CN108137820B - 化妆品组合物、化妆品和皮肤外用制剂 - Google Patents
化妆品组合物、化妆品和皮肤外用制剂 Download PDFInfo
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- CN108137820B CN108137820B CN201680059279.8A CN201680059279A CN108137820B CN 108137820 B CN108137820 B CN 108137820B CN 201680059279 A CN201680059279 A CN 201680059279A CN 108137820 B CN108137820 B CN 108137820B
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- silicone rubber
- rubber particles
- composite silicone
- particles
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Abstract
本发明公开了一种复合硅橡胶颗粒,其特征在于,硅橡胶颗粒的一部分或全部表面被精细颗粒覆盖,其表面被含有季铵盐的官能团改性。本发明涉及复合硅橡胶颗粒的制造方法以及使用该复合硅橡胶颗粒的分散体和化妆产品组合物。具有亲水性和分散性同时保持优异流动性的复合硅橡胶颗粒不含有害甲醇,并且具有抗微生物活性。
Description
技术领域
本发明涉及化妆品组合物和化妆品以及包含化妆品组合物和化妆品的皮肤外用制剂。
背景技术
硅橡胶颗粒用作化妆产品、涂料、油墨、热固性有机树脂、热塑性有机树脂等的添加剂,并且特别适合用作热固性有机树脂的内部应力松弛剂、用于有机树脂膜的表面润滑剂和用于化妆产品组合物的触感增强剂。然而,此类硅橡胶颗粒易于聚集,并且因此具有差的流动性以及在水性组合物如水基涂料和化妆产品中的差的分散性。因此,如果固化的有机硅颗粒不能均匀地分散到水性组合物中并且以聚集状态存在于水性组合物中,则存在以下问题:就水基涂料而言固化的有机硅颗粒不能充分地提供均匀的亚光效果,以及就化妆产品而言,外观或触感差。
已经提出了通过用无机精细颗粒覆盖硅橡胶颗粒的表面来改善流动性的复合硅橡胶颗粒(参见日本未经审查的专利申请公布No.H4-348143,日本未经审查的专利申请公布No.H7-102075,日本未经审查的专利申请公布No.H9-208709和日本未经审查的专利申请公布No.2007-176822)。然而,此类复合硅橡胶颗粒表现出差的亲水性,当将颗粒共混入水性组合物中时,这导致对水性组合物的亲和力差的问题。此外,将此类颗粒共混入化妆产品组合物中时,存在硬质无机颗粒的触感问题。
已经引入了通过粘附表面活性剂、无机精细颗粒和复合硅橡胶颗粒而具有增强的亲水性的复合硅橡胶颗粒以及通过将多元醇粘附到无机精细颗粒而增强了亲水性的复合硅橡胶颗粒(国际专利号WO/2004/055099和日本未经审查的专利申请公布No.2011-026469)。然而,存在使用此类复合硅橡胶颗粒的化妆产品的组成设计有限的问题,这是因为为了维持足够的亲水性有必要粘附大量的表面活性剂或多元醇。
已经提出了一种复合硅橡胶颗粒,其中由无机精细颗粒覆盖的硅橡胶颗粒的表面用有机硅化合物或其(部分)水解产物处理以降低聚集性(日本未审专利申请公布No.2006-188592)。然而,已有教导或暗示在有机硅化合物中没有含铵基有机基团的有机硅化合物。此外,用有机硅化合物覆盖的复合硅橡胶颗粒存在的问题是复合硅橡胶颗粒含有与硅键合的甲氧基基团或甲醇,并且因此难以共混入化妆产品组合物中。此外,没有考虑将含有极性铵盐官能团的有机基团添加到硅橡胶颗粒的想法,因为聚集首先成为问题。
关于抗微生物的硅橡胶颗粒,提出了一种负载含银颗粒的载银硅橡胶颗粒具有抗微生物效果(日本未经审查的专利申请公布(PCT申请的翻译)No.2015-520291)。在含银颗粒和硅橡胶颗粒的混合步骤中,其是在硅橡胶颗粒表面上负载含银颗粒的干燥制造方法,由于银化合物粘附到混合容器的内部,容器污染或银材料的使用效率差都是问题。在湿法中,由于诸如银离子沉积、硅橡胶颗粒表面上的银离子的还原以及诸如水的溶剂的去除的因素,在硅橡胶的表面上负载银材料的产率较低。此外,已知含银颗粒的粒径和颗粒数对抗微生物作用具有实质性影响;因此为了提高抗微生物活性,需要增加银化合物的配混量,这导致制造成本高,产生使用范围受限的问题。
引用列表
专利文献
专利文献1:日本未经审查的专利申请公布No.H04-348143A
专利文献2:日本未经审查的专利申请公布No.H7-102075A
专利文献3:日本未经审查的专利申请公布No.H9-208709A
专利文献4:日本未经审查的专利申请公布No.2007-176822
专利文献5:WO/2004/055099
专利文献6:日本未经审查的专利申请公布No.2011-026469A
专利文献7:日本未经审查的专利申请公布No.2006-188592A
专利文献8:日本未经审查的专利申请公布No.2015-520291A
发明内容
技术问题
本发明的一个目的是提供一种复合硅橡胶颗粒,其具有亲水性和分散性,同时保持优异的流动性且能够表现出诸如抗微生物活性或毛发粘附的功能。本发明的另一个目的是提供一种甲醇含量极低的复合硅橡胶颗粒。本发明的另一个目的是提供具有改善的触感的复合硅橡胶颗粒、有效生产颗粒的制造方法、颗粒的均匀分散以及包含该颗粒的化妆产品组合物。
问题的解决方案
本发明的复合硅橡胶颗粒的特征在于,硅橡胶颗粒的一部分或全部表面被精细颗粒覆盖,其表面被含有季铵盐的官能团改性。
本发明的复合硅橡胶颗粒的制造方法至少具有以下步骤:
步骤1:通过使用机械力混合精细颗粒和硅橡胶颗粒来形成复合硅橡胶颗粒;以及
步骤2:用具有含有季铵盐的官能团且能够在精细颗粒的表面上形成化学键的硅化合物对步骤1中得到的复合硅橡胶颗粒的精细颗粒的表面进行改性。
本发明的分散体是本发明的复合硅橡胶颗粒与液体化合物的均匀混合物。
本发明的化妆产品组合物含有本发明的复合硅橡胶颗粒。
本发明的有利效果
本发明的复合硅橡胶颗粒的特征在于,复合硅橡胶颗粒具有亲水性和分散性,同时保持优异的流动性,具有抗微生物活性和毛发粘附性,并且不含甲醇。
本发明的制造方法的特征在于,可有效地制造具有抗微生物和毛发粘附性且不含甲醇的复合硅橡胶颗粒。本发明的分散体的特征在于,复合硅橡胶颗粒均匀分散,并且其中该分散体具有抗微生物活性和毛发粘附性并且不含甲醇。本发明的化妆产品组合物具有良好的使用感,同时具有抗微生物活性和毛发粘附性并且不含甲醇。
具体实施方式
本发明的复合硅橡胶颗粒的特征在于,硅橡胶颗粒的一部分或全部表面被精细颗粒覆盖,其表面被含有季铵盐的官能团改性。
本发明的复合硅橡胶颗粒的含有季铵盐的官能团具有烃基团,且为直链(包括实质上的直链)。“基本上直链”是指在一些基团中包括支链但是这种支链不影响季铵盐的结构或官能团本身的性质的链。本发明的复合硅橡胶颗粒可具有含有一种或多种季铵盐的官能团。
硅橡胶颗粒的平均粒径优选在0.1μm至500μm的范围内,更优选在0.1μm至200μm的范围内,甚至更优选在0.1μm至100μm的范围内,并且特别优选在0.1μm至50μm的范围内。这是因为难以制备平均粒径小于上述范围的下限的硅橡胶颗粒,并且其表面难以用精细颗粒覆盖,而当平均粒径超过上述范围的上限时,所得到的复合硅橡胶颗粒在溶剂、涂料或化妆品中的分散性降低。
硅橡胶颗粒的平均粒径可使用可商购的激光衍射式粒径分布分析仪(例如由Horiba,Ltd.生产的LA-750)测定硅橡胶颗粒的水分散或乙醇分散,例如,并且可根据其中值直径(对应于50%的累积分布的粒径;50%粒径)确定。硅橡胶颗粒的形状没有特别限制,但从确保在涂料或化妆品中的优异的分散性、可大幅改善涂料的亚光或化妆品的使用感的观点出发,优选为球状或基本上球状。
JIS K6253中限定的硅橡胶颗粒的A型硬度测验器硬度优选为10至90,更优选在15至80的范围内,并且特别优选在20至70的范围内。这是因为,当A型硬度测验器硬度低于上述范围的下限时,所得复合硅橡胶颗粒的流动性降低,并且当颗粒共混入涂料时难以形成具有良好的亚光的涂料,而当A型硬度测验器硬度超过上述范围的上限时,难以增强化妆品的使用感。A型硬度测验器硬度可通过固化硅橡胶组合物以将硅橡胶颗粒形成为片状并测量橡胶片的硬度来确定。
用于形成硅橡胶颗粒的硅橡胶组合物的示例包括:加成反应可固化的硅橡胶组合物,其至少包含每分子具有至少两个烯基基团的有机聚硅氧烷、每分子具有至少两个硅键合的氢原子的有机聚硅氧烷和铂基化合物;缩合反应可固化的硅橡胶组合物,其至少包含每分子具有至少两个有机硅键合的羟基基团或可水解基团如烷氧基基团、肟基团、乙酰氧基基团或氨氧基基团的有机聚硅氧烷,每分子具有至少三个硅键合的可水解基团如烷氧基基团、肟基团、乙酰氧基基团或氨氧基基团的硅烷交联剂,以及缩合反应催化剂如有机锡化合物或有机钛化合物;以及有机过氧化物可固化的硅橡胶组合物,其至少包含每分子具有至少一个烯基基团的二有机聚硅氧烷和有机过氧化物,并且加成反应可固化的硅橡胶组合物是特别优选的。这是因为由加成反应可固化的硅橡胶组合物形成的硅橡胶颗粒适用于化妆产品等领域。
用于形成硅橡胶颗粒的方法的示例包括:使用粉碎机如研磨机粉碎通过固化上述硅橡胶组合物而获得的硅橡胶的方法;用喷雾器诸如喷雾干燥器喷射硅橡胶组合物并固化硅橡胶组合物的方法;以及将硅橡胶组合物分散在水或表面活性剂水性溶液中并固化硅橡胶组合物的方法。将硅橡胶组合物分散在水或表面活性剂水性溶液中并固化硅橡胶组合物的方法是特别优选的,因为该方法可增加在涂料或化妆品中具有优异分散性的大量球形或基本上球形颗粒存在的可能性。为了制备硅橡胶组合物的水基分散液,可使用诸如胶体磨的搅拌器或诸如超声波振动器的混合装置。在制备硅橡胶组合物的水基分散液之前,优选预先冷却硅橡胶组合物以控制其固化性。可通过在该水分散液中使硅橡胶组合物固化并且然后从水基分散液中除去水来制备硅橡胶颗粒。用于从水基分散液除去水的方法的示例为使用真空干燥机、循环热风烘箱或喷雾干燥机进行干燥的方法。
本发明的复合硅橡胶颗粒也适用于通过将颗粒分散在水基组合物中制备的分散体。为了使硅橡胶组合物作为颗粒稳定在水基分散液中,优选使用表面活性剂。表面活性剂的添加量优选为每100重量份硅橡胶组合物0.1至20重量份的范围内,并且更优选为0.5至5重量份的范围内。水的添加量优选为每100重量份硅橡胶组合物40至2,000重量份的范围内,并且特别优选40至1,000重量份的范围内。这是因为当水的添加量小于上述范围的下限时,难以形成硅橡胶组合物的均匀的水基分散液,而当水的添加量超过上述范围的上限时,硅橡胶颗粒的生产率显着降低。
