CN103210030B - 复合颗粒和具有复合颗粒的组合物 - Google Patents
复合颗粒和具有复合颗粒的组合物 Download PDFInfo
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- CN103210030B CN103210030B CN201180056362.7A CN201180056362A CN103210030B CN 103210030 B CN103210030 B CN 103210030B CN 201180056362 A CN201180056362 A CN 201180056362A CN 103210030 B CN103210030 B CN 103210030B
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- specific refractory
- refractory power
- composite particles
- polymeric matrix
- submicron particle
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Abstract
记述了复合颗粒和具有复合颗粒的组合物。所述颗粒具有含有或不含有空穴的聚合物基体和亚颗粒,由此亚颗粒具有高于和低于聚合物基体折射率的折射率。当通常施加时,该组合物在用户的皮肤上赋予优异的柔焦结果。
Description
技术领域
本发明涉及复合颗粒以及包含该复合颗粒的组合物。更特别地,该复合颗粒包含聚合物基体,该聚合物基体包含折射率高于聚合物基体折射率的亚颗粒(subparticle)以及折射率低于聚合物基体折射率的亚颗粒和/或空穴。包含所述复合颗粒的组合物具有优异的感官特性,并且令人惊奇地,与常规光散射颗粒(其为局部施用其的用户赋予改进的外观)相比展现了可测量的和显著更高的柔焦。
发明背景
许多用户期望看上去更年轻并且降低尤其是在他们面部和手上的瑕疵、细纹和皱纹的可见性。这种需求与这样的事实相联系,用户希望看上去容光焕发并且是自然的,而不存在传统的粉底基产品(其本质上倾向于过度不透明并且可能具有审美和/或文化上的负面作用)通常提供的人工的无光泽外观(artificial matte
look)。
已经做出了“完美”皮肤的尝试。通常,制备了具有吸收剂填料(例如,滑石、硅石、高岭土)的局部组合物,其中这些无机填料与颜料一样吸收一些光并且简单地反射回光来掩盖皮肤缺陷。另一种替代方法被称为实现柔焦效应。当入射光被通过散射(分散)扭曲时(其中光被扭转到不同的方向),发生该效应。柔焦通常被认为是与朦胧化(haze)类似的方法,但可适用于薄产品膜。不幸的是,传统的方法要么掩盖缺陷但缺乏光采要么产生光采和健康的光泽但具有审美上令人不快的皮肤外观,例如,通过提高的皮肤形貌可视性。
对于研发能产生优异的柔焦的复合颗粒和具有复合颗粒的组合物存在日益增加的兴趣。因此,本发明涉及期望产生优异的感官特性并令人惊奇地赋予出众的柔焦结果的复合颗粒和包含这种复合颗粒的组合物。所述复合颗粒包含聚合物基体和具有或不具有空穴的亚颗粒,一些亚颗粒的折射率高于聚合物基体折射率且一些亚颗粒的折射率低于聚合物基体折射率。
附加信息
已经公开了制备赋予柔焦的组合物的努力。在US专利申请2008/0152682中,描述了包含单晶扁平状硫酸钡的组合物。
还已经公开了制备改善皮肤特性的局部组合物的其它努力。在US专利申请2005/0100568和2009/0155321中,描述了用于改善皮肤外观的化妆品组合物。
还已经公开了制备改善皮肤特性的局部组合物的另一些努力。在US专利5,972,359、5,997,890和6,174,533中,描述了覆盖皮肤缺陷的局部组合物。
上述附加信息均未描述本发明要求保护的复合颗粒和组合物。
发明概述
在第一方面,本发明涉及一种复合颗粒,包含:
(a) 聚合物基体;
(b) 折射率高于聚合物基体折射率的亚颗粒;和
(c) 折射率低于聚合物基体折射率的亚颗粒、空穴或二者。
在第二方面,本发明涉及包含本发明第一方面的复合颗粒的组合物。
在第三方面,本发明涉及通过向皮肤施加本发明第二方面的组合物来改善皮肤特性的方法。
在考虑以下详细的说明和实施例之后,本发明的所有其它方面将更容易变得显而易见。
