CN112533575B - 在含有疏水改性或非疏水改性的阴离子聚合物的清洁液中增强的保湿剂沉积 - Google Patents
在含有疏水改性或非疏水改性的阴离子聚合物的清洁液中增强的保湿剂沉积 Download PDFInfo
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- CN112533575B CN112533575B CN201980051361.XA CN201980051361A CN112533575B CN 112533575 B CN112533575 B CN 112533575B CN 201980051361 A CN201980051361 A CN 201980051361A CN 112533575 B CN112533575 B CN 112533575B
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A61K8/737—Galactomannans, e.g. guar; Derivatives thereof
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- A—HUMAN NECESSITIES
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- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/03—Liquid compositions with two or more distinct layers
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- A—HUMAN NECESSITIES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/31—Hydrocarbons
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
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Abstract
本发明涉及包含疏水改性和非疏水改性的交联阴离子聚合物的组合物，所述聚合物已被发现在包含阳离子沉积聚合物的组合物中最小程度地阻碍了保湿剂的沉积。
Description
技术领域
本发明涉及片状结构化的身体和毛发清洁组合物，其包含油基保湿剂，例如矿脂和甘油三酯油(以下称为“保湿剂”)。这样的保湿剂通常作为纯材料或以预乳化形式添加到清洁组合物中。本发明的组合物还包含通常用于增强保湿剂沉积的阳离子沉积聚合物。这样的阳离子沉积聚合物通常与阴离子结构化聚合物相互作用，通常也用于这样的层状结构化保湿组合物中；阳离子沉积聚合物(“CDP”)和阴离子结构化聚合物之间的这种相互作用降低了CDP的沉积效率，使得更少的保湿剂沉积。
背景技术
消费者非常希望使用保湿性且对皮肤和毛发损害较小的皮肤和毛发清洁制剂。用温和表面活性剂配制的层状清洁组合物符合上述标准，因为层状结构提供了提示保湿性的类似于洗剂的稠度，且温和表面活性剂对皮肤和毛发的损害较小。此外，与各向同性制剂不同，层状制剂还可以含有大量的疏水性润肤剂，例如甘油三酯油和矿脂，其提供临床保湿益处。这些保湿剂的沉积是通过添加阳离子沉积聚合物(例如瓜尔胶羟丙基三甲基氯化铵)来促进的(US 5,085,857)。
在授予Puvvada等的几项专利中已经举例说明了含有高含量润肤油(保湿剂)的层状制剂。参见，例如，US 5,952,286、US 5,962,395、US 6,150,312和US 6,426,326。然而，这些参考文献均未公开使用疏水改性或非疏水改性的阴离子聚合物结构化剂来稳定亚微米尺寸的保湿剂液滴，其可有效地沉积在包含阳离子沉积聚合物的层状液体中。
