CN113661183A - 具有碳硅氧烷树枝状大分子结构的共聚物、以及含有该共聚物的组合物、化妆料原料、成膜剂及化妆料 - Google Patents
具有碳硅氧烷树枝状大分子结构的共聚物、以及含有该共聚物的组合物、化妆料原料、成膜剂及化妆料 Download PDFInfo
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- CN113661183A CN113661183A CN202080024488.5A CN202080024488A CN113661183A CN 113661183 A CN113661183 A CN 113661183A CN 202080024488 A CN202080024488 A CN 202080024488A CN 113661183 A CN113661183 A CN 113661183A
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- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
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- 239000002383 tung oil Substances 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
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- ORGHESHFQPYLAO-UHFFFAOYSA-N vinyl radical Chemical compound C=[CH] ORGHESHFQPYLAO-UHFFFAOYSA-N 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
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- 230000002087 whitening effect Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- 125000005023 xylyl group Chemical group 0.000 description 1
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- 229940098697 zinc laurate Drugs 0.000 description 1
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- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 1
- GPYYEEJOMCKTPR-UHFFFAOYSA-L zinc;dodecanoate Chemical compound [Zn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O GPYYEEJOMCKTPR-UHFFFAOYSA-L 0.000 description 1
- GJAPSKMAVXDBIU-UHFFFAOYSA-L zinc;hexadecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCC([O-])=O GJAPSKMAVXDBIU-UHFFFAOYSA-L 0.000 description 1
- KUPGJMJHAFGISS-UHFFFAOYSA-L zinc;hexadecyl phosphate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCOP([O-])([O-])=O KUPGJMJHAFGISS-UHFFFAOYSA-L 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- FYGDTMLNYKFZSV-BYLHFPJWSA-N β-1,4-galactotrioside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@H](CO)O[C@@H](O[C@@H]2[C@@H](O[C@@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-BYLHFPJWSA-N 0.000 description 1
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Abstract
提供一种具有碳硅氧烷树枝状大分子结构的共聚物、含有该共聚物的组合物、化妆料原料、成膜剂及化妆料、该共聚物等的制备方法,该共聚物的特征在于,显著降低具有碳硅氧烷树枝状大分子结构的单体含量。一种共聚物及其用途,该共聚物为具有含有能够自由基聚合的有机基团的碳硅氧烷树枝状大分子结构的不饱和单体(a1)和具有自由基聚合性乙烯基的与成分(a1)不同的不饱和单体(a2)的共聚物,相对于共聚物,未反应不饱和单体(a1)及衍生自该未反应不饱和单体(a1)的饱和单体的含量为2500ppm以下。
Description
技术领域
本发明涉及以显著降低具有碳硅氧烷树枝状大分子结构的单体含量为特征的具有碳硅氧烷树枝状大分子结构的共聚物、含有该共聚物的组合物、化妆料原料、成膜剂及化妆料,进一步地,涉及具有该碳硅氧烷树枝状大分子结构的共聚物及共聚物组合物的制备方法。
背景技术
众所周知,将具有优异的成膜性的具有碳硅氧烷树枝状大分子结构的共聚物用于化妆料以改善化妆料的持妆效果,并提高耐水性、耐皮脂性等(例如,专利文献1等)。这种具有碳硅氧烷树枝状大分子结构的共聚物是通过具有碳硅氧烷树枝状大分子结构的不饱和单体与其他不饱和单体的自由基共聚合反应形成的。
另一方面,近年来,除了上述的化妆料的耐久性的提高之外,还需要对皮肤和毛发具有低刺激性的化妆料,但自由基聚合性不饱和单体存在这种刺激性问题,因此,需要具有少量未反应单体的共聚物及共聚物组合物。然而,具有碳硅氧烷树枝状大分子结构的不饱和单体或衍生自其的饱和单体的分子量较大,是所谓的大分子单体,存在通常难以通过蒸馏来从共聚物或其组合物中除去的问题。
例如,在所述的专利文献1中,提出了用甲醇对所获得的共聚物进行再沉淀并对所获得的固体进行干燥的提纯方法,但需要大量甲醇,并且难以在化妆油剂中对所获得的固体进行重新分散或溶解,不适合液态组合物的实际生产。并且,用于提纯的甲醇本身具有刺激性和毒性,这种残留物令人担忧。除此之外,当如羧酸改性基团的极性官能团被引入具有碳硅氧烷树枝状大分子结构的共聚物时,变成极性分子,甲醇变成不良溶剂,因此需要改变为另一种溶剂,但是,例如在乙醇等中所获得的共聚物和具有碳硅氧烷树枝状大分子结构的不饱和单体均溶解,因此存在无法再沉淀等技术问题。
并且,着眼于降低残留在体系中的具有碳硅氧烷树枝状大分子结构的不饱和单体及其他不饱和单体的臭味,在专利文献2中,提出了通过加氢反应来将残留的饱和单体转换为对应的酯(饱和单体)以减少臭味。然而,存在的问题是,等量的衍生自具有碳硅氧烷树枝状大分子结构的不饱和单体的被氢化的未反应单体(饱和单体)残留在共聚物中,并且难以实现减少具有碳硅氧烷树枝状大分子结构的单体的目的。另外,存在的问题是,该氢化反应本身需要特殊装置,尤其无法简单地进行大规模生产。
现有技术文献
专利文献
专利文献1:日本专利特开2000-63225号公报
专利文献2:日本专利特开2014-40512号公报
发明内容
发明所要解决的问题
鉴于上述的问题和技术情况,本发明的目的在于,通过显著降低具有碳硅氧烷树枝状大分子结构的单体含量来提供低刺激性且具有优异的安全性能、高纯度的具有碳硅氧烷树枝状大分子结构的共聚物、含有该共聚物的组合物、化妆料原料、成膜剂及化妆料。另外,本发明的目的在于,提供可在工业生产规模上容易实施的该具有碳硅氧烷树枝状大分子结构的共聚物及共聚物组合物的制备方法。
用于解决问题的方案
经过本发明人锐意研究,发现在具有碳硅氧烷树枝状大分子结构的不饱和单体和其他不饱和单体的自由基共聚合反应中,对聚合引发剂设定加入时差以两步加入,任意地添加另外的其他不饱和单体,以使未反应的具有碳硅氧烷树枝状大分子结构的不饱和单体进行反应,且该工序之后,通过在常压或减压条件下,蒸馏残留在体系中的未反应不饱和单体或饱和单体,从而可显著降低具有碳硅氧烷树枝状大分子结构的单体含量,以完成了本发明。本发明的具有碳硅氧烷树枝状大分子结构的共聚物的特征在于,通常难以除去的具有碳硅氧烷树枝状大分子结构的单体(不饱和单体及饱和单体)的含量非常低。
即,本发明的第一方面为一种共聚物,该共聚物为具有含有能够自由基聚合的有机基团的碳硅氧烷树枝状大分子结构的不饱和单体(a1)和具有自由基聚合性乙烯基的与成分(a1)不同的不饱和单体(a2)的共聚物,相对于共聚物,未反应不饱和单体(a1)和衍生自该未反应不饱和单体(a1)的饱和单体的含量为2500ppm以下。其中,优选地,相对于构成共聚物的成分(a1)及成分(a2)的总质量,上述的成分(a1)的质量%为20质量%以上。
本发明的第二方面为含有上述的共聚物及一种以上的醇类(C)和/或油剂(D)的共聚物组合物。
本发明的第三方面为含有上述的共聚物或其组合物的化妆料原料、成膜剂及化妆料。
本发明的第四方面为上述的共聚物的制备方法,其包括向具有含有能够自由基聚合的有机基团的碳硅氧烷树枝状大分子结构的不饱和单体(a1)和
具有自由基聚合性乙烯基的与成分(a1)不同的不饱和单体(a2)中添加聚合引发剂以进行自由基聚合反应的工序,且包括工序(I):
在自由基聚合反应中的聚合引发剂的第一次添加后经过至少两小时之后,再添加与第一次添加的聚合引发剂相同或不同的聚合引发剂的工序(Ia)。
该制备方法在工序(I)中可任意地包括添加常压(1atm)下沸点低于160℃的具有自由基聚合性乙烯基的单体(a2′)以促进未反应的成分(a1)的自由基聚合反应的工序(Ib),另外,
还可包括工序(II):在工序(I)之后,在常压或减压下蒸馏出残留在体系中的未反应不饱和单体或饱和单体的工序。
该制备方法还可包括工序(III):对残留在体系中的未反应不饱和单体进行加氢反应以将不饱和单体转化为饱和单体的工序,为了获得所述的共聚物组合物,还可包括工序(IV):向体系中添加一种以上的醇类(C)和/或油剂(D)以除去自由基聚合反应中的反应溶剂的工序。
有益效果
根据本发明,可提供低刺激性且具有优异的安全性能、高纯度的具有碳硅氧烷树枝状大分子结构的共聚物、含有该共聚物的组合物、化妆料原料、成膜剂及化妆料。另外,通过本发明,可在工业生产规模上容易实施的具有该碳硅氧烷树枝状大分子结构的共聚物及共聚物组合物的制备方法。
具体实施方式
在本文中,“(甲基)丙烯酸”表示包含丙烯酸和甲基丙烯酸两种。类似地,“(甲基)丙烯酸酯”、“(甲基)丙烯酰氧基”、“(甲基)丙烯酰胺”也分别表示包含丙烯酸酯及甲基丙烯酸酯、丙烯酰氧基及甲基丙烯酰氧基、丙烯酰胺及甲基丙烯酰胺的两种。在本文中,“化妆料”及“化妆品”可互换使用。
本发明的具有碳硅氧烷树枝状大分子结构的共聚物是由具有碳硅氧烷树枝状大分子结构的不饱和单体的成分(a1)和不同于成分(a1)的不饱和单体的成分(a2)共聚而成。优选地,成分(a1)为由式(1)表示的具有碳硅氧烷树枝状大分子结构的不饱和单体。
式(1):
[化学式1]
{在式中,
Z为2价有机基团,
p为0或1,
R1及R2分别独立地为碳原子数1~10的烷基、芳基或芳烷基,
当i=1时,L1为由下式(2)表示的甲硅烷基烷基,
[化学式2]
(在式中,
Z及p与上文定义相同,
R1及R2与上文定义相同,
i为表示所述甲硅烷基烷基的总层数的1~10的整数,
Li+1为选自由氢原子、碳原子数1~10的烷基、芳基、芳烷基及所述甲硅烷基烷基组成的组中的基团,但当i=c(c为表示所述甲硅烷基烷基的层的1~10的整数)时,Li+1为氢原子、碳原子数1~10的烷基、芳基或芳烷基,当i<c时,Li+1为所述甲硅烷基烷基,ai为0~3的整数)。
此外,碳硅氧烷树枝状大分子结构为从一个硅原子放射状地高度支链化的化学结构,表示所述甲硅烷基烷基的总层数的i表示支链化的程度。例如,总层数i为1且Li+1为诸如甲基之类时,所述碳硅氧烷树枝状大分子结构意味着以下结构。
[化学式3]
(在式中,Z、p、R1及R2与上文定义相同,a1为0~3的整数)
类似地,当层i为2且Li+1为诸如甲基之类时,所述碳硅氧烷树枝状大分子结构意味着以下结构(但设定p=1)。
[化学式4]
(在式中,Z、R1及R2与上文定义相同,a1及a2为0~3的整数)
优选地,所述的a、a1及a2为0,作为所述碳硅氧烷树枝状大分子结构,以下结构为特别优选。
[化学式5]
(在式中,Z及R2与上文定义相同)
[化学式6]
(在式中,Z及R2与上文定义相同)
成分(a1)的所述含不饱和性的基团没有限制,只要具有能够自由基聚合的不饱和即可,并且其实例包括乙烯基、烯丙基、(甲基)丙烯酰基等。尤其,优选地,成分(a1)为上述的具有碳硅氧烷树枝状大分子结构的丙烯酸酯系单体或甲基丙烯酸酯系单体,其中,特别优选的不饱和单体为由以下结构表示的含不饱和性的基团通过上述的碳硅氧烷树枝状大分子结构中的-(Z)p-或-Z-与硅原子(Si)结合的不饱和单体,或者为直接与硅原子(Si)结合的不饱和单体。
[化学式7]