如本文所使用的,皮肤旨在包括在面部、颈部、胸部、背部、手臂、手、腿、臀部和头皮上的皮肤。如本文所使用的,亚颗粒,旨在表示小于复合颗粒但为其组分的颗粒。复合颗粒和亚颗粒优选表示球状颗粒,由此亚颗粒的直径通常可以比复合颗粒的直径小10-2100倍。亚颗粒意在分散在整个聚合物基体中。在未形成完美球体的程度,直径旨在表示在颗粒上可测量的最长的横截面距离。如本文所使用的,空穴是指填充有真空或空气的间隙、空间或口袋(pocket),并且优选通过使用致孔剂(如乙酸乙酯)获得。这种空穴可以与折射率低于聚合物基体折射率的亚颗粒一起使用或代替折射率低于聚合物基体折射率的亚颗粒使用。可以可替换地使用低和低于,高和高于来分别描述低折射率亚颗粒和高折射率亚颗粒。可以例如通过扫描电子显微镜(SEM)测量复合颗粒的直径。可以例如通过透射电子显微镜(TEM)测量亚颗粒和/或空穴的直径。可以通过本领域常规的方法测定折射率,优选用波长为589nm的光在25℃下测量。
如本发明所使用的,包含旨在包括基本由…组成和由…组成。如果例如没有明确提及,则本文确定的所有范围都旨在包括包含在其中的所有范围。
优选实施方案的详细说明
对于可以用于本发明的聚合物基体的唯一限制为该基体适用于局部施加的组合物并且具有在所使用的亚颗粒的折射率之间的折射率。通常,聚合物基体具有1.3-1.8的折射率,并且优选1.4-1.7,和最优选1.45-1.7,包括所有其中包含的范围。在一个通常优选的实施方案中,在本发明中使用的聚合物基体为可以衍生自适于经受自由基聚合的单体的聚合物基体。
对于聚合物基体在本发明中可以使用的示例性而非限制性的单体类型的实例包括苯乙烯和其衍生物,如1-甲基-4-乙烯基苯、1-叔丁基-4-乙烯基苯、1-溴-4-乙烯基苯、1-甲氧基-4-乙烯基苯、4-乙烯基苯乙酸酯,和丙烯酸酯,如丙烯酸2-羟乙酯(HEA)、丙烯酸叔丁酯(t-BA)、甲基丙烯酸甲酯(MMA)、甲基丙烯酸2-(二甲基氨基)乙酯(DMAEMA)、甲基丙烯酸2-羟乙酯(HEMA)、甲基丙烯酸缩水甘油酯(GMA),和丙烯酰胺,如二甲基丙烯酰胺(DMA)、N-异丙基丙烯酰胺(NIPAM),和丙烯酸及其衍生物,如甲基丙烯酸,和丙烯腈,如甲基丙烯腈,和二烯,如4-乙烯基吡啶(4VP)、丙酸乙烯酯、丁酸乙烯酯、乙烯基醚、烯丙基丁基醚(allybutyl
ether)、烯丙基缩水甘油基醚、马来酸、乙酸乙烯酯以及它们的共聚物和由它们获得的聚合物的混溶和不混溶的共混物。在尤其优选的实施方案中,采用的单体为甲基丙烯酸甲酯和聚合物基体为聚(甲基丙烯酸甲酯)。
在另一尤其优选的实施方案中,聚合物基体具有比所用的折射率低于聚合物基体的亚颗粒的折射率高30-80%,并且优选高35-60%的折射率,和具有比所用的折射率高于聚合物基体的亚颗粒的折射率低10-50%,并且优选15-45%的折射率。
当需要更致密的复合颗粒时,可以任选地使用交联剂。可以使用的合适的交联剂包括,例如二乙烯基苯、1,4-二乙烯氧基丁烷、二乙烯砜、二烯丙基苯二甲酸酯、二烯丙基丙烯酰胺、三烯丙基异氰酸酯(tirallylisocyanurate)、三烯丙基偏苯三酸酯、二甲基丙烯酸乙二醇酯、二甲基丙烯酸丙二醇酯、四甲基丙烯酸季戊四醇酯、三甲基丙烯酸季戊四醇酯、二甲基丙烯酸季戊四醇酯、三羟甲基丙烷三甲基丙烯酸酯、六甲基丙烯酸二季戊四醇酯、五甲基丙烯酸二季戊四醇酯、三甲基丙烯酸甘油酯、其混合物等。当使用时,最优选的交联剂为二甲基丙烯酸乙二醇酯。通常,如果使用,基于聚合物基体的总重量交联剂占0.01-20、优选0.1-15、最优选0.5-10wt%。
通常,聚合物基体(不存在交联剂)具有75000-120万的分子量(Mn),并且优选100000-800000,和最优选400000-600000,包括所有包含在其中的范围。这种基体可由如Sigma-Aldrich的供应商商购。
折射率高于聚合物基体的折射率的亚颗粒(例如,折射率为1.65-3.0,和优选1.7-2.8,和最优选1.9-2.6,包括所有包含在其中的范围)的唯一限制是其可用于旨在局部施加的组合物。折射率高于聚合物基体折射率的亚颗粒类型的示例性实例为氧化锌、二氧化钛、氧化锆、氧化铁或其混合物。通常,这种亚颗粒具有约20-800nm的直径,并且优选25-500nm,和更优选30-400nm,包括所有包含在其中的范围。
所使用的这种高折射率亚颗粒的量通常为0.1-35wt%,和优选0.3-25wt%,和最优选8-20wt%,基于复合颗粒的总重量,并包括所有包含在其中的范围。
对于折射率低于聚合物基体折射率的亚颗粒,其通常具有1-1.4的折射率,和优选1-1.35,和最优选1.0-1.3,包括所有包含在其中的范围。这种亚颗粒的示例性实例包括包封了空气、气体或真空或其混合物的颗粒。通常,这些颗粒具有约50-800nm的直径,和优选60-700nm,和最优选70-600nm,包括所有包含在其中的范围。
这些亚颗粒可以具有壳(例如,包层或密封剂(encapsulant)),所述壳具有一种或多种非离子烯属不饱和单体。任选地,可以将一种或多种包含至少一个羧酸基团的单烯属不饱和单体在壳中聚合,例如,丙烯酸、甲基丙烯酸、丙烯酰氧基丙酸、甲基丙烯酰氧基丙酸、acotinic acid、马来酸、富马酸、衣康酸、柠康酸、它们的共聚物和它们的衍生物。优选的包含羧酸的单体为丙烯酸和甲基丙烯酸。当在壳中存在时,壳中通常包含0.1-12wt%的包含羧酸的单体。
