CN113226476A - 用于光泽和模糊的新方法和化妆品组合物 - Google Patents
用于光泽和模糊的新方法和化妆品组合物 Download PDFInfo
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- CN113226476A CN113226476A CN201980086795.3A CN201980086795A CN113226476A CN 113226476 A CN113226476 A CN 113226476A CN 201980086795 A CN201980086795 A CN 201980086795A CN 113226476 A CN113226476 A CN 113226476A
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Abstract
公开了一种制备复合颗粒的方法，所述复合颗粒包含沉积在片状无机材料上的无孔球形微粒无机材料，其中所述微粒无机材料的折射率大于所述片状无机材料的折射率，其中所述球形材料占所述片状材料总表面积的20至80％，并且其中所述球形材料的量占所述复合颗粒的2至20重量％，进一步地其中所述片状无机材料为云母，所述无孔球形微粒无机材料为二氧化硅，所述方法包括以下步骤：(iv)将所述片状无机材料硅烷化，以得到具有官能团“A”的硅烷化材料；(v)将所述无孔球形微粒无机材料硅烷化以得到具有官能团“B”的硅烷化材料，其中A≠B；并且其中所述“A”和所述“B”能够彼此反应，使得通过它们的反应，所述无孔球形微粒无机材料沉积在所述片状无机材料上；和(vi)使所述具有官能团“A”的硅烷化材料与所述具有官能团“B”的硅烷化材料反应。
Description
技术领域
本发明涉及能够通过新方法获得的在化妆品组合物中使用的材料。更具体地，本发明涉及能够通过新方法获得的在通过在皮肤上产生光学效应来模糊或遮盖皮肤表层或表面瑕疵如细纹和皱纹的组合物中使用的材料。
背景技术
我们的皮肤容易因皮肤病症、环境因素如强烈阳光和因正常老化过程(时间老化)而变差，这可以由于暴露在阳光下而加速(光老化)。近年来，对用于改善皮肤外观的化妆品组合物和美容方法的需求急剧增长。消费者越来越多地寻求化妆品组合物来处理、延迟或遮蔽时间老化和光老化皮肤的可见迹象，诸如皱纹、细纹、下垂、色素沉着过度和老年斑。
通过操纵光的透射，可以通过两种方式隐藏不完美的皮肤。在第一种方式中，化妆品组合物的一种或多种成分可以简单地反射光。通常，配制化妆品组合物的科学家更喜欢依赖滑石、二氧化硅、高岭土和其他具有高折射率的无机微粒材料。备选方法被称为实现柔焦效果，也称为模糊效果。在这种情况下，入射光会因散射(扭曲)而失真，而某些成分可用于产生这种效果。这些成分充当在多个方向弯曲和扭曲光线的透镜。上述的一个例子是微粒有机硅弹性体。
柔焦或模糊是一种可用于隐藏或遮蔽皮肤表层或表面瑕疵的技术。入射光因散射(扭曲)而失真。当微粒组分作为透镜用以在多个方向弯曲和扭曲光线时，入射光因散射(扭曲)而失真。在这样的组合物中，化妆品的一种或多种成分充当透镜用以在多个方向上弯曲和扭曲光线。由于光线落在并停留在那里，皱纹和细纹主要被认为是黑暗的、非反射区域。相反，如果光线被反射和漫射，则皱纹就会变得不那么明显。已经开发出将光线投射到皱纹中并立即消除使褶皱明显的暗区的方法。‘柔焦效应’由Emmert博士在"Quantification ofthe Soft-Focus Effect",Cosmetics and Toiletries,Vol.111,57-61(1996)中进行了描述。
在光透射没有受到充分阻碍的情况下，可能会发生相反的情况。在这里，发光可能是健康的，但现在不美观的皮肤纹理和颜色可能是明显的。皮肤的微观纹理会影响光如何反射，因为表面曲率会改变光的入射角。入射角的这种变化决定了反射到(观察的)特定位置的光是镜面光还是漫射光，即它在被反射之前首先与皮肤相互作用。
虽然希望通过哑光效果隐藏不完美的皮肤，但也希望获得健康的皮肤光亮(radiance)。太不透明的化妆品会将皮肤隐藏在类似涂料的涂层下。有些人将此称为美白。
已知通过使用某些微粒材料可以隐藏或遮蔽表层瑕疵。然而，如果化妆品组合物中包含更多这样的颗粒，则所述颗粒开始影响光泽或光亮。因此，在使用相对较少量的微粒材料时，在努力遮蔽或隐藏皮肤的表面瑕疵的同时平衡所需的皮肤光泽是一个技术问题。
WO2017220310 A1(Unilever)公开了一种包含视黄醇、多孔二氧化硅、有机硅弹性体的个人护理组合物。该组合物对于柔焦有用。
在上文紧接着提到的出版物中，称为L&W指数的指数被用于比较给定化妆品组合物相比其他组合物的功效。该指数与性能成正比。
