TWI825218B - 粉末分散組成物及其製造方法 - Google Patents
粉末分散組成物及其製造方法 Download PDFInfo
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- TWI825218B TWI825218B TW108140995A TW108140995A TWI825218B TW I825218 B TWI825218 B TW I825218B TW 108140995 A TW108140995 A TW 108140995A TW 108140995 A TW108140995 A TW 108140995A TW I825218 B TWI825218 B TW I825218B
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Abstract
本發明所欲解決之課題在於,提供一種粉末分散組成物,該粉末分散組成物可保持水中油型乳化化妝料所要求之水潤感以及展開性優良的使用感,同時可減輕對肌膚造成的負擔感,且能夠達成高防禦紫外線之效果。
本發明所提供之粉末分散組成物係粉末經分散的粉末分散組成物,其中,前述分散組成物中的粉末的平均粒徑為粉末之一次粒徑的10倍以下,前述分散組成物中的平均粒徑的多分散性指數(PDI值)為0.14以下,前述粉末每1%的吸光度為150以上。
Description
本案主張於2018年11月12日提出申請的日本專利申請2018-212413號的優先權,並將其援用至此。
本發明係關於粉末分散組成物,特別是關於其微粒子分散技術的改良。
防曬化妝料之目的在於阻擋太陽光線中的紫外線,以保護肌膚免受紫外線的不良影響,其基劑可列舉:乳化型、乳液(lotion)型、油型等,乳化型係大致分為以水性成分為外相(連續相)的水中油型乳化化妝料、與以油性成分為外相(連續相)的油中水型乳化化妝料。以往即對於防曬化妝料要求水潤的使用感,在水中油型乳化化妝料中,尤以使經過疏水化處理的紫外線散射劑乳化的水中油型乳化化妝料因為可以抑制黏膩感,而能夠實現水潤的使用感(例如專利文獻1)。
另一方面,為了阻斷紫外線對皮膚的照射而得到高防曬係數(SPF,Sun Protection Factor)值,防曬化妝料中必須高度調配紫外線吸收劑或紫外線散射劑。
然而,若高度調配如紫外線散射劑的粉體,則在作為化妝料而塗佈於皮膚時,會帶來澀滯的觸感。減輕這種對肌膚造成的負擔感是非常困難的。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2014-101335號公報
本發明係有鑒於前述以往技術而完成者,所欲解決之課題之目的係在於提供一種粉末分散組成物,其係能夠保持化妝料所要求之水潤感以及展開性優良的使用感,同時減輕對肌膚造成的負擔感而能夠達成高SPF值者。
為了解決前述課題,本案發明人研究的結果發現,若使用新穎的粉末分散組成物,則可在化妝料中,抑制如紫外線散射劑的粉體之調配,而可減輕對肌膚造成的負擔感,進而完成本發明。
再者,發現用於提供上述粉末分散組成物的新穎分散方法,遂完成本發明。
發現使用本發明之粉末分散組成物,則可在化妝料中,抑制如紫外線散射劑的粉體之調配,而可減輕對肌膚造成的負擔感,進而完成本發明。
亦即,本發明之粉末分散組成物係粉末經分散的粉末分散組成物;其中,前述分散組成物中的粉末之平均粒徑為粉末之一次粒徑的10倍以下,前述分散組成物中的平均粒徑的多分散性指數(PDI值)為0.4以下,前述粉末每1%的吸光度為150以上。
又,本發明中,粉末分散組成物係以分散劑為HLB係2以下的聚矽氧油者為佳。
又,本發明中,粉末分散組成物係以分散劑為兩末端聚矽氧化聚甘油者為佳。
又,本發明中,粉末分散組成物係以粉末為氧化鈦、氧化鋅、氧化鈰者為佳。
又,本發明中,粉末分散組成物係以粉末為75%以下者為佳。
又,本發明中,粉末分散組成物較佳為藉由下述第1步驟與第2步驟而得者,在第1步驟中,係將油相與粉末攪拌之同時進行混合,在第2步驟中,根據空蝕的原理來使第1步驟中所得之混合物均質化。
依據本發明之粉末分散組成物,在化妝料中,可抑制如紫外線散射劑的粉體之調配,可減輕對肌膚造成的負擔感。
第1圖係顯示使用均質混合機所得之粉末分散組成物與本發明中使用空蝕(cavitation)所得之粉末分散組成物在分散後經過5天之後的黏度之圖。
第2圖係顯示在剛將低級醇(乙醇)加入至依據本發明之使用空蝕所得之粉末分散組成物後之吸光度之圖。
第3圖係顯示在剛將低級醇(乙醇)加入至本發明中使用空蝕所得之粉末組成物後之黏度之圖。
以下詳述本發明的實施態樣。
[粉末分散組成物]
