式(2)表示者為佳: o-s[Wherein R 'is an alkyl group, an aryl group or an aromatic group having 1 to 22 carbon atoms, and may be the same or different. Y is a group represented by one R, one 0—or —r1—Si (—〇 一) 3 (however, R1 is an alkylene group having 1 to 5 carbon atoms), which may be the same or different, but at least One is a 0 — or a R1 — Si (~ 0 —) 3. In addition, η = ι to 100, and m = 0 to 5] The present invention is a powder for cosmetics composed of the above-mentioned surface-coated powder, and a cosmetic containing the powder for cosmetics. In addition, the method for producing a surface-coated powder according to the present invention is characterized in that a mixed product obtained by reacting a partial hydrolysate of a metal alkoxide with an organic polysiloxane having a reactive functional group at a terminal or side chain, The powder is subjected to a surface coating treatment and then dried to obtain a surface-coated powder. The organopolysiloxane is preferably represented by the following general formula (2): o-s

Ό-SΌ-S

R IR I

I Ο-Si —X (2)I Ο-Si —X (2)

II

R ^ m RR ^ m R

[式中,R為碳數1〜22之烷基、芳香基或芳烷基,可為 相同或相I 〇Χ為HH、_R或―Rl— si(_〇R2— ^表示 之基(惟,Rl為碳數1〜5之烷撐基,R2為氫或碳數1〜5之烷 基)可為相㈤或相異,但其中至少有1個為~H或一R1 — (OR ~ )。又,n==l〜100、m=0〜5]。 200521159 【實施方式】 本發明之表面被覆粉體中,被覆粉體表面之金屬氧化 物·有機聚矽氧烷混成物,係有機聚矽氧烷與金屬氧化物 於分子層次複合化而形成者。此處「於分子層次複合化」 係指將有機聚矽氧烷相與金屬氧化物相2個相以奈米級混 合。混成物之有機聚矽氧烷相與金屬氧化物相之相域大小 為可見光波長(400nm)以下,無法以光學顯微鏡確認有機聚 石夕氧烧相與金屬氧化物相2個相。又,於有機聚石夕氧烧相 與金屬氧化物相之界面,具有透過氧將金屬原子之一部分 與有機聚矽氧烷之矽原子進行鍵結之共價鍵。藉由該共價 鍵之存在,可以得到使金屬氧化物與有機聚矽氧烷均質地 複合化之混成物。 本發明中,係將金屬氧化物•有機聚矽氧烷混成物, 以前驅物之溶膠狀態被覆於粉體表面。而於粉體表面,生 成金屬氧化物•有機聚矽氧烷混成物。 上述金屬氧化物•有機聚矽氧烷混成物中,與有機聚 矽氧烷複合之金屬氧化物之金屬,可舉例如鈦、錯、鋁等, 亦可使用石夕。該等金屬之1化物环公如难田★ _ 1 A 、[In the formula, R is an alkyl group, an aromatic group, or an aralkyl group having 1 to 22 carbon atoms, and may be the same or a phase I OX is a group represented by HH, _R, or —R1—si (_〇R2— ^ R1 is an alkylene group having 1 to 5 carbon atoms, R2 is hydrogen or an alkyl group having 1 to 5 carbon atoms) may be different or different, but at least one of them is ~ H or one R1 — (OR ~ ). Also, n == l ~ 100, m = 0 ~ 5] 200521159 [Embodiment] In the surface-coated powder of the present invention, the metal oxide-organic polysiloxane mixture on the surface of the powder-coated powder is a system Organic polysiloxane and metal oxide are compounded at the molecular level. Here, "composite at the molecular level" refers to the mixing of two phases of the organic polysiloxane and the metal oxide phase at the nanometer level. The phase domain size of the organic polysiloxane phase and the metal oxide phase of the mixture is below the visible light wavelength (400 nm). It is not possible to confirm the two phases of the organic polysilica sintered phase and the metal oxide phase by an optical microscope. The interface between the organic polyoxygen sintered phase and the metal oxide phase has a bond between a part of the metal atom and the silicon atom of the organic polysiloxane through oxygen. Valence bond. By the existence of this covalent bond, a mixture obtained by homogeneously complexing a metal oxide and an organopolysiloxane can be obtained. In the present invention, a mixture of a metal oxide and an organopolysiloxane, The sol state of the precursor is coated on the surface of the powder. On the surface of the powder, a metal oxide / organic polysiloxane mixture is formed. The above metal oxide / organic polysiloxane mixture is mixed with organic polysiloxane Metals of metal oxides such as alkane complexes can include, for example, titanium, aluminum, aluminum, etc. Shi Xi can also be used. The first compounds of these metals are as difficult as a field ★ _ 1 A 、

戈口甲醇鹽、乙醇鹽、 屬會變化為金屬氧化物。醇鹽可舉例 丙醇鹽、丁醇鹽、異丙醇鹽等。 又,與金屬氧化物複合時所使用之有機聚矽氧烷,只 200521159 要疋末端或側鏈具有反應性官能基之有機聚矽氧烷(本發明 稱為反應性有機聚矽氧烷)即可,無特別限定。反應性官能 基係例如烷氧基、矽醇基、羧基、胺基、環氧基等,較佳 為〃有烧氧基之有機聚矽氧烧或具有矽醇基之有機聚矽氧 烷(此處,有時將此等具有烷氧基或矽醇基之有機聚矽氧 烷,簡單地稱作含烷氧基有機聚矽氧烷或含矽醇基有機聚 矽氧烷)。 上述烷氧基係甲氧基、丙氧基、丁氧基、異丙氧基等。 特別以如下式通式(2)所示具有烷氧基之有機聚矽氧烷衍生 物為較佳之使用者。Gekou methoxide, ethoxide, and metal species change to metal oxides. Examples of the alkoxide include propanol, butanol, and isopropoxide. In addition, the organopolysiloxane used when compounding with a metal oxide is only 200521159, which requires an organopolysiloxane having a reactive functional group at a terminal or side chain (the present invention is called a reactive organic polysiloxane). Yes, it is not particularly limited. The reactive functional group is, for example, an alkoxy group, a silanol group, a carboxyl group, an amine group, an epoxy group, and the like, and is preferably an organic polysiloxane having a thiol group or an organic polysiloxane having a silanol group ( Herein, these organic polysiloxanes having an alkoxy group or a silanol group are sometimes simply referred to as alkoxy-containing organic polysiloxanes or silanol-containing organic polysiloxanes). The alkoxy group is a methoxy group, a propoxy group, a butoxy group, an isopropoxy group, and the like. Particularly, an organopolysiloxane derivative having an alkoxy group represented by the following general formula (2) is a preferable user.

I χ-s i I RI χ-s i I R

(2)(2)

Ο—S i--O—S i—XΟ—S i--O—S i—X

I II I

R RR R

[式中,R為碳數1〜22之烷基、芳香基或芳烷基,可為 相同或相異。X為以—H、一 R或—R1 _ Si( — — )3表示 之基(惟,Rl為碳數1〜5之烷撐基,R2為氫或碳數1〜5之烷 基)’可為相同或相異,其中至少有i個為—H或一 Rl — 8丨(— OR )。又 ’ n= 1 〜1 〇〇、m=〇〜5]。 上述R之烷基,係甲基、乙基、丙基等,特別以甲基 之化合物為較佳之使用者。又,上述R之芳香基係苯基、 甲苯基等’芳烧基係苯乙基等。該等有機聚錢燒衍生物 可舉例如通式(3)(此通式(3)中,Rl、R2、n與通式(1)中之定 義相同)。具體而言,可舉出下式⑷、(5)所示之化合物。 200521159 CHa | ✓ i — }. CHa < ?Hv H>—S i - __ 1 CHa CHa 〇Ha o—s CHa f -〇"S i CHa CH3 1 ,o-s i-CaKe_s i (OR总), (3) CH^ > CH> (〇ch3), ⑷ s,i tOC2HB)e[In the formula, R is an alkyl group, an aromatic group, or an aralkyl group having 1 to 22 carbon atoms, and may be the same or different. X is a group represented by —H, —R or —R1 — Si (— —) 3 (however, R1 is an alkylene group having 1 to 5 carbon atoms, and R2 is hydrogen or an alkyl group having 1 to 5 carbon atoms) ' They can be the same or different, at least i of which are -H or an Rl — 8 丨 (—OR). Also, "n = 1 to 1 00, m = 0 to 5]. The alkyl group of the above-mentioned R is methyl, ethyl, propyl, etc., and a methyl compound is particularly preferred. Further, the above-mentioned aromatic phenyl groups such as aromatic phenyl and tolyl are aromatic phenethyl and the like. Examples of the organic polysaccharin derivative include general formula (3) (in this general formula (3), R1, R2, and n have the same definitions as in general formula (1)). Specific examples include compounds represented by the following formulae (5) and (5). 200521159 CHa | ✓ i —}. CHa <? Hv H > —S i-__ 1 CHa CHa 〇Ha o—s CHa f -〇 " S i CHa CH3 1, os i-CaKe_s i (OR total), (3) CH ^ > CH > (〇ch3), ⑷ s, i tOC2HB) e