US20130164356 A1(Merck)公开了发明目的是找到具有高色彩饱和度和高遮盖力而不会失去其光学特性如光泽和色纯度的效应颜料。发现基于具有略圆形的薄片状基材的效应颜料与基于具有更大边缘粗糙度的椭圆形形状的基材的现有技术的效应颜料相比增加了颜色饱和度并增加了遮盖力。该申请公开了基于薄片状基材的效应颜料，其中所述基材具有1.2至2的圆形形状因子(标准化为圆形的周长2/面积)，并涂覆有至少一个具有1.8的折射率的高折射率层。
US2002011186A(JGC)公开了一种薄片状细粉，其包含作为基质的薄片状物质和二氧化硅颗粒，该二氧化硅颗粒覆盖基质表面以降低由基质表面上的不规则光反射引起的基质光泽度，并提高了光滑性。该粉末包含薄片状基质物质如天然云母，和沉积在基质表面的二氧化硅颗粒，其中二氧化硅颗粒可以任选地进一步被烷氧基硅烷的水解物或硅胶固定。所述薄片状细粉是通过将烷氧基硅烷添加到含有薄片状物质和二氧化硅颗粒的分散体中并使其水解，通过将硅酸溶液添加到分散体中并使其凝胶化，或者通过添加烷氧基硅烷和硅酸溶液的组合而制备的。这种粉末可以与各种成分混合，并可用于化妆品。
US6432535 BA(Merck)公开了一种复合材料，其中片状颜料的薄片包含在平均粒径为0.5至10μm的薄片状基材表面上的平均粒径为20至400nm的球形二氧化硅颗粒，然后进一步用超细二氧化钛颗粒涂覆球形二氧化硅。所述复合颗粒有利于柔焦效果、扩散、紫外线防护和白度。
US2002011186 A(Merck)公开了薄片状细粉，其包含作为基质的薄片状物质和覆盖基质表面的二氧化硅颗粒。该颗粒可用于降低由基质表面上的不规则光反射引起的基质光泽度，并提高光滑性。所述薄片状细粉是通过将烷氧基硅烷添加到含有薄片状物质和二氧化硅颗粒的分散体中并使其水解，通过将硅酸溶液添加到分散体中并使其凝胶化，或者通过添加烷氧基硅烷和硅酸溶液的组合而制备的。颗粒不太容易附聚。
发明内容
众所周知，某些微粒材料可以隐藏或遮蔽皮肤的表层缺陷，如细纹和皱纹。然而，随着此类颗粒的用量或剂量增加，它们开始对皮肤的光泽或光亮产生不利影响。
能够通过根据本发明的新方法获得的复合颗粒包含沉积在片状无机材料上的无孔球形微粒无机材料。该颗粒适用于化妆品组合物，以在光泽和模糊或糊化这两种光学效果之间获得最佳平衡。本发明人相信，由于无孔球形微粒无机材料如二氧化硅的经控制的量，并且因为球形材料占片状材料总表面积的20％至80％，因此这种光学性质的平衡是可能的。
根据本发明的材料，即复合颗粒包含沉积在片状无机材料上的无孔球形微粒无机材料。所述球形微粒无机材料的折射率大于所述片状无机材料的折射率。球形材料占据片状颗粒的特定限定表面积，并且所述球形材料的量被适当地平衡，以优化颗粒的使用中性能。
根据第一方面，公开了一种制备复合颗粒的方法，该复合颗粒包含沉积在片状无机材料上的无孔球形微粒无机材料，其中所述微粒无机材料的折射率大于所述片状无机微粒材料的折射率，其中所述球形材料占所述片状材料总表面积的20至80％，并且其中所述球形材料的量占所述复合颗粒的2至20重量％，进一步地其中所述片状无机材料为云母，并且所述无孔球形微粒无机材料为二氧化硅，所述方法包括以下步骤：
(i)将所述片状无机材料硅烷化，以得到具有官能团“A”的硅烷化材料；
(ii)将所述无孔球形微粒无机材料硅烷化以得到具有官能团“B”的硅烷化材料，其中A≠B；并且其中所述“A”和所述“B”能够彼此反应，使得通过它们的反应，所述无孔球形微粒无机材料沉积在所述片状无机材料上；和
(iii)使所述具有官能团“A”的硅烷化材料与所述具有官能团“B”的硅烷化材料反应。
在考虑以下详细描述和实施例后，本发明的所有其他方面将更容易变得清楚。
根据第二方面，公开了一种化妆品组合物，其包含能够通过第一方面的方法获得的复合颗粒。
根据第三方面，公开了能够通过第一方面的方法获得的复合颗粒在化妆品组合物中用于增强皮肤光泽的用途。
根据第四方面，公开了能够通过第一方面的方法获得的复合颗粒在化妆品组合物中用于遮盖皮肤表层瑕疵的用途。
根据第五方面，公开了一种增强皮肤光泽的方法，包括向其施用包含能够通过本发明第一方面的方法获得的复合颗粒的化妆品组合物的步骤。
根据第六方面，公开了一种遮盖皮肤表层瑕疵的美容方法，包括向其施用包含能够通过本发明第一方面的方法获得的复合颗粒的化妆品组合物的步骤。
定义
如本文所用，“皮肤”是指包括面部、颈部、头皮、腋下、胸部、背部、手臂、手、腿、头皮、脚、臀部和腹部上的皮肤，优选手、颈部、面部和腋下上的皮肤。
皮肤的表层瑕疵是指并包括缺点(老年斑、皮肤上的疹斑)、毛孔、细纹和皱纹，以及凹坑(“细纹”、“皱纹”和凹坑在本文中可互换使用)。如本文所用的“老年斑”是指任何色素沉着过度(例如包括日光性斑点)、斑点和/或雀斑。
如本文所用，术语处理或处理(treating或treatment)包括在其范围内减少、延迟和/或预防上述皮肤状况(condition)，并且通常提高皮肤质量并改善其外观和质地。
