TWI818076B - 油中水型乳化化妝料 - Google Patents
油中水型乳化化妝料 Download PDFInfo
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- TWI818076B TWI818076B TW108132775A TW108132775A TWI818076B TW I818076 B TWI818076 B TW I818076B TW 108132775 A TW108132775 A TW 108132775A TW 108132775 A TW108132775 A TW 108132775A TW I818076 B TWI818076 B TW I818076B
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Abstract
本發明係提供一種使用感和使用性經改善之油中水型乳化化妝料。
本發明之油中水型乳化化妝料係包含下述成分(a)至(d);
(a)選自由聚丙烯酸、聚丙烯酸之鹽、聚(2-丙烯醯胺-2-甲基丙磺酸)、及聚(2-丙烯醯胺-2-甲基丙磺酸)之鹽所組成群組之1種以上的聚合物,且
該聚合物之重量平均分子量為100萬至400萬,而且,
作成1質量%水溶液時在25℃的黏度為1Pa‧s以下;
(b)成分(a)以外之水相成分;
(c)油性成分為60質量%以下;
(d)乳化劑。
Description
本申請案係主張於2018年9月14日申請之日本專利申請案2018-173046號的優先權,並引用於此者。
本發明係關於一種調配有分子量經調控之水溶性聚合物的調配油中水型乳化化妝料。
水溶性之合成高分子對於以水或水性溶劑作為連續相之組成物的黏度調節大有貢獻。尤其是聚丙烯酸或其鹽、或是聚(2-丙烯醯胺-2-甲基丙磺酸)(於下,有簡稱為PAMPS之情形)或其鹽係因為其水溶性之高,而被廣泛使用於各種領域之水系及水中油型組成物來作為增黏劑。
然而,此等水溶性合成高分子係不僅顯示增黏作用,亦顯示拉絲之性質(牽絲性),故對於要避免牽絲性之組成物(例如,化妝料)係有調配量受到限制之情況。
對此問題,本發明人發現在市場上流通之聚丙烯酸鹽等所顯示的牽絲性係其中所混入之巨大分子(具體而言,係分子量為1000萬以上之分子)的
效果(專利文獻1)。此等係在合成過程所過聚合而成者,在以無法充分調控聚合起始頻率、聚合速度之一般方法合成時,為無法避免的副產物。
本發明人已釐清,藉由以RAFT聚合法進行合成而使前述巨大分子之含量成為10質量%以下之聚丙烯酸鹽及PAMPS鹽,會維持原本的增黏效果,且只有牽絲性會大幅地降低。而且,已提出藉由使用該分子量經調控之聚合物來取代習知的(市售之)聚合物作為增黏劑,可製造出感受不到牽絲性之水系及水中油型乳化化妝料之報告(專利文獻1)。
然而,上述係此於將分子量經調控之聚丙烯酸或其鹽等調配於“水相為連續相之系統”的情形之效果,但調配於“油相為連續相之系統”(亦即,油中水型乳化組成物之內水相)的情形之效果則完全為未知數。
[專利文獻1]WO2015/052804號公報
本發明之目的在於提供一種使用感和使用性經改善之油中水型乳化化妝料。
對於前述課題,本發明人累積致力研究之結果,係發現:若於油性成分之調配量為60%以下之油中水型乳化化妝料的內水相中調配分子量經調
控的聚丙烯酸鹽,則延展性會變得非常良好,發黏感會減少,濃厚感增加,賦予肌膚柔潤度及光滑度之效果更為優異,遂完成本發明。
亦即,本發明係包含以下。
〔1〕一種油中水型乳化化妝料,係包含下述成分(a)至(d);
(a)選自由聚丙烯酸、聚丙烯酸之鹽、聚(2-丙烯醯胺-2-甲基丙磺酸)、及聚(2-丙烯醯胺-2-甲基丙磺酸)之鹽所組成群組之1種以上的聚合物,且為
該聚合物之重量平均分子量為100萬至400萬,而且,
作成1質量%水溶液時在25℃的黏度為1Pa‧s以下;