本发明的复合硅橡胶颗粒可含有未交联的油组分,但其含量优选为在硅橡胶颗粒中不超过10重量%,并且更优选为不超过5重量%。这是因为当含量超过上述范围的上限时,复合硅橡胶颗粒的流动性往往降低。硅橡胶颗粒还可含有在其制造过程中使用的表面活性剂,但其含量优选不大于5重量%,并且更优选不大于1重量%。当含量超过上述范围的上限时,复合硅橡胶颗粒的流动性下降很小。
精细颗粒的表面被一个或多个具有含有季铵盐的官能团的甲硅烷基基团改性。
精细颗粒的具体示例包括:金属氧化物精细颗粒,诸如氧化硅、氧化钛、氧化铝、氧化锆和氧化锑;金属氮化物精细颗粒,诸如氮化硼和氮化铝;金属氢氧化物精细颗粒,诸如氢氧化铝和氢氧化镁;金属碳酸盐,诸如碳酸钙;金属精细颗粒,诸如铁、银、铜和金;硫化物精细颗粒、氯化物精细颗粒、倍半硅氧烷、树脂化有机硅颗粒、以及粒径非常小的硅橡胶颗粒,使得其物理性质与倍半硅氧烷的物理性质没有实质差异。这些颗粒的表面可预先通过有机硅化合物诸如有机烷氧基硅烷、有机氯硅烷、有机硅氮烷等处理成疏水性的。精细颗粒优选为无机精细颗粒,更优选金属氧化物精细颗粒,并且甚至更优选二氧化硅精细颗粒。与许多倍半硅氧烷的情况一样,颗粒可以是在精细颗粒的表面层上具有有机基团的无机精细颗粒,并且在本公开中,以这种方式在表面层上具有有机基团的精细颗粒也被认为是无机精细颗粒的一个实施方案。优选的二氧化硅精细颗粒是干燥二氧化硅,其示例包括热解法二氧化硅、沉淀二氧化硅、粉碎的二氧化硅、合成二氧化硅和球形二氧化硅,但优选具有小粒径的热解法二氧化硅。这是因为较小的粒径使得可减少复合硅橡胶颗粒的配混量并且还促进与硅化合物的缩合物的反应。热解法二氧化硅的BET比表面积不小于10m2/g,并且优选50m2/g。
精细颗粒的原生粒径为5nm至350nm,并且BET比表面积为200m2/g。在任何一种情况下,粒径优选小于硅橡胶颗粒的粒径,使得可覆盖硅橡胶颗粒。
本发明的复合硅橡胶颗粒的优选示例是其中含有季铵盐的官能团由以下通式(1)表示的物质:
(1):R1-((N+X-R2 2)-R3)a-Y
(其中R1为具有1至30个碳原子的烃基团;每个R2独立地为氢原子或具有1至4个碳原子的烃基团;每个R3独立地选自具有1至8个碳原子的烃基团;X为一价阴离子基团;a为1至4的整数;并且Y为可含有与精细颗粒的表面键合的杂原子的二价或更高价的连接基团)。
在本发明的复合硅橡胶颗粒中,R1优选选自具有1至26个碳原子,更优选7至24个碳原子,并且甚至更优选12至22个碳原子的烃基团。R1可以是直链或支链的,但优选为直链或部分直链的,并且甚至更优选为直链的。每个R2优选为氢原子或具有1或2个碳原子的烃基团,并且更优选选择甲基基团。每个R3优选选自具有1至4个碳原子并且更优选1至3个碳原子的烃基团。R3可以是直链或支链的,但优选为直链或部分直链的,并且甚至更优选直链的。X优选为卤素基团,并且更优选为氯基团。此外,a优选为1或2的整数,并且更优选1。Y为与精细颗粒的表面键合的连接基团,并且连接基团可直接或通过其它原子与另一个连接基团形成键。Y优选具有硅原子和氧原子(-O-)。
本发明的复合硅橡胶颗粒可具有一种或多种结构,其中含有季铵盐的官能团通过含硅(Si)的连接基团与精细颗粒的表面键合,并且连接基团中的硅原子和精细颗粒的表面通过氧原子(-O-)键合。
本发明的复合硅橡胶颗粒中含有的季铵盐的示例包括:十八烷基二甲基(3-三羟基甲硅烷基丙基)氯化铵、十八烷基-双(三乙氧基甲硅烷基丙基)氯化铵、N-三甲氧基甲硅烷基十一烷基-N,N,N-三正丁基溴化铵、4-(三甲氧基甲硅烷基乙基)苄基三甲基氯化铵、(苯乙烯基甲基)双(三乙氧基甲硅烷基丙基)氯化铵、N-三甲氧基甲硅烷基丙基-N,N,N-三正丁基溴化铵、N-三甲氧基甲硅烷基丙基-N,N,N-三正丁基氯化铵、N-三甲氧基甲硅烷基丙基-N,N,N-三甲基氯化铵、十四烷基(3-三甲氧基甲硅烷基丙基)氯化铵和十八烷基二甲基[3-(三甲氧基甲硅烷基)丙基]氯化铵。其中,优选N,N,N-十八烷基二甲基氯化铵或N,N,N-三甲基氯化铵。此外,更优选十八烷基二甲基[3-(三甲氧基甲硅烷基)丙基]氯化铵、N-三甲氧基甲硅烷基丙基-N,N,N-三甲基氯化铵或N-三乙氧基甲硅烷基丙基-N,N,N-三甲基氯化铵。
在本发明的复合硅橡胶颗粒中,含有季铵盐的官能团的含量优选为整体复合硅橡胶颗粒的重量的0.1重量%至10重量%。该含量更优选为0.3重量%至9.0重量%,甚至更优选为0.3重量%至8.0重量%,并且甚至更优选为0.6重量%至7.5重量%。当含量低于上述范围的下限时,复合硅橡胶颗粒的特征几乎不显现,并且诸如抗微生物活性或毛发粘附性的特征不容易表现出来。另一方面,当含量超过上述范围的上限时,复合硅橡胶颗粒的流动性往往降低。
这些值是根据原料的反应率算出的值,并且当在诸如二氧化硅的精细颗粒的表面存在过量的反应性官能团时,可在颗粒被全部量修改的假设下算出的化学计量值来确定这些值。下文中将应用相同的假设。
含有季铵盐的由以下通式(1')表示的官能团在本发明的复合硅橡胶颗粒中的重量比(官能化甲硅烷基基团/精细颗粒)优选为0.03至0.70,更优选为0.05至0.60,并且甚至更优选为0.10至0.50,
通式(1’):R1-((N+X-R2 2)-R3)a-Y’
(其中R1至R3、X和a与通式(1)中的相同;并且Y′为具有与精细颗粒表面上的氧原子(-O-)键合的硅原子的连接基团)。
这是因为当重量比小于上述范围的下限时,复合硅橡胶颗粒的流动性往往降低,并且当重量比超过上述范围的上限时,复合硅橡胶颗粒的除了流动性之外的特征可能表现不出来。
本发明的复合硅橡胶颗粒中的精细颗粒的含量(除了通式(1′)中的官能团的重量之外)为整个复合硅橡胶的0.5重量%至10重量%。含量更优选为0.5重量%至8.0重量%,并且甚至更优选为1.0重量%至6.0重量%。这是因为当含量小于上述范围的下限时,复合硅橡胶颗粒的流动性不易改善,并且当含量超过上述范围的上限时,存在颗粒将以从表面除去而不是在复合硅橡胶颗粒的表面上的状态存在的更高的可能性。
抗微生物活性表示相对于微生物(包括一种或多种类型的微生物或多细胞生物诸如藻类、苔藓或蕨类,例如,其选自广泛范围的微生物诸如细菌、真菌、酵母和藻类)的杀菌活性,当本发明的复合硅橡胶颗粒存在于物体上、材料中或物体中时,抗微生物活性抑制微生物的生长。抗微生物活性也是指由于这些生物体对外部物体表面的固定的不利影响而丧失了这些生物体稳定存活的能力。此外,具有抗微生物活性的复合硅橡胶颗粒也可具有抗病毒作用。
本发明的复合硅橡胶颗粒的甲醇含量不大于1,000ppm。含量优选不大于100ppm,更优选不大于10ppm,并且最优选不大于1ppm。这是因为当甲醇被包含在化妆产品或皮肤外用制剂中的量大于一定量时,甲醇对人体有害。
下文中将详细描述作为本发明之一的复合硅橡胶颗粒的制造方法。
本发明的复合硅橡胶颗粒的制造方法的第一实施方案至少具有以下步骤:
步骤1:通过使用机械力混合精细颗粒和硅橡胶颗粒来形成复合硅橡胶颗粒;以及
步骤2:用具有含有季铵盐的官能团且能够在精细颗粒的表面上形成化学键的硅化合物对步骤1中得到的复合硅橡胶颗粒的精细颗粒的表面进行改性。
在该第一实施方案中,分散性可通过使用机械力混合精细颗粒和硅橡胶颗粒以用精细颗粒覆盖硅橡胶颗粒的表面并形成复合硅橡胶颗粒得到增强。接下来,用具有含有季铵盐的官能团且能够在精细颗粒的表面上形成化学键的硅化合物对所得的复合硅橡胶颗粒的精细颗粒的表面进行改性。这使得可用具有硅化合物的官能团改性精细颗粒的表面。步骤1和2也可同时执行。
第二实施方案至少具有以下步骤:
步骤1:用具有含有季铵盐的官能团且能够在精细颗粒的表面上形成化学键的硅化合物对精细颗粒的表面进行改性;以及
步骤2:通过使用机械力将步骤1中得到的精细颗粒与硅橡胶颗粒混合来形成复合硅橡胶颗粒。
与第一实施方案相比之下,首先仅对精细颗粒的表面进行改性使得可对精细颗粒进行可选的处理而不会使硅橡胶颗粒靶向,这使得更容易控制处理。此外,可减少生产复合硅橡胶颗粒所需的工时和成本。
结果,可通过用精细颗粒覆盖硅橡胶颗粒的表面来增强分散性,以形成复合硅橡胶颗粒。具有季铵盐的硅化合物的官能团可改性精细颗粒的表面,并且当产生甲醇时,易于处理它们的处理。此外,通过预先处理精细颗粒的表面,可促进作为任选工艺的热处理,并减少制造所需的工时和成本。
本发明的复合硅橡胶颗粒的制造方法还可包括如下步骤:在上述第一实施方案和第二实施方案中在对精细颗粒的表面进行改性的步骤之后,将复合硅橡胶颗粒的甲醇含量降低至不大于1,000ppm。具体地,这可通过在65℃或更高的温度下加热精细颗粒来实现。
硅橡胶颗粒的表面被含有季铵盐的硅化合物和精细颗粒的水解/缩合反应产物所覆盖。在该方法中,二氧化硅精细颗粒的表面用具有含有季铵盐的官能团或其(部分)缩合物的硅化合物处理,并且该反应通过加热进一步进行以获得缩合物与精细颗粒的反应产物。然后将精细颗粒的反应产物与硅橡胶颗粒混合以制备复合硅橡胶颗粒。混合装置与上述混合装置相同,并且由于干法简便化,也优于湿法优选干法。
在该制造方法中,用精细颗粒覆盖硅橡胶颗粒的表面的步骤可使用湿法或干法进行,但从简便化的观点出发,优选干式处理法。用于混合这些组分的装置不受限制,并且它们的示例包括Henschel混合机和超级混合机。混合时的温度没有特别限制,并且例如可在室温下进行混合。由于流动性差的硅橡胶颗粒在精细颗粒粘附于其表面时表现出流动性,所以必须通过观察其状态的变化适当地确定混合时间。第二实施方案的制造方法的优点在于,在制造过程中存在很少的原料损失。
在该制造方法中,对精细颗粒表面进行改性的步骤是指含有季铵盐的硅化合物与精细颗粒形成化学键的步骤。在该步骤中,可使用与覆盖硅橡胶颗粒表面的步骤相同的工艺。这是因为,由于硅化合物本身的反应性高,所以当硅化合物与精细颗粒接触时,会诱发与存在于精细颗粒的表面上的反应性基团的反应。在表面改性的一个实施方案中,具有硅烷的硅化合物(或其(部分)缩合物)与其表面上具有羟基基团的精细颗粒反应。在本发明的另一个实施方案中,如工作例中所述,二氧化硅表面上的硅烷醇基团和硅化合物(或其缩合物)反应以在二氧化硅颗粒的表面上产生反应产物。
用于制造本发明的复合硅橡胶颗粒的具有季铵盐官能团的硅化合物的部分可(部分地)进行水解缩合。硅化合物优选具有烷氧基基团、羟基基团、烷基基团或亚烷基基团(其中至少一个基团为烷氧基基团),并且更优选具有甲氧基基团或乙氧基基团以促进与精细颗粒(或硅橡胶)的水解缩合反应。硅化合物优选具有十三烷基基团、十四烷基基团、十五烷基基团、十六烷基基团、十七烷基基团、十八烷基基团、十九烷基基团、二十烷基基团、二十一烷基基团、二十二烷基基团、二十三烷基基团、二十四烷基基团、二十五烷基基团或二十六烷基基团。其中,从与硅橡胶颗粒的相容性和对其它组分的化学效果的最小化的观点出发,硅化合物优选具有十六烷基基团、十七烷基基团、十八烷基基团、十九烷基基团或二十烷基基团。