(在式中,R4为氢原子或甲基,R5为碳原子数1~10的亚烷基。)或者
[化学式8]
(在式中,R4及R5与上文定义相同。)表示的丙烯酰基或甲基丙烯酰基含有有机基团。
更具体而言,作为本成分,例举包含由以下平均组成式表示的具有碳硅氧烷树枝状大分子结构的不饱和单体。
[化学式9]
[化学式10]
[化学式11]
[化学式12]
[化学式13]
[化学式14]
[化学式15]
[化学式16]
[化学式17]
[化学式18]
[化学式19]
[化学式20]
[化学式21]
[化学式22]
针对具有碳硅氧烷树枝状大分子结构的不饱和单体的聚合,可以依照日本专利特开平11-1530号公报、日本专利特开2000-63225号公报、日本专利特开2001-192424号公报、日本专利特开2014-40512号公报等所述的制备方法来制备。
构成本发明的具有碳硅氧烷树枝状大分子结构的共聚物的成分(a2)为不同于成分(a1)的不饱和单体,且优选是具有自由基聚合性乙烯基的单体,对其种类没有特别限定。更具体而言,其为分子中不具有碳硅氧烷树枝状大分子结构的乙烯基系单体。
作为这种乙烯基系单体,通常有作为被称为乙烯基系树脂的有机树脂的起始原料的单体,具体而言,可举例示出:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸异丙酯等(甲基)丙烯酸低级烷基酯;(甲基)丙烯酸缩水甘油酯;(甲基)丙烯酸正丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸正己酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸辛酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸硬脂基酯等高级(甲基)丙烯酸酯;乙酸乙烯酯、丙酸乙烯酯等低级脂肪酸乙烯酯;丁酸乙烯酯、己酸乙烯酯、2-乙基己酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯等高级脂肪酸酯;苯乙烯、乙烯基甲苯、(甲基)丙烯酸苄基酯、(甲基)丙烯酸苯氧基乙基酯、乙烯基吡咯烷酮等芳香族乙烯基型单体;(甲基)丙烯酰胺、N-羟甲基(甲基)丙烯酰胺、N-甲氧基甲基(甲基)丙烯酰胺、异丁氧基甲氧基(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺等含酰胺基的乙烯基型单体;(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸2-羟丁酯、(甲基)丙烯酸2-羟丙酯等含羟基的乙烯基型单体:三氟丙基(甲基)丙烯酸酯、全氟丁基乙基(甲基)丙烯酸酯、全氟辛基乙基(甲基)丙烯酸酯等含氟乙烯基型单体;(甲基)丙烯酸缩水甘油酯、3,4环氧环己基甲基(甲基)丙烯酸酯等含环氧基的乙烯基型单体;(甲基)丙烯酸、衣康酸、巴豆酸、富马酸、马来酸等含羧酸的乙烯基型单体、四氢糠基(甲基)丙烯酸酯、丁氧基乙基(甲基)丙烯酸酯、乙氧基二乙二醇(甲基)丙烯酸酯、聚乙二醇(甲基)丙烯酸酯、聚丙二醇单(甲基)丙烯酸酯、羟丁基乙烯基醚、鲸蜡基乙烯基醚、2-乙基己基乙烯基醚等含醚键的乙烯基型单体;(甲基)丙烯酰氧基丙基三甲氧基硅烷、在单末端含有(甲基)丙烯酰基的(支链状或者直链状)聚二甲基硅氧烷、在单末端含有苯乙烯基的聚二甲基硅氧烷等含不饱和基团的有机硅化合物;丁二烯;氯乙烯;偏氯乙烯;(甲基)丙烯腈;富马酸二丁酯;马来酸酐;十二烷基琥珀酸酐;(甲基)丙烯酸缩水甘油醚:(甲基)丙烯酸、衣康酸、巴豆酸、富马酸、马来酸等自由基聚合性不饱和羧酸的碱金属盐、铵盐、有机胺盐;苯乙烯磺酸之类的具有磺酸基的自由基聚合性不饱和单体以及它们的碱金属盐、铵盐、有机胺盐;2-羟基-3-甲基丙烯酰氧基丙基三甲基氯化铵之类的由(甲基)丙烯酸衍生的季铵盐、甲基丙烯酸二乙基胺酯之类的具有叔胺基的醇的甲基丙烯酸酯以及它们的季铵盐。
而且,也可以使用多官能乙烯基系单体,可举例示出三羟甲基丙烷三(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、乙二醇二(甲基)丙烯酸酯、四乙二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、三羟甲基丙烷三氧乙基(甲基)丙烯酸酯、三(2-羟基乙基)异氰脲酸酯二(甲基)丙烯酸酯、三(2-羟基乙基)异氰脲酸酯三(甲基)丙烯酸酯、双酚A的环氧乙烷或环氧丙烷的加成物的二醇的二(甲基)丙烯酸酯、氢化双酚A的环氧乙烷或环氧丙烷的加成物的二醇的二(甲基)丙烯酸酯、三乙二醇二乙烯基醚等含(甲基)丙烯酰基的单体、两末端由苯乙烯基封端的聚二甲基硅氧烷、两末端由甲基丙烯酰氧基丙基封端的聚二甲基硅氧烷等含不饱和基团的有机硅化合物等。
并且,还可使用具有乙烯基系自由基聚合性不饱和基团和水解性基团的有机硅化合物。在这种情况下,膜强度变硬并且防水持续性提高,因此优选。其中,作为自由基聚合性基团,其实例包括含(甲基)丙烯酰氧基的有机基团、含(甲基)丙烯酰胺基的有机基团、含苯乙烯基的有机基团或碳原子数2~10的烯基、乙烯氧基或烯丙氧基等。
类似地,还可使用分子中具有至少一个酸性基团或其盐的不饱和单体。分子中具有至少一个酸性基团或其盐的不饱和单体为在分子中具有自由基聚合性的乙烯基和至少一个酸性基团或其盐的化合物。酸性基团的实例包括羧酸、磺酸及膦酸。这种盐的实例包括碱金属盐、碱土金属盐、碱性氨基酸盐、铵盐、烷基铵盐、烷基胺盐、烷醇胺盐,具体而言,钠盐、钾盐、镁盐、钙盐、L-精氨酸盐,L-组氨酸盐,L-赖氨酸盐、铵盐、三乙醇胺盐、氨基甲基丙二醇盐及它们的复合盐。具有这种酸性基团的化合物在水溶液中分别在特定的pH值下游离质子(H+)或与溶液中的阳离子成分结合形成盐,从而使化合物的亲水性-疏水性发生变化。类似地,具有酸性基团的盐的化合物也在特定的pH值下发生盐的解离,并表现出化合物的亲水性-疏水性变化。因此,通过在化妆料中适当配合具有这种酸性基团或其盐的化合物,而发挥即使持妆性能优异,也会在清洗时容易洗掉的效果。
类似地,为了提高本发明中的含有碳硅氧烷树枝状大分子结构的共聚物的防水性等,可使用具有全氟烷基等的含氟有机基团的不饱和单体。例如,具有全氟烷基等的含氟有机基团的丙烯酸单体或甲基丙烯酸单体等的乙烯基系单体。
本发明中的含有碳硅氧烷树枝状大分子结构的共聚物由上述的成分(a1)与成分(a2)共聚而成,优选地,其共聚时的质量比为(a1)∶(a2)=10∶90~90∶10,更优选地,其共聚时的质量比为20∶80~85∶15,进一步优选地,其共聚时的质量比为30∶70~60∶40的范围。尤其,优选地,相对于成分(a1)及成分(a2)的总质量,上述的成分(a1)的质量%为20质量%以上、30质量%以上,特别优选地,成分(a1)为总单体单位中的20质量%~60质量%。
本发明中的含有碳硅氧烷树枝状大分子结构的共聚物包括将聚合引发剂加入含有所述单体的原料组合物中以进行聚合反应的工序。接着,还可任意包括使获得的聚合反应物与镍催化剂或钯催化剂接触以进行加氢反应的工序。
作为聚合反应中使用的聚合方法,使用自由基聚合法或离子聚合法,但自由基聚合法为优选。在该自由基聚合法中,优选使用溶液聚合法。该溶液聚合是通过在自由基引发剂的存在下在溶剂中50~150℃的温度条件下使包含所述成分(a1)及成分(a2)的单体组合物反应3~20小时来进行的。作为聚合反应时使用的溶剂,其实例包括:如己烷、辛烷、癸烷、环己烷等脂肪族烃;如苯、甲苯、二甲苯等的芳香族烃;如二乙醚、二丁醚、四氢呋喃、二恶烷等的醚类;如丙酮、甲乙酮、甲基异丁基酮、二异丁基酮等的酮类;如醋酸甲酯、醋酸乙酯、醋酸丁酯、醋酸异丁酯等的酯类;如甲醇、乙醇、异丙醇、丁醇等的醇类;以及如八甲基环四硅氧烷、十甲基环戊硅氧烷、六甲基二硅氧烷、八甲基三硅氧烷等的有机硅氧烷低聚物。这种溶剂可以单独使用一种,或者可以混合两种以上使用。
作为自由基引发剂,使用自由基聚合法中通常使用的以往公知的化合物,具体而言,其实例包括:如2,2′-偶氮双(异丁腈)、2,2′-偶氮双(2-甲基丁腈)、2,2′-偶氮双(2,4-二甲基戊腈)等的偶氮二系化合物;以及如过氧化苯甲酰、过氧化月桂酰、过氧化苯甲酸叔丁酯、过氧化-2-乙基己酸叔丁酯、过氧化-2-乙基己酸叔己酯等的有机过氧化物。该自由基引发剂可以单独使用一种,或者可以混合两种以上使用。优选地,相对于上述的单体组合物的合计100重量份,自由基引发剂的使用量在0.1~5重量份的范围内。
并且,可在聚合时加入链转移剂。具体而言,作为该链转移剂,其实例包括:如2-巯基乙醇、丁基硫醇、正十二烷基硫醇、3-巯基丙基三甲氧基硅烷、具有巯丙基的聚二甲基硅氧烷等的巯基化合物;以及如二氯甲烷、氯仿、四氯化碳、丁基溴、3-氯丙基三甲氧基硅烷等的卤化物。
聚合反应物可以与作为加氢反应催化剂的镍催化剂或钯催化剂接触。通过与这种催化剂接触,聚合反应物中残留的未反应单体的乙烯基饱和,因此可降低添加到化妆料中时的刺激性或异味。作为镍催化剂,其实例包括镍/硅藻土或雷尼镍催化剂,但未必限定于此。作为钯催化剂,其实例包括如四(三苯基膦)钯(0)及二氯双(三苯基膦)钯(II)等的钯化合物、碳载钯、碳载氢氧化钯及氧化铂等,但未必限定于此。
聚合反应物与镍催化剂或钯催化剂接触时的温度为50~200℃,优选地,为70~130℃。压力为1~1000kg/cm2(绝对压力),优选地,为2~100kg/cm2。接触时间为1~15小时,优选地,为3~10小时。反应可在溶剂中进行,所述聚合时使用的溶剂可以直接使用,还可进行溶剂置换。可以使用的溶剂与所述聚合反应时描述的溶剂相同。
[具有碳硅氧烷树枝状大分子结构的单体含量及其意义]
本发明中的含有碳硅氧烷树枝状大分子结构的共聚物的特征在于,相对于共聚物,本发明的未反应不饱和单体(a1)和衍生自该未反应不饱和单体(a1)的饱和单体的含量为2500ppm以下。优选地,这种具有碳硅氧烷树枝状大分子结构的单体含量为2400ppm以下,通过使用下文中描述的制备方法,根据需要,还可制备含量降低为2000ppm以下,1500ppm以下的共聚物,作为化妆料原料,可获得具有产生刺激性的风险的含有碳硅氧烷树枝状大分子结构的单体含量极低的共聚物。
本发明的目的在于,提供减少了含有碳硅氧烷树枝状大分子结构的单体(不饱和单体及作为其加氢物的饱和单体)的含量的共聚物,该含有碳硅氧烷树枝状大分子结构的单体具有产生刺激性的风险且具有通过常规蒸馏方法难以从共聚物分离或除去的性质,当未反应不饱和单体(a1)及衍生自该未反应不饱和单体(a1)的饱和单体的含量减少至低于所述减少量时,作为化妆料原料或成膜剂,在一般组成中,本共聚物的使用量为化妆料总量的约4质量%,当配合到化妆料(包括外用制剂或准药品)中时,最终组成或制剂中的该单体含量为100ppm以下,其影响基本上可忽略不计。此外,该单体可通过下文中所述的方法来降低共聚物中的含量,且即使降低其含量,也不损害作为含有碳硅氧烷树枝状大分子结构的共聚物的化妆料原料或成膜剂的功能。
上述的共聚物中的未反应不饱和单体(a1)及衍生自该未反应不饱和单体(a1)的饱和单体含量可通过高效液相色谱法(HPLC)等方法确定,并可基于其峰值强度来计算。并且,即使是将该共聚物分散在有机溶剂(D)等中的共聚物组合物、化妆料原料或成膜剂,也可以容易计算单独或不包括其分散介质的共聚物部分的该单体含量。另外,最终化妆料中的未反应不饱和单体(a1)及衍生自该未反应不饱和单体(a1)的饱和单体含量也可通过相同的方法比较高精度地特定,含有本发明中的共聚物,且相对于这种化妆料总量,该单体含量为100ppm以下的化妆料包含在本发明的优选实施方式中。
例如,当将减少了上述的特定的未反应单体的共聚物配合至化妆料中时,其配合量没有特别限定,但作为不包含溶媒·溶剂等的本发明的共聚物单独的质量,可在化妆料总量的0.1~4质量%的范围内配合,优选地,可设定为1~4重量%。尤其,在该范围内配合的情况下,可提供如下的化妆料,即可为化妆料赋予成膜性等功能,并且具有产生刺激性的风险且具有通过常规蒸馏方法难以从共聚物分离出或除去的性质的含有碳硅氧烷树枝状大分子结构的单体为100ppm以下,另外,基本上不包含该单体。
类似地,在将减少了上述的特定的未反应单体的共聚物分散在下文中所述的有机溶剂(D)等中,且该共聚物的含量为40质量%的共聚物组合物、化妆料原料或成膜剂的情况下,可提供如下的共聚物组合物、化妆料原料或成膜剂,即,具有产生刺激性的风险且具有通过常规蒸馏方法难以从共聚物分离或除去的性质的含有碳硅氧烷树枝状大分子结构的单体的含量为1000ppm以下,另外,基本上不包含该单体。
本发明的共聚物能够以直接或溶解在溶剂中或分散在分散介质中等的组合物的方式配合在化妆料等中。这种溶剂、分散介质没有特别限定,但其实例包括醇类(C)或油剂(D),尤其,在作为化妆料原料或成膜剂的实际应用中,包含选自醇类(C)及油剂(D)的一种以上的分散介质的共聚物组合物的方式是特别优选的。
[共聚物组合物]
即,本发明的共聚物组合物为含有减少了上述的特定的未反应单体的共聚物和选自醇类(C)及油剂(D)的一种以上的组合物。当将作为本发明的第一发明的共聚物配合到化妆料中时,可使用溶解在溶剂中的溶液或分散在分散介质中的分散液或粉末状、颗粒状、块状等的固体形状。尤其,优选地,根据本发明的共聚物是通过溶解或分散在一种以上的醇类(C)和/或油剂(D)中以含有所述共聚物和这种分散介质的共聚物组合物的方式来配合到化妆料中。