(b)成分(a)以外之水相成分;
(c)油性成分為60質量%以下;
(d)乳化劑。
〔2〕如[1]項所述之油中水型乳化化妝料,其中,成分(a)之含量為0.005%至2%。
〔3〕如[1]或[2]項所述之油中水型乳化化妝料,其中,前述成分(a)之重量平均分子量為150萬至400萬。
〔4〕如[1]至[3]項中任一項所述之油中水型乳化化妝料,係更包含成分(e)疏水化處理粉體。
藉由本發明,可提供一種油中水型乳化化妝料,其係延展性非常良好,發黏感少,且富有濃厚感,賦予肌膚柔潤度和光滑度之效果優異。
說明有關本發明之適當的實施形態。
本發明之油中水型乳化化妝料係由成分(a)及成分(b)所構成的水相藉由成分(d)之作用而作為乳化粒子分散在含有成分(c)之油相中者。以下,詳述各成分。
(a)成分
本發明中之(a)成分係選自由聚丙烯酸、聚丙烯酸之鹽、聚(2-丙烯醯胺-2-甲基丙磺酸)、及聚(2-丙烯醯胺-2-甲基丙磺酸)之鹽所組成群組之1種以上的聚合物,且為重量平均分子量為100萬至400萬,而且作成1質量%水溶液時在25℃的黏度為1Pa‧s以下之聚合物。又,本發明之(a)成分為直鏈狀之聚合物。
前述所謂“作成1質量%水溶液時在25℃的黏度為1Pa‧s以下”之要素,係意指在該聚合物中“僅包含10質量%以下的分子量為1000萬以上之分子物種”。這是因為在重量平均分子量為100萬至400萬之直鏈狀的聚合物中,若分子量為1000萬以上之分子物種的含量為10質量%以下,則作成1質量%水溶液時在25℃之黏度係成為1Pa‧s以下之故。
前述黏度係使用應力調控型流變儀所測定之在10s-1之應變速度的60秒後之表觀黏度值。應力調控型流變儀係可適合使用圓錐板型幾何流變儀(cone-and-plate geometry)。
在本書中係有將“重量平均分子量為100萬至400萬,而且作成1質量%水溶液時在25℃的黏度為1Pa‧s以下之直鏈狀聚合物”稱為“分子量調控聚合物”之情形。而且,有將滿足前述分子量調控聚合物之要素的聚丙烯酸、聚(2-丙烯醯胺-2-甲基丙磺酸)分別稱為”分子量調控聚丙烯酸”、”分子量調控PAMPS”之情形。在此,所謂“PAMPS”係聚(2-丙烯醯胺-2-甲基丙磺酸)之簡稱。
有關本發明之成分(a)的重量平均分子量係100萬至400萬,較佳係150萬至400萬,更佳係200萬至350萬,再更佳係200萬至300萬。若重量
平均分子量小於100萬,則有無法獲得適當的濃厚感之情形,若大於400萬,有產生發黏性之情形。
前述鹽之種類可舉出:鹼金屬鹽(例如:鈉鹽、鉀鹽、鎂鹽、鈣鹽等)、有機胺鹽(例如:單乙醇胺鹽、二乙醇胺鹽、三乙醇胺鹽、三異丙醇胺鹽等)及2-胺基-2-甲基-1-丙醇、2-胺基-2-甲基-1,3-丙二醇、2-胺基-2-羥基甲基-1,3-丙二醇、L-精胺酸、L-離胺酸、L-烷基牛磺酸等鹼性含氮化合物之鹽等。其中,以一價之鹼金屬鹽及有機胺鹽為較佳,更佳係鈉鹽、鉀鹽、三乙醇胺鹽,最佳係鈉鹽。
在本發明中,所謂聚丙烯酸鹽或PAMPS鹽係意指藉由將聚丙烯酸或PAMPS以前述鹼(亦即,前述鹼金屬、有機胺、鹼性含氮化合物等)進行中和所得之化合物,或藉由使以前述鹼預先中和了酸部分之丙烯酸或2-丙烯醯胺-2-甲基丙磺酸(以下,簡稱為AMPS)進行聚合所得之化合物。
‧分子量調控聚合物之合成方法
本發明之成分(a)係可藉由公知之活性聚合法進行合成。活性聚合係可舉出:活性陰離子聚合、活性陽離子聚合、活性自由基聚合(精密自由基聚合、或調控自由基聚合)。
活性自由基聚合係可舉出:經由氮氧自由基(nitroxide)(自由基(radical))聚合、或氮氧自由基介質(自由基)聚合(NLRP)、原子轉移自由基聚合(ATRP,Atom Transfer Radical Polymerization)、可逆性加成-斷裂鏈轉移(RAFT,Reversible Addition-Fragmentation Chain Transfer Polymerization)聚合等。原子轉移自由基聚合(ATRP)係可舉出源自電子轉移之活化因子ATRP、或藉由電子轉移而生成之活性化劑ATRP(AGET ATRP)、源自電子轉移之再生活化因子ATRP或藉由電子轉
