CN109715133A - 使用了核-壳型微粒的化妆品原料和水包油型乳化化妆品 - Google Patents
使用了核-壳型微粒的化妆品原料和水包油型乳化化妆品 Download PDFInfo
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- CN109715133A CN109715133A CN201780059745.7A CN201780059745A CN109715133A CN 109715133 A CN109715133 A CN 109715133A CN 201780059745 A CN201780059745 A CN 201780059745A CN 109715133 A CN109715133 A CN 109715133A
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Abstract
本发明提供由乳化力不被交联水平所左右的核‑壳型微粒构成的乳化剂、和通过该乳化剂进行乳化而得的水包油型乳化化妆品。使用一种化妆品用原料,所述化妆品用原料的特征在于:由核‑壳型微粒构成,所述核‑壳型微粒是在(A)~(D)的条件下将式(1)所表示的聚氧化乙烯大分子单体、和选自式(2)所表示的丙烯酸酯衍生物单体和式(3)所表示的丙烯酰胺衍生物单体的1种或者2种以上的疏水性单体进行自由基聚合而得到的。
Description
相关申请
本申请主张2016年09月27日申请的日本专利申请2016-188437号的优先权,并将其纳入本申请中。
技术领域
本发明涉及化妆品用原料,更详细而言,涉及由核-壳(core-corona,核-冠)型微粒构成的化妆品原料和使用了该化妆品原料的水包油型乳化化妆品。
背景技术
近年来,随着重视安全性的消费者的增加,实质上不含表面活性剂的化妆品处于受欢迎的趋势。另外,由于表面活性剂的大量混合会成为发粘感的原因,因此希望有一种不依赖于表面活性剂进行乳化的方法。
作为不使用表面活性剂而制作水包油型乳化物的方法,已知有使粉末吸附于油相和水相的界面进行乳化的皮克林乳液(Pickering emulsion)法(例如专利文献1、非专利文献1)。作为该粉末,广泛使用金属氧化物或矿物(例如二氧化硅)等无机粉末,这些粉末的乳化能力弱,需要大量混合,因此存在着所得化妆品感觉到粉末感或粗糙感的问题。而且,通过无机粉末乳化而得的油滴耐冲击性弱,通过搅拌或振动容易融合为一体,因此化妆品的乳化稳定性低已成为课题。
因此,由本发明人提出了使用核-壳型微凝胶进行乳化的方法。核-壳型微凝胶是1种或者2种以上的聚合物交联而形成的颗粒,且形成了亲水性区域暴露于核部表面的结构,所述核部是聚合物的疏水性区域交联形成球状而得到的。核-壳型微凝胶吸收溶剂时会溶胀而形成凝胶状,因此在化妆品领域主要用作增稠剂或覆膜剂(非专利文献2)。
本发明人发现了:将特定的聚氧化乙烯大分子单体、特定的丙烯酸酯衍生物单体和特定的交联性单体在特定条件下进行自由基聚合得到的核-壳型微凝胶,相对于有机溶剂的溶胀性非常高,可以稳定地将各种油分乳化。而且,还报道了:通过以该微凝胶作为乳化剂,可得到乳化稳定性优异、发粘感少、粉末感或粗糙感少的水包油型乳化化妆品(专利文献2-4)。
然而,上述微凝胶存在以下问题:若核部的交联密度低,则溶胀时核结构崩解,若交联密度过高,则微凝胶彼此凝集,任一种情况下均无法起到乳化剂的作用。
现有技术文献
专利文献
专利文献1:日本特表2001-518111号公报;
专利文献2:日本特开2006-161026号公报;
专利文献3:日本专利第4577721号公报;
专利文献4:日本专利第5207424号公报;
非专利文献
非专利文献1:B. Binks等人, Advances in Colloid and Interface Science, 100-102(2003);
非专利文献2:J. Colloid Interface Sci., 274, 49(2004)。
发明内容
发明所要解决的课题
本发明是鉴于上述情形而进行的,目的在于提供:由乳化力不被交联水平所左右的核-壳型微粒构成的乳化剂;以及通过该乳化剂进行乳化而得的水包油型乳化化妆品。
用于解决课题的手段
本发明人对上述课题进行了深入研究,结果发现了:通过使特定的丙烯酰胺衍生物和丙烯酸酯衍生物在特定条件下进行自由基聚合而不进行交联,得到可以广泛用作水包油型乳化剂的核-壳型微粒。而且还发现了:通过该微粒乳化而得的水包油型乳化化妆品,其乳化稳定性优异、发粘感少、粉末感或粗糙感少,而且水洗性也优异,从而完成了本发明。
即,本发明包含以下内容。
[1] 化妆品用原料,其特征在于:由核-壳型微粒构成,所述核-壳型微粒是在下述(A)~(D)的条件下将下述式(1)所表示的聚氧化乙烯大分子单体、和选自下述式(2)所表示的丙烯酸酯衍生物单体和下述式(3)所表示的丙烯酰胺衍生物单体的1种或者2种以上的疏水性单体进行自由基聚合而得到的;
(A) 以上述聚氧化乙烯大分子单体的加料摩尔量/(上述丙烯酸酯衍生物单体和/或丙烯酰胺衍生物单体)的加料摩尔量表示的摩尔比为1:10~1:250;
(B) 下述式(1)所示的大分子单体是具有重复单元为8~200的聚乙二醇基的丙烯酸衍生物或甲基丙烯酸衍生物;
下述式(2)所示的丙烯酸酯衍生物单体是具有包含碳原子数为1~12的烷基的取代基的丙烯酸衍生物或甲基丙烯酸衍生物;
下述式(3)所示的丙烯酰胺衍生物单体是具有包含碳原子数为1~18的烷基的取代基的丙烯酰胺衍生物或甲基丙烯酰胺衍生物;
(C) 聚合溶剂为水-醇混合溶剂,醇为选自乙醇、二丙二醇、1,3-丁二醇、异戊二醇的1种或2种以上;
(D) 水-醇混合溶剂的溶剂组成以20℃的质量比计为水:醇=90~10:10~90。
[化学式1]
R1表示H或者碳原子数为1~3的烷基,n为8~200的数。X表示H或者CH3。
[化学式2]
R2表示H或者碳原子数为1~3的烷基,R3表示包含碳原子数为1~12的烷基的取代基。
[化学式3]
R4表示H或者碳原子数为1~3的烷基,R5和R6表示H或者包含碳原子数为1~18的烷基的取代基。
[2] [1]所述的化妆品用原料,其特征在于:上述核-壳型微粒的粒径为50~400nm。
[3] 乳化剂,其特征在于:由上述[1]或[2]所述的化妆品用原料构成。
[4] 水包油型乳化化妆品,其特征在于:通过上述[3]所述的乳化剂进行乳化而得。
[5] 白浊化剂,其特征在于:由上述[1]或[2]所述的化妆品用原料构成。
发明效果
根据本发明,提供由非交联性的核-壳型微粒构成的乳化剂。另外,通过使用该乳化剂,提供乳化稳定性优异、发粘感少、粉末感或粗糙感少、而且水洗性也优异的水包油型乳化化妆品。
附图简述
[图1]是分析本发明所涉及的核-壳型微粒(制备例5)和现有型的交联型核-壳型微粒((丙烯酸酯类/甲氧基PEG-90甲基丙烯酸酯)交联聚合物)给油/水表面张力带来的效果的曲线图。
