TWI670083B - 組成物及其用途 - Google Patents
組成物及其用途 Download PDFInfo
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- TWI670083B TWI670083B TW104123018A TW104123018A TWI670083B TW I670083 B TWI670083 B TW I670083B TW 104123018 A TW104123018 A TW 104123018A TW 104123018 A TW104123018 A TW 104123018A TW I670083 B TWI670083 B TW I670083B
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- inorganic particles
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Classifications
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- 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
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- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
- A61K8/025—Explicitly spheroidal or spherical shape
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- A—HUMAN NECESSITIES
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- 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
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- 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
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- 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
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- 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
- A61K2800/42—Colour properties
- A61K2800/43—Pigments; Dyes
- A61K2800/434—Luminescent, Fluorescent; Optical brighteners; Photosensitizers
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- Health & Medical Sciences (AREA)
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- Public Health (AREA)
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- Birds (AREA)
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
Abstract
本發明之課題係對安全並且表現高顯色性之螢光體進行研究,獲得由無需擔憂對人體之不良影響之元素構成之無機系紅色螢光體。
本發明之化妝料含有由通式MgxTiyO(x+2y+2z):Mn4+ z
(此處,1.5<x<2.5,0.5<y≦1.5,0.0001<z<0.1)
所表示之化合物構成之無機粒子。
Description
本發明係關於一種含有作為螢光體之鈦酸鎂複合氧化物之化妝料。