本发明的共聚物与各种油剂之间的相溶性·分散性特别优异,可长期获得均匀的聚合物组合物。这种组合物可直接配合到化妆料中,从处理性、储存稳定性观点来看,作为化妆料原料或成膜剂极其有用。具体而言,相对于100质量份的本发明的共聚物,可优选使用包含5~1000质量份的至少一种油剂,优选地,使用包含50~500质量份的共聚物组合物,更优选地,使用包含100~400质量份的共聚物组合物。此外,当获得包含共聚物和油剂的共聚物组合物时,可使用机械力来使在聚合反应之后除去了溶剂和未反应单体的共聚物均匀分散在油剂中,也可通过上述的油剂来置换聚合反应时的挥发性溶剂,这是特别优选的。此外,如上所述,在作为分散介质含有醇类(C)和/或油剂(D)且共聚物含量为40质量%的共聚物组合物的情况下,可提供或设计含有碳硅氧烷树枝状大分子结构的单体的含量为1000ppm以下的组合物。
醇类(C)
本发明的共聚物可分散或溶解在醇类中使用,并且,本发明的共聚物与作为化妆料的通用成分的醇类具有规定的亲和性,因此,可作为化妆料的配合配方共存。作为醇类,可使用一种或两种以上的多元醇和/或低级一元醇。作为低级醇,其实例包括乙醇、异丙醇、正丙醇、叔丁醇、仲丁醇等,乙醇为优选。作为多元醇,可举例示出:如1,3-丙二醇、1,3-丁二醇、1,2-丁二醇、丙二醇、三亚甲基二醇、四亚甲基二醇、2,3-丁二醇、五亚甲基二醇、2-丁烯-1,4-二醇、二丁二醇、戊二醇、己二醇、辛二醇等的二元醇;如甘油、三羟甲基丙烷、1,2,6-己三醇等的三元醇;如季戊四醇、木糖醇等四元以上的多元醇;以及如山梨糖醇、甘露糖醇、麦芽糖醇、麦芽三糖、蔗糖、赤藓糖醇、葡萄糖、果糖、淀粉降解产物、麦芽糖、木糖醇、淀粉降解糖还原醇等的糖醇。进而,除了这些低分子多元醇之外,还可举例示出如二乙二醇、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、聚甘油等的多元醇聚合物等。其中,特别优选乙醇、1,3-丙二醇、1,3-丁二醇、山梨糖醇、二丙二醇、甘油、聚乙二醇。在这种醇类之中,异丙醇等还可以用作上述的反应溶剂,因此含有这种醇类的聚合反应组合物可以直接用作共聚物组合物。
油剂(D)
本发明的共聚物可分散或溶解在油剂中使用,作为所述的油剂,其实例包括化妆料中常用的动物油、植物油、合成油等。所述油剂可以为固体、半固体或液体,也可以为非挥发性、半挥发性或挥发性油剂。油剂用于向皮肤或头发赋予润滑性,软化皮肤并赋予湿润感。并且,油剂还可以用于稀释本发明的共聚物以获得共聚物组合物的目的,尤其,在5~100℃下为液态,优选地,选自有机硅系油剂(D1)及有机系油剂(D2)的至少一种,可根据化妆料的种类、用途适当选择这种油剂的种类、粘度等。这种油剂与上述的共聚物组合物同时配合在本发明的化妆料中。
有机硅系油剂(D1)
有机硅系油剂通常为疏水性,其分子结构可以为直链状、环状或支链状。有机硅油类在25℃下的粘度通常在0.65~100000mm2/s的范围内,优选地,在0.65~10000mm2/s的范围内。并且,该有机硅系油剂可具有挥发性,且优选具有挥发性。
作为所述有机硅油类,其具体实例包括环状有机聚硅氧烷、直链状有机聚硅氧烷及支链状有机聚硅氧烷。其中,具有挥发性的直链状有机聚硅氧烷、支链状有机聚硅氧烷及环状有机聚硅氧烷是优选的。
作为所述有机硅油类,例如,可使用由以下通式(3)、(4)或(5)表示的有机聚硅氧烷。
[化学式23]
(在式中,R9为选自氢原子、羟基或碳原子数1~30的一价未取代或经氟或氨基取代的烷基、芳基、烷氧基及由(CH3)3SiO{(CH3)2SiO}lSi(CH3)2CH2CH2-(1为0~1000的整数)表示的基团,a’为0~3的整数,b为0~1000的整数,c为0~1000的整数,但1≤b+c≤2000)
[化学式24]
(在式中,R9与上文定义相同,d为0~8的整数,e为0~8的整数,但3≤d+e≤8)
[化学式25]
(在式中,R9与上文定义相同,f为1~4的整数,g为0~500的整数)
作为碳原子数1~30的一价未取代或经氟或氨基取代烷基、芳基及烷氧基,其实例包括甲基、乙基、丙基、丁基、戊基、己基、庚基、辛基、癸基、十二烷基等的碳原子数1~30的直链状或支链状的烷基;环戊基、环己基等的碳原子数3~30的环烷基;苯基、甲苯基、二甲苯基、萘基等的碳原子数6~30的芳基;甲氧基、乙氧基、丙氧基等的碳原子数1~30的烷氧基;以及与这种基团的碳原子键合的氢原子至少部分由氟或氨基取代的基团。优选地,为未取代的烷基或芳基,更优选地,为未取代的碳原子数1~6的烷基或芳基,特别优选地,为甲基、乙基或苯基。
作为具有这种结构的有机硅油的具体实例,更具体而言,作为环状有机聚硅氧烷,可举例示出六甲基环三硅氧烷、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、1,1-二乙基六甲基环四硅氧烷、苯基七甲基环四硅氧烷、1,1-二苯基六甲基环四硅氧烷、1,3,5,7-四乙烯基四甲基环四硅氧烷、1,3,5,7-四甲基环四硅氧烷、1,3,5,7-四环己基四甲基环四硅氧烷、三(3,3,3-三氟丙基)三甲基环三硅氧烷、1,3,5,7-四(3-甲基丙烯酰氧基丙基)四甲基环四硅氧烷、1,3,5,7-四(3-丙烯酰氧基丙基)四甲基环四硅氧烷、1,3,5,7-四(3-羧丙基)四甲基环四硅氧烷、1,3,5,7-四(3-乙烯氧基丙基)四甲基环四硅氧烷、1,3,5,7-四(对乙烯基苯基)四甲基环四硅氧烷、1,3,5,7-四[3-(对乙烯基苯基)丙基]四甲基环四硅氧烷、1,3,5,7-四(N-丙烯酰基-N-甲基-3-氨基丙基)四甲基环四硅氧烷、1,3,5,7-四(N,N-双(月桂酰基)-3-氨基丙基)四甲基环四硅氧烷等。
作为直链状有机聚硅氧烷,其实例包括:分子链两端由三甲基硅烷氧基封端的二甲基聚硅氧烷(粘度为2mPa·s或6mPa·s等的低粘度~100万mpa·s等高粘度的二甲基有机硅)、有机氢聚硅氧烷、分子链两端由三甲基硅烷氧基封端的甲基苯基聚硅氧烷、分子链两端由三甲基硅烷氧基封端的二甲基硅氧烷/甲基苯基硅氧烷共聚物、分子链两端由三甲基硅烷氧基封端的二苯基聚硅氧烷、分子链两端由三甲基硅烷氧基封端的二甲基硅氧烷/二苯基硅氧烷共聚物、三甲基五苯基三硅氧烷、苯基(三甲基硅烷氧基)硅氧烷、分子链两端由三甲基硅烷氧基封端的甲基烷基聚硅氧烷、分子链两端由三甲基硅烷氧基封端的二甲基聚硅氧烷/甲基烷基硅氧烷共聚物、分子链两端由三甲基硅烷氧基封端的二甲基硅氧烷/甲基(3,3,3-三氟丙基)硅氧烷共聚物、α,ω-二羟基聚二甲基硅氧烷、α,ω-二乙氧基聚二甲基硅氧烷、1,1,1,3,5,5,5-七甲基-3-辛基三硅氧烷、1,1,1,3,5,5,5-七甲基-3-十二烷基三硅氧烷、1,1,1,3,5,5,5-七甲基-3-十六烷基三硅氧烷、三-三甲基硅烷氧基甲基硅烷、三-三甲基硅烷氧基烷基硅烷、四-三甲基硅烷氧基硅烷、四甲基-1,3-二羟基二硅氧烷、八甲基-1,7-二羟基四硅氧烷、六甲基-1,5-二乙氧基三硅氧烷、六甲基二硅氧烷、八甲基三硅氧烷、高级烷氧基改性有机硅、高级脂肪酸改性有机硅等。
作为支链状有机聚硅氧烷,其实例包括甲基三-三甲基硅烷氧基硅烷、乙基三-三甲基硅烷氧基硅烷、丙基三-三甲基硅烷氧基硅烷、四-三甲基甲硅烷氧基硅烷、苯基三-三甲基硅烷氧基硅烷等。
当本发明的化妆料或本组合物用作化妆料原料时,如果含有这种有机硅系油剂的至少一种,则可提高经时稳定性,并可实现有机硅油特有的清爽感。特别优选使用在上述的有机硅系油剂中的具有2~6mPa·s的低粘度范围内的粘度的十甲基环五硅氧烷和直链状有机聚硅氧烷、1,1,1,3,5,5,5-七甲基-3-辛基三硅氧烷(也称为“辛基聚甲基硅氧烷”)、三-三甲基硅烷氧基甲基硅烷(也称为“M3T”)。
有机系油剂(D2)
代表性的有机系油剂是烃油(D2-1)、脂肪酸酯油(D2-2)、高级醇、高级脂肪酸、油脂、氟系油剂,本发明对此没有特别限定,有机系油剂优选在5~100℃下为液态。并且,烃油和/或脂肪酸酯油为优选。它们可单独使用也可组合使用,还可与所述有机硅系油剂组合使用。通过组合适当的油剂,提高组合物和/或化妆料的经时稳定性的同时,可为每个化妆料赋予所需的触感。通过配合所述有机硅系油剂,可赋予有机硅油特有的清爽感,另外,通过使用高挥发性油剂,为皮肤赋予清爽感,并且,还通过将烃油和/或脂肪酸酯油与所述有机硅系油剂组合使用,可以给皮肤或毛发赋予滋润保湿感(也称为“湿润感”)和光滑感。
作为烃油(D2-1),其实例包括液态链烷烃、轻质液态异链烷烃、重质液态异链烷烃、凡士林、正链烷烃、异链烷烃、异十二烷、异十六烷、聚异丁烯、氢化聚异丁烯、聚丁烯、地蜡(ozokerite)、纯地蜡(ceresin)、微晶蜡、石蜡、聚乙烯蜡、聚乙烯/聚丙烯蜡、角鲨烷、角鲨烯、姥鲛烷、聚异戊二烯等。尤其,优选地,在本发明的组合物中使用异十二烷,这是因为它具有优异的挥发性,与其他化妆料原料之间的相溶性和亲和性(配合稳定性)优秀,并为皮肤赋予清爽感。
作为脂肪酸酯油(D2-2),其实例包括辛酸己基癸酯、辛酸十六烷基酯、肉豆蔻酸异丙酯、棕榈酸异丙酯、硬脂酸丁酯、月桂酸己酯、肉豆蔻酸肉豆蔻酯、油酸油酯、油酸癸酯、肉豆蔻酸辛基十二烷基酯、二甲基辛酸己基癸酯、乳酸鲸蜡酯、乳酸肉豆蔻酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、醋酸羊毛脂、乙二醇单硬脂酸酯、丙二醇单硬脂酸酯、丙二醇二油酸酯、单硬脂酸甘油酯、单油酸甘油酯、三2-乙基己酸甘油酯、三羟甲基丙烷三2-乙基己酸酯、双三羟甲基丙烷三乙基己酸酯、双三羟甲基丙烷(异硬脂酸/癸二酸)酯、三羟甲基丙烷三辛酸酯、三羟甲基丙烷三异硬脂酸酯、己二酸二异丙酯、己二酸二异丁酯、己二酸2-己基癸酯、己二酸二-2-庚基十一烷基酯、苹果酸二异硬脂酯、氢化蓖麻油单异硬脂酸酯、N-烷基二醇单异硬脂酸酯、异硬脂酸辛基十二烷基酯、异硬脂酸异丙酯、异硬脂酸异十六烷基酯、乙二醇二-2-乙基己酸酯、2-乙基己酸十六烷基酯、季戊四醇四-2-乙基己酸酯、辛基十二烷基胶酯、油酸乙酯、油酸辛基十二烷基酯、新戊二醇二癸酸酯、柠檬酸三乙酯、琥珀酸2-乙基己酯、琥珀酸二辛酯、硬脂酸异十六烷基酯、癸二酸二异丙酯、癸二酸二-2-乙基己酯、癸二酸二乙基、癸二酸二辛酯、癸二酸二丁辛酯、棕榈酸十六烷基酯、棕榈酸辛基十二烷基酯、棕榈酸辛酯、棕榈酸2-乙基己酯、棕榈酸2-己基癸酯、棕榈酸2-庚基十一烷基酯、胆固醇12-羟基硬脂酸酯、二季戊四醇脂肪酸酯、肉豆蔻酸2-己基癸酯、月桂酸乙酯、N-月桂酰-L-谷氨酸-2-辛基十二烷基酯、N-月桂酰-L-谷氨酸二(胆固醇/山嵛基/辛基十二烷基)酯、N-月桂酰-L-谷氨酸二(胆固醇/辛基十二烷基)酯、N-月桂酰-L-谷氨酸二(植物甾醇/山嵛基/辛基十二烷基)酯、N-月桂酰-L-谷氨酸二(植物甾醇/辛基十二烷基)酯、N-月桂酰肌氨酸异丙酯、苹果酸二异硬脂酯、新戊二醇二辛酸酯、新戊酸异癸酯、新戊酸异十三烷基酯、新戊酸异硬脂酯、异壬酸异壬酯、异壬酸异十三烷基酯、异壬酸辛酯、异壬酸异十三烷基酯、二新戊酸二乙基戊二醇酯、二新戊酸甲基戊二醇酯、新癸酸辛基十二烷基酯、二辛酸2-丁基-2-乙基-1,3-丙二醇酯、季戊四醇四辛酸酯、氢化松香季戊四醇酯、季戊四醇三乙基己酸酯、二季戊四醇(羟基硬脂酸/硬脂酸/松香酸)酯、四异硬脂酸聚甘油酯、九异硬脂酸聚甘油-10酯、癸(芥酸/异硬脂酸/蓖麻油酸)聚甘油-8酯、(己基癸酸/癸二酸)二甘油低聚酯、二硬脂酸二醇酯(二硬脂酸乙二醇酯)、二聚亚油酸二异丙酯、二聚亚油酸二异硬脂酯、二聚亚油酸二(异硬脂基/植物甾醇)酯、二聚亚油酸(植物甾醇/山嵛基)酯、二聚亚油酸(植物甾醇/异硬脂基/十六烷基/硬脂基/山嵛基)酯、二聚亚油醇二聚亚油酸酯、二聚亚油醇二异硬脂酸酯、氢化松香二聚亚油醇酯缩合物、硬化蓖麻油二聚亚油酸酯、羟烷基二聚二亚油基醚、三异辛酸甘油酯、三异硬脂酸甘油酯、三肉豆蔻酸甘油酯、三异棕榈酸甘油酯、三辛酸甘油酯、三油酸甘油酯、二异硬脂酸甘油酯、三(辛酸/癸酸)甘油酯、三(辛酸/癸酸/肉豆蔻酸/硬脂酸)甘油酯、氢化松香甘油三酯(氢化酯胶)、松香甘油三酯(酯胶)、山萮酸二十烷二酸甘油酯、二-2-庚基十一酸甘油酯、肉豆蔻酸异硬脂酸二甘油酯、胆固醇酢酸酯、胆固醇壬酸酯、胆固醇硬脂酸酯、胆固醇异硬脂酸酯、胆固醇油酸酯、胆固醇12-羟基硬脂酸酯、胆固醇澳洲坚果油脂肪酸酯、植物甾醇澳洲坚果油脂肪酸、植物甾醇异硬脂酸酯、胆固醇软羊毛脂脂肪酸酯、胆固醇硬羊毛脂脂肪酸酯、胆固醇长链支链脂肪酸酯、胆固醇长链α-羟基脂肪酸、蓖麻醇酸辛基十二烷基酯、羊毛脂脂肪酸辛基十二烷基、芥酸辛基十二烷基酯、硬化蓖麻油异硬脂酸酯、鳄梨油脂肪酸乙酯、羊毛脂脂肪酸异丙酯等。羊毛脂及羊毛脂衍生物也可用作脂肪酸酯油。
除了上述的以外,还可使用油脂类、高级醇、高级脂肪酸、氟系油等作为油剂,也可以组合两种以上使用。例如,可组合两种以上的以下示出的油剂。以下,更具体地举例示出可用于本发明的其他油剂。具体而言,举例示出选自油脂、高级醇、高级脂肪酸及氟系油剂的一种以上的使用。
作为油脂,作为天然动植物油脂类及半合成油脂,其实例包括鳄梨油、亚麻籽油、扁桃油、白蜡、紫苏油、橄榄油、可可脂、木棉蜡、榧子油、巴西棕榈蜡、肝油、小烛树蜡、牛脂、牛腿脂、牛骨脂、硬化牛脂、杏仁油、鲸蜡、硬化油、小麦胚芽油、芝麻油、米胚芽油、米糠油、甘蔗蜡、山茶花油、红花油、乳木果油、泡桐油、肉桂油、荷荷芭蜡、橄榄角鲨烷、虫胶蜡、龟油、大豆油、茶籽油、山茶油、月见草油、玉米油、猪脂、菜籽油、日本桐油、米糠蜡、胚芽油、马脂、桃仁油、棕榈油、棕榈仁油、蓖麻油、硬化蓖麻油、蓖麻油脂肪酸甲酯、葵花油、葡萄籽油、月桂果蜡、荷荷巴油、氢化荷荷巴酯、澳洲坚果油、蜂蜡、貂油、棉籽油、棉蜡、木蜡、木蜡核油、褐煤蜡、椰子油、硬化椰子油、三椰子油脂肪酸甘油酯、羊脂、落花生油、羊毛脂、液态羊毛脂、还原羊毛脂、羊毛脂醇、硬质羊毛脂、醋酸羊毛脂、羊毛脂脂肪酸异丙酯、POE羊毛脂醇醚、POE羊毛脂醇醋酸酯、聚乙二醇羊毛脂脂肪酸酯、POE氢化羊毛脂醇醚、蛋黄油等。但POE意味着聚氧乙烯。