Wei等的美国专利8,105,996和8,158,566教导了疏水改性的阴离子聚合物在含有保湿剂(例如润肤油)的层状制剂中的用途。然而，这些参考文献中举例说明的层状制剂是用大量非离子乳化剂来结构化的。
它们还需要使用高含量的盐来形成层状结构。相比之下，我们的组合物含有0.4％，优选0.35％和更低的含量的HLB为1.4-13的非离子乳化剂。此外，在Wei的组合物中看到的高盐在我们的发明的制剂中也是不可取的，因为它们可以在生产过程中对设备造成腐蚀。相比之下，我们的制剂是用2.75％，优选2.7％或更少的氯化钠来配制。此外，在这些Wei参考文献中，并未认识到结构化聚合物如何影响保湿霜的沉积；以及制剂的温和性在这样的保湿剂的沉积中起什么作用。我们发明的组合物具有限定的温和度值(通过使用角质表面测定(Corneosurfametry)的CIM值测量)，该方法稍后定义。
如上所述，阳离子沉积聚合物通常用于促进油基保湿剂在层状液体中的沉积。同样如前所述，阴离子聚合物用于使液体结构化，但这些通常与阳离子沉积聚合物相互作用以降低沉积。
发明内容
预料不到地，申请人发现，特定类型的结构化聚合物，尤其是阴离子结构化聚合物，尤其是特定的交联的疏水改性或非疏水改性的阴离子聚合物，最小程度地干扰通过阳离子沉积聚合物沉积亚微米尺寸的保湿剂液滴，同时提供优异的稳定性。
更具体地，申请人发现，本发明的疏水改性或非疏水改性的阴离子聚合物可以通过以下的组合来限定：(a)在2％聚合物溶液中在特定pH水平下测量的粘度；和(b)聚合物溶液的剪切速率曲线的粘度的斜率。尽管不希望受限于理论，但这些变量据信与聚合物的阴离子性和分子量有关。当聚合物落在上述值(a)和(b)限定的范围内时，发现在存在阳离子沉积聚合物的情况下增强的保湿剂沉积。
制剂的温和性进一步影响了该效果(制剂具有大于53，优选大于55的角质表面测定温和度量热指数(corneosurfametry Calorimetric Index of Mildness)CIM)。同样如上所述，本发明的组合物包含0.4％或更少，优选0.3％或更少，更优选0.2％或更少，最优选0.1％或更少的HLB为1.4-13的非离子乳化剂，同时保持层状组合物的稳定性。相比之下，Wei的组合物需要高于该量的乳化剂来维持层状稳定性(参见结尾的表6)。本发明的组合物还优选包含2.7％或更少，优选2.5％或更少，更优选2％或更少，例如0.1-2重量％的盐。
更具体地，本发明的组合物可定义如下。
它们是具有温和表面活性剂体系的层状结构化清洁剂，其包含：
a)1-70％，优选2-30％，更优选5-20％的阴离子表面活性剂、两性表面活性剂和/或两性离子表面活性剂以及任选的非离子和其他表面活性剂的混合物；
b)0.1-20％，优选1-10％，更优选2-5重量％的中链(例如C8至C14)脂肪酸，例如辛酸、癸酸、月桂酸、肉豆蔻酸或其混合物；
c)0.1-25％，优选1-15％，更优选2-10％的保湿调理剂，例如矿脂和/或甘油三酯油的乳液；
d)0.01％-5％，优选0.1％-2％，更优选0.2-1％的阳离子沉积聚合物(也可称为阳离子调理聚合物)；和
e)0.01-5％，优选0.05-2％或0.1-1％的疏水改性或非疏水改性的阴离子交联聚合物，当在pH 6.35和5s-1的剪切速率下测量时，所述聚合物的2％溶液的粘度在1-100厘泊，更优选10-80厘泊，最优选20-60厘泊的范围内；
其中粘度剪切速率曲线的斜率在-0.6至-1.2的范围内，更优选在-0.7至-1.1的范围内，最优选在-0.8至-1.0的范围内；和
其中所述清洁制剂包含0.4％或更低、优选0.3％或更低、更优选0.2％或更低、最优选0.1％或更低的HLB为1.4-13的非离子乳化剂，和2.7％或更低、优选2.5％或更低且更优选2％或更低的盐，尤其是氯化钠，并且优选具有53或更大，优选55或更大，更优选55-65的角质表面测定温和度量热指数CIM。
具体实施方式
除实施例中或另有明确说明外，否则本说明书中所有表明材料数量或反应条件、材料物理性质和/或用途的数字均应理解为由“约”一词修饰。