“镜面反射”是指来自表面的光的镜面状反射，其中来自单个入射源的光被反射到单个出射方向。光可以具有能够从面部皮肤表面进行镜面反射的任何波长，优选地它是可见光。
如本文所用，“化妆品组合物”意在包括用于局部施用于哺乳动物，尤其是人类皮肤的组合物。这种组合物通常可分为免洗型或洗去型，但优选为免洗型。该组合物被配制成一种被施用于人体、特定地用于改善外观的产品。本发明的组合物可以呈液体、乳剂、霜剂、泡沫、擦洗剂、凝胶或爽肤水的形式，或者用工具或通过面罩或垫子施用。此类组合物的非限制性实例包括免洗型皮肤乳剂、霜剂、粉底、免晒美黑剂和防晒乳剂。
本文所指的折射率值是在25℃和589nm波长下测定的。
在提及一次粒子的粒径的情况下，这意味着粒径(直径)是能够通过诸如S.Gu等在Journal of Colloid and Interface Science,289(2005)419-426页描述的方法，通过透射电子显微镜(TEM)可测量的。
除了在实施例中，或者另外被明确指出情况之外，本说明书中的表示材料的量或者反应条件、材料物理性质和/或用途的所有数字可以理解为任选地被词语“约”所修饰。除非另有说明，所有量均按最终组合物的重量计。本文使用的术语“固体”是指材料在25℃下不是流体。应该注意的是，在指定任何范围的值时，给定的上限值可以与任何下限值相关联。为免生疑问，词语“包含”旨在意指“包括”，但不必是“由…构成”或“由…组成”。换言之，所列步骤或者选项不必是穷尽的。在此发现的本发明公开内容应被认为覆盖了如权利要求彼此之间是多重从属的权利要求中所发现的所有实施方案，与可能发现权利要求没有多重从属性和冗余性的事实无关。
在针对本发明的特定方面(例如，本发明的组合物)公开了某特征的情况下，这样的公开也应被认为是在必要的修改后适用于本发明的任何其他方面(例如，本发明的方法)。
发明详述
复合颗粒
能够通过本发明的方法获得的复合颗粒包含沉积在片状无机材料上的无孔球形微粒无机材料。换言之，无孔球形微粒无机材料粘附在片状无机材料上。
微粒无机材料的折射率大于所述片状无机微粒材料的折射率。
优选的片状无机材料是云母、滑石、蒙脱石、高岭土、石墨、片状氧化铁、玻璃鳞片、绢云母、片状二氧化硅、石墨烯、片状氧化铝、气相氧化铝、氧化铝水合物、氢氧化铝和铝沉积膜、硫酸钡、氯氧化铋、勃姆石、硼硅酸铝钙、碳酸钙、粘土、胶原、胶体二氧化硅、刚玉、硅藻、硅藻泥、硅藻土、三水铝石、鸟嘌呤、石墨、六方氮化硼、硅酸镁、云母氧化铁、叶蜡石或干涉云母，如Timica FR530、Timica V或Soft Luster White。
这种材料通常具有范围从约10,000至约30,000nm的平均粒径D50。对于片状材料，平均粒径是数均值。假定片晶具有圆形形状，其中圆形表面的直径对多个颗粒取平均值。片状颗粒的厚度被认为是单独的参数。例如，片状材料或片晶可以具有35,000nm的平均粒径和400nm的平均厚度。出于本文的目的，厚度被认为在约100至约600nm的范围内。激光散射可用于进行测量，只是光散射数据必须从球形到非球形进行数学校正。光学和电子显微镜可用于确定平均粒径。厚度通常仅通过光学或电子显微镜确定。
优选的是，这种材料的折射率为至少约1.8，通常为约1.9至约4，更优选为约2至约3，最佳为约2.5至约2.8。
片状材料的尺寸也可以很重要，因为较小的颗粒反射太少的光而不易被发现，而较大的颗粒将以离散物体的形式可见，从而提供过多的闪光或反射。片状晶体的反射率(折光率)(index of refraction)不能太高。太高的折光率会抑制自然肤色的传输并产生化妆品光泽。折光率太低时，颗粒将具有与皮肤或产品薄膜大致相同的折光率，导致反射弱，从而减弱了发光的外观。
光反射颗粒的说明性但非限制性实例是氯氧化铋(单晶片晶)和二氧化钛涂覆的云母。合适的氯氧化铋晶体可从EM Industries,Inc.以商标
NLY-L-2X CO和
Silver CO(其中片晶分散在蓖麻油中)；
Liquid Silver(其中颗粒分散在硬脂酸酯中)；以及
IGO、
C2X和
Platinum 25(其中片晶分散在硝化纤维中)获得。最优选的是其中氯氧化铋分散在C2-C40烷基酯中的体系，如
Silver。
在合适的二氧化钛涂覆的云母片晶中的是可从EM Industries,Inc.获得的材料。这些材料包括
(粒径范围10,000-30,000nm)、
(粒径范围5,000-30,000nm)、
(粒径范围2,000-20,000nm)、
(粒径范围5,000-45,000nm)、
(粒径范围5,000-40,000nm)、
(粒径范围5,000-20,000nm)、
(粒径范围10,000-40,000nm)、
(粒径范围10,000-40,000)、