作为高级醇,可举例示出碳原子数10~30的高级醇。所述高级醇为饱和或不饱和的一元脂肪醇,其烃基部分可以为直链状或支链状,但直链状更为优选。作为碳原子数10~30的高级醇,其实例包括月桂醇、肉豆蔻醇、棕榈醇、硬脂醇、山嵛醇、十六烷基醇、油醇、异硬脂醇、己基十二烷醇、辛基十二烷醇、鲸蜡硬脂醇、2-癸基十四烷醇、胆固醇、谷甾醇、植物甾醇、羊毛甾醇、羊毛脂醇、氢化羊毛脂醇、POE胆固醇醚、单硬脂甘油醚(鲨肝醇)、单油基甘油醚(鲨油醇)等。需要说明的是,在本发明中,优选单独使用熔点为40~80℃的高级醇,或以熔点成为40~70℃的方式组合多种高级醇。由于这些高级醇类具有与表面活性剂一同形成被称为α-凝胶的聚集体,并使制剂的粘度增加,以便使乳液稳定化,因此,在作为乳液形态的化妆料的基剂的方面上特别有用。
作为高级脂肪酸,其实例包括:月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、山萮酸、十一碳烯酸、油酸、亚油酸、亚麻酸、花生四烯酸、二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)、异硬脂酸、12-羟基硬脂酸等。
作为氟系油,其实例包括全氟聚醚、全氟萘烷、全氟辛烷等。
[化妆料及其任意成分]
本发明涉及含有上述的共聚物的化妆料。其中,在化妆料中配合减少了上述的特定的未反应单体的共聚物的情况下的配合量的优选范围如上所述在前文中描述,可设计或提供上述的特定的未反应单体含量为100ppm以下的化妆料。
除了上述的共聚物之外,本发明的化妆料可包含各种化妆料用原料。化妆料可包括以下两种情况,即以本发明的第三方面所述的共聚物组合物的形式配合到化妆料中的情况以及将共聚物和其他化妆料用原料分别配合到化妆料中的情况。这种任意成分没有特别限定,其优选实例包括含有选自由水(B)、醇(C)、油剂(D)、粉末或着色剂(E)、表面活性剂(F)、油溶性胶凝剂(G)、有机改性粘土矿物(H)、有机硅树脂(I)、有机硅橡胶(J)、有机硅弹性体(K)、有机改性的有机硅(L)、防紫外线成分(M)及水溶性聚合物(N)组成的组中的至少一种的化妆料。
本发明的化妆料中使用的水(B)为化妆料的介质,不含对人体有害的成分,只要干净即可,其实例包括自来水、蒸馏水或离子交换水等的纯净水、矿泉水、深海水等。并且,根据需要,还可以为生理盐水、磷酸缓冲水溶液等的形式。
醇类(C)的实例包括所述相同的化合物。
油剂(D)的实例包括所述相同的化合物。
粉末或着色剂(E)
含有本发明的共聚物或共聚物组合物的化妆料还可配合粉末或着色剂、尤其是用于化妆品中的任意粉末(包括用作着色剂的粉末/颜料)。如果粉末或着色剂用于普通的化妆料,则不管其形状(球状、棒状、针状、板状、片状、不定形状、纺锤状、碗状、覆盆子状等)或粒径(烟雾状、细颗粒、颜料级等)、粒子结构(多孔、无孔、二次聚集等),都可以使用,但这种粉末和/或着色剂作为颜料进行配合时,优选配合选自平均粒径在1nm~20μm的范围内的无机颜料粉末、有机颜料粉末、树脂粉末的一种或两种以上。
粉末或着色剂的具体实例包括无机粉末、有机粉末、表面活性剂金属盐粉末(金属皂)、有色颜料、珠光颜料、金属粉末颜料、有机硅弹性体粉末等,此外,还可使用它们的复合物。此外,这种粉末或着色剂包含用作防紫外线成分的成分。
具体而言,作为无机粉末,可举例示出出:氧化钛、氧化锆、氧化锌、氧化铈、氧化镁、硫酸钡、硫酸钙、硫酸镁、碳酸钙、碳酸镁、滑石、云母、高岭土、绢云母、白云母、合成云母、金云母、红云母、黑云母、锂云母(lepidolite)、硅酸、硅酸酐、硅酸铝、硅酸钠、硅酸钠镁、硅酸镁、硅酸铝镁、硅酸钙、硅酸钡、硅酸锶、钨酸金属盐、羟基磷灰石、蛭石(vermiculite)、Higilite、膨润土、蒙脱石、水辉石、沸石、陶瓷粉末、磷酸氢二钙、氧化铝、氢氧化铝、氮化硼、氮化硼等;作为有机粉末,可举例示出出:聚酰胺粉末、聚酯粉末、聚乙烯粉末、聚丙烯粉末、聚苯乙烯粉末、聚氨酯粉末、苯并胍胺粉末、聚甲基苯并胍胺粉末、聚四氟乙烯粉末、聚甲基丙烯酸甲酯粉末、纤维素、丝粉(silkpowder)、尼龙粉末、12尼龙、6尼龙、有机硅粉末、有机硅橡胶粉末、表面涂覆有聚甲基倍半硅氧烷的有机硅弹性体球状粉末、聚甲基倍半硅氧烷球状粉末、苯乙烯/丙烯酸共聚物、二乙烯基苯/苯乙烯共聚物、乙烯基树脂、尿素树脂、酚树脂、氟树脂、有机硅树脂、丙烯酸树脂、蜜胺树脂、环氧树脂、聚碳酸酯树脂、微结晶纤维粉末、淀粉粉末、月桂酰赖氨酸等;作为表面活性剂金属盐粉末,可举例示出出:硬脂酸锌、硬脂酸铝、硬脂酸钙、硬脂酸镁、肉豆蔻酸锌、肉豆蔻酸镁、棕榈酸锌、月桂酸锌、鲸蜡基磷酸锌、鲸蜡基磷酸钙、鲸蜡基磷酸锌钠等;作为有色颜料,可举例示出出:氧化铁红、氧化铁、氢氧化铁、钛酸铁的无机红色颜料、γ-氧化铁等无机褐色系颜料、黄氧化铁、黄赭石等无机黄色系颜料、黑氧化铁、碳黑等无机黑色颜料、锰紫、钴紫等无机紫色颜料、氢氧化铬、氧化铬、氧化钴、钛酸钴等无机绿色颜料、铁蓝、群青等无机蓝色系颜料、将红色3号、红色104号、红色106号、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227号、红色228号、红色230号、红色401号、红色505号、黄色4号、黄色5号、黄色202号、黄色203号、黄色204号、黄色401号、蓝色1号、蓝色2号、蓝色201号、蓝色404号、绿色3号、绿色201号、绿色204号、绿色205号、橙色201号、橙色203号、橙色204号、橙色206号、橙色207号等焦油系色素色淀化而成的颜料、将胭脂红酸、紫胶酸、红花素(carthamin)、巴西红木红(Brazilin)、藏红花素(crocin)等天然色素色淀化而成的颜料等;作为珠光颜料,可举例示出出:氧化钛覆盖云母、云母钛、氧化铁处理云母钛、氧化钛覆盖云母、氧氯化铋、氧化钛覆盖氧氯化铋、氧化钛覆盖滑石、鱼鳞箔、氧化钛覆盖着色云母等;作为金属粉末颜料,可举例示出出铝、金、银、铜、铂、不锈钢等金属粉末。
有机硅弹性体粉末为下文中所述的有机硅弹性体(K)之中的粉末状成分。它们是主要由二二有机硅烷氧基单元(D单元)构成的直链状二有机聚硅氧烷的交联产物,可通过在硅氢化反应催化剂下的交联反应来优选获得在侧链或末端具有与硅键合的氢原子的有机氢聚硅氧烷以及在侧链或末端具有烯基等的不饱和烃基的二有机聚硅氧烷。硅酮弹性体粉末比包含T单元和Q单元的有机硅树脂粉末柔软、有弹力,此外,吸油性优异,因此能吸收皮肤上的油脂,防止脱妆。
有机硅弹性体粉末可呈球形、扁平形、不定形状等各种形状。有机硅弹性体粉末可以为油分散体的形式。在本发明的化妆料中,可优选配合如下的有机硅弹性体粉末,即,该有机硅弹性体粉末呈颗粒形状,且利用通过电子显微镜观察的初级粒径和/或激光衍射/散射法测量的平均初级粒径在0.1~50μm的范围内,且初级粒子的形状呈球形。根据日本工业标准JIS K 6253“硫化橡胶和热塑性橡胶的硬度测试方法”的A型硬度计测量,形成有机硅弹性体粉末的有机硅弹性体的硬度优选在80以下,更优选在65以下。
此外,有机硅弹性体粉末也能够以水分散液的形式用于本发明的化妆料中。作为这种水分散液的市售产品,其实例包括由东丽道康宁(Toray Dow Corning)公司出品的BY29-129、PF-2001 PIF Emulsion等。
也可以对硅酮弹性体粉末任意实施利用有机硅树脂、二氧化硅等进行的表面处理等。作为所述表面处理,其实例包括日本专利特开平2-243612号公报、日本专利特开平8-12545号公报、日本专利特开平8-12546号公报、日本专利特开平8-12524号公报、日本专利特开平9-241511号公报、日本专利特开平10-36219号公报、日本专利特开平11-193331号公报、日本专利特开2000-281523号公报等中所描述的处理方法。此外,有机硅弹性体粉末对应于“化妆料类型配合成分标准”中列出的交联型有机硅粉末。作为有机硅弹性体粉末的市售产品,其实例包括东丽道康宁(Toray Dow Corning)公司出品的Trefil E-506S、TrefilE-508、9701 Cosmetic Powder、9702Powder等。
另外,特别优选地,这种粉末或着色剂中的一部分或全部经过防水处理。由此,可稳定地配合在油相中。并且,这种粉末或着色剂可彼此复合化,或使用普通油剂、除了本发明的有机聚硅氧烷共聚物以外的有机硅化合物、或氟化合物、表面活性剂等进行表面处理后来使用。
作为其他防水化处理,其实例包括利用各种防水化表面处理剂对所述的粉末或着色剂进行处理的情况,可举例示出甲基氢聚硅氧烷处理、有机硅树脂处理、有机硅橡胶处理、丙烯酸有机硅处理、氟化有机硅处理等的有机硅氧烷处理、硬脂酸锌处理等的金属皂处理、硅烷偶联剂处理、烷基硅烷处理等的硅烷处理、全氟烷基硅烷、全氟烷基磷酸酯盐、全氟聚醚处理等的氟化合物处理、N-月桂酰-L-赖氨酸处理等的氨基酸处理、角鲨烷处理等的油剂处理、丙烯酸烷基酯处理等的丙烯酸处理等,可组合使用它们中的一种以上。
优选地,上述的粉末或着色剂使用其他粉末分散剂或表面处理剂进行处理,尤其,可通过本申请的发明人在国际公开公报WO2009/022621号公报、日本专利特开2011-148784号公报、日本专利特开2011-149017号公报、日本专利特开2011-246704号公报、日本专利特开2011-246705号公报、日本专利特开2011-246706号公报、国际公开公报WO2009/022621号公报、国际公开公报WO2011/049246号公报、国际公开公报WO2011/049248号公报、日本专利申请2011-286973号等中提出的新型粉末处理剂及处理方法来进行分散或表面处理,或者使用这种新型粉末处理剂和所述油剂来进行处理,由此处理成浆状。这种新型处理剂在固有的触感的改善效果、分散稳定性等的性能上更加优异,因此,通过与本发明的新型化妆料原料组合使用,可有望进一步改善化妆料的功能、触感、储存稳定性等的效果。
另外,这种粉末或着色剂的一部分或全部可进行亲水化处理。由此,可配合与水相相关的粉末或着色剂。
另外,这种粉末或着色剂的一部分或全部可进行疏水化及亲水化处理。由此,可为粉末本身赋予乳化特性。作为市售产品,可举例示出日本帝国化工(TAYCA)公司生产的MZY-500SHE等。
本发明的共聚物组合物中或化妆料中的粉末或着色剂(E)可根据需要来使用一种或两种以上,其配合量没有特别限定,但可以在组合物中或化妆料总量的0.1~99.5质量%的范围内进行配合,优选地,为1~99重量%。尤其,作为粉末固形化妆料情况的配合量,化妆料总量的80~99质量%的范围内为优选。
含有本发明的共聚物组合物或共聚物的化妆料可含有表面活性剂(F)作为任意成分。根据其目的,表面活性剂(F)可与选自由有机硅系表面活性剂(F1)、阴离子性表面活性剂(F2)、阳离子性表面活性剂(F3)、非离子性表面活性剂(F4)、两性表面活性剂(F5)、半极性表面活性剂(F6)组成的组中的一种或两种以上的表面活性剂并用。
作为有机硅系表面活性剂(F1),其实例包括聚甘油基改性有机硅,二甘油基改性有机硅、甘油基改性有机硅,糖改性有机硅、氟聚醚改性有机硅、聚醚改性有机硅、羧酸改性有机硅,直链状有机硅·聚醚嵌段共聚物(聚硅氧烷-13等)、长链烷基/聚醚共改性有机硅、聚甘油基改性有机硅弹性体、二甘油基改性弹性体、甘油酯基改性弹性体、聚醚改性弹性体等。另外,可以优选使用根据需要对上述的有机硅类或弹性体类同时施加烷基支链、直链有机硅支链、硅氧烷树枝状聚合物支链等和亲水基而得到的表面活性剂。作为市售产品,其实例包括SH3771M、SH3772M、SH3773M、SH3775M、BY22-008M、BY11-030、ES-5373FORMULATIONAID、ES-5612FORMULATION AID、ES-5300FORMULATION AID、ES-5600SILICONE GLYCEROL EMULSIFIER(均为东丽道康宁(Toray Dow Corning)公司出品)。
作为阴离子性表面活性剂(F2),其实例包括饱和或不饱和脂肪酸盐(月桂酸钠、硬脂酸钠、油酸钠、亚麻酸钠等)、烷基硫酸盐、烷基苯磺酸(己基苯磺酸、辛基苯磺酸、十二烷基苯磺酸等)及其盐、聚氧化烯烷基醚硫酸盐、聚氧化烯烯基醚硫酸盐、聚氧乙烯烷基硫酸酯盐、磺基琥珀酸烷基酯盐、聚氧化烯磺基琥珀酸烷基酯盐、聚氧化烯烷基苯基醚硫酸盐、烷烃磺酸盐、辛基三甲基氢氧化铵、十二烷基三甲基氢氧化铵、烷基磺酸盐、聚氧乙烯烷基苯基醚硫酸盐、聚氧化烯烷基醚乙酸酯,烷基磷酸盐,聚氧化烯烷基醚磷酸盐,酰基谷氨酸盐、α-酰基磺酸盐、烷基磺酸盐、烷基烯丙基磺酸盐、α-烯烃磺酸盐、烷基萘磺酸盐、烷烃磺酸盐、烷基或烯基硫酸盐、烷基酰胺硫酸盐、烷基或烯基磷酸盐、烷基酰胺磷酸盐、烷酰基烷基牛磺酸盐、N-酰基氨基酸盐、磺基琥珀酸盐、烷基醚羧酸盐、酰胺醚羧酸盐、α-磺基脂肪酸酯盐、丙氨酸衍生物、甘氨酸衍生物、精氨酸衍生物。作为盐,其实例包括钠盐等的碱金属盐、镁盐等的碱土金属盐、三乙醇胺盐等的烷醇胺盐,还可例举铵盐。
作为阳离子性表面活性剂(F3),其实例包括烷基三甲基氯化铵、硬脂基三甲基氯化铵、月桂基三甲基氯化铵、十六烷基三甲基氯化铵、牛脂烷基三甲基氯化铵、山嵛基三甲基氯化铵、硬脂基三甲基溴化铵、山嵛基三甲基溴化铵、二硬脂基二甲基氯化铵、二椰油基二甲基氯化铵、二辛基二甲基氯化铵、二(POE)油基甲基氯化铵(2EO)、苯扎氯铵、烷基苯扎氯铵、烷基二甲基苯扎氯铵、苄索氯铵、硬脂基二甲基苄基氯化铵、羊毛脂衍生季铵盐、二乙氨基乙基酰胺硬脂酸酯、二甲氨基丙基酰胺硬脂酸酯、山萮酸酰胺丙基二甲基羟基丙基氯化铵、硬脂酰基胆氨基甲酰基甲基氯化吡啶鎓、十六烷基氯化吡啶鎓、妥尔油烷基苄基羟乙基氯化咪唑啉鎓、苄基铵盐。