移而再生之活性化劑ATRP(ARGET ATRP)、用以使活性物種連續地再生之起始劑ATRP或活性化劑常態性再生之起始劑ATRP(ICAR ATRP)、反向ATRP(Reverse ATRP)。就可逆性加成-斷裂鏈轉移(RAFT)聚合之衍生技術而言,可舉出以有機碲作為成長末端之活性自由基聚合、或有機碲介質活性自由基聚合(TERP)、銻介質活性自由基聚合(SBRP)、鉍介質活性自由基聚合(BIRP)。就其它之活性自由基聚合而言,可舉出碘轉移自由基聚合(IRP)、鈷介質自由基聚合(CMRP)等。
從聚合之簡便性而言,係以丙烯酸之直接聚合為較佳,惟在觸媒等不溶鹽的生成等難以聚合的情形下,係可藉由使用丙烯酸第三丁酯、丙烯酸甲氧基甲酯、丙烯酸甲酯等之保護丙烯酸酯,並於其後進行去保護而獲得目的之高分子化合物。
在本發明中,特別是就能夠調控高分子量體之分子量(亦即,分子量分布狹窄的高分子化合物之合成)之點而言,係以可逆性加成-斷裂鏈轉移聚合法(RAFT聚合法)為較佳(專利文獻4)。鏈轉移劑係以二硫型、三硫型為較佳。聚合起始劑係以化學構造接近於鏈轉移劑者為較佳,而以偶氮系起始劑為較佳。聚合溶劑並無特別限定,能夠適宜地選擇對於單體、聚合物之溶解性高者。聚合時間係從數小時至100小時左右為適宜。
‧分子量測定方法
分子量調控聚合物之分子量就重量平均分子量而言,係可藉由光散射法、超離心法、色層分析法等進行測定,就數量平均分子量而言,係可藉由滲透壓法、色層分析法等公知之方法進行測定。其中,就以少量之試料簡便地獲得重量平均
分子量、數量平均分子量、及分子量分布之點而言,尤以色層分析法為較佳,再者,以凝膠滲透色層分析法(以下,簡稱為GPC)為適宜。
又,在本案所使用之分子量分布,係將藉由GPC解析所得之重量平均分子量除以數量平均分子量之值。
本發明之油中水型乳化化妝料中之成分(a)的調配量係0.005至2質量%,較佳係0.005至1.5質量%,更佳係0.005至1質量%。調配量若未達0.005質量%,則有無法獲得適當的濃厚感之情形,若調配超過2質量%,則有產生發黏性之情形。
(b)成分(a)以外之水相成分
於本發明中,就成分(a)以外之水相成分而言,除了可調配水等水系溶劑之外,還可以在無損於本發明效果之範圍調配通常化妝品所使用之水性成分。
水系溶劑之例可舉出:水、水溶性醇等。
水係可使用蒸餾水、逆浸透水、離子交換水等精製水及自來水等。
水溶性醇係可舉出例如:低級醇、多元醇、多元醇聚合物、2元醇烷基醚類、2元醇烷基醚類、2元醇醚酯、甘油單烷基醚、糖醇等。
低級醇可舉出例如:乙醇、丙醇、異丙醇、異丁醇、第三丁醇等。
多元醇可舉出例如:2元醇(例如:二丙二醇、1,3-丁二醇、乙二醇、三亞甲基二醇、1,2-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)、3元醇(例如:甘油、三羥甲基丙烷等)、4元醇(例如:二甘油、1,2,6-己三醇等新戊四醇等)、5元醇(例如木醣醇、三甘油等)、6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-三甘油、四甘油、聚甘油等)、2元醇
烷基醚類(例如:乙二醇單甲基醚、乙二醇單乙基醚、乙二醇單丁基醚、乙二醇單苯基醚、乙二醇單己基醚、乙二醇單2-甲基己基醚、乙二醇異戊基醚、乙二醇苯甲基醚、乙二醇異丙基醚、乙二醇二甲基醚、乙二醇二乙基醚、乙二醇二丁基醚等)等。
水性成分之例係可舉出:保濕劑、水溶性高分子、親水性粉體、無機鹽、有機鹽、維生素類、pH調整劑等。