由于水解缩合,硅化合物的一些基团可与另一硅化合物化学键合而不是与精细颗粒化学键合。
此外,硅化合物的优选示例由以下通式(2)表示:
(2):R4-((N+Z-R5 2)-R6)b-R7-SiR8 3
(其中R4为具有1至30个碳原子的烃基团;每个R5为氢原子或具有1至4个碳原子的烃基团;每个R6为具有1至8个碳原子的烃基团;R7为二价有机基团或杂原子;每个R8为烷氧基基团、羟基基团、烷基基团或亚烷基基团(其中至少一个R8为烷氧基基团);Z为一价阴离子基团;并且b为1至4的整数)。
在本发明的复合硅橡胶颗粒中,R4优选选自具有1至26个碳原子,更优选7至24个碳原子,并且甚至更优选12至22个碳原子的烃基团。R4可以是直链或支链的,但优选为直链或部分直链的,并且甚至更优选为直链的。每个R5优选为氢原子或具有1或2个碳原子的烃基团,并且更优选选择甲基基团。每个R6优选选自具有1至4个碳原子并且更优选1至3个碳原子的烃基团。R6可以是直链或支链的,但优选为直链或部分直链的,并且甚至更优选为直链的。R7优选为二价有机基团或杂原子,并且基本上为直链的。每个R8为烷氧基基团、羟基基团、烷基基团或亚烷基基团(其中至少一个R8是烷氧基基团);Z优选为卤素基团,并且更优选为氯基团。此外,b优选为1或2的整数,并且更优选1。
季铵盐硅化合物的示例包括:十八烷基二甲基(3-三羟基甲硅烷基丙基)氯化铵、十八烷基-双(三乙氧基甲硅烷基丙基)氯化铵、N-三甲氧基甲硅烷基十一烷基-N,N,N-三正丁基溴化铵、4-(三甲氧基甲硅烷基乙基)苄基三甲基氯化铵、(苯乙烯基甲基)双(三乙氧基甲硅烷基丙基)氯化铵、N-三甲氧基甲硅烷基丙基-N,N,N-三正丁基溴化铵、N-三甲氧基甲硅烷基丙基-N,N,N-三正丁基氯化铵、N-三甲氧基甲硅烷基丙基-N,N,N-三甲基氯化铵、十四烷基(3-三甲氧基甲硅烷基丙基)氯化铵和十八烷基二甲基[3-(三甲氧基甲硅烷基)丙基]氯化铵。其中,优选N,N,N-十八烷基二甲基氯化铵或N,N,N-三甲基氯化铵。此外,甚至更优选十八烷基二甲基[3-(三甲氧基甲硅烷基)丙基]氯化铵、N-三甲氧基甲硅烷基丙基-N,N,N-三甲基氯化铵或N-三乙氧基甲硅烷基丙基-N,N,N-三甲基氯化铵。
在本发明的复合硅橡胶颗粒中,具有季铵盐官能团的硅化合物的含量优选为复合硅橡胶颗粒的重量的0.1重量%至10重量%。该含量更优选为0.3重量%至9.0重量%,甚至更优选为0.3重量%至8.0重量%,并且甚至更优选为0.6重量%至7.5重量%。当含量低于上述范围的下限时,复合硅橡胶颗粒的特征可能不显现,并且诸如抗微生物活性或毛发粘附等特征也不容易表现出来。另一方面,当含量超过上述范围的上限时,复合硅橡胶颗粒的流动性往往降低。
在本发明的复合硅橡胶颗粒的制造方法中,将精细颗粒与具有季铵盐官能团的硅化合物混合时的重量比(官能化硅烷/精细颗粒)优选为0.03至0.70,更优选为0.05至0.60,并且甚至更优选为0.10至0.50。这是因为当重量比小于上述范围的下限时,复合硅橡胶颗粒的流动性往往降低,并且当二氧化硅颗粒超过上述范围的上限时,复合硅橡胶颗粒的除了流动性之外的特征不易表现出来。
在本发明的复合硅橡胶颗粒的制造方法中,精细颗粒的含量为整个复合硅橡胶颗粒的0.5重量%至10重量%。该含量更优选为0.5重量%至8.0重量%,并且甚至更优选为1.0重量%至6.0重量%。这是因为当含量小于上述范围的下限时,复合硅橡胶颗粒的流动性不易改善,并且当含量超过上述范围的上限时,存在颗粒将以从表面除去而不是在复合硅橡胶颗粒表面上的状态存在的更高的可能性。
通过在本发明的制造方法中容许加热步骤,本发明的复合硅橡胶颗粒的甲醇含量不大于1,000ppm。含量比优选不大于100ppm,更优选不大于10ppm,并且最优选不大于1ppm。
本发明的复合硅橡胶颗粒可用作用于化妆产品的组合物或皮肤局部剂型。
本发明的化妆品含有上述复合硅橡胶颗粒。这种化妆品的示例包括:洗涤化妆品,诸如皂、沐浴露和面霜;基础化妆产品,诸如皮肤乳液、霜膏、乳液和面膜;基础化妆化妆品,诸如粉饼和粉底;唇膏、胭脂、眼睛/睫毛化妆品,诸如眼影、眼线和睫毛膏;化妆化妆品,诸如指甲油;毛发化妆品,诸如洗发剂、护发液、理发剂、生发剂、毛发生长促进剂和染发剂;芳香剂化妆品,诸如香水和古龙水;牙膏;沐浴准备剂;以及特殊化妆品,诸如脱毛产品、剃须膏、止汗剂/除臭剂和防晒产品。该化妆品的剂型的示例包括:水性液体、油性液体、乳液、霜膏、泡沫、半固体、固体和粉末。该化妆品也可以喷雾的形式使用。
在该化妆品中,上述复合硅橡胶颗粒的含量优选为在化妆品中的0.5重量%至99.0重量%的范围内,并且特别优选为1.0重量%至95重量%的范围内。这是因为,当上述复合硅橡胶颗粒的含量超过上述上限值时,则作为化妆品的效果丧失,并且当含量低于上述范围的下限值时,则难以增强化妆品的使用感。
作为化妆品原料,也可使用以下段落和此后中描述的化妆产品组分作为介质(水性介质或油基介质),将复合硅橡胶颗粒分散到水相或油相中。作为水性介质,可使用水,诸如纯化水、离子交换水、碱离子水、深水、波浪水和天然水;低级醇,诸如乙醇、丙醇和异丙醇;以及可与水混溶的水性溶剂,诸如多元醇,包括甘油、1,3-丁二醇、异戊二醇和二丙二醇。
油基介质(油剂)的示例包括有机硅油、烃油、高级脂肪酸、高级醇、酯油(包括油和脂肪)、醚油、矿物油和氟油。其中,从使用感的角度来看,有机硅油、烃油和酯油是更优选的。具体示例包括:有机硅油,诸如二甲基聚硅氧烷、甲基氢聚硅氧烷、甲基苯基聚硅氧烷、聚醚改性的有机聚硅氧烷、氟代烷基/聚氧化烯共改性的有机聚硅氧烷、烷基改性的有机聚硅氧烷、端基改性的有机聚硅氧烷、氟改性的有机聚硅氧烷、氨基封端聚二甲基硅氧烷、氨基改性的有机聚硅氧烷、丙烯酰基有机硅和三甲基甲硅烷氧基硅酸;烃油,诸如液状石蜡、凡士林和角鲨烷;以及酯油,诸如肉豆蔻酸肉豆蔻酯、月桂酸己酯、油酸癸酯、肉豆蔻酸异丙酯、二甲基辛酸己基癸酯、甘油单硬脂酸、邻苯二甲酸二乙酯、乙二醇单硬脂酸酯、辛基氧代硬脂酸酯、异壬酸异壬酯和异壬酸异十三烷基酯。可使用一种或多种类型的油剂。从使用感和储存稳定性的观点出发,油剂相对于用于本发明的全部油包水乳液化妆品的含量优选为10重量%至50重量%,并且更优选为20重量%至40重量%。
在化妆品中通常使用的以下其它组分可加入到本发明的化妆品中,前提条件是此类组分不会抑制本发明的效果:水、着色剂、醇、水溶性聚合物、成膜剂、油剂、油溶性胶凝剂、有机改性的粘土矿物质、表面活性剂、树脂、盐、保湿剂、防腐剂、抗微生物剂、抗氧化剂、pH调节剂、螯合剂、清新剂、抗炎剂、美肤组分(亮肤剂、细胞活化剂、皮肤粗糙改善剂、循环促进剂、收敛剂、抗皮脂溢剂等)、维生素、氨基酸、核酸、激素、包合物等;生物活性物质、药物活性成分和芳香剂。然而,添加剂不特别限定于这些。除了水之外,这些化妆品组分中的每一种的含量在化妆品中优选在0.5重量%至99.0重量%的范围内,并且特别优选在1.0重量%至95重量%的范围内。这是因为当化妆品组分中之一的含量超过上述范围的上限时,作为化妆品的使用感不是优选的。当添加时,如果含量小于上述范围的下限,则诸如增强化妆品使用感的效果变得难以实现。此处包括日本未经审查的专利申请公布No.2015-113303A中公开的化妆品组分及它们的配混量供参考。
水是清洁且不含对人体有害的组分,并且其示例包括自来水、纯化水、矿泉水和深海水。当本发明的化妆品是水基时,在不损害本发明效果的范围内,水溶性附加组分可任选地配混到水相中。此外,为了实现增强化妆品的储存稳定性等的目标,也可适当地配混公知的pH调节剂、防腐剂、抗微生物剂、抗氧化剂。
着色剂的示例包括:无机红色颜料,诸如氧化铁红、氧化铁、氢氧化铁和钛酸铁;无机棕色颜料,诸如γ-氧化铁;无机黄色颜料,诸如氧化铁黄和赭色;无机黑色颜料,诸如氧化铁黑和炭黑;无机紫色颜料,诸如锰紫和钴紫;无机绿色颜料,诸如氢氧化铬、氧化铬、氧化钴和钛酸钴;无机蓝色颜料,诸如铁蓝和群青;有机颜料,诸如通过耙焦油基着色物质制备的颜料,诸如红色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号和橙色207号,以及通过耙天然着色物质制备的颜料,诸如胭脂红酸、紫胶酸、红花素、巴西苏木素、和藏红花素;珠光颜料,诸如钛氧化物包覆的云母、钛云母、氧化铁处理的钛云母、氧化钛包覆的云母、氯氧化铋、氧化钛包覆的氯氧化铋、氧化钛包覆的滑石粉、鱼鳞和氧化钛包覆的有色云母;以及金属粉末,诸如铝、金、银、铜、铂和不锈钢。
这些着色剂优选进行防水处理。也可使用将这些着色剂彼此组合而制备的组合物,或者用一般的油剂、有机硅化合物、氟化合物或表面活性剂进行表面处理的组合物,并且根据需要可使用一种或多种类型。
此类防水处理的示例包括其中着色剂用各种防水剂诸如辛基硅烷处理的处理。其具体示例包括有机硅氧烷处理,诸如甲基氢聚硅氧烷处理、有机硅树脂处理、硅橡胶处理、丙烯酰基有机硅处理、氟化有机硅处理等;金属皂处理,诸如硬脂酸锌处理等;硅烷处理,诸如硅烷偶联剂处理、烷基硅烷处理等等;氟化合物处理,诸如全氟烷基硅烷处理、全氟烷基磷酸酯处理、全氟聚醚处理等等;氨基酸处理,诸如N-月桂酰基-L-赖氨酸处理等;油剂处理,诸如角鲨烷处理等;以及丙烯酰处理,诸如丙烯酸烷基酯处理等等。可组合使用上述一种或多种处理。
选自低级醇、糖醇和高级醇中的一种或多种可用作醇。具体示例包括:低级醇,诸如乙醇和异丙醇;糖醇,诸如山梨糖醇和麦芽糖;以及高级醇,诸如月桂醇、肉豆蔻醇、棕榈醇、硬脂醇、山嵛醇、十六烷醇、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、POE胆固醇醚、单硬脂基甘油醚(鲨肝醇)和单油基甘油醚(鲨油醇)等。
为了增强化妆品的使用感的目的,将水溶性聚合物配混,并且任何两性、阳离子、阴离子、非离子或水溶胀性粘土矿物可用作水性聚合物,只要它是普通化妆品中使用的物质,并且也可组合使用一种或多种水性聚合物。这些水性聚合物对含水组分具有增稠作用,并且因此可用于获得凝胶状含水化妆品、油包水乳液化妆品或水包油乳液化妆品。一些水溶性聚合物也可用作表面活性剂。
两性水溶性聚合物的具体示例包括:两性淀粉、二甲基二烯丙基氯化铵衍生物(例如,丙烯酰胺、丙烯酸和二甲基二烯丙基氯化铵的共聚物,以及丙烯酸和二甲基二烯丙基氯化铵的共聚物)和甲基丙烯酸衍生物(例如聚甲基丙烯酰基乙基二甲基甜菜碱、N-甲基丙烯酰氧基乙基N,N-二甲基铵-α-甲基羧基甜菜碱/甲基丙烯酸烷基酯共聚物等)。