在全文中，范围被用作描述范围内的每一个值的简写。范围内的任何值均可选择作为范围的终点。使用“和/或”表示可以单独选择列表中的任何一个，或者可以选择列表中的任何组合。
在为避免疑义，“包含”一词旨在指“包括”但不一定是“由……组成”或“由……构成”换句话说，列出的步骤或选项不需要是穷举性的。
除非另有说明，否则所用成分的一个或多个量的所有百分比应理解为基于材料在组合物的总重量中的有效重量的重量百分比，其总计为100％。(参见第15页)
本发明的组合物是层状结构化液体清洁组合物，其包含保湿调理剂，也称为保湿剂(例如矿脂、甘油三酯)；并且进一步包含阳离子沉积聚合物。
在存在阴离子增稠聚合物的情况下，阳离子沉积聚合物通常将与这样的增稠剂相互作用，并且该相互作用将对保湿剂的沉积产生负面影响。
预料不到地，申请人发现，当选择特定的疏水改性或非疏水改性的阴离子交联增稠聚合物时(通过在限定条件下的粘度和粘度剪切速率曲线的斜率两者限定)，相对于通常使用的阴离子结构化聚合物，保湿剂的沉积显著增强。非常令人惊讶的是，通过CIM测量的组合物的温和性进一步增强了沉积增强的效果。此外，本发明的组合物使用0.4％或更少，优选0.3％或更少，更优选0.2％或更少，最优选0.1％或更少的HLB为1.4-13的非离子乳化剂，和2.7％或更少，优选2.5％或更少，更优选2％或更少的盐，尤其是氯化钠，同时保持层状组合物的稳定性。较高含量的盐可对用于制备组合物的机械造成腐蚀。
更具体地，本发明的组合物包含：
a)1-70％，优选2-30％，更优选5-20％的(a)至少一种阴离子表面活性剂；(b)至少一种两性和/或两性离子表面活性剂；和(c)任选地，一种或多种非离子表面活性剂、阳离子表面活性剂或其混合物；
b)0.1-20％，优选1-10％，更优选2-5重量％的形成层状相的结构化剂；这可以是例如中链(例如，C8至C14)脂肪酸，例如月桂酸、肉豆蔻酸或其混合物；
c)0.1-25％，优选1-15％，更优选2-10％的保湿调理剂(油或润肤剂)，例如矿脂和/或甘油三酯油的乳液；
d)0.01-5％，优选0.1-2％，更优选0.2-1％的阳离子沉积聚合物(也称为阳离子调节剂)；和
e)0.01-5％，优选0.05-2％或0.1-1％的疏水改性或非疏水改性的阴离子交联聚合物，优选交联聚合物，当在pH 6.35和5s-1的剪切速率下测量时，所述聚合物的2％溶液的粘度在1-100厘泊，更优选10-80厘泊，最优选20-60厘泊的范围内；其中粘度剪切速率曲线的斜率在-0.6至-1.2的范围内，更优选在-0.7至-1.1的范围内，最优选在-0.8至-1.0的范围内；
其中所述清洁制剂包含0.4％或更少，优选0.1-0.35％的HLB为1.4-13的非离子乳化剂；和2.7％或更少，优选2.5％或更少，更优选2％或更少的盐，尤其是氯化钠，并且优选具有53或更高，优选55或更高，更优选55至65的角质表面测定温和度量热指数CIM。
下文将更具体地描述该组合物：
表面活性剂
本发明的表面活性剂体系占组合物的1-50重量％，优选2-30重量％，更优选5-20重量％，并且包含：
a)至少一种阴离子表面活性剂；
b)至少一种两性和/或两性离子表面活性剂；和
c)任选地，一种或多种非离子表面活性剂、阳离子表面活性剂或其混合物。
阴离子表面活性剂(其可占总组合物的2-40重量％)可以是例如脂族磺酸盐，例如伯烷(例如C8-C22)磺酸盐、伯烷(例如C8-C22)二磺酸盐、C8-C22烯磺酸盐、C8-C22羟烷磺酸盐或烷基甘油醚磺酸盐(AGS)；或芳族磺酸盐，例如烷基苯磺酸盐等。
阴离子表面活性剂也可以是烷基硫酸盐(例如，C12-C18烷基硫酸盐)或烷基醚硫酸盐(包括烷基甘油基醚硫酸盐)等。烷基醚硫酸盐包括具有下式的那些：
RO(CH2CH2O)nSO3M
其中R是具有8-18个碳，优选12-18个碳的烷基或烯基，n的平均值大于1.0，优选2-3；M是增溶性阳离子，例如钠、钾、铵或取代的铵。月桂基醚硫酸铵和钠是优选的。