CHg — s CHe ✓ c,h4 •Ο-— S i —-> I 1 ,0 — S i L ^ f 20 、ch3 J CM,CHg — s CHe ✓ c, h4 • Ο-— S i —- > I 1, 0 — S i L ^ f 20, ch3 J CM,

I (5) ,〇 — S i — CHi • f CHa 以下說明本發明之表面被覆粉體之製造方法。本發明 係:用金屬氧化物·有機聚矽氧烷混成物其前驅體之溶膠 狀態,進行粉體之表面被覆,並於粉體表自完成金屬氧化 物·有機聚矽氧烷混成物。此處說明之例子中,金屬氧化 物係選擇氧化鈦,其起始原料係使用鈦之醇鹽,反應性有 機聚石夕氧烷則使用含烷氧基之二甲基聚矽氧烷。 將水與有機溶劑與酸之混合液滴入鈦之醇鹽進行部分 水解’以生成二氧化鈦溶膠。此時,較佳為緩慢添加混合 液以得到透明溶膠。藉由添加該含烷氧基之二甲基聚矽氧 烧衍生物,生成混成物溶膠。此階段,水解、聚合為未完 全完成的狀態。而將該混成物溶膠用於粉體之表面被覆。 該混成物溶膠具有形成透明薄膜的性質。以該混成物 /谷膠被覆粉體表面,於粉體表面再進行混成物溶膠之水 10 200521159 甲基聚石夕氧烧混成物 解、聚合,藉此可得到以氧化鈦· 進行表面被覆之表面被覆粉體。 本發明+,以混成物溶膠被覆粉體表自,並於粉體表 面形成氧化鈦•二甲基聚石夕氧心成物之方法,可舉出: 將混成物溶膠與粉體混合,之後再進行乾燥的方法;或將 混成物溶料霧於粉體表面,之後再進行乾燥之方法;或 將混成物溶膠與粉體混合後,再添加氣水等驗劑使混成物 析出於粉體表面再進行乾燥的方法等。 使用混成物溶膠所形成之混成物薄膜,係透明柔軟之 均勻皮膜。該混成物薄膑,#由改變氧化鈦與二甲基聚石夕 氧院之組成比,可控制其撥水性、折射率。又,若將欽之 醇鹽單獨進行水解、聚合,則會生成氧化鈦,料難以製 成透明薄膜。另—方面,若將含烷氧基之有機聚矽氧烷單 獨進行水解、聚合,亦僅會單純的高分子量化,並不會形 成強固的皮膜。 本毛月中以金屬氧化物•有機聚矽氧烷混成物進行 表面被覆之粉體’若為一般使用於化粧品之粉體,可為板 狀、、方錘狀、針狀等形狀,且粒子徑、多孔質、益孔質等 之粒子構造並無特別限定,可舉出無機粉體類、:澤性粉 體類有機&體類、色素粉體類、複合粉體類等。具體而 :’可列舉·普魯士藍、群青、氧化鐵紅、黃氧化鐵、黑 ?化鐵、氧化鈦、氧化辞、氧化鋁、氧化鈽、二氧化矽: ,化鎮、乳化錯、石炭酸鎮、碳酸辦、氧化絡、氯氧化絡、 “、、石夕I鋁鎂、雲母、合成雲母、合成絹雲母、絹雲母、 11 200521159 滑石、高嶺土、碳化矽、硫酸鋇、膨土、蒙脫石、氮化硼 等無機粉體類;氯氧化鉍、雲母鈦、氧化鐵覆膜雲母、氧 化鐵雲母鈦、有機顏料處理雲母鈦、鋁粉等光澤性粉體類; 硬脂酸鎂、硬脂酸鋅、N —醯基賴氨酸、尼龍等有機粉體 類;有機焦油系顏料、有機色素之色澱顏料等色素粉體類; 微粒子氧化鈦被覆雲母鈦、微粒子氧化鋅被覆雲母鈦、硫 酸鋇被覆雲母鈦、含氧化鈦二氧化矽、含氧化鋅二氧化矽 等複合粉體等,該等粉體可使用1種或組合2種以上使用。 又,該等粉體亦可使用1種或使至少2種複合化後再使用。_ 本發明中’金屬氧化物·有機聚矽氧烷混成物對粉體 之量並無特別限定,以對粉體為1〜99質量%(以下,單以% 表示)為佳,更佳為3 %以上。 本么明之表面被覆粉體,係於塗料、墨水、化粧料中 作為粉體使用。特別是作為化粧用粉體係有用。 - 本發明之表面被覆粉體其撥水性,係以被水與有機溶 劑(2 —丙醇)之混合液沾濕的容易度來評價。若將粉體添加 於混合液中,則不沾濕之場合粉體會浮游於液面,但若將2 · 一丙醇對水的比例增加,則最後粉體會沉降下來。以此時2 丙醇對水的容量比例定義為撥水化度。例如,若對於水 25ml,2 -丙醇之量為1〇ml,則撥水化度為〇·4。撥水化度 愈大表示粉體具較高的撥水性。將表面被覆粉體用於化 粧料日寸’若撥水化度過低,則會因被汗水沾溼而使化粧持 久丨生是差。另一方面,若撥水性太高則使親膚性變差,化 粧持久性亦不佳。具體而言,撥水化度之值較佳為〇.6以 12 200521159 上、未滿1.2。 開發用於化粧料之粉底等之粉體時,為使塗布時外觀 自然,一般會控制粉體之光學特性。具體而言,例如減少 光入射至粉體時之表面反射光比例,並增加散射光,藉此 使塗布時不自然的光澤消失,且可以隱藏皮膚的缺點。藉 由在粉體表面被覆不同折射率之二氧化石夕或二氧化鈦,可 以相對性地增加散射光。但,使用該等無機氧化物之混成 物時’若直接使用會有堅硬的觸感,且為賦予撥水性必須 實施表面處理。相對於該等,本發明藉由以金屬氧化物· _ 有機聚矽氧烷混成物被覆於粉體,可以同時賦予柔軟觸感 及適當之撥水性,並藉由在粉體表面形成透明之金屬氧化 物•有機聚矽氧烷混成物層,可增加散射光。 其次說明配合本發明被覆粉體之化粧料。藉由配合以 金屬氧化物•有機聚矽氧烷混成物進行表面被覆之本發明 之表面被覆粉體, 觀優異的化粧料。 容化粧料為中心, 等皮膚保養化粧料、 量並無特別限定,但 可以得到化粧持久性、使用感、自然外 化粧料之劑型,主要以粉底、香粉等美 亦可使用為防曬化粧料、乳液、化粧水 、頭髮化粧料等。表面被覆粉體之配合 但較佳為0.1質量%以上。 再者於不知害本發明效果之範圍内,可於本發明之I (5), 0 — Si — CHi • f CHa The method for producing the surface-coated powder of the present invention will be described below. In the present invention, the surface of the powder is coated with the sol state of the precursor of the metal oxide-organopolysiloxane mixture, and the metal oxide-organopolysiloxane mixture is self-completed on the surface of the powder. In the example described here, titanium oxide is selected as the metal oxide. The titanium alkoxide is used as the starting material, and dimethylpolysiloxane containing an alkoxy group is used as the reactive organic polysiloxane. A mixed solution of water, an organic solvent and an acid is dropped into a titanium alkoxide for partial hydrolysis' to produce a titanium dioxide sol. At this time, it is preferable to slowly add the mixed solution to obtain a transparent sol. By adding the alkoxy-containing dimethylpolysiloxane derivative, a mixed sol is formed. At this stage, hydrolysis and polymerization are incompletely completed. The mixed sol is used for surface coating of powder. This mixed sol has the property of forming a transparent film. Coating the surface of the powder with this mixture / gluten, and then carrying out the mixing of the sol water on the surface of the powder 10 200521159 The decomposition and polymerization of the methyl polysilicone sintered mixture, thereby obtaining the surface coating with titanium oxide. The surface is covered with powder. In the present invention, a method for coating a powder surface with a mixed substance sol and forming a titanium oxide / dimethyl polylithium oxide core substance on the surface of the powder includes: mixing the mixed substance sol with the powder, and thereafter Then dry the method; or spray the mixture on the surface of the powder, and then dry it; or mix the mixture sol with the powder, and then add test agents such as gas and water to precipitate the mixture out of the powder A method of drying the surface. The mixed film formed by using the mixed sol is a transparent and soft uniform film. The mixture thin 膑, # can be controlled by changing the composition ratio of titanium oxide and dimethyl polysilicone to control its water repellency and refractive index. In addition, if the chitin alkoxide is hydrolyzed and polymerized separately, titanium oxide is formed, and it is difficult to produce a transparent film. On the other hand, if the alkoxy group-containing organic polysiloxane is hydrolyzed and polymerized alone, it will only have a simple high molecular weight and will not form a strong film. In the course of this hair month, a powder coated with a metal oxide / organic polysiloxane mixture is used as a surface powder. If it is a powder generally used in cosmetics, it can be plate-shaped, square-hammer-shaped, needle-shaped, and other particles. The particle structure such as diameter, porosity, and beneficial porosity is not particularly limited, and examples include inorganic powders, organic powders, pigment powders, and composite powders. Specifically: 'Can be listed: Prussian Blue, Ultramarine, Iron Oxide Red, Yellow Iron Oxide, Black Iron, Titanium Oxide, Oxidation, Alumina, Hafnium Oxide, Silicon Dioxide: Chemical, Emulsified, Carbonyl Acid Carbonate Office, Oxidation Complex, Chlorine Oxidation Complex, ",, Shixi I Aluminum Magnesium, Mica, Synthetic Mica, Synthetic Sericite, Sericite, 11 200521159 Talc, Kaolin, Silicon Carbide, Barium Sulfate, Bentonite, Montmorillonite And other inorganic powders such as boron nitride; bismuth oxychloride, titanium mica, iron oxide coated mica, iron oxide mica titanium, organic pigment treated mica titanium, aluminum powder and other glossy powders; magnesium stearate, stearin Organic powders such as zinc acid, N-fluorenyl lysine, nylon; pigment powders such as organic tar pigments, lake pigments of organic pigments; microparticle titanium oxide coated with mica titanium, microparticle zinc oxide coated with mica titanium, sulfuric acid Composite powders such as barium-coated titanium mica, titanium oxide-containing silicon dioxide, zinc oxide-containing silicon dioxide, etc., these powders can be used singly or in combination of two or more kinds. Or compound at least two Use it later._ In the present invention, the amount of the powder of the "metal oxide · organic polysiloxane" mixture is not particularly limited, and the powder is preferably 1 to 99% by mass (hereinafter, expressed in%). , More preferably 3% or more. The surface-coated powder of Benmemin is used as a powder in coatings, inks, and cosmetics. It is particularly useful as a cosmetic powder system.-The surface-coated powder of the present invention has water repellency. It is evaluated by the ease of getting wet with the mixed solution of water and organic solvent (2-propanol). If the powder is added to the mixed solution, the powder will float on the liquid surface when it is not wet, but if Increasing the ratio of 2-propanol to water will eventually settle the powder. The capacity ratio of 2 propanol to water at this time is defined as the degree of water repellency. For example, for 25 ml of water, the amount of 2-propanol If it is 10ml, the degree of water repellency is 0.4. The greater the degree of water repellency, the higher the water repellency of the powder. Use the surface-coated powder for cosmetics. If the water repellency is too low, , It will make makeup lasting because of being wet by sweat. On the other hand, if the water repellency is too high, Makes skin inferior, and makeup durability is not good. Specifically, the value of water repellency is preferably 0.6 to 12 200521159, and less than 1.2. Developed powders for foundations of cosmetics, etc. In order to make the appearance natural when coating, the optical characteristics of the powder are generally controlled. Specifically, for example, reducing the proportion of light reflected on the surface when light is incident on the powder and increasing the scattered light, thereby making the coating look unnatural. It disappears and can hide the shortcomings of the skin. By covering the surface of the powder with silica or titanium dioxide with different refractive indices, the scattered light can be increased relatively. However, when using a mixture of these inorganic oxides, 'if directly It has a hard feel when used, and it is necessary to perform a surface treatment in order to impart water repellency. In contrast, the present invention can simultaneously provide a soft touch by coating the powder with a metal oxide · _organic polysiloxane mixture. Sensitive water repellency, and by forming a transparent metal oxide-organic polysiloxane mixture layer on the surface of the powder, the scattered light can be increased. Next, a cosmetic material blended with the coated powder of the present invention will be described. The surface-coated powder of the present invention is surface-coated with a metal oxide-organopolysiloxane mixture, and is an excellent cosmetic material. The cosmetic center is the center, and there are no particular restrictions on the amount of skin care cosmetics, etc., but you can get the durability of the makeup, the feeling of use, and the natural outer cosmetic dosage form. , Lotion, lotion, hair cosmetic, etc. The blending of the surface-coated powder is preferably 0.1% by mass or more. Moreover, within the scope of not knowing the effects of the present invention,