阳离子水溶性聚合物的示例包括:季氮改性的多糖(例如阳离子改性的纤维素、阳离子改性的羟乙基纤维素、阳离子改性的瓜耳胶、阳离子改性的刺槐豆胶、阳离子改性的淀粉等);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与丙烯酰胺的共聚物、多氯化二甲基亚甲基哌啶鎓等);乙烯基吡咯烷酮衍生物(例如,乙烯基吡咯烷酮和二甲基氨基乙基甲基丙烯酸的共聚物盐、乙烯基吡咯烷酮和甲基丙烯酰胺丙基三甲基氯化铵的共聚物、乙烯基吡咯烷酮和甲基乙烯基咪唑鎓氯化物的共聚物等);甲基丙烯酸衍生物(例如,甲基丙烯酰基乙基二甲基甜菜碱、甲基丙烯酰基乙基三甲基氯化铵和甲基丙烯酸2-羟基乙酯的共聚物,甲基丙烯酰基乙基二甲基甜菜碱、甲基丙烯酰基乙基三甲基氯化铵和甲氧基聚乙二醇甲基丙烯酸酯的共聚物等)。
阴离子水溶性聚合物的示例包括:聚丙烯酸或其碱金属盐,聚甲基丙烯酸或其碱金属盐,透明质酸或其碱金属盐,乙酰化透明质酸或其碱金属盐,以及脂族羧酸(如甲基乙烯基醚/马来酸酐共聚物的水解产物或其金属盐的水溶性聚合物),羧甲基纤维素或其碱金属盐,甲基乙烯基醚/马来酸半酯共聚物,丙烯酸树脂链烷醇胺溶液和羧乙烯基聚合物。
非离子水溶性聚合物的示例包括:天然聚合物化合物,诸如聚乙烯吡咯烷酮、高度聚合的聚乙二醇、乙烯基吡咯烷酮/乙酸乙烯酯共聚物、乙烯基吡咯烷酮/甲基丙烯酸二甲氨基乙酯共聚物、乙烯基己内酰胺/乙烯基吡咯烷酮/甲基丙烯酸二甲氨基乙酯共聚物,其纤维素或衍生物(例如甲基纤维素、乙基纤维素、羟乙基纤维素、羟丙基纤维素和羧甲基纤维素),角蛋白和胶原蛋白或其衍生物,藻酸钙,支链淀粉,琼脂,明胶,罗望子多糖,黄原胶,角叉菜胶,高甲氧基果胶,低甲氧基果胶,瓜尔胶,果胶,阿拉伯树胶,结晶纤维素,阿拉伯半乳聚糖,刺梧桐胶,黄蓍胶,海藻酸,白蛋白,酪蛋白,凝胶多糖,结冷胶,葡聚糖,木瓜籽胶,西黄蓍胶,几丁质/壳聚糖衍生物,淀粉(大米,玉米,土豆,小麦等)以及角蛋白和胶原蛋白或其衍生物。
水溶胀性粘土矿物是无机水溶性聚合物,它是一种具有三层结构的含胶体硅酸铝;其示例通常包括由下式(A)表示的组合物:
(X,Y)2-3(Si,Al)4O10(OH)2Z1/3-nH2O(A)
(其中X为Al、Fe(III)、Mn(III)或Cr(III);Y为Mg、Fe(II)、Ni、Zn或Li;并且Z为K、Na或Ca)。此类无机水溶性聚合物的具体示例包括:膨润土、蒙脱石、贝得石、绿脱石、皂石、锂蒙脱石、硅酸铝镁和硅酸酐,并且它们可用作天然产物或合成产物。
有机硅油的示例包括:环状有机聚硅氧烷,诸如六甲基环三硅氧烷(D3)、八甲基环四硅氧烷(D4)、十甲基环戊硅氧烷(D5)、十二甲基环六硅氧烷(D6)、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-乙烯基氧基丙基)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。直链有机聚硅氧烷的示例包括:两个分子末端均被三甲基甲硅烷氧基基团封端的二甲基聚硅氧烷(具有低粘度诸如2cst或6cst的二甲基有机硅至具有高粘度诸如1,000,000cst的二甲基有机硅)、有机氢聚硅氧烷、两个分子末端均被三甲基甲硅烷氧基基团封端的甲基苯基聚硅氧烷、两个分子末端均被三甲基甲硅烷氧基基团封端的甲基苯基硅氧烷与二甲基硅氧烷的共聚物、两个分子末端均被三甲基甲硅烷氧基基团封端的二苯基聚硅氧烷、两个分子末端均被三甲基甲硅烷氧基基团封端的二苯基硅氧烷与二甲基硅氧烷的共聚物、三甲基五苯基三硅氧烷、苯基(三甲基甲硅烷氧基)硅氧烷、两个分子末端均被三甲基甲硅烷氧基基团封端的甲基烷基聚硅氧烷、两个分子末端均被三甲基甲硅烷氧基基团封端的甲基烷基硅氧烷与二甲基聚硅氧烷的共聚物、两个分子末端均被三甲基甲硅烷氧基基团封端的甲基(3,3,3-三氟丙基)硅氧烷与二甲基硅氧烷的共聚物、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、三三甲基甲硅烷氧基甲基硅烷、三三甲基甲硅烷氧基烷基硅烷、四三甲基甲硅烷氧基硅烷、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、高级烷氧基改性的有机硅、高级脂肪酸改性的有机硅等。
烃油的示例包括:液体石蜡、轻质液体异链烷烃、重质液体异链烷烃、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、纯地蜡、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、聚异戊二烯等等。
酯油的示例包括:辛酸己基癸酯、辛酸鲸蜡醇酯、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、油酸油醇酯、油酸癸酯、肉豆蔻酸辛基十二烷醇酯、二甲基辛酸己基癸酯、乳酸鲸蜡醇酯、乳酸肉豆蔻酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、乙酸羊毛脂酯、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酯/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-庚基十一烷醇酯、二异硬脂醇苹果酸酯、氢化蓖麻油单硬脂酸酯、N-烷基二醇单异硬脂酸酯、异硬脂酸辛基十二烷醇酯、异硬脂酸异丙酯、异硬脂酸异鲸蜡醇酯、乙二醇二-2-乙基己酸酯、2-乙基己酸鲸蜡醇酯、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、硬脂酸异鲸蜡醇酯、癸二酸二异丙酯、癸二酸二-2-乙基己酯、癸二酸二乙酯、癸二酸二辛酯、癸二酸二丁基辛酯、棕榈酸鲸蜡醇酯、棕榈酸辛基十二烷酯、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-庚基十一烷酯、胆甾醇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-月桂酰基-L-谷氨酸2-辛基十二烷酯、二(胆甾醇/山嵛醇/辛基十二烷醇)N-月桂酰基-L-谷氨酸酯、二(胆甾醇/辛基十二烷醇)N-月桂酰基-L-谷氨酸酯、二(植物甾醇/山嵛醇/辛基十二烷醇)N-月桂酰基-L-谷氨酸酯、二(植物甾醇/辛基十二烷醇)N-月桂酰基-L-谷氨酸酯、N-月桂酰基肌氨酸异丙酯、二异硬脂醇苹果酸酯、新戊二醇二辛酸酯、新戊酸异癸酯、新戊酸异十三烷酯、异硬脂醇新戊酸酯、异壬酸异壬酯、异壬酸异十三烷基酯、异壬酸辛酯、异壬酸十三烷基酯、二乙基戊二醇二新戊酸酯、甲基戊二醇二新戊酸酯、新癸酸辛基十二烷酯、2-丁基-2-乙基-1,3-丙二醇二辛酸酯、季戊四醇四辛酸酯、季戊四醇氢化松香、季戊四醇三乙基己酸酯、二季戊四醇(羟基硬脂酸酯/硬脂酸酯/松脂酸酯)、聚甘油四异硬脂酸酯、聚甘油-10九异硬脂酸酯、聚甘油-8十(芥酸酯/异硬脂酸酯/蓖麻醇酸酯)、(己基癸酸/癸二酸)二甘油基低聚酯、乙二醇二硬脂酸酯(glycol distearate)(乙二醇二硬脂酸酯(ethylene glycol distearate))、二聚亚油酸二异丙酯、二异硬脂醇二聚亚油酸酯、二(异硬脂醇/植物甾醇)二聚亚油酸酯、(植物甾醇/山嵛醇)二聚亚油酸酯、(植物甾醇/异硬脂醇/鲸蜡醇/硬脂醇/山嵛醇)二聚亚油酸酯、二聚亚油醇二聚亚油酸酯、二聚亚油醇二异硬脂酸酯、二聚亚油醇氢化松香浓缩物、二聚二亚油酸可固化蓖麻油、羟基烷基二聚亚油醇醚、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、甘油三(辛酸酯/癸酸酯)、甘油三(辛酸酯/癸酸酯/肉豆蔻酸酯/硬脂酸酯)、氢化松香甘油三酯(氢化酯胶)、松香甘油三酯(酯胶)、甘油山嵛酸酯二十烷二酸酯(glyceryl behenateeicosane dioate)、二-2-庚基十一烷酸甘油酯、二甘油肉豆蔻酸酯异硬脂酸酯、胆甾醇乙酸酯、胆甾醇壬酸酯、胆甾醇硬脂酸酯、胆甾醇异硬脂酸酯、胆甾醇油酸酯、胆甾醇12-羟基硬脂酸酯、澳洲坚果油脂肪酸的胆甾醇酯、澳洲坚果油脂肪酸的植物甾醇酯、植物甾醇异硬脂酸酯、软羊毛脂脂肪酸的胆甾醇酯、硬羊毛脂脂肪酸的胆甾醇酯、长链支链脂肪酸的胆甾醇酯、长链α-羟基脂肪酸的胆甾醇酯、蓖麻醇酸辛基十二烷酯、羊毛脂脂肪酸的辛基十二烷酯、芥酸辛基十二烷酯、异硬脂酸可固化蓖麻油、鳄梨脂肪酸的乙酯和羊毛脂脂肪酸的异丙酯等。
天然动物或植物脂肪和油以及半合成脂肪和油的示例包括:鳄梨油、亚麻籽油、扁桃仁油、水蜡树蜡、紫苏子油、橄榄油、可可脂、木棉蜡、榧子油、卡洛巴蜡、肝油、小烛树蜡、牛脂、牛脚油、牛骨脂、氢化牛脂、杏仁油、鲸蜡、氢化油、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、牛油树脂、中国桐油、肉桂油、霍霍巴蜡、橄榄角鲨烷、紫胶蜡、海龟油、大豆油、茶籽油、山茶油、月见草油、玉米油、猪油、油菜籽油、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、氢化蓖麻油、蓖麻油脂肪酸甲酯、向日葵油、葡萄油、杨梅蜡、霍霍巴油、氢化霍霍巴酯、澳洲坚果油、蜂蜡、貂油、棉籽油、棉蜡、日本蜡、日本蜡核油、蒙旦蜡、椰子油、氢化椰子油、三椰子油脂肪酸甘油酯、羊脂、花生油、羊毛脂、液体羊毛脂、还原的羊毛脂、羊毛脂醇、硬羊毛脂、羊毛脂乙酸酯、羊毛脂脂肪酸异丙酯、POE羊毛脂醇醚、POE羊毛脂醇乙酸酯、羊毛脂脂肪酸聚乙二醇、POE氢化羊毛脂醇醚、蛋黄油等。本文中,“POE”意指“聚氧乙烯”。
高级脂肪酸的示例包括:月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、山嵛酸、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-羟基硬脂酸等等。
高级醇的示例包括:月桂醇、肉豆蔻醇、棕榈醇、硬脂醇、山嵛醇、十六烷醇、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、POE胆固醇醚、单硬脂基甘油醚(鲨肝醇)、单油基甘油醚(鲨油醇)等等。
氟基油剂的示例包括:全氟聚醚,全氟萘烷,全氟辛烷等,并且可根据需要使用这些油剂中的一种或多种类型。
油溶性胶凝剂的示例包括:金属皂,诸如硬脂酸铝、硬脂酸镁和肉豆蔻酸锌;氨基酸衍生物,诸如N-月桂酰基-L-谷氨酸和α,γ-二正丁胺;糊精脂肪酸酯,诸如糊精棕榈酸酯、糊精硬脂酸酯和糊精2-乙基己酸酯棕榈酸酯;蔗糖脂肪酸酯,诸如蔗糖棕榈酸酯和蔗糖硬脂酸酯;低聚果糖脂肪酸酯,诸如菊糖硬脂酸酯以及低聚果糖-2-乙基己酸酯,山梨糖醇的亚苄基衍生物,诸如单亚苄基山梨糖醇和二亚苄基山梨糖醇;以及有机改性粘土矿物,诸如二甲基苄基十二烷基铵蒙脱石粘土和二甲基双十八烷基铵蒙脱石粘土。可根据需要使用这些试剂中一种或多种类型。
选自有机硅基表面活性剂、阴离子表面活性剂、阳离子表面活性剂、非离子表面活性剂、两性表面活性剂和半极性表面活性剂中的一种或多种类型的表面活性剂可组合用作表面活性剂。