[图2]是分析本申请实施例和比较例的化妆品的水洗性的曲线图。
具体实施方式
下面,对本发明的(I)化妆品用原料和(II)该原料的用途进行详细说明。
(I) 化妆品用原料
本发明所涉及的化妆品用原料是在特定条件下将下述式(1)~(3)所示的单体进行自由基聚合而得到的核-壳型微粒的分散液。
[化学式4]
R1是碳原子数为1~3的烷基,n(聚氧化乙烯部分的分子量)为8~200的数。X为H或者CH3。
上述式(1)所表示的聚氧化乙烯大分子单体优选为丙烯酸衍生物或甲基丙烯酸衍生物。例如可以使用由Aldrich公司市售的市售品、或者由日油株式会社出售的BLEMMER(注册商标)等市售品。作为例子,可以使用作为甲氧基聚乙二醇单甲基丙烯酸酯的PME-400、PME-1000、PME-4000 (式(1)中的n值分别如下:n=9、n=23、n=90,均由日油株式会社制造)。
[化学式5]
R2表示碳原子数为1~3的烷基,R3表示包含碳原子数为1~12的烷基的取代基。
上述式(2)所表示的疏水性单体优选为丙烯酸衍生物或者甲基丙烯酸衍生物,例如可以使用丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸丁酯、丙烯酸戊酯、丙烯酸己酯、丙烯酸庚酯、丙烯酸辛酯、丙烯酸癸酯、丙烯酸十二烷基酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸丁酯、甲基丙烯酸戊酯、甲基丙烯酸己酯、甲基丙烯酸庚酯、甲基丙烯酸辛酯、甲基丙烯酸癸酯、甲基丙烯酸十二烷基酯等。其中,特别优选为甲基丙烯酸甲酯(别名:Methyl methacrylate)、甲基丙烯酸丁酯(别名:Butyl Methacrylate)、甲基丙烯酸辛酯。
这些疏水性单体是通用原料,作为普通工业原料也可以容易地获取。例如可以使用由Aldrich公司或者东京化成公司市售的市售品。
[化学式6]
R4表示H或者碳原子数为1~3的烷基,R5和R6表示H或者包含碳原子数为1~18的烷基的取代基。
上述式(3)所表示的疏水性单体优选为丙烯酰胺衍生物或者甲基丙烯酰胺衍生物。例如,可以优选使用叔丁基丙烯酰胺、N,N-二甲基丙烯酰胺、N-[3-(二甲基氨基)丙基]丙烯酰胺、叔丁基甲基丙烯酰胺、辛基丙烯酰胺、辛基甲基丙烯酰胺、十八烷基丙烯酰胺等。其中,特别优选叔丁基丙烯酰胺、N,N-二甲基丙烯酰胺、N-[3-(二甲基氨基)丙基]丙烯酰胺。
这些疏水性单体能够以市售品或者工业用原料的形式获取。
构成本发明所涉及的核-壳型微粒的共聚物是按照下述(A)~(D)的条件,通过任意的自由基聚合法使上述式(1)所表示的大分子单体、和选自上述式(2)和(3)所表示的疏水性单体的1种或者2种以上共聚而得到的。
(A) 以上述聚氧化乙烯大分子单体的加料摩尔量/(上述丙烯酸酯衍生物单体和/或丙烯酰胺衍生物单体)的加料摩尔量表示的摩尔比为1:10~1:250;
(B) 下述式(1)所示的大分子单体是具有重复单元为8~200的聚乙二醇基的丙烯酸衍生物或者甲基丙烯酸衍生物;
下述式(2)所示的丙烯酸酯衍生物单体是具有包含碳原子数为1~12的烷基的取代基的丙烯酸衍生物或者甲基丙烯酸衍生物;
下述式(3)所示的丙烯酰胺衍生物单体是具有包含碳原子数为1~18的烷基的取代基的丙烯酰胺衍生物或者甲基丙烯酰胺衍生物;
(C) 聚合溶剂为水-醇混合溶剂,醇为选自乙醇、二丙二醇、1,3-丁二醇、异戊二醇的1种或者2种以上。
(D) 水-醇混合溶剂的溶剂组成以20℃的质量比计为水:醇=90~10:10~90。
下面,对各条件进一步详述。
(条件(A))
上述聚氧化乙烯大分子单体和上述疏水性单体(即丙烯酸酯衍生物单体和/或丙烯酰胺衍生物单体的总和)的加料摩尔量在聚氧化乙烯大分子单体:疏水性单体=1:10~1:250(摩尔比)的范围内能够聚合。上述加料摩尔量优选1:10~1:200,更优选1:25~1:100。
疏水性单体的摩尔量相对于聚氧化乙烯大分子单体的摩尔量不足10倍时,所聚合的聚合物呈水溶性,不会形成核-壳型颗粒。另外,疏水性单体的摩尔量相对于聚氧化乙烯大分子单体的摩尔量为250倍以上时,聚氧化乙烯大分子单体所产生的分散稳定化不完全,由不溶性的疏水性单体形成的疏水性聚合物发生凝集、沉淀。
(条件(B))
条件(B)包含下述的(B-1)~(B-3)这3个条件。
(B-1)
式(1)所表示的大分子单体是具有重复单元为8~200的聚乙二醇基的丙烯酸衍生物或者甲基丙烯酸衍生物。重复单元为7以下时,有时无法得到稳定分散于溶剂的颗粒,超过200时,颗粒发生微细化,混合于化妆品时有时会变得不稳定。
(B-2)
上述式(2)所示的丙烯酸酯衍生物单体是具有包含碳原子数为1~12的烷基的取代基的丙烯酸衍生物或者甲基丙烯酸衍生物。碳原子数为0(没有末端酯键的单体)时,单体过于亲水,有时无法顺利地进行乳化聚合。另一方面,碳原子数为13以上时,有时无法得到令人满意的使用感。
(B-3)
上述式(3)所示的丙烯酰胺衍生物单体是具有包含碳原子数为1~18的烷基的取代基的丙烯酰胺衍生物或者甲基丙烯酰胺衍生物。
本发明所涉及的疏水性单体需要是选自上述式(2)所表示的丙烯酸酯衍生物单体和式(3)所表示的丙烯酰胺衍生物单体的1种或者2种以上混合而成的单体组成。
在本发明中,作为疏水性单体,特别优选使用甲基丙烯酸甲酯和甲基丙烯酸丁酯这2种,或者甲基丙烯酸甲酯、叔丁基丙烯酰胺、N,N-二甲基丙烯酰胺和N-[3-(二甲基氨基)丙基]丙烯酰胺这4种。在这些疏水性单体的组合中,进一步优选使用甲氧基聚乙二醇单甲基丙烯酸酯作为大分子单体。
作为本发明中最优选的大分子单体和疏水性单体的组合,可以列举如下,但并不限于此:
・聚乙二醇基的重复单元为8~90、最优选为15的甲氧基聚乙二醇单甲基丙烯酸酯、甲基丙烯酸甲酯和甲基丙烯酸丁酯;
・聚乙二醇基的重复单元为8~200、最优选为90的甲氧基聚乙二醇单甲基丙烯酸酯、甲基丙烯酸甲酯、甲基丙烯酸丁酯、叔丁基丙烯酰胺、N,N-二甲基丙烯酰胺和N-[3-(二甲基氨基)丙基]丙烯酰胺、叔丁基甲基丙烯酰胺、辛基丙烯酰胺、辛基甲基丙烯酰胺、十八烷基丙烯酰胺。
(条件(C))
聚合溶剂需要是水-醇混合溶剂。作为醇,优选可以溶解式(2)和(3)所示的疏水性单体的醇。因此,优选选自乙醇、二丙二醇、1,3-丁二醇、异戊二醇的1种或者2种以上。
(条件(D))
作为聚合溶剂的水-醇混合溶剂的溶剂组成以20℃的质量比计优选为水:醇=90~10:10~90,进一步优选为水:醇=80~20:20~80。醇的混合比低于10容量比时,疏水性单体的溶解能力变得极低,有时无法生成微粒。另外,醇的混合比超过90容量比时,无法通过疏水性相互作用生成疏水性单体的乳液,乳化聚合没有进行,有时无法得到微粒。
(II)用途