本發明適合使用的粉末分散組成物,係由粉末、使其分散的分散劑及分散媒所構成。
[粉末]
本發明所使用之粉末可適當地調配紫外線散射劑。紫外線散射劑可列舉例如:氧化鈦、氧化鋅、氧化鈰等無機粉末、或藉由下述處理使該無機粉末的表面經被覆之表面被覆無機粉末:甲基氫聚矽氧烷、甲基聚矽氧烷、甲基苯基聚矽氧烷等聚矽氧處理;藉由全氟烷基磷酸酯、全氟醇等進行的氟處理;藉由N-醯基麩胺酸等進行的胺基酸處理;卵磷脂處理;硬脂酸鋁、硬脂酸鈣、硬脂酸鎂等金屬皂處理;棕櫚酸、異硬脂酸、硬脂酸、月桂酸、肉豆蔻酸、二十二酸、油酸、松香酸、12-羥基硬脂酸等脂肪酸處理;烷基磷酸酯處理、甲基三甲氧基矽烷、乙基三甲氧基矽烷、己基三甲氧基矽烷、辛基三甲氧基矽烷、辛基三乙氧基矽烷等烷氧基矽烷處理;三氟甲基乙基三甲氧基矽烷、十七氟癸基三甲氧基矽烷等氟
烷基矽烷處理;糊精脂肪酸酯、膽固醇脂肪酸酯、蔗糖脂肪酸酯、澱粉脂肪酸酯等脂肪酸酯處理;二氧化矽處理等。
亦可選擇性調配上述紫外線散射劑的1種或2種以上。在粉末分散組成物中,紫外線散射劑的調配量係以0.1至75.0質量%為佳,以1.0至60.0質量%更佳。紫外線散射劑的調配量若太少,則有無法呈現充分的紫外線防禦效果之情形,若太多則有損及調配有粉末分散組成物之化妝料的使用感之情形。
該等粉末的市售品可列舉:TTO-S4、TTO-V4(石原產業製);ST485SA(TitanKogyo製);MZX-5080TS、MZY-505S、MT-100TV(TAYCA股份有限公司製);FINEX-50W-LP2、STR-100C-LP(堺化學工業公司製)等。
[分散媒]
本發明所用的使粉末分散之分散媒可列舉:聚矽氧油、烴油、酯油等油成分。
在粉末分散組成物中,分散媒的調配量較佳為25至80質量%,更佳為30至70質量%。若超過80質量%,則有無法調配充分量的紫外線散射劑之情形,故為不佳。若未達25質量%,則有分散媒太少而無法分散之情形,故為不佳。
該等分散媒的市售品可列舉:KF-96L-1.5cs(信越化學工業公司製)、KF-995(信越化學工業公司製)、FZ-3196(Dow Corning Toray公司製)等。
[聚矽氧系分散劑]
本發明中,所使用之聚矽氧系分散劑係下述通式(a)表示的兩末端聚矽氧化聚甘油。
上述式中,R1為碳數1至12的直鏈或分枝烷基、或是苯基;R2為碳數2至11的伸烷基;m為10至120;n為1至11。
本發明所使用之兩末端聚矽氧化聚甘油的基本結構為BAB型三嵌段共聚物,B可使用例如下述結構(c)所示之單側末端氫殘基聚矽氧等。於通式(a)中,各R1可為相同亦可為不同。又,各R2可為相同亦可為不同。
A為甘油殘基。
下述結構(c)的單側末端氫聚矽氧為習知的化合物。接著,任意聚合度的BAB型三嵌段共聚物可藉由習知的方法來製造。
式中,R1分別為碳數1至12的直鏈或分枝烷基、或是苯基;m為10至120的數。R1分別可為相同亦可為不同。
對於本發明而言,A與B之間的鍵結並非本質性結構,但本發明中所例示之兩末端聚矽氧化聚甘油係使用鉑觸媒來使化合物(c)與下述結構式(d)所示之化合物藉由醚鍵鍵結而成者。
式中;n為1至11的數。
BAB型三嵌段共聚物可藉由習知的方法來合成。能夠得到下述結構式(a){較佳為結構式(b)}表示的兩末端聚矽氧化聚甘油。
式中,R1為碳數1至12的直鏈或分枝烷基、或是苯基;R2為碳數2至11的烷基;m為10至120;n為1至11。
式中,R1為碳數1至12的直鏈或分枝烷基、或是苯基;m為10至120;n為1至11。
聚矽氧鏈之聚合度的m較佳為10至120。側鏈取代基較佳為甲基,惟被取代為苯基或其它烷基亦無妨。
甘油鏈之聚合度的n較佳為1至11。
防止粉體彼此凝聚的A嵌段鏈的展開係取決於高分子的分子量,當A嵌段鏈的分子量越高,則防止凝聚的效果越高。另一方面,認為對粉體之吸附是由於B嵌段鏈的凡德瓦力、氫鍵等較弱的力所致。然而,藉由使用聚甘油作為B嵌段鏈,能夠得到比聚乙二醇等更強的吸附力,因此可以較低的分子量來得到充分的吸附力。又,AB兩嵌段的分子量過高時,則可能導致化妝料難以塗抹開之情形,而且有在推開時感到沉重之情形。由以上情形,就分子量而言亦有適當的範圍,而分子量較佳為2000至20000。
本發明所使用之粉末分散組成物較佳係藉由以下的方法所得。
第1步驟中,在分散媒中將粉末與分散劑於攪拌之同時進行混合。接著,第2步驟中,根據空蝕的原理來使第1步驟中所得之混合物均質化。
空蝕係指在液體的流動中,藉由壓力差而在短時間內使泡沫產生與消失的物理現象。
在本發明中,為了得到粉末分散組成物,係使對第1步驟中所得之混合物賦予流速的液體通過縮徑流路,藉此使液體中產生空蝕所致的微細氣泡,而藉由其衝擊力來得到粉末分散組成物。
所賦予之流速係可施加50至200MPa的超高壓流量。若未達50,則有不具分散效果之情形,故為不佳。