阴离子表面活性剂也可以是烷基磺基琥珀酸盐(包括单烷基和二烷基，例如C6-C22磺基琥珀酸盐)；烷基和酰基牛磺酸盐、烷基和酰基肌氨酸盐、磺基乙酸盐、C8-C22烷基磷酸盐和磷酸盐、烷基磷酸酯和烷氧基烷基磷酸酯、酰基乳酸盐、C8-C22单烷基琥珀酸盐和马来酸盐、磺基乙酸盐和酰基羟乙基磺酸盐等。
磺基琥珀酸盐可以是具有下式的单烷基磺基琥珀酸盐：
R4O2CCH2CH(SO3M)CO2M
下式的酰胺基-MEA磺基琥珀酸盐：
R4CONHCH2CH2O2CCH2CH(SO3M)CO2M
其中R4的范围为C8-C22烷基，并且M是增溶性阳离子；
下式的酰胺基-MIPA磺基琥珀酸盐：
RCONH(CH2)CH(CH3)SO3M)CO2M
其中M定义见上文。
还包括烷氧基化的柠檬酸磺基琥珀酸盐；和烷氧基化的磺基琥珀酸盐，例如：
其中n＝1至20；M定义见上文。
肌氨酸盐通常由式RCON(CH3)CH2CO2M表示，其中R为C8至C20烷基，M为增溶性阳离子。
牛磺酸盐通常由下式表示：
R2CONR3CH2CH2SO3M
其中R2为C8-C20烷基，R3为C1-C4烷基，M为增溶性阳离子。
另一类阴离子表面活性剂是羧酸盐，例如：
R-(CH2CH2O)nCO2M
其中R为C8-C20烷基；n为0至20；M定义见上文。
可使用的另一种羧酸盐是酰胺基烷基多肽羧酸盐，例如Seppic的Monteine
可使用的另一种表面活性剂是C8-C18酰基羟乙基磺酸盐。这些酯是通过碱金属羟乙基磺酸盐与具有6-18个碳原子且碘值低于20的混合脂族脂肪酸之间的反应制备。至少75％的混合脂肪酸具有12至18个碳，且至多25％具有6至10个碳原子。
酰基羟乙基磺酸盐当存在时通常占总组合物的约0.5-15重量％。优选地，该组分以约1％至约10％存在。
酰基羟乙基磺酸盐可以是烷氧基化的羟乙基磺酸盐，如1995年2月28日授予Ilardi等的美国专利第5,393,466号，标题为“Fatty Acid Esters of PolyalkoxylatedIsethionic Acid”所述，其通过引用并入本申请。该化合物具有如下通式：
其中R是具有8-18个碳的烷基，M是1-4的整数，X和Y是氢或具有1-4个碳的烷基，M+是单价阳离子，例如钠、钾或铵。
另一类优选的阴离子表面活性剂是氨基酸的N-酰基衍生物。在相同的优选形式中，基本上不存在含硫酸盐的表面活性剂。优选0.1％或甚至0.05％或更低。优选完全不存在含硫酸盐的表面活性剂。
优选的表面活性剂是酰基谷氨酸盐、酰基天冬氨酸盐、酰基甘氨酸盐和酰基丙氨酸盐表面活性剂。优选地，这些是酰基谷氨酸盐或酰基天冬氨酸盐或酰基甘氨酸盐或酰基丙氨酸盐的钾和/或钠盐，其中超过65％的酰基链具有C14或更短，例如C8至C14(例如衍生自椰子脂肪酸)的链长。酰基链优选具有大于75％，更优选大于80％的C14或更短的链长。优选地，链长的大于75％，最优选大于80％的是C12、C14或其混合物。
有两种形式的可商购氨基酸表面活性剂。一种是粉末或薄片形式，通常更昂贵且纯度更高。固体二羧酸氨基酸表面活性剂的例子包括：
·N-椰油酰基-L-谷氨酸钠(例如，Ajinomoto的CS-11)
·N-月桂酰基-L-谷氨酸钠(例如Ajinomoto的LS-11)
·N-肉豆蔻酰基-L-谷氨酸钠(例如Ajinomoto的LS-11)
·N-椰油酰基-L-谷氨酸钾(例如Ajinomoto的CK-11)
·N-肉豆蔻酰基-L-谷氨酸钾(Ajinomoto的MK-11)
·N-月桂酰基-L-谷氨酸钾(Ajinomoto的LK-11)
·月桂酰基天冬氨酸钠(Asahi Kasei Chemical Corporation的AminoFoammerTMFLMS-P1)
·月桂酰基谷氨酸钠(Asahi Kasei Chemical Corporation的AminosurfactTMALMS-P1/S1)
·肉豆蔻酰基谷氨酸钠(Asahi Kasei Chemical Corporation的AminosurfactTMAMMS-P1/S1)
固体单羧酸氨基酸表面活性剂的例子包括：
·椰油酰基甘氨酸钠(例如Ajinomoto的GCS-11)