在本发明的范围内,任选在壳中包含一种或多种不含羧酸基团的单烯属不饱和单体。这些包括例如,烯丙基磺酸、烯丙基膦酸、烯丙基氧基苯磺酸、2-甲基-2-丙烯-1-磺酸、乙烯基磺酸、苯乙烯磺酸、2-丙烯酰氨基-2-甲基-丙磺酸以及它们的衍生物和共聚物。当存在时,这些单体通常占壳总重量的0.1-12wt%。
在制备壳聚合物中可用的其它不饱和单体包括例如乙酸乙烯酯、丙烯腈、甲基丙烯腈、含氮环状化合物不饱和单体、乙烯基芳族单体、烯属单体和选择的(甲基)丙烯酸衍生物。优选地,基于壳部分的总重量,亚颗粒的壳部分包含0.001-90%的(甲基)丙烯酸衍生物单体和0.001-80%的乙烯基芳族单体作为聚合单元。
通常,基于壳部分的总重量,低折射率颗粒的壳包含5-95%,并且优选10-80%,并且最优选20-70%的(甲基)丙烯酸衍生物单体作为聚合单元,所述(甲基)丙烯酸衍生物单体选自以下的一种或多种:丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸丁酯、丙烯酸异丁酯、甲基丙烯酸异丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯、甲基丙烯酸二甲基氨基乙酯和甲基丙烯酸二甲基氨基丙酯。
在低折射率颗粒中用作壳的合适的乙烯基芳族单体包括例如,苯乙烯、α-甲基苯乙烯、乙烯基甲苯、烷基取代的苯乙烯(例如叔丁基苯乙烯和乙基乙烯基苯)、卤化的苯乙烯(例如氯苯乙烯和3,5-双(三氟甲基)苯乙烯)、乙基乙烯基苯、叔丁基苯乙烯和它们的共聚物。当在壳聚合物中存在时,基于聚合物颗粒壳部分的总重量,乙烯基芳族单体单元的量通常为1-85%,和优选5-75%,和最优选10-50%。
适用的含氮不饱和环状化合物单体的实例包括乙烯基吡啶、2-甲基-5-乙烯基吡啶、2-乙基-5-乙烯基吡啶、3-甲基-5-乙烯基吡啶、2,3-二甲基-5-乙烯基吡啶、2-甲基-3-乙基-5-乙烯基吡啶、甲基取代的喹啉和异喹啉(soquinoline)、1-乙烯基咪唑、2-甲基-1-乙烯基咪唑、N-乙烯基己内酰胺、N-乙烯基丁内酰胺和N-乙烯基吡咯烷酮和共聚物。
可以用于制备用于本发明组合物中的低折射率颗粒的壳的另外的合适单体包括烯属单体(例如,乙烯、丙烯、异丁烯、长链烷基α-烯烃(例如C10-C20烷基α-烯烃))、乙烯基卤化物(例如乙烯基氯化物、乙烯基氟化物、乙烯基溴化物)、亚乙烯基卤化物(例如亚乙烯基氯化物和亚乙烯基氟化物)、部分卤化的(甲基)丙烯酸酯(例如丙烯酸2-(全氟十二烷基)乙酯、甲基丙烯酸2-(全氟十二烷基)乙酯、丙烯酸2-(全氟己基)乙酯、甲基丙烯酸2-(全氟己基)乙酯、甲基丙烯酸六氟异丙基酯、丙烯酸2,2,3,3-四氟丙酯和甲基丙烯酸2,2,2-三氟乙酯),和部分卤化的烯烃(例如1,1,1-三氟-2,2-(三氟甲基)-丁烯)。这些亚颗粒是可商购的,其中本文优选使用的是可由Rohm and Haas以SunSphereTM名称商购的。
基于复合颗粒的总重量,所用的这种低折射率亚颗粒的量通常为0.1-20%,并且优选0.2-10%,和最优选0.3-6%,并且包括所有包含在其中的范围。聚合可以用引发剂(如过氧化苯甲酰)增强。
在另一尤其优选的实施方案中,在制备本发明的复合颗粒的过程期间,可以使用成孔剂或致孔剂,例如环己醇、甲苯、2-乙基己酸、二丁基苯二甲酸、1-甲基-2-吡咯烷酮、1-癸醇、庚烷、硅油、聚(亚烷基)二醇(poly(alkylene)
glycol)、乙酸乙酯或它们的混合物等。这些致孔剂可以用溶剂和/或热移除以在复合颗粒中产生空穴。这些空穴(其折射率将低于聚合物基体的折射率)可以与折射率低于聚合物基体折射率的亚颗粒一起使用或代替折射率低于聚合物基体折射率的亚颗粒。当存在空穴时,期望它们具有与折射率低于聚合物基体折射率的亚颗粒的尺寸一致的尺寸。此外,当单独使用或与低折射率亚颗粒结合使用时,聚合物基体中空穴的总量通常为0.1-30vol%,并且优选0.5-20vol%,并且最优选1-8vol%,基于聚合物基体的总体积,并包括所有包含在其中的范围。
在尤其优选的实施方案中,复合颗粒(优选原位制造)通常具有0.5-75微米的直径,并且优选1-50微米,并且最优选4-20微米,包括所有包含在其中的范围。
当制备组合物时,基于组合物的总重量,组合物通常包含0.1-20wt%,并且优选0.2-15wt%,并且最优选0.75-6wt%的复合颗粒,并且包括所有包含在其中的范围。
在包含本发明复合颗粒的组合物中可以存在各种材料以作为化妆品可接受的载体。这种载体可以例如为油包水、水包油的乳液,其中水包油型是优选的。最好水作为载体。水的量可以为组合物重量的约1-约90%,优选约30-约80%,任选地约50-约70%。
在本发明的组合物中可以包含润肤剂材料作为载体。这些可以为硅油、合成酯和烃的形式。润肤剂的量可以为组合物重量的约0.1-约95%、优选约1-约50%之间的任何范围。