眾所周知於化妝料中調配螢光體(例如專利文獻1)。於此種化妝料中,利用藉由螢光體所產生之顯色而調整皮膚之色調,或利用藉由螢光所產生之特異之色調而可期待先前所不具有之化妝特性。特別是具有紅色螢光之化合物藉由對皮膚賦予紅色調而可期待使臉色看起來明亮之效果。
然而,先前提出之3-羥基芘-5,8,10-三磺酸之類的有機螢光體、或NaCl:Mn之類的無機螢光體,由於是由有對人體產生不良影響之擔憂之元素或分子所構成,無法確認安全性,故而實質上未使用。又,亦提出有認為相對安全之礦物系之斧石(硼矽酸鋁鈣)、方解石(碳酸鈣)、葉長石(矽酸鋁鋰)之類的螢光體(例如專利文獻2),但顯色不足,無法以化妝料之形式使用。
Mg2TiO4:Mn4+所表示之化合物為公知者(例如,專利文獻3、非專利文獻1)。然而,專利文獻3之化合物係作為LED用之螢光體等進行
研究者,尚不知摻合於化妝料。
專利文獻4中揭示有將複合金屬化合物用作紫外線吸收劑。然而,專利文獻4之記載僅是有關非常廣泛之化合物的一般記載,完全未具體記載關於具有螢光之化合物。
[專利文獻1]日本特開平5-117127號
[專利文獻2]日本特表2003-500429號
[專利文獻3]日本特開2010-265448號
[專利文獻4]日本特開平11-171540號
[非專利文獻1]J. STADE et al, "New aspects of the luminescence of magnesiumtitanate partII: activation with manganese" Journal of Luminescence, 8, p318-325(1974)
發明人對安全並且表現高顯色性之螢光體進行研究,以獲得由不會擔憂對人體之不良影響之元素所構成的無機系紅色螢光體為目的進行了研究。
本發明係一種化妝料,其特徵在於含有由通式MgxTiyO(x+2y+2z):Mn4+ z
(此處,1.5<x<2.5,0.5<y≦1.5,0.0001<z<0.1)
所表示之化合物構成之無機粒子。
上述無機粒子之含量較佳為相對於化妝料整體為0.1~90重量%。
上述無機粒子較佳為球狀。
上述無機粒子之平均粒徑較佳為1μm~200μm。
上述無機粒子較佳為於照射激發波長為365nm之光時之亮度Y為0.1以上。
本發明之化妝料具有如下效果:具有優異之顯色性,且安全性亦高。
圖1係表示藉由實施例1所獲得之粒子之SEM照片之圖(倍率:500倍)。
圖2係表示藉由實施例2所獲得之粒子之SEM照片之圖(倍率:500倍)。
圖3係表示藉由實施例3所獲得之粒子之SEM照片之圖(倍率:500倍)。
圖4係表示藉由實施例1所獲得之粒子之XRD之圖。
圖5係表示藉由實施例1、2所獲得之粒子之激發光譜之圖。
圖6係表示藉由實施例1、2所獲得之粒子之發光光譜之圖。
本發明係一種摻合由MgxTiyO(x+2y+2z):Mn4+ z(此處,1.5<x<
2.5,0.5<y≦1.5,0.0001<z<0.1)所表示之化合物構成之無機粒子(再者,以下有時將其簡寫為「本發明之無機粒子」)的化妝料。即,係一種摻合由「對通式MgxTiyO(x+2y)所表示之化合物摻雜Mn4+而成之化合物」構成之無機粒子的化妝料。Mg2TiO4:Mn4+螢光體係於1948年所開發(非專利文獻1)。
近年來,正在進行作為白色LED用紅色螢光體之Mg2TiO4:Mn4+之研究開發。然而,完全未進行用以將此種紅色螢光體化合物摻合於化妝料之研究。
本發明人等藉由發現上述「本發明之無機粒子」可較佳地用作化妝品用之原材料而完成本發明。即,上述「本發明之無機粒子」係不會對人類健康造成不良影響的安全之原材料,進而係穩定性亦較高、使用時紅色之顯色性能亦優異者。因此,可獲得具有此前所不具有之良好之化妝外觀之化妝料。
上述「本發明之無機粒子」的式中之x、y、z分別為上述範圍。就可獲得適宜之螢光特性之方面而言,較佳為設為如下之範圍內者。
上述x之下限更佳為1.8,上述x之上限更佳為2.2。
上述y之下限更佳為0.8,上述y之上限更佳為1.2。
上述z之下限更佳為0.001,上述z之上限更佳為0.05。
此時,上述x、y、z之x/(y+z)之下限較佳為1.5,更佳為1.9。又,上限較佳為2.7,更佳為2.1。
上述「本發明之無機粒子」較佳為於照射激發波長為365nm之光時,XYZ表現系之亮度Y為0.1以上。其原因在於:若亮度Y未達0.1,則於以化妝料之形式使用時難以辨識出紅色調。此種亮度Y會根據組成之
調整或後述之添加物而變化,藉由調整該等要素,可將亮度Y設為0.1以上。上述亮度Y更佳為0.3以上,進而較佳為0.5以上。再者,本說明書中之亮度Y係藉由實施例所記載之方法所測得之值。