本發明的分散組成物中的粉末之平均粒徑,必須為粉末之一次粒徑的10倍以下。若大於10倍,則有無法發揮紫外線防禦效果之情形,故為不佳。
分散組成物中的粉末每1%的吸光度較佳為150以上。未達150時會有紫外線防禦效果小之情形,故為不佳。
以DLS測量粒子尺寸的結果係有多分散性指數(PDI值),其已知為表示粒子尺寸之均勻性的指標。其係以0到1的範圍表示,0表示為粒子尺寸為無分布的理想性單一尺寸的粒子。
PDI為0.1以下時為單分散性的粒子,又,具有超過0.1且在0.4之間之值的分散體,認為是具有狹窄的粒子尺寸分布。PDI超過0.4且在0.5以下時,認為係粒子尺寸分布較廣,再者,若PDI大於0.5,則認為該分散體係多分散性。
本發明中的粉末分散組成物之平均粒徑的多分散性指數(PDI值)必須為0.4以下。若超過0.4,則有粉末分散組成物無法得到充分的吸光度之情形,故為不佳。
本發明中的分散組成物的SPF較佳為15以上。
上述分散組成物中所使用之粉末的一次粒徑,係使用氮吸附法測量。
針對上述分散組成物中的粉末的平均粒徑及多分散性指數,係使用動態光散射法(Dynamic light scattering)來測量分散在液體中之次微米粒子的平均粒徑及粒徑分布。
若對於在溶液或懸浮液中進行布朗運動中的粒子照射雷射光,則來自粒子的散射光中會產生對應於擴散係數的波動。因為大的粒子移動較慢,故散射光強度的波動會較為平緩,另一方面,因為小的粒子移動較快,故散射光強度的波動會急速改變。
動態光散射法中,係檢測出反映該擴散係數的散射光之波動,並使用史托克斯-愛因斯坦(Stokes-Einstein)式測量粒徑。
d=(kT/3πηD)×1012
上述式中,d:粒徑(nm),k:波茲曼常數(1.38×10-23J.K-1),T:絕對溫度(K),η:黏度(mPa.s),D:擴散係數(m2.s-1)。
光子相關法中,係將該散射光的經時性變化(波動)、即該散射光強度之信號送至相關器。由根據相關器所處理的資料而算出之散射光強度的自相關函數來得到平均粒徑及多分散性指數。頻率解析法中,係將該散射光強度的信號所包含之頻率成分進行傅立葉轉換,藉此算出頻率的強度分布,而能夠得到平均粒徑及多分散性指數。
[其它]
本發明的粉末分散組成物中,除了上述必要成分以外,可以調配能夠用於一般化妝品或準藥品的組成物中的成分,且可因應一般的方法來製造。以下雖然是列舉出具體之能夠調配的成分,但除了前述必要成分之外,可調配下述成分的一種或二種以上來調製本發明的組成物。可調配之成分並不限於下述成分,亦能夠調配下述以外的任意成分。
保濕劑可列舉例如:聚乙二醇、丙二醇、甘油、1,3-丁二醇、木糖醇、山梨糖醇、麥芽糖醇、硫酸軟骨素、玻尿酸、黏液素硫酸、瓜蔞仁酸(charonic acid)、去端肽膠原蛋白(atelocollagen)、乳酸鈉、膽酸鹽、dl-吡咯啶酮羧酸鹽、短鏈可溶性膠原蛋白、二甘油(EO)PO加成物、繅絲花萃取物、西洋蓍草萃取物、草木樨萃取物等。
無紫外線防禦效果的粉末成分可列舉例如:無機粉末(例如:滑石、高嶺土、雲母、絹雲母(sericite)、白雲母、金雲母、合成雲母、紅雲母、黑雲母、蛭石、碳酸鎂、碳酸鈣、矽酸鋁、矽酸鋇、矽酸鈣、矽酸鎂、矽酸鍶、鎢酸金屬
鹽、鎂、二氧化矽、沸石、硫酸鋇、煅燒硫酸鈣(燒石膏)、磷酸鈣、氟磷灰石、羥基磷灰石、陶瓷粉末、金屬皂(例如:肉豆蔻酸鋅、棕櫚酸鈣、硬脂酸鋁、氮化硼等);有機粉末(例如:聚醯胺樹脂粉末(尼龍粉末)、聚乙烯粉末、聚甲基丙烯酸甲酯粉末、聚苯乙烯粉末、苯乙烯與丙烯酸之共聚物樹脂粉末、苯并胍胺樹脂粉末、聚四氟乙烯粉末、纖維素粉末等);無機白色顏料(例如氧化鋅等);無機紅色系顏料(例如鈦酸鐵等);無機紫色系顏料(例如:錳紫、鈷紫等);無機綠色系顏料(例如:氧化鉻、氫氧化鉻、鈦酸鈷等);無機藍色系顏料(例如:群青、普魯士藍等);珠光顏料(例如:氧化鈦包覆雲母、氧化鈦包覆氯氧化鉍、氧化鈦包覆滑石、著色氧化鈦包覆雲母、氯氧化鉍、魚鱗箔等);金屬粉末顏料(例如:鋁粉、銅粉等);鋯、鋇或鋁色澱等有機顏料(例如:紅色201號、紅色202號、紅色204號、紅色205號、紅色220號、紅色226號、紅色228號、紅色405號、橙色203號、橙色204號、黃色205號、黃色401號及藍色404號等有機顏料;紅色3號、紅色104號、紅色106號、紅色227號、紅色230號、紅色401號、紅色505號、橙色205號、黃色4號、黃色5號、黃色202號、黃色203號、綠色3號及藍色1號等);天然色素(例如:葉綠素、β-胡蘿蔔素等)等。
但是,在調配高折射率(折射率2以上等)之無機粉體的情況下,在組成物中較佳係以5質量%以下,更佳為1質量%以下。