硅油可以分为挥发性和非挥发性种类。本文所用的术语“挥发性”是指在环境温度(20-25℃)具有可测量的蒸气压的那些材料。挥发性硅油优选选自包含3-9优选4-5个硅原子的环状(环甲硅油)或线性聚二甲基硅氧烷。在根据本发明组合物的许多液体变体中,挥发性硅油可以形成组合物中较大的组分作为载体。量可以为组合物重量的约5-约80%,优选约20%-约70%。
可用作润肤剂材料的非挥发性硅油包括聚烷基硅氧烷、聚烷基芳基硅氧烷和聚醚硅氧烷共聚物。本文可用的基本上非挥发性的聚烷基硅氧烷包括例如在25℃具有约5 x 10-6 至0.1 m2/s粘度的聚二甲基硅氧烷。在本组合物中可用的优选的非挥发性润肤剂之中包括在25℃具有约1 x 10-s至约4 x
10-4 m2/s粘度的聚二甲基硅氧烷。
可以有益地采用有机聚硅氧烷交联聚合物。这些材料的代表为可由许多供应商获得的二甲硅油/乙烯基二甲硅油交联聚合物和二甲硅油交联聚合物,包括Dow Corning (9040, 9041, 9045, 9506和9509)、General Electric
(SFE 839), Shin Etsu (KSG-15, 16 和18 [二甲硅油/苯基乙烯基二甲硅油交联共聚物])、和Grant Industries (Gransil 商标的材料)、Shin Etsu提供的月桂基二甲硅油/乙烯基二甲硅油交联共聚物(例如,KSG-31、KSG-32、KSG-41、KSG-42、KSG-43 和KSG-44)。通常,上述硅油弹性体通常将以0.1-20wt%的量通常溶解在挥发性硅油(如环甲硅油)中。
当硅油作为载体大量存在并且还存在水时,体系可以是油连续的。这些通常将需要用油包水乳化剂(如二甲硅油共聚醇(例如,Abil
EM-90,其是十六烷基二甲硅油共聚醇))乳化。
在酯润肤剂之中包括:
a) 具有10-20个碳原子的脂肪酸的烯基或烷基酯。它们的实例包括新戊酸异二十烷基酯、新戊酸异癸酯、异壬酸异壬酯、蓖麻醇酸十六烷基酯、豆蔻酸油醇酯、硬脂酸油醇酯和油酸油醇酯。
b) 醚-酯,如乙氧基化脂肪醇的脂肪酸酯。
c) 多元醇酯。丁二醇、乙二醇单和二脂肪酸酯、二乙二醇单和二脂肪酸酯、聚乙二醇(200-6000)单和二脂肪酸酯、丙二醇单和二脂肪酸酯、聚丙二醇2000单油酸酯、聚丙二醇2000单硬脂酸酯、乙氧基化的丙二醇单硬脂酸酯、甘油基单和二脂肪酸酯、多甘油多脂肪酯、乙氧基化的甘油基单硬脂酸酯、1,3-丁二醇单硬脂酸酯、1,3-丁二醇二硬脂酸酯、聚氧乙烯多元醇脂肪酸酯(polyoxyethylene polyol fatty acid
ester)、山梨糖醇酐脂肪酸酯和聚氧乙烯山梨糖醇酐脂肪酸酯是令人满意的多元醇酯。特别有用的是C1-C30醇的季戊四醇、三羟甲基丙烷和新戊二醇酯。示例性的为季戊四醇四乙基己酸酯。
d) 蜡酯,如蜂蜡、鲸油蜡和三山嵛精蜡。
e) 甾醇酯,其实例为胆固醇脂肪酸酯。
f) 脂肪酸的糖酯,如蔗糖多山嵛酸酯和蔗糖棉子酸酯。
特别有用的还有苯甲酸C 12-15 烷基酯,以Finsolve商标销售。
为适合的化妆品可接受的载体的烃包括矿脂、矿物油、C 11 -C 13 异链烷烃、聚α烯烃和尤其是异十六烷,可作为Permethyl
101A商购自Presperse Inc。
多元醇类型的保湿剂可以作为化妆品可接受的载体使用。典型的多元醇包括聚亚烷基二醇和更优选亚烷基多醇和它们的衍生物,包括丙二醇、二丙二醇、聚丙二醇、聚乙二醇和其衍生物、山梨糖醇、羟丙基山梨糖醇、己二醇、1,3-丁二醇、异戊二醇、1,2,6- 已三醇、丙三醇、乙氧基化丙三醇、丙氧基化丙三醇和其混合物。保湿剂的量可以在组合物重量的0.5-50%,优选1-15%的任何范围。最优选的是丙三醇(也称为甘油)。甘油的量可以为组合物重量的约1%-约50%,优选10-35%,最佳地15-30%。
除了化妆品可接受的载体,本发明的组合物还可以包含各种各样的其它功能成分。在本发明的组合物中可以包含遮光剂活性成分。这些将为具有至少一个在290-400nm范围的紫外光吸收的发色团的有机化合物。发色团有机遮光剂可以分成以下的种类(带有具体实例):对-氨基苯甲酸,其盐和其衍生物(乙基、异丁基、甘油基酯;对-二甲基氨基苯甲酸);氨基苯甲酸酯(邻氨基苯甲酸酯;甲基、薄荷基、苯基、苯甲基、苯乙基、里哪基、松油基和环己烯基酯);水杨酸酯(辛基、戊基、苯基、苄基、薄荷基、甘油基和二丙二醇酯);肉桂酸衍生物(薄荷基和苄基酯、α-苯基肉桂腈;丁基肉桂酰丙酮酸酯);二羟基肉桂酸衍生物(伞形酮、甲基伞形酮、甲基乙酰-伞形酮);三羟基肉桂酸衍生物(七叶亭、甲基七叶亭、瑞香素,和糖甙、七叶灵和瑞香苷);烃(二苯基丁二烯,芪);二亚苄基丙酮和亚苄基苯乙酮;萘酚磺酸盐(2-萘酚-3,6-二磺酸和2-萘酚-6,8-二磺酸的钠盐);二羟基-萘甲酸和其盐;邻-和对-羟基二苯基二磺酸盐(酯);香豆素衍生物(7-羟基、7-甲基、3-苯基);二唑(2-乙酰-3-溴吲唑,苯基苯并噁唑、甲基萘并噁唑、各种芳基苯并噻唑);奎宁盐(二硫酸盐、硫酸盐、氯化物、油酸盐和丹宁酸盐);喹啉衍生物(8-羟基喹啉盐、2-苯基喹啉);羟基-或甲氧基-取代的苯甲酮;尿酸和vilouric