有机硅基表面活性剂经常用作油剂乳液或洗涤用组分或用于粉末分散或表面处理的组分,并且典型的示例包括;聚甘油改性的有机硅、甘油改性的有机硅、糖改性的有机硅、氟聚醚改性的有机硅、聚醚改性的有机硅、羧酸改性的有机硅、糖改性的有机硅、直链有机硅/聚醚嵌段共聚物(聚有机硅-13等)和长链烷基/聚醚共改性的有机硅。
阴离子表面活性剂的示例包括:饱和或不饱和脂肪酸盐(如月桂酸钠、硬脂酸钠、油酸钠、亚麻酸钠等);烷基硫酸盐;烷基苯磺酸(例如己基苯磺酸、辛基苯磺酸、十二烷基苯磺酸等等)及其盐;聚氧化烯烷基醚硫酸盐;聚氧化烯烯基醚硫酸盐;聚氧乙烯烷基硫酸盐;烷基磺基琥珀酸盐;聚氧化烯磺基琥珀酸盐;聚氧化烯烷基苯基醚硫酸盐;烷基磺酸盐;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盐;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;烷基磺酸盐;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;和精氨酸衍生物。盐的示例包括碱金属盐,诸如钠盐等;碱土金属盐,诸如镁盐等;链烷醇胺盐,诸如三乙醇胺盐等,以及铵盐。
阳离子表面活性剂的示例包括: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、鲸蜡基三甲基氯化铵、牛油烷基三甲基氯化铵、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)油烯基甲基氯化铵(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、羊毛脂衍生物季铵盐、二乙氨基乙基硬脂酰胺、二甲基氨基丙基硬脂酰胺、山嵛酰胺丙基二甲基羟丙基氯化铵、氯化硬脂酰氧乙基氨基甲酰基甲基吡啶鎓、氯化鲸蜡基吡啶鎓、氯化妥尔油烷基苄基羟乙基咪唑鎓和苄基铵盐。
非离子表面活性剂的示例包括:聚甘油二异硬脂酸酯、二甘油基聚羟基硬脂酸酯、异硬脂基甘油醚、聚氧化烯醚、聚氧化烯烷基醚、聚氧化烯脂肪酸酯、聚氧化烯脂肪酸二酯、聚氧化烯树脂酸酯、聚氧化烯(氢化)蓖麻油、聚氧化烯烷基酚、聚氧化烯烷基苯基醚、聚氧化烯苯基苯基醚、聚氧化烯烷基酯、失水山梨醇脂肪酸酯、聚氧化烯失水山梨醇烷基酯、聚氧化烯失水山梨醇脂肪酸酯、聚氧化烯山梨醇脂肪酸酯、聚氧化烯甘油脂肪酸酯、聚甘油烷基醚、聚甘油脂肪酸酯、蔗糖脂肪酸酯、脂肪酸烷醇酰胺、烷基葡糖苷、聚氧化烯脂肪酸双苯醚、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和氟基表面活性剂。
两性表面活性剂的示例包括咪唑啉型、酰胺基甜菜碱型、烷基甜菜碱型、烷基酰胺基甜菜碱型、烷基磺基甜菜碱型、酰胺基磺基甜菜碱型、羟基磺基甜菜碱型、羰基甜菜碱型、磷酸酯甜菜碱型、氨基羧酸型和酰胺基氨基酸型两性表面活性剂。具体地,咪唑啉型两性表面活性剂,诸如2-十一烷基-N,N,N-(羟乙基羧基甲基)-2-咪唑啉钠、2-椰油酰基-2-咪唑啉鎓氢氧化物-1-羧基乙氧基二钠盐等;烷基甜菜碱型两性表面活性剂,诸如月桂基二甲基氨基乙酸甜菜碱、肉豆蔻基甜菜碱等;酰胺基甜菜碱型两性表面活性剂,诸如椰子油脂肪酸酰胺基丙基二甲氨基乙酸甜菜碱、棕榈仁油脂肪酸酰胺基丙基二甲氨基乙酸甜菜碱、牛脂脂肪酸酰胺基丙基二甲氨基乙酸甜菜碱、硬化牛脂脂肪酸酰胺基丙基二甲氨基乙酸甜菜碱、月桂酸酰胺基丙基二甲氨基乙酸甜菜碱、肉豆蔻酸酰胺基丙基二甲氨基乙酸甜菜碱、棕榈酸酰胺基丙基二甲氨基乙酸甜菜碱、硬脂酸酰胺基丙基二甲氨基乙酸甜菜碱、油酸酰胺基丙基二甲氨基乙酸甜菜碱等;烷基磺基甜菜碱型两性表面活性剂,诸如椰子油脂肪酸二甲基磺基丙基甜菜碱等;烷基羟基磺基甜菜碱型两性表面活性剂,诸如月桂基二甲氨基羟基磺基甜菜碱等;磷酸酯甜菜碱型两性表面活性剂,诸如月桂基羟基磷酸酯甜菜碱等;以及酰胺基氨基酸型两性表面活性剂,诸如N-月桂酰基-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-椰油基-N’-羟乙基-N′-羧甲基乙二胺钠、N-月桂酰基-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-月桂酰基-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-椰油基-N-羟乙基-N′-羧甲基乙二胺钠、N-月桂酰基-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-椰油基-N-羟乙基-N′,N'-二羧甲基乙二胺单钠、N-月桂酰基-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-椰油基-N-羟乙基-N',N'-二羧甲基乙二胺二钠等。
半极性表面活性剂的示侧包括烷基胺氧化物型表面活性剂、烷基胺氧化物、烷基酰胺胺氧化物、烷基羟胺氧化物等。优选地使用具有10至18个碳的烷基二甲基胺氧化物、具有8至18个碳的烷氧基乙基二羟乙基胺氧化物等。其具体示例包括十二烷基二甲基氧化胺、二甲基辛基氧化胺、二乙基癸基氧化胺、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、十二烷基酰胺基丙基二甲基氧化胺、鲸蜡基二甲基氧化胺、硬脂酰基二甲基氧化胺、牛油二甲基氧化胺、二甲基-2-羟基十八烷基氧化胺、月桂酰基二甲基氧化胺、肉豆蔻基二甲基氧化胺、硬脂酰基二甲基氧化胺、异硬脂酰基二甲基氧化胺、可可脂肪酸烷基二甲基氧化胺、辛酰胺丙基二甲基氧化胺、癸酰胺丙基二甲基氧化胺、月桂酰胺丙基二甲基氧化胺、肉豆蔻酰胺丙基二甲基氧化胺、棕榈酰胺丙基二甲基氧化胺、硬脂酰胺丙基二甲基氧化胺、异硬脂酰胺丙基二甲基氧化胺、油酰胺丙基二甲基氧化胺、蓖麻酰胺丙基二甲基氧化胺、12-羟基硬脂酰胺丙基二甲基氧化胺、可可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、月桂酰胺乙基二甲基氧化胺、肉豆蔻酰胺乙基二甲基氧化胺、可可脂肪酸酰胺乙基二甲基氧化胺、月桂酰胺乙基二乙基氧化胺、肉豆蔻酰胺乙基二乙基氧化胺、可可脂肪酸酰胺乙基二乙基氧化胺、月桂酰胺乙基二羟乙基氧化胺、肉豆蔻酰胺乙基二羟乙基氧化胺和可可脂肪酸酰胺乙基二羟乙基氧化胺。
盐的示例包括无机盐、有机酸盐、胺盐和氨基酸盐。无机盐的示例包括无机酸诸如盐酸、硫酸、碳酸和硝酸的钠盐、钾盐、镁盐、钙盐、铝盐、锆盐和锌盐。有机酸盐的示例包括有机酸诸如乙酸、脱氢乙酸、柠檬酸、苹果酸、琥珀酸、抗坏血酸和硬脂酸的盐。胺盐和氨基酸盐的示例包括胺诸如三乙醇胺的盐和氨基酸诸如谷氨酸的盐。此外,也可使用透明质酸、硫酸软骨素等的盐,化妆产品处理中使用的铝锆甘氨酸络合物、酸碱中和盐等。
保湿剂的示例包括多元醇,诸如甘油、山梨糖醇、丙二醇、二丙二醇、1,3-丁二醇、葡萄糖、木糖醇、麦芽糖醇和聚乙二醇;透明质酸、硫酸软骨素、吡咯烷酮羧酸酯、聚氧乙烯甲基葡糖苷、聚氧丙烯甲基葡糖苷和PEG/PPG二甲醚。
防腐剂的示例包括对羟基苯甲酸烷基酯、苯甲酸、苯甲酸钠、山梨酸、山梨酸钾和苯氧基乙醇。抗微生物剂的示例包括苯甲酸、水杨酸、苯酚、山梨酸、对羟基苯甲酸烷基酯、对氯间甲酚、六氯酚、烷基苄基二甲基氯化铵、氯己定、三氯碳酰苯胺、三氯生、光敏元素和苯氧乙醇。就胭脂而言,组合物优选不含防腐剂。
抗氧化剂的示例包括生育酚、丁基羟基茴香醚、二丁基羟基甲苯和植酸。
pH调节剂的示例包括乳酸、柠檬酸、乙醇酸、琥珀酸、酒石酸、dl-苹果酸、碳酸钾、碳酸氢钠和碳酸氢铵。
螯合剂的示例包括丙氨酸、依地酸的钠盐、多磷酸钠、偏磷酸钠和磷酸。
清新剂的示例包括L-薄荷醇和樟脑,以及抗炎剂的示例包括尿囊素、甘草次酸、甘草酸、氨甲环酸和薁。
美肤剂的示例包括亮肤剂,诸如胎盘提取物、熊果苷、谷胱甘肽和虎耳草提取物;细胞活化剂,诸如蜂王浆;皮肤粗糙改善剂;循环促进剂,诸如壬酸戊二酰胺、烟酸苄酯、烟酸β-丁氧基乙酯、辣椒碱、金杰伦、斑蝥酊、鱼石脂、咖啡因、鞣酸、α-冰片、生育酚烟酸酯、六烟酸肌醇酯、环扁桃酸酯、肉桂酸赖氨酸、妥拉唑林、乙酰胆碱、维拉帕米、西法安生和γ-谷维素;皮肤收敛剂,诸如氧化锌和鞣酸;抗皮脂溢剂,如硫磺和二甲噻蒽。维生素的示例包括维生素A诸如维生素A油、视黄醇、视黄醇乙酸酯和视黄醇棕榈酸酯;维生素B2,诸如核黄素、丁酸核黄素和黄素腺嘌呤核苷酸;维生素B6,诸如盐酸吡哆醇、二辛酸吡哆醇和三棕榈酸吡哆醇;维生素B,诸如维生素B12及其衍生物、维生素B15及其衍生物;维生素C,诸如L-抗坏血酸、L-抗坏血酸二棕榈酸酯、L-抗坏血酸-2-硫酸钠和L-抗坏血酸磷酸二酯二钾;维生素D,诸如麦角钙化醇和胆钙化醇;维生素E,诸如α-生育酚、β-生育酚、γ-生育酚、d1-α-生育酚乙酸酯、dl-α-生育酚烟酸酯和dl-α-生育酚琥珀酸酯;维生素H;维生素P;烟酸,诸如烟酸和烟酸苄酯;以及泛酸,诸如泛酸钙、D-泛醇、泛基乙基醚和乙酰基戊基苯基乙基醚。
氨基酸的示例包括氨基酸诸如甘氨酸、缬氨酸、亮氨酸、异亮氨酸、丝氨酸、苏氨酸、苯丙氨酸、精氨酸、赖氨酸、天冬氨酸、谷氨酸、胱氨酸、半胱氨酸、甲硫氨酸和色氨酸和/或它们的盐。
核酸的示例是脱氧核糖核酸,并且激素的示例包括雌二醇和乙烯基雌二醇。
生物活性组分是当应用于皮肤或毛发时为皮肤或毛发提供某种生物活性的物质;其一个示例是亲脂性组分。示例包括抗炎剂、抗衰老剂、收紧剂、毛发再生剂、毛发生长促进剂、保湿剂、循环促进剂、干燥剂、温热剂、维生素、伤口愈合加速剂、刺激缓解剂、镇痛剂、细胞活化剂和酶组分。类似地,组合物还可优选含有天然植物提取物组分、海藻提取物组分和/或草药组分。
药物活性成分是具有治疗效果的物质;该示例包括蛋白质、肽和低分子量化合物。
芳香剂没有特别限定,只要芳香剂是亲脂性的即可,并且示例包括从各种植物的花、种子、叶、根等中提取的芳香剂,从海藻中提取的芳香剂、从动物的各种部位或分泌物提取的芳香剂(例如麝香或抹香鲸)和人工合成的芳香剂(例如薄荷醇、麝香、醋酸酯和香草)。配混芳香剂以赋予化妆品芳香或香味。着色剂的示例包括油溶性染料、体质颜料、无机颜料、有机颜料和亲脂性荧光增白剂。
本发明的化妆产品可通过将上述本发明的化妆产品原料与其它化妆产品原料简单地均匀混合而容易地制造。通常用于制造化妆产品的各种混合装置和捏合装置可用作混合部件。这些装置的示例包括均混器、桨式混合器、Henschel混合器、高速分散器(homo-disper)、胶体磨、旋桨式搅拌器、均化器、串联式连续乳化器、超声乳化器和真空捏和机。
实施例
将使用实施例更具体地描述本发明,但是其不仅限于这些工作例。注意,实施例中的粘度为在25℃下的值。