·椰油酰基甘氨酸钾(例如Ajinomoto的GCK-11)
液体氨基酸表面活性剂通常含有20～35％的表面活性剂活性物，并且具有高的pH和无机盐(例如3～6％的NaCl)。例子包括：
·ECS-22SB：椰油酰基谷氨酸二钠(30％水溶液)
·CS-22：椰油酰基谷氨酸二钠椰油酰基谷氨酸钠(25％水溶液)
·CK-22：椰油酰基谷氨酸钾(30％水溶液)
·LT-12：TEA-月桂酰基谷氨酸盐(30％水溶液)
·CT-12：TEA-椰油酰基谷氨酸盐(30％水溶液)
·ACT-12：TEA-椰油酰基甘氨酸盐(30％水溶液)
·ACS-12：椰油酰基丙酸钠(30％水溶液)
·GCK-12/GCK-12K：椰油酰基甘氨酸钾(30％水溶液)
·AminosurfactTMACDS-L：椰油酰基谷氨酸钠(25％水溶液)
·AminosurfactTMACDP-L：椰油酰基谷氨酸钾(22％)+椰油酰基谷氨酸钠(7％)
·AminosurfactTMACMT-L：TEA-椰油酰基谷氨酸盐(30％水溶液)
·AminoFoamerTMFLDS-L：月桂酰基天冬氨酸钠(25％水溶液)
两性离子和两性表面活性剂
两性离子表面活性剂的例子是可广泛描述为脂族季铵、鏻和锍化合物的衍生物的那些，其中脂族基可以是直链或支链，并且其中脂族取代基之一包含约8至约18个碳原子，一个包含阴离子基团，例如羧基、磺酸根、硫酸根、磷酸根或膦酸根。这些化合物的通式为：
其中R2含有约8至约18个碳原子、0至约10个环氧乙烷部分和0至约1个甘油基部分的烷基、烯基或羟基烷基；Y选自氮、磷和硫原子，R3是含有约1至约3个碳原子的烷基或单羟基烷基；当Y为硫原子时，X为1；当Y为氮或磷原子时，X为2；R4是具有约1至约4个碳原子的亚烷基或羟基亚烷基，Z是选自羧酸根、磺酸根、硫酸根、膦酸根和磷酸根的基团。
这种表面活性剂的例子包括：
4-[N,N-二(2-羟乙基)-N-十八烷基铵基]-丁烷-1-羧酸盐；
5-[S-3羟丙基-S-十六烷基磺基]-3-羟基戊烷-1-硫酸盐；
3-[P,P-二乙基-P-3,6,9-三氧杂四癸基(dexocyl)磷基]-2-羟基丙烷-1-磷酸盐；
3-[N,N-二丙基-N-3-十二烷氧基-2-羟基丙基铵基]-丙烷-1-膦酸盐；
3-[N,N-二甲基-N-十六烷基铵基]丙烷-1-磺酸盐；
3-[N,N-二甲基-N-十六烷基铵基)-2-羟基丙烷-1-磺酸盐；
4-[N,N-二(2-羟乙基)-N-(2-羟基十二烷基)氨基]-丁烷-1-羧酸盐；
3-[S-乙基-S-(3-十二烷氧基-2-羟丙基)磺基]-[丙烷-1磷酸盐；
3-[P,P-二甲基-P-十二烷基磷基]-丙烷-1-膦酸盐；和
5-[N,N-二(3-羟丙基)-N-十六烷基铵基]-2-羟基-戊烷-1-硫酸盐。
可用于本发明的两性洗涤剂包括至少一个酸基团。这可以是羧酸或磺酸基团。它们包括季氮，因此是季酰胺基酸。它们通常应包含7至18个碳原子的烷基或烯基。它们通常符合整体结构式：
其中R1是7-18个碳原子的烷基或烯基；
R2和R3各自独立地为1-3个碳原子的烷基、羟烷基或羧烷基；
n为2至4；
m为0至1；
X是任选地被羟基取代的1-3个碳原子的亚烷基，并且
Y是-CO2-或-SO3-。
上述通式内的合适的两性洗涤剂包括下式的简单甜菜碱：
和下式的酰胺基甜菜碱：
其中m为2或3。
在这两种情况下，式R1、R2和R3的定义如前。特别地，R1可以是衍生自椰子的C12和C14烷基的混合物，使得至少一半、优选至少四分之三的R1基团具有10至14个碳原子。R2和R3优选为甲基。合适的甜菜碱是椰油酰胺丙基甜菜碱。
另一种可能性是两性洗涤剂是具有下式的磺基甜菜碱：
其中m为2或3，或这些的变体，其中
被
替换。
在这些式中，R1、R2和R3如前所述。
两性乙酸盐和二两性乙酸盐也旨在被可以使用的可能的两性离子和/或两性化合物覆盖，尤其是C8-C20两性乙酸盐或其混合物等。合适的两性乙酸盐是月桂基两性乙酸钠。
两性/两性离子表面活性剂在使用时通常占0.1-30重量％，优选1-20重量％。