作为非离子性表面活性剂(F4),其实例包括聚甘油二异硬脂酸酯或二甘油聚羟基硬脂酸酯、异硬脂基甘油醚、聚氧化烯醚类、聚氧化烯烷基醚类、聚氧化烯脂肪酸酯类、聚氧化烯脂肪酸二酯类、聚氧化烯树脂酸酯类、聚氧化烯(硬化)蓖麻油类、聚氧化烯烷基苯酚类、聚氧化烯烷基苯基醚类、聚氧化烯苯基苯基醚类、聚氧化烯烷基酯类,聚氧化烯烷基酯类、山梨糖醇脂肪酸酯、聚氧化烯山梨糖醇烷基酯类、聚氧化烯山梨醇酐脂肪酸酯类、聚氧化烯山梨糖醇脂肪酸酯类、聚氧化烯甘油脂肪酸酯类、聚甘油烷基醚类、聚甘油脂肪酸酯类、蔗糖脂肪酸酯类、脂肪酸链烷醇酰胺、烷基糖苷类、聚氧化烯脂肪酸双苯基醚类、聚丙二醇、二乙二醇、聚氧乙烯/聚氧丙烯嵌段聚合物、烷基聚氧乙烯/聚氧丙烯嵌段聚合物醚、聚氧乙烯/聚氧丙烯嵌段聚合物、烷基聚氧乙烯/聚氧丙烯嵌段聚合物醚、氟系表面活性剂等。
作为两性表面活性剂(F5),其实例包括咪唑啉型、酰胺甜菜碱型、烷基甜菜碱型、烷基酰胺甜菜碱型、烷基磺基甜菜碱型、酰胺磺基甜菜碱型、羟基磺基甜菜碱型、羰基甜菜碱型、磷酸甜菜碱型、氨基羧酸型、酰胺氨基酸型两性表面活性剂。具体而言,其实例包括: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-咪唑啉鎓氢氧化物-1-羧乙氧基二钠盐等的咪唑啉型两性表面活性剂;月桂基二甲氨基乙酸甜菜碱、肉豆蔻基甜菜碱等的烷基甜菜碱型两性表面活性剂;如椰子油脂肪酸酰胺丙基二甲氨基乙酸甜菜碱、棕榈仁油脂肪酸酰胺丙基二甲氨基乙酸甜菜碱、牛脂脂肪酸酰胺丙基二甲氨基乙酸甜菜碱、硬化牛脂脂肪酸酰胺丙基二甲氨基乙酸甜菜碱、月桂酰胺丙基二甲基氨基乙酸甜菜碱、肉豆蔻酰胺丙基二甲氨基乙酸甜菜碱、棕榈酸酰胺丙基二甲氨基乙酸甜菜碱、硬脂酰胺丙基二甲氨基乙酸甜菜碱、油酸酰胺丙基二甲氨基乙酸甜菜碱等的酰胺甜菜碱型两性表面活性剂;椰子油脂肪酸二甲基磺基丙基甜菜碱等的烷基磺基甜菜碱型两性表面活性剂;月桂基二甲氨基羟基磺基甜菜碱等的烷基羟基磺基甜菜碱型两性表面活性剂;月桂基羟基磷酸甜菜碱等的磷酸甜菜碱型两性表面活性剂;N-月桂酰-N'-羟乙基-N'-羧甲基乙二胺钠、N-油酰基-N'-羟乙基-N'-羧甲基乙二胺钠、N-椰油酰基-N'-羟乙基-N'-羧甲基乙二胺钠、N-月桂酰-N'-羟乙基-N’-羧甲基乙二胺钾、N-油酰基-N'-羟乙基-N'-羧甲基乙二胺钾、N-月桂酰-N-羟乙基-N'-羧甲基乙二胺钠、N-油酰基-N-羟乙基-N'-羧甲基乙二胺钠、N-椰油酰基-N-羟乙基-N’-羧甲基乙二胺钠、N-月桂酰-N-羟乙基-N’、N’-二羧甲基乙二胺单钠、N-油酰基-N-羟乙基-N’、N’-二羧甲基乙二胺单钠、N-椰油酰基-N-羟乙基-N’、N’-二羧甲基乙二胺单钠、N-月桂酰-N-羟乙基-N’、N’-二羧甲基乙二胺二钠、N-油酰基-N-羟乙基-N',N’-二羧甲基乙二胺二钠、N-椰油酰基-N-羟乙基-N’,N’-二羧甲基乙二胺二钠等的酰胺氨基酸型两性表面活性剂。
作为半极性表面活性剂(F6),可例举烷基氧化胺型表面活性剂、烷基氧化胺、烷基酰胺氧化胺、烷基羟基氧化胺等,优选地,使用碳原子数10~18的烷基二甲氧化胺、碳原子数8~18的烷氧基乙基二羟基乙基氧化胺等。具体实例包括十二烷基二甲氧化胺、二甲基辛氧化胺、二乙基癸氧化胺、双-(2-羟乙基)十二烷基氧化胺、二丙基十四烷基氧化胺、甲基乙基十六烷基氧化胺、十二烷基酰胺丙基二甲基氧化胺、十六烷基二甲氧化胺、硬脂基二甲氧化胺、牛脂二甲氧化胺、二甲基-2-羟基十八烷基氧化胺、月桂基二甲基氧化胺、肉豆蔻基二甲基氧化胺、硬脂基二甲基氧化胺、异硬脂基二甲基氧化胺、棕榈脂肪酸烷基二甲基氧化胺、辛酸酰胺丙基二甲氧化胺、癸酸酰胺丙基二甲氧化胺、月桂酸酰胺丙基二甲氧化胺、肉豆蔻酸酰胺丙基二甲氧化胺、棕榈酸酰胺丙基二甲基氧化胺、硬脂酸酰胺丙基二甲基氧化胺、异硬脂酸酰胺丙基二甲基氧化胺、油酸酰胺丙基二甲基氧化胺、蓖麻油酸酰胺丙基二甲基氧化胺、12-羟基硬脂酸酰胺丙基二甲基氧化胺、棕榈脂肪酸酰胺丙基二甲基氧化胺、棕榈仁油脂肪酸酰胺丙基二甲基氧化胺、蓖麻油脂肪酸酰胺丙基二甲基氧化胺、月桂酸酰胺乙基二甲基氧化胺、肉豆蔻酸酰胺乙基二甲基氧化胺、棕榈脂肪酸酰胺乙基二甲基氧化胺、月桂酸酰胺乙基二乙基氧化胺、肉豆蔻酸酰胺乙基二乙基氧化胺、棕榈脂肪酸酰胺乙基二乙基氧化胺、月桂酸酰胺乙基二羟基乙基氧化胺、肉豆蔻酸酰胺乙基二羟基乙基氧化胺、及棕榈脂肪酸酰胺乙基二羟基乙基氧化胺。
本发明的乳化组合物中的表面活性剂(F)的配合量没有特别限定,但为了使乳化物或分散体稳定化,例如乳化组合物中或分散体组合物中在0.05~90重量%的范围内可配合,每组合物重量优选为0.1~50重量%,更优选为0.5~25重量%。
油溶性凝胶剂(G)
作为凝胶剂,油溶性的凝胶剂为优选,具有凝胶化或增稠效果。其具体实例包括硬脂酸铝、硬脂酸镁、肉豆蔻酸锌等的金属皂、N-月桂酰-L-谷氨酸、α,γ-二-正丁胺等的氨基酸衍生物、糊精棕榈酸酯、糊精硬脂酸酯、糊精2-乙基己烷酸棕榈酸酯等的糊精脂肪酸酯、蔗糖棕榈酸酯、蔗糖硬脂酸酯等的蔗糖脂肪酸酯、单亚苄基山梨糖醇、二亚苄基山梨糖醇等的山梨糖醇的亚苄基衍生物等。这些可以根据需要使用一种或两种以上。
有机改性粘土矿物(H)
作为有机改性粘土矿物,其实例包括二甲基苄基十二烷基铵蒙脱石粘土、二甲基双十八烷基铵蒙脱石土、二甲基烷基铵锂蒙脱石、苄基二甲基硬脂基铵锂蒙脱石、二硬脂基二甲基氯化铵处理的硅酸铝镁等。作为这种市售产品,有BENTONE27(苄基二甲基硬脂基氯化铵处理的锂蒙脱石,美国国家铅业(National Lead)公司出品)、BENTONE38(二硬脂基二甲基氯化铵处理的锂蒙脱石,美国国家铅业(National Lead)公司出品)等。
有机硅树脂(I)
有机硅树脂是具有高度支链状结构、网状结构或笼状结构的有机聚硅氧烷,在常温下为液态或固态,除非与本发明的目的相悖,只要是通常用于化妆料的有机硅树脂即可。作为固态有机硅树脂,可例举包括三有机硅烷氧基单元(M单元)(有机基团仅为甲基、甲基和乙烯基或苯基)、二有机硅烷氧基单元(D单元)(有机基团仅为甲基、甲基和乙烯基或苯基)、单有机硅烷氧基单元(T单元)(有机基团为甲基、乙烯基、或苯基)及硅烷氧基单元(Q单元)的任意组合的MQ树脂、MDQ树脂、MTQ树脂、MDTQ树脂、TD树脂、TQ树脂、TDQ树脂。并且,可例举三甲基硅烷氧基硅酸、聚烷基硅烷氧基硅酸、含有二甲基硅烷氧基单元的三甲基硅烷氧基硅酸、烷基(全氟烷基)硅烷氧基硅酸。这些有机硅树脂为油溶性,特别优选能溶解于D4、D5。
有机硅树脂在涂敷于皮肤、毛发等上时形成均匀的薄膜,以赋予对干燥及低温的保护效果。进而,具有这种支链单元的有机硅树脂紧贴在皮肤、毛发上以对皮肤、毛发赋予光泽和透明感。
有机硅橡胶(J)
在本发明中,还可将被称为有机硅橡胶的1000000mm2/s以上的超高粘度的有机聚硅氧烷用作有机硅油。有机硅橡胶为超高聚合度的直链状二有机聚硅氧烷,也被称为有机硅生胶或有机聚硅氧烷橡胶。有机硅橡胶与所述的油状有机硅的区别在于,因其聚合度高,因此具有可测量的可塑性。作为这种有机硅生胶,可举例示出二甲基聚硅氧烷、甲基苯基聚硅氧烷、氨基聚硅氧烷、甲基氟烷基聚硅氧烷等具有二烷基硅烷氧基单元(D单元)的取代或未取代的有机聚硅氧烷或具有它们的微交联结构的有机聚硅氧烷,作为典型例,由通式:R10(CH3)2SiO{(CH3)2SiO}s{(CH3)R11SiO}tSi(CH3)2R10(在式中,R11为选自乙烯基、苯基、碳原子数6~20的烷基、碳原子数3~15的氨基烷基、碳原子数3~15的全氟烷基、碳原子数3~15的含季铵盐基的烷基的基团,末端基团R10为选自碳原子数1~8的烷基、苯基、乙烯基、碳原子数3~15的氨基烷基、羟基及碳原子数1~8的烷氧基的基团。并且,s=2000~6000,t=0~1000,s+t=2000~6000)表示。其中,聚合度为3000~20000的二甲基聚硅氧烷生橡胶为优选。并且,这种有机硅橡胶可直接或分散在油状有机硅中的液态橡胶分散液(有机硅橡胶的油分散液)配合在本发明的化妆料中。
作为这种有机硅生胶,其实例包括二甲基聚硅氧烷、甲基苯基聚硅氧烷、氨基聚硅氧烷、甲基氟烷基聚硅氧烷等的具有二烷基硅烷氧基单元(D单元)的取代或未取代有机聚硅氧烷、或具有它们的微交联结构的有机聚硅氧烷等,作为典型例,由通式:R10(CH3)2SiO{(CH3)2SiO}s{(CH3)R12SiO}tSi(CH3)2R10(在式中,R12为选自乙烯基、苯基、碳原子数6~20的烷基、碳原子数3~15的氨基烷基、碳原子数3~15的全氟烷基、碳原子数3~15的含季铵盐基的烷基的基团,末端基R10为选自碳原子数1~8的烷基、苯基、乙烯基、碳原子数3~15的氨基烷基、羟基及碳原子数1~8的烷氧基的基团。并且,s=2000~6000、t=0~1000、s+t=2000~6000)表示。其中,聚合度为3000~20000的二甲基聚硅氧烷生橡胶为优选。并且,分子的侧链或末端中具有3-氨基丙基、N-(2-氨基乙基)3-氨基丙基等的氨基改性甲基聚硅氧烷生橡胶为优选。并且,在本发明中,有机硅橡胶可根据需要使用一种或两种以上组合使用。
有机硅橡胶具有超高聚合度,因此,对皮肤及毛发具有优异的持久性,并形成透气性优异的保护膜。因此,有机硅橡胶尤其是一种为皮肤和毛发赋予润泽和光泽,在使用过程中和使用后为整个皮肤及毛发赋予张力和紧致的质感的成分。
例如,有机硅橡胶的配合量在化妆料总量的0.05~30重量(质量)%的范围内,优选地,在1~1 5重量(质量)%的范围内。此外,有机硅橡胶事先经过乳化工序(包括乳化聚合)来配制的乳化组合物来使用时,其配合更容易,并可稳定地配合本发明的化妆料。若有机硅橡胶的配合量低于所述下限,则存在对皮肤及毛发的光泽效果不充分的风险。
有机硅弹性体(K)
有机硅弹性体可根据其目的以任意形式来配合到化妆料中,但尤其,所述的[粉末(E)」中说明的有机硅弹性体粉末之外,优选地,作为交联性有机聚硅氧烷配合。有机硅弹性体粉末还能够以水分散液的形式用于本发明的化妆料中。作为这种水分散液的市售产品,可例举东丽道康宁(Toray Dow Corning)公司出品的BY29-129、PF-2001 PIF Emulsion等。通过配合这种有机硅弹性体粉末的水系分散体(=悬浮液),可进一步提高本发明的化妆料的使用感,在这一点上是极其有用的。
作为交联性有机聚硅氧烷,有机聚硅氧烷链通过与交联性成分等之间的反应而形成三维交联的结构,且不具有聚氧化烯单元等的亲水部的非乳化性有机聚硅氧烷为优选。只要是这种交联性有机聚硅氧烷,就可不受稀释/性状等的物理形式或制备方法等制限而使用,特别优选地,可例举美国专利第5654362号中描述的α,ω-二烯交联有机硅弹性体(作为市售产品,DC 9040Silicone Elastomer Blend,DC 9041Silicone Elastomer Blend,DC9045 Silicone Elastomer Blend,DC 9046Silicone Elastomer Blend,美国道康宁公司出品)。并且,还可以优选使用在室温下具有流动性的交联性有机聚硅氧烷,可例举3901LIQUID SATIN BLEND(美国道康宁公司出品)等。
有机改性的有机硅(L)
优选地,有机改性的有机硅具有亲油性。具体而言,除了上述的之外,其实例可包括氨基改性有机硅、氨基聚醚改性有机硅、环氧改性有机硅、羧基改性有机硅、氨基酸改性有机硅、甲醇改性有机硅、丙烯酸改性有机硅、酚改性有机硅、酰胺烷基改性有机硅、氨基二醇改性有机硅、烷氧基改性有机硅。除了以聚硅氧烷键为主链之外,该有机改性的有机硅类可以具有亚烷基链、氨基亚烷基链或化合物不具有亲水性的程度的聚醚链,有机改性基团可以包含在聚硅氧烷链的侧链或末端的一端或两端。在使用本发明的化妆料作为毛发化妆料的情况下,可优选使用氨基改性有机硅、甲醇改性有机硅、氨基聚醚改性有机硅或氨基二醇改性有机硅,具有3-氨基丙基、N-(2-氨基乙基)3-氨基丙基等的氨基改性有机硅可以用作一般实例。
以下,对作为有机改性的有机硅特别优选的高级烷基改性有机硅、烷基改性有机硅树脂及聚酰胺改性有机硅树脂进行描述。高级烷基改性有机硅在室温呈蜡状,是一种有用的化妆料用原料成分。因此,本发明的化妆料中可优选使用。作为这种高级烷基改性有机硅蜡,其实例包括分子链两端由三甲基硅烷氧基封端的甲基长链烷基聚硅氧烷、分子链两端由三甲基硅烷氧基封端的二甲基聚硅氧烷/甲基长链烷基硅氧烷共聚物、分子链两端长链烷基改性二甲基聚硅氧烷等。作为这种市售产品,可例举AMS-C30Cosmetic Wax、2503Cosmetic Wax等(美国道康宁公司出品)。
在本发明的化妆料中,优选地,从持妆性能效果及高温稳定性的观点来看,高级烷基改性有机硅蜡的熔点为60℃以上。
烷基改性有机硅树脂为给化妆料赋予皮脂耐久性、保湿性、肌理细腻触感的成分,可以优选在室温下使用蜡状树脂。优选地,优选例举日本专利特表2007-532754号公报中描述的倍半硅氧烷树脂蜡。作为这种市售产品,可例举SW-8005C30 RESIN WAX等(美国道康宁公司出品)。
作为聚酰胺改性有机硅,可例举美国专利5981680号(日本专利特开2000-038450号公报)和日本专利特表2001-512164号公报中描述的以硅氧烷为基底的聚酰胺化合物,作为市售产品,可例举2-8178Gellant、2-8179Gellant等(美国道康宁公司出品)。聚酰胺改性有机硅还用作油性原料,特别是用作有机硅油的增稠/胶凝剂。
