CN115279485A - 微胶囊和包含该微胶囊的化妆品组合物 - Google Patents
微胶囊和包含该微胶囊的化妆品组合物 Download PDFInfo
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- CN115279485A CN115279485A CN202080090302.6A CN202080090302A CN115279485A CN 115279485 A CN115279485 A CN 115279485A CN 202080090302 A CN202080090302 A CN 202080090302A CN 115279485 A CN115279485 A CN 115279485A
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- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
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- 229910052682 stishovite Inorganic materials 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 239000011667 zinc carbonate Substances 0.000 description 1
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- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
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- 239000011592 zinc chloride Substances 0.000 description 1
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- 229940007718 zinc hydroxide Drugs 0.000 description 1
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- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- OWVLYQRCCIEOPF-QHTZZOMLSA-L zinc;(2s)-5-oxopyrrolidine-2-carboxylate Chemical compound [Zn+2].[O-]C(=O)[C@@H]1CCC(=O)N1.[O-]C(=O)[C@@H]1CCC(=O)N1 OWVLYQRCCIEOPF-QHTZZOMLSA-L 0.000 description 1
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- QUEDXNHFTDJVIY-UHFFFAOYSA-N γ-tocopherol Chemical class OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-UHFFFAOYSA-N 0.000 description 1
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Abstract
公开了一种微胶囊,其包括:(i)包含有益试剂的核;和(ii)包含二氧化硅的壳;其中所述壳包括平均厚度为1‑1000nm的片状无机材料;其中所述有益试剂是芳香剂、芳香剂前体、毛发调理剂、去屑剂、保湿剂、润肤剂、染料和/或颜料、颜色护理添加剂(包括染料固色剂)或它们的混合物。
Description
技术领域
本发明涉及微胶囊以及包含微胶囊的化妆品组合物。
背景技术
许多个人护理和家庭护理产品寻求将有益试剂输送到头发、皮肤、纺织品和硬表面等基底上。为了获得持久的性能,已提出将有益试剂封装在微胶囊中作为一种手段,特别是对香味剂(perfume)来说。当应用时,微胶囊可以沉积在基底上,例如沉积在皮肤上,并通过压力和/或摩擦作用而破裂。香味剂被释放出来,并给消费者带来优质的感官体验。
然而,仍存在很大的改进空间,因为消费者对洗涤过程的多个阶段如在洗涤结束时的改善的芳香剂(fragrance)感知,以及更持久的芳香性能的偏好推动了对该领域的商业兴趣。
封装体的泄漏仍然是一个问题,其不仅会导致性能降低,而且还会限制可用于封装的保护性壁材的材料。三聚氰胺甲醛树脂胶囊是众所周知的,但不利地是,需要与甲醛清除剂结合使用。
开发具有安全性的环境友好型微胶囊、以开发具有产生所需性能的此类微胶囊颗粒的组合物越来越引起人们的兴趣。
US 2016/177156 A1公开了用于增加热交换材料或者还有热流体的热导率和热容量的导热胶囊。它没有公开可用于化妆品组合物中的有益试剂,并且与有益试剂的负载/释放无关。
发明内容
申请人开发了微胶囊,该微胶囊包含位于核中的有益试剂,并具有包含二氧化硅的壳,其中所述壳包括平均厚度为1-1000nm的片状无机材料。令人惊讶地发现,当将此类微胶囊包含在化妆品组合物中时,它们可以具有有益试剂的良好负载效率和持久释放,同时保持可接受的储存泄漏。