本发明所涉及的化妆品用原料于表面具有作为非离子性高分子的聚氧化乙烯链,因此在水中稳定分散。而且,在油相成分和水相成分这双方存在的条件下,核部吸收油相成分而溶胀,作为核表面的壳部与水相成分溶合,因此吸附于油相成分和水相成分的界面。因此,利用通常的乳化方法(将油相成分和水相成分搅拌混合进行乳化),可以得到表面吸附有本发明所涉及的化妆品原料的油滴分散在水相成分中的水包油型乳化体系。该油滴在进一步的搅拌或振动的冲击中不会轻易融合为一体,因此与使用了现有的无机粉体的皮克林乳液相比非常稳定。
这样,本发明所涉及的化妆品用原料可以适合用作进行水包油型乳化的乳化剂。本发明所涉及的化妆品用原料不会产生像普通的表面活性剂这样的发粘感,也不会产生像无机粉体这样的粉末感或粗糙感。而且,由于是皮克林乳液法,因此能够进行种类广泛的油分的乳化。
(水包油型乳化化妆品)
本发明所涉及的水包油型乳化化妆品是通过由上述核-壳型微粒构成的化妆品原料进行乳化而得的。这种情形的“乳化”可以改写为“该微粒存在于油滴与水相(连续相)的界面的状态”。由于本发明所涉及的水包油型乳化化妆品是通过该微粒进行乳化而得的,因此具有乳化稳定性高、发粘感少、粉末感或粗糙感少的特征。
相对于化妆品总量,化妆品中的本发明的化妆品用原料的混合量换算成核-壳型微粒的纯组分(純分)为0.01~10质量%,更优选0.05~5质量%,进一步优选0.05~2质量%。混合量不足0.01%时,有时无法得到稳定的化妆品,混合量超过10%时,在高温条件下的长期保存中有时稳定性差、或者有时使用感差。
本发明所涉及的水包油型乳化化妆品可以通过将上述化妆品用原料混合分散在水或者水相成分中,利用常规方法添加油相成分和其他成分进行搅拌、并施加剪切力进行乳化来制备。
下面,对本发明中可以使用的油相成分和水相成分等进行说明。
・油相成分
作为油相成分,可以列举:普通化妆品、准药品等中使用的烃油、高级脂肪酸、高级醇、合成酯油、硅油、液体油脂、固体油脂、蜡、香料等。
作为烃油,例如可以列举:异十二烷、异十六烷、异链烷烃、液体石蜡、地蜡、角鲨烷、降植烷、石蜡、纯地蜡、角鲨烯、凡士林、微晶蜡等。
作为高级脂肪酸,例如可以列举:月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、二十二烷酸(ベヘン酸)、油酸、十一碳烯酸、妥尔酸、异硬脂酸、亚油酸、亚麻酸、二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)等。
作为高级醇,例如可以列举:直链醇(例如,月桂醇、鲸蜡醇、硬脂醇、二十二烷醇、肉豆蔻醇、油醇、十六十八醇等);支链醇(例如,单硬脂基甘油醚(鲨肝醇)-2-癸基十四烷醇、羊毛脂醇、胆甾醇、植物甾醇、己基十二烷醇、异硬脂醇、辛基十二烷醇等)等。
作为合成酯油,例如可以列举:辛酸辛酯、壬酸壬酯、辛酸鲸蜡酯、肉豆蔻酸异丙酯、肉豆蔻酸辛基十二烷基酯、棕榈酸异丙酯、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、乳酸鲸蜡酯、乳酸肉豆蔻酯、乙酸羊毛脂、硬脂酸异鲸蜡酯、异硬脂酸异鲸蜡酯、12-羟基硬脂酸胆甾醇酯、二-2-乙基己酸乙二醇酯、二季戊四醇脂肪酸酯、单异硬脂酸N-烷基乙二醇酯、二癸酸新戊二醇酯、新戊酸二缩三丙二醇酯、苹果酸二异硬脂酯、二-2-庚基十一烷酸甘油酯、二异硬脂酸甘油酯、三羟甲基丙烷三-2-乙基己酸酯、三羟甲基丙烷三异硬脂酸酯、四-2-乙基己酸季戊四醇酯、三-2-乙基己酸甘油酯、三辛酸甘油酯、三异棕榈酸甘油酯、三羟甲基丙烷三异硬脂酸酯、鲸蜡基2-乙基己酸酯、2-乙基己基棕榈酸酯、三肉豆蔻酸甘油酯、三-2-庚基十一烷酸甘油酯、蓖麻油脂肪酸甲酯、油酸油酯、乙酰甘油酯、棕榈酸2-庚基十一烷基酯、已二酸二异丁酯、N-月桂酰-L-谷氨酸-2-辛基十二烷基酯、已二酸二-2-庚基十一烷基酯、月桂酸乙酯、癸二酸二-2-乙基己酯、肉豆蔻酸2-己基癸酯、棕榈酸2-己基癸酯、已二酸2-己基癸酯、癸二酸二异丙酯、琥珀酸2-乙基己酯、枸橼酸三乙酯等。
作为硅油,例如可以列举:链状聚硅氧烷(例如,二甲基聚硅氧烷、甲基苯基聚硅氧烷、二苯基聚硅氧烷等);环状聚硅氧烷(例如,八甲基环四硅氧烷、十甲基环五硅氧烷、十二甲基环六硅氧烷等);形成三维网状结构的硅树脂;硅橡胶;各种改性聚硅氧烷(氨基改性聚硅氧烷、聚醚改性聚硅氧烷、烷基改性聚硅氧烷、氟改性聚硅氧烷等);丙烯酸型硅氧烷类(アクリルシリコーン類)等。
作为液体油脂,例如可以列举:鳄梨油、山茶油、海龟油、澳洲坚果油、玉米油、貂油、橄榄油、菜籽油、蛋黄油、芝麻油、桃仁油、小麦胚芽油、山茶花油、蓖麻油、亚麻籽油、红花油、棉籽油、紫苏子油、大豆油、花生油、茶籽油、榧子油、米糠油、中国桐油、日本桐油、霍霍巴油、胚芽油、三甘油等。
作为固体油脂,例如可以列举:可可脂、椰子油、马油、氢化椰子油、棕榈油、牛油、羊油、氢化牛油、棕榈仁油、猪油、牛骨油、木蜡核油、氢化油、牛脚油、木蜡、氢化蓖麻油等。
作为蜡类,例如可以列举:蜂蜡、小烛树蜡、棉蜡、巴西棕榈蜡、杨梅蜡、虫蜡、鲸蜡、褐煤蜡、糠蜡、羊毛脂、木棉蜡、乙酸羊毛脂、液态羊毛脂、甘蔗蜡、羊毛脂脂肪酸异丙酯、月桂酸己酯、还原羊毛脂、霍霍巴蜡、硬质羊毛脂、虫胶蜡、POE羊毛脂醇醚、POE羊毛脂醇乙酸酯、POE胆甾醇醚、羊毛脂脂肪酸聚乙二醇酯、POE氢化羊毛脂醇醚等。
作为香料,可以列举:得自动物或植物的天然香料、通过化学合成手段制备的合成香料、和作为它们的混合物的调合香料,没有特别限定。通过混合香料,可以得到香味持久性优异的化妆品。
作为香料,具体而言,可以列举:アセチベノール、茴香醛、茴香脑、乙酸戊酯、水杨酸戊酯、乙醇酸烯丙基戊酯、己酸烯丙基酯、醛C6~20、黄葵内酯、麝葵内酯、降龙涎香醚、紫罗酮、イソイースーパー、丁香油酚、オウランチオール、佳乐麝香、蒈酮、香豆素、香叶醇、乙酸香叶酯、新檀香仲醇(Sandalore)、檀香醇、檀香(Sandela)、兔耳草醛(CyclamenAldehyde)、顺式-3-乙酸己烯酯、顺式-3-己醇、柠檬醛、乙酸香茅基酯、香茅醇、桉油醇、二氢月桂烯醇、茉莉内酯、肉桂醇、肉桂醛、乙酸苏合香酯、乙酸柏木酯、雪松醇、突厥酮、突厥烯酮、癸内酯、乙酸松油基酯、松油醇、トナリッド、吐纳麝香、女贞醛(triplal)、橙花醇、白檀醇、香兰素、羟基香茅醛、苯基乙酸乙酯、苯基乙基醇、水杨酸己酯、乙酸香根酯、希蒂莺(Hedione)、胡椒醛、新洋茉莉醛、ベルトフィックス、乙酸苄酯、水杨酸苄酯、苯甲酸苄酯、Pentalide(ペンタリッド)、ペンタリド、乙酸龙脑酯、マイオール、麝香酮、氨茴酸甲酯、二氢茉莉酮酸甲酯、2-甲氧基萘、氧化白柠檬、乙酸芳樟酯、芳樟醇、柠檬烯、新铃兰醛、铃兰醛、玫瑰醚、玫瑰醇、当归油、茴香油、青蒿油、罗勒油、月桂叶油、香柠檬油、白菖蒲油、樟脑油、依兰油、小豆蔻油、肉桂油、雪松油、芹菜油、春黄菊油、桂皮油、丁香油、芜荽油、枯茗油、莳萝油、榄香脂油、龙蒿油、桉树油、茴香精油、胡芦巴油、格蓬油、天竺葵精油、姜油、葡萄柚油、愈疮木油、桧叶油、桧木油、杜松子油、杂薰衣草油、薰衣草油、柠檬油、梨莓油、橘子油、ジラムオイル、含羞草油、薄荷油、留兰香油、水松油(ミルオイル)、桃金娘油(ミルトルオイル)、肉豆蔻油、橡苔精油、乳香油、防风根油、橙油、欧芹籽油、广藿香油、辣椒油、紫苏油、苦橙叶油、橙花精油、橙花油、甘椒油、多香果油、松油、玫瑰花油、迷迭香精油、香紫苏油、洋苏叶油、檀香油、苏合香油、タジェオイル、百里油、晚香玉油、缬草油、香根草油、紫罗兰叶油、冬青油、艾蒿油、依兰精油、柚子油、カッシーアブソリュート、ジュネアブソリュート、风信子原精、腊菊净油、茉莉原精、ジョンキルアブソリュート、水仙原精、玫瑰原精、紫罗兰叶原精、ベンベンゾイン等。