液體油脂可列舉例如:酪梨油、日本山茶油、海龜油、夏威夷豆油、玉米油、貂油、橄欖油、菜籽油、蛋黃油、芝麻油、杏仁油、小麥胚芽油、山茶花油、蓖麻油、亞麻仁油、紅花油、棉籽油、紫蘇油、大豆油、花生油、茶籽油、榧子油、米糠油、支那桐油、日本桐油、荷荷芭油、胚芽油、三甘油等。
固體油脂可列舉例如:可可脂、椰子油、馬脂、氫化椰子油、棕櫚油、牛脂、羊脂、氫化牛脂、棕櫚仁油、豬脂、牛骨脂、木蠟核油、氫化油、牛腳油、木蠟、氫化蓖麻油等。
蠟類可列舉例如:蜜蠟、堪地里拉蠟(candelilla wax)、棉蠟、卡拿巴蠟(carnauba wax)、楊梅蠟、蟲蠟(insects wax)、鯨蠟、褐煤蠟、糠蠟、羊毛脂、木棉蠟、乙酸羊毛脂、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、聚乙二醇羊毛脂脂肪酸酯、POE氫化羊毛脂醇醚等。
烴油可列舉例如:液體石蠟、地蠟、姥鮫烷(pristane)、石蠟、純地蠟、角鯊烯、凡士林、微晶蠟、癸烷、十二烷、異十二烷、異十六烷、液體石蠟、角鯊烷、角鯊烯、二新戊酸三丙二醇酯、異壬酸異壬酯、肉豆蔻酸異丙酯、辛酸鯨蠟酯、肉豆蔻酸辛基十二酯、棕櫚酸異丙酯、硬脂酸丁酯、月桂酸己酯、肉豆蔻酸肉豆蔻酯、油酸癸酯、二甲基辛酸己基癸酯、乳酸鯨蠟酯、乳酸肉豆蔻酯、乙酸羊毛脂、硬脂酸異鯨蠟酯、異硬脂酸異鯨蠟酯、12-羥基硬脂酸膽固醇酯、乙基己酸鯨蠟酯、乙二醇二-2-乙基己酸酯、二新戊四醇脂肪酸酯、N-烷二醇單異硬脂酸酯、新戊二醇二癸酸酯、蘋果酸二異硬脂酯、二-2-庚基十一酸甘油酯、三羥甲基丙烷三-2-乙基己酸酯、三羥甲基丙烷三異硬脂酸酯、新戊四醇四(2-乙基己酸)酯、三異辛酸甘油酯(triethylhexanoin)(三-2-乙基己酸甘油酯)、三辛酸甘油酯、三異棕櫚酸甘油酯、三羥甲基丙烷三異硬脂酸酯、鯨蠟基2-乙基己酸酯、2-乙基己基棕櫚酸酯、三肉豆蔻酸甘油酯、三-2-庚基十一酸甘油酯、蓖麻油脂肪酸甲酯、油酸油酯、乙醯甘油酯、棕櫚酸2-庚基十一酯、己二酸二異丁酯、N-月桂醯基-L-麩胺酸-2-辛基十二酯、己二酸二-2-庚基十一酯、月桂酸乙酯、癸
二酸二-2-乙基己酯、肉豆蔻酸2-己基癸酯、棕櫚酸2-己基癸酯、己二酸2-己基癸酯、癸二酸二異丙酯、琥珀酸2-乙基己酯、檸檬酸三乙酯等。
聚矽氧油可列舉:聚二甲基矽氧烷、甲基苯基聚矽氧烷、甲基氫聚矽氧烷等鏈狀聚矽氧油;及八甲基環四矽氧烷、十甲基環五矽氧烷、十二甲基環六矽氧烷等環狀聚矽氧油等。
高級脂肪酸可列舉例如:月桂酸、肉豆蔻酸、棕櫚酸、硬脂酸、山萮酸、油酸、十一碳烯酸、妥爾油酸(tall oil acid)、異硬脂酸、亞麻油酸、次亞麻油酸、二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)等。
高級醇可列舉例如:直鏈醇(例如:月桂醇、鯨蠟醇、硬脂醇、山萮醇、肉豆蔻醇、油醇、鯨蠟硬脂醇等);支鏈醇(例如:單硬脂基甘油醚(鯊肝醇)、2-癸基十四醇、羊毛脂醇、膽固醇、植固醇、己基十二醇、異硬脂醇、辛基十二醇等)等。
又,本發明之粉末分散組成物亦可調配各種的界面活性劑。
陰離子界面活性劑可列舉例如:脂肪酸皂(例如:月桂酸鈉、棕櫚酸鈉等);高級烷基硫酸酯鹽(例如:月桂基硫酸鈉、月桂基硫酸鉀等);烷基醚硫酸酯鹽(例如:POE-月桂基硫酸三乙醇胺、POE-月桂基硫酸鈉等);N-醯基肌胺酸(例如:月桂醯基肌胺酸鈉等);高級脂肪醯胺磺酸鹽(例如:N-肉豆蒄醯基-N-甲基牛磺酸鈉、椰子油脂肪酸甲基牛磺酸鈉、月桂基甲基牛磺酸鈉等);磷酸酯鹽(POE-油基醚磷酸鈉、POE-硬脂基醚磷酸等);磺基琥珀酸鹽(例如:二-2-乙基己基磺基琥珀酸鈉、單月桂醯基單乙醇醯胺聚氧乙烯磺基琥珀酸鈉、月桂基聚丙二醇磺基琥珀酸鈉等);烷基苯磺酸鹽(例如:線性十二基苯磺酸鈉、線性十二基苯磺酸三乙醇胺、線性十二基苯磺酸等);高級脂肪酸酯硫酸酯鹽(例如氫化椰子油脂肪酸甘油
硫酸鈉等);N-醯基麩胺酸鹽(例如N-月桂醯基麩胺酸單鈉、N-硬脂醯基麩胺酸二鈉、N-肉豆蒄醯基-L-麩胺酸單鈉等);硫酸化油(例如土耳其紅油等);POE-烷基醚羧酸;POE-烷基烯丙基醚羧酸鹽;α-烯烴磺酸鹽;高級脂肪酸酯磺酸鹽;二級醇硫酸酯鹽;高級脂肪酸烷醇醯胺硫酸酯鹽;月桂醯基單乙醇醯胺琥珀酸鈉;N-棕櫚醯基天冬胺酸二(三乙醇胺);酪蛋白鈉等。
陽離子界面活性劑可列舉例如:烷基三甲基銨鹽(例如,硬脂基三甲基氯化銨、月桂基三甲基氯化銨等);烷基吡啶鎓鹽(例如,氯化鯨蠟基吡啶鎓等);氯化二硬脂基二甲基銨二烷基二甲基銨鹽;氯化聚(N,N’-二甲基-3,5-亞甲基哌啶鎓);烷基四級銨鹽;烷基二甲基苯甲基銨鹽;烷基異喹啉鎓鹽;二烷基嗎啉鎓鹽;POE-烷基胺;烷基胺鹽;聚胺脂肪酸衍生物;戊醇脂肪酸衍生物;氯化烷基二甲基苄基銨(benzalkonium chloride);氯化苯索寧(benzethonium chloride)等。