保濕劑係可舉出:1,3-丁二醇、聚乙二醇、丙二醇、二丙二醇、己二醇、甘油、二甘油、木醣醇、麥芽糖醇、麥芽糖、D-甘露醇等。再者,亦可調配聚氧乙烯(以下記為POE)/聚氧丙烯(以下記為POP)共聚物二烷基醚。POE/POP共聚物二烷基醚之烷基係可為相同亦可為相異之碳數1至4的烷基,較佳係甲基、乙基,特佳係甲基。相對於POE基及POP基之合計,POE基係以20至80重量%為較佳。POE/POP係無規型、嵌段型之任一者,但較佳係無規型。如此之POE/POP共聚物二烷基醚係例如記載於日本特開2004-83541號公報、日本特開2006-265135號公報等中。如此之化合物係可舉出例如:POE(9)POP(2)二甲基醚、POE(7)POP(12)二甲基醚、POE(14)POP(7)二甲基醚、POE(17)POP(4)二甲基醚、POE(10)POP(10)二甲基醚、POE(6)POP(14)二甲基醚、POE(15)POP(5)二甲基醚、POE(25)POP(25)二甲基醚、POE(27)POP(14)二甲基醚、POE(55)POP(28)二甲基醚、POE(36)POP(41)二甲基醚、POE(9)POB(2)二甲基醚、POE(14)POB(7)二甲基醚、POE(10)POP(10)二乙基醚、POE(10)POP(10)二丙基醚、POE(10)POP(10)二丁基醚等。
水溶性高分子係可舉出:阿拉伯橡膠、角叉菜膠(carrageenan)、果膠、瓊脂、榅桲籽(quince seed)(榅桲,cydonia oblonga)、澱粉、藻膠(褐藻萃取物)
等植物系高分子;糊精、聚三葡萄糖(pullulan)等微生物系高分子;膠原蛋白、酪蛋白、明膠等動物系高分子;羧甲基澱粉、甲基羥丙基澱粉等澱粉系高分子;藻酸鈉等藻酸系高分子;麩醯胺酸鈉、羧基乙烯基聚合物(CARBOPOL等)等乙烯基系高分子;聚氧乙烯系高分子、聚氧乙烯聚氧丙烯共聚物系高分子;聚丙烯酸鈉、聚丙烯醯胺等丙烯酸系高分子;膨土、矽酸鋁鎂、合成鋰皂石(laponite)等無機系水溶性高分子等。
親水性粉體係可舉出:無機粉末(例如:滑石、高嶺土、絹雲母、白雲母、合成雲母、金雲母、紅雲母、黑雲母、鋰雲母、蛭石、碳酸鎂、碳酸鈣、矽藻土、矽酸鎂、矽酸鈣、矽酸鋁、矽酸鋇、矽酸鍶、鎢酸金屬鹽、二氧化矽、羥磷灰石、沸石、氮化硼、陶瓷粉末等);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、苯乙烯及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(例如芒紫、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:氧化鈦塗覆雲母、氧化鈦塗覆氧氯化鉍、氧化鈦塗覆滑石、著色氧化鈦塗覆雲母、氧氯化鉍、魚鱗箔等);金屬粉末顏料(例如:鋁粉末、銅粉末等);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。
(c)油性成分
本發明中,就(c)油性成分而言,係可在無損於本發明效果之範圍調配通常化妝品所使用之油分。
可調配於本發明之油分的例子係可舉出:烴、酯油、植物性油脂、動物性油脂、高級醇、高級脂肪酸、聚矽氧油等。
烴可舉出:液體石蠟、石蠟、角鯊烷、角鯊烯、地蠟(ozocerite)、降植烷、純地蠟(ceresin)、凡士林、微晶蠟等。
酯油係可舉出: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、二2-乙基己酸乙二醇、二新戊四醇脂肪酸酯、單異硬脂酸N-烷二醇、二癸酸新戊二醇、蘋果酸二異硬脂酯、二2-庚基十一酸甘油酯、三2-乙基己酸三羥甲基丙烷、三異硬脂酸三羥甲基丙烷、三辛酸甘油酯、三異棕櫚酸甘油酯、鯨蠟基2-乙基己酸酯、四2-乙基己酸新戊四醇、三2-乙基己酸甘油酯、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、蓖麻油脂肪酸甲基酯、油酸油酯、乙醯基甘油酯、棕櫚酸2-庚基十一酯、己二酸二異丁酯、N-月桂醯基-L-麩醯胺酸-2-辛基十二酯、己二酸二-2-庚基十一酯、乙基月桂酸酯、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、己二酸二2-己基癸酯、癸二酸二異丙酯、檸檬酸三乙酯、琥珀酸二乙基己酯等。