目的之通常化 果或粉末感, 粉體、無機粉體、 或水溶性高分子、 可適當配合油性成分以賦予潤 體、顏料等粉體以賦予著色效 子、醇類、水等水性成分以賦 13 200521159 予濕潤感,或添加用以分散粉體、調整觸感之界面活性劑、 聚合物乳化劑等皮膜形成劑、紫外線吸收劑、保濕劑、抗 氧化劑、美容成分、pH調整劑、消泡劑、褪色防止劑、防 腐劑、香料等賦予各種效果之成分。 以下舉實施例說明本發明,但本發明不限定於該等實 施例。 處成物溶膠之壤造例1 於玻璃製燒杯内放入lm〇l鈦四異丙醇鹽(和光純藥 製)’ 一面以磁攪拌子攪拌,將lm〇1水、0 06m〇1鹽酸、異 丙醇400ml之混合液以約2ml/min的速度滴入,而製得透明 一氧化鈦溶膠。於滴入結束後立刻添加〇.2m〇1之前述化學 式(4)所不含烧氧基之二曱基聚矽氧烷與異丙醇2〇〇ml混合 液’而付到氧化鈦•二甲基聚矽氧烷混成物凝膠。因鈦四 異丙氧化物與含烷氧基之二甲基聚矽氧烷之加入莫耳比為 5 · 1,故以下將此處製得之溶膠稱為5/1混成物溶膠。 ^於玻璃製燒杯内放入Imol鈦四異丙氧化物(和光純藥 製)^ 一面以磁攪拌子攪拌,將lm〇1水、〇〇6m〇1鹽酸、異 丙醇4〇〇ml之混合液以、約2ml/min的速度滴入,而製得透明 一氧化鈦溶膠。於、、翁 -&滴入結束後立刻添加O.lmol之前述化學 式(4)所示含焓Μ I 4 _ 乳基之一甲基聚矽氧烷與異丙醇100ml混合 液而何·到氣y/l- ^JL. ^ 斌•二甲基聚矽氧烷混成物凝膠。因鈦四 、丙氧化物與含燒氧基之二曱基聚矽氧烷之加入莫耳比為 1 : 1,故以下將卟忐制 对此處製得之溶膠稱為10/1混成物溶膠。 200521159 實施例1 對氧化鈦(金紅石型,試藥特級,關東化學製)丨00份, 加入製造例1之5/1混成物溶膠20份並混合,再加入異丙 醇使其成為漿狀。基於混成物溶膠中之異丙醇及脫離之烷 氧基之考量’將被覆於粉體表面之氧化鈦/二甲基聚矽氧烷 混成物之固體成分量設定成對生成物(稱為處理後之粉體, 以下同)為約5質量%。將該等一面以電動研蛛混合粉碎, 一面使異丙醇揮發。將該等於l〇〇°c乾燥後粉碎,製得5/i 混成物被覆氧化欽。 實施例2 對乳化鈦(金紅石型,試藥特級,關東化學製)1⑽份, 加入製造例2之10/1混成物溶膠25份並混合,再加入異丙 醇使其成為漿狀。基於混成物溶膠中之異丙醇及脫離之烧 氧基之考量’將被覆於粉體表面之氧化鈦/二甲基聚矽氧燒 混成物之固體成分量設定成對生成物為約5質量%。將該等 一面以電動研蛛混合粉碎,一面使異丙醇揮發。將該等於 100 C乾燥後粉碎’製得1 〇/1混成物被覆氧化鈦。 比較例1 對氧化鈦(金紅石型,試藥特級,關東化學製)1⑼份, 將上述化學式(4)之含烷氧基之二甲基聚矽氧烷4份以異丙 醇稀釋後加入混合’再加入異丙醇使其成為漿狀。將該等 一面以電動研蛛混合粉碎,一面使異丙醇揮發。將該等於 10〇°C乾燥後粉碎,製得矽酮被覆氧化鈦。 比較例2 15 200521159 對氧化鈦(金紅石型,試藥特級,關東化學製)98 2份, 將甲基氫二院揮二甲基聚石夕氧烧〇.8份以異丙醇稀釋後加 入混合,再加入異丙醇使其成為漿狀。將該等一面以電動 研蛛混合粉碎…面使異丙醇揮發。將該等於IGGt乾燥後 粉碎’製得0.8%甲基氫二㈣二甲基聚♦氧炫被覆氧化欽。 lb較例3 對氧化鈦(金紅石型,試藥特級,關東化學製)1〇〇份, 將甲基氫二烷撐二甲基聚矽氧烷4份以異丙醇稀釋後加入 混合,再加入異丙醇使其成為漿狀❶將該等一面以電動研鲁 缽混合粉碎,一面使異丙醇揮發。將該等於loot乾燥後粉 碎t知3.8/〇甲基氫二烧撐二甲基聚石夕氧焼被覆氧化欽。 撥水性詖脸 對實軛例1、2及比較例1〜3進行撥水性評價。撥水性 評價係依以下方法進行。 , 於100ml燒杯内加入水25ml及測定樣本0 05g,一面 X磁攪拌子攪拌,一面用滴管低入2 一丙醇。於攪拌狀態下 貝取無法以目視確認浮游於液面之樣本時點之滴入量。將 、、口果整理於以下之表丨。表中之撥水化度,取2 _丙醇之滴 下置與水之容量比之值,撥水化度愈高表示撥水性愈高。The purpose is to normalize the feeling of fruit or powder, powder, inorganic powder, or water-soluble polymer, which can be appropriately blended with oily ingredients to impart powders such as emollients and pigments to impart coloring effects, alcohols, water and other aqueous ingredients to Add 13 200521159 to give a moist feeling, or add film-forming agents such as surfactants to disperse powders and adjust touch, polymer emulsifiers, UV absorbers, humectants, antioxidants, beauty ingredients, pH adjusters, consumer A foaming agent, a discoloration preventing agent, a preservative, a fragrance, and other components that impart various effects. The following examples illustrate the present invention, but the present invention is not limited to these examples. Preparation Example 1 of sol-containing soils In a glass beaker, lmmol of titanium tetraisopropoxide (manufactured by Wako Pure Chemical Industries, Ltd.) was placed in the glass beaker. While stirring with a magnetic stirrer, lmmol of water and 0 06mol of hydrochloric acid A mixture of 400 ml of isopropyl alcohol was dropped at a rate of about 2 ml / min to prepare a transparent titanium oxide sol. Immediately after the dripping was completed, 0.2 ml of a mixed solution of difluorenyl polysiloxane and isopropyl alcohol 200 ml not contained in the aforementioned chemical formula (4) of 0.2 m01 was added to pay titanium oxide. Methyl polysiloxane gel. Because the molar ratio of titanium tetraisopropoxide and dimethyl polysiloxane containing alkoxy group is 5 · 1, the sol prepared here is referred to as a 5/1 mixed sol. ^ In a glass beaker, put 1 mol of titanium tetraisopropoxide (manufactured by Wako Pure Chemicals) ^ While stirring with a magnetic stirrer, lm01 water, 006m1 hydrochloric acid, isopropyl alcohol (400ml) The mixed solution was dropped at a rate of about 2 ml / min to prepare a transparent titanium oxide sol. At the end of the dripping, immediately add 0.1 ml of the mixed solution of methyl polysiloxane and 100 ml of isopropyl alcohol containing enthalpy M I 4 _ shown in the aforementioned chemical formula (4) of 0.1 mol. To air y / l- ^ JL. ^ Bin • Dimethyl polysiloxane mixture gel. Because the molar ratio of titanium tetra, propoxide, and difluorenyl polysiloxane containing oxyl group is 1: 1, the sol prepared here is referred to as a 10/1 mixture. Sol. 200521159 Example 1 To 00 parts of titanium oxide (rutile type, reagent grade, manufactured by Kanto Chemical Co., Ltd.) 丨 00 parts, adding 20 parts of the 5/1 mixture sol of manufacturing example 1 and mixing, and then adding isopropanol to make a slurry . Based on the consideration of isopropanol and detached alkoxy groups in the mixed sol ', the solid content of the titanium oxide / dimethyl polysiloxane compound coated on the surface of the powder is set as a pair of products (called treatment The latter powder is the same hereinafter as about 5 mass%. These sides are pulverized by mixing with an electric grind spider, and the isopropyl alcohol is volatilized. This is equal to 100 ° C., dried, and pulverized to obtain a 5 / i mixture coated with oxanthine. Example 2 To 1 part of emulsified titanium (rutile type, test reagent special grade, manufactured by Kanto Chemical), 25 parts of the 10/1 mixed product sol of Manufacturing Example 2 was added and mixed, and then isopropyl alcohol was added to make a slurry. Based on the consideration of isopropanol in the mixed sol and the sintered oxyl group, the solid content of the titanium oxide / dimethyl polysiloxane fired mixture coated on the powder surface was set to about 5 masses for the product. %. These sides were mixed and pulverized with an electric grinding spider, while isopropyl alcohol was volatilized. This was equal to 100 C and then pulverized, to obtain a 10/1 mixture-coated titanium oxide. Comparative Example 1 To 1 part of titanium oxide (rutile type, reagent grade, manufactured by Kanto Chemical), 4 parts of alkoxy-containing dimethylpolysiloxane of the above chemical formula (4) was diluted with isopropanol and added. Mix 'and add isopropanol to make a slurry. These sides were mixed and pulverized with an electric grinding spider, while isopropyl alcohol was volatilized. This was dried at a temperature of 100 ° C and then pulverized to obtain a silicone-coated titanium oxide. Comparative Example 2 15 200521159 To 98 parts of titanium oxide (rutile type, test reagent special grade, manufactured by Kanto Chemical), 0.8 parts of methyl hydrogen dihydrogenated dimethyl polystone was burned with isopropyl alcohol Add the mixture and add isopropanol to make it a slurry. These sides are pulverized by mixing with an electric grinding spider ... the sides are allowed to volatilize isopropyl alcohol. This equal to IGGt was dried and pulverized 'to obtain 0.8% methyl hydrogen difluoride dimethylpolyoxoxan coated oxin. lb Comparative Example 3 For 100 parts of titanium oxide (rutile type, reagent grade, manufactured by Kanto Chemical), 4 parts of methylhydrodialkyldimethylpolysiloxane were diluted with isopropanol and mixed. Isopropanol was further added to make it into a slurry form. The isopropanol was mixed and pulverized with an electric grinder while the isopropanol was volatilized. This powder was crushed after drying, and 3.8 / 0 methyl hydrogen disulfide dimethylpolylithium oxoxane was coated with oxin. Water-repellent face removal The water-repellent evaluation was performed on the actual yoke examples 1, 2 and comparative examples 1 to 3. The water repellency evaluation was performed according to the following method. Into a 100ml beaker, add 25ml of water and 0 05g of the measurement sample, while stirring with an X magnetic stir bar, and lowering 2 propanol with a dropper. In the stirring state, the drop amount at the time of taking a sample that cannot be visually confirmed floating on the liquid surface. Organize,, and fruit in the following table 丨. For the degree of water repellency in the table, take the value of the volume ratio of 2 _ propanol drop and water, the higher the water repellency, the higher the water repellency.