acids;丹宁酸和其衍生物(例如,六乙基醚);胡椒基丁醚((Butyl carbityl) (6-propyl piperonyl) ether);氢醌;苯甲酮(氧苯酮、磺异苯酮、二氧基苯酮、苯酰间苯二酚、2,2',4,4'-四羟基二苯甲酮、2,2’-二羟基-4,4’-二甲氧基二苯甲酮、奥他苯酮、4-异丙基二苯甲酰甲烷;丁基甲氧基二苯甲酰甲烷、依讬立林和4-异丙基-二苯甲酰甲烷)。特别有用的是:对-甲氧基肉桂酸2-乙基己酯、4,4’-叔丁基甲氧基二苯甲酰甲烷、2-羟基-4-甲氧基二苯甲酮、辛基二甲基对-氨基苯甲酸、二棓酰基三油酸酯、2,2-二羟基-4-甲氧基二苯甲酮、4-[双(羟丙基)]氨基苯甲酸乙酯、2-乙基己基-2-氰基-3,3-二苯基丙烯酸酯、2-乙基己基水杨酸酯、对-氨基苯甲酸甘油酯、3,3,5-三甲基环己基水杨酸酯、甲基氨基苯甲酸酯、对-二甲基氨基苯甲酸或氨基苯甲酸酯、对-二甲基氨基苯甲酸2-乙基己酯、2-苯基苯并咪唑-5-磺酸、2-(对-二甲基氨基苯基)-5-锍基苯并噁唑酸(2-(p-dimethylaminophenyl)-5-sulfoniobenzoxazoic
acid)和它们的混合物。
特别优选的为例如对-甲氧基肉桂酸乙基己酯的材料,可作为Parsol MCX®获得,阿伏苯宗,可作为Parsol 1789®,
Dermablock OS® (辛基水杨酸酯)和Mexoryl SX®(INCI名称为对苯二亚甲基二樟脑磺酸)获得。
有机遮光剂的量可以为组合物的约0.1-约15wt%,优选约0.5wt%-约10wt%,最佳地为约1wt%-约8wt%。
在组合物中可以包含各种各样的增稠剂。示例性但非限制性的实例为硬脂酸、丙烯酰胺/ 丙烯酰二甲基牛磺酸钠共聚物(Aristoflex
AVC)、丙烯酸羟乙酯/丙烯酰二甲基牛磺酸钠共聚物、淀粉辛烯基琥珀酸铝、聚丙烯酸盐 (例如Carbomers,包括Carbopol® 980、Carbopol® 1342、Pemulen
TR-2®和Ultrez®增稠剂)、多糖 (包括黄原胶、瓜尔胶、果胶、卡拉胶和菌类植物胶)、纤维素 (包括羧甲基纤维素、乙基纤维素、羟乙基纤维素和甲基羟甲基纤维素)、矿物质 (包括滑石、硅石、氧化铝、云母和粘土,后者的代表为膨润土、锂皂石和凹凸棒石)、硅酸镁铝和它们的混合物。增稠剂的量可以为组合物的约0.05-约10wt%的范围,优选约0.3-约2wt%。
可以将防腐剂合意地引入到本发明的化妆品组合物中以防止潜在的有害微生物的生长。适于本发明组合物的传统防腐剂为对-羟基苯甲酸的烷基酯。其它最近使用的防腐剂包括乙内酰脲衍生物、丙酸盐和各种季铵化合物。化妆品化学家熟悉合适的防腐剂并且常规地选自它们以满足防腐挑战测试并且提供产品稳定性。特别优选的防腐剂为苯氧基乙醇、对羟基苯甲酸甲酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯、对羟基苯甲酸异丁酯、咪唑烷基脲、去氢醋酸钠和苄醇。选择防腐剂时应当重视组合物的用途和防腐剂与乳液中的其它成分之间可能的不兼容性。防腐剂优选以组合物的0.01-2wt%的量使用。
本发明的组合物还可以包含维生素和类黄酮。示例性的水溶性维生素为烟酰胺、维生素B2、维生素B6、维生素C和生物素。可用的水不溶性维生素之中有维生素A(视黄醇)、维生素A棕榈酸酯、抗坏血酸四异棕榈酸酯、维生素E(生育酚)、维生素E乙酸酯和DL-泛醇。特别合适的维生素B6衍生物为维生素B6棕榈酸酯。优选的类黄酮之中有葡萄糖基橘皮苷和芸香苷。当在根据本发明的组合物中存在时,维生素或类黄酮的总量可以为组合物的0.001-10wt%,优选0.01-1wt%,最佳为0.1-0.5wt%。
剥离剂是另一任选的组分。示例性的为α-羟基羧酸和β-羟基羧酸和这些酸的盐。前者之中有乙醇酸、乳酸和苹果酸的盐。水杨酸为β-羟基羧酸的代表。当存在时这些材料的量可以为组合物的约0.1-约15wt%。
任选地可以在本发明的组合物中包含各种草本提取物。示例性的为石榴、白桦树(Betula Alba)、绿茶、洋甘菊、甘草、齿叶乳香树、橄榄(油橄榄)叶、蒙大拿山金车花、薰衣草和它们的提取物组合。提取物可以是水溶性或溶剂中携带的水不溶性的,其分别为亲水性或疏水性的。水和乙醇是优选的提取物溶剂。