上述「本發明之無機粒子」可於在不對人體之安全性、或性能方面產生影響之範圍內含有Li、Na、K等鹼金屬、Be、Ca、Sr、Ba、Ra之類之鹼土金屬、Y、Zr、V、Nb、Cr、Mo、W、Fe、Co、Ni、Pd、Pt、Cu、Ag、Zn、B、Al、Ga、Si、Ge、Sn、Pb、P、Gd等其他金屬、S等非金屬。具體含量並無特別限定,上述其他金屬較佳為相對於「本發明之無機粒子」為10重量%以下。
上述「本發明之無機粒子」對其形狀或粒徑等並不特別限定,例如,可使用球狀者。球狀者就具有向皮膚塗抹時之觸感優異之性能,故而可尤佳地用作化妝品用原料之方面而言較佳。
所謂「球狀者」,更具體而言,較佳為縱橫比為1.00~1.50者。更佳為1.00~1.30。只要藉由詳述之測定方法所測得之縱橫比為上述範圍內,則可於不對性能產生影響之範圍內含有縱橫比超過1.50之非球狀之粒子(例如,多個粒子頸縮而成者、擷取鄰接之粒子而成為楕圓形狀者)。非球狀粒子之存在量較佳為「本發明之無機粒子」整體之10%(個數換算)以下,進而較佳為5%以下,最佳為1%以下。
再者,該縱橫比係設為根據500倍之SEM照片對2000個粒子之長徑、及作為短徑之徑(直通過長徑之中間點之直徑)進行測定並將長徑除以短徑所得之值。
「本發明之無機粒子」之平均粒徑(D50)較佳為1~200
μm,更佳為1~50μm。又,D90/D50較佳為3以下。若D50低於1μm,則發光強度降低,又,若D50超過200μm,進而D90/D50超過3,則較大之粒子過多,於以化妝料之形式使用之情形時,有會出現粗澀感之擔憂。作為測定粒徑之方法,可列舉:離心沈澱法、電子區域法(electrozone method)、繞射-散射法、SEM照片之圖像分析法等。
「本發明之無機粒子」較佳為BET比表面積為0.03~1.5m2/g。若未達0.03m2/g,則有發光強度降低之虞,即便超過1.5m2/g,亦有發光強度降低之虞。
「本發明之無機粒子」可為一次粒子,亦可為一次粒子凝集而成之凝集粒子。凝集粒子就容易製成粒徑較大之粒子或真球狀之形狀之方面而言較佳。再者,於「本發明之無機粒子」為凝集粒子之情形時,上述縱橫比係基於凝集粒子所測得之值。
上述「本發明之無機粒子」對其製造方法並無特別限定,例如,可藉由將作為原料之鎂源化合物、錳源化合物及鈦源化合物以與目標化合物之莫耳比相應之比例進行混合製成前驅物之後進行燒成而獲得。
作為上述鎂源化合物,可列舉:碳酸鎂、氫氧化鎂、氧化鎂、氯化鎂、硝酸鎂、硫酸鎂、氟化鎂、溴化鎂、碘化鎂等。又,亦可將該等2種以上併用而使用。
作為上述鈦源化合物,可列舉:氧化鈦、四氯化鈦、硫酸鈦、氫氧化鈦等。又,亦可將該等2種以上併用而使用。
作為上述錳源化合物,可列舉:碳酸錳、乙酸錳、氧化錳、硫酸錳、硝酸錳、氟化錳、溴化錳等。又,亦可將該等2種以上併用而使
用。
又,於進行燒成時,亦可視需要摻合助熔劑(flux)成分。
該等原料化合物之混合方法可為習知所知之任何方法。例如可列舉:將原料化合物製成水性分散液並攪拌或者使用水磨機(aqua mille)或行星式球磨機等濕式介質研磨機進行混合之後將全量蒸發乾燥之方法,或使用亨舍爾混合機(Henschel mixer)、滾筒等普通混合裝置、或錘磨機或高壓空氣噴射磨機、或將該等組合而成者以乾式進行混合之方法。
又,為了獲得為球狀且D50為1μm以上之粒徑之「本發明之無機粒子」,較佳為藉由利用噴霧乾燥機使如上所述之水性分散液乾燥而獲得前驅物並對其進行燒成之方法而獲得。
對利用上述方法所獲得之前驅物進行燒成之方法可為習知所知之任何方法。例如可為使用陶瓷製坩堝進行燒成之方法,亦可為使用旋轉窯一面旋轉一面進行燒成之方法。
上述燒成較佳為於大氣中之燒成等氧化性之燒成條件下進行。燒成溫度並無特別限定,較佳為於1100~1800℃下進行。進而較佳為於1150~1600℃下進行。若為1100℃以下,則容易生成MgTiO3,有發光變得極弱之擔憂,因此較佳為於1150℃以上進行燒成使之相變為Mg2TiO4。若超過1800℃,則有如下擔憂:燒結變強而分散性降低,或發光強度因表面積之降低而降低。
燒成後之粒子視需要亦可為經過藉由篩之分級、藉由水或酸或鹼之洗淨、粉碎等者。尤其是重複1次或者2次以上將燒成後之粒子再次燒成之步驟所獲得之粒子由於會使發光強度提昇,故而較佳。
尤佳為第1次燒成於上述溫度範圍進行,第2次燒成於400℃~1000℃下進行。