16 200521159 由實施例1、2之結果,可了解藉由改變起始物質之比 (鈦四異丙氧化物與含烷氧基之二甲基聚矽氧烷之加入 比),即使於同一處理量亦能控制撥水性的程度。由比較例 1之結果,可了解僅有混成物原料之含烷氧基二甲基聚矽氧 烷並無法呈現充分的撥水性。 對實施例1、2及被覆處理前之氧化鈦,使用變角色差 計進行評價。於半透明之膠帶(住友3訄製)之黏著面,用刷 子塗布評價樣本,並以變角色差計(特克瓦魯多公司製,多 重分光勾尼歐光度計)進行測定。入射角定為一 5〇、受光角 癱 定為5〇〜80〇之範圍(圖丨)。將此時亮度(γ)與受光角之關係 作圖,由結果可確認實施例丨、2之被覆處理後氧化鈦較未 處理之氧化鈦,於低角度側之亮度下降,相對的高角度側 之免度則上升。因低角度側係對應於正反射光,高角度側 對應於散射光,故可確認以混成物溶膠被覆可以提高光之 · 散射能力。 實施例3、4 製造配合上述實施例1、2及比較例1〜3之粉末狀粉 _ 底即以下表所不組成之粉末狀粉底’由40名專門評審員 對塗勻擴展」、「密合感」、「化粧持久性」、「自然 外觀」等特性進行使用測試。由判定為良好之人數,依以 下基準進行評價。評價結果整理於表2。 評價 ◎ : 3 5名以上 Ο :25〜34名 17 200521159 △ :15〜24名 X:未滿1 5名 表2 成分名稱 實施例 比較例 3 4 4 5 6 1 5/1混成物被覆氧化鈦(實施例1) 15 — — — — 2 10/1混成物被覆氧化鈦(實施例2) — 15 — — — 3 含烷氧基之二甲基聚矽氧烷被覆氧化鈦 (比較例1) _ _ 15 — _ 4 甲基氫二烷撐聚矽氧烷被覆氧化鈦(比較 例2) _ _ — 15 — 5 甲基氫二烷撐聚矽氧烷被覆氧化鈦(比較 例3) — — _ — 15 6 雲母 10 10 10 10 10 7 滑石 5 5 5 5 5 8 尼龍粉末 5 5 5 5 5 9 微粒子氧化鋅 10 10 10 10 10 10 著色顏料 8 8 8 8 8 11 絹雲母 剩餘 剩餘 剩餘 剩餘 剩餘 12 角鯊烧 5 5 5 5 5 13 凡士林 4 4 4 4 4 14 矽酮油 3 3 3 3 3 15 防腐劑 適量 適量 適量 適量 適量 16 香料 適量 適量 適量 適量 適量 (評價項目) 塗勻擴展 ◎ ◎ Δ Δ 〇 密合感 〇 ◎ 〇 Δ X 化粧持久性 ◎ ◎ Δ Δ X 自然外觀 ◎ ◎ Δ X Δ16 200521159 From the results of Examples 1 and 2, it can be understood that by changing the ratio of starting materials (addition ratio of titanium tetraisopropoxide to alkoxy-containing dimethylpolysiloxane), even in the same treatment The amount can also control the degree of water repellency. From the results of Comparative Example 1, it is understood that only the alkoxydimethyl-containing polysiloxane containing the raw material of the mixture cannot exhibit sufficient water repellency. The titanium oxides in Examples 1 and 2 and before the coating treatment were evaluated using a variable-ratio differential meter. The evaluation sample was coated with a brush on the adhesive surface of a translucent tape (manufactured by Sumitomo 3), and measured with a variable-actimeter (manufactured by Tecvarudo, multi-spectrometer). The incident angle is set to be 50, and the light receiving angle is set to range from 50 to 80 (Figure 丨). By plotting the relationship between the brightness (γ) and the light receiving angle at this time, it can be confirmed from the results that the coated titanium oxide of Example 丨 and 2 has a lower brightness on the low-angle side and a higher-angle side than the untreated titanium oxide. The degree of relief is increased. Since the low-angle side corresponds to the specular reflection light and the high-angle side corresponds to the scattered light, it can be confirmed that coating with a mixed substance sol can improve the light-scattering ability. Examples 3 and 4 Production of powdery powders according to the above Examples 1, 2 and Comparative Examples 1 to 3 _ The bottom is a powdery foundation not composed of the following table. 'The uniform spreading was extended by 40 special reviewers.' "Combination", "makeup durability", "natural appearance" and other characteristics. The number of people judged to be good was evaluated based on the following criteria. The evaluation results are summarized in Table 2. Evaluation ◎: 3 or more 5 0: 25 to 34 17 200521159 △: 15 to 24 X: less than 1 5 Table 2 Composition name examples Comparative Example 3 4 4 5 6 1 5/1 mixture coated with titanium oxide ( Example 1) 15 — — — — 2 10/1 mixture coated with titanium oxide (Example 2) — 15 — — — 3 Alkoxy-containing dimethylpolysiloxane coated titanium oxide (Comparative Example 1) _ _ 15 — _ 4 Methyldioxane-polysiloxane coated titanium oxide (Comparative Example 2) _ — 15 — 5 Methyldioxane-polysiloxane coated titanium oxide (Comparative Example 3) — — _ — 15 6 Mica 10 10 10 10 10 7 Talc 5 5 5 5 5 8 Nylon powder 5 5 5 5 5 9 Micro-particle zinc oxide 10 10 10 10 10 10 Colored pigment 8 8 8 8 8 11 Sericite remaining remaining remaining remaining remaining 12 Horned Shark 5 5 5 5 5 13 Vaseline 4 4 4 4 4 14 Silicone oil 3 3 3 3 3 15 Preservatives appropriate amount appropriate amount appropriate amount 16 Spices appropriate amount appropriate amount appropriate amount (evaluation item) Spread evenly extended ◎ Δ Δ 〇 Feeling of closeness ◎ ◎ ΔX Makeup durability ◎ Δ Δ X Natural appearance ◎ Δ Δ X Δ