作为水相成分,可以混合普通化妆品、准药品等中使用的水、水溶性醇、增稠剂等,并且根据需要可以适当混合保湿剂、螯合剂、防腐剂、色素等。
对本发明的水包油型乳化化妆品中所含的水没有特别限定,例如可以列举:纯净水、离子交换水、自来水等。
作为水溶性醇,例如可以列举:低级醇、多元醇、多元醇聚合物、二元醇烷基醚类、二元醇烷基醚类、二元醇醚酯、甘油单烷基醚、糖醇、单糖、寡糖、多糖、和它们的衍生物等。
作为低级醇,例如可以列举:乙醇(有时简称为EtOH)、丙醇、异丙醇、异丁醇、叔丁醇等。
作为多元醇,例如可以列举:二元醇(例如,一缩二丙二醇、1,3-丁二醇、乙二醇、三亚甲基二醇、1,2-丁二醇、四亚甲基二醇、2,3-丁二醇、五亚甲基、2-丁烯-1,4-二醇、己二醇、辛二醇等),三元醇(例如,甘油、三羟甲基丙烷等),四元醇(例如,二甘油、1,2,6-己三醇等季戊四醇等),五元醇(例如,木糖醇、三甘油等),六元醇(例如,山梨糖醇、甘露糖醇等),多元醇聚合物(例如,二甘醇、一缩二丙二醇、三甘醇、聚丙二醇、四甘醇、二甘油、三甘油、四甘油、聚甘油等),二元醇烷基醚类(例如,乙二醇单甲基醚、乙二醇单乙基醚、乙二醇单丁基醚、乙二醇单苯基醚、乙二醇单己基醚、乙二醇单2-甲基己基醚、乙二醇异戊基醚、乙二醇苄基醚、乙二醇异丙基醚、乙二醇二甲基醚、乙二醇二乙基醚、乙二醇二丁基醚等),二元醇烷基醚类(例如,二甘醇单甲基醚、二甘醇单乙基醚、二甘醇单丁基醚、二甘醇二甲基醚、二甘醇二乙基醚、二甘醇丁基醚、二甘醇甲基乙基醚、三甘醇单甲基醚、三甘醇单乙基醚、丙二醇单甲基醚、丙二醇单乙基醚、丙二醇单丁基醚、丙二醇异丙基醚、一缩二丙二醇甲基醚、一缩二丙二醇乙基醚、一缩二丙二醇丁基醚等),二元醇醚酯(例如,乙二醇单甲基醚乙酸酯、乙二醇单乙基醚乙酸酯、乙二醇单丁基醚乙酸酯、乙二醇单苯基醚乙酸酯、乙二醇二己二酸酯、乙二醇二琥珀酸酯、二甘醇单乙基醚乙酸酯、二甘醇单丁基醚乙酸酯、丙二醇单甲基醚乙酸酯、丙二醇单乙基醚乙酸酯、丙二醇单丙基醚乙酸酯、丙二醇单苯基醚乙酸酯等),甘油单烷基醚(例如,鲛肝醇、鲨油醇、鲨肝醇等),糖醇(例如,麦芽三糖、甘露糖醇、蔗糖、赤藓醇、葡萄糖、果糖、淀粉分解糖、麦芽糖、淀粉分解糖还原醇等),多元缩醇(Glysolid,グリソリッド),四氢糠醇,POE-四氢糠醇,POP-丁基醚、POP・POE-丁基醚,三聚氧丙烯甘油醚,POP-甘油醚、POP-甘油醚磷酸,POP・POE-季戊四醇醚、聚甘油等。
作为单糖,例如可以列举:三碳糖(例如,D-甘油醛、二羟基丙酮等),四碳糖(例如,D-赤藓糖、D-赤藓酮糖、D-苏糖、赤藓糖醇等),五碳糖(例如,L-阿拉伯糖、D-木糖、L-来苏糖、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-塔罗糖、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),脱氧糖(例如,2-脱氧-D-核糖、6-脱氧-L-半乳糖、6-脱氧-L-甘露糖等),氨基糖(例如,D-葡糖胺、D-半乳糖胺、唾液酸、氨基糖醛酸、胞壁酸等),糖醛酸(例如,D-葡糖醛酸、D-甘露糖醛酸、L-古罗糖醛酸、D-半乳糖醛酸、L-艾杜糖醛酸等)等。
作为寡糖,例如可以列举:蔗糖、龙胆三糖、伞形糖、乳糖、车前糖、异剪秋罗糖、α,α-海藻糖、棉子糖、剪秋罗糖类、umbilicin、水苏糖、毛蕊花糖类等。
作为多糖,例如可以列举:纤维素、榅桲籽、淀粉、半乳聚糖、硫酸皮肤素、糖原、阿拉伯胶、硫酸乙酰肝素、黄蓍胶、硫酸角质素(keratan sulfate)、软骨素、黄原胶、瓜尔胶、葡聚糖、硫酸角质(keratosulfate)、刺槐豆胶、琥珀酰聚糖等。
作为其它的多元醇,例如可以列举:聚氧乙烯甲基葡糖苷(グルカムE-10)、聚氧丙烯甲基葡糖苷(グルカムP-10)等。
作为增稠剂,例如可以列举:阿拉伯胶、卡拉胶、梧桐胶、黄蓍胶、卡罗布胶、榅桲籽(榅桲)、酪蛋白、糊精、明胶、果胶酸钠、海藻酸钠、甲基纤维素、乙基纤维素、CMC、羟乙基纤维素、羟丙基纤维素、PVA、PVM、PVP、聚丙烯酸钠、羧基乙烯基聚合物、刺槐豆胶、瓜尔胶、罗望子胶、二烷基二甲基铵硫酸纤维素、黄原胶、硅酸铝镁、膨润土、锂蒙脱石、硅酸铝镁(Veegum)、合成锂皂石(Laponite)、硅酸酐等。
作为天然的水溶性高分子,例如可以列举:植物类高分子(例如,阿拉伯胶、黄蓍胶、半乳聚糖、瓜尔胶、卡罗布胶、梧桐胶、角叉菜胶、果胶、琼脂、榅桲籽(榅桲)、海藻胶体(褐藻萃取物)、淀粉(大米淀粉、玉米淀粉、马铃薯淀粉、小麦淀粉)、甘草酸);微生物类高分子(例如,黄原胶、葡聚糖、琥珀酰聚糖、支链淀粉等);动物类高分子(例如,胶原、酪蛋白、白蛋白、明胶等)等。
作为半合成的水溶性高分子,例如可以列举:淀粉类高分子(例如,羧甲基淀粉、甲基羟丙基淀粉等);纤维素类高分子(甲基纤维素、乙基纤维素、甲基羟丙基纤维素、羟乙基纤维素、纤维素硫酸钠、羟丙基纤维素、羧甲基纤维素、羧甲基纤维素钠、结晶纤维素、纤维素粉末等);海藻酸类高分子(例如,海藻酸钠、海藻酸丙二醇酯等)等。
作为合成的水溶性高分子,例如可以列举:乙烯基类高分子(例如,聚乙烯醇、聚乙烯基甲基醚、聚乙烯吡咯烷酮、羧基乙烯基聚合物等);聚氧乙烯类高分子(例如,聚乙二醇20,000、40,000、60,000等);丙烯酸类高分子(例如,聚丙烯酸钠、聚丙烯酸乙酯、聚丙烯酰胺等);聚乙烯亚胺;阳离子聚合物等。
作为保湿剂,例如可以列举:硫酸软骨素、透明质酸、硫酸粘液素、卡洛宁酸、缺端胶原、胆甾醇基-12-羟基硬脂酸酯、乳酸钠、胆汁酸盐、DL-吡咯烷酮羧酸盐、短链可溶性胶原、二甘油(EO)PO加成物、刺梨(イザヨイバラ)萃取物、西洋蓍草(セイヨウノコギリソウ)萃取物、黄木樨(メリロート)萃取物等。
作为金属离子封闭剂,例如可以列举:1-羟基乙烷-1,1-二膦酸、1-羟基乙烷-1,1-二膦酸四钠盐、依地酸二钠、依地酸三钠、依地酸四钠、枸橼酸钠、多聚磷酸钠、偏磷酸钠、葡萄糖酸、磷酸、枸橼酸、抗坏血酸、琥珀酸、依地酸、乙二胺羟乙基三乙酸三钠等。
作为氨基酸,例如可以列举:中性氨基酸(例如,苏氨酸、半胱氨酸等);碱性氨基酸(例如,羟赖氨酸等)等。另外,作为氨基酸衍生物,例如可以列举:酰基肌氨酸钠(月桂酰肌氨酸钠)、酰基谷氨酸盐、酰基β-丙氨酸钠、谷胱甘肽等。