「本發明之無機粒子」可直接摻合於化妝料,但亦可視需要實施以往習知之各種表面處理並進行摻合。
關於表面處理之種類,只要為可用於化妝料之物質,則利用任何物質進行處理均可,並無特別限制,例如亦可設置矽、鋅、鈦、鋁、鋯、錫等之氧化物或氫氧化物、碳酸鹽、磷酸鹽等無機化合物之被覆層。又,為了賦予撥水性,可列舉:二甲基聚矽氧烷、甲基氫聚矽氧烷、甲基苯基聚矽氧烷、甲基甲氧基聚矽氧烷、二甲基聚矽氧烷二氫等或該等之共聚物;硬脂酸、月桂酸、油酸及該等之金屬鹽(鋁鹽、鋅鹽、鎂鹽、鈣鹽等);及聚乙烯醇、乙二醇、丙二醇、單乙醇胺、胺基甲基丙醇、二乙醇胺、三乙醇胺、單丙醇胺、二丙醇胺、三丙醇胺、石蠟、聚乙烯蠟、胺基矽烷、環氧矽烷、甲基丙烯基矽烷(methacryl silane)、乙烯基矽烷、巰基矽烷、氯烷基矽烷、烷基矽烷、氟烷基矽烷、六甲基矽氮烷、六甲基環三矽氮烷、三羥甲基丙烷、三羥甲基乙烷、新戊四醇。
又,該等表面處理可為1種,亦可將數種組合進行積層或混合處理。進而,亦可於利用無機化合物進行處理之後設置有機化合物之被覆層,但重要的是無損原本所具有之發光。
無機化合物、有機化合物之被覆量較佳為相對於無機粒子為0.1~30重量%之範圍,進而較佳為0.1~20重量%之範圍。藉由設為0.1重量%以上,可表現由表面處理所帶來之功能性提昇效果,藉由設為30重量%以下,可無損原本之發光特性而進行處理,又,就經濟性之觀點而言有利。
表面處理方法並無特別限定,可藉由於無機粒子之水性分散液中添加無機化合物或有機化合物之後對pH進行調整而被覆。又,於被覆並非水溶性之有機化合物時,可藉由以乾式之方式添加有機化合物並且進行粉碎或混合,視需要進行加熱,而進行表面處理。
本發明之化妝料較佳為以0.1~90重量%之比例含有如上所述之「本發明之無機粒子」。若含量未達0.1重量%,則有無法充分地獲得效果之擔憂,若含量超過90重量%,則粉體變得過量,變得無法充分地含有液狀成分等,作為化妝料之摻合自由度變小,變得難以處理,就該方面而言欠佳。上述含量更佳為0.1~50重量%,進而較佳為0.1~30重量%。
作為本發明之化妝料,可列舉:粉餅、妝前霜、眼影、腮紅、睫毛膏、口紅、防曬劑等。本發明之化妝料可製成油性化妝料、水性化妝料、O/W型化妝料、W/O型化妝料之任意之形態。其中,可尤佳地用於粉餅、妝前霜、眼影等彩妝化妝料或防曬劑中。
本發明之化妝料除上述「本發明之無機粒子」以外,亦可併用可於化妝品領域中使用之任意之水性成分、油性成分。作為上述水性成分及油性成分,並無特別限定,例如可含有油分、界面活性劑、保濕劑、高級醇、金屬離子封阻劑、天然及合成高分子、水溶性及油溶性高分子、紫外線遮蔽劑、各種萃取液、無機及有機顏料、無機及有機黏土礦物等各種粉體、經金屬皂處理或利用聚矽氧處理過之無機及有機顏料、有機染料等色劑、防腐劑、抗氧化劑、色素、增黏劑、pH調整劑、香料、冷感劑、止汗劑、殺菌劑、皮膚賦活劑等成分。具體而言,可任意地摻合1種或2種以上以下列舉之摻合成分並藉由常規方法製造目標化妝料。該等摻合成
分之摻合量只要為無損本發明之效果之範圍,則並無特別限定。
作為上述油分,並無特別限定,例如可列舉:鱷梨油、山茶油、龜油、澳洲胡桃油、玉米油、貂油、橄欖油、菜籽油、蛋黃油、芝麻油、杏仁油(persic oil)、小麥胚芽油、山茶花油、蓖麻油、亞麻籽油、紅花油、棉籽油、紫蘇油、大豆油、花生油、茶籽油、日本榧樹油、米糠油、中國桐樹油(China tung oil)、日本桐樹油、荷荷芭油、胚芽油、三甘油、三辛酸甘油酯、三異棕櫚酸甘油酯、可可脂、椰子油、馬油、氫化椰子油、棕櫚油、牛油、羊脂、氫化牛油、棕櫚仁油、豬油、牛骨脂、木蠟仁油、氫化油、牛腳脂、木蠟、氫化蓖麻油、蜂蠟、小燭樹蠟、棉蠟、巴西棕櫚蠟、月桂果蠟(bayberry wax)、蟲蠟、鯨蠟、褐煤蠟、米糠蠟、羊毛脂、木棉蠟、乙醯化羊毛脂(acetylated lanolin)、液狀羊毛脂、甘蔗蠟、羊毛脂脂肪酸異丙酯、月桂酸己酯、還原羊毛脂、荷荷芭蠟、硬質羊毛脂、蟲膠蠟、POE羊毛脂醇醚、POE羊毛脂醇乙酸酯、POE膽固醇醚、羊毛脂脂肪酸聚乙二醇酯、POE氫化羊毛脂醇醚、液態石蠟、地蠟、姥鮫烷(pristane)、石蠟、地蠟、角鯊烯、凡士林、微晶蠟等。
作為上述親油性非離子界面活性劑,並無特別限定,例如可列舉:山梨醇酐單油酸酯、山梨醇酐單異硬脂酸酯、山梨醇酐單月桂酸酯、山梨醇酐單棕櫚酸酯、山梨醇酐單硬脂酸酯、山梨醇酐倍半油酸酯、山梨醇酐三油酸酯、二甘油山梨醇酐五-2-乙基己酸酯、二甘油山梨醇酐四-2-乙基己酸酯等山梨醇酐脂肪酸酯類;甘油單棉籽油脂肪酸酯、甘油單芥酸酯、甘油倍半油酸酯、甘油單硬脂酸酯、甘油α,α'-油酸酯焦麩胺酸酯、單硬脂酸甘油蘋果酸酯等甘油聚甘油脂肪酸酯類;丙二醇單硬脂酸酯等丙