製造方法 A:將成分1〜11混合分散。 B:將成分12〜16混合。 C:將B加入混合至A,並粉碎以製得粉末狀粉底。 由表之結果可以了解,本發明之實施例3、4在所有項 18 200521159 目中皆得到良好之結果。 實施例5 對黃氧化鐵100份,添加混合製造例丨之5/1混成物溶 膠20份並混合,再加入異丙醇使其成為漿狀。考量混成物 溶膠中之異丙醇及脫離之烷氧基,將被覆於粉體表面之氧 化鈦/二甲基聚矽氧烷混成物之固體成分量設定成對生成物 為約5質量%。將該等一面以電動研砵混合粉碎,一面使異 丙醇揮發。將該等於l00°c乾燥後粉碎,製得5/1混成物被 覆頁虱化鐵。以同樣方式進行,以製得5/1混成物被覆氧化 鐵紅、黑氧域。所得到之料5/1混成物被覆氧化鐵顏色 不污濁,與僅以石夕_被覆處理者相比為㈤等程度。撥水化 度皆為0.6以上、未滿〇·8之範圍。 實施合,丨 、·子畀氧化鐵100份,添加製造例2之1〇/1混成物溶膠 ”份並混',再加入異丙醇使其成為漿狀。考量混成物溶 膠中_之異丙醇及脫離之烷氧基,將被覆於粉體表面之氧化 :太/ -甲旦基聚矽氧烷混成物之固體成分量設定成對生成物為 j 5質里%。將該等一面以電動研缽混合粉碎,一面使異丙 二至,I亥等於1()(rc乾燥後粉碎,製得聰混成物被 二Γ乳t鐵。以同樣方式進行’製得1G/1混成物被覆氧化 色化鐵。所得狀料削混成物被覆氧化鐵顏 與僅以⑦_被覆處理者相比為同等程度。撥水 化度皆為0.8以上、未滿"之範圍。 200521159 對絹雲母100份,添加製造例1之5/1混成物溶膠2〇 份並混合,再加入異丙醇使其成為漿狀。考量混成物溶膠 中之異丙醇及脫離之烷氧基,將被覆於粉體表面之氧化鈦/ 二甲基聚石夕氧烧混成物之固體成分量設定成對生成物為約 5質量%。將該等一面以電動研蛛混合粉碎,一面使異丙醇 揮發。將該等於l〇〇°C乾燥後粉碎,製得5/1混成物被覆絹 雲母。以同樣方式進行,製得到5/1混成物被覆滑石、雲母。 撥水化度皆為0 · 6以上、未滿〇 · 8之範圍。 實施例8 對絹雲母100份,添加製造例2之1 〇/1混成物溶膠25 份並混合,再加入異丙醇使其成為漿狀。考量混成物溶膠 中之異丙醇及脫離之烷氧基,將被覆於粉體表面之氧化鈦/ 二甲基聚矽氧烷混成物之固體成分量設定成對生成物為約 5質量%。將該等一面以電動研蛛混合粉碎,一面使異丙醇 揮發。將該等於100°C乾燥後粉碎,製得1〇/1混成物被覆 絹雲母。以同樣方式進行,製得1〇/1混成物被覆滑石、雲 母。撥水化度皆為1.0以上、未滿1.2之範圍。 實施例9粉末狀粉底 成分 (%) 1· 5/1混成物被覆氧化鈦(實施例1) 1〇.〇 2· 10/1混成物被覆氧化鈦(實施例2) 1〇.〇 3· 5/1混成物被覆滑石(實施例8) 15.0 4· 10/1混成物被覆絹雲母(實施例8) 剩餘 5.球狀尼龍粉末 5«0 200521159 6 ·—氧化碎 7· 10/1混成物被覆黃氧化鐵、氧化鐵紅、 黑氧化鐵(實施例6) 5.0 5.0 8·液體石蠟 9·聚異丁稀 10 ·三異硬脂酸二甘油酯 11·美容成分 12 ·香料 製造方法 4.0 2.0 3.0 適量 適量Production method A: Ingredients 1 to 11 are mixed and dispersed. B: Mix ingredients 12-16. C: B was added to A, and pulverized to obtain a powdery foundation. As can be understood from the results of the table, Examples 3 and 4 of the present invention obtained good results in all items. Example 5 To 100 parts of yellow iron oxide, 20 parts of the 5/1 mixture of the manufacturing example 丨 was added and mixed, and then isopropyl alcohol was added to make it into a slurry. Taking into account the isopropanol and detached alkoxy groups in the sol, the solid content of the titanium oxide / dimethylpolysiloxane mixture coated on the surface of the powder was set to about 5% by mass to the product. These sides were pulverized by electric research and mixing, while isopropanol was volatilized. This was equal to 100 ° C and dried and pulverized to obtain a 5/1 mixture coated with iron flea. In the same manner, a 5/1 mixture was coated with iron oxide red and black oxygen domains. The obtained material 5/1 mixture was coated with iron oxide with a non-staining color, and was about ㈤ grade compared to those treated with Shi Xi_ only. The water repellency is in the range of 0.6 or more and less than 0.8. To carry out the combination, add 100 parts of ferric oxide, add "part 10/1 mixed sol" of Manufacturing Example 2 and mix it, and then add isopropanol to make it into a slurry. Consider the difference in the mixed sol Propanol and detached alkoxy groups are used to oxidize the surface of the powder: too much-the solid content of the methyldenyl polysiloxane mixture is set to 5% by mass of the product. Use an electric mortar to mix and pulverize, while isopropyl diisocyanate is equal to 1 () (rc after drying and crushing, the Cong mixture is made of two Γ milk t iron. The same method is used to obtain 1G / 1 mixture. Coated with oxidized iron. The iron oxide pigment coated with the obtained material is equivalent to that treated with ⑦ only. The degree of water repellency is above 0.8 and less than ". 200521159 for sericite 100 parts, 20 parts of the 5/1 mixed product sol of Manufacturing Example 1 was added and mixed, and then isopropyl alcohol was added to make a slurry. Considering the isopropyl alcohol and the detached alkoxy group in the mixed material sol, it will be covered with The solid content of the titanium oxide / dimethyl polyoxygen sintered mixture on the surface of the powder is set to about 5 for the product. The mixture is pulverized by electric grinding spider while volatilizing isopropanol. The dried powder is equal to 100 ° C and pulverized to obtain a 5/1 mixture coated sericite. A mixture of 5/1 was coated with talc and mica. The degree of water repellency was in the range of 0. 6 or more and less than 0.8. Example 8 100 parts of sericite was added and 1/10/1 mixture of Production Example 2 was added. 25 parts of sol are mixed, and then isopropanol is added to make it into a slurry. Considering the isopropanol and detached alkoxy group in the sol, the titanium oxide / dimethyl polysiloxane will be coated on the surface of the powder. The solid content of the mixture is set to about 5% by mass of the product. These are mixed and pulverized with an electric spider, and the isopropyl alcohol is volatilized. This is dried at 100 ° C and pulverized to obtain 10 / 1. The mixture is coated with sericite. In the same manner, a 10/1 mixture is coated with talc and mica. The degree of water repellency is in the range of 1.0 or more and less than 1.2. Example 9 Powdery foundation component (%) 1 · 5/1 mixture coated with titanium oxide (Example 1) 10.0. 2 · 10/1 mixture coated Titanium (Example 2) 10.0. 5/1 mixture coated talc (Example 8) 15.0 4 · 10/1 mixture coated sericite (Example 8) Remaining 5. Spherical nylon powder 5 « 0 200521159 6 · —oxidized crushed 7 · 10/1 mixture coated with yellow iron oxide, iron oxide red, black iron oxide (Example 6) 5.0 5.0 8 · liquid paraffin 9 · polyisobutylene 10 · triisostearic acid Diglyceride 11 · Beauty ingredients 12 · Perfume manufacturing method 4.0 2.0 3.0 Appropriate amount