兩性界面活性劑可列舉例如:咪唑啉系兩性界面活性劑(例如:2-十一基-N,N,N-(羥乙基羧甲基)-2-咪唑啉鈉、2-椰油醯基-2-氫氧化咪唑啉鎓-1-羧基乙氧基2鈉鹽等);甜菜鹼系界面活性劑(例如2-十七基-N-羧甲基-N-羥乙基咪唑啉鎓甜菜鹼、月桂基二甲胺基乙酸甜菜鹼、烷基甜菜鹼、醯胺甜菜鹼、磺基甜菜鹼等)等。
親油性非離子界面活性劑可列舉例如:山梨醇酐脂肪酸酯類(例如: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、五-2-乙基己酸二甘油山梨醇酐酯、四-2-乙基己酸二甘油山梨醇酐酯等);聚甘油脂肪酸甘油酯類(例如:單棉籽油脂肪酸甘油酯、單芥酸甘油酯、倍半油酸甘油
酯、單硬脂酸甘油酯、α,α’-油酸焦麩胺酸甘油酯、單硬脂酸甘油蘋果酸等);丙二醇脂肪酸酯類(例如單硬脂酸丙二醇酯等)、氫化蓖麻油衍生物、甘油烷基醚等。
親水性非離子界面活性劑可列舉例如:POE-山梨醇酐脂肪酸酯類(例如:POE-山梨醇酐單油酸酯、POE-山梨醇酐單硬脂酸酯、POE-山梨醇酐單油酯、POE-山梨醇酐四油酸酯等);POE山梨糖醇脂肪酸酯類(例如:POE-山梨糖醇單月桂酸酯、POE-山梨糖醇單油酸酯、POE-山梨糖醇五油酸酯、POE-山梨糖醇單硬脂酸酯等);POE-甘油脂肪酸酯類(例如: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-單油酸酯等);POE-脂肪酸酯類(例如:POE-二硬脂酸酯、POE-單(二油酸酯)、乙二醇二硬脂酸酯等);POE-烷基醚類(例如:POE-月桂基醚、POE-油基醚、POE-硬脂基醚、POE-山萮基醚、POE-2-辛基十二基醚、POE-二氫膽固醇醚等);三嵌段聚合物(pluronic)型類(例如三嵌段聚合物等);POE/POP-烷基醚類(例如:POE/POP-鯨蠟基醚、POE/POP-2-癸基十四基醚、POE/POP-單丁基醚、POE/POP-氫化羊毛脂、POE/POP-甘油醚等);四POE/四POP-伸乙二胺縮合物類(例如四嵌段聚合物(tetronic)等);POE-蓖麻油氫化蓖麻油衍生物(例如: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-氫化蓖麻油馬來酸等);POE-蜜蠟/羊毛脂衍生物(例如POE-山梨糖醇蜜蠟等);烷醇醯胺(例如: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);POE-丙二醇脂肪酸酯;POE-烷基胺;POE-脂肪醯胺;蔗糖脂肪酸酯;烷基乙氧基二甲基胺氧化物;磷酸三油酯(trioleyl phosphate)等。
天然的水溶性高分子可列舉例如:植物系高分子(例如:阿拉伯膠、黃蓍膠、半乳聚糖、刺槐豆膠、瓜爾膠、羅望子膠(tamarind gum)、角豆膠、
刺梧桐膠、角叉菜膠、果膠、瓊脂、榅桲籽(quince seed)(榅桲(cydoniaoblonga))、藻膠(褐藻萃取物)、澱粉(米、玉米、馬鈴薯、小麥)、甘草酸;微生物系高分子(例如:三仙膠、葡聚糖、琥珀醯聚糖、聚三葡萄糖(pullulan)等);動物系高分子(例如:膠原蛋白、酪蛋白、白蛋白、明膠等)等。
半合成的水溶性高分子可列舉例如:澱粉系高分子(例如:羧甲基澱粉、甲基羥丙基澱粉等);纖維素系高分子(甲基纖維素、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、羧甲基纖維素鈉、結晶纖維素、纖維素粉末等);藻酸系高分子(例如藻酸鈉、藻酸丙二醇酯等)等。
合成的水溶性高分子可列舉例如:乙烯系高分子(例如聚乙烯醇、聚乙烯甲醚、聚乙烯吡咯啶酮、羧乙烯聚合物等);聚氧乙烯系高分子(例如聚乙二醇20,000、40,000、60,000等);丙烯酸系高分子(例如:聚丙烯酸鈉、聚丙烯酸乙酯、聚丙烯醯胺等);聚乙烯亞胺;陽離子聚合物等。
作為該水溶性高分子以外的增黏劑,可列舉例如:糊精、果膠酸鈉、藻酸鈉、二烷基二甲基硫酸銨纖維素、矽酸鋁鎂、膨土、水輝石、矽酸鋁鎂(Vee gum)、鋰藻土、矽酸酐等。
紫外線吸收劑可列舉例如:苯甲酸系紫外線吸收劑(例如:對胺基苯甲酸(以下簡稱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、N,N-二甲基PABA乙酯等);鄰胺苯甲酸系紫外線吸收劑(例如:N-乙醯基鄰胺苯甲酸三甲環己酯等);水楊酸系紫外線吸收劑(例如:水楊酸戊酯、水楊酸薄荷腦酯、水楊酸三甲環己酯、水楊酸辛酯、水楊酸苯酯、水楊酸苯甲酯、對異丙醇苯基水楊