二醇脂肪酸酯類;氫化蓖麻油衍生物、甘油烷基醚等。
作為親水性非離子界面活性劑,並無特別限定,例如可列舉:POE山梨醇酐單油酸酯、POE山梨醇酐單硬脂酸酯、POE山梨醇酐四油酸酯等POE山梨醇酐脂肪酸酯類;POE山梨醇單月桂酸酯、POE山梨醇單油酸酯、POE山梨醇五油酸酯、POE山梨醇單硬脂酸酯等POE山梨醇脂肪酸酯類;POE甘油單硬脂酸酯、POE甘油單異硬脂酸酯、POE甘油三異硬脂酸酯等POE甘油脂肪酸酯類;POE單油酸酯、POE二硬脂酸酯、POE單二油酸酯、乙二醇二硬脂酸酯等POE脂肪酸酯類;POE月桂醚、POE油醚、POE硬脂醚、POE山萮醚、POE2-辛基十二烷基醚、POE二氫膽固醇醚等POE烷基醚類;POE辛基苯基醚、POE壬基苯基醚、POE二壬基苯基醚等POE烷基苯基醚類;Pluronic等Pluaronic類;POE.POP鯨蠟醚、POE.POP2-癸基十四烷基醚、POE.POP單丁醚、POE.POP氫化羊毛脂、POE.POP甘油醚等POE.POP烷基醚類;Tetronic等四POE.四POP乙二胺縮合物類;POE蓖麻油、POE氫化蓖麻油、POE氫化蓖麻油單異硬脂酸酯、POE氫化蓖麻油三異硬脂酸酯、POE氫化蓖麻油單焦麩胺酸單異硬脂酸二酯、POE氫化蓖麻油順丁烯二酸酯等POE蓖麻油氫化蓖麻油衍生物;POE山梨醇蜂蠟等POE蜂蠟.羊毛脂衍生物;椰子油脂肪酸二乙醇醯胺、月桂酸單乙醇醯胺、脂肪酸異丙醇醯胺等烷醇醯胺;POE丙二醇脂肪酸酯、POE烷基胺、POE脂肪醯胺、蔗糖脂肪酸酯、POE壬基苯基甲醛縮合物、烷基乙氧基二甲基氧化胺、磷酸三油酯等。
作為其他界面活性劑,例如可於穩定性及皮膚刺激性無問題之範圍內摻合:脂肪酸皂、高級烷基硫酸酯鹽、POE月桂基硫酸三乙醇胺、
烷基醚硫酸酯鹽等陰離子界面活性劑;烷基三甲基銨鹽、烷基吡啶鎓鹽、烷基四級銨鹽、烷基二甲基苄基銨鹽、POE烷基胺、烷基胺鹽、聚胺脂肪酸衍生物等陽離子界面活性劑;及咪唑啉系兩性界面活性劑、甜菜鹼系界面活性劑等兩性界面活性劑。
作為上述保濕劑,並無特別限定、例如可列舉:木糖醇、山梨醇、麥芽糖醇、硫酸軟骨素、玻尿酸、硫酸黏多糖、栝樓仁酸、缺端膠原(atelocollagen)、膽固醇-12-羥基硬脂酸酯、乳酸鈉、膽汁酸鹽、dl-吡咯啶酮羧酸鹽、短鏈可溶性膠原、雙甘油(EO)PO加成物、刺蘼(rosa roxburghii)萃取物、洋蓍草(achillea millefolium)萃取物、黃香草木樨(melilot)萃取物等。
作為上述高級醇,並無特別限定,例如可列舉:月桂醇、鯨蠟醇、硬脂醇、山萮醇、肉豆蔻醇、油醇、鯨蠟硬脂醇等直鏈醇;單硬脂基甘油醚(鯊肝醇)、2-癸基十四烷醇、羊毛脂醇、膽固醇、植固醇、己基十二烷醇、異硬脂醇、辛基十二烷醇等支鏈醇等。
作為金屬離子封阻劑,並無特別限定,例如可列舉:1-羥基乙烷-1,1-二膦酸、1-羥基乙烷-1,1-二膦酸四鈉鹽、檸檬酸鈉、聚磷酸鈉、偏磷酸鈉、葡萄糖酸、磷酸、檸檬酸、抗壞血酸、琥珀酸、乙二胺四乙酸等。
作為上述天然之水溶性高分子,並無特別限定,例如可列舉:阿拉伯膠、黃蓍膠、聚半乳糖、瓜爾膠(guar gum)、刺槐豆膠(carob gum)、刺梧桐樹膠、角叉菜膠(carrageenan)、果膠、瓊脂、榅桲籽(marmelo)、海藻膠(褐藻萃取物)、澱粉(稻米、玉米、馬鈴薯、小麥)、甘草酸等植物
系高分子;三仙膠、葡聚糖、琥珀醯聚糖(succinoglucan)、聚三葡萄糖等微生物系高分子;膠原蛋白、酪蛋白、白蛋白、明膠等動物系高分子。
作為半合成之水溶性高分子,並無特別限定,例如可列舉:羧甲基澱粉、甲基羥丙基澱粉等澱粉系高分子;甲基纖維素、硝化纖維素、乙基纖維素、甲基羥丙基纖維素、羥乙基纖維素、纖維素硫酸鈉、羥丙基纖維素、羧甲基纖維素鈉(CMC)、結晶纖維素、纖維素末等纖維素系高分子;海藻酸鈉、丙二醇海藻酸酯等海藻酸系高分子等。
作為合成之水溶性高分子,並無特別限定,例如可列舉:聚乙烯醇、聚乙烯甲醚、聚乙烯吡咯啶酮等乙烯系高分子;聚乙二醇20,000、40,000、60,000等聚氧乙烯系高分子;聚氧乙烯聚氧丙烯共聚物等共聚系高分子;聚丙烯酸鈉、聚丙烯酸乙酯、聚丙烯醯胺等丙烯酸系高分子;聚伸乙基亞胺、陽離子聚合物等。
作為無機之水溶性高分子,並無特別限定,例如可列舉:膨潤土、矽酸鋁鎂(veegum)、合成鋰皂石、鋰膨潤石、矽酸酐等。