(粒径范围10,000-40,000nm)，以及
(粒径范围10,000-40,000nm)。最优选的是
二氧化钛涂层与云母片晶的重量比按重量计可以为约1∶10至约5∶1，优选约1∶1至约1∶6，更优选约1∶3至约1∶4。有利地，除了涂覆云母所需的二氧化钛之外，优选的组合物通常基本上不含二氧化钛。
除二氧化钛以外的合适的云母涂层也可以获得本发明所需的适当的光学特性。这些类型的涂覆云母还必须满足至少约1.8的折射率。其他涂层包括云母片晶上的二氧化硅。
优选地，无孔球形微粒无机材料是氧化铝、氧化铋、氧化铈、氧化铬、氧化铁(II)、氧化铁(II、III)、氧化铁(III)、硅酸镁、二氧化硅、二氧化钛、氧化锌、氧化锆，以及它们的混合物或合金。或者，二氧化硅(Silicon dioxide)也称为硅石(silica)。
为了能够在这个意义上获得最佳效果，球形材料的直径优选小于片状材料的。由于具有约1至500μm的最大直径的片晶材料特别合适，因此优选具有约0.05至50μm范围内的直径的球形材料。优选的是，无孔球形微粒无机材料的粒径为50至1000nm。
粒径范围为约3至15μm的基于SiO2的球形颗粒例如作为高压液相色谱的材料是已知的，并且例如由E.Merck,Darmstadtt以
销售。优选地，片状材料具有大于球形颗粒的直径约10至20倍的直径。
然而，特别优选使用甚至更细碎的材料，尤其是粒度在约0.05至1μm范围内的材料。这种颗粒优选以单分散形式使用，也就是说；具有尽可能均匀的粒径。单分散TiO2的商业来源是意大利Novara的Istituto Guido Donegani。
特别优选的是，当无孔球形微粒无机材料是二氧化硅时，片状无机材料是云母。
根据本发明，球形材料占片状材料总表面积的20至80％，更优选地25至80％。
进一步根据本发明，球形材料的量占复合颗粒的2至20重量％。优选地，余量是片状材料。
进一步优选地，无孔球形微粒无机材料以单层沉积在片状无机材料上。
在复合材料的合成过程期间，通过控制无孔球形微粒无机材料与片状无机材料之间的进料比，就可以操控或调整覆盖率。通过增加此覆盖率，可以增加模糊效果并降低光泽。
广泛用于产生模糊效果或柔焦的已知技术基于微粒有机硅弹性体、二氧化硅或其他常规模糊颗粒。这种颗粒确实会产生哑光感。然而，如果期望增加或增强使用传统的模糊颗粒实现的模糊效果，则外观暗淡无光亮，因为入射光主要被颗粒漫射。然而，如果想要通过添加油或云母来增加光泽(这可以增加镜面反射率)，则可能会影响模糊效果。
一些市售的复合材料具有随机量的例如涂覆在云母上的二氧化硅，通过诱导一些偶联剂如硅烷或钛酸酯，二氧化硅球可以涂覆在云母上，而一些在云母表面上或之外形成聚集体。然而，除非在合成中使用过量的二氧化硅球体，否则无法实现如本发明中公开和要求保护的那些高覆盖率的复合材料。
合成方法
根据本发明，公开了一种制备复合颗粒的方法，该复合颗粒包含沉积在片状无机材料上的无孔球形微粒无机材料，其中所述微粒无机材料的折射率大于所述片状无机微粒材料的折射率，其中所述球形材料占所述片状材料总表面积的20至80％，并且其中所述球形材料的量占所述复合颗粒的2至20重量％，进一步地其中所述片状无机材料为云母，并且所述无孔球形微粒无机材料为二氧化硅，所述方法包括以下步骤：
(i)将所述片状无机材料硅烷化，以得到具有官能团“A”的硅烷化材料；
(ii)将所述无孔球形微粒无机材料硅烷化以得到具有官能团“B”的硅烷化材料，其中A≠B；并且其中所述“A”和所述“B”能够彼此反应，使得通过它们的反应，所述无孔球形微粒无机材料沉积在所述片状无机材料上；和
(iii)使所述具有官能团“A”的硅烷化材料与所述具有官能团“B”的硅烷化材料反应。
优选的是，片状无机材料为云母。进一步优选的是，无孔球形微粒无机材料是二氧化硅。
优选通过首先在醇介质中使云母与(3-氨基丙基)三乙氧基硅烷(APTES)反应得到胺改性的云母，然后在二甲基甲酰胺介质中使胺改性的云母与琥珀酸酐反应，得到具有官能团“A”的硅烷化材料，从而使云母硅烷化，其中A是羧酸基团。另外优选地，通过在醇介质中使二氧化硅与(3-氨基丙基)三乙氧基硅烷(APTES)反应，得到具有官能团“B”的硅烷化材料，从而硅烷化二氧化硅，其中B是氨基。然后在(1-(3-二甲基氨基丙基)-3-乙基碳二亚胺)[EDC]和N-羟基琥珀酰亚胺[NHS]的存在下，使具有官能团“A”的硅烷化材料与具有官能团“B”的硅烷化材料反应。
本发明的化妆品组合物
根据另一方面，公开了一种包含本发明第一方面的复合颗粒的化妆品组合物。优选地，组合物包含0.2至10重量％、更优选地0.5至5重量％且最优选地0.5至4重量％的复合颗粒。
优选地，该组合物另外包含一种或多种以下成分。
如本文所用，“有机硅弹性体”是指具有粘弹性质的可变形有机聚硅氧烷。优选地，化妆品组合物包含有机硅弹性体。