作为pH调节剂,例如可以列举:乳酸-乳酸钠、枸橼酸-枸橼酸钠、琥珀酸-琥珀酸钠等缓冲剂等。
对本发明的水包油型乳化化妆品中混合的油相成分和水相成分的混合量没有特别限定。通过使用化妆品用原料作为乳化剂,可以得到油相成分/水相成分比少的、即从油相成分混合量少的实施方式(美容液、乳液等)到混合量多的实施方式(清洁霜、防晒剂、发乳等)广范围的油相成分/水相成分比的水包油型乳化化妆品。
在本发明所涉及的化妆品中,在不损及本发明效果的范围内,可以适当混合普通化妆品、准药品等中使用的其它成分,例如紫外线吸收剂、粉末、有机胺、高分子乳液、维生素类、抗氧化剂等。
作为水溶性紫外线吸收剂,例如可以列举:2,4-二羟基二苯甲酮、2,2’-二羟基-4-甲氧基二苯甲酮、2,2’-二羟基-4,4’-二甲氧基二苯甲酮、2,2’,4,4’-四羟基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2-羟基-4-甲氧基二苯甲酮、2-羟基-4-甲氧基-4’-甲基二苯甲酮、2-羟基-4-甲氧基二苯甲酮-5-磺酸盐、4-苯基二苯甲酮、2-乙基己基-4’-苯基-二苯甲酮-2-甲酸酯、2-羟基-4-正辛氧基二苯甲酮、4-羟基-3-羧基二苯甲酮等二苯甲酮类紫外线吸收剂;苯基苯并咪唑-5-磺酸及其盐、亚苯基-双-苯并咪唑-四磺酸及其盐等苯并咪唑类紫外线吸收剂;3-(4’-甲基亚苄基)-d,l-樟脑、3-亚苄基-d,l-樟脑;尿刊酸、尿刊酸乙酯等。
作为油溶性紫外线吸收剂,例如可以列举:对氨基苯甲酸(PABA)、PABA单甘油酯、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丁酯等苯甲酸类紫外线吸收剂;N-乙酰基氨茴酸高薄荷酯等氨茴酸类紫外线吸收剂;水杨酸戊酯、水杨酸薄荷酯、水杨酸高薄荷酯、水杨酸辛酯、水杨酸苯酯、水杨酸苄酯、对异丙醇苯基水杨酸酯等水杨酸类紫外线吸收剂;肉桂酸辛酯、乙基-4-异丙基肉桂酸酯、甲基-2,5-二异丙基肉桂酸酯、乙基-2,4-二异丙基肉桂酸酯、甲基-2,4-二异丙基肉桂酸酯、丙基-对甲氧基肉桂酸酯、异丙基-对甲氧基肉桂酸酯、异戊基-对甲氧基肉桂酸酯、辛基-对甲氧基肉桂酸酯、2-乙基己基-对甲氧基肉桂酸酯、2-乙氧基乙基-对甲氧基肉桂酸酯、环己基-对甲氧基肉桂酸酯、乙基-α-氰基-β-苯基肉桂酸酯、2-乙基己基-α-氰基-β-苯基肉桂酸酯、甘油基单-2-乙基己酰基-二对甲氧基肉桂酸酯、3,4,5-三甲氧基肉桂酸3-甲基-4-[甲基双(三甲基甲硅烷氧基)甲硅烷基]丁酯等肉桂酸类紫外线吸收剂;2-苯基-5-甲基苯并噁唑;2,2’-羟基-5-甲基苯基苯并三唑;2-(2’-羟基-5’-叔辛基苯基)苯并三唑;2-(2’-羟基-5’-甲基苯基苯并三唑、二亚苄基吖嗪(ジベンザラジン)、二茴香酰甲烷;4-甲氧基-4’-叔丁基二苯甲酰基甲烷、5-(3,3-二甲基-2-亚降冰片基)-3-戊烷-2-酮、奥克立林等。
作为粉末成分,例如可以列举:无机粉末(例如,滑石粉、高岭土、云母、绢云母(Sericite)、白云母、金云母、合成云母、红云母、黑云母、蛭石、碳酸镁、碳酸钙、硅酸铝、硅酸钡、硅酸钙、硅酸镁、硅酸锶、钨酸金属盐、镁、二氧化硅、沸石、硫酸钡、烧结硫酸钙(烧石膏)、磷酸钙、氟磷灰石、羟基磷灰石、陶瓷粉末、金属皂(例如,肉豆蔻酸锌、棕榈酸钙、硬脂酸铝)、氮化硼等);有机粉末(例如,聚酰胺树脂粉末(尼龙粉末)、聚乙烯粉末、聚甲基丙烯酸甲酯粉末、聚苯乙烯粉末、苯乙烯与丙烯酸的共聚物树脂粉末、苯并胍胺树脂粉末、聚四氟化乙烯粉末、纤维素粉末等);无机白色颜料(例如,二氧化钛、氧化锌等);无机红色类颜料(例如,氧化铁(氧化铁红)、钛酸铁等);无机褐色类颜料(例如,γ-氧化铁等);无机黄色类颜料(例如,黄氧化铁、黄土等);无机黑色类颜料(例如,氧化铁黑、低价氧化钛等);无机紫色类颜料(例如,芒果紫(マンゴバイオレット,mango violet)、钴紫等);无机绿色类颜料(例如,氧化铬、氢氧化铬、钛酸钴等);无机蓝色类颜料(例如,群青、绀青等);珠光颜料(例如,氧化钛包覆的云母、氧化钛包覆的氯氧化铋、氧化钛包覆的滑石粉、着色氧化钛包覆的云母、氯氧化铋、鱼鳞箔(魚鱗箔)等);金属粉末颜料(例如,铝粉末、铜粉末等);锆、钡或铝色淀等有机颜料(例如,红色201号、红色202号、红色204号、红色205号、红色220号、红色226号、红色228号、红色405号、橙色203号、橙色204号、黄色205号、黄色401号、和蓝色404号等的有机颜料、红色3号、红色104号、红色106号、红色227号、红色230号、红色401号、红色505号、橙色205号、黄色4号、黄色5号、黄色202号、黄色203号、绿色3号和蓝色1号等);天然色素(例如,叶绿素、β-胡萝卜素等)等。
需要说明的是,如上所述,已知某种无机粉体能够起到皮克林乳化剂的作用,因此乳化颗粒的表面需要被无机粉体完全覆盖。表面被无机粉体完全覆盖的乳化颗粒是在大量的无机粉体的存在下将配方和搅拌等条件全部最优化而逐渐得到的。因此,通常即使在化妆品中混合无机粉体,也几乎不会起到皮克林乳化剂的作用。
作为有机胺,例如可以列举:单乙醇胺、二乙醇胺、三乙醇胺、吗啉、四(2-羟基丙基)乙二胺、三异丙醇胺、2-氨基-2-甲基-1,3-丙二醇、2-氨基-2-甲基-1-丙醇等。
作为高分子乳液,例如可以列举:丙烯酸树脂乳液、聚丙烯酸乙酯乳液、丙烯酸树脂溶液、聚丙烯酸烷基酯乳液、聚乙酸乙烯树脂乳液、天然橡胶胶乳等。
作为维生素类,例如可以列举:维生素A、B1、B2、B6、C、E及其衍生物、泛酸及其衍生物、生物素等。
作为抗氧化剂,例如可以列举:生育酚类、二丁基羟基甲苯、丁基羟基茴香醚、没食子酸酯类等。
作为抗氧化助剂,例如可以列举:磷酸、枸橼酸、抗坏血酸、马来酸、丙二酸、琥珀酸、富马酸、脑磷脂、六偏磷酸盐、肌醇六磷酸、乙二胺四乙酸等。
作为其它可混合成分,例如可以列举:防腐剂(尼泊金甲酯、尼泊金乙酯、尼泊金丁酯、苯氧乙醇等);消炎剂(例如,甘草酸衍生物、甘草次酸衍生物、水杨酸衍生物、日柏醇、氧化锌、尿囊素等);美白剂(例如,胎盘萃取物、虎耳草萃取物、熊果苷等);各种萃取物(例如,黄柏、黄连、紫草根、芍药、当药、桦树、鼠尾草、枇杷、胡萝卜、芦荟、锦葵、鸢尾草、葡萄、薏苡仁、丝瓜、百合、藏红花、川芎、ショウキュウ、小连翘、刺芒柄花、大蒜、辣椒、陈皮、当归、海藻等);赋活剂(例如,蜂王浆、感光素、胆甾醇衍生物等);血液循环促进剂(例如,壬酸戊酰胺、烟酸苄酯、烟酸β-丁氧基乙酯、辣椒素、姜油酮、斑蝥酊、鱼石脂、单宁酸、α-茨醇、烟酸生育酚、六烟酸肌醇酯、环扁桃酯、桂利嗪、妥拉唑啉、乙酰胆碱、维拉帕米、千金藤碱、γ-谷维素等)、抗脂溢性剂(例如,硫、二甲硫蒽等)、抗炎剂(例如,氨甲环酸、硫代牛磺酸、亚牛磺酸等)等。