防紫外线成分(M)
防紫外线成分中具有无机系防紫外线成分和有机系防紫外线成分。优选地,如果本发明的化妆料是防晒化妆料,就含有至少一种无机系或有机系,特别是含有有机系防紫外线成分。本发明的共聚物与通常难溶性的有机系防紫外线成分,例如,作为“Uvinul A”周知的二乙基氨基羟基苯甲酰苯甲酸己酯、作为“Tinosorb S”周知的双乙基己氧基苯酚甲氧基苯基三嗪、作为“奥克立林(Octocrylene)”周知的2-氰基-3,3-二苯基丙-2-烯酸2-乙基己酯、其他桂酸类紫外线吸收剂等之间具有优异的相容性,可提高与本发明的共聚物的配合稳定性。
无机系防紫外线成分可以将所述的无机系颜料粉末、金属粉末颜料等作为紫外线分散剂来进行配合,其实例包括氧化钛、氧化锌、氧化铈、低阶氧化钛、铁掺杂氧化钛等的金属氧化物、氢氧化铁等的金属氢氧化物、板状氧化铁、铝片等的金属片类、碳化硅等的陶瓷类。其中,特别优选地,选自平均粒径在1~100nm的范围内的粒状、板状、针状或纤维状的细颗粒金属氧化物及细颗粒金属氢氧化物的至少一种。优选地,对这种粉末进行以往公知的表面处理,例如氟化合物处理(全氟烷基磷酸酯处理或全氟烷基硅烷处理、全氟聚醚处理、氟有机硅处理、氟化有机硅树脂处理为优选)、有机硅处理(甲基氢聚硅氧烷处理、二甲基聚硅氧烷处理、气相法四甲基四氢环四硅氧烷处理为优选)、有机硅树脂处理(三甲基硅烷氧基硅酸处理为优选)、侧链处理(气相法有机硅处理后添加烷基链等的方法)、硅烷偶联剂处理、钛偶联剂处理、硅烷处理(烷基硅烷或烷基硅氮烷处理为优选)、油剂处理、N-酰基化赖氨酸处理、聚丙烯酸处理、金属皂处理(硬脂酸或肉豆蔻酸盐为优选)、丙烯酸树脂处理、金属氧化物处理等,优选地,多次进行这种处理。其实例包括用氧化硅或氧化铝等的金属氧化物涂敷细颗粒氧化钛表面之后,用烷基硅烷进行表面处理等。优选地,相对于粉末,表面处理总量在0.1~50质量%的范围内。
有机系防紫外线成分为亲油性防紫外线成分,其实例包括:对氨基苯甲酸(以下简称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、二乙氨基羟基苯甲酰基苯甲酸己酯等的苯甲酸系紫外线吸收剂;高孟基-N-乙酰邻氨基苯甲酸酯等的邻氨基苯甲酸系紫外线吸收剂;水杨酸戊酯、水杨酸薄荷酯、水杨酸高孟酯、水杨酸辛酯、水杨酸苯酯,水杨酸苄酯,p-异丙醇水杨酸苯酯等的水杨酸系紫外线吸收剂;肉桂酸辛酯、4-异丙基肉桂酸乙酯、2,5-二异丙基肉桂酸甲酯、2,4-二异丙基肉桂酸乙酯、2,4-二异丙基肉桂酸甲酯、对甲氧基肉桂酸丙酯、对甲氧基肉桂酸异丙酯、对甲氧基肉桂酸异戊酯、对甲氧基肉桂酸辛酯(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(三甲基硅烷氧基)硅烷基]丁酯等的肉桂酸系紫外线吸收剂;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-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-羧酸酯、羟基-4-正辛氧基二苯甲酮、4-羟基-3-羧基二苯甲酮等的二苯甲酮系紫外线吸收剂;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、2-苯基-5-甲基苯并恶唑、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、二苄连氮、联大茴香甲酰基甲烷、4-甲氧基-4’-叔丁基二苯甲酰甲烷、5-(3,3-二甲基-2-亚降冰片基(norbonylidene))-3-戊烷-2-酮等。
并且,也可使用在疏水性聚合物粉末中含有所述的有机系防紫外线成分的粉末。聚合物粉末可以是中空的,也可不是中空的,只要平均初级粒径在0.1~50μm的范围内即可,粒度分布可以较宽,也可以尖锐。作为聚合物种类,其实例包括丙烯酸树脂、甲基丙烯酸树脂、苯乙烯树脂、聚氨酯树脂、聚乙烯、聚丙烯、聚对苯二甲酸乙二醇酯、有机硅树脂、尼龙、丙烯酰胺树脂、硅烷基化多肽树脂。优选以0.1~30质量%的范围含有有机系防紫外线成分的聚合物粉末,特别优选地,为含有作为UV-A吸收剂的4-叔丁基-4’-甲氧基二苯甲酰甲烷的聚合物粉末。
并且,还可以使用分散在水中的所述的有机系防紫外线成分。作为市售产品,可举例示出Tinosorb A2B(德国巴斯夫(BASF)公司出品)。
在本发明的化妆料中,可优选使用的防紫外线成分为选自由细颗粒氧化钛、细颗粒氧化锌、对甲氧基肉桂酸2-乙基己酯、4-叔丁基-4’-甲氧基二苯甲酰甲烷、二乙氨基羟基苯甲酰基苯甲酸己酯、双乙基己氧基苯酚甲氧基苯基三嗪、2-氰基-3,3-二苯基丙-2-烯酸2-乙基己酯以及其他二苯甲酮系紫外线吸收剂组成的组中的至少一种。这种防紫外线成分为通用成分,容易获得,且具有高防紫外线效果,因此可优选使用。尤其,优选地,组合使用无机系和有机系的防紫外线成分,更优选地,组合使用对应于UV-A的防紫外线成分和对应于UV-B的防紫外线成分。
水溶性聚合物(N)
另一方面,本发明的化妆料可以为包含大量水溶性成分的水性或乳液型化妆料,可根据其剂型,配合水溶性聚合物(N),且为优选。作为水溶性聚合物,可使用一种或两种以上水溶性聚合物。作为天然的水溶性聚合物,其实例包括阿拉伯胶、黄芪胶、半乳聚糖、瓜尔豆胶、角豆胶、刺梧桐胶、角叉菜胶、果胶、琼脂、榅椁籽(榅椁)、褐藻胶(褐藻提取物)、淀粉(大米、玉米、马铃薯、小麦)、甘草酸等的植物系聚合物、黄原胶、葡聚糖、琥珀葡聚糖、支链淀粉等的微生物系聚合物、胶原蛋白、酪蛋白、白蛋白、明胶等的动物系聚合物。并且,作为半合成水溶性聚合物,其实例包括羧甲基淀粉、甲基羟丙基淀粉等的淀粉系聚合物、甲基纤维素、硝基纤维素、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、羧甲基纤维素钠(CMC)、结晶纤维素、纤维素粉等的纤维素系聚合物、海藻酸钠、海藻酸丙二醇酯等的海藻酸系聚合物。作为合成水溶性聚合物,其实例包括聚乙烯醇、聚乙烯基甲基醚系聚合物、聚乙烯吡咯烷酮、羧乙烯基聚合物(CARBOPOL940,941:美国百路驰(BFGoodrich)公司)等的乙烯基系聚合物、聚乙二醇20000、聚乙二醇6000、聚乙二醇4000等的聚氧乙烯系聚合物、聚氧乙烯/聚氧丙烯共聚物、PEG/PPG甲基醚等的共聚物系聚合物、聚丙烯酸钠、聚丙烯酸乙酯、聚丙烯酰胺等的丙烯酸系聚合物、聚乙烯亚胺、阳离子聚合物等。作为其他阳离子水溶性聚合物,尤其是作为可优选配合到毛发化妆料中的成分,其实例包括四级氮改性多糖(例如,阳离子改性纤维素、阳离子改性羟乙基纤维素、阳离子改性瓜尔豆胶、阳离子改性刺槐豆胶、阳离子改性淀粉等)、二甲基二烯丙基氯化铵衍生物(例如,二甲基二烯丙基氯化铵/丙烯酰胺共聚物、聚氯化二甲基亚甲基哌啶鎓等)、乙烯吡咯烷酮衍生物(例如,乙烯吡咯烷酮/二甲氨基乙基甲基丙烯酸共聚物盐、乙烯吡咯烷酮/甲基丙烯酸酰胺丙基三甲基氯化铵共聚物、乙烯吡咯烷酮/甲基乙烯基咪唑鎓氯化铵共聚物等)。
在不干扰本发明的效果的范围内,本发明的化妆料中可添加用于常规化妆料中的其他成分:有机树脂、保湿剂、防腐剂、抗菌剂、香料、盐类、抗氧化剂、pH调节剂、螯合剂、清爽剂、抗炎剂、美肤成分(美白剂、细胞活化剂、皮肤粗糙改善剂、血液循环促进剂、皮肤收敛剂、抗脂溢剂等)、维生素类、氨基酸类、核酸、激素、包合物等。这些具体例与日本专利特开2011-149017号公报的第0100~0113段中具体公开的内容相同,但不限于此。
本发明的化妆料根据其目的可配合天然系植物提取成分、海藻提取成分、生药成分。可配合两种以上的这种成分。这些具体例与日本专利特开2011-149017号公报的第0115段中具体公开的内容相同,但不限于此。
本发明的化妆料中还可根据其目的配合如轻质异链烷烃、醚类、LPG(liquefiedpetroleum gas,液化石油气)、N-甲基吡咯烷酮、下一代氯氟烃等的溶剂。
并且,除了本发明的共聚物之外,本发明的化妆料中可使用烷基改性有机硅树脂蜡。这些是成模性成分,与本发明的共聚物相同。
作为烷基改性有机硅树脂蜡,优选地,可例举日本专利特表2007-532754号公报中描述的倍半硅氧烷树脂蜡。
[化妆料的种类与制剂]
并且,化妆料的种类及其制剂形式没有特别限定,可以为如护肤产品、止汗剂产品、除臭剂产品、化妆产品、防紫外线产品等的皮肤用化妆品;如睫毛化妆料产品、毛发清洁剂产品、毛发整理用产品、染发用产品、毛发滋养产品、护发产品(Hair rinse products)、护发素产品(Hair conditioner products)、毛发护理产品(Hair treatment products)等的毛发用化妆品;浴用化妆品等的毛发化妆料产品。并且,其形式没有特别限定,但可以为溶液状、乳液状、膏状、固体状、半固体状、糊状、凝胶状、粉状、多层状、摩丝状、油包水型或水包油型的乳化组合物(乳液组合物)中任一种。
其中,外用制剂是适用于人体的皮肤、指甲、毛发等的物质,例如,可配合药物活性成分以用于各种疾病的治疗。化妆料也是适用于人体的皮肤、指甲、毛发等的物质,但也是用于美容目的的物质。即使用作“外用制剂”,实际上也可能以与化妆料相同的剂量和用量使用。因此,本发明的化妆料中,这些外用制剂也被描述为作为化妆料而包含的物质。其一实例包括止汗剂、皮肤清洁剂、皮肤外用制剂、毛发清洁剂、毛发外用制剂等。当例举作为该外用制剂药剂的用途时,可举例示生发剂、养发剂、镇痛剂、杀菌剂、抗炎剂、清爽剂、皮肤抗衰老剂,但不限定于此。
(成膜性/毛发的触感效果)
本发明的化妆料包含上述的共聚物,因此可在皮肤或毛发上形成具有优异的防水性能且具有优异的持续性及皮脂耐久性的薄膜。尤其,在本发明的共聚物中,具有产生刺激性的风险且具有通过常规蒸馏方法难以从共聚物分离出或除去的性质的含有碳硅氧烷树枝状大分子结构的单体含量极少,并且可在皮肤或毛发上形成具有优异的耐水性及耐皮脂性的薄膜,因此可设计无刺激性问题并赋予这种功能性薄膜的化妆料。
所述的皮肤用化妆品可用于头皮、面部(包括嘴唇、眉毛、脸颊)、手指、指甲、全身的任何部位。其具体实例包括:洁面凝胶、洁面霜、洁面泡沫、洗面奶、眼部卸妆液、洗面奶、液体皂(沐浴露)、洗手液、凝胶皂、剃须膏、洗甲液、祛痘化妆料等的皮肤清洁剂产品;护肤霜、头皮修护素、护肤乳、牛奶润肤露、乳液、面膜、爽身粉、精华液、剃须乳液、按摩液等的护肤产品;粉底、粉底液、油性粉底、化妆肌底液、白粉、蜜粉、腮红、唇膏、胭脂、唇彩、眼霜、睫毛膏、眉毛笔、眉毛化妆品等的化妆产品;除臭剂等止汗剂;以及防晒剂、晒黑剂(晒黑剂)等防紫外线产品。
所述的毛发用化妆品的实例包括洗发水、洗护一体等的毛发用清洁剂;发蜡、毛发用卷发保持剂、定型剂、发膏、发胶、发液等的美发产品;染发剂、染发喷剂、染发剂、染发棒等的染发用产品;护发素、护发精华素、发膜等的头发滋养产品;护发油、润丝膏、修护液、润发素、修护素等的洗发或护发产品。并且,所述的洗浴用化妆品可例举泡沫浴。
[本发明的包含共聚物的化妆料配方的设计和指南]
在本发明的共聚物中,具有产生刺激性的风险且具有通过常规蒸馏方法难以从共聚物分离出或除去的性质的含有碳硅氧烷树枝状大分子结构的单体含量极少,除此之外,具有与已知的丙烯酸有机硅树枝状聚合物相同的防水性、去污性、成膜性等的特性。因此,例如,在日本专利第4009382号公报(日本专利特开2000-063225号公报)等中所描述的在侧链具有碳硅氧烷树枝状大分子结构的乙烯基系聚合物等中的公知配方中,可取代其中一部分或全部来使用。即,在包含公知的在侧链具有碳硅氧烷树枝状大分子结构的乙烯基系聚合物的化妆料配方中,通过本发明的共聚物来取代对应的乙烯基系聚合物以设计或制备化妆料配方,这是本申请人在本文中明确教导的。
类似地,在提出侧链具有碳硅氧烷树枝状大分子结构的乙烯基系聚合物的市售产品的公知配方中,本发明的共聚物可取代其中一部分或全部来使用。例如,作为市售产品,其实例包括道康宁东丽株式会社(Dow Corning Toray Co Ltd)出品的FA 4001 CMSilicone Acrylate、FA 4002 ID Silicone Acrylate、DOWSIL(TM)FA 4003 DM SiliconeAcrylate等,使用这些的化妆料配方在多数产品、专利、DOW SILICONE CORPORATION提供的配方样品、IP.com中的公开信息等中已知,但本发明的共聚物可通过无限制地取代在侧链具有碳硅氧烷树枝状大分子结构的乙烯基系聚合物的一部分或全部来使用,且为优选。
当根据本发明的共聚物来取代公知化妆料配方中的在侧链具有碳硅氧烷树枝状大分子结构的乙烯基系聚合物时,根据本领域技术人员的常规配合配方,可简单地通过该共聚物来取代化妆料配方中的相应材料,不仅如此,使用公知配方且不损害其化妆料的性能/特性,存在如下实际有益之处,即可提供仅减少或基本上不含有具有产生刺激性的风险且具有通过常规蒸馏方法难以从共聚物分离出或除去的性质的含有碳硅氧烷树枝状大分子结构的单体含量的化妆料。
本发明的共聚物可用于其他用途,还可配合到化妆料以外的产品中,例如各种外用制剂、涂料、涂敷剂、消泡剂、除臭剂等。
<成膜剂>
作为本发明的共聚物成膜剂,还可用于化妆料以外的用途上。即,只要要求在薄膜上具有防水效果、防油效果、完整性(integrity)、强度及耐摩擦性的用途,就可以不分领域使用。尤其,还可用于对涂料组合物和纤维的防水效果赋予剂、无机材料/有机材料的处理剂等。并且,根据需要,本发明的成膜剂可以在水性环境下使用,因此易于处理。