优选的是，有机硅弹性体是交联的。有机硅弹性体可由可固化的有机聚硅氧烷获得。这方面的实例是：通过含SiH的二有机聚硅氧烷与具有硅键合乙烯基的有机聚硅氧烷之间的加成反应，在铂金属催化下固化的加成反应-固化有机聚硅氧烷组合物；通过羟基封端的二有机聚硅氧烷与含SiH的二有机聚硅氧烷之间的脱氢反应，在有机锡化合物存在下固化的缩合-固化的有机聚硅氧烷组合物；通过羟基封端的二有机聚硅氧烷与可水解的有机硅烷之间的缩合反应(此缩合反应以脱水、醇释放、肟释放、胺释放、酰胺释放、羧基释放和酮释放反应为范例)，在有机锡化合物或钛酸酯存在下固化的缩合-固化有机聚硅氧烷组合物；在有机过氧化物催化剂存在下热固化的过氧化物-固化有机聚硅氧烷组合物；以及通过高能辐射固化的有机聚硅氧烷组合物，例如通过γ射线、紫外线辐射或电子束。有机硅弹性体优选地通过加成反应-固化有机聚硅氧烷组合物获得，该组合物通过含SiH的二有机聚硅氧烷与具有硅键合乙烯基的有机聚硅氧烷之间的加成反应，在铂金属催化下固化。
有机硅弹性体可以是乳化的或非乳化的交联有机硅弹性体或其组合，但是优选地，有机硅弹性体是非乳化的。如本文所用，术语“非乳化”定义了不存在聚氧化烯单元的交联的有机硅弹性体。如本文所用，术语“乳化”是指具有至少一个聚氧化烯(例如，聚氧化乙烯或聚氧化丙烯)单元的交联的有机聚硅氧烷弹性体。
优选的有机硅弹性体是可以以聚二甲基硅氧烷(dimethicone)/乙烯基聚二甲基硅氧烷交联聚合物、聚二甲基硅氧烷交联聚合物和聚硅氧烷-11的INCI名称获得的有机聚硅氧烷。更优选地，有机硅弹性体体是聚二甲基硅氧烷/乙烯基聚二甲基硅氧烷交联聚合物。
通常可得且合适弹性体是DC9509(63％固含量)聚二甲基硅氧烷/乙烯基聚二甲基硅氧烷交联聚合物(和)C12-14 Pareth-12。DOW CORNING 9509有机硅弹性体悬浮体是球状有机硅弹性体粉末在水中的63％的非离子悬浮体。
优选地，本发明的化妆品组合物包含0.1至10重量％的有机硅弹性体，更优选0.5至8重量％，甚至更优选1至5重量％。
优选地，载体包含不是弹性体的硅酮。
硅酮可以分为挥发性种类和非挥发性种类。挥发性硅油(如果使用了的话)优选地选自含有3至9个，优选4至5个硅原子的环状(环甲硅油)或线性聚二甲基硅氧烷。
非硅酮润肤剂的具体例子包括硬脂醇、甘油单蓖麻油酸酯、貂油、鲸蜡醇、异硬脂酸异丙酯、硬脂酸、棕榈酸异丁酯、硬脂酸异鲸蜡酯、油醇、月桂酸异丙酯、月桂酸己酯、油酸癸酯、十八烷基-2-醇、异鲸蜡醇、二十烷醇、山萮醇、棕榈酸鲸蜡酯、诸如二甲基聚硅氧烷之类的硅油、癸二酸二正丁酯、肉豆蔻酸异丙酯、棕榈酸异丙酯、硬脂酸异丙酯、硬脂酸丁酯、聚乙二醇、三甘醇、羊毛脂、可可脂、玉米油、棉籽油、橄榄油、棕榈仁油、菜籽油、红花籽油、月见草油、大豆油、葵花籽油、鳄梨油、芝麻籽油、椰子油、花生油、蓖麻油、乙酰化羊毛脂醇、矿脂、矿物油、肉豆蔻酸丁酯、异硬脂酸、棕榈酸、亚油酸异丙酯、乳酸月桂酯、乳酸肉豆蔻酯、油酸癸酯、肉豆蔻酸肉豆蔻酸酯，以及它们的混合物。
以
品牌出售的C12-15烷基苯甲酸酯也特别有用。
或者，载体包含按组合物的重量计1至25重量％的脂肪酸或0.1至80重量％的皂。脂肪酸与皂的混合物也是合适的，例如形成雪花膏基质，这使皮肤具有哑光感。特别优选的是C12-20脂肪酸，更优选的是C14-18脂肪酸。最优选的脂肪酸是硬脂酸、肉豆蔻酸或它们的混合物。当存在时，组合物包含5至20重量％的脂肪酸或皂。疏水性材料中的皂类可以包括脂肪酸的碱金属盐，如钠盐或钾盐，最优选的是硬脂酸钾。通常，化妆品组合物中的雪花膏基质是通过取所需量的总脂肪物质并与所需量的氢氧化钾进行混合来制备的。所述皂通常在混合期间原位形成。
优选地，载体包含水。依据组合物的性质，水的量可以按化妆品组合物的重量计例如为1至85％，更优选5至90％，甚至更优选35至80％，最佳在40至70％之间。
进一步优选地，本发明的组合物包含亮肤剂。亮肤剂优选地选自以下中的一种或多种：维生素B3化合物或其衍生物，例如尼克酸、烟酸或烟酰胺或其他公知的亮肤剂，例如阿达帕林、芦荟提取物、乳酸铵、茴香脑衍生物、苹果提取物、熊果苷、壬二酸、曲酸、竹提取物、熊果提取物、白芨块茎、柴胡提取物、地榆提取物、丁基羟基茴香醚、丁基羟基甲苯、柠檬酸酯、川芎、当归、脱氧熊果苷、1,3-二苯丙烷衍生物、2,5-二羟基苯甲酸及其衍生物、2-(4-乙酰氧苯基)-1,3-代森锌、2-(4-羟苯基)-1,3-代森锌、鞣花酸、七叶醇(escinol)、草蒿脑衍生物、渐隐(Fadeout)(Pentapharm)、防风、茴香提取物、灵芝提取物、藁本、加图林美白(Gattlefosse)、遗传酸及其衍生物、光甘草定及其衍生物、葡萄糖吡喃糖基-1-抗坏血酸盐、葡萄糖酸、乙醇酸、绿茶提取物、4-羟基-5-甲基-3[2H]-呋喃酮、氢醌、4-羟基茴香醚及其衍生物、4-羟基苯甲酸衍生物、羟基辛酸、肌醇抗坏血酸酯、柠檬提取物、亚油酸、抗坏血酸磷酸镁、美拉白(Pentapharm)、桑树提取物、桑根提取物、5-辛酰基水杨酸、欧芹提取物、桑黄提取物、焦棓酚衍生物、2,4-间苯二酚衍生物、3,5-间苯二酚衍生物、玫瑰果提取物、水杨酸、Song-Yi提取物、3,4,5-三羟基苄基衍生物、氨甲环酸、维生素类如维生素B6、维生素B12、维生素C、维生素A、二羧酸、间苯二酚衍生物、来自植物即茜草属和山矾属的提取物、羟基羧酸(如乳酸)及其盐(如乳酸钠)，以及它们的混合物。