作為紫外線遮蔽劑,並無特別限定,例如可列舉:對胺基苯甲酸(以下簡寫為PABA)、PABA單甘油酯、N,N-二丙氧基PABA乙酯、N,N-二乙氧基PABA乙酯、N,N-二甲基PABA乙酯、N,N-二甲基PABA丁酯等苯甲酸系紫外線遮蔽劑;N-乙醯基鄰胺基苯甲酸高薄荷酯(homo menthyl N-acetyl anthranilate)等鄰胺基苯甲酸系紫外線遮蔽劑;水楊酸戊酯、水楊酸薄荷酯、水楊酸高薄荷酯、水楊酸辛酯、水楊酸苯酯、水楊酸苄酯、水楊酸對異丙醇苯酯等水楊酸系紫外線遮蔽劑;肉桂酸辛酯、4-異丙基肉桂酸乙酯、2,5-二異丙基肉桂酸甲酯、2,4-二異丙基肉桂酸乙酯、2,4-二
異丙基肉桂酸甲酯、對甲氧基肉桂酸丙酯、對甲氧基肉桂酸異丙酯、對甲氧基肉桂酸異戊酯、對甲氧基肉桂酸2-乙氧基乙酯、對甲氧基肉桂酸環己酯、α-氰基-β-苯基肉桂酸乙酯、α-氰基-β-苯基肉桂酸2-乙基己酯、甘油單-2-乙基己醯基-二對甲氧基肉桂酸酯等肉桂酸系紫外線遮蔽劑;2,4-二羥基二苯甲酮、2,2'-二羥基-4-甲氧基二苯甲酮、2,2'-二羥基-4,4'-二甲氧基二苯甲酮、2,2',4,4'-四羥基二苯甲酮、2-羥基-4-甲氧基二苯甲酮、2-羥基-4-甲氧基-4'-甲基二苯甲酮、2-羥基-4-甲氧基二苯甲酮-5-磺酸鹽、4-苯基二苯甲酮、4'-苯基-二苯甲酮-2-羧酸2-乙基己酯、2-羥基-4-正辛氧基二苯甲酮、4-羥基-3-羧基二苯甲酮等二苯甲酮系紫外線遮蔽劑;3-(4'-甲基亞苄基)-d,l-樟腦、3-亞苄基-d,l-樟腦、4-咪唑丙烯酸(urocanic acid)、4-咪唑丙烯酸乙酯、2-苯基-5-甲基苯并唑、2,2'-羥基-5-甲基苯基苯并三唑、2-(2'-羥基-5'-第三辛基苯基)苯并三唑、2-(2'-羥基-5'-甲基苯基)苯并三唑、二雙亞苄肼(dibenzalazine)、聯大茴香甲醯基甲烷(dianisoyl methane)、4-甲氧基-4'-第三丁基二苯甲醯甲烷、5-(3,3-二甲基-2-亞降莰基)-3-戊烷-2-酮等。
作為其他藥劑成分並無特別限定,例如可列舉:維生素A油、視黃醇、視黃醇棕櫚酸酯、肌醇、鹽酸吡哆醇、菸鹼酸苄酯、菸鹼醯胺、DL-α-生育酚菸鹼酸酯、抗壞血酸磷酸鎂、2-O-α-D-吡喃葡萄糖-L-抗壞血酸、維生素D2(麥角鈣化固醇)、dl-α-生育酚、乙酸dl-α-生育酚、泛酸、生物素等維生素類;雌二醇、乙炔雌二醇等激素;精胺酸、天冬胺酸、胱胺酸、半胱胺酸、甲硫胺酸、絲胺酸、白胺酸、色
胺酸等胺基酸;尿囊素(allantoin)、薁等抗炎劑、熊果苷等美白劑;單寧酸等收斂劑;L-薄荷腦、樟腦等清涼劑;或硫、氯化溶菌酶、氯化吡哆醇等。
作為各種萃取液並無特別限定,例如可列舉:魚腥草萃取物、黃柏萃取物、黃香草木樨萃取物、短柄野芝麻萃取物、甘草萃取物、芍藥萃取物、皂草(Saponaria officinalis)萃取物、絲瓜萃取物、雞納樹(cinchona)萃取物、虎耳草萃取物、苦參萃取物、萍蓬草萃取物、茴香萃取物、報春花(oxlip)萃取物、薔薇萃取物、地黃萃取物、檸檬萃取物、紫根萃取物、蘆薈萃取物、菖蒲根萃取物、桉樹萃取物、木賊萃取物、鼠尾草萃取物、麝香草萃取物、茶萃取物、海藻萃取物、黃瓜萃取物、丁香萃取物、覆盆子萃取物、蜂草(melissa)萃取物、人蔘萃取物、七葉樹萃取物、桃萃取物、桃葉萃取物、桑樹萃取物、矢車菊萃取物、金縷梅萃取物、胎盤萃取物、胸腺萃取物、蠶絲萃取液、甘草萃取物等。
作為上述各種粉體,可列舉:鐵丹、氧化鐵黃、氧化鐵黑、雲母鈦、氧化鐵被覆雲母鈦、氧化鈦被覆玻璃薄片等光亮性著色顏料;雲母、滑石、高嶺土、絹雲母、二氧化鈦、二氧化矽等無機粉末;或聚乙烯粉末、尼龍粉末、交聯聚苯乙烯、纖維素粉末、聚矽氧粉末等有機粉末等。較佳為:為了提昇官能特性、及提昇化妝持續性,而將粉末成分之一部分或全部利用聚矽氧類、氟化合物、金屬皂、油劑、醯基麩胺酸鹽等物質藉由公知之方法進行疏水化處理而使用。
[實施例]
以下,列舉實施例對本發明進行說明,但本發明絲毫不受該等實施例限定。
(由Mg2TiO4:Mn4+所表示之化合物構成之無機粒子之製造方法)
實施例1