酸酯等);桂皮酸系紫外線吸收劑(例如:桂皮酸辛酯、桂皮酸乙基-4-異丙酯、桂皮酸甲基-2,5-二異丙酯、桂皮酸乙基-2,4-二異丙酯、桂皮酸甲基-2,4-二異丙酯、對-甲氧基桂皮酸丙酯、對-甲氧基桂皮酸異丙酯、對-甲氧基桂皮酸異戊酯、對-甲氧基桂皮酸辛酯(對-甲氧基桂皮酸2-乙基己酯)、對-甲氧基桂皮酸2-乙氧基乙酯、對-甲氧基桂皮酸環己酯、桂皮酸乙基-α-氰基-β-苯酯、桂皮酸2-乙基己基-α-氰基-β-苯酯、對-甲氧基桂皮酸甘油單-2-乙基己醯基酯等);二苯甲酮系紫外線吸收劑(例如: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、2-乙基己基-4’-苯基-二苯甲酮-2-羧酸酯、2-羥基-4-正辛氧基二苯甲酮、4-羥基-3-羧基二苯甲酮等);3-(4’-甲基苯亞甲基)-d,l-樟腦、3-苯亞甲基-d,l-樟腦;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;二苯甲醛肼(dibenzalazine);聯大茴香醯基甲烷;4-甲氧基-4’-第三丁基二苯甲醯基甲烷;5-(3,3-二甲基-2-亞降冰片基)-3-戊烷-2-酮等。
低級醇可列舉例如:乙醇、丙醇、異丙醇、異丁醇、第三丁醇等。
多元醇可列舉例如:二元醇(例如:乙二醇、丙二醇、三亞甲基二醇、1,2-丁二醇、1,3-丁二醇、四亞甲基二醇、2,3-丁二醇、五亞甲基二醇、2-丁烯-1,4-二醇、己二醇、辛二醇等);三元醇(例如:甘油、三羥甲基丙烷等);四元醇(例如:1,2,6-己三醇等新戊四醇等);五元醇(例如木糖醇等);六元醇(例如:山梨糖醇、甘露醇等);多元醇聚合物(例如:二乙二醇、二丙二醇、三乙二醇、聚丙二醇、四乙二醇、二甘油、聚乙二醇、三甘油、四甘油、聚甘油等);二元醇
烷基醚類(例如:乙二醇單甲醚、乙二醇單乙醚、乙二醇單丁醚、乙二醇單苯醚、乙二醇單己醚、乙二醇單2-甲基己醚、乙二醇異戊醚、乙二醇苯甲醚、乙二醇異丙醚、乙二醇二甲醚、乙二醇二乙醚、乙二醇二丁醚等);二元醇烷醚類(例如:二乙二醇單甲醚、二乙二醇單乙醚、二乙二醇單丁醚、二乙二醇二甲醚、二乙二醇二乙醚、二乙二醇丁醚、二乙二醇甲基乙醚、三乙二醇單甲醚、三乙二醇單乙醚、丙二醇單甲醚、丙二醇單乙醚、丙二醇單丁醚、丙二醇異丙醚、二丙二醇甲醚、二丙二醇乙醚、二丙二醇丁醚等);二元醇醚酯(例如:乙二醇單甲醚乙酸酯、乙二醇單乙醚乙酸酯、乙二醇單丁醚乙酸酯、乙二醇單苯醚乙酸酯、乙二醇二己二酸酯、乙二醇二琥珀酸酯、二乙二醇單乙醚乙酸酯、二乙二醇單丁醚乙酸酯、丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯、丙二醇單丙醚乙酸酯、丙二醇單苯醚乙酸酯等);甘油單烷醚(例如:鮫肝醇、鯊油醇、鯊肝醇等);糖醇(例如:山梨糖醇、麥芽糖醇、麥芽三糖、甘露糖醇、赤藻糖醇等);多元縮醇(glysolid);四氫糠醇;POE-四氫糠醇;POP-丁醚;POP/POE-丁醚;三聚氧丙烯甘油醚;POP-甘油醚;POP-甘油醚磷酸;POP/POE-新戊四醇醚、聚甘油等。
單糖可列舉例如:三碳糖(例如:D-甘油醛、二羥基丙酮等);四碳糖(例如:D-赤藻糖、D-赤藻酮糖、D-蘇糖等)、五碳糖(例如:L-阿拉伯糖、D-木糖、L-來蘇糖、D-阿拉伯糖、D-核糖、D-核酮糖、D-木酮糖、L-木酮糖等);六碳糖(例如:D-葡萄糖、D-塔羅糖、D-阿洛酮糖、D-半乳糖、D-果糖、L-半乳糖、L-甘露糖、D-塔格糖等);七碳糖(例如:庚醛糖、庚酮糖等);八碳糖(例如辛酮糖等);去氧糖(例如:2-去氧-D-核糖、6-去氧-L-半乳糖、6-去氧-L-甘露糖等);胺基糖(例如:D-葡萄胺糖、D-半乳胺糖、涎酸、胺基糖醛酸、胞壁酸等);糖醛
酸(例如:D-葡萄糖醛酸、D-甘露糖醛酸、L-古洛糖醛酸、D-半乳糖醛酸、L-艾杜糖醛酸等)等。
低聚醣可列舉例如:蔗糖、龍膽三糖、傘形糖(umbelliferose)、乳糖、車前糖、異剪秋羅糖類、α,α-海藻糖、棉子糖、剪秋羅糖類、瓦松糖(umbilicin)、水蘇糖、毛蕊花糖類等。
胺基酸可列舉例如:中性胺基酸(例如:蘇胺酸、半胱胺酸等);鹼性胺基酸(例如,羥基離胺酸等)等。又,胺基酸衍生物可列舉例如:醯基肌胺酸鈉(月桂醯基肌胺酸鈉)、醯基麩胺酸鹽、醯基β-丙胺酸鈉、麩胱甘肽、吡咯啶酮羧酸等。
有機胺可列舉例如:單乙醇胺、二乙醇胺、三乙醇胺、嗎啉、三異丙醇胺、2-胺基-2-甲基-1,3-丙二醇、2-胺基-2-甲基-1-丙醇等。