Α:將成分1〜7混合。 Β:將成分8〜10加溫溶解,並添加成分u及成分a。 C:將B加入至A並混練,以鎚粉碎機粉碎。 D:加壓成型於金屬盒而製得粉末狀粉底。 所得到之粉末狀粉底,塗勻擴展性、親膚性良好,具 有適度之密合感,且得到自然外觀,化粧持久性亦優異f 實施例10油性粉底 成分 1 · 5 /1混成物被覆氧化鈦(實施例1) 2 · 10 /1混成物被覆氧化鈦(實施例2 ) 3. 氧化鋅 4. 5/1混成物被覆絹雲母(實施例7) 5· 10/1混成物被覆雲母(實施例7) 6· 5/1混成物被覆黃氧化鐵、氧化鐵紅、 黑氧化鐵(實施例5) (%) 8.0 6.0 10.0 剩餘 10.0 7.0A: Ingredients 1 to 7 are mixed. Β: Components 8 to 10 are dissolved by heating, and component u and component a are added. C: B is added to A and kneaded, and crushed with a hammer mill. D: A powdery foundation is obtained by pressure molding on a metal box. The obtained powdery foundation has uniform spreadability, good skin-friendliness, moderate adhesion, natural appearance, and excellent makeup durability. Example 10 Oily foundation component 1 · 5/1 mixture is coated and oxidized Titanium (Example 1) 2 · 10/1 mixture coated with titanium oxide (Example 2) 3. Zinc oxide 4. 5/1 mixture coated sericite (Example 7) 5 · 10/1 mixture coated mica ( Example 7) The 6 · 5/1 mixture was coated with yellow iron oxide, red iron oxide, and black iron oxide (Example 5) (%) 8.0 6.0 10.0 Remaining 10.0 7.0

21 200521159 7 ·角震燒 15.0 8 ·巴西棕櫚蝶 3.0 9 ·微結晶性蟻 5.0 10·甲基聚矽氧烷 10.0 H·十甲基環戊石夕氧烧 1〇.〇 12·美容成分 適量 13 ·香料 適量 製造方法21 200521159 7 · Horn shock burn 15.0 8 · Brazil palm butterfly 3.0 9 · Microcrystalline ant 5.0 10 · Methylpolysiloxane 10.0 H · Decamethylcyclopentyl oxane burn 10.0012 · Appropriate amount of beauty ingredients 13 · Proportion of flavor production method

A:將成分1〜6混合。 B:將成分7〜10以90°C溶解,並添加成分11。 C:將B加入至A,使之融合。 D:加入成分12〜13至C,並混合均勻。 E:將D加溫成型於金屬盒而製得油性粉底。 所得到之油性粉底具塗勻擴展性、密合感,得到自然 外觀,且化粧持久性優異。 (%) 5.0 3.0 5.0 % 4.0 6.0 1.0A: Mix ingredients 1-6. B: Components 7 to 10 are dissolved at 90 ° C, and component 11 is added. C: Add B to A to blend. D: Add ingredients 12-13 to C and mix well. E: An oily foundation was prepared by heating D into a metal box. The obtained oily foundation has uniform spreadability, a close feeling, a natural appearance, and excellent makeup durability. (%) 5.0 3.0 5.0% 4.0 6.0 1.0