具体而言,本发明的成膜剂具有优异的配合稳定性,且不损害成膜性及使用感,因此,也可优选用作作为纤维处理剂或棉布/织物处理剂的工业用途的成膜剂。
[本发明的共聚物的制备方法]
如上所述,作为本发明的共聚物的原料的含有碳硅氧烷树枝状大分子结构的单体具有通过常规蒸馏方法难以从共聚物分离出或除去的性质。然而,通过本发明的共聚物的制备方法,可将该单体减少至相对于共聚物的2500ppm以下。另外,通过包括以下工序(I)的制备方法,可缩短自由基聚合反应所需的反应时间并改善工业的生产效率。
本发明的共聚物的制备方法的特征在于,
向具有含有能够自由基聚合的有机基团的碳硅氧烷树枝状大分子结构的不饱和单体(a1)和
具有自由基聚合性乙烯基的与成分(a1)不同的不饱和单体(a2)中添加聚合引发剂以进行自由基聚合反应的工序,且包括
工序(I):在自由基聚合反应中的聚合引发剂的第一次添加后经过至少两小时之后,再添加与第一次添加的聚合引发剂相同或不同的聚合引发剂的工序(Ia)。该制备方法的所述的工序(I)可任意包括添加(Ib)常压(1atm)下沸点低于160℃的具有自由基聚合性乙烯基的单体(a2′)以促进未反应的成分(a1)的自由基聚合反应的工序,也可包括工序(II):在工序(I)之后,在常压或减压下蒸馏出残留在体系中的未反应不饱和单体或饱和单体的工序,且为优选。
其中,成分(a1)、成分(a2)及聚合引发剂如上所述。并且,作为在常压(1atm)下沸点低于160℃的具有自由基聚合性乙烯基的单体(a2′),只要具有该性质就没有特别限制,但是成分(a2)可优选例举沸点低且容易减压蒸馏的(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯等。并且,自由基聚合反应可在上述的反应溶剂中进行,该反应溶剂可通过下文中所述的工序(IV)进行溶剂置换,并且为优选。
上述的工序(I)为用于提高应减少的(a1)具有含有能够自由基聚合的有机基团的碳硅氧烷树枝状大分子结构的不饱和单体的反应效率并抑制其残留量而所需的工序,并且为在自由基聚合反应中的聚合引发剂的第一次添加后经过至少两小时之后,再添加与第一次添加的聚合引发剂相同或不同的聚合引发剂的工序(Ia)。从第一次添加聚合引发剂开始设置时间差,具体而言,至少设置两小时,优选地,在两个半小时以上以后,向反应体系中加入额外的聚合引发剂,从而初始自由基聚合反应中未消耗的成分(a1)的自由基聚合反应进行,并且体系中的残留量明显减少。其中,再添加的聚合引发剂的量无特别限制,但相对于第一次添加的聚合引发剂,可以在0.5~5.0等量的范围内,特别优选地,在0.6~4.5等量的范围内。另外,通过从第一次添加聚合引发剂开始设置时间差,额外地添加聚合引发剂,可使自由基聚合反应所需的反应时间缩短,并且可提高本发明的共聚物的工业的生产效率。
并且,上述的工序(I)还可以任意包括添加常压(1atm)下沸点低于160℃的具有自由基聚合性乙烯基的单体(a2′)以促进未反应的成分(a1)的自由基聚合反应的工序(Ib)。从第一次添加聚合引发剂开始设置时间差,向反应体系中加入额外的聚合引发剂及其他反应性的不饱和单体,从而初始自由基聚合反应中未消耗的成分(a1)与额外的成分(a2′)一同进行自由基聚合反应,体系中的残留量明显减少。另外,该成分(a2′)具有低沸点,因此,在使成分(a1)反应后,可易于进行减压蒸馏。
通过以上工序(I),可预先有效地使具有难以通过减压蒸馏等方法从共聚物中分离/除去的性质的成分(a1)或作为其氢化产物的饱和单体进行反应以消耗,使得该体系中的残留量明显减少。
在本发明的制备方法中,在上述的工序(I)之后,还可包括常压或减压下蒸馏出残留在体系中的未反应不饱和单体或饱和单体的工序(II)。此外,该工序的目的在于,蒸馏未反应单体中的低沸点成分以进行提纯,成分(a1)的含量已经经过其前阶段步骤的工序(I)而减少。工序(II)中的常压或减压下的未反应不饱和单体或饱和单体的蒸馏可无特别限制地使用汽提等的公知方法来进行。
此外,在工序(I)之后,在其后阶段的工序过程中,可在之前或之后的任一时间点上进行回流、再沉淀、过滤等的工序。
在本发明的制备方法中,上述的在工序(I)之后,在工序(II)之前或与工序(II)同时,还可包括对残留在体系中的未反应不饱和单体进行加氢反应以将不饱和单体转化为饱和单体的工序(III)。该工序通过使所述加氢反应催化剂(镍催化剂或钯催化剂)与工序(I)的聚合反应物接触来进行,以形成作为未反应的成分(a1)等的氢化反应物的饱和单体,且可减少共聚物的气味。此外,工序(III)为将未反应的成分(a1)转换为饱和单体的工序,因此,该工序(III)中,衍生自未反应的成分(a1)的单体量并不减少。
在本发明的制备方法中,在任意的时间点上,优选地,在上述的工序(II)之前或与工序(II)同时,包括向体系中添加一种以上的醇类(C)和/或油剂(D)以作为分散介质,并除去自由基聚合反应中的反应溶剂的工序(IV)。通过该工序,可获得包含化妆料等中的配合稳定性及处理加工性优异的醇类(C)和/或油剂(D)的共聚物组合物。与所述的工序(II)类似地,自由基聚合反应中的反应溶剂可在常压或减压条件下使用汽提等的公知方法来除去而没有特别限制,并且可与所述的醇类(C)和/或油剂(D)的一种以上进行替换。此外,在自由基聚合反应中的反应溶剂为醇类(C)的情况下,自由基聚合反应溶液本身形成包含醇类(C)的共聚物组合物,因此,根据需要,可直接用作化妆料原料或成膜剂。
实施例
以下,通过实施例进一步详细说明本发明,但本发明并不限定于这些实施例。
实施例等中的各个特性通过以下方法测量。
[GPC峰值分子量]
在洗脱溶剂中使用甲苯,并在柱上使用TSKgel Multipore HXL-M来进行GPC分析,并使用标准聚苯乙烯的校准曲线求得分子量。
[残留碳硅氧烷树枝状聚合物单体(A-1)的定量]
通过高效液相色谱法(日本岛津(Shimadzu)制作所的Prominence-i LC-2030C3D、柱:Atlantis T3-3μm(3.0×100mm)、紫外线可见吸收检测部、洗脱溶剂:水/甲醇/THF的梯度模式)进行定量。
[运动粘度]
使用乌氏粘度管,测量了组合物在25℃下的粘度。
[非挥发性成分]
在直径6cm的铝盘上称量1g样品,并在150℃下加热1小时之后残留的样品中求得。
[薄膜粘性]
当以与上述相同的方式用手指触摸形成在铝盘上的薄膜时,并判断与薄膜成一体的铝盘是否膨起。
[接触角(水)]
在玻璃板上涂敷乙烯基系共聚物的IPA溶液之后,在室温下干燥除去溶剂以获得乙烯基系聚合物的覆膜。在该覆膜表面上放置5μL水滴,并测量相对于水的接触角。测量装置使用液滴形状分析系统(Drop shape analysis system)(KRUSS DSA10 Mk-2),并求得n=5以上的平均值。
[接触角(人工皮脂)]
在玻璃板上涂敷乙烯基系共聚物的IPA溶液之后,在室温下干燥除去溶剂以获得乙烯基系聚合物的覆膜。在该覆膜表面上放置5μL人工皮脂(三油精:油酸:角鲨烷=3∶1∶1的混合物)的液滴,并测量相对于人工皮脂的接触角。测量装置使用液滴形状分析系统(Drop shape analysis system)(KRUSS DSA10 Mk-2),并求得n=5以上的平均值。
[实施例1]
[共聚物及其液态组合物的配制]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,装入163g异丙醇(IPA),通入氮气鼓泡,充分脱气,加热至70℃。向滴液漏斗中加入110g甲基丙烯酸甲酯(55重量%)、10g丙烯酸正丁酯(5重量%)、80g由下式(A-1):
[化学式26]
表示的碳硅氧烷树枝状聚合物单体(40重量%)、4.4g的2,2’-偶氮双-2-异丁酸甲酯(V-601,富士胶片和光纯药生产)(2.2重量%)、107gIPA并进行溶解。在氮气气氛中,在保持70℃温度的同时从滴液漏斗滴加单体混合物1小时。滴加结束后,在氮气氛下加热搅拌3小时,加入将4.4g的V-601(2.2重量%)溶解在30gIPA中而形成的溶液。并且,搅拌9小时之后,获得40.8%的非挥发性成分的反应产物。GPC分析表明,其为峰值分子量为15900的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有1330ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[参考例1]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,加入163gIPA,通入氮气鼓泡,充分脱气,加热至70℃。在滴液漏斗中加入110g甲基丙烯酸甲酯(55重量%)、10g丙烯酸正丁酯(5重量%)、80g碳硅氧烷树枝状聚合物单体(A-1)(40重量%)、2gV-601(1重量%)、107gIPA并进行溶解。在氮气气氛中,在保持70℃温度的同时从滴液漏斗滴加单体混合物1小时。滴加结束后,在氮气氛下加热搅拌8小时,获得40.6%的非挥发性成分的反应产物。GPC分析表明,其为峰值分子量为23600的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有30750ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[参考例2]
除了将参考例1的V-601的量设定为4.4g(2.2重量%)以外,其他操作相同,从而获得反应产物。GPC分析表明,其为峰值分子量为16000的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有11000ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[参考例3]
除了将参考例1的V-601的量设定为8.8g(4.4重量%)以外,其他操作相同,从而获得反应产物。GPC分析表明,其为峰值分子量为12600的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有2250ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[总结1]
上述结果总结在表1中。由实施例1与参考例2之间的对比、以及与参考例l~3之间对比可知,根据作为第一次加入的聚合引发剂的V-601的量来确定聚合物分子量。并且,通过间隔时间差来额外添加聚合引发剂V-601,可显著减少反应性差的碳硅氧烷树枝状聚合物单体(A-1)的残留量。
[表1]
[实施例2]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,加入163gIPA,通入氮气鼓泡,充分脱气,加热至70℃。向滴液漏斗中加入110g甲基丙烯酸甲酯(55重量%)、10g丙烯酸正丁酯(5重量%)、80g碳硅氧烷树枝状聚合物单体(A-1)(40重量%)、4.4gV-601(2.2重量%)、107gIPA并进行溶解。在氮气气氛中,在保持70℃温度的同时从滴液漏斗滴加单体混合物1小时。滴加结束后,在氮气氛下加热搅拌6小时,并加入将0.6g的V-601(0.3重量%)溶解在30gIPA中而形成的溶液。并且,搅拌6小时之后,获得40.0%非挥发性成分的反应产物。GPC分析表明,其为峰值分子量为17200的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有2350ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[比较例1]
除了将参考例1的V-601的量设定为4.4g(2.2重量%)并将加热搅拌的时间设定为12小时以外,其他操作相同,从而获得反应产物。GPC分析表明,其为峰值分子量为17000的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有5200ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[比较例2]
除了将参考例1的V-601的量设定为4.4g(2.2重量%)并将将加热搅拌的时间设定为24小时以外,其他操作相同,从而获得反应产物。GPC分析表明,其为峰值分子量为18000的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有2740ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[总结2]
上述结果总结在表2中。由此可知,通过添加引发剂,不仅可以减少反应性差的碳硅氧烷树枝状聚合物单体(A-1)的残留量,还可大幅缩短反应时间。
[表2]