可适于本发明的组合物的各种其它辅助化妆品成分包括神经酰胺(例如,Ceramide 3和Ceramide 6)、共轭亚油酸、着色剂(例如氧化铁)、金属(锰、铜和/或锌)葡糖酸盐、尿囊素、棕榈酸五胜肽-3、 氨基酸 (例如丙胺酸、精氨酸、甘氨酸、赖氨酸、脯氨酸、丝氨酸、苏氨酸、谷氨酸和它们的混合物)、三甲基甘氨酸、PCA钠、 螯合剂(如EDTA二钠)、不透明剂(如二氧化钛)、天冬氨酸镁和它们的组合。量可以组合物的 0.000001- 3wt%变化。
可以存在少量的乳化表面活性剂。表面活性剂可以是阴离子、非离子、阳离子、两性和它们的混合物。含量可以为0.1-5wt%,优选0.1-2wt%,最佳为0.1-1wt%。有利地,表面活性剂的存在量应当不足以使泡沫形成。在这些情况下,存在小于2wt%,优选小于1wt%,和最佳地小于0.5wt%的表面活性剂。可以使用乳化剂(如PEG-100硬脂酸酯)以及乳液稳定剂(如鲸蜡硬脂醇)并且可以使用ceteareth-20(鲸蜡硬脂醇聚醚),通常以不超过组合物的5wt%的量使用。
适用于本发明组合物的其它任选的添加剂包括阳离子铵化合物以增强保湿(moisturization)。这类化合物包括羟丙基三(C1-C3 烷基)铵单取代的糖的盐、羟丙基三(C1-C3 烷基)铵单取代的多醇的盐、二羟丙基三(C1-C3 烷基)铵盐、二羟丙基二(C1-C3
烷基)单(羟乙基)铵盐、瓜尔羟丙基三甲基铵盐、2,3-二羟丙基三(C1-C3 烷基或羟烷基)铵盐或其混合物。在最优选的实施方案中并且当需要时,在本发明中采用的阳离子铵化合物为季铵化合物1,2-二羟丙基三甲基氯化铵。如果使用,这些化合物通常占组合物的约0.01-约30wt%,和优选约0.1-约15wt%。
当使用阳离子铵化合物时,与其一起使用的任选的添加剂为保湿剂,例如取代的脲,如羟甲基脲、羟乙基脲、羟丙基脲;双(羟甲基)脲;双(羟乙基)脲;双(羟丙基)脲;N,N’-二羟甲基脲;N,N’-二羟乙基脲;N,N’-二羟丙基脲、N,N,N’-三羟乙基脲;四(羟甲基)脲;四(羟乙基)脲;四(羟丙基)脲;N-甲基-N’-羟乙基脲;N-乙基-N’-羟乙基脲;N-羟丙基-N’-羟乙基脲和N,N’二甲基-N-羟乙基脲或其混合物。当术语羟丙基出现时,含义为3-羟基-正-丙基、2-羟基-正-丙基、3-羟基-异丙基或2-羟基-异丙基的统称。最优选的是羟乙基脲。后者可作为50%的水性液体由National Starch & Chemical Division of ICI以商品名Hydrovance获得。这类取代的脲,虽然在保湿配制物中是合意的,但仅当与本发明组合物中使用的所需的免晒美黑剂兼容时才选择使用。
当使用时,基于组合物的总重量,在本发明组合物中取代脲的量为约0.01-约20%,并且优选约0.5-约15%,并且最优选约2-约10%,并且包括所有包含在其中的范围。
当使用阳离子铵化合物和取代的脲时,在其最特别优选的实施方案中,基于组合物的总重量,使用至少约0.01-约25%,并且优选约0.2-约20%,并且最优选约1-约15%的湿润剂(如甘油),并且包括所有包含在其中的范围。
当制备本发明的组合物时,通常将成分在大气条件下以适中的剪切混合。可以局部施用该组合物并且通常每平方厘米施加1-4毫克组合物。通常,组合物显示4-6的pH。本发明的组合物的包装可以是罐或管以及任何其它在化妆品、乳膏、洗涤和露类型的产品常见的形式。
提供以下实施例来帮助理解本发明。实施例不旨在限制权利要求的范围。
实施例1
用以下方法制备本发明的复合颗粒
将氧化锌、MZY-303S(可由TAYCA
Corporation商购)、尺寸为约35nm的硅处理的颗粒用作具有约2.0折射率的亚颗粒。基于复合颗粒的总重量,使用的氧化锌的量在0、5、10、15、20、25、30和35wt%变化。将甲基丙烯酸甲酯用作单体来生产聚合物基体。作为交联剂以基于所用单体的重量10wt%的量添加二甲基丙烯酸乙二醇酯。使用过氧化苯甲酰(1wt%)作为引发剂。使用乙酸乙酯作为致孔剂(乙酸乙酯:单体的重量比为约1:2)。在室温下,通过超声将氧化锌颗粒分散到甲基丙烯酸甲酯、二甲基丙烯酸乙二醇酯、过氧化苯甲酰和乙酸乙酯的混合物中。将得到的混合物倒入2wt%的聚(乙烯醇)水溶液中并在6000rpm的剪切应力下均质化5分钟来乳化。在装备有搅拌器、回流冷凝器和氮气入口系统的玻璃反应器中进行聚合。在整个过程中将搅拌速度固定在300rpm。反应温度为75℃,并且反应时间为5小时。在完成之后,将得到的产物离心以通过用乙醇和蒸馏水洗涤数次并在真空下干燥移除残留反应物,以作为与本发明一致的粉末获得氧化锌-聚甲基丙烯酸甲酯-中空(即,含空穴)复合颗粒并且具有约10vol%的空穴。获得的颗粒适于配制成最终用途用户产品例如露和乳膏。
实施例2
重复类似于在实施例1中描述的步骤,只是使用BASF提供的Z-cote HP1氧化锌颗粒(用三乙氧基辛酰基硅烷进行过表面处理)替代MZY-3035来制备与本发明一致的氧化锌-聚甲基丙烯酸甲酯-中空复合颗粒。
实施例3