環氧烷衍生物可列舉例如:POE(9)POP(2)二甲醚、POE(14)POP(7)二甲醚、POE(10)POP(10)二甲醚、POE(6)POP(14)二甲醚、POE(15)POP(5)二甲醚、POE(25)POP(25)二甲醚、POE(7)POP(12)二甲醚、POE(22)POP(40)二甲醚、POE(35)POP(40)二甲醚、POE(50)POP(40)二甲醚、POE(55)POP(30)二甲醚、POE(30)POP(34)二甲醚、POE(25)POP(30)二甲醚、POE(27)POP(14)二甲醚、POE(55)POP(28)二甲醚、POE(36)POP(41)二甲醚、POE(7)POP(12)二甲醚、POE(17)POP(4)二甲醚等。
螯合劑可列舉例如:1-羥基乙烷-1,1-二膦酸、1-羥基乙烷-1,1-二膦酸四鈉鹽、乙二胺四乙酸二鈉、乙二胺四乙酸三鈉、乙二胺四乙酸四鈉、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、伸乙二胺羥乙基三乙酸三鈉等。
抗氧化助劑可列舉例如:磷酸、檸檬酸、抗壞血酸、馬來酸、丙二酸、琥珀酸、反丁烯二酸(fumaric acid)、腦磷脂、六偏磷酸酯、植酸、伸乙二胺四乙酸等。
其它能夠調配的成分可列舉例如:防腐劑(對羥基苯甲酸乙酯、對羥基苯甲酸丁酯等);美白劑(例如:胎盤萃取物、虎耳草萃取物、熊果苷等);血液循環促進劑(菸鹼酸、菸鹼酸苯甲酯、菸鹼酸生育酚、菸鹼酸β-丁氧基酯、米諾地爾(音譯,minoxidil)或其類似物、維生素E類、γ-穀維素、烷氧基羰基吡啶N-氧化物、卡普氯銨(carpronium chloride)、及乙醯膽鹼或其衍生物等);各種萃取物(例如:薑、黃柏、黃蓮、紫根、樺木、枇杷、人參、蘆薈、錦葵、鳶尾、葡萄、絲瓜、百合、番紅花、川芎、生薑、小連翹、芒柄花屬、大蒜、辣椒、陳皮、當歸、牡丹、海藻等);活化劑(例如:泛醇基乙基醚(panthenyl ethyl ether)、菸鹼醯胺、生物素、泛酸、蜂王漿、膽固醇衍生物等);抗脂漏劑(例如:吡哆醇類、二甲噻蒽(thianthol)等)等。
本發明之粉末分散組成物的使用用途並未特別限定。例如,能夠應用於化妝水、乳液、乳霜、粉底、口紅、泡沫卸妝劑、洗髮精、潤絲精、護唇膏、髮用噴霧、髮用慕斯、防曬霜、防曬霜、眼線、睫毛膏、指甲霜、身體彩妝化妝料等各種製品。
以下,詳細說明本發明之較佳實施態樣。
首先說明試驗方法。
(分散狀態)
藉由顯微鏡確認所製作之樣本的分散狀態。在以100倍觀察時的視野中,係將無凝聚物的狀態設為A、10個以下設為B、50個以下設為C、超過50個設為D,並將A與B判斷為分散狀態良好。
(SPF)
防曬係數(Sun Protection Factor;SPF)係使用SPF測量裝置「SPFMASTER」(註冊商標)(資生堂)來進行測定。
(粉末分散組成物的粉末的多分散性指數(PDI值))
多分散性指數係藉由動態光散射法(DLS)測定粒子尺寸而進行測定。
(粉末分散組成物中的粉末的平均粒徑)
粉末分散組成物中的粉末的粒徑係藉由動態光散射法進行測定。
(粉末分散組成物所使用之粉末的平均一次粒徑)
粉末分散組成物中所使用之粉末的平均一次粒徑係以氮吸附法進行測定。
(粉末分散組成物的吸光度)
粉末分散組成物的吸光度係以分散媒稀釋粉末分散組成物,並放入10mm見方的液體容器而進行測定。
(粉末分散組成物的黏度)
粉末分散組成物的黏度係藉由錐板型黏度計進行測定。
首先,就用以得到粉末分散組成物的分散方法而言,係針對採用空蝕的分散方法與採用以往技術之均質混合機的分散方法來進行研討。
接著,本案發明人等首先係針對以試驗例1及2的組成來使粉末分散於粉末分散組成物的分散媒之分散劑與上述2種製造方法進行研討。
1)硬脂酸/氧化鋁處理微粒子氧化鈦
如第1圖的試驗例1所示,作為分散劑,可知相較於以往的分散劑使用均質混合機所得之粉末分散組成物,本發明中使用空蝕所得之粉末分散組成物會隨著時間而增黏。另一方面,如第1圖的試驗例2所示,可知若使用兩末端聚矽氧化聚甘油來作為分散劑,則本發明中使用空蝕所得之粉末分散組成物係經時之黏度穩定性優良。
接著,本案發明人等係針對使用以往的均質混合機所得之粉末分散組成物、與本發明中使用空蝕所得之粉末分散組成物進行研討。
如前述表2所示,可知就使用均質混合機所得之粉末分散組成物與本發明中使用空蝕所得之粉末分散組成物而言,在分散組成物中之粉末的平均粒徑相較於分散前的粉末之一次粒徑,係該分散組成物中的粉末之平均粒徑為粉末之一次粒徑的10倍以下。
而且,可知相較於均質混合機,藉由空蝕所得之粉末分散組成物的多分散性指數係在0.4以下,因此被認為是理想的單一尺寸,而具有狹窄的粒子尺寸分布。
再者,可知由空蝕所得之粉末分散組成物所使用的粉末,氧化鈦以外的其它粉末亦可進行微粒子化,經時黏度為穩定。