在工作例和比较例中制造复合硅橡胶颗粒。对于复合硅橡胶颗粒通过计算和从固体NMR证实了官能硅烷的含量比(wt%)、二氧化硅的含量比(wt%)以及同一颗粒中的官能硅烷和二氧化硅的重量比,并且测量平均粒径、亲水性、流动性、甲醇含量比和抗微生物活性。
<工作例1>
首先,将0.5970g二氧化硅(由Nippon Aerosil Co.,Ltd.生产的Aerosil200,干二氧化硅,平均原生粒径:5nm至15nm,硅烷醇密度:BET比表面积:200m2/g)和20.2954g加成可固化的交联硅橡胶颗粒(平均原生粒径:5μm至10μm,JIS-A硬度:60,含有1质量份(重量%)有机硅油)装入到高速搅拌器。将组分以约10,000rpm搅拌并混合约1分钟。接下来,将0.1974g十八烷基二甲基[3-(三甲氧基甲硅烷基)丙基]氯化铵的50%甲醇溶液(下文中称为“硅烷的甲醇溶液”)加入到该混合物中,并进一步以10,000rpm搅拌并混合约2分钟。将混合物在120℃的烘箱中热处理2小时,并且挥发甲醇以使二氧化硅和硅烷反应。
<工作例2>
除了将二氧化硅的量变为0.4049g,将硅烷的甲醇溶液的量变为0.2229g,并且将硅橡胶颗粒的量变为20.1310g之外,以与工作例1中相同的方式制备复合硅橡胶颗粒。
<工作例3>
除了将二氧化硅的量变为0.4187g,将硅烷的甲醇溶液的量变为0.3977g,并且将硅橡胶颗粒的量变为20.5924g之外,以与工作例1中相同的方式制备复合硅橡胶颗粒。
在工作例4至7中,与工作例1至3相比,首先对二氧化硅进行硅烷处理。
<工作例4>
首先,将4.0276g二氧化硅(由Nippon Aerosil Co.,Ltd.生产的Aerosil200,干燥二氧化硅,平均原生粒径:5nm至15nm,硅烷醇密度: BET比表面积:200m2/g)加入到高速搅拌器中,并且向该二氧化硅中加入1.954g十八烷基二甲基[3-(三甲氧基甲硅烷基)丙基]氯化铵的50%甲醇溶液,并以约10,000rpm搅拌并混合约两分钟。将混合物在120℃的烘箱中热处理2小时,并且挥发甲醇以使二氧化硅和硅烷反应。这被称为硅烷缩合物和精细颗粒二氧化硅的反应产物(2)。除了未使用硅烷,并且使用0.4091g硅烷缩合物和精细颗粒二氧化硅的反应产物(1)和20.1415g硅橡胶颗粒之外,以与工作例1中相同的方式制备复合硅橡胶颗粒。
<工作例5>
除了二氧化硅的装入量为4.0427g,并且十八烷基二甲基[3-(三甲氧基甲硅烷基)丙基]氯化铵的50%甲醇溶液的添加量为3.9358g之外,以与工作例4中的硅烷缩合物和精细颗粒二氧化硅的反应产物(1)的制备相同的方式制备产物。这被制备为硅烷缩合物和精细颗粒二氧化硅的反应产物(2)。
除了未使用硅烷,并且使用0.4091g硅烷缩合物和精细颗粒二氧化硅的反应产物(2)和20.1415g硅橡胶颗粒之外,以与工作例1中相同的方式制备复合硅橡胶颗粒。
<工作例6>
除了未使用硅烷,并且使用0.6138g工作例5的硅烷缩合物和细颗粒二氧化硅的反应产物(2)和20.2914g硅橡胶颗粒之外,以与工作例1中相同的方式制备复合硅橡胶颗粒。
<工作例7>
除了二氧化硅的装入量为6.1560g,并且使用3.1608g[3-(三乙氧基甲硅烷基)丙基]氯化铵和1.6208g乙醇的混合溶液代替三甲基[3-(三乙氧基甲硅烷基)丙基]氯化铵之外,以与工作示例4中硅烷缩合物和精细颗粒二氧化硅的反应产物(1)的制备相同的方式制备产物。这被称为硅烷缩合物和精细颗粒二氧化硅的反应产物(3)。
除了未使用硅烷,并且使用0.6111g硅烷缩合物和精细颗粒二氧化硅的反应产物(3)和20.5776g硅橡胶颗粒之外,以与工作例1中相同的方式制备复合硅橡胶颗粒(A)。
<比较例1>
除了不混合二氧化硅,将20.1233g硅橡胶颗粒装入高速搅拌器(开口直径:10cm,深度:5cm),并向该混合物中加入0.4103g十八烷基二甲基[3-(三甲氧基甲硅烷基)丙基]氯化铵的50%甲醇溶液后硅橡胶颗粒的量为20.1233g之外,以与工作例1相同的方式制备复合硅橡胶颗粒将组分以约10,000rpm搅拌并混合约2分钟。将该混合物转移到200mL烧杯中,并且在120℃的氮气烘箱中热处理2小时,并且挥发甲醇使硅烷冷凝反应。具有该正十八烷基二甲基氯化铵基团的复合硅橡胶颗粒在200mL烧杯中表现出强的聚集性并形成几厘米的团块。即使用手指碾碎,团块也不会变细小,所以使用研钵将团块粉碎至不大于1mm的粒径。粉碎后的平均粒径超过测量装置的测量上限值,并且推测平均粒径为不小于200μm。
<比较例2>
首先,将0.6195g与工作例1中相同的二氧化硅和21.0718g与工作例1中使用的相同的可加成固化交联的硅橡胶颗粒加入到高速搅拌器(与工作例1中相同)中。将组分以约10,000rpm搅拌并混合约2分钟。获得表现流动性的粉末。这被用作比较例2。
<比较例3>
使用热处理前的工作例1的混合物被用作比较例3。
<比较例4>
使用工作例1的可加成固化型交联的硅橡胶颗粒(平均粒径:14μm,JIS-A硬度:60,含有1质量%的有机硅油)作为比较例4。
对工作例1至7和比较例1至4中得到的硅橡胶颗粒的流动性、分散性、抗微生物活性和甲醇含量进行性能评价。
<甲醇含量,甲醇生成>
在20mL小瓶中称量约0.85g样品。使用顶空进样器在80℃加热小瓶30分钟后,从小瓶的顶部空间吸出1mL空气并将空气注入气相色谱仪并进行测量。从基于甲醇的添加量产生的校准曲线计算浓度。
<平均粒径>
使用乙醇作为分散介质,使用激光衍射式粒径分布分析装置(由Horiba,Ltd.生产的LA-750)测定复合硅橡胶颗粒的粒径,并且使用中值粒径作为平均粒径尺寸。
<亲水性>
首先,将3.0g复合硅橡胶颗粒添加到100g水和3g乙醇中并搅拌,并用高速分散器以1,000rpm搅拌该混合物1分钟。观察颗粒是否分散为精细颗粒,颗粒是否不分散成精细颗粒而是聚集,或者颗粒是否与水分离。均匀分散评价为良好,表示“亲水”;聚集颗粒被评价为CA(条件合格),表示“略微亲水”;并将分离情况评估为NA(不合格),表示“疏水”。
<流动性>
将大约20g制备的改性有机硅颗粒置于聚乙烯袋(开口:15cm)中,并且在将颗粒收集在袋的底部之后,基于颗粒是否流动以及当袋子旋转90度时颗粒聚集体塌缩的形状来评估流动性。形状塌缩的情况评估为良好,表示“流动”;并且形状没有塌缩的情况被评估为NA(不可接受)指示“不流动”。
<抗微生物活性测试>
根据ASTM E2149-10:“在动态接触条件下确定固定化抗微生物剂的抗微生物活性的标准测试方法(Standard Test Method for Determining the Antimicrobialactivity of Immobilized Antimicrobial Agents Under Dynamic ContactConditions)”进行抗微生物测试。将大肠杆菌(操作细菌浓度:5.48×106cfu/mL)或金黄色葡萄球菌(操作细菌浓度:9.5×106cfu/mL)和1g硅橡胶颗粒的5mL混合物振荡24小时,并且将其1mL样品与杀菌稀释剂混合以制备各种浓度的稀释溶液。计算40小时(28℃至30℃)后稀释溶液的CFU(菌落形成单位),并比较对数减少率。
表1
(化妆品评估/测量方法)
<毛发粘附性>
首先,将3.0g复合硅橡胶颗粒加入到100g水和3g乙醇中并搅拌,并且用高速分散器以1,000rpm搅拌1分钟,以制备以复合硅橡胶颗粒的水基分散体形式用于毛发处理的水基化妆品。
作为评价用毛发,在50℃下漂白30分钟后,使用可商购的中国发束(得自Beaulax公司,17cm,2g),并且用10%月桂基聚氧乙烯醚硫酸钠溶液洗涤。将发束在用于毛发处理的水基化妆品中浸渍30秒后,用1L水冲洗发束并使其干燥。测量粘附到发束上的有机硅的量。此外,评价经处理的毛发干燥后的触觉(湿润感和沉降感)。所有评估项目被评估为优秀的情况记录为5分;被评估为劣质的情况记录为1分;中间情况记录为2份、3份或4分。平均得分被用作使用感的评估结果。评估结果示于表2中。
<工作例8>
水基化妆品(1):
首先,将100重量份水、3重量份乙醇和10.0重量份工作例7的复合硅橡胶颗粒用高速分散器以1,000rpm搅拌1分钟以制备水基分散体的形式的水基化妆品。漂白后,将用10%月桂基聚氧乙烯醚硫酸钠溶液洗涤并干燥的发束浸入化妆品中,并且然后干燥,并且评价发束的毛发粘附性、湿度和沉降感。结果示于表2中。
<工作例9>
水基化妆品(2):
以与工作例8相同的方式进行。然而,使用的工作例7的复合硅橡胶颗粒的重量为3.0重量份。
<工作例10>
水基组合物(3):
以与工作例9相同的方式进行。然而,使用由工作例8得到的颗粒作为要使用的复合硅橡胶颗粒,并且其重量为3.0重量份。
<比较例5>
水基化妆品(4):
尝试以与工作例9中相同的方式制备水基分散体形式的用于毛发处理的水基化妆品,除了使用3.0重量份的比较例2的复合硅橡胶颗粒之外,但复合硅橡胶颗粒分离并漂浮在水面上,并且得不到均匀的溶液。
<比较例6>
水基化妆品(5):
尝试以与工作例9中相同的方式制备水基分散体形式的用于毛发处理的水基化妆品,除了使用3重量份的比较例4的硅橡胶颗粒之外,但复合硅橡胶颗粒分离并漂浮在水面上,并且得不到均匀的溶液。
工作例8至11和比较例5和6示于表2中。
表2
下文中描述其中可配混本发明的固化有机硅颗粒的本发明化妆品的制剂例。但是,本发明不限于这些实施例。
制剂例1:W/O BB霜
(组分)
相A
1)月桂基PEG/PPG-18/18聚二甲基硅氧烷(*1):4质量份
2)辛基甲基聚硅氧烷(*2):14质量份
3)甲氧基肉桂酸乙基己酯(*3):7.5质量份
4)二乙基氨基羟基苯甲酰基苯甲酸己酯(*4):1.5质量份
5)琥珀酸乙基己酯:2.5质量份
6)三甲基甲硅烷氧基硅酸和聚丙基倍半硅氧烷(*5):2质量份
7)工作例1至5的复合硅橡胶颗粒:3质量份
8)生育酚乙酸酯:0.5质量份
相B
9)抗坏血酸硫酸钠:0.5质量份
10)甘油:8质量份
11)氯化钠:0.7质量份
12)纯化水:39.8质量份
相C
13)氧化钛:5.6质量份
14)氧化铁黄(*6):0.25质量份
15)氧化铁红(*7):0.1质量份
16)氧化铁黑(*8):0.05质量份
17)苯基聚三甲基硅氧烷(*9):9.2质量份
18)氧化锌(*10):0.8质量份
*1:5200配方助剂,由Dow Corning Toray Co.,Ltd.制造
*2:FZ-3196,由Dow Corning Toray Co.制造
*3:Uvinul MC80N,由BASF公司制造
*4:Uvinul A Plus Glanular,由BASF制造
*5:MQ-1640薄片树脂,由Dow Corning Toray Co.,Ltd.制造
*6:SA-10Y-8,由Miyoshi Kasei,Inc.制造