根据第一方面,公开了一种微胶囊,其包括:
(i)包含有益试剂的核;和
(ii)包含二氧化硅的壳;其中所述壳包括平均厚度为1-1000nm的片状无机材料;其中所述有益试剂是芳香剂、芳香剂前体(pro-fragrance)、毛发调理剂、去屑剂、保湿剂、润肤剂、染料和/或颜料、颜色护理添加剂(包括染料固色剂)或它们的混合物。
根据第二方面,公开了一种制备本发明第一方面的微胶囊的方法,包括以下步骤:
a)制备包含二氧化硅前体和有益试剂的油相液体;
b)通过将片状无机材料和去离子水的混合物均质化来制备水性悬浮液。
c)通过将片状无机材料的水性悬浮液加入油相液体中并均质化以形成乳液来制备o/w乳液。
d)将o/w乳液放入40℃烘箱中至少24小时,以得到微胶囊浆液产品。
根据第三方面,公开了包含第一方面的微胶囊的化妆品组合物。
发明详述
为了避免疑问,本发明的一个方面的任何特征可用于本发明的任何其它方面。词语“包含”旨在表示“包括”,但不一定是“由……组成(consisting of)”或“由……构成(composed of)”。换句话说,所列出的步骤或选项不必是详尽的。应注意,以下描述中给出的实施例旨在阐明本发明,并不旨在将本发明限制于这些实施例本身。类似地,除非另有说明,所有百分比均为重量/重量百分比。除了在操作例和对比例中,或在另外明确指出的地方,本说明书和权利要求中表示材料的量或反应的条件、材料的物理性质和/或用途的所有数字应理解为由词语“约”修饰。以格式“x-y”表示的数值范围应理解为包括x和y。当对于特定特征以格式“x-y”描述多个优选范围时,应理解还涵盖组合不同端点的所有范围。除非另有说明,如本文所用的不定冠词“一个”或“一种”及其相应的定冠词“该”表示至少一个,或一个或多个。在上述各节中提到的本发明的各种特征在适当的情况下适用于其它经过必要修正的节。因此,在一个节中指定的特征可以在适当的情况下与在其它节中指定的特征组合。添加任何节标题仅为了方便起见,并且不旨在以任何方式限制本公开。
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,尤其是人类的皮肤的组合物。这种组合物通常可分类为免洗型或洗去型,但优选为免洗型。该组合物被配制成一种产品,该产品专门用于人体以改善外观,但另外还可以提供清洁、气味控制或一般美感。本发明的组合物可以是液体、乳剂、霜剂、泡沫、磨砂膏、凝胶或爽肤水的形式,或用工具施加或经由面罩或垫施加。此类组合物的非限制性实例包括免洗型润肤乳、霜、止汗剂、除臭剂、口红、粉底、睫毛膏、免晒美黑剂和防晒乳。本发明的组合物优选为免洗型组合物。如本文所用,“皮肤”意在包括面部和身体(例如,颈部、胸部、背部、手臂、腋下、手、腿、臀部和头皮)上的皮肤,尤其是其暴露于阳光的部分。
如本文所用,“毛发护理组合物”意在包括用于局部施用于哺乳动物,尤其是人类的头发或头皮的组合物。局部是指将产品施用于身体的外表面。在本发明中,这是通过将毛发护理组合物施用于头发或头皮来实现的。此类产品通常可分为免洗型或洗去型,并且包括用于改善头皮和头发的外观、清洁、气味控制或一般美感的任何产品。本发明的毛发护理组合物优选为免洗型产品。或者,本发明的毛发护理组合物是洗去型组合物。根据本发明的毛发护理组合物优选为洗发剂、护发素、发膏、护发精华、摩丝、发胶或发油。
“长度”、“宽度”和“厚度”是指未聚集状态下的颗粒或微胶囊的长度、宽度和厚度。术语“长度”是指颗粒或微胶囊的通常沿纵轴的平均尺寸。术语“宽度”是指颗粒或微胶囊的垂直于长度并且通常垂直于纵轴的平均尺寸。术语“厚度”是指颗粒或微胶囊垂直于长度和宽度的平均尺寸。长度、宽度和厚度可以例如通过扫描电子显微镜(SEM)通过将至少十个颗粒的值平均来测量。
如本文所用“粒径”是指非聚集状态的颗粒直径,除非另有说明。对于直径不大于1微米的颗粒的多分散性样品,直径是指使用利用诸如Zetasizer NanoTM(MalvernInstruments Ltd,UK)之类的仪器进行的动态光散射(参见国际标准ISO 13321)测量的z平均粒径。对于直径大于1微米的颗粒的多分散性样品,直径是指可通过例如激光衍射、使用满足ISO 13320中规定要求的系统(诸如可从Malvern Instruments Ltd获得的MastersizerTM2000)测量的颗粒的表观体积中值粒径(D50,也称为x50,或有时称为d(0.5))。
根据第一方面,公开了一种微胶囊,其包括:
(i)包含有益试剂的核;和
(ii)包含二氧化硅的壳;其中所述壳包括平均厚度为1-1000nm的片状无机材料;其中所述有益试剂是芳香剂、芳香剂前体、毛发调理剂、去屑剂、保湿剂、润肤剂、染料和/或颜料、颜色护理添加剂(包括染料固色剂)或它们的混合物。
术语微胶囊是指尺寸优选为0.5至100微米、更优选2至50微米、进一步优选5至30微米、最优选5至20微米的核-壳微胶囊。
优选的是壳的厚度为0.01-10微米、优选0.05-1微米、更优选0.1-0.3微米。
优选地,本发明的微胶囊是粉末状的或水性悬浮液形式,更优选水性悬浮液形式。这种微胶囊的水性形式优选包含1-90重量%的微胶囊,余量为水。或者,微胶囊为粉末状,优选为冻干粉。
根据本发明的微胶囊的壳包含二氧化硅。优选地,所述二氧化硅很好地分散在壳中,并与片状无机材料组合。