重复类似于在实施例1中描述的步骤,只是使用KOBO提供的ZnO-C-DMC2氧化锌颗粒替代MZY-3035来制备与本发明一致的氧化锌-聚甲基丙烯酸甲酯-中空复合颗粒。
实施例4
重复类似于在实施例1中描述的步骤,只是使用Rohm
and Haas提供的SunSphereTM中空球替代致孔剂制造的空穴来制备与本发明一致的氧化锌-聚甲基丙烯酸甲酯-中空复合颗粒。使用的中空球的量在0、1、3、5、7、10、15和20wt%变化,低到高的量分别与实施例1中制备的复合颗粒中使用的低到高的氧化锌量相匹配。
实施例5
重复类似于在实施例1中描述的步骤,只是使用二氧化钛MT-700Z(TAYCA Corporation提供)颗粒替代氧化锌来制备与本发明一致的二氧化钛-聚甲基丙烯酸甲酯-中空复合颗粒。
实施例6
重复类似于在实施例1中描述的步骤,只是使用二氧化钛TR-10(MIYOSHI KASEI提供)颗粒替代氧化锌来制备与本发明一致的二氧化钛-聚甲基丙烯酸甲酯-中空复合颗粒。
实施例7
重复类似于在实施例1中描述的步骤,只是使用氧化铁Unipure
Red LC 381 AS-EM(SENSIENT提供)颗粒替代氧化锌来制备与本发明一致的氧化铁-聚甲基丙烯酸甲酯-中空复合颗粒。
实施例8
重复类似于在实施例1中描述的步骤,只是使用50:50重量比的氧化锌和二氧化钛替代仅使用氧化锌来制备与本发明一致的氧化锌-二氧化钛-聚甲基丙烯酸甲酯-中空复合颗粒。所使用的氧化锌和二氧化钛粉末的混合物的量与在实施例1中描述的量一致。
实施例9
重复类似于在实施例1中描述的步骤,只是使用50:50重量比的氧化锌和氧化铁来制备与本发明一致的氧化锌-氧化铁-聚甲基丙烯酸甲酯-中空复合颗粒。所使用的氧化锌和氧化铁粉末的混合物与在实施例1中描述的量一致。
实施例10
配制了包含本发明的复合颗粒和可商购颗粒(参见表1)的组合物(水包油乳液)。组成提供在表2中。
将实施例1中复合颗粒(10wt%的氧化锌)与另外的成分完全分散在油相中并且彻底混合。将得到的油基混合物逐渐加入到水相中。将得到的混合物在9000rpm的剪切应力下乳化10分钟并逐渐搅拌和冷却至室温。
表1
No. | 商标名称 | 组成 | 供应商 |
1 | BPD 500W | HDI/三羟甲基己基内酯交联共聚物和二氧化硅 | KOBO |
2 | EA209 | 乙烯/丙烯酸酯共聚物 | KOBO |
3 | Ganzpearl 0820 | 微孔聚(甲基丙烯酸甲酯) | Ganz |
表2
材料 | 配制物 (wt %) | 对比配制物1 (wt %) | 对比配制物2 (wt %) | 对比配制物3 (wt %) |
异十六烷 | 0.5 | 0.5 | 0.5 | 0.5 |
鲸蜡硬脂醇&鲸蜡硬脂醇聚醚-20 | 3.0 | 3.0 | 3.0 | 3.0 |
硬脂酸 | 0.2 | 0.2 | 0.2 | 0.2 |
二甲基硅油 | 5.0 | 5.0 | 5.0 | 5.0 |
PEG-100 硬脂酸酯 | 2.0 | 2.0 | 2.0 | 2.0 |
乙基己基甲氧基肉桂酸酯 | 7.0 | 7.0 | 7.0 | 7.0 |
Aristoflex AVC | 1.0 | 1.0 | 1.0 | 1.0 |
TiO2 | 2.0 | 2.0 | 2.0 | 2.0 |
ZnO-PMMA-中空 | 5.0 | -- | -- | -- |
EA209 | -- | -- | 5.0 | -- |
Ganzpearl 0820 | -- | 5.0 | -- | -- |
PPD500W | -- | -- | -- | 5.0 |
丁二醇 | 5.0 | 5.0 | 5.0 | 5.0 |
EDTA二钠 | 0.1 | 0.1 | 0.1 | 0.1 |
Glydant +液体 | 0.2 | 0.2 | 0.2 | 0.2 |
烟酰胺 | 2.0 | 2.0 | 2.0 | 2.0 |
水 | 余量 | 余量 | 余量 | 余量 |
用方形涂膜器(Sheen 1103)将75微米厚的组合物膜施加到载玻片上。使用测角仪通过类似于在US专利申请 2008/0152682中描述方法的方法检测该膜的双向反射和透射分布函数。使用下式计算柔焦(SF):
T(θ)是在角θ的透过率;ST是镜面透射角。入射角设置为48°。
在恒定温度和湿度的房间中在相同温度(22℃)和相同湿度(45%)下测量所有柔焦值。
在表3中给出的柔焦结果出人意料地显示,与包含常规颗粒的组合物相比,包含本发明的复合颗粒的组合物表现更好的柔焦结果。
表3
颗粒 | 柔焦 |
EA209 | 0.22 |
BPD 500W | 0.33 |
Ganzpearl 0820 | 0.38 |
复合颗粒 | 0.56 |
实施例11
将类似于实施例1中制备的复合颗粒的复合颗粒加入到商品乳膏中。在表4中列出了所述商品。