另外,在本发明的水包油型乳化化妆品中,不是作为乳化剂、而是为了控制使用感触、控制药物浸透性等、或者提高混合到皮肤或毛发的清洗剂中时的清洗性等目的,可以在不损及本发明效果的范围内(作为标准是2质量%、更优选1质量%、进一步优选0.5质量%以下)混合表面活性剂作为水相或油相成分。
两性表面活性剂至少具有各一个的阳离子性官能团和阴离子性官能团,当溶液为酸性时呈阳离子性,当溶液为碱性时呈阴离子性,在等电点附近具有接近于非离子表面活性剂的性质。
关于两性表面活性剂,根据阴离子基团的种类分为:羧酸型、硫酸酯型、磺酸型和磷酸酯型。本发明中优选为羧酸型、硫酸酯型、和磺酸型。羧酸型进一步分为氨基酸型和甜菜碱型。特别优选为甜菜碱型。
具体而言,例如可以列举:咪唑啉类两性表面活性剂(例如,2-十一烷基-N,N,N-(羟乙基羧甲基)-2-咪唑啉钠、2-椰油酰基-2-咪唑啉氢氧化物-1-羧基乙氧基二钠盐等);甜菜碱类表面活性剂(例如,2-十七烷基-N-羧甲基-N-羟乙基咪唑啉甜菜碱、月桂基二甲基氨基乙酸甜菜碱、烷基甜菜碱、酰氨基甜菜碱、磺基甜菜碱等)等。
作为阳离子性表面活性剂,例如可以列举:鲸蜡基三甲基氯化铵、硬脂基三甲基氯化铵、二十二烷基三甲基氯化铵、二十二烷基二甲基羟乙基氯化铵、硬脂基二甲基苄基氯化铵、鲸蜡基三乙基铵甲基硫酸盐等季铵盐。另外,可以列举:硬脂酸二乙基氨基乙基酰胺、硬脂酸二甲基氨基乙基酰胺、棕榈酸二乙基氨基乙基酰胺、棕榈酸二甲基氨基乙基酰胺、肉豆蔻酸二乙基氨基乙基酰胺、肉豆蔻酸二甲基氨基乙基酰胺、二十二烷酸二乙基氨基乙基酰胺、二十二烷酸二甲基氨基乙基酰胺、硬脂酸二乙基氨基丙基酰胺、硬脂酸二甲基氨基丙基酰胺、棕榈酸二乙基氨基丙基酰胺、棕榈酸二甲基氨基丙基酰胺、肉豆蔻酸二乙基氨基丙基酰胺、肉豆蔻酸二甲基氨基丙基酰胺、二十二烷酸二乙基氨基丙基酰胺、二十二烷酸二甲基氨基丙基酰胺等酰氨基胺化合物。
作为阴离子性表面活性剂,分为脂肪酸皂、N-酰基谷氨酸盐、烷基醚乙酸等羧酸盐型,α-烯烃磺酸盐、链烷磺酸盐、烷基苯磺酸等磺酸型,高级醇硫酸酯盐等硫酸酯盐型,磷酸酯盐型等。优选为羧酸盐型、磺酸型、和硫酸酯盐型,特别优选为硫酸酯盐型。
具体而言,例如可以列举:脂肪酸皂(例如,月桂酸钠、棕榈酸钠等)、高级烷基硫酸酯盐(例如,月桂基硫酸钠、月桂基硫酸钾等)、烷基醚硫酸酯盐(例如,POE-月桂基硫酸三乙醇胺、POE-月桂基硫酸钠等)、N-酰基肌氨酸(例如,月桂酰肌氨酸钠等)、高级脂肪酸酰胺磺酸盐(例如,N-肉豆蔻酰-N-甲基牛磺酸钠、椰子油脂肪酸甲基牛磺酸钠、月桂基甲基牛磺酸钠等)、磷酸酯盐(POE-油醚磷酸钠、POE-硬脂基醚磷酸酯等)、磺基琥珀酸盐(例如,二-2-乙基己基磺基琥珀酸钠、单月桂酰单乙醇酰胺聚氧乙烯磺基琥珀酸钠、月桂基聚丙二醇磺基琥珀酸钠等)、烷基苯磺酸盐(例如,直链十二烷基苯磺酸钠、直链十二烷基苯磺酸三乙醇胺、直链十二烷基苯磺酸等)、高级脂肪酸酯硫酸酯盐(例如,氢化椰子油脂肪酸甘油酯硫酸钠等)、N-酰基谷氨酸盐(例如,N-月桂酰谷氨酸一钠、N-硬脂酰谷氨酸二钠、N-肉豆蔻酰-L-谷氨酸一钠等)、硫酸化油(例如,土耳其红油等)、POE-烷基醚羧酸、POE-烷基烯丙基醚羧酸盐、α-烯烃磺酸盐、高级脂肪酸酯磺酸盐、仲醇硫酸酯盐、高级脂肪酸烷基醇酰胺硫酸酯盐、月桂酰单乙醇酰胺琥珀酸钠、N-棕榈酰天冬氨酸二(三乙醇)胺、酪蛋白钠等。
作为非离子性表面活性剂,是不会在水溶液中发生电离而带有电荷的表面活性剂。作为疏水基,已知有使用烷基的类型和使用二甲基硅氧烷的类型等。作为前者,具体而言,例如可以列举:甘油脂肪酸酯、甘油脂肪酸酯的氧化乙烯衍生物、聚甘油脂肪酸酯、丙二醇脂肪酸酯、丙二醇脂肪酸酯的氧化乙烯衍生物、聚乙二醇脂肪酸酯、聚乙二醇烷基醚、聚乙二醇烷基苯基醚、聚乙二醇蓖麻油衍生物、聚乙二醇氢化蓖麻油衍生物等。作为后者,可以列举:聚醚改性硅氧烷、聚甘油改性硅氧烷等。优选为使用烷基作为疏水基的类型。
具体而言,作为亲油性非离子表面活性剂,例如可以列举:脱水山梨糖醇脂肪酸酯类(例如,脱水山梨糖醇单油酸酯、脱水山梨糖醇单异硬脂酸酯、脱水山梨糖醇单月桂酸酯、脱水山梨糖醇单棕榈酸酯、脱水山梨糖醇单硬脂酸酯、脱水山梨糖醇倍半油酸酯、脱水山梨糖醇三油酸酯、脱水山梨糖醇五-2-乙基己酸二甘油酯、脱水山梨糖醇四-2-乙基己酸二甘油酯等)、甘油聚甘油脂肪酸类(例如,单棉籽油脂肪酸甘油酯、单芥酸甘油酯、倍半油酸甘油酯、单硬脂酸甘油酯、α,α’-油酸焦谷氨酸甘油酯、单硬脂酸甘油酯苹果酸等)、丙二醇脂肪酸酯类(例如,单硬脂酸丙二醇酯等)、氢化蓖麻油衍生物、甘油烷基醚等。
作为亲水性非离子表面活性剂,例如可以列举:POE-脱水山梨糖醇脂肪酸酯类(例如,POE-脱水山梨糖醇单油酸酯、POE-脱水山梨糖醇单硬脂酸酯、POE-脱水山梨糖醇单油酸酯、POE-脱水山梨糖醇四油酸酯等)、POE山梨糖醇脂肪酸酯类(例如,POE-山梨糖醇单月桂酸酯、POE-山梨糖醇单油酸酯、POE-山梨糖醇五油酸酯、POE-山梨糖醇单硬脂酸酯等)、POE-甘油脂肪酸酯类(例如,POE-甘油单硬脂酸酯、POE-甘油单异硬脂酸酯、POE-甘油三异硬脂酸酯等POE-单油酸酯等)、POE-脂肪酸酯类(例,POE-二硬脂酸酯、POE-单二油酸酯、二硬脂酸乙二醇酯等)、POE-烷基醚类(例如,POE-月桂醚、POE-油醚、POE-硬脂醚、POE-二十二烷基醚、POE-2-辛基十二烷基醚、POE-胆甾烷醇醚等)、泊洛沙姆型类(例如,Pluronic等)、POE·POP-烷基醚类(例如,POE·POP-鲸蜡醚、POE·POP-2-癸基十四烷基醚、POE·POP-单丁基醚、POE·POP-氢化羊毛脂、POE·POP-甘油醚等)、四 POE·四POP-乙二胺缩合物类(例如,Tetronic等)、POE-蓖麻油氢化蓖麻油衍生物(例如,POE-蓖麻油、POE-氢化蓖麻油、POE-氢化蓖麻油单异硬脂酸酯、POE-氢化蓖麻油三异硬脂酸酯、POE-氢化蓖麻油单焦谷氨酸单异硬脂酸二酯、POE-氢化蓖麻油马来酸酯等)、POE-蜂蜡·羊毛脂衍生物(例如,POE-山梨糖醇蜂蜡等)、烷醇酰胺(例如,椰子油脂肪酸二乙醇酰胺、月桂酸单乙醇酰胺、脂肪酸异丙醇酰胺等)、POE-丙二醇脂肪酸酯、POE-烷基胺、POE-脂肪酸酰胺、蔗糖脂肪酸酯、烷基乙氧基二甲基氧化胺、三油烯基磷酸酯等。
另外,本发明的化妆品用原料还可用作白浊化剂。
在化妆品(特别是化妆水)中,白浊这种外观特征作为使人想起对肌肤的保湿感、滋润感、浓稠感(こく感)等,而得到一部分消费者的强烈支持。白浊化妆品通常是将溶解有表面活性剂和油分的乙醇分散在水相中来制备,但表面活性剂与油分的平衡难以调整,不容易得到经时稳定性优异的白浊化妆品。
本发明所涉及的化妆品用原料只要在水中混合少许的0.01%(核-壳型微粒纯组分换算值)即可看到白浊,以0.01~0.1%的混合可以得到使用麦克贝斯(MacBeth)色差计测定的L值(亮度)为1~80的白浊度。