植物性油脂係可舉出:酪梨油、日本山茶油、夏威夷豆油、玉米油、橄欖油、菜籽油、芝麻油、蓖麻油、花生油、杏仁油、大豆油、茶籽油、荷荷芭油、胚芽油等。
動物性油脂係可舉出:海龜油、蛋黃油、貂油等。
高級醇係可舉出:油醇、硬脂醇、異硬脂醇、山萮醇(behenyl alcohol)、辛基十二醇、癸基十四醇、荷荷芭醇、鯨蠟醇、肉豆蔻醇等,高級脂肪酸係可舉出:油酸、異硬脂酸、亞麻油酸、次亞麻油酸、二十碳五烯酸、棕櫚酸、硬脂酸、山萮酸等。
聚矽氧油係可舉出例如:鏈狀聚矽氧烷(例如二甲基聚矽氧烷、甲基苯基聚矽氧烷、二苯基聚矽氧烷、甲基氫聚矽氧烷等)、形成3維網目狀構造之聚矽氧樹脂、聚矽氧橡膠、丙烯酸聚矽氧類等。
又,上述以外,亦可調配可吸收(含水)大量的水之「含水性油分」。所謂的含水性油分係具有保持水之性質的油分,特佳係含水力為100%以上者,亦即,可保持本身重量以上之水者。
含水性油分係可舉出:二新戊四醇六羥基硬脂酸酯、四(山萮酸/安息香酸/乙基己酸)新戊四醇、夏威夷豆油脂肪酸植物固醇酯、N-月桂醯基-L-麩醯胺酸二(植物固醇基、2-辛基十二基)酯、三異硬脂酸甘油酯、夏威夷豆油聚甘油基-6酯類山萮酸酯等。
上述油分之中,於本發明係可適合使用揮發性油分。藉由連續相之油相係含有揮發性油分,而期待對肌膚之親膚感及光澤感等使用性的提升。在此所謂的揮發性油分,係指在常壓之沸點為260℃以下之油分(低沸點油分)。代表性者係可舉出:異石蠟系烴油和聚矽氧油。
低沸點異石蠟系烴油係可舉出例如:異十二烷、異十六烷等。又,低沸點聚矽氧油係可舉出:矽數4至6之環狀二甲基聚矽氧烷、矽數2至5之鏈狀二甲基聚矽氧烷。
在本發明之油中水型乳化化妝料中係可使用上述油分1種或2種以上。本發明之油中水型乳化化妝料中的油分之適當調配量係10至60質量%,特佳係15至50質量%。
又,本發明亦可調配紫外線吸收劑作為成分(c)。
紫外線吸收劑之例係可舉出例如:安息香酸系紫外線吸收劑(例如:對胺基安息香酸(以下記為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);蒽酸系紫外線吸收劑(例如:升薄荷腦基-N-乙醯基鄰胺苯甲酸酯等);水楊酸系紫外線吸收劑(例如:水楊酸戊酯、水楊酸薄荷腦酯、水楊酸升薄荷腦酯、水楊酸辛酯、水楊酸苯酯、水楊酸苯甲酯、水楊酸對-異丙醇苯基酯等);桂皮酸系紫外線吸收劑(例如:甲氧基桂皮酸辛酯、4-異丙基桂皮酸乙酯、2,5-二異丙基桂皮酸甲酯、2,4-二異丙基桂皮酸乙酯、2,4-二異丙基桂皮酸甲酯、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-乙基乙酯、對-甲氧基桂皮酸環己酯、α-氰基-β-苯基桂皮酸乙酯、α-氰基-β-苯基桂皮酸2-乙基己酯、單-2-乙基己醯基-二對甲氧基桂皮酸甘油酯等);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(dianisoyl methane);4-甲氧基-4'-第三丁基二苯甲醯基甲烷;5-(3,3-二甲基-2-亞降莰基)-3-戊烷-2-酮、二嗎啉基嗒酮(dimorpholinopyridazinone);2-乙基己基-2-氰基-3,3-二苯基丙烯酸酯;2,4-雙-{[4-(2-乙基己基氧基)-2-羥基]-苯基}-6-(4-甲氧基苯基)-(1,3,5)-三等。
又,本發明中,成分(c)可調配油溶性藥劑、香料等。油溶性藥劑之例可舉出:維生素A、維生素A衍生物等油溶性維生素等。