*7:SA-IOR-8,由Miyoshi Kasei,Inc.制造
*8:SA-IOB-8,由Miyoshi Kasei,Inc.制造
*9:SH556,由Dow Corning Toray Co.,Ltd.制造
*10:Z-Cote,由BASF制造
根据以下过程制备制剂例1的BB霜。
1.将组分1至8混合。
2.将组分9至12混合。
3.将组分13至18混合。
4.将步骤1中获得的相A与步骤3中获得的相C混合。
5.在搅拌步骤4中获得的混合物的同时逐渐加入在步骤2中获得的相B并乳化。
制剂例2:非水性防晒乳液
(组分)
氧化锌(*1):6质量份
甲氧基肉桂酸乙基己酯(*2):7.5质量份
聚二甲基硅氧烷,聚二甲基硅氧烷交联聚合物(*3):24质量份
环戊硅氧烷(*4):60.5质量份
工作例2的复合硅橡胶颗粒:2质量份
*1:MZ-303S,由TAYCA制造
*2:Uvinul MC80N,由BASF公司制造
*3:9041有机硅弹性体共混物,由Dow Coming Corporation制造
*4:SH245,由Dow Corning Toray Co.,Ltd.制造
根据以下过程制备制剂例2的非水性防晒乳液。
1.搅拌组分4和5直至均匀。
2.将上述1的混合物加入到组分3中并搅拌直至均匀。
3.将组分1和2混合。
4.搅拌上述2和3的混合物直至均匀。
制剂例3:O/W抗衰老霜
(组分)
相A
纯化水:余量
甲基丙烯酸甲酯交联聚合物(*1):5质量份
相B
环戊硅氧烷,环己硅氧烷(*2):35质量份
工作例5的有机硅交联物:5质量份
(丙烯酸羟乙酯/丙烯酰二甲基牛磺酸钠)共聚物、角鲨烷、聚山梨醇酯80、水和山梨糖醇油酸酯(*3):0.7质量份
(丙烯酸羟乙酯/丙烯酰二甲基牛磺酸钠)共聚物、异十六烷、聚山梨醇酯60、水和脱水山梨糖醇异硬脂酸酯(*4):0.7质量份
相C
聚二甲基硅氧烷:5质量份
二棕榈酰羟脯氨酸(*5):0.5质量份
相D
葡萄酒提取物(*6):0.01质量份
芳香剂:0.2质量份
相E
苯氧基乙醇:0.9质量份
*1:Micropearl M305,由SEPPIC S.A.制造
*2:DC345,由Dow Corning Toray Co.,Ltd制造
*3:Simulgel EG,由SEPPIC S.A.制造
*4:Simulgel NS,由SEPPIC S.A.制造
*5:Simulgel DPHP,由SEPPIC S.A.制造
*6:Sepivinol R,由SEPPIC S.A.制造
根据以下过程制备制剂例3的O/W抗衰老霜。
1.将组分2分散到组分1中。
2.将组分4分散到组分3中。
3.将组分5和6加入上述2的混合物中并混合。(混合物3)
4.将组分8溶解到组分7中。(裂解物4)
5.在搅拌上述1的混合物的同时加入上述混合物3、裂解物4和相D并乳化。
制剂例4:O/W皱纹护理霜
(组分)
相A
1)环戊硅氧烷(*1):11质量份
2)工作例6的复合硅橡胶颗粒:10质量份
3)月桂基PEG/PPG-18/18聚二甲基硅氧烷(*2):0.5质量份
4)PEG-12聚二甲基硅氧烷(*3):4质量份
相B
5)纯化水:72.5质量份
相C
聚丙烯酰胺、水、(C13,14)异链烷烃和月桂基聚氧乙烯醚-7(*4):2质量份
*1:SH245,由Dow Corning Toray Co.,Ltd.制造
*2:5200配方助剂,由Dow Corning Toray Co.,Ltd.制造
*3:OFX-5329,由Dow Corning Toray Co.,Ltd制造
*4:Simulgel 305,由SEPPIC S.A.制造
根据以下过程制备制剂例4的O/W皱纹护理霜。
1.将相A混合至均匀。
2.在搅拌相B的同时逐渐加入上述1的混合物。
3.将相C加入上述2的混合物中并混合至均匀。
制剂例5:致密粉底
(组分)
相A
1)环戊硅氧烷,环己硅氧烷(*1):4质量份
2)鲸蜡基聚二甲基硅氧烷(*2):2质量份
3)硬脂基聚二甲基硅氧烷(*3):6质量份
4)烷基(C30-45)聚甲基硅氧烷,烯烃(C30-45)(*4):3质量份
5)蜂蜡(*5):8质量份
6)环戊硅氧烷,聚丙基倍半硅氧烷(*6):5质量份
7)防腐剂:0.5质量份
相B
8)环戊硅氧烷(*7):44质量份
9)氧化铁红(*8):1.5质量份
10)氧化铁黄(*9):2.5质量份
11)氧化铁黑(*10):0.75质量份
12)氧化铁棕(*11):5.75质量份
相C
13)二氧化硅(*12):1质量份
14)工作例6的复合硅橡胶颗粒:6质量份
15)辛烯基琥珀酸玉米淀粉Al(*13):4质量份
16)滑石:2质量份
17)尿囊素(*14):1质量份
18)氧化钛:(*15):3质量份
*1:DC345,由Dow Corning Toray Co.,Ltd.制造
*2:2502美容液,由Dow Corning Toray Co.,Ltd.制造
*3:2503美容液,由Dow Corning Toray Co.,Ltd.制造
*4:AMS-C30美容液,由Dow Corning Toray Co.,Ltd.制造
*5:Cerabeil White No.1,由Baerlocher France S.A.制造。
*6:670流体,由Dow Corning Toray Co.,Ltd.制造
*7:SH245,由Dow Corning Toray Co.,Ltd.制造
*8:Unipure Red LC 381 AS-EM,由Sensient Cosmetic Technologies制造
*9:Unipure Yellow LC 182 AS-EM,由Sensient Cosmetic Technologies制造
*10:Unipure Black LC 989 AS-EM,由Sensient Cosmetic Technologies制造
*11:Unipure Brown LC 881,由Sensient Cosmetic Technologies制造
*12:LDP 1500,由Sensient Cosmetic Technologies制造
*13:Dry Flo Plus.由National Starch&Chemical Company制造
*14:尿囊素/ISP
*15:Matlake OPA-AS,由Sensient Cosmetic Technologies制造根据以下过程制备制剂例5的致密粉底。
1.将相A加热至80℃并溶解。(裂解物1)
2.将组分9至12混合直至均匀。(混合物2)
3.将组分8分散到混合物2中。(分散体3)
4.将相C混合至均匀(混合物4)
5.将分散体3和混合物4混合。(混合物5)
6.加入混合物5,同时搅拌裂解物1,并搅拌混合物(80℃)。
7.将混合物转移到容器中,冷却并硬化。
制剂例6:发油
(组分)
1)环戊硅氧烷(*1):45质量份
2)工作例7的复合硅橡胶颗粒:2.7质量份
3)辛基甲基聚硅氧烷(*2):20质量份
4)摩洛哥坚果油:0.1质量份
5)橄榄油:0.1质量份
6)苯基聚三甲基硅氧烷(*3):2质量份
7)环戊硅氧烷,聚二甲基硅烷醇(*4):30质量份
8)芳香剂:0.1质量份
*1:SH245,由Dow Corning Toray Co.,Ltd.制造
*2:SS-3408,由Dow Corning Toray Co.,Ltd.制造
*3:556流体,由Dow Corning Toray Co.,Ltd.制造
*4:PMX-1501流体,由Dow Corning Toray Co.,Ltd.制造根据以下过程制备制剂例7的发油。
1.将组分2分散到组分1中。(分散体1)
2.将剩余的组分3至8加入到分散体1中并混合。
制剂例7:发胶
各组分名称后的数值表示重量份(质量)。
未经稀释的溶液
(组分)
1.乙醇:余量
2.丙烯酸树脂链烷醇胺溶液(有效成分:50%):7.0
3.鲸蜡醇:0.1
4.工作例7的复合硅橡胶颗粒:0.5
5.芳香剂:适量
填料
6.未稀释溶液:50.0
7.二甲醚:50.0
(制造过程)
步骤1:将组分2至5加到组分1中并且混合并溶解。
步骤2:将步骤1中获得的组合物过滤。
步骤3:用步骤2中获得的组合物(未稀释溶液)填充容器(罐),并且在安装阀装置之后,用组分7填充容器。
制剂例8:调理剂
各组分名称后的数值表示重量份(质量)。
(组分)
1.硬脂基三甲基氯化铵:1.44
2.鲸蜡醇:2.4
3.辛基十二烷醇:0.5
4.鲸蜡基乙基己酸酯:0.6
5.角鲨烷:0.2
6.纯化水:余量
7.甘油:2.0
8.防腐剂:适量
9.芳香剂:适量
10.工作例3的复合硅橡胶颗粒(*):3.0
11.柠檬酸:适量
*)通过将工作例3的复合硅橡胶颗粒和二甲基聚硅氧烷(2cSt)以1/9的重量比混合,并且然后乳化至固体含量为30质量%而制备的O/W乳液。
(制造过程)
步骤1:将组分1至5加热且混合并溶解。
步骤2:将组分6至7加热且混合并溶解。
步骤3:将步骤2中获得的组合物加入到步骤1中获得的组合物中并且乳化。
步骤4:将步骤3中获得的组合物冷却,并加入组分8至10。另外根据需要加入组分11。
在步骤4之后,进一步加入二甲基硅氧烷、分子两端用二甲基硅烷醇基团(聚二甲基硅烷醇)、苯基改性的有机硅、氨基改性的有机硅、乳液如氨基聚醚共改性的有机硅、有机硅弹性体粉末的水性分散体和/或水溶性有机硅油如聚醚改性的有机硅可预期各组分的协同效应。
制剂例9:毛发处理冲洗型
各组分名称后的数值表示重量份(质量)。
(组分)
1.鲸蜡醇:5.6
2.矿物油:1.0
3.硬脂基三甲基氯化铵:1.2
4.二十二烷基三甲基氯化铵:0.64
5.环戊硅氧烷:2.0
6.聚二甲基硅氧烷(2cSt):1.0
7.聚二甲基硅氧烷(5,000cSt):1.0
8.苯基甲基硅氧烷:2.0
9.甘油:2.0
10.EDTA-2Na:0.1
11.纯化水:余量
12.泛醇:0.1
13.生育酚:0.04
14.赖氨酸HCl:0.02
15.甘氨酸:0.02
16.组氨酸:0.02
17.工作例3的复合硅橡胶颗粒:0.5
18.防腐剂:适量
19.芳香剂:适量
(制造过程)
步骤1:将组分1至8加热并且混合并溶解。
步骤2:将组分9至11加热并且混合并溶解。
步骤3:将步骤2中获得的组合物加入到步骤1中获得的组合物中并且乳化。
步骤4:将步骤3中获得的组合物冷却,并加入组分12至19。
在步骤1中,除了组分1至8之外,还加入在分子两端用二甲基硅烷醇基团(聚二甲基硅烷醇)封端的二甲基聚硅氧烷、氨基改性的有机硅、氨基聚醚共改性的有机硅等使得可预期每种组分的协同作用。
制剂例10:毛发处理冲洗型
各组分名称后的数值表示重量份(质量)。
(组分)
1.鲸蜡醇:4.0
2.矿物油:1.0
3.硬脂基三甲基氯化铵:1.0