在本发明中,白浊化妆品是指其外观通过目视可识别为白浊的化妆品。作为L值,优选1~90。
以制备白浊化妆品为目的时,本发明的白浊化剂可以在普通的化妆品的制备工序中通过常规方法混合分散在水(或者溶解有水性成分的水相)中进行使用。相对于化妆品总量,该混合量以核-壳型微粒的纯组分计为0.01~10质量%,更优选0.05~2质量%,进一步优选为0.05~1质量%。混合量不足0.01质量%时,有时无法充分地白浊,混合量超过10质量%时,在高温条件下的长期保存中有时稳定性差、或者有时使用感差。
本发明所涉及的水包油型乳化化妆品和白浊化妆品适合用作皮肤化妆品和皮肤外用剂等。
实施例
其次,列举实施例说明本发明,本发明不限于这些实施例。在没有特别说明的情况下,混合量以质量%表示。另外,表中记载的EtOH、DPG、BG分别是乙醇、二丙二醇、1,3-丁二醇的简称。
[实施例1:核-壳型微粒分散液的制备例]
在表1和表2记载的聚合条件下,按照下述制备方法(方法1)将表1中记载的大分子单体和疏水性单体进行自由基聚合。通过目视评价所得的共聚物分散液的外观,按照方法2评价共聚物的粒径和分散度。结果见表3。
<方法1:核-壳型微粒的制备方法>
在具备回流管和氮导入管的三颈烧瓶中,向90g的水-醇混合溶剂中添加聚氧化乙烯大分子单体、疏水性单体。充分溶解或者分散后,进行20分钟的氮置换以去除溶解氧。将相对于总单体量为1mol%的聚合引发剂2,2’-偶氮二(2-甲基丙脒二盐酸盐) (2,2’-アゾビス(2-メチルプロピオンアミジン2塩酸塩))溶解于少量水中再添加至其中,进一步溶解或者分散。对均匀溶解或者分散的聚合溶液进行20分钟的氮置换以去除溶解氧,之后使用磁力搅拌器进行搅拌,同时在油浴中于65~70℃下保持8小时进行聚合反应。聚合结束后,将聚合液恢复到室温,由此得到核-壳型微粒分散液。
需要说明的是,作为聚氧化乙烯大分子单体,使用了BLEMMER PME-4000 (日油株式会社制造)。另外,作为疏水性单体,使用了甲基丙烯酸甲酯(MMA)、甲基丙烯酸丁酯(n-BMA)、叔丁基丙烯酰胺(t-BAA)、N,N-二甲基丙烯酰胺(DMAA)、N-[3-(二甲基氨基)丙基]丙烯酰胺(DMAPA)。
<方法2:粒径和分散度的测定方法>
共聚物的粒径的测定,使用Malvern公司制造的Zetasizer进行了测定。通过水稀释调制微粒分散液的微粒浓度为约0.1%的测定样品,用0.45μm的过滤器去除废物(ごみ)后,在散射角173°(后方散射光)下测定25℃下的散射强度,利用搭载于测定装置的分析软件算出平均粒径和分散度。粒径通过累积量分析法进行分析,分散度是将通过累积量分析得到的二次累积量的值进行标准化而得的数值。该分散度是通常使用的参数,使用市售的动态光散射测定装置能够自动地进行分析。粒径分析所必需的溶剂的粘度采用了25℃的纯水的粘度、即0.89mPa·s的值。
[表1]
[表2]
[表3]
如表3所示,在使甲氧基聚乙二醇单甲基丙烯酸酯(大分子单体)、和选自具有包含碳原子数为1~4的烷基的取代基的甲基丙烯酸甲酯、甲基丙烯酸丁酯、叔丁基丙烯酰胺、N,N-二甲基丙烯酰胺、N-[3-(二甲基氨基)丙基]丙烯酰胺的1种或者2种以上的疏水性单体,在水-乙醇混合溶剂(水:乙醇=40~60:18~82)中、在“大分子单体的加料摩尔量/疏水性单体的加料摩尔量”的值为1:50~100的条件下聚合的制备例1~10中,得到了白浊溶液状的分散液,能够评价粒径和分散度。即,可以确认到颗粒状聚合物(核-壳型微粒)的生成。另外,制备例1~10的核-壳型微粒的粒径为153.6~250.0nm、且分散度小至0.002~0.149,明确了粒径一致。
因此,明确了:通过使上述式(1)所表示的聚氧化乙烯大分子单体、和选自上述式(2)所表示的丙烯酸酯衍生物单体和下述式(3)所表示的丙烯酰胺衍生物单体的1种或者2种以上的疏水性单体,按照下述条件((A)~(D))进行自由基聚合,可得到粒径一致的核-壳型微粒:
(A) 以上述聚氧化乙烯大分子单体的加料摩尔量/(上述丙烯酸酯衍生物单体和/或丙烯酰胺衍生物单体)的加料摩尔量表示的摩尔比为1:10~1:250;
(B) 上述式(1)所示的大分子单体是具有重复单元为8~200的聚乙二醇基的丙烯酸衍生物或者甲基丙烯酸衍生物,
上述式(2)所示的丙烯酸酯衍生物单体是具有包含碳原子数为1~12的烷基的取代基的丙烯酸衍生物或者甲基丙烯酸衍生物,
上述式(3)所示的丙烯酰胺衍生物单体是具有包含碳原子数为1~18的烷基的取代基的丙烯酰胺衍生物或者甲基丙烯酰胺衍生物;
(C) 聚合溶剂为水-醇混合溶剂,醇为选自乙醇、二丙二醇、1,3-丁二醇、异戊二醇的1种或者2种以上;
(D) 水-醇混合溶剂的溶剂组成以20℃的质量比计为水:醇=90~10:10~90。
[实施例2:表面张力降低作用]
关于本发明所涉及的核-壳型微粒,分析了其给油/水表面张力带来的效果。
通过悬滴法(协和界面科学制造、自动接触角计DM-501)测定任意的分散液浓度下的十二烷/水表面张力,所述悬滴法是拿着注射器在十二烷中制作制备例5的核-壳型微粒水分散液的液滴,通过分析其液滴形状而得到表面张力值。另外,使用现有型的交联型核-壳型微粒((丙烯酸酯类/甲氧基PEG-90甲基丙烯酸酯)交联聚合物)作为对照。结果见图1。
在(丙烯酸酯类/甲氧基PEG-90甲基丙烯酸酯)交联聚合物中,添加浓度超过0.0001重量%时,十二烷/水表面张力急剧降低,但之后表面张力的降低平缓。
相对于此,在制备例5的核-壳型微粒中,添加浓度达到0.01重量%之前与上述交联聚合物几乎相同,但之后随着添加浓度的增加,表面张力显著降低。
因此,显示出:与现有型的交联型核-壳型微粒相比,本发明所涉及的核-壳型微粒使油/水表面张力降低的作用优异。
[实施例3:水包油型乳化化妆品]
其次,显示通过上述制备例的核-壳型微粒进行乳化而得的化妆品的实施例。按照方法3制备表4中记载的配方的化妆品,按照方法4进行评价。结果一并见表4。
<方法3:水包油型乳化化妆品的制备方法>
在纯净水中添加多元醇类、增稠剂等各种水相成分进行混合。向其中添加另外分散于纯净水中的本发明所涉及的化妆品用原料,进行搅拌混合。使化妆品用原料和水相成分均匀地分散后,加入油相成分,使用均化搅拌机进行剪切混合直至均匀,得到了水包油型乳化化妆品。
<方法4:化妆品的评价方法>
评价(1):透明性(白浊度)
利用分光光度计V-630(日本分光公司制造)在波长600nm下测定样品,通过可见光透过率(光路长度为1cm)进行了评价。参照为离子交换水。
评价(2-1):稳定性(外观)
在样品调制后的1天后,通过目视观察外观,按照下述标准进行评价。
A:样品均匀,且未观察到浮油(油浮き)或粉末的凝集;
B:样品大致均匀,但观察到少许的浮油或粉末的凝集;
C:样品不均匀,或者观察到显著的油相分离、或粉末的凝集。
评价(2-2):乳化稳定性(乳化颗粒)
利用光学显微镜观察了样品的乳化颗粒。
A:乳化颗粒均匀,且未观察到融合为一体或凝集;