优选的是,根据本发明的微胶囊的核包含增稠剂。所述增稠剂可以是在室温下为固体但通过加热液化的脂质,或是可以吸收油并提高粘度的矿物质。优选地,增稠剂可以是选自脂肪醇、脂肪酸和蜡的脂质。优选地,增稠剂可以是选自二氧化硅、膨润土和硅酸铝镁的矿物质。更优选地,增稠剂是疏水性二氧化硅。
片状无机材料
根据本发明的微胶囊的壳还包含片状无机材料。
本发明的无机材料为片状,并且具有1-1000nm、优选5-500nm、更优选10-100nm、进一步优选10-50nm的平均厚度。
优选的是无机材料的平均粒径为直径10-2000nm、更优选50-1000nm、最优选100-500nm。
优选的是无机材料选自MgAl层状双氢氧化物、羟基磷灰石、硅藻土、氢氧化镁、氢氧化钙、沸石MCM-22、氮化硼或它们的组合,更优选地,无机材料是MgAl层状双氢氧化物。
优选的是无机材料是阴离子表面改性的。优选的是阴离子表面改性的无机材料包含选自以下的组:硫酸盐、次硫酸盐、次亚硫酸盐、亚硫酸盐、硫酸氢盐(bisulphate)、亚硫酸氢盐、碳酸盐、碳酸氢盐、羟基、氯酸盐、高氯酸盐、亚氯酸盐、次氯酸盐、铬酸盐、亚铬酸盐、重铬酸盐、碘酸盐、硝酸盐、亚硝酸盐、磷酸盐、次磷酸盐、过磷酸盐、亚磷酸盐、磷酸一氢盐、磷酸二氢盐、锰酸盐、高锰酸盐、硫代硫酸盐、硫酸氢盐(hydrosulfate)、硅酸盐、偏硅酸盐、铝硅酸盐、乙酸盐、甲酸盐、草酸盐、草酸氢盐、硫化氢盐(hydrogen sulfide)、氰酸盐、硫氰酸盐、溴化物、氯化物、氟化物、碘化物、硼酸盐、溴酸盐、次溴酸盐。更优选的是阴离子表面改性的无机材料包含选自以下的组:硫酸盐、次硫酸盐、次亚硫酸盐、亚硫酸盐、硫酸氢盐、亚硫酸氢盐、碳酸盐、碳酸氢盐、羟基、氯酸盐、高氯酸盐、亚氯酸盐、次氯酸盐、铬酸盐、亚铬酸盐、重铬酸盐、磷酸盐、次磷酸盐、过磷酸盐、亚磷酸盐、磷酸一氢盐、磷酸二氢盐、硫代硫酸盐、硫酸氢盐、硅酸盐、偏硅酸盐、铝硅酸盐、乙酸盐、甲酸盐、草酸盐、草酸氢盐、硫化氢盐。进一步优选的是阴离子表面改性的无机材料包含硫酸根基团。
最优选的是无机材料包含阴离子表面改性的MgAl层状双氢氧化物。
优选的是无机材料具有多层,并且层间距离为0.1-10nm,更优选0.2-5nm,进一步优选0.5-2nm。无机材料优选具有5-1000m2/g、更优选10-500m2/g、进一步优选50-200m2/g的比表面积。
有益试剂
根据本发明的有益试剂可以指可以为头发和/或头皮,更优选为人头发提供一系列益处的试剂。有益试剂通常以按微胶囊的总重量计10-90%、更优选按微胶囊的总重量计30-80%的量存在。
本发明的有益试剂包括芳香剂、芳香剂前体、毛发调理剂、去屑剂、保湿剂、润肤剂、染料和/或颜料、颜色护理添加剂(包括染料固色剂)或它们的混合物。更优选地,有益试剂包括芳香剂、芳香剂前体、毛发调理剂、去屑剂或它们的混合物。此外优选地,有益试剂选自芳香剂、芳香剂前体或它们的混合物,并且最优选地,有益试剂是芳香剂。
芳香剂的有用组成包括天然和合成来源的材料。它们包括单一化合物和混合物。此类组分的具体实例可在以下的当前文献中找到:例如,Fenaroli的Handbook of FlavourIngredients,1975,CRC Press;Synthetic Food Adjuncts,1947,M.B.Jacobs,由VanNostrand编辑;或S.Arctander的Fragrance and Flavour Chemicals 1969,Montclair,N.J.(USA)。这些物质对于对消费产品加香、调味和/或芳香化(即赋予传统上加香或调味的消费品气味和/或风味或味道,或改变所述消费品的气味和/或味道)领域的技术人员来说是众所周知的。
本上下文中的芳香剂不仅是指全配制的产品芳香剂,而且指该芳香剂的选定组分,尤其是容易流失的那些,诸如所谓的“前调(top note)”。
前调由Poucher定义(Journal of the Society of Cosmetic Chemists 6(2):80[1955])。众所周知的前调的实例包括柑橘油、芳樟醇、乙酸芳樟酯、薰衣草、二氢月桂烯醇、氧化玫瑰和顺-3-己醇。前调通常占芳香剂组合物的15-25重量%,并且在本发明的那些包含增加前调含量的实施方案中,设想至少20重量%的前调可以存在于颗粒中。
本发明可以适用的另一组芳香剂是所谓的“芳香疗法”材料。这些包括许多也用于香味(fragrancery)的组分,包括以下精油的组分:诸如香紫苏(Clary Sage)、桉树(Eucalyptus)、天竺葵(Geranium)、薰衣草(Lavender)、Mace提取物、橙花(Neroli)、肉豆蔻(Nutmeg)、留兰香(Spearmint)、甜紫罗兰叶(Sweet Violet Leaf)和缬草(Valerian)。
在本发明的实施方案中有利地使用的典型芳香剂组分包括具有相对低沸点的那些,优选沸点低于300℃、优选100-250℃的那些,所述沸点是在一个大气压下测量的。
封装具有低LogP的芳香剂组分(即,将被分配到水中的那些),优选LogP小于3.0的芳香剂组分也是有利的。
举例来说,芳香剂前体可以是食品脂质。食品脂质通常包含具有明显疏水性的结构单元。大多数脂质来源于脂肪酸。在这些“酰基”脂质中,脂肪酸主要以酯的形式存在,并且包括单酰基甘油、二酰基甘油、三酰基甘油、磷脂、糖脂、二醇脂质、蜡、甾醇酯和生育酚。
芳香剂通常以按颗粒的总重量计10-85%、优选按颗粒的总重量计15-75%的量存在。芳香剂适宜地具有50至500道尔顿的分子量。芳香剂前体可以具有更高的分子量,通常为1-10kD。