维生素B3化合物或其衍生物如尼克酸、烟酸或烟酰胺是根据本发明更优选的亮肤剂，最优选的是烟酰胺。烟酰胺在使用时优选0.1-10重量％，更优选0.2-5重量％。
化妆品可接受的载体中可包括的其他材料包括湿润剂、增稠剂和粉末。
组合物可以任何已知的形式配制，更优选的形式是霜剂和乳剂。本发明的化妆品组合物可以进一步包含本领域中常见的其他成分，以增强物理性质和性能。合适的成分包括但不限于：粘合剂、着色剂和颜料、pH调节剂、防腐剂、光学剂、香料、粘度调节剂、生物添加剂、缓冲剂、调理剂、天然提取物、精油以及皮肤有益剂，包括抗炎剂、凉爽剂、止汗剂、抗衰老剂、抗痤疮剂、抗微生物剂和抗氧化剂。
本发明的化妆品组合物是适合局部施用于人类皮肤的组合物，包括免洗型和洗去型产品。优选的是，本发明的组合物是免洗型组合物。
可以将所述组合物适当地包装在大小合适的包装物或分配器中。包装物可以是罐子或管，以及用于化妆品、霜剂、洗涤和乳剂类产品的常见的任何其他形式。组合物可以局部施用，并且优选地每平方厘米的皮肤施用1至4毫克的组合物。
方法和用途
本发明还公开了能够通过第一方面的方法获得的复合颗粒在化妆品组合物中用于增强皮肤光泽的用途。
本发明还公开了能够通过第一方面的方法获得的复合颗粒在化妆品组合物中用于遮盖皮肤表层瑕疵的用途。
本发明进一步公开了一种增强皮肤光泽的方法，包括向其施用包含能够通过本发明第一方面的方法获得的复合颗粒的化妆品组合物的步骤。
本发明还进一步公开了一种遮盖皮肤表层瑕疵的美容方法，包括向其施用包含能够通过本发明第一方面的方法获得的复合颗粒的化妆品组合物的步骤。
本发明还公开了能够通过第一方面的方法获得的复合颗粒在制备用于增强皮肤光泽的化妆品组合物中的用途。
本发明还进一步公开了能够通过该方法获得的第一方面的复合颗粒在制造用于遮盖皮肤表层瑕疵的化妆品组合物中的用途。
提供下面的实施例是为了促进对本发明的理解。这些实施例不是为了限制权利要求的范围。
具体实施方式
实施例
实施例1：根据本发明的复合颗粒的制备：
使用了以下材料：
(i)粒径为50nm的硅溶胶(silica sol)
(j)N-(3-二甲基氨基丙基)-N’-乙基碳二亚胺盐酸盐(EDC)
(k)(3-氨基丙基)三乙氧基硅烷(APETS)
(l)琥珀酸酐(SA)
(m)N-羟基琥珀酰亚胺(NHS)
(n)二甲基甲酰胺(DMF)
(o)云母，以Mica
商标名称来自JGC Corporation。
步骤1：二氧化硅纳米颗粒的硅烷化
将一(1)mL APTES逐滴加入10ml的二氧化硅纳米颗粒的乙醇分散体(0.1g/mL)中并搅拌两小时。通过离心分离和洗涤产物。将氨基改性的二氧化硅纳米颗粒收集为水分散体(0.1g/mL)以供进一步使用，并且所有反应均在室温下进行。
步骤2：云母片材的羧化
在搅拌10分钟下将一(1)g研磨的云母分散到100ml乙醇中以制备云母分散体，然后将1mL APTES逐滴加入云母分散体中并搅拌另外2小时。通过离心分离和洗涤产物，然后将得到的氨基改性的研磨云母重新分散在DMF中。将100mg SA以粉末形式加入分散体中，然后将分散体保持搅拌另外2小时。通过离心分离和洗涤产物，以粉末的形式收集所得羧基改性的研磨云母以供进一步使用，所有反应均在室温下进行。
步骤3：云母片材和二氧化硅纳米颗粒的酰胺化连接
在搅拌下将五(5)g改性的研磨云母分散到8ml去离子水中以制备云母分散体。将两(2)mL一定浓度的改性二氧化硅纳米颗粒分散体(500mg/mL、100mg/mL、50mg/mL)逐滴加入云母分散体中。然后将200mg EDC和200mg NHS以粉末的形式加入到混合分散体中。反应在搅拌下进行两小时。
通过调节二氧化硅纳米颗粒的添加量，实现了纳米颗粒在片材表面上的各覆盖率。
分析方法
在以100kV的加速电压操作的H-7650(Hitachi,Japan)上进行透射电子显微镜检查(TEM)。使用场发射扫描电子显微分析仪(Zeiss Supra 40)在5kV的加速电压下进行扫描电子显微镜(SEM)检查。通过Image J分析复合材料的SEM图像，以通过二氧化硅和云母基材的亮度对比来估计云母表面上的二氧化硅覆盖率。
三种不同类型的复合颗粒用上述方法制备。有关颗粒的信息示于表1中。
表面覆盖率