實施例11油中水型乳化耠底 成分 1 · 5/1混成物被覆氧化鈦(實施例1) 2· 10/1混成物被覆氧化鈦(實施例2) 3· 5/1混成物被覆絹雲母(實施例7) 4_ 5/1混成物被覆黃氧化鐵、氧化鐵紅 黑氧化鐵(實施例5) 5. 二癸酸新戊二醇酯 6. 黃豆卵磷脂 22 200521159 7. 山梨糖醇酐倍半油酸酯 2.0 8. 純水 剩餘 9. 丙二醇 9.0 10. 防腐劑 適量 11. 十甲基環戊矽氧烷 20.0 12. 角鯊烷 5.0 13. 聚丙烯酸烧酯粉體 3.0 14. 美容成分 適量 15. 香料 適量 製造方法 A:將成分5〜7溶解後,添加成分1〜4並充分混合。 B:將成分11〜15以均質機混合後,加入A並分散混合。 C:將另外溶解混合之成分8〜10添加至B加並乳化混 合。 D:將C進行脫泡以製得油中水型粉底。 (%) 35.0 剩餘 5.0 10.0 所製得之油中水型粉底具塗勻擴展性、密合感,得到 然外觀,且化粧持久性亦優異。 f施例12眼影 成分 1 · 10/1混成物被覆絹雲母(實施例8) 2. 10/1混成物被覆滑石(實施例8) 3· 10/1混成物被覆氧化鈦(實施例2) 4· 1 〇/1混成物被覆黃氧化鐵、氧化鐵紅 黑氧化鐵(實施例6) 23 200521159 5. 氧化鐵紅被覆被覆雲母氧化鈦 1〇.〇 6. 球狀聚苯乙烯粉末 5.0 7. 無孔質球狀二氧化矽 5.0 8. 蘋果酸二異硬脂酸酯 4.0 9. 角鯊烷 4.0 10. 三異硬脂酸二甘油酯 4.0 14. 美容成分 適量 15. 香料 適量 製造方法 — A:將成分1〜7混合。 B:將成分8〜10加溫溶解,並於其中添加成分11及成 分 12 ° , C:將B加入A並混練後,以鎚粉碎機粉碎。 鼻 D:擠壓成型於金屬盤内而製得眼影Example 11 Oil-in-water emulsified base component 1 · 5/1 mixture coated with titanium oxide (Example 1) 2 · 10/1 mixture coated with titanium oxide (Example 2) 3 · 5/1 mixture-coated silk Mica (Example 7) 4_ 5/1 mixture coated with yellow iron oxide, iron oxide red and black iron oxide (Example 5) 5. Neopentyl glycol dicaprate 6. Soy lecithin 22 200521159 7. Sorbitol Anhydride sesquioleate 2.0 8. Pure water remaining 9. Propylene glycol 9.0 10. Preservative amount 11. Decamethylcyclopentasiloxane 20.0 12. Squalane 5.0 13. Polyacrylic acid powder 3.0 14. Beauty Appropriate amount of ingredients 15. Producing method of proper amount of flavor A: After dissolving ingredients 5 to 7, add ingredients 1 to 4 and mix well. B: After mixing ingredients 11-15 with a homogenizer, add A and disperse and mix. C: 8 to 10 ingredients which are separately dissolved and mixed are added to B and emulsified and mixed. D: C is defoamed to obtain an oil-in-water foundation. (%) 35.0 Remaining 5.0 10.0 The oil-in-water foundation prepared has a uniform spreadability and a sense of closeness, giving a natural appearance and excellent makeup durability. f Example 12 Eye shadow component 1 · 10/1 mixture coated with sericite (Example 8) 2. 10/1 mixture coated with talc (Example 8) 3 · 10/1 mixture coated with titanium oxide (Example 2) 4. · 1〇 / 1 mixture was coated with yellow iron oxide, iron oxide red and black iron oxide (Example 6) 23 200521159 5. Iron oxide red covered with mica titanium oxide 10.0.0. Spherical polystyrene powder 5.0 7 Nonporous spherical silica 5.0 8. Diisostearate malate 4.0 9. Squalane 4.0 10. Diglyceryl triisostearate 4.0 14. Proper amount of beauty ingredients 15. Proper method of fragrance — A: Mix ingredients 1-7. B: dissolve ingredients 8 to 10 under heating, add ingredients 11 and 12 ° to them, C: add B to A and knead it, and pulverize with a hammer mill. Nose D: squeezed into a metal plate to make an eye shadow

所製得之眼影發色良好,與親膚性良好,有適度之密 合感,且化粧持久性優異。 I 實施例13睫毛膏 成分 (%) 1. 巴西棕櫚蠟 4.0 2. 蜜躐 4.0 3. 香茅酸季戊四酯 2.0 4. 山俞醇 1.5 5. 蔗糖脂肪酸酯 1.5 6. 山梨糖醇酐倍半油酸酯 2.0 24 200521159 7. 聚氧乙烯山梨糖醇酐單油酸酯1·〇 (20Ε.Ο.) 8· 5/1混成物被覆氧化鈦(實施例1) 2.0 9·含全氟烷基酯被覆黑色氧化鐵 8.0 10· 5/1混成物被覆雲母(實施例7) 6.0 11. 純水 剩餘 12. 氫氧化鈉 0.5The produced eyeshadows had good hair color, good skin-friendliness, moderate adhesion, and excellent makeup durability. I Example 13 Mascara Ingredients (%) 1. Carnauba wax 4.0 2. Melissa 4.0 3. Pentaerythryl citronellate 2.0 4. Sorbitol 1.5 5. Sucrose fatty acid ester 1.5 6. Sorbitol anhydride Silsesquioleate 2.0 24 200521159 7. Polyoxyethylene sorbitan monooleate 1.0 · (20E.O.) 8 · 5/1 mixture coated with titanium oxide (Example 1) 2.0 9 · All containing Fluoroalkyl ester coated black iron oxide 8.0 10 · 5/1 mixture coated mica (Example 7) 6.0 11. Pure water remaining 12. Sodium hydroxide 0.5

13· 1,3— 丁二醇 8.0 14·防腐劑 適量 15.聚丙烯酸烷酯水分散溶液 300 16·尼龍粉末 4〇 17·美容成分 適量 1 8 ·香料 適量 製造方法 Α:將成分1〜4以l〇〇°C加熱溶解,添加成分5〜7並使其13 · 1,3—butanediol 8.0 14 · appropriate amount of antiseptic 15. polyalkyl acrylate aqueous dispersion solution 300 16 · nylon powder 4〇17 · appropriate amount of cosmetic ingredients 1 8 · appropriate amount of perfume A: Ingredients 1 ~ 4 Heat and dissolve at 100 ° C, add ingredients 5 to 7 and make

溶解。添加成分8〜10於其,並充分混練使粉體分散,並使 溫度成為75°C。 B:將成分U〜17混合溶解,並使溫度成為75°C。 C·將B加入A並乳化混合。之後進行脫泡並冷卻後, 添加成分18而製得睫毛膏。 的附著性良好 (%) 10.0 所製付之睫毛膏發色性及對睫毛 實施例 成分 1 ·微結晶性蠛 25 200521159 5.0 5.0 7.0 5.0 10.0 剩餘 10.0 10.0 5.0 1.0 適量 適量 之後進行脫 2. 精製地蠟 3. 聚乙烯聚丙烯共聚物 4. 液狀含水羊毛脂 5. 凡士林 6. 異辛酸鯨蠟酯 7. 液體石蠟 8. 著色顏料 9. 雲母鈦 10· 5/1混成物被覆氧化鈦(實施例1) 11.染料 1 2.美容成分 13.香料 製造方法 A:將成分1〜7以110°C加熱溶解。 B:於A中加入成分8〜13,並以90°C分散 泡 C:將B充填於容器,冷卻以製得口紅。 所製得之口紅延展性良好且具潤滑性,使用性良好。 實施例15防曬化粧料 成分 (%) 1. 5/1混成物被複氧化鈦(實施例1) 1〇.〇 2. 5/1混成物被複氧化鈦(實施例2) 1〇.〇 3. 十甲基環戊矽氧烷 20.0 4. 二癸酸新戊二醇酯 5.0 26 200521159 5·對曱氧基桂皮酸2〜乙基己酯 1〇 () 6. 4—第三丁基一 4’~甲氧基二苯甲醯基5.〇 甲烷 3.0 適量 5.0 適量 剩餘Dissolve. Add ingredients 8 to 10 and mix thoroughly to disperse the powder and bring the temperature to 75 ° C. B: The components U to 17 were mixed and dissolved, and the temperature was set to 75 ° C. C. Add B to A and emulsify and mix. After defoaming and cooling, component 18 was added to prepare a mascara. Good adhesion (%) 10.0 The color development of the mascara made and the ingredients for the eyelashes Example 1 · Microcrystalline 蠛 25 200521159 5.0 5.0 7.0 5.0 10.0 The remaining 10.0 10.0 5.0 1.0 The appropriate amount and the amount is removed 2. Refinedly Wax 3. Polyethylene polypropylene copolymer 4. Liquid lanolin 5. Vaseline 6. Cetyl isooctanoate 7. Liquid paraffin 8. Color pigment 9. Mica titanium 10. 5/1 mixture coated with titanium oxide (implementation Example 1) 11. Dye 1 2. Cosmetic ingredients 13. Flavor manufacturing method A: Ingredients 1 to 7 are dissolved by heating at 110 ° C. B: Add ingredients 8 to 13 to A and disperse at 90 ° C. C: Fill the container with B and cool to make lipstick. The obtained lipstick has good ductility, lubricity and good usability. Example 15 Sunscreen cosmetic ingredients (%) 1. The 5/1 mixture was coated with titanium oxide (Example 1) 10.2. The 5/1 mixture was coated with titanium oxide (Example 2) 10.0. 3. Decamethylcyclopentylsiloxane 20.0 4. Neopentyl glycol didecanoate 5.0 26 200521159 5. P-oxyl cinnamic acid 2 ~ ethylhexyl ester 10 () 6. 4-Third-butyl One 4 '~ methoxydibenzylidene 5.0 methane 3.0 appropriate amount 5.0 appropriate amount remaining