皮克林乳液方法:
如本文所用,“皮克林乳液”是指通过吸附在两相之间的界面上的固体颗粒(例如胶态二氧化硅)而稳定的乳液。皮克林乳液液滴也是微囊化和形成封闭的非渗透性胶囊的合适模板。
本发明还涉及制备微胶囊的方法。
根据本发明的微胶囊优选通过使用皮克林乳液法制备。
制备微胶囊的方法:
本发明还涉及制备微胶囊的方法。该方法包括以下步骤:
a)制备包含二氧化硅前体和有益试剂的油相液体;
b)通过将片状无机材料和去离子水的混合物均质化来制备水性悬浮液。
c)通过将片状无机材料的水性悬浮液加入油相液体中并均质化以形成乳液来制备o/w乳液。
d)将o/w乳液放入40℃烘箱中至少24小时以得到微胶囊浆液产品。
优选的是二氧化硅前体选自烷氧基硅烷和水溶性硅酸盐。优选地,所述烷氧基硅烷选自原硅酸四乙酯、原硅酸四甲酯、甲基三乙氧基硅烷、甲基三甲氧基硅烷、乙烯基三甲氧基硅烷、3-氨基丙基三甲氧基硅烷、氨基丙基三乙氧基硅烷或它们的混合物。更优选地,烷氧基硅烷选自原硅酸四乙酯、氨基丙基三乙氧基硅烷或它们的混合物。
优选的是步骤a)的油相液体包含增加油相液体粘度的增稠剂。增稠剂可以是在室温下为固体但通过加热而液化的脂质,或是可以吸收油并提高粘度的矿物质。优选地,增稠剂可以是选自脂肪醇、脂肪酸和蜡的脂质。优选地,增稠剂可以是选自二氧化硅、膨润土和硅酸铝镁的矿物质。更优选地,增稠剂是疏水二氧化硅。
优选的是将氨引入步骤b)的水性悬浮液中。
化妆品组合物
根据另一方面,公开了一种化妆品组合物,其包含在化妆品可接受的载体中的第一方面的微胶囊。基于组合物的总重量,优选的是化妆品组合物包含按重量计0.001-10%、更优选0.005-7.55%、最优选0.01-5%的微胶囊。
多种材料可存在于包含本发明的微胶囊的组合物中,以用作化妆品可接受的载体。
优选地,载体包括水。取决于组合物的性质,按化妆品组合物的重量计,水的量可以例如为1-85重量%、更优选5-90%、甚至更优选35-80%、最佳地40-70%。优选地,载体包含表面活性剂。
本发明的化妆品组合物可进一步包含本领域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、光学物质(optics)、香味剂、粘度调节剂、生物添加剂、缓冲剂、调理剂、天然提取物、精油和有益试剂,包括抗炎剂、清凉剂、止汗剂、抗衰老剂、抗痤疮剂、去屑剂、毛发调理剂、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皮肤、头皮/头发的组合物,包括免洗型和洗去型产品。优选的是本发明的组合物是洗去型组合物。更优选的是本发明的化妆品组合物是毛发护理组合物。
毛发护理组合物
优选地,毛发护理产品是洗发剂、护发素、护发膏、护发精华、摩丝、发胶或发油。
根据本发明的毛发护理组合物还可包含去屑剂。本发明的毛发护理组合物优选包含0.05-5重量%的去屑剂。去屑剂是对头皮屑有活性的化合物,并且通常是抗微生物剂,优选地是抗真菌剂。抗真菌剂通常对马拉色菌(Malassezia spp)展示出约50mg/ml或更低的最小抑制浓度。
本发明的毛发护理组合物可进一步包含锌盐。额外的锌盐可以适当地选自有机酸的锌盐、无机酸的锌盐、氧化锌、氢氧化锌或它们的混合物。
优选的锌盐的实例包括氧化锌、吡咯烷酮羧酸锌、柠檬酸锌、碳酸锌、氯化锌、硫酸锌、甘氨酸锌、乙酸锌、乳酸锌及它们的混合物。当存在时,优选的是本发明的毛发护理组合物包含基于组合物的总重量的0.1-5重量%、优选0.2-3重量%、更优选0.25-2.5重量%的所述盐。
本发明的毛发护理组合物包含选自阴离子表面活性剂、非离子表面活性剂、两性离子表面活性剂及它们的混合物的表面活性剂。可以使用的性质、类型、数量和具体组合取决于组合物的配方,并且很大程度上取决于它是洗发剂还是护发素或调理洗发剂。
优选地,本发明的毛发护理组合物是洗发剂。优选地,其包含以下的表面活性剂:月桂基硫酸钠、月桂基醚硫酸钠、月桂基醚磺基琥珀酸钠、月桂基硫酸铵、月桂基醚硫酸铵、椰油基羟乙基磺酸钠和月桂基醚羧酸、椰油甜菜碱、椰油酰胺丙基甜菜碱、椰油两性乙酸钠或它们的混合物。
优选地,本发明的毛发护理组合物包含1-50%、优选2-40%、更优选4-25%的总表面活性剂。
进一步优选的是本发明的毛发护理组合物包含化妆品成分。优选地,化妆品成分选自硅酮、除去屑剂以外的抗菌剂、发泡促进剂、香味剂、包封物(例如包封的芳香剂)、染料、着色剂、颜料、防腐剂、增稠剂、蛋白质、磷酸酯、缓冲剂、pH调节剂、珠光剂(例如云母、二氧化钛、二氧化钛涂覆的云母、乙二醇二硬脂酸酯(INCI乙二醇二硬脂酸酯))和/或不透明剂、粘度调节剂、润肤剂、防晒剂、乳化剂、知觉活性物(例如薄荷醇和薄荷醇衍生物)、维生素、矿物油、精油、脂质、天然活性物、甘油、天然毛发营养素如植物提取物、水果提取物、糖衍生物和氨基酸、微晶纤维素,及它们的混合物。
优选地,本发明的毛发护理组合物包括按总组合物的重量计0.01-20重量%的至少一种化妆品成分,更优选为0.05-10重量%、还更优选0.075-7.5重量%、最优选0.1-5重量%的至少一种化妆品成分。
本发明的毛发护理组合物还可以包含协同抗微生物化合物,当与去头屑活性物(例如吡啶硫酮锌)组合使用以增强其性能并进一步抑制糠秕马拉色菌(Malasseziafurfur)的生长时,该协同抗微生物化合物产生协同抗微生物益处。这些化合物的非限制性实例包括具有醇基的化合物(例如和厚朴酚、厚朴酚或丹皮酚)、哌嗪和在天然植物提取物中发现的酚类化合物,即,百里酚和萜烯醇。