在本發明中,(c)油性成分之調配量係60質量%以下,較佳係50質量%以下,更佳係40質量%以下。若成分(c)之調配量超過60質量%,則會變得難以獲得具備本發明之全部效果的油中水型乳化化妝料。
(d)乳化劑
在本發明,(d)乳化劑可使用通常能夠使用在化妝料者。
乳化劑係可使用HLB為7以下者,特別以5以下者為佳。又,上述HLB之值係可藉由以HLB=7+11.7‧LOG(MW/MO)(惟,MW係表示親水基部之分子量,MO係表示親油基部之分子量)表示之川上式來算出。
可適合使用於本發明之乳化劑可舉出例如:有機改質黏土礦物、聚矽氧系界面活性劑、多元醇脂肪酸酯系界面活性劑等。
有機改質黏土礦物係可舉出例如:二甲基烷基銨水輝石、苯甲基二甲基硬脂基銨水輝石、氯化二硬脂基二甲基銨處理矽酸鋁鎂等。
聚矽氧系界面活性劑係可舉出例如:聚(氧乙烯/氧丙烯)甲基聚矽氧烷共聚物、聚氧乙烯甲基聚矽氧烷共聚物、聚矽氧鏈分枝型甲基聚矽氧烷共聚物、烷鏈分枝型聚氧乙烯甲基聚矽氧烷共聚物、烷基鏈/聚矽氧鏈分枝型聚氧乙烯甲基聚矽氧烷共聚物、交聯型聚氧乙烯甲基聚矽氧烷、含有烷基之交聯型聚氧乙烯甲基聚矽氧烷、分枝型聚甘油改質聚矽氧、烷基分枝型聚甘油改質聚矽氧等。
多元醇脂肪酸酯系界面活性劑可舉出例如:甘油脂肪酸酯、聚甘油脂肪酸酯、聚氧乙烯甘油脂肪酸酯、山梨醇酐脂肪酸酯、聚氧乙烯山梨醇酐脂肪酸酯等。
相對於組成物全部量,本發明之油中之水型乳化化妝料的(d)乳化劑之調配量係以0.01至10質量%為較佳,更佳係0.1至5質量%。
(e)疏水化處理粉體
本發明之油中水型乳化化妝料中亦可進一步調配(e)疏水化處理粉體。
疏水化處理粉體之例可舉出例如:將粉體之表面使用甲基氫聚矽氧烷、二甲基聚矽氧烷等聚矽氧類(包括聚矽氧彈性物)、糊精脂肪酸酯、高級脂肪酸、高級醇、脂肪酸酯、金屬皂、烷基磷酸醚、氟化合物或角鯊烷、石蠟等烴類等,而藉由使用溶劑之濕式法、氣相法、機械化學法等進行疏水化處理者;或者,以二氧化矽被覆了粉體之後,藉由經烷基改質之矽烷偶合劑等施予疏水化處理者等。
其中,疏水化處理較佳係以聚矽氧類進行處理,特別是可適合使用彈性物處置。可適合使用於本發明之聚矽氧彈性物之例係可舉出:將具有胺基之聚矽氧聚合物(特佳係側鏈型胺基改質聚矽氧)及具有羧基之聚矽氧聚合物予以混合,並藉由加熱所製造之彈性物(參照WO2017/209077)。
進行前述疏水化處理之粉體並無特別限制,可舉出例如:滑石、高嶺土、絹雲母、白雲母、氧化鈦、氧化鐵等無機白色顏料;氧化鐵(鐵丹)、鈦酸鐵等無機紅色系顏料;黃色氧化鐵、黃土等無機黃色系顏料;芒紫、鈷紫等無機紫色系顏料;氧化鉻、氫氧化鉻、鈷鈦酸等無機綠色系顏料;群青、普魯士藍等無機藍色系顏料;氧化鈦塗覆雲母、氧化鈦塗覆羥氧化鉍、氧氯化鉍、氧化鈦塗覆滑石、魚鱗箔、著色氧化鈦塗覆雲母等珠光顏料;鋁粉末、銅粉末等金屬粉末顏料;合成雲母、金雲母、紅雲母、黑雲母、鋰雲母、蛭石、碳酸鎂、碳酸鈣、矽藻土、矽酸鎂、矽酸鈣、矽酸鋁、矽酸鋇、矽酸鍶、鎢酸金屬鹽、α-氧化鐵、水合氧化鐵、氧化矽、羥磷灰石等無機粉末;尼龍粉末、聚乙烯粉末、苯并胍胺粉末、微晶性纖維素、聚矽氧粉末等有機粉末等。又,亦可舉出微粒子氧化鈦和微粒子氧化鋅等抗紫外線粉末、或在有機粉末被覆有無機粉末之複合粉末等。
本發明係藉由一同調配成分(a)與疏水化處理粉體,而可更為提升賦予肌膚光滑度之效果及無發黏性。尤其,在使用聚矽氧彈性物作為疏水化處理粉體之情形下,可獲得更加顯著的效果。
相對於化妝料,本發明之油中水型乳化化妝料中的疏水化處理粉體之調配量係0.1至20質量%,較佳係1至10質量%。若疏水化處理粉體之調配量若少於0.1質量%,則有無法感受到光滑度之情形;若超過20質量%,則有喪失易延展性之情形。
本發明之油中水型乳化化妝料中,係可在無損於本發明效果之範圍適當調配通常被使用在化妝品之其它成分,而製造化妝料。