[实施例3]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,加入163gIPA,通入氮气鼓泡,充分脱气,加热至70℃。在滴液漏斗中加入110g甲基丙烯酸甲酯(55重量%)、10g丙烯酸正丁酯(5重量%)、80g碳硅氧烷树枝状聚合物单体(A-1)(40重量%)、4.4g的1,1,3,3-四甲基丁基过氧-2-乙基己酸酯(PEROCTA O,日本日油株式会社出品)(2.2重量%)、107gIPA并进行溶解。在氮气气氛中,在保持70℃温度的同时从滴液漏斗滴加单体混合物1小时。滴加结束后,在氮气氛下加热搅拌4小时,加入将4.4g的PEROCTA(注册商标)O(1,1,3,3-四甲基丁基过氧-2-乙基己酸酯)(2.2重量%)溶解在30gIPA中而形成的溶液。在进一步搅拌4小时之后,获得反应产物。GPC分析表明,其为峰值分子量为19400的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有1350ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[实施例4]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,加入163gIPA,通入氮气鼓泡,充分脱气,加热至70℃。在滴液漏斗中计入110g甲基丙烯酸甲酯(55重量%)、10g丙烯酸正丁酯(5重量%)、80g碳硅氧烷树枝状聚合物单体(A-1)(40重量%)、4.4g的PEROCTA O(2.2重量%)、107gIPA并进行溶解。在氮气气氛中,在保持70℃温度的同时从滴液漏斗滴加单体混合物1小时。滴加结束后,在氮气氛下加热搅拌6小时,加入将0.6g的PEROCTA(注册商标)O(1,1,3,3-四甲基丁基过氧-2-乙基己酸酯)(0.3重量%)溶解在30g的IPA而形成的溶液中。在进一步搅拌6小时之后,获得反应产物。GPC分析表明,其为峰值分子量为18700的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有1320ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[比较例3]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,加入163gIPA,通入氮气鼓泡,充分脱气,加热至70℃。在滴液漏斗中加入110g甲基丙烯酸甲酯(55重量%)、10g丙烯酸正丁酯(5重量%)、80g碳硅氧烷树枝状聚合物单体(A-1)(40重量%)、4.4g的PEROCTA O(2.2重量%)、107gIPA并进行溶解。在氮气气氛中,在保持70℃温度的同时从滴液漏斗滴加单体混合物1小时。滴加结束后,在氮气氛下加热搅拌12小时以获得反应产物。GPC分析表明,其为峰值分子量17000的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有9.580ppm的碳硅氧烷树枝状聚合物单体(A-1)。
[总结3]
上述结果总结在表3中。即使使用过氧化物类引发剂作为聚合引发剂,也获得类似的趋势和结果。
[表3]
以下,在实施例5、实施例6、比较例4、比较例5中,对单体组成不同的聚合物进行研究。
[实施例5]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,加入163gIPA,通入氮气鼓泡,充分脱气,并加热至75℃。在滴液漏斗中加入76g甲基丙烯酸甲酯(38重量%)、24g丙烯酸正丁酯(12重量%)、100g碳硅氧烷树枝状聚合物单体(A-1)(50重量%)、2g的V-601(1重量%)、107gIPA并进行溶解。在氮气气氛中,在保持75℃温度的同时从滴液漏斗滴加单体混合物3小时。滴加结束后,在氮气氛下加热搅拌4小时,并加入将8g的V-601(4重量%)溶解在30g的IPA中而形成的溶液和0.6g丙烯酸正丁酯(0.3重量%)。在进一步搅拌6小时之后,获得非挥发性成分40.0%的反应产物。GPC分析表明,其为峰值分子量为23100的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有1380ppm碳硅氧烷树枝状聚合物单体(A-1)。
[实施例6]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,加入163gIPA,通入氮气鼓泡,充分脱气,加热至70℃。在滴液漏斗中加入76g甲基丙烯酸甲酯(38重量%)、24g丙烯酸正丁酯(12重量%)、100g碳硅氧烷树枝状聚合物单体(A-1)(50重量%)、2g的V-601(1重量%)、107gIPA并进行溶解。在氮气气氛中,在保持70℃温度的同时从滴液漏斗滴加单体混合物3小时。滴加结束后,在氮气氛下加热搅拌4小时,并加入将8g的V-601(4重量%)溶解在30g的IPA中而形成的溶液和0.6g丙烯酸正丁酯(0.3重量%)。在进一步搅拌两小时之后,获得非挥发性成分39.8%的反应产物。GPC分析表明,其为峰值分子量为28900的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有2240ppm碳硅氧烷树枝状聚合物单体(A-1)。
[比较例4]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,加入163gIPA,通入氮气鼓泡,充分脱气,加热至70℃。在滴液漏斗中加入76g甲基丙烯酸甲酯(38重量%)、24g丙烯酸正丁酯(12重量%)、100g碳硅氧烷树枝状聚合物单体(A-1)(50重量%)、2g的V-601(1重量%)、107gIPA并进行溶解。在氮气气氛中,在保持70℃温度的同时从滴液漏斗滴加单体混合物3小时。滴加结束后,在氮气氛下加热搅拌1小时,并加入将2g的V-601(1重量%)溶解在30g的IPA而形成的溶液。在进一步搅拌两小时之后,获得非挥发性成分40.7质量%的反应产物。GPC分析表明,其为峰值分子量为28400的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有4320ppm碳硅氧烷树枝状聚合物单体(A-1)。
[比较例5]
在安装有搅拌装置、温度计、回流管的1升的四口烧瓶中,加入163gIPA,通入氮气鼓泡,充分脱气,加热至70℃。在滴液漏斗中加入76g甲基丙烯酸甲酯(38重量%)、24g丙烯酸正丁酯(12重量%)、100g碳硅氧烷树枝状聚合物单体(A-1)(50重量%)、2g的V-601(1重量%)、107gIPA并进行溶解。在氮气气氛中,在保持70℃温度的同时从滴液漏斗滴加单体混合物3小时。滴加结束后,在氮气氛下加热搅拌7小时,获得非挥发性成分40.9质量%的反应产物。GPC分析表明,其为峰值分子量为29300的聚合物。并且,使用高效液相色谱法分析的结果,发现残留有14750ppm碳硅氧烷树枝状聚合物单体(A-1)。
[总结4]
上述结果总结在表4中。在组成不同的单体聚合中,通过将低分子单体与聚合引发剂一同添加,以能够减少反应性差的碳硅氧烷树枝状聚合物单体(A-1)的残留量。
[表4]
[实施例7~11]
以下,将上述的实施例中获得的聚合物通过油剂(异十二烷等)来替换反应溶剂,以获得液态共聚物组合物。其详细信息及属性总结在表5中。此外,非挥发性成分为各实施例中的具有碳硅氧烷树枝状大分子结构的乙烯基共聚物,这种液态共聚物组合物中(A-1)成分的含量
降低至1000ppm以下。
[实施例7]
在作为实施例1的乙烯基系聚合物的异丙醇溶液200g中加入120g异十二烷(Mercazole R,日本丸善石油公司出品)之后,在120℃温度下蒸馏IPA。在减压条件下,蒸馏未反应单体,以获得液态组合物。非挥发性成分为37.0质量%,运动粘度为27mm2/s。接触角(水)为105°,接触角(人工皮脂)为52°,并且,薄膜无粘性,作为化妆料用薄膜剂有用。
[实施例8]
在作为实施例2的乙烯基系聚合物的异丙醇溶液200g中加入120gMercazole R之后,在120℃温度下蒸馏IPA。在减压条件下,蒸馏未反应单体,以获得液态组合物。非挥发性成分为40.5质量%、运动粘度为66mm2/s。
[实施例9]
在作为实施例3的乙烯基系聚合物的异丙醇溶液200g中加入120gMercazole R之后,在120℃温度下蒸馏IPA。在减压条件下,蒸馏未反应单体,以获得液态组合物。非挥发性成分为41.6质量%,运动粘度为172mm2/s。
[实施例10]
在作为实施例5的乙烯基系聚合物的异丙醇溶液200g中加入120g十二烷(PARAFOL12-97,德国沙索公司出品)之后,在120℃温度下蒸馏IPA。在减压条件下,蒸馏未反应单体,以获得液态组合物。非挥发性成分为39.4质量%,运动粘度为76mm2/s。接触角(水)为113°,接触角(人工皮脂)为59°,并且,薄膜无粘性,作为化妆料用薄膜剂有用。
[实施例11]
在作为实施例5的乙烯基系聚合物的异丙醇溶液200g中加入120g的十一烷和十三烷的混合液(CETIOL ULTIMATE、德国巴斯夫(BASF)公司出品)之后,在120℃温度下蒸馏IPA。在减压条件下,蒸馏未反应单体,以获得液态组合物。非挥发性成分为37.6质量%,运动粘度为49mm2/s。接触角(水)为109°,接触角(人工皮脂)为51°,并且,薄膜无粘性,作为化妆料用薄膜剂有用。
[表5]
Claims (15)
1.一种共聚物,其特征在于,所述共聚物为具有含有能够自由基聚合的有机基团的碳硅氧烷树枝状大分子结构的不饱和单体(a1)和
具有自由基聚合性乙烯基的与成分(a1)不同的不饱和单体(a2)的共聚物,
相对于共聚物,未反应不饱和单体(a1)和衍生自该未反应不饱和单体(a1)的饱和单体的含量为2500ppm以下。
2.根据权利要求1所述的共聚物,其特征在于,相对于构成共聚物的成分(a1)及成分(a2)的总质量,所述的成分(a1)的质量%为20质量%以上。
3.根据权利要求1或2所述的共聚物,其特征在于,成分(a1)为由式(1)表示的具有碳硅氧烷树枝状大分子结构的不饱和单体,
式(1):
[化学式1]
{在式中,
Z为2价有机基团,
p为0或1,
R1及R2分别独立地为碳原子数1~10的烷基、芳基或芳烷基,
当i=1时,L1为由下式(2)表示的甲硅烷基烷基,
[化学式2]
(在式中,
Z及p与上文定义相同,
R1及R2与上文定义相同,
i为表示所述甲硅烷基烷基的总层数的1~10的整数,
Li+1为选自由氢原子、碳原子数1~10的烷基、芳基、芳烷基及所述甲硅烷基烷基组成的组中的基团,但当i=c(c为表示所述甲硅烷基烷基的层的1~10的整数)时,Li+1为氢原子、碳原子数1~10的烷基、芳基或芳烷基,当i<c时,Li+1为所述甲硅烷基烷基,ai为0~3的整数)}。
4.一种共聚物组合物,其特征在于,
所述共聚物组合物包含根据权利要求1至3中任一项所述的共聚物、
以及一种以上的醇类(C)和/或油剂(D)。
5.一种化妆料原料,其特征在于,所述化妆料原料包含根据权利要求1至3中任一项所述的共聚物。
6.一种成膜剂,其特征在于,所述成膜剂包含根据权利要求1至3中任一项所述的共聚物。
7.一种化妆料,其特征在于,所述化妆料包含根据权利要求1至3中任一项所述的共聚物。
8.一种化妆料,其特征在于,所述化妆料包含根据权利要求4所述的共聚物组合物。
9.一种化妆料,其特征在于,所述化妆料包含根据权利要求1至3中任一项所述的共聚物且
包含选自由水(B)、醇类(C)、油剂(D)、粉末或着色剂(E)、表面活性剂(F)、油溶性胶凝剂(G)、有机改性粘土矿物(H)、有机硅树脂(I)、有机硅橡胶(J)、有机硅弹性体(K)、有机改性的有机硅(L)、防紫外线成分(M)、及水溶性聚合物(N)组成的组中的至少一种。
10.根据权利要求7至9中任一项所述的化妆料,其特征在于,所述化妆料为选自护肤产品、毛发产品、止汗剂产品、除臭剂产品、化妆产品及防紫外线产品的一种以上的化妆料。
11.一种共聚物的制备方法,所述共聚物为根据权利要求1至3中任一项所述的共聚物,所述共聚物的制备方法的特征在于,包括向具有含有能够自由基聚合的有机基团的碳硅氧烷树枝状大分子结构的不饱和单体(a1)和
具有自由基聚合性乙烯基的与成分(a1)不同的不饱和单体(a2)中添加聚合引发剂以进行自由基聚合反应的工序,
且包括工序(I):在自由基聚合反应中的聚合引发剂的第一次添加后经过至少两小时之后,
再添加与第一次添加的聚合引发剂相同或不同的聚合引发剂的工序(Ia)。
12.根据权利要求11所述的共聚物的制备方法,其特征在于,所述的工序(I)还包括添加常压(1atm)下沸点低于160℃的具有自由基聚合性乙烯基的单体(a2′)以促进未反应的成分(a1)的自由基聚合反应的工序(Ib)。
13.根据权利要求11或12所述的共聚物的制备方法,其特征在于,所述制备方法还包括工序(II):在工序(I)之后,在常压或减压下蒸馏出残留在体系中的未反应不饱和单体或饱和单体的工序。
14.根据权利要求11至13中任一项所述的共聚物的制备方法,其特征在于,所述制备方法还包括工序(III):对残留在体系中的未反应不饱和单体进行加氢反应以将不饱和单体转化为饱和单体的工序。
15.根据权利要求11至14中任一项所述的共聚物的制备方法,其特征在于,所述制备方法还包括工序(IV):向体系中添加一种以上的醇类(C)和/或油剂(D)以除去自由基聚合反应中的反应溶剂的工序。
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US20220213309A1 (en) | 2022-07-07 |
CN118255914A (zh) | 2024-06-28 |
KR20210150441A (ko) | 2021-12-10 |
EP3950727A4 (en) | 2022-12-07 |
JPWO2020203145A1 (zh) | 2020-10-08 |
JP7481326B2 (ja) | 2024-05-10 |
WO2020203145A1 (ja) | 2020-10-08 |
EP3950727A1 (en) | 2022-02-09 |
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