毛发护理产品可以另外包含维生素B3化合物。优选的维生素B3化合物是烟酰胺。
烟酰胺因从角质细胞分泌AMP(抗微生物蛋白)而为人所知。如此分泌的AMP提供用于提高例如头皮的免疫力。因此,借助于使用烟酰胺,不仅可以通过抗真菌活性,而且可以通过使用烟酰胺增强头皮自身对细菌的保护屏障来增强去头屑功效。这种组合可以提供更持久的保护,例如长达24小时的对细菌的防护。
当存在时,优选的是本发明的毛发护理组合物包含按组合物的重量计0.1-5%、更优选0.5-5%、进一步优选0.5-3%、最佳1.0-3.0%的烟酰胺。
硅酮
优选的是本发明的毛发护理组合物包含硅酮。
例如,本发明的组合物可以包含硅酮调理剂的乳化液滴,以用于增强调理性能。
合适的硅酮包括聚二有机硅氧烷、具有CTFA名称聚二甲基硅氧烷(dimethicone)的聚二甲基硅氧烷。此外,适用于本发明的组合物(特别是洗发剂和护发素)的是具有端羟基的聚二甲基硅氧烷,其具有CTFA名称聚二甲基硅氧烷醇(dimethiconol)。
优选地,乳化硅酮的粘度在25℃下为至少10,000cst,硅酮的粘度优选至少为60,000cst、最优选至少500,000cst、理想地为至少1,000,000cst。优选地,为了便于配制,粘度不超过109cst。
合适的预成型乳液的实例包括可从Dow Corning获得的Xiameter MEM 1785和微乳液DC2-1865。这些是聚二甲基硅氧烷醇的乳液/微乳液。交联的硅酮胶(silicone gum)也可以预乳化的形式获得,这对于方便配制是有利的。包含在洗发剂和护发素中的另一类优选的硅酮是氨基官能的硅酮。“氨基官能的硅酮”是指含有至少一个伯胺、仲胺或叔胺基团或季铵基团的硅酮。合适的氨基官能的硅酮的实例包括:具有CTFA名称“氨端聚二甲基硅氧烷(amodimethicone)”的聚硅氧烷。
适用于本发明的氨基官能硅酮的具体实例是氨基硅油DC2-8220、DC2-8166和DC2-8566(均购自Dow Corning)。
优选的是硅酮的总量为0.01-10重量%、更优选0.1-5重量%、最优选0.5-3重量%。
洗发剂
当本发明的毛发护理产品是洗发剂时,它通常是水性的,即它们具有水或水溶液或易溶的(lyotropic)液晶相作为它们的主要组分。
合适地,洗发剂组合物包含50-98%、优选60-92%的水。
优选地,洗发剂组合物包含一种或多种用于调理头发的阳离子聚合物。
合适的阳离子聚合物包括阳离子取代的或可由两种或更多种单体形成的均聚物。聚合物的重均(Mw)分子量通常在100000至300万道尔顿之间。聚合物可以具有阳离子含氮基团,诸如季铵或质子化氨基,或它们的混合物。如果聚合物的分子量太低,则调理效果很差。如果太高,则可能存在高拉伸粘度的问题,从而导致组合物在倾倒时变得粘性。
阳离子含氮基团通常作为取代基存在于阳离子聚合物的总单体单元的一部分上。因此,当聚合物不是均聚物时,它可以包含间隔非阳离子单体单元。此类聚合物在CTFA化妆品成分名录(Cosmetic Ingredient Directory)第3版中有所描述。阳离子单体单元与非阳离子单体单元的比例选择为得到具有所需范围内的阳离子电荷密度的聚合物,该范围通常为0.2-3.0meq/gm。聚合物的阳离子电荷密度可适当地通过如US Pharmacopoeia(美国药典)中描述的在用于氮测定的化学试验下的凯氏定氮法(Kjeldahl method)测定。
合适的阳离子聚合物包括具有阳离子胺或季铵官能团的乙烯基单体与水溶性间隔单体诸如(甲基)丙烯酰胺、烷基和二烷基(甲基)丙烯酰胺、(甲基)丙烯酸烷基酯、乙烯基己内酯和乙烯基吡咯烷的共聚物。烷基和二烷基取代的单体优选具有C1-C7烷基,更优选具有C1-3烷基。其他合适的间隔体包括乙烯基酯、乙烯醇、马来酸酐、丙二醇和乙二醇。
取决于组合物的特定种类和pH,阳离子胺可以是伯胺、仲胺或叔胺。通常,优选仲胺和叔胺,尤其是叔胺。
胺取代的乙烯基单体和胺可以以胺形式聚合,然后通过季铵化转化为铵。
阳离子聚合物可包含衍生自胺-和/或季铵-取代的单体和/或相容的间隔单体的单体单元的混合物。
合适的(非限制性实例)阳离子聚合物包括:
-含阳离子二烯丙基季铵的聚合物,包括例如二甲基二烯丙基氯化铵均聚物以及丙烯酰胺和二甲基二烯丙基氯化铵的共聚物,它们在工业中(CTFA)分别被称为聚季铵盐6和聚季铵盐7;
-具有3至5个碳原子的不饱和羧酸的均聚物和共聚物的氨基-烷基酯的无机酸盐(如美国专利号4,009,256中所述);
-阳离子聚丙烯酰胺(如WO95/22311中所述)。
可以使用的其他阳离子聚合物包括阳离子多糖聚合物,诸如阳离子纤维素衍生物、阳离子淀粉衍生物和阳离子瓜尔胶衍生物。
可以使用的特别合适类型的阳离子多糖聚合物是阳离子瓜尔胶衍生物,诸如瓜尔胶羟丙基三甲基氯化铵(可从Rhodia以其JAGUAR商标系列商购获得)。此类材料的实例是JAGUAR C13S、JAGUAR C14和JAGUAR C17。
可以使用任何上述阳离子聚合物的混合物。
优选的是,本发明的毛发护理组合物包含0.01-5%、优选0.02-1%、更优选0.05-0.8%的阳离子聚合物。
本发明的毛发护理组合物可另外包含阳离子沉积聚合物,其为具有100万至220万g/mol的平均分子量(Mw)和0.13至0.3的阳离子取代度的阳离子聚半乳甘露聚糖。