表面覆盖率定义为无孔球形微粒无机材料覆盖的面积与片状无机材料覆盖的面积之比。
在以100kV的加速电压操作的H-7650(Hitachi,Japan)上进行透射电子显微镜检查(TEM)。使用场发射扫描电子显微分析仪(Zeiss Supra 40)在5kV的加速电压下进行扫描电子显微镜(SEM)检查。通过Image J分析复合材料的SEM图像，以通过二氧化硅和云母基材之间的亮度对比确定表面覆盖率。
使用名为Image J(版本1.51K)的市售软件来测量面积。该过程在下文中以逐步的方式详述。
步骤1通过选择文件(File)→打开样例(Open samples)→命名SEM文件来打开SEM图像
步骤2如果不是灰度，则将图像转换为灰度：图像(Image)→类型(Type)→8-bit(8位)
步骤3 Sep测量刻度：在SEM图像底部上的比例尺上画一条线，然后分析(Analyze)→设定刻度(Set Scale)。画一条新线并确认测量刻度是正确的。
步骤4使用手动设置对新的图像设置阈值：图像(Image)→调节(Adjust)→阈值(Threshold)，拖动滑块以将片晶上的所有球形颗粒都包含在红色中，并点击“应用(Apply)”。手动阈值设置包括所有颗粒区域。
步骤5计算所有球形颗粒的面积：用矩形选择工具将分析区域围起来：分析(Analyze)→分析颗粒(Analyze Particles)。在窗口中，切换“显示轮廓(showoutlines)”，选中“显示结果(Display Results)”、“总结(Summary)”和“忽略边缘颗粒(Exclude on edges)”，然后单击“OK”。
自动绘制球形颗粒的轮廓。数据窗口给出了面积％的比例，该比例是表面覆盖率。
表1
| 低表面覆盖率复合颗粒 | 3.5％二氧化硅和96.5％云母 | 24％覆盖率 |
| 中等表面覆盖率复合颗粒 | 4.7％二氧化硅和95.3％云母 | 34％覆盖率 |
| 高表面覆盖率复合颗粒 | 19％二氧化硅和81％云母 | 76％覆盖率 |
在SEM图像中，由于二氧化硅的导电性较差，二氧化硅看起来比云母更亮。因此，二氧化硅在云母上的覆盖率可以等同于亮区的比例。对于高表面覆盖率复合颗粒，覆盖率高达76％。进一步地观察到，所有二氧化硅球在云母表面上形成单层。
实施例2
将表1的复合材料配制成护肤组合物。表2示出了组合物的基本细节，其需要与表3的交叉引用内容一起阅读。
表2
表3
注意：
以下缩略语已用于表示某些已测试的市售材料。
SS：购自Merck的RonaFlair
TiO2(33-41％)/SiO2(28-34％)云母(20-37％)Al2O3(2-5％)，云母<15μm
3H：MSS-500/3H，KOBO，用于模糊功效的市售多孔硅胶
CC6097 Momentive湍流状氮化硼<5μm
V640：购自JGC的Velvet
640，40％的涂覆在云母A上的二氧化硅(600nm)
S6：
S6:JGC，63.7％的涂覆在云母A上的二氧化硅(600nm)
S3：购自JGC的
S3，48％的涂覆在云母A上的二氧化硅(300nm)
AR 80：购自JGC的
AR-80，滑石∶TiO2∶Al2O3∶SiO2＝55∶10∶16∶19
KII：
KII：JGC，46.5％的涂覆在云母A上的二氧化硅(300nm)
VA:购自JGC的Velvet
A，～8％的涂覆在云母A上的二氧化硅(300nm)
V310：购自JGC的Velvet
310，10％的涂覆在云母A上的二氧化硅(300nm)
A55：购自JGC的
55，固体二氧化硅球，600nm
A250：AE1：250nm二氧化硅球
MII：购自BASF的
II，云母，35μm
MCF：购自BASF的
CF，云母，25μm
DC9509：购自Dow corning的有机硅弹性体颗粒(63％活性物质)
TR-10：Miyoshi Kasei Inc.，93％TiO2，4％Al2O3，3％聚二甲基硅氧烷，～700nm
实施例参考编号A和B含有两种颜料的组合，C含有三种颜料/颗粒，组合物D至M含有单一的市售复合颗粒，组合物N至Q含有市售复合颗粒的组合，R含有颗粒的组合，组合物S、T和U(均在本发明内)含有根据本发明的复合颗粒。
模糊指数
该指数是组合物在遮蔽皮肤表层瑕疵方面有多好的指标。模糊指数(也称为L&W指数)是通过两步法测量的。在第一步骤中，在施用任何化妆品组合物之前，测量人造皮肤的光泽度。