7·聚氧乙烯曱基聚矽氧烷共聚物 8. 香料 9. 乙醇 I 〇 ·美容成分 II _純水 製造方法 Α:將成分1〜8以均質機分散混合。 合 Β:於Α中添加成分9〜11之混合溶解物並將其乳化混 而製得防曬化粧料。 所製得之防曬化粧料具有高紫外線遮蔽效果,且白色 度亦不顯眼,塗勻擴展性等使用性良好。 本發明之表面被覆粉體中被覆表面之金屬氧化物•有 機聚矽氧烷混成物,藉由改變金屬氧化物與有機聚矽氧烷7. Polyoxyethylene fluorenyl polysiloxane copolymer 8. Fragrance 9. Ethanol I 〇 · Cosmetic ingredients II _ pure water Manufacturing method A: Disperse and mix ingredients 1 to 8 with a homogenizer. Combination Β: Adding a mixed solution of ingredients 9 to 11 to Α and emulsifying and mixing them to prepare a sunscreen cosmetic. The prepared sunscreen cosmetic has a high ultraviolet shielding effect, and the whiteness is not conspicuous, and the usability such as spreading and spreading is good. The metal oxide-organic polysiloxane mixture of the surface-coated powder in the surface-coated powder of the present invention, by changing the metal oxide and the organic polysiloxane

之比例,可以調整撥水性,故藉由調整撥水性,即使對作 為母體之粉體附著同量之混成物,亦可改變粉體表面之撥 水性。 又’上述金屬氧化物•有機聚矽氧烷混成物於可見光 區具有南透明性’故不會損害作為母體之粉體的色澤,且 可以於粉體表面形成折射率經控制之均一的膜,故可改變 母粉體之光學性質。 再者’金屬氧化物•有機聚矽氧烷混成物因具有來自 27 200521159 有機聚石夕氧烷之柔軟性,故可得到具良好使用感之表面被 覆粉體。又,配合本發明表面被覆粉體之化粧料在塗布時 觸感良好’且實施化粧時外觀自然。 【圖式簡單說明】 之受 圖1 ’係表示本發明之表面被覆氧化鈦與未處理 光角與亮度(Y)之關係圖。 肽The proportion can adjust the water repellency, so by adjusting the water repellency, the water repellency on the surface of the powder can be changed even if the same amount of mixture is attached to the powder as the mother body. Also, the above-mentioned metal oxide-organic polysiloxane mixture has southern transparency in the visible light region, so it does not damage the color of the powder as a matrix, and it can form a uniform and controlled refractive index film on the surface of the powder. Therefore, the optical properties of the mother powder can be changed. Furthermore, the metal oxide / organic polysiloxane mixture has the softness of 27 200521159 organic polysiloxanes, so a surface-coated powder having a good feeling of use can be obtained. In addition, the cosmetic material blended with the surface-coated powder of the present invention has a good feel when applied 'and a natural appearance when makeup is applied. [Brief description of the drawings] Acceptance Fig. 1 'is a graph showing the relationship between the surface-coated titanium oxide and the untreated light angle and brightness (Y) of the present invention. Peptide

【主要元件符號說明】 益[Description of main component symbols]

2828

Claims (1)

200521159 十、申請專利範圍: 1 · 一種表面被覆粉體,係以有機聚矽氧烷與金屬氧化物 ;刀子層人複合化之金屬氧化物•有機聚矽氧燒混成物, 進行表面被覆。 2·如申請專利範圍第1項之表面被覆粉體,其中該金屬 氧化物•有機聚矽氧烷混成物中之金屬氧化物,係擇自氧 化鈦氧化鍅及二氧化矽中之1種或2種以上之金屬氧化 物0 3·如申請專利範圍第1項或第2項之表面被覆粉體,其 籲 中A金屬氧化物•有機聚石夕氧烧混成物中之有機聚石夕氧 燒*’係以下述通式(1)所表示之殘基:200521159 10. Scope of patent application: 1. A surface-coated powder, which is composed of organic polysiloxane and metal oxide; a metal oxide-organic polysiloxane sintered composite compounded by a knife layer, for surface coating. 2. The surface-coated powder according to item 1 of the scope of patent application, wherein the metal oxide in the metal oxide-organic polysiloxane mixture is selected from one of titanium oxide hafnium oxide and silicon dioxide or Two or more kinds of metal oxides 0 3 · If the surface-coated powder of item 1 or item 2 of the scope of patent application, it calls for A metal oxides / organic polyliths Burning * 'is a residue represented by the following general formula (1): Y — S i — — S i--— S i O —S i —Ύ ί 1) R ^ R ^ a ^ R R [式中’ R為碳數i〜22之烷基、芳香基或芳烷基,可為 相同或相異;γ為以—R、—0一或_111_8丨(—〇_)3表示Y — S i — — S i --— S i O —S i —Ύ ί 1) R ^ R ^ a ^ RR [wherein R is an alkyl, aromatic or aralkyl group having a carbon number of i to 22 , Can be the same or different; γ is represented by —R, —0 一 or _111_8 丨 (—〇_) 3 之基(惟,R1為碳數1〜5之烷撐基),可為相同或相異,其中 至少有 1 個為一 0 —或—R1 — Si( — 0 — )3 ;又,n=1〜1〇〇、 m=〇〜5]。 4.如申請專利範圍第1項之表面被覆粉體,其中,通式 (1)中之R為甲基。 5 · —種表面被覆粉體之製造方法,係用來製造申請專利 範圍第1項之表面被覆粉體,其特徵為:將金屬醇鹽之部分 水解物與末端或側鏈具有反應性官能基之有機聚石夕氧燒反 應而製得之混成物’被覆於粉體表面,之後再進行乾燥。 29 200521159 6·如中請專利範㈣5項之方法,其中,該末端或側鍵 反應性g能基之有機聚矽氧烷,係以下述通式 示之有機聚矽氧烷衍生物:(But R1 is an alkylene group having 1 to 5 carbon atoms), which may be the same or different, at least one of which is a 0 —or —R1 —Si (— 0 —) 3; and, n = 1 to 100, m = 0 to 5]. 4. The surface-coated powder according to item 1 of the patent application scope, wherein R in the general formula (1) is a methyl group. 5 · —A method for manufacturing a surface-coated powder, which is used to manufacture the surface-coated powder of the first scope of the patent application, which is characterized in that a part of the hydrolysate of the metal alkoxide has a reactive functional group at the terminal or side chain The mixture obtained by the organic polylithic oxy-baking reaction is coated on the surface of the powder and then dried. 29 200521159 6. The method according to item 5 of the patent application, wherein the terminal or side-bond reactive g-energy-containing organopolysiloxane is an organopolysiloxane derivative represented by the following general formula: [式中,R為碳數1〜22之烷基、芳香基或芳烷基, 相同或相異;X為以—H、— R或―Rl_Si(—〇r2—)3表; 之基(惟,R1為碳*卜5之烧撐基,R2U或碳數J J 基)’可為相同或相異,其中至少# i個為—H或—r : ΓΛΏ 2 _ \ · 1 卜 OR2—);又 100、m=0〜5] 7.如申請專利範圍第6項之方法,其中通式 為曱基。 之R 8.如申請專利範圍第6項之方法,其中通式(2)之有機 聚矽氧烷衍生物,係以下述通式(3)所表示之化合物: CHi . CHa l <R20)aS i -R、S i_ I CHa -o-S CHi I i — R1 —S i (〇m (3) CHB CHa (式中,R1表示碳數2〜4之烷撐基,R2為一 CIi3或— C2H5,η 為 6〜16) 〇 9.-種化粧品用粉體,係由中請專利範圍第ι項~第4 項中任一項之表面被覆粉體所構成。 Η)·-種化粧料’係含有中請專利範圍第9項之化粧品 用粉體。 30[Wherein R is an alkyl group, aromatic group or aralkyl group having 1 to 22 carbon atoms, which is the same or different; X is a group represented by —H, —R or —Rl_Si (—〇r2—) 3; However, R1 is a carbon support group of carbon * Bu5, R2U or carbon number JJ group) can be the same or different, at least # i of which are -H or -r: ΓΛΏ 2 _ \ · 1 BU OR2—) And 100, m = 0 ~ 5] 7. The method according to item 6 of the patent application, wherein the general formula is fluorenyl. R 8. The method according to item 6 of the scope of patent application, wherein the organopolysiloxane derivative of the general formula (2) is a compound represented by the following general formula (3): CHi. CHal < R20) aS i -R, S i_ I CHa -oS CHi I i — R1 —S i (〇m (3) CHB CHa (where R1 represents an alkylene group having 2 to 4 carbon atoms, and R2 is a CIi3 or — C2H5 , Η is 6 ~ 16) 〇 ..- A kind of cosmetic powder, which is composed of the surface-coated powder according to any one of the patent claims No. I to No. 4 Η) · -Cosmetics' Cosmetic powder containing item 9 of the patent claim. 30
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