聚半乳甘露聚糖是主要由半乳糖和甘露糖单元组成的多糖,并且通常发现于豆科植物诸如瓜尔豆、刺槐豆、皂荚树、凤凰木和豆科的其他成员的种子的胚乳材料中。聚半乳甘露聚糖由1→4-链接的β-D-吡喃甘露糖基主链单元(也称为甘露糖苷单元或残基)的骨架与从聚合物骨架中的吡喃甘露糖残基的第6个碳原子分支的重复的1→6-链接的α-D-半乳糖基侧基(也称为半乳糖苷单元或残基)组成。不同豆科物种的聚半乳甘露聚糖在从聚甘露糖苷骨架分支的半乳糖苷侧单元的出现频率方面彼此不同。甘露糖苷和半乳糖苷单元在本文中统称为糖苷单元或残基。瓜尔胶(以下称为“瓜尔胶(guar)”)中所含的聚半乳甘露聚糖中甘露糖苷与半乳糖苷单元的平均比例约为2∶1。
合适的阳离子聚半乳甘露聚糖包括已通过与一种或多种衍生化试剂的化学反应而阳离子改性的瓜尔胶和羟烷基瓜尔胶(例如羟乙基瓜尔胶或羟丙基瓜尔胶)。
在典型的组合物中,按组合物的重量计,阳离子聚半乳甘露聚糖的量通常为约0.05-1%、优选0.1-0.8%、更优选0.2-0.6%。
本发明的毛发护理产品还可额外包含阴离子聚合物流变改性剂,诸如羧酸聚合物。
本发明上下文中的术语“羧酸聚合物”通常表示由含有侧挂羧酸基团的烯键式不饱和单体(下文称为“羧酸单体”)聚合获得的均聚物或共聚物。
合适的羧酸单体通常具有一个或两个羧酸基团、一个碳碳双键,并且含有总共3至约10个碳原子、更优选3至约5个碳原子。
合适的羧酸单体的具体实例包括α-β-不饱和一元羧酸如丙烯酸、甲基丙烯酸和巴豆酸;以及α-β-不饱和二元羧酸如衣康酸、富马酸、马来酸、乌头酸。也可以使用上述α-β-不饱和一元或二元羧酸的盐、酯或酸酐。实例包括α-β-不饱和二元羧酸与C1-4烷醇的半酯,诸如富马酸单甲酯;α-β-不饱和二元羧酸的环状酸酐,诸如马来酸酐、衣康酸酐和柠康酸酐;以及丙烯酸或甲基丙烯酸与C1-30烷醇的酯,诸如丙烯酸乙酯、丙烯酸丁酯、丙烯酸2-乙基己酯、丙烯酸十二烷基酯、丙烯酸十六烷基酯和丙烯酸十八烷基酯。
任选地,其他烯键式不饱和单体可以共聚到羧酸聚合物骨架中。此类其他烯键式不饱和单体的实例包括苯乙烯、乙酸乙烯酯、乙烯、丁二烯、丙烯腈及它们的混合物。羧酸聚合物可优选具有至少100万道尔顿的分子量。
合适的实例包括由丙烯酸或甲基丙烯酸C1-4烷基酯(例如丙烯酸乙酯)与一种或多种选自丙烯酸、甲基丙烯酸及它们的混合物的共聚单体聚合而成的交联共聚物。此类材料通常可以在INCI名称下称为丙烯酸酯共聚物。可商购的实例包括来自Rohm and Haas的33。
同样合适的是由丙烯酸或甲基丙烯酸的C10-30烷基酯与一种或多种选自丙烯酸、甲基丙烯酸和它们相应的C1-4烷基酯的共聚单体聚合而成的交联共聚物。此类材料通常可以在INCI名称下称为丙烯酸酯/C10-30烷基丙烯酸酯交联聚合物。可商购的实例包括来自Lubrizol Advanced Materials的聚合物1342和1382。
同样合适的是丙烯酸或甲基丙烯酸与丙烯酸烷基酯和乙氧基化疏水改性丙烯酸烷基酯的任选交联的共聚物。此类材料通常可以在INCI名称下称为丙烯酸酯/硬脂醇聚醚-20甲基丙烯酸酯共聚物、丙烯酸酯/山萮醇聚醚-25甲基丙烯酸酯共聚物、丙烯酸酯/硬脂醇聚醚-20甲基丙烯酸酯交联聚合物和丙烯酸酯/棕榈油醇聚醚-25丙烯酸酯共聚物。可商购的实例包括来自Rohm&Haas的22、28或88,和来自3V Sigma的
优选的是羧酸是卡波姆,诸如用季戊四醇的烯丙基醚或蔗糖的烯丙基醚交联的丙烯酸的均聚物。
也可以使用任何上述材料的混合物。
优选地,本发明的毛发护理组合物包含按组合物的重量计0.1-3.0%、更优选0.4-1.5%的羧酸聚合物。
在含有阴离子聚合物流变改性剂如上述羧酸聚合物的配制物中,通常需要通过添加无机或有机碱来中和至少一部分游离羧基。合适的无机或有机碱的实例包括碱金属氢氧化物(例如氢氧化钠或氢氧化钾)、碳酸钠、氢氧化铵、甲胺、二乙胺、三甲胺、单乙醇胺、三乙醇胺及它们的混合物。
本发明的毛发护理组合物还可包含选自一种或多种非离子纤维素醚的非离子聚合物流变改性剂。
在本发明中用作非离子聚合物流变改性剂的合适的非离子纤维素醚包括(C1-3烷基)纤维素醚,诸如甲基纤维素和乙基纤维素;羟基(C1-3烷基)纤维素醚,诸如羟乙基纤维素和羟丙基纤维素;混合的羟基(C1-3烷基)纤维素醚,诸如羟乙基羟丙基纤维素;以及(C1-3烷基)羟基(C1-3烷基)纤维素醚,诸如羟乙基甲基纤维素和羟丙基甲基纤维素。
在本发明中用作非离子聚合物流变改性剂的优选的非离子纤维素醚是水溶性非离子纤维素醚,诸如甲基纤维素和羟丙基甲基纤维素。本上下文中的术语“水溶性”表示在25℃和1个大气压下,在100克蒸馏水中至少1克、更优选至少3克、最优选至少5克的水中溶解度。该水平表示产生宏观各向同性或透明、有色或无色的溶液。
任何非离子纤维素醚的混合物也可以是合适的。在根据本发明的典型组合物中,非离子纤维素醚的水平基于组合物的总重量通常为约0.01-约2.0重量%,并且优选0.1-0.5重量%、更优选0.1-0.3重量%。
优选地,本发明的毛发护理产品包含0.1-0.3重量%的非离子纤维素醚。
本发明的毛发护理组合物可包含其他任选成分以增强性能和/或消费者可接受性。这种成分的实例包括芳香剂、染料和颜料以及防腐剂。这些成分中的每一种都可以以有效实现其目的的量存在。通常,基于组合物的总重量,以至多5重量%的水平单独包含这些任选的成分。
使用模式
本发明的化妆品组合物主要旨在用于局部施用于皮肤、头皮和头发。