B:乳化颗粒大致均匀,但观察到少许的融合为一体或凝集等;
C:乳化颗粒不均匀,观察到明显的融合为一体或凝集。
评价(3):皮肤刺激试验
在10名敏感肌肤评审员(パネル)的上臂内侧部施用24小时的封闭性斑贴,按照下述基准判定了皮肤的状态。
0…完全未观察到异常;
1…观察到稍微发红;
2…观察到发红;
3…观察到发红和丘疹。
“皮肤刺激试验”的评价基准如下。
A:10名评审员的平均值为0以上且不足0.15;
B:10名评审员的平均值为0.15以上且不足0.2;
C:10名评审员的平均值为0.2以上且不足0.3;
D:10名评审员的平均值为0.3以上。
评价(4):使用感
通过10名专业评审员(専門パネル),按照下述标准评价了将样品涂抹于皮肤时的使用感(“有无发粘感”、“浓稠感”、“溶合的速度”)。
A:7名以上回答为“好”、“可以实际感觉到效果(実感できる)”;
B:5名以上且不足7名回答为“好”、“可以实际感觉到效果”;
C:3名以上且不足5名回答为“好”、“可以实际感觉到效果”;
D:2名以下回答为“好”、“可以实际感觉到效果”。
评价(5):经时稳定性
通过肉眼观察了从制备起经过1个月后的水包油型乳化化妆品的状态。
A:样品保持制备时的乳化状态;
B:虽然见到轻微的沉淀/漂浮,但样品大致保持乳化状态;
C:乳化颗粒沉淀/漂浮,还观察到颗粒融合为一体;
D:样品中的乳化颗粒沉淀/漂浮、融合为一体,油相完全分离。
评价(6):水洗性
在树脂板上涂布2mg/cm2的样品,测定280~400nm的UV吸收光谱。使用双面胶将该板粘合在容器壁面,在该容器中装入20L左右的水,在500rpm下用水流冲洗30分钟,之后再次测定光谱。算出水洗后的光谱的积分值相对于水洗前的光谱的积分值的比例(百分比),作为“水洗残留率”。因此,水洗残留率=0%表示样品被完全冲洗掉。
[表4]
如表4所示,实施例1-1~1-10的水包油型乳化化妆品均乳化稳定性优异、发粘感少、娇嫩感优异,几乎感觉不到粉末感或粗糙感。
因此,显示出:通过以本发明所涉及的核-壳型微粒作为乳化剂,可得到乳化稳定性优异、发粘感少、娇嫩感优异、粉末感或粗糙感少的水包油型乳化化妆品。
[实施例4:白浊化妆品]
接着,显示因上述制备例的核-壳型微粒而发生了白浊化的化妆品的实施例。按照常规方法制造表5中记载的配方的化妆水,按照方法4进行评价。结果一并见表5。
[表5]
如表5所示,混合有制备例1~10的核-壳型微粒分散液的实施例2-1~2-10的化妆品均呈白浊~青白半透明的白浊外观。另外,乳化稳定性优异、发粘感少、有浓稠感、溶合快,而且几乎感觉不到粉末感或粗糙感。
因此,显示出本发明所涉及的核-壳型微粒可用作化妆品的白浊化剂。
[实施例5:水洗性]
其次,按照常规方法制备表6中记载的配方的化妆品,按照方法4评价水洗性。结果一并见表6。
[表6]
如表6所示,在混合有制备例10或者5的核-壳型微粒分散液的实施例3-1或者3-2的化妆品中,水洗后的残留率充分低至52或者49。相对于此,在混合有现有型的交联型核-壳型微粒((丙烯酸酯类/甲氧基PEG-90甲基丙烯酸酯)交联聚合物)的化妆品中,水洗残留率高达84%。
因此,明确了:使用现有型的交联型核-壳型微粒进行乳化而得的化妆品通过水洗几乎没有被除去,而利用本发明所涉及的核-壳型微粒进行乳化而得的化妆品只通过水洗就除去了大约一半。
Claims (5)
1.化妆品用原料,其特征在于:由核-壳型微粒构成,所述核-壳型微粒是在下述(A)~(D)的条件下将下述式(1)所表示的聚氧化乙烯大分子单体、和选自下述式(2)所表示的丙烯酸酯衍生物单体和下述式(3)所表示的丙烯酰胺衍生物单体的1种或者2种以上的疏水性单体进行自由基聚合而得到的;
(A) 以上述聚氧化乙烯大分子单体的加料摩尔量/(上述丙烯酸酯衍生物单体和/或丙烯酰胺衍生物单体)的加料摩尔量表示的摩尔比为1:10~1:250;
(B) 下述式(1)所示的大分子单体是具有重复单元为8~200的聚乙二醇基的丙烯酸衍生物或甲基丙烯酸衍生物;
下述式(2)所示的丙烯酸酯衍生物单体是具有包含碳原子数为1~12的烷基的取代基的丙烯酸衍生物或甲基丙烯酸衍生物;
下述式(3)所示的丙烯酰胺衍生物单体是具有包含碳原子数为1~18的烷基的取代基的丙烯酰胺衍生物或甲基丙烯酰胺衍生物;
(C) 聚合溶剂为水-醇混合溶剂,醇为选自乙醇、二丙二醇、1,3-丁二醇、异戊二醇的1种或2种以上;
(D) 水-醇混合溶剂的溶剂组成以20℃的质量比计为水:醇=90~10:10~90;
[化学式1]
R1表示H或者碳原子数为1~3的烷基,n为8~200的数,X表示H或者CH3;
[化学式2]
R2表示H或者碳原子数为1~3的烷基,R3表示包含碳原子数为1~12的烷基的取代基;
[化学式3]
R4表示H或者碳原子数为1~3的烷基,R5和R6表示H或者包含碳原子数为1~18的烷基的取代基。
2.权利要求1所述的化妆品用原料,其特征在于:上述核-壳型微粒的粒径为50~400nm。
3.乳化剂,其特征在于:由权利要求1或2所述的化妆品用原料构成。
4.水包油型乳化化妆品,其特征在于:通过权利要求3所述的乳化剂进行乳化而得。
5.白浊化剂,其特征在于:由权利要求1或2所述的化妆品用原料构成。
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EP3520772A4 (en) | 2020-04-29 |
BR112019005771A2 (pt) | 2019-06-11 |
US20210330573A1 (en) | 2021-10-28 |
JP2018052925A (ja) | 2018-04-05 |
TW201817799A (zh) | 2018-05-16 |
SG11201902759SA (en) | 2019-05-30 |
JP6403854B2 (ja) | 2018-10-10 |
CN109715133B (zh) | 2022-05-17 |
US11964043B2 (en) | 2024-04-23 |
EP3520772B1 (en) | 2023-12-20 |
AU2017338045A1 (en) | 2019-04-18 |
EP3520772A1 (en) | 2019-08-07 |
WO2018061755A1 (ja) | 2018-04-05 |
KR102439974B1 (ko) | 2022-09-02 |
BR112019005771B1 (pt) | 2022-08-16 |
TWI760367B (zh) | 2022-04-11 |
US20190290572A1 (en) | 2019-09-26 |
KR20190060773A (ko) | 2019-06-03 |
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