4.二十二烷基三甲基氯化铵:0.2
5.环戊硅氧烷:1.2
6.聚二甲基硅氧烷(2cSt):0.6
7.聚二甲基硅氧烷(5,000cSt):0.6
8.苯基甲基硅氧烷:1.2
9.甘油:2.0
10.EDTA-2Na:0.1
11.纯化水:余量
12:泛醇:0.1
13:生育酚:0.04
14:赖氨酸HCl:0.02
15:甘氨酸:0.02
16:组氨酸:0.02
17.工作例3的复合硅橡胶颗粒:0.3
18.防腐剂:适量
19.芳香剂:适量
(制造过程)
步骤1:将组分1至8加热并且混合并溶解。
步骤2:将组分9至11加热并且混合并溶解。
步骤3:将步骤2中获得的组合物加入到步骤1中获得的组合物中并且乳化。
步骤4:将步骤3中获得的组合物冷却,并加入组分12至19。
在步骤1中,除了组分1至9之外,还加入在分子两端用二甲基硅烷醇基团(聚二甲基硅烷醇)封端的二甲基聚硅氧烷、氨基改性的有机硅、氨基聚醚共改性的有机硅等使得可预期每种组分的协同作用。
制剂例11:油包水型止汗剂
组成重量(%)
1.有机硅弹性体(*1)7.0
2.十甲基环戊硅氧烷:10.0
3.三辛酸甘油酯:7.0
4.二丙二醇:5.0
5.柠檬酸钠:0.2
6.铝/锆四氯水合物:18.0
7.工作例6的复合硅橡胶颗粒:7.0
8.芳香剂:适量
9.纯化水:45.8
总计:100.0
*1∶9045有机硅弹性体共混物(制造方法),由Dow Corning Corporation制造
A:将组分1至3混合。
B:将组分4至9混合。
C:将B加入A中并且混合并乳化。
如上所述获得的油包水型止汗剂表现出光线传播,没有粘性或油腻感,并且不会由于温度或随时间推移而改变,并且使用性和稳定性也是优异的。
制剂例:冲洗型止汗剂
组成重量(%)
1.有机硅弹性体(*1):20.0
2.二甲基聚硅氧烷(6mm2/s(25℃)):10.0
3.聚二甲基硅氧烷交联聚合物(*2):15.0
4.十甲基环戊硅氧烷:30.0
5.铝/锆四氯水合物:20.0
6.工作例6的复合硅橡胶颗粒:5.0
7.芳香剂:适量
总计:100.0
*1:使用了由Dow Corning Corporation制造的9045有机硅弹性体共混物。
*2:使用了由Dow Corning Corporation制造的9011有机硅弹性体共混物。
(制造方法)
A:将组分1至4混合。
B:将组分5至7加入到A中并均匀分散。
如上所述获得的冲洗型止汗剂表现出光线传播,没有粘性或油腻感,并且不会由于温度或随时间推移而改变,并且使用性和稳定性也是优异的。
制剂例:护肤霜
表3
组分 | 重量份 | |
油相 | ||
1 | 月桂基PEG/PPG-18/18聚二甲基硅氧烷<sup>*1</sup> | 2 |
2 | 双(羟乙氧丙基)聚二甲基硅氧烷<sup>*2</sup> | 2 |
3 | 棕榈酸异丙酯<sup>*3</sup> | 1 |
4 | 环戊硅氧烷<sup>*4</sup> | 6.5 |
5 | 矿物油<sup>*5</sup> | 10 |
6 | 凡士林 | 1.5 |
7 | 复合硅橡胶颗粒(工作例3) | 5 |
水相 | ||
8 | 甘油 | 5 |
9 | 氯化钠 | 1 |
10 | 水 | 66 |
*1:5200配方助剂,由Dow Corning Toray Co.,Ltd.制造
*2:5562甲醇流体,由Dow Corning Toray Co.,Ltd.制造
*3:Exceparl IPM,由Kao Chemicals制造
*4:SH245,由Dow Corning Toray Co.,Ltd.制造
*5:Hicall K-230,由Kaneda Co.,Ltd.制造
制剂例:爽身粉
表4:
组分 | 重量份 | |
1 | 氧化钛 | 13.43 |
2 | 氧化铁黄<sup>*1</sup> | 2.43 |
3 | 氧化铁红<sup>*2</sup> | 0.97 |
4 | 氧化铁黑<sup>*3</sup> | 0.17 |
5 | 复合硅橡胶颗粒(工作例3) | 51 |
6 | 芳香剂 | 2.5 |
7 | 环戊硅氧烷<sup>*4</sup> | 27.5 |
8 | (Ca/Na)硼硅酸盐,氧化钛<sup>*5</sup> | 2 |
*1:SA-IOY-8,由Miyoshi Kasei,Inc.制造
*2:SA-IOR-8,由Miyoshi Kasei,Inc.制造
*3:SA-IOB-8,由Miyoshi Kasei,Inc.制造
*4:SH245,由Dow Corning Toray Co.,Ltd.制造
*5:Pinpoints of Pearl,由BASF制造
工业适用性
本发明的固化有机硅颗粒在乙醇和有机硅油中具有优异的分散性,并且因此容易作为添加剂配混。此外,当作为化妆品组合物配混到皮肤用化妆品或皮肤外用剂中时,可改善其触感,因此有机硅颗粒可用作皮肤化妆品、化妆化妆品、软膏剂、毛发化妆品等。此外,利用其物理性质,本发明的固化有机硅颗粒也可用作诸如热固性树脂组合物或热塑性树脂组合物的添加剂或塑料膜的表面润滑剂。
Claims (12)
1.一种复合硅橡胶颗粒,所述硅橡胶颗粒的部分或全部表面被精细二氧化硅颗粒覆盖,所述精细二氧化硅颗粒的表面被硅化合物改性,所述硅化合物具有含季铵盐的官能团,其中,具有含季铵盐的官能团的所述硅化合物的含量为复合硅橡胶颗粒的重量的0.1重量%至10重量%;
其中,所述含有季铵盐的官能团由以下通式(1)表示:
(1):R1-((N+X-R2 2)-R3)a-Y
其中,R1为具有1至30个碳原子的烃基团;每个R2独立地为氢原子或具有1至4个碳原子的烃基团;每个R3独立地选自具有1至8个碳原子的烃基团;X为一价阴离子基团;a为1或2;并且Y为可含有与精细二氧化硅颗粒表面键合的杂原子的二价或更高价的连接基团;
其中,所述复合硅橡胶颗粒具有一个或多个键,所述键包含所述含有季铵盐的官能团,所述含有季铵盐的官能团经由含硅(Si)的连接基团与所述精细二氧化硅颗粒的表面键合,所述连接基团中的硅原子经由氧原子(-O-)与所述精细二氧化硅颗粒的表面键合;所述含有季铵盐的官能团的含量为整个复合硅橡胶颗粒的0.10重量%至10重量%;所述复合硅橡胶颗粒的甲醇含量不大于10ppm。
2.根据权利要求1所述的复合硅橡胶颗粒,其中所述含有季铵盐的官能团为N,N,N-十八烷基二甲基氯化铵官能团或N,N,N-三甲基氯化铵官能团。
3.根据权利要求1所述的复合硅橡胶颗粒,其中含有季铵盐的由以下通式(1')表示的所述官能团相对于所述精细二氧化硅颗粒的重量比为0.03至0.70,
通式(1’):R1-((N+X-R2 2)-R3)a-Y’
其中R1至R3、X和a与通式(1)中的相同;并且Y'为具有与所述精细二氧化硅颗粒的表面上的氧原子(-O-)键合的硅原子的连接基团。
4.根据权利要求1所述的复合硅橡胶颗粒,其中除了通式(1')中的所述官能团的重量之外,所述精细二氧化硅颗粒的含量为整个复合硅橡胶的0.5重量%至10重量%。
5.根据权利要求1所述的复合硅橡胶颗粒,其中所述复合硅橡胶颗粒具有抗微生物能力。
6.根据权利要求1所述的复合硅橡胶颗粒,其中所述复合硅橡胶颗粒中的甲醇含量不大于1ppm。
7.一种化妆产品组合物,含有根据权利要求1至6中任一项所述的复合硅橡胶颗粒。
8.一种权利要求1-6任一项所述复合硅橡胶颗粒的制造方法,至少包括以下步骤:
步骤1:通过使用机械力混合精细二氧化硅颗粒和硅橡胶颗粒来形成复合硅橡胶颗粒;以及
步骤2:用具有含有季铵盐的官能团且能够在所述精细二氧化硅颗粒的表面上形成化学键的硅化合物对步骤1中得到的所述复合硅橡胶颗粒的所述精细二氧化硅颗粒的表面进行改性。
9.一种权利要求1-6任一项所述复合硅橡胶颗粒的制造方法,至少包括以下步骤:
步骤1:用具有含有季铵盐的官能团且能够在所述精细二氧化硅颗粒的表面上形成化学键的硅化合物对所述精细二氧化硅颗粒的表面进行改性;以及
步骤2:通过使用机械力将步骤1中得到的所述精细二氧化硅颗粒与硅橡胶颗粒混合来形成复合硅橡胶颗粒。
10.根据权利要求8或9所述的复合硅橡胶颗粒的制造方法,其中所述方法包括在对所述精细二氧化硅颗粒的表面进行改性的步骤后,在65℃或以上加热所述精细二氧化硅颗粒,并且所述复合硅橡胶颗粒的甲醇含量不大于10ppm。
11.根据权利要求8或9所述的复合硅橡胶颗粒的制造方法,其中具有含有季铵盐的官能团且能够在所述精细二氧化硅颗粒的表面形成化学键的所述硅化合物由以下通式(2)表示:
(2):R4-((N+Z-R5 2)-R6)b-R7-SiR8 3
其中R4为具有1至30个碳原子的烃基团;每个R5独立地为氢原子或具有1至4个碳原子的烃基团;每个R6独立地为具有1至8个碳原子的烃基团;R7为二价有机基团或杂原子;每个R8独立地为烷氧基基团、羟基基团或烷基基团,其中至少一个R8为烷氧基基团;Z为一价阴离子基团;并且b为1至4的整数。
12.根据权利要求8或9所述的复合硅橡胶颗粒的制造方法,其中所述精细二氧化硅颗粒在其表面上具有羟基基团。
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CN102083309A (zh) * | 2008-06-24 | 2011-06-01 | 圣戈班高性能塑胶弗纳雷特公司 | 具有杀生物活性的硅氧烷弹性体产品 |
CN102061092A (zh) * | 2009-11-11 | 2011-05-18 | 信越化学工业株式会社 | 硅氧烷复合颗粒,制备方法和化妆品组合物 |
CN104472530A (zh) * | 2014-12-07 | 2015-04-01 | 南雄鼎成化工有限公司 | 一种固体粉末状有机硅季铵盐抗菌剂及其制作方法 |
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EP3368592A1 (en) | 2018-09-05 |
JP2018533641A (ja) | 2018-11-15 |
CN108137820A (zh) | 2018-06-08 |
US20190055365A1 (en) | 2019-02-21 |
WO2017073755A1 (en) | 2017-05-04 |
KR20180067596A (ko) | 2018-06-20 |
US10793685B2 (en) | 2020-10-06 |
EP3368592A4 (en) | 2019-06-05 |
KR102664508B1 (ko) | 2024-05-17 |
JP6859015B2 (ja) | 2021-04-14 |
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