本发明还提供一种处理基底的方法,该方法包括用包含本发明的微胶囊的组合物处理基底的步骤。优选地,基底是皮肤、头发和/或头皮。更优选地,基底是头发和/或头皮。
化妆品组合物优选为毛发护理组合物,并且当毛发护理组合物为洗发剂时,将其局部施用于头发,然后按摩到头发和头皮中。再然后在干燥头发之前用水冲洗。在冲洗掉之前,将作为免洗型毛发护理组合物的发油或护发精华在施用后保持1至10小时。
本发明将通过以下非限制性实施例进一步进行说明,其中除非另有说明,所有引用的百分比均以基于总重量的重量计。
本发明不限于附图中所举例说明的实施方案。因此应当理解,在权利要求中提及的特征后面有附图标记的情况下,这些附图标记仅出于增强权利要求的可理解性的目的而被包括在内,其绝不是对权利要求保护范围的限制。
实施例旨在说明本发明,不旨在将本发明限制于这些实施例本身。
具体实施方式
实施例
材料:
实施例中使用的其他化学品购自Sinopharm Chemical Reagent Co.,Ltd(国药集团化学试剂有限公司)。
实施例1:本发明内微胶囊的制备
(1)片状MgAl-LDH材料的制备:
将Mg(NO3)2.6H2O(0.0115mol,5.128g)、Al(NO3)3.9H2O(0.005mol,3.751g)和六亚甲基四胺(0.026mol,3.645g)与80ml去离子水混合,然后磁力搅拌混合物直至所有化学品完全溶解。将溶液转移到高压釜中并在140℃下加热24小时。然后,将高压釜中的混合物分离到10ml塑料离心管中,并通过离心得到粗产物。然后将粗产物用乙醇溶液(乙醇∶去离子水=1∶1v/v)在4k rpm的搅拌速度下洗涤3分钟,并且在离心后丢弃上清液。洗涤/离心过程重复3次,最后将产物在50℃烘箱中干燥。
(2)片状SDS(十二烷基磺酸钠)改性的MgAl-LDH材料的制备:
制备方法与MgAl-LDH材料(见上文)类似,除了在混合步骤中还加入十二烷基磺酸钠(0.0052mol,1.498g)。
(3)使用MgAl-LDH材料作为稳定剂制备微胶囊:
a)油相液体(A)的制备:将0.5ml原硅酸四乙酯和0.05ml氨基丙基三乙氧基硅烷与2ml柠檬烯混合,并摇动混合物直至完全均匀。在某些情况下,将0.034g疏水性SiO2添加到混合物中,以增加油相液体的粘度。
b)乳化剂溶液(B)的制备:将0.4g MgAl-LDH颗粒(或SDS改性的MgAl-LDH颗粒)添加到20ml去离子水中,并以3k rpm将混合物均化30秒。在某些情况下,将0.25ml氨加入到混合物中,以加快壳制造的反应速度。
c)然后,将溶液B加入到液体A中,并以8k rpm将混合物均化3分钟以形成乳液。
d)然后将乳液放入40℃烘箱中至少24小时,以得到微胶囊浆液产品。
(4)所制备的微胶囊的表征:
使用透射电子显微镜(TEM,JEOL JEM-2011)在200kV下表征MgAl-LDH材料的形态。采用CuKα辐射(l=0.15418nm),在BRUKER D2-PHASER X射线衍射仪上以4/min的扫描速率在10°–70°的2θ范围内进行X射线粉末衍射(XRD)分析。使用扫描电子显微镜(SEM,PHENOMPROX)表征或使用显微镜(上海精密仪器有限公司的带20×物镜的XSP-3C)观察微胶囊样品的形态。在马尔文2000型粒度仪(Mastersizer 2000Particle Size)上评估微胶囊的大小。
为了进一步测试壳的强度,通过使用乙醇洗涤微胶囊水性悬浮液来去除微胶囊中的香味剂。微胶囊的强度可以通过观察乙醇处理后微胶囊结构是否塌陷来进行评估。如果微胶囊的壳在乙醇处理后仍保持完整,则壳的强度非常好。
在显微镜下观察通过上述方法制备的本发明的微胶囊,并且总见下表1
表1
从表1可以看出,本发明的微胶囊(参考编号1-4)可以采用皮克林乳液法形成。这也表明由于阴离子表面改性,可以降低片状无机材料的厚度,并且其有助于稳定乳液,从而使形成的微胶囊更加完整。还发现当核包含用于油相液体的增稠剂(例如二氧化硅)时,可以形成质量更好的微胶囊。
还发现微胶囊的壳(参考编号4)即使在乙醇处理后仍能保持完整,因此微胶囊(参考编号4)的壳的强度高于其他。壳厚度为约100-300nm。
实施例2:本发明微胶囊的香味剂负载效率和负载率(以参考编号4为例)
典型的程序描述如下:在使用玻璃棒轻轻搅拌下,将0.5ml微胶囊(参考编号4)浆液与2ml去离子水混合。然后使用注射器驱动的过滤器(0.45μm,聚醚砜膜,ANPELscientific Instrument Co.,Ltd.)过滤经稀释的浆液以去除微胶囊。在20ml小瓶中将滤液与4ml乙醇混合。使用GC-FID评估滤液(未负载的香味剂)中的香味剂的量,将数据记录为Wu。在分开的情况下,将0.5ml微胶囊浆液与2ml去离子水混合。然后将1.0ml稀释的浆液和4.0ml乙醇加入到20ml小瓶中。将小瓶密封并在IKA MS2 Minishaker上以1000rpm振动1分钟。使用GC-FID评估浆液中香味剂的量(总香味剂)并将数据记录为WT。然后根据以下等式可计算香味剂负载效率。
香味剂负载效率%=(WT-WU)/WT*100(等式1)
其中:
WT=总香味剂的重量
WU=未负载香味剂的重量
此外,也可以根据以下等式计算香味剂负载率
香味剂负载率%=(WT-WU)/(Ws+WT-WU)*100(等式2)
其中:
Ws=胶囊壳的重量,其是根据用于壳形成的原料的进料量计算的。
数据总结在表2中。
表2
微胶囊(参考编号4) | 值 |