稱量鹼性碳酸鎂(神島化學工業公司製造之GP-30N以Mg計含量為26.12重量%)1395.5g、碳酸錳(中央電氣製造純度94.58%)3.6461g、氧化鈦(堺化學工業製造之A-120純度99.00%)602.7g,加入純化水7.5L及氧化鋯顆粒8L並使用水磨機以250rpm歷時30分鐘充分地混合。利用噴霧乾燥器(機種名稱:大川原化工機BDP-22E,轉盤轉數116000轉,出口溫度:105~110℃)使混合漿料蒸發乾燥而獲得燒成前驅物粉末。繼而,將該燒成前驅物填充至氧化鋁製坩鍋,於大氣環境中以200℃/小時升溫至1250℃,並於該狀態下保持10小時後,以200℃/小時降溫至室溫。繼而,於大氣環境中以200℃/小時升溫至600℃,並於該狀態下保持24小時後,以200℃/小時降溫至室溫。
將以此方式所獲得之P1之電子顯微鏡照片示於圖1。再者,若將P1以MgxTiyO(x+2y+2z):Mn4+ z之通式表示,則x=2.00,y=0.996,z=0.004。
實施例2
稱量鹼性碳酸鎂(神島化學工業公司製造之GP-30N以Mg計含量為26.12重量%)9.303g、碳酸錳(中央電氣製造純度94.58% 0.0243g)、氧化鈦(昭和電工製造之Super Titania純度99.92%)3.9822g、純化水50g,使用行星式球磨機以250rpm歷時30分鐘充分地混合。利用130℃之乾燥機使混合漿料蒸發乾燥1晚而獲得燒成前驅物粉末。繼而,將該燒成前驅物填充至氧化鋁製坩鍋,於大氣環境中以200℃/小時升溫至1250℃,並於該狀
態下保持10小時後,以200℃/小時降溫至室溫。繼而,於大氣環境中以200℃/小時升溫至600℃,並於該狀態下保持24小時後,以200℃/小時降溫至室溫。
將以此方式所獲得之P2之電子顯微鏡照片示於圖2。再者,若將P2以MgxTiyO(x+2y+2z):Mn4+ z之通式表示,則x=2.00,y=0.996,z=0.004。
實施例3
稱量鹼性碳酸鎂(神島化學工業公司製造之GP-30N以Mg計含量為26.12重量%)1395.5g、碳酸錳(中央電氣製造純度94.58%)3.6461g、氧化鈦(堺化學工業製造之A-120純度99.00%)602.7g,加入純化水7.5L及氧化鋯顆粒8L,並使用水磨機以250rpm歷時30分鐘充分地混合。利用噴霧乾燥器(機種名稱:大川原化工機BDP-22E,轉盤轉數:16000轉,出口溫度:105~110℃)使混合漿料蒸發乾燥而獲得燒成前驅物粉末。繼而,將該燒成前驅物填充至氧化鋁製坩鍋,於大氣環境中以200℃/小時升溫至1250℃,並於該狀態下保持10小時後,以200℃/小時降溫至室溫。繼而,放入至水中並使用行星式球磨機以250rpm歷時40分鐘充分地粉碎。分離顆粒後,通過網眼15μm之篩除去粗粒並進行過濾,其後使之於130℃進行乾燥。將所獲得之固形物於大氣環境中以200℃/小時升溫至600℃,並於該狀態下保持24小時後,以200℃/小時降溫至室溫。
將以此方式所獲得之P3之電子顯微鏡照片示於圖3。再者,若將P3以MgxTiyO(x+2y+2z):Mn4+ z之通式表示,則x=2.00,y=0.996,z=0.004。
評價例1(作為螢光體之評價)
對實施例所獲得之螢光體樣品進行評價。
[亮度Y、色度(x、y)、激發光譜、發光光譜之測定]
激發、發光光譜係使用日本分光公司製造之EP-6500進行測定,且激發波長設為365nm,發光波長設為657nm。螢光積分球係使用ISF-513型,並將光電倍增管(PMT)之電壓之設定值設為340。
[螢光體粒子之形狀]
為了觀測螢光體粒子之形狀,於P1~P3中,使用SEM(日本電子製造之7000F)拍攝SEM照片。將結果示於圖1~3。由圖1明瞭:藉由實施例1所獲得之無機粒子為球狀。
[螢光體之鑑定]
為了鑑定實施例1所獲得之P1之產物,進行了XRD(Rigaku公司製造之RINT-TTRIII,X射線=CuK α,λ=1.5406Å、50kV、300mA)之測定。測定結果與PDF卡#01-072-6975或#01-079-0830一致,可確認P1、P2、P3之母體之組成與Mg2TiO4大致相同。將結果示於圖4。
[比表面積及粒度分佈之測定]
使用Mountech製造之Macsorb HM-1220以脫氣溫度230℃、脫氣時間35分鐘,對比表面積進行測定,將結果示於表1。又,利用雷射繞射式粒度分佈裝置(日機裝股份有限公司製造MT3000)對粒度分佈進行測定(測定條件:使用六偏磷酸鈉作為分散劑,以繞射光量(DV)成為0.01~0.2之方式將離子交換水、分散劑、及樣品混合進行測定),將結果示於表1。
[縱橫比之測定]
根據500倍之SEM照片,對2000個粒子之長徑、及作為短徑之徑(直通過長徑之中間點之直徑)進行測定。將長徑除以短徑之值作為縱橫比。
算出測得之縱橫比之平均值、及縱橫比超過1.5之粒子之個數之比例。