本發明之化妝料之製品形態並無特別限制,可舉出例如:粉底、底妝料、腮紅、眼影、眼線筆、眉粉、睫毛膏等上妝化妝料;和乳霜、乳液、面膜、防曬化妝料等護膚化妝料。
有關本發明之油中水型乳化化妝料係可依照一定方法來製作。例如,可將油相成分進行混合溶解,並將其於攪拌同時添加至水相成分而進行乳化來製造。
以下,係使用實施例來進一步詳細說明本發明,但不藉由該等實施例來限定本發明之範圍。又,本實施例中之調配量若無特別聲明,即為質量%。
首先,表示在實施例所使用之分子量調控聚丙烯酸鈉之合成方法。
<製造例1>
使用活性自由基聚合之RAFT聚合法合成出分子量經調控之聚丙烯酸鈉。使用4,4’-偶氮雙-(4-氰基纈草酸)(V-501,和光純藥工業公司製)作為聚合起始劑,並使用4-氰基戊酸二硫苯甲酸酯(依據非專利文獻1合成,於後稱為CPD)作為鏈轉移劑。
於離子交換水(9ml)中溶解丙烯酸(2514mg)、亞甲基雙丙烯醯胺(9.6μg)及V-501(0.17mg),加入溶解有CPD(0.17mg)之甲醇溶液(1ml),於氬氣環境下,在60℃進行聚合反應24小時。聚合反應後,添加氫氧化鈉水溶液,中和至pH6至7左右之後,對於精製水透析4日,其後,藉由進行凍結乾燥而回收分子量調控聚丙烯酸鈉-3(1.99g,產率79%)。使用GPC進行解析,結果係重量平均分子量為326萬,分子量分布為1.7。
在下表中,以*標記出之成分係如以下者。*1:將滑石JA-68R(淺田製粉公司製)以彈性物進行了表面處理者(相當於WO2017/209077之試驗例3-1之彈性物處理滑石),該彈性物係由胺基乙基胺基丙基甲基矽氧烷/二甲基矽氧烷共聚物及PCA聚二甲基矽氧烷所構成者。
依據下述製造方法製作出記載於表1-4之配方的油中水型乳化化妝料,並藉由下述方法評估物性。表1及表2係乳霜之配方,表3係粉底之配方,表4係粉底之配方。再者,有關下述項目(7)至(10),係任用專業評測員來進行實際使用試驗。將結果一併表示於各表。
<製造方法>
將彈性物處理滑石以外之油相成分混合,並加熱至約80℃而溶解之後,添加混合彈性物處理滑石並使其分散。另一方面,混合水相成分,加熱至約80℃。將前述油相成分之部分進行較強烈的攪拌,同時徐緩添加前述水相成分之部分,使其乳化之後,進行攪拌冷卻而獲得油中水型乳化化妝料。
<物性評估等>
‧硬度
在25℃之環境下,使用流變儀(不動工業股份有限公司製:NRM-3002D;直徑11.3mm、針入3mm)測定硬度。在本發明中,硬度為5以上之情形係判斷為形成乳霜之適當的硬度。
‧黏度
在30℃使用旋轉型黏度計(BL型、12rpm、1分鐘)測定剛調製後之各試料的黏度(mPa.s)。
‧乳化粒子徑
藉由光學顯微鏡(OLYMPUS公司製:BX60)進行觀察。
‧製劑化
在各表中,係將成為所希望之化妝料的劑型者以A表示,並將未成為所希望之化妝料的劑型者以C表示。
<實際使用試驗>
讓10名專業評測員將試驗組成物塗佈於臉上,並對於濃厚感、延展性良好度、肌膚之柔潤度、肌膚之光滑度、無發黏性進行回答有無該效果。依據以下之基準累積統計回答結果,並記載於表中。
S:9名以上回答為有效果。
A:7名以上8名以下回答為有效果。
B:5名以上6名以下回答為有效果。
C:4名以下回答為有效果。
在本發明中,係將S及A設為合格,將B及C設為不合格。
如表1所示,在比較例1之乳霜係延展性差,亦會感受到發黏性,但在該配方中追加了(a)分子量調控聚丙烯酸鈉(製造例1)作為水相成分之實施例1的乳霜則係延展性非常良好,無發黏性優異,同時賦予肌膚柔潤度之效果亦為非常優異。又,該乳霜的濃厚感及賦予肌膚光滑度之效果亦優異(實施例1)。
再者,在實施例1之配方中追加了彈性物處理滑石之乳霜(實施例2)的賦予肌膚光滑度之效果及無發黏性亦非常優異。
又,如表2所示,比較例2之乳霜係延展性差,亦感受到發黏性,但在該配方中追加了(a)分子量調控聚丙烯酸鈉(製造例1)作為水相成分之實施例3的乳霜則係延展性非常良好,無發黏性優異,同時賦予肌膚柔潤度之效果亦為非常優異。又,該乳霜的濃厚感及賦予肌膚光滑度之效果亦優異(實施例3)。