香味剂进料量的重量(理论) | 840mg |
W<sub>T</sub> | 630mg |
W<sub>U</sub> | 0mg(未检出) |
W<sub>s</sub>(理论) | 220mg |
香味剂负载效率 | 100% |
香味剂负载率 | 74% |
如表2中所示,由于未检测到未负载的香味剂,香味剂负载效率接近100%。然后计算出香味剂负载率为74%。因此,本发明的微胶囊的香味剂负载效率和负载率相当好。
实施例3:本发明微胶囊在配制物中的香味剂泄漏(以参考编号4为例)
表3中示出了简化的沐浴露配方(不含香味剂)
表3
成分 | 成分的重量% |
月桂醇醚硫酸钠 | 12.86 |
椰油酰胺丙基甜菜碱 | 5.67 |
椰油酰胺MEA | 1.35 |
丙烯酸酯共聚物 | 6 |
添加剂和防腐剂 | 1.95 |
水 | 至87 |
香味剂泄漏评估典型程序描述如下:将40mg微胶囊(参考编号4)(400mg微胶囊浆液,固体含量约10%,香味剂负载率74%)放入20ml小瓶中,向其加入3ml沐浴露配制物以得到约10mg/ml的最终香味剂浓度。将小瓶密封并在IKA MS2 Minishaker上以1000rpm振动1.5分钟以使配制物和胶囊充分混合。之后,将小瓶在室温下放置2、4或24小时。然后通过与36ml去离子水混合将混合物稀释约10倍,使用注射器驱动的过滤器(0.45μm,聚醚砜膜,ANPEL scientific Instrument Co.,Ltd.)过滤以去除胶囊。稀释的目的是降低配制物样品的粘度以促进过滤。然后将2ml上述滤液放入20ml小瓶中并与8ml乙醇混合(以确保香味剂浓度在用于GC-FID评估的预定校准曲线范围内),使用GC-FID评估滤液中的香味剂的量(香味剂泄漏)。
数据总结在表4中。
表4
沐浴露配制物中的储存时间(小时) | 泄露百分比(%) |
2 | 22±3 |
4 | 19±1 |
24 | 29±1 |
表4中的数据表明,24小时储存期间泄漏百分比在20-30%之间,并且随着储存时间的增加,没有观察到泄漏的明显增加。因此,所制备的香味剂胶囊的泄漏处于可接受的水平。
实施例4:本发明的微胶囊的香味剂释放(以参考编号4为例)
香味剂释放评估的典型程序描述如下:通过将100μl微胶囊浆液放入20ml小瓶中来制备微胶囊样品(参考编号4)。将小瓶(无盖)在通风橱中于室温(25℃)下放置0、1、2、3、4、5或6小时。通过将1.0g柠檬烯、2.3g吐温40和10.0g去离子水混合在一起来制备对照样品。对照样品中柠檬烯和吐温40的含量分别为7.5%和17.3%。将100μl对照样品放入20ml小瓶中,并将小瓶(无盖)在通风橱中于室温(25℃)下放置0、1、2、3、4、5或6小时。然后向装有胶囊样品或对照样品的小瓶中加入5ml乙醇,并密封小瓶。然后将小瓶在IKA MS2Minishaker上以1000rpm振动60秒。使用GC-FID评估乙醇中的香味剂的量(未释放的香味剂)。
数据总结在表5中。
表5
表5中的数据表明在3小时内几乎100%的香味剂从对照样品中释放出来,而在6小时从胶囊样品中仅释放了约60%的香味剂。因此,它表明了本发明的微胶囊的持久释放的特性。
Claims (15)
1.一种微胶囊,其包括:
(i)包含有益试剂的核;和
(ii)包含二氧化硅的壳;其中所述壳包括平均厚度为1-1000nm的片状无机材料;其中所述有益试剂是芳香剂、芳香剂前体、毛发调理剂、去屑剂、保湿剂、润肤剂、染料和/或颜料、颜色护理添加剂(包括染料固色剂)或它们的混合物。
2.如权利要求1所述的微胶囊,其中所述片状无机材料的平均粒径为以直径计10-2000nm。
3.如权利要求1或2所述的微胶囊,其中所述片状无机材料选自MgAl层状双氢氧化物、羟基磷灰石、硅藻土、氢氧化镁、氢氧化钙、沸石MCM-22、氮化硼。
4.如权利要求1至3中任一项所述的微胶囊,其中所述片状无机材料是MgAl层状双氢氧化物。
5.如权利要求1至4中任一项所述的微胶囊,其中所述片状无机材料是阴离子表面改性的。
6.如权利要求1至5中任一项所述的微胶囊,其中所述片状无机材料具有5-1000m2/g的比表面积。
7.如权利要求1至6中任一项所述的微胶囊,其中所述有益试剂选自芳香剂、芳香剂前体或它们的混合物。
8.如权利要求1至7中任一项所述的微胶囊,其中所述核包含增稠剂。
9.如权利要求1至8中任一项所述的微胶囊,其中所述微胶囊具有0.5-100微米的平均粒径。
10.如权利要求1至9中任一项所述的微胶囊,其中所述微胶囊是水性悬浮液的形式。
11.一种制备如权利要求1至10中任一项所述的微胶囊的方法,该方法包括以下步骤:
a)制备包含二氧化硅前体和有益试剂的油相液体;
b)通过将片状无机材料和去离子水的混合物均质化来制备水性悬浮液;
c)通过将片状无机材料的所述水性悬浮液加入所述油相液体中并均质化以形成乳液来制备o/w乳液;
d)将所述o/w乳液放入40℃烘箱中至少24小时,得到微胶囊浆液产品。
12.一种化妆品组合物,其包含在化妆品可接受的载体中的如权利要求1至10中任一项所述的微胶囊。
13.如权利要求12所述的组合物,其中所述组合物包含表面活性剂。
14.如权利要求12或13所述的组合物,其中所述组合物是洗去型产品。
15.如权利要求12至14所述的组合物,其中所述组合物是毛发护理组合物。
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