由聚氨酯弹性体制成的起皱生物皮肤板(BP-EW1#BSC，日本东京的Beaulax Co.,Ltd.)被用来模拟起皱的人类皮肤。在下文中，将它们缩写为BSP。按照Matsubara等人在[Skin Translucency:What Is It&How Is It Measured,The International Federationof Societies of Cosmetic Chemists(IFSCC)Congress 2006,Osaka,Japan]中描述的方法和原理，采用被称为SAMBA(Bossa Nova Technologies，美国)的双偏振图像系统来测量BSP的光泽度。使用名为SAMBA脸系统(版本4.3)的软件进行分析。在曝光时间为80毫秒的情况下相对于入射光测试BSP。使用了两种操作模式：平行极化和交叉极化。此后，在其上施用28mg的相关组合物，并通过手指套(cot)将其分散在7cm2的圆形区域内。在进一步测试之前，使样品静置干燥30分钟。此后，如之前所做的一样再次测量光泽度。
在第二步骤中，L&W(细纹和皱纹)指数按如下进行确定。
入射光被BSP反射和散射。镜面反射光保持与入射光相同的极化，而来自体积的散射光(漫射光)则是未极化的。相机连续地获取与两个极化状态(平行和交叉)相对应的两张图像。平行图像的强度(P)由反射光和散射光贡献，而交叉图像强度(C)由散射光贡献。平行图像加上交叉图像等于传统相机所传递的或人眼所感知的总图像。光泽度按如下：(P-C)/(P+C)。此后，计算每个像素的光泽度。光泽度的标准偏差(STD)是皮肤外观均匀性的量度。偏差越高，均匀性就越低。L&W指数由以下等式计算：
(施用样品前的光泽度的STD-施用样品后的光泽度的STD)/(施用样品前的光泽度的STD)
该指数与组合物在遮蔽皮肤表层瑕疵的功效方面成正比。
数据如表4所示。
表4
实施例参考编号D是包含Velvet
640，40％涂覆在云母A上的二氧化硅(600nm)的组合物就模糊指数和光泽度而言显示出最佳性能。然而，结果表明，实施例S、T和U(均在本发明的范围内)的性能与实施例D的性能相当，并且在S、T和U中，组合物U显示出最好的性能，即高光泽度和隐藏皮肤表层瑕疵的更好能力，如模糊指数所示的。组合物U含有包含19％二氧化硅和81％云母的高表面覆盖率的复合颗粒，其中球形材料(二氧化硅)占片状材料(云母)总表面积的76％。另一方面，V640包含40％的涂覆在云母A上的二氧化硅(600nm)，云母A形成余量60％。
较暗的部分，如起皱皮肤的凹处是黑暗的，因为光线无法到达凹处的深处。然而，在组合物S、T和U的情况下，较亮部分和较暗部分之间的对比更加明显。增加的模糊指数可能意味着增加且均匀明亮的像素，并且随着光泽度的增加，皮肤的更精细纹理可以更好地可见。
从组合物A和B获得的模糊指数和光泽度足够高，但这是成分/颗粒组合的结果。与V640所提供的相比，从组合物E向前到R，模糊指数或光泽度中的至少一个过低。
Claims (12)
1.一种制备复合颗粒的方法，所述复合颗粒包含沉积在片状无机材料上的无孔球形微粒无机材料，其中所述微粒无机材料的折射率大于所述片状无机微粒材料的折射率，其中所述球形材料占所述片状材料总表面积的20至80％，并且其中所述球形材料的量占所述复合颗粒的2至20重量％，进一步地，其中所述片状无机材料为云母，并且所述无孔球形微粒无机材料为二氧化硅，所述方法包括以下步骤：
(i)将所述片状无机材料硅烷化，以得到具有官能团“A”的硅烷化材料；
(ii)将所述无孔球形微粒无机材料硅烷化以得到具有官能团“B”的硅烷化材料，其中A≠B；并且其中所述“A”和所述“B”能够彼此反应，使得通过它们的反应，所述无孔球形微粒无机材料沉积在所述片状无机材料上；和
(iii)使所述具有官能团“A”的硅烷化材料与所述具有官能团“B”的硅烷化材料反应。
2.根据权利要求1所述的方法，其中A是羧酸基团。
3.根据权利要求1所述的方法，其中B是氨基。
4.根据权利要求1所述的方法，其中所述无孔球形微粒无机材料的粒径为50nm至1000nm。
5.根据前述权利要求1或2中任一项所述的方法，其中所述无孔球形微粒无机材料以单层沉积在所述片状无机材料上。
6.能够通过根据前述权利要求1至5中任一项所述的方法获得的复合颗粒。
7.能够通过根据前述权利要求1至5中任一项所述的方法获得的复合颗粒在化妆品组合物中用于增强皮肤光泽的用途。
8.能够通过根据权利要求1至5中任一项所述的方法获得的复合颗粒在化妆品组合物中用于遮蔽皮肤表层瑕疵的用途。
9.一种增强皮肤光泽的方法，该方法包括向皮肤施用包含能够通过权利要求1至5中任一项所述的方法获得的复合颗粒的化妆品组合物的步骤。
10.一种遮盖皮肤表层瑕疵的美容方法，该方法包括向皮肤施用包含能够通过权利要求1至5中任一项所述的方法获得的复合颗粒的化妆品组合物的步骤。
11.能够通过根据权利要求1至5中任一项所述的方法获得的复合颗粒在制备用于增强皮肤光泽的化妆品组合物中的用途。
12.能够通过根据权利要求1至5中任一项所述的方法获得的复合颗粒在制备用于遮蔽皮肤表层瑕疵的化妆品组合物中的用途。
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