評價例2(官能評價)
對10位官能檢查員以不知道編號之方式向皮膚塗抹實施例1~3所獲得之螢光體P1~P3,針對粉體之觸感進行官能試驗。將評價觸感之結果示於表2。
評價例3(作為化妝料之評價)
使用實施例1~2所獲得之化合物P1~P2,以如以下表3所具有之組成製備粉餅F1、F2。又,以如下述組成表4所具有之組成製備不含本發明之無機粒子之粉餅F3。再者,下述粉餅所使用之材料如表之等級,除P1、P2以外,全部為化妝品等級。
以此種組成量取各原材料,使用咖啡磨豆機攪拌混合1分30秒鐘。量取所獲得之粉體狀之混合物0.8g,在直徑20mm 之模具,使用壓製機以200kgf/cm2之壓力保持30秒鐘,而獲得粉餅F1~F3。
對10位官能檢查員以不知道編號之方式塗抹粉餅F1~F3,針對365nm黑光燈照射下之色調進行試驗。將以5個等級評價紅色調之感受之結果示於表5。再者,評價之基準如下。
5:8人以上或全體人員感覺到紅色調;4:5~7人感覺到紅色調;3:2~4人感覺到紅色調;2:1人感覺到紅色調;1:無人感覺到紅色調
對10位官能檢查員以不知道編號之方式塗抹粉餅F1~F3,針對室外且自然光下之色調進行試驗。將以5個等級評價紅色調之感受之結果示於表6。
對10位官能檢查員以不知道編號之方式塗抹粉餅F1~F3,針對室內且LED燈等之照明下之色調進行試驗。將以5個等級評價紅色調之感受之結果示於表7。
若將色度x與色度y之值應用於色度圖,則可知P1、P2之紅色調均較強。亮度亦為1左右而較高。由激發光譜可知,不僅可利用紫外線激發,亦可利用可見光激發。進而,於作為化妝料摻合之情形時,可於室外之自然光下、室內之螢光燈下、LED照明下等增加紅色調,可實現良好之化妝外觀。由該等結果明瞭:本發明之無機粒子可提高光學功能。
又,球狀之P1於觸感方面亦具有優異之性質。
[產業上之可利用性]
本發明之化妝料由於具有遮蓋皮膚之色調並且對皮膚賦予透明感或緊致感、或修正色調而呈現美麗之膚色的優異效果,故而可較佳地用於粉餅等彩妝化妝料等。
特別是藉由照射到365nm之自然光(太陽光)所含之紫外線,紅色調會變強,故而本發明之化妝料於自然光下、特別是於室外會發揮效力。又,由於在可見區域亦會發光,故而於室內或拍攝照片時使用閃光燈或閃光儀之情形時亦會發揮效力。
Claims (7)
- 一種組成物之用途,其用於化妝,該組成物含有由通式MgxTiyO(x+2y+2z):Mn4+ z(此處,1.5<x<2.5,0.5<y≦1.5,0.0001<z<0.1)所表示之化合物構成之無機粒子,上述無機粒子中之縱橫比超過1.50之非球狀粒子的存在量為無機粒子整體之10%(個數換算)以下。
- 如申請專利範圍第1項之組成物之用途,其中,無機粒子之含量相對於組成物整體為0.1~90重量%。
- 如申請專利範圍第1項之組成物之用途,其中,無機粒子為球狀。
- 如申請專利範圍第2項之組成物之用途,其中,無機粒子為球狀。
- 如申請專利範圍第1、2、3或4項之組成物之用途,其中,無機粒子之平均粒徑為1μm~200μm。
- 如申請專利範圍第1、2、3或4項之組成物之用途,其中,無機粒子於照射激發波長為365nm之光時亮度Y為0.1以上。
- 如申請專利範圍第5項之組成物之用途,其中,無機粒子於照射激發波長為365nm之光時之亮度Y為0.1以上。
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US20170202759A1 (en) | 2017-07-20 |
WO2016017372A1 (ja) | 2016-02-04 |
TW201609162A (zh) | 2016-03-16 |
KR102303423B1 (ko) | 2021-09-23 |
JP6583273B2 (ja) | 2019-10-02 |
EP3175836A4 (en) | 2018-02-07 |
EP3175836A1 (en) | 2017-06-07 |
JPWO2016017372A1 (ja) | 2017-05-18 |
KR20170031083A (ko) | 2017-03-20 |
US9937114B2 (en) | 2018-04-10 |
EP3175836B1 (en) | 2018-10-31 |
CN106456470B (zh) | 2019-07-16 |
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