本发明优选的表面活性剂体系包含：阴离子表面活性剂(例如，碱金属烷基醚硫酸盐)为2-50％；两性表面活性剂(例如烷基甜菜碱或烷基两性乙酸盐)为1-20％。
表面活性剂体系也可任选地包含非离子表面活性剂。如上所述，本发明的特征在于，即使非离子乳化剂的含量为0.4％或更低，组合物仍保持层状结构。
可使用的非离子表面活性剂尤其包括具有疏水基和反应性氢原子的化合物(例如脂族醇、酸、酰胺或烷基酚)与环氧烷(特别是环氧乙烷单独或与环氧丙烷一起)的反应产物。具体非离子洗涤剂化合物为烷基(C6-C22)酚-环氧乙烷缩合物、脂肪族(C8-C18)直链或支链伯或仲醇与环氧乙烷的缩合产物、以及通过环氧乙烷与环氧丙烷和乙二胺的反应产物的缩合制备的产物。其他所谓的非离子洗涤剂化合物包括长链叔胺氧化物、长链叔膦氧化物和二烷基亚砜等。
非离子表面活性剂也可以是糖酰胺，例如多糖酰胺。具体地，该表面活性剂可以是1995年2月14日授予Au等的标题为“Compositions comprising nonionic glycolipidsurfactants”的美国专利第5,389,279号描述的乳糖醛酸酰胺(lactobionamides)之一，该专利通过引入并入本文，或者其可以是1991年4月23日授予Kelkenberg的标题为“Use ofn-polyhydroxyalkyl fatty acid amides as thickening agents for liquid aqueoussurfactant systems”的美国专利第5,009,814号描述的糖酰胺之一，该专利通过引入并入本申请。
Parran Jr.的美国专利第3,723,325号和1986年1月21日授予Llenado的题为“Foaming surfactant compositions”的美国专利第4,565,647号公开的烷基多糖非离子表面活性剂描述了其他可使用的表面活性剂，这两个专利通过引入并入本申请。
优选的烷基多糖是下式的烷基多糖苷：
R2O(CnH2nO)t(糖基)x
其中R2选自烷基、烷基苯基、羟烷基、羟烷基苯基及其混合物，其中烷基含有约10至约18个、优选约12至约14个碳原子；n为0至3，优选为2；t为0至约10，优选为0；x为1.3至约10，优选1.3至约2.7。糖基优选衍生自葡萄糖。为了制备这些化合物，首先形成醇或烷基聚乙氧基醇，然后与葡萄糖或葡萄糖源反应以形成糖苷(在1-位连接)。然后，额外的糖基单元可以连接在它们的1-位和前面的糖基单元2-位、3-位、4-位和/或6-位之间，优选主要在2-位。
非离子表面活性剂可以占组合物的0-10重量％或0-5重量％。然而，在优选实施方式中，具有Wei示例的类型的非离子乳化剂占组合物的0.4重量％或更低，优选0.3重量％，更优选0.2重量％或更低，最优选0.1重量％或更低。与上文讨论的Wei参考文献不同，即使在这些低含量的非离子乳化剂下，层状结构仍保持稳定。
层状结构化剂
本发明的组合物使用约0.1-20重量％。优选1-10重量％，更优选2-5重量％的在组合物中起作用以形成层状相的结构化剂。这种层状相使得组合物能够更容易地悬浮颗粒(例如润肤剂颗粒)，同时仍保持良好的剪切稀化性能。层状相还为消费者提供所需的流变性(“堆积(heaping)”)。
结构化剂优选为脂肪酸或其酯衍生物、脂肪醇或三羟基硬脂精等。更优选地，结构化剂选自辛酸、癸酸、月桂酸、肉豆蔻酸及其混合物。
可使用的脂肪酸的例子是C8-C22酸，例如如下：月桂酸、油酸、异硬脂酸、亚油酸、亚麻酸、蓖麻油酸、反油酸、花生四烯酸、肉豆蔻油酸和棕榈油酸等。酯衍生物包括丙二醇异硬酯酸盐、丙二醇油酸盐、甘油异硬酯酸盐、甘油油酸盐和聚甘油二异硬脂酸盐等。
保湿和调理剂(例如油/润肤剂)
本发明的主要益处之一是能够将油/润肤剂颗粒悬浮在层状相组合物中(并且能够在少量非离子表面活性剂存在的情况下这样做)。例如，下列油/润肤剂可以任选地悬浮在本发明的组合物中。
各种类型的油如下所述。
植物油：花生油、蓖麻油、可可油、椰子油、玉米油、棉籽油、橄