在60℃下,将复合颗粒(5wt%)完全分散在商品乳膏中。将得到的产物在9000rpm的剪切应力下乳化10分钟,并且逐渐搅拌冷却至室温。
表4
No. | 商品 |
1 | NIVEA® 晶纯皙白纯净日霜 |
2 | Olay® 多效修护防晒霜 SPF 15 |
通过在实施例10中描述的方法测定产品的柔焦。结果表明本发明的复合颗粒在10分钟后可以改善NIVEA日霜的柔焦约200%,和在2小时后可改善Olay多效约225%。
实施例12
向第一组类似于表4中所描述的可商购的局部组合物中作为单独的添加剂加入氧化锌(0.5wt%)、SunSphereTM中空球(0.25wt%)和聚甲基丙烯酸甲酯(4.25wt%)。
向第二组相同的组合物中加入相同的成分,只是氧化锌、中空球和聚甲基丙烯酸甲酯呈通过类似于实施例4中描述的方法制备的复合颗粒的形式。根据实施例10中给出的方法评价两组组合物的柔焦。
结果出人意料地显示,在两小时之后,与本发明一致的组合物的柔焦比具有作为单独的添加剂添加的颗粒的组合物好大约5倍。
Claims (16)
1.一种复合颗粒,包含:
(a) 聚合物基体;
(b) 折射率高于聚合物基体折射率的亚颗粒;和
(c) 占所述复合颗粒的0.1-20wt%的折射率低于聚合物基体折射率的亚颗粒、
占所述聚合物基体的0.1-30vol%的折射率低于聚合物基体折射率的空穴、
或二者,
其中所述聚合物基体具有1.3-1.8的折射率。
2.根据权利要求1的复合颗粒,其中50-100wt%的折射率高于聚合物基体折射率的亚颗粒分散在聚合物基体中。
3.根据权利要求1或2的复合颗粒,其中亚颗粒的直径比复合颗粒的直径小10-2100倍。
4.根据权利要求1或2的复合颗粒,其中所述聚合物基体的折射率比所述折射率低于聚合物基体折射率的亚颗粒或空穴的折射率高30-80%,且比所述折射率高于聚合物基体折射率的亚颗粒的折射率低10-50%。
5.根据权利要求1或2的复合颗粒,其中所述聚合物基体为聚(甲基丙烯酸甲酯)。
6.根据权利要求1或2的复合颗粒,其中所述折射率高于聚合物基体折射率的亚颗粒为氧化锌、二氧化钛、氧化锆、氧化铁或它们的混合物。
7.根据权利要求1或2的复合颗粒,其中所述折射率低于聚合物基体折射率的亚颗粒为包封的气体。
8.根据权利要求1或2的复合颗粒,其中所述折射率低于聚合物基体折射率的亚颗粒为包封的空气或真空。
9.根据权利要求1或2的复合颗粒,其中所述空穴是由致孔剂产生的。
10.根据权利要求1或2的复合颗粒,其中所述复合颗粒具有约0.5-75微米的直径。
11.根据权利要求1或2的复合颗粒,其中所述折射率高于聚合物基体折射率的亚颗粒具有1.65-3的折射率,占复合颗粒的0.1-35wt%并且具有20-800nm的直径,所述折射率低于聚合物基体折射率的亚颗粒和/或空穴具有1-1.4的折射率和50-800nm的直径。
12.根据权利要求11的复合颗粒,其中所述空穴占所述聚合物基体的0.1-30vol%,且所述折射率低于聚合物颗粒折射率的亚颗粒占复合颗粒的0.1-20wt%。
13.一种化妆品组合物,包含:
(i) 前述权利要求任一项的复合颗粒;和
(ii) 化妆品可接受的载体。
14.根据权利要求13的化妆品组合物,其中所述化妆品可接受的载体是乳液。
15.根据权利要求13或14的化妆品组合物,其中所述组合物包含0.1-20wt%的所述复合颗粒。
16.用于改善皮肤特性的方法,包括局部施加权利要求13-15任一项的组合物至皮肤的步骤。
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CN1905854A (zh) * | 2004-01-23 | 2007-01-31 | 荷兰联合利华有限公司 | 具有照射与聚焦柔和的含颜料化妆品组合物 |
CN101568321A (zh) * | 2006-12-22 | 2009-10-28 | 荷兰联合利华有限公司 | 在化妆品组合物中的单晶片状硫酸钡 |
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EP2643397A1 (en) | 2013-10-02 |
US20130287826A1 (en) | 2013-10-31 |
EP2643397B1 (en) | 2014-09-10 |
EA201300612A1 (ru) | 2013-12-30 |
BR112013012039A2 (pt) | 2016-08-16 |
WO2012069291A1 (en) | 2012-05-31 |
EA024756B1 (ru) | 2016-10-31 |
CN103210030A (zh) | 2013-07-17 |
US9993397B2 (en) | 2018-06-12 |
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