接著,本案發明人等係針對在將採用以往的均質混合機所得之粉末分散組成物與本發明中採用空蝕所得之粉末分散組成物用於OW化妝料的情況下,是否即使減少粉末的調配量仍可維持高的紫外線防禦效果進行研討。
比較配方例;以均質混合機分散。
配方例1及2:空蝕分散
再者,本案發明人等係針對在將採用以往的均質混合機所得之粉末分散組成物與本發明中採用空蝕所得之粉末分散組成物用於OW化妝料的情況下,是否即使減少粉末的調配量仍可維持高的紫外線防禦效果進行研討。
藉由該等研討結果可知採用了由空蝕所得之粉末分散組成物之OW化妝料即便在粉末的調配量為一半之情況下,仍可維持高的紫外線防禦效果。而且,就使用感而言,可知採用了由空蝕所得之粉末分散組成物的OW化妝料在使用感上亦為優良。
接著,本案發明人等係針對於WO化妝料使用以往的均質混合機所得之粉末分散組成物、與本發明中使用空蝕所得之粉末分散組成物的情況,就在減少粉末的調配量之情況下是否仍可維持高的紫外線防禦效果一事進行研討。
比較配方例2;以均質混合機分散。
配方例3及4;空蝕分散
藉由此等研討結果,可知即便使粉末的調配量為三分之一,採用了由空蝕所得之粉末分散組成物的WO化妝料仍可維持高的紫外線防禦效果。而且,可知就使用感而言,也是採用了由空蝕所得之粉末分散組成物的WO化妝料之使用感仍優良。
再者,本發明者等在表1之試驗例2的組成中,將低級醇(乙醇)加入至本發明之使用空蝕所得之粉末分散組成物來測定組成物的吸光度。
結果如第2圖所示,可知即使加入2重量%的乙醇,與未加入乙醇時相比,吸光度亦無變化,且即使加入乙醇,亦未阻礙防紫外線之效果。
再者,亦測定加入有乙醇之粉末分散組成物的黏度。
如第3圖所示,觀察到添加有1.5%乙醇之粉末分散組成物的黏度急遽上升。因此,為了在一定程度上維持原懸浮液的黏度的同時提升經時穩定性,低級醇的添加量較佳為1.2重量%以下。
其次,進行上述之加入有乙醇之粉末分散組成物的外觀穩定性的評估。
以目視觀察試料剛調製後、1週後、2週後、1個月後的外觀,並依據下述基準進行評估。
A:均勻地分散
B:確認到輕微的沉澱、凝集
C:殘留有結塊或強凝集
D:確認到凝集
又,對於確認到凝集者,以手振盪數次後,進行外觀的觀察。
如表7所示,添加有0.5%或1.2%之乙醇的粉末分散組成物之懸濁液,在調製1個月後,其外觀亦為穩定。由此可知,添加有乙醇者,較能保持粉末分散組成物之穩定性。然而,當添加1.5%之乙醇時,在2週後可觀察到凝集,因此添加量較佳為1.2%以下。
藉由此等檢討結果,可知當將低級醇加入至本發明之使用空蝕所得之粉末分散組成物時,可提升長期穩定性。低級醇之添加量較佳為1.2%以下。
Claims (9)
- 一種粉末分散組成物的製造方法,其包含第1步驟與第2步驟;其中,前述第1步驟係將粉末、分散劑、及分散媒進行混合,前述第2步驟係使對第1步驟中所得之混合物賦予50至200MPa的流速而成的液體通過縮徑流路,使前述液體中產生空蝕所致的微細氣泡,而藉由前述微細氣泡之衝擊力來得到粉末分散組成物,前述粉末包含氧化鈦及/或氧化鋅,前述分散劑為兩末端聚矽氧化聚甘油,前述分散組成物中的前述粉末之平均粒徑為前述粉末之一次粒徑的10倍以下,前述分散組成物中的前述粉末的平均粒徑的多分散性指數(PDI值)為0.4以下,前述粉末每1%的吸光度為150以上。
- 如申請專利範圍第1項所述之粉末分散組成物的製造方法,其中,前述粉末包含氧化鈦及氧化鋅。
- 如申請專利範圍第1或2項所述之粉末分散組成物的製造方法,其中,前述粉末的調配量為0.1質量%以上75質量%以下。
- 如申請專利範圍第1或2項所述之粉末分散組成物的製造方法,其中,前述粉末分散組成物更包含低級醇,前述低級醇之碳數為1至4,前述低級醇之含量為0.5質量%以上1.2質量%以下。
- 如申請專利範圍第4項所述之粉末分散組成物的製造方法,前述低級醇為選自乙醇、丙醇、異丙醇、異丁醇、及第三丁醇之至少一種。
- 如申請專利範圍第4項所述之粉末分散組成物的製造方法,前述低級醇為乙醇。
- 一種粉末分散組成物,其係粉末、分散劑、分散媒、及低級醇經分散,前述粉末包含氧化鈦及/或氧化鋅,前述分散劑為兩末端聚矽氧化聚甘油,前述低級醇之碳數為1至4,前述低級醇之含量為0.5質量%以上1.2質量%以下,前述分散組成物中的前述粉末之平均粒徑為前述粉末之一次粒徑的10倍以下,前述分散組成物中的前述粉末的平均粒徑的多分散性指數(PDI值)為0.4以下,前述粉末每1%的吸光度為150以上。
- 如申請專利範圍第7項所述之粉末分散組成物,前述低級醇為乙醇。
- 如申請專利範圍第7或8項所述之粉末分散組成物,其係使用於O/W化妝料或W/O化妝料。
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