再者,在實施例3之配方中追加了彈性物處理滑石之乳霜(實施例4)的賦予肌膚光滑度之效果及無發黏性亦非常優異。
上述係雖然係成分(c)的調配量較少之乳霜間的比較(調配量為15質量%或26質量%),但在成分(c)的調配量為49質量%(比較例3、實施例5)及60質量%(比較例4、實施例6)之乳霜中,藉由追加(a)分子量調控聚丙烯酸鈉(製造例1),濃厚感、延展性良好度、無發黏性係顯著提升(比較例3對照實施例5、比較例4對照實施例6)。
再者,在將油分之調配量提高至成分(c)之調配量成為68質量%為止之情形下,雖然未成為能稱作乳霜之劑型(比較例5),但若在該配方中追加(a)分子量調
控聚丙烯酸鈉(製造例1),則可獲得乳霜(比較例6)。然而,比較例6之乳霜並未獲得良好延展性、肌膚之柔潤度、肌膚之光滑度及無發黏性。
因而,若在成分(c)之調配量為60質量%以下之油中水型乳化化妝料之內水相中調配分子量經調控之聚丙烯酸鹽,則延展性會變得非常良好,且發黏感少,濃厚感增加,顯示更優異的賦予肌膚柔潤度及光滑度之效果。
其次,就與分子量未經調控之聚丙烯酸鹽之效果的差異進行研討。該聚丙烯酸鹽係使用將重量平均分子量為75萬與400萬之市售品的聚丙烯酸(Sigma Aldrich公司製)與本案製造例1同樣地以氫氧化鈉進行了中和者。
如表3所示,若在比較例2之配方中追加分子量未經調控之聚丙烯酸,則雖然改善了無發黏性,但延展性良好度、或賦予肌膚柔潤度和光滑度之效果係無變化(比較例7、8)。
因而,表示前述之使用感的提升,尤其延展性良好度及賦予肌膚柔潤度和光滑度之效果的顯著提升係因為於水相中所追加之聚丙烯酸鹽經分子量調控的緣故。
如表4所示,就在比較例9之配方中追加了(a)分子量調控聚丙烯酸鈉(製造例1)之粉底(實施例7)而言,相較於比較例9之配方之粉底係濃厚感、延展性良好度、賦予肌膚柔潤度和光滑度之效果、無發黏性為優異。而且,進一步追加了彈性物處理滑石之粉底(實施例8)係賦予肌膚光滑度之效果亦優異。
依以上之結果,當在(c)油性成分之調配量為60質量%以下之油中水型乳化化妝料中調配經分子量調控之聚丙烯酸鹽時,則延展性變得非常良好,發黏感少,濃厚感增加,顯示更優異的賦予肌膚柔潤度及光滑度之效果。
以下,舉出本發明之油中水型乳化化妝料之配方例。而本發明不以此等配方例作任何限定,自不待言。又,調配量係表示相對於全部化妝料總量之質量%。
配方例1:身體乳霜
配方例2:防曬乳霜
配方例3:防曬乳霜
配方例4:防曬乳霜
配方例5:乳霜
配方例6:乳霜
成分 調配量(質量%)
配方例7:乳霜
配方例8:乳霜
配方例9:粉底
配方例10:粉底
配方例11:粉底
成分 調配量(質量%)
配方例12:二層型粉底
配方例13:乳霜粉底
配方例14:底妝料
配方例15:遮瑕膏
Claims (4)
- 一種油中水型乳化化妝料,係包含下述成分(a)至(d);(a)選自由聚丙烯酸、聚丙烯酸之鹽、聚(2-丙烯醯胺-2-甲基丙磺酸)、及聚(2-丙烯醯胺-2-甲基丙磺酸)之鹽所組成群組之1種以上的聚合物,且該聚合物之重量平均分子量為100萬至400萬,而且,作成1質量%水溶液時在25℃的黏度為1Pa‧s以下,該聚合物中,分子量為1000萬以上之分子物種的含量為10質量%以下;(b)成分(a)以外之水相成分;(c)油性成分為60質量%以下;(d)HLB為7以下之乳化劑。
- 如申請專利範圍第1項所述之油中水型乳化化妝料,其中,成分(a)之含量為0.005%至2%。
- 如申請專利範圍第1或2項所述之油中水型乳化化妝料,其中,前述成分(a)之重量平均分子量為150萬至400萬。
- 如申請專利範圍第1或2項所述之油中水型乳化化妝料,更包含成分(e)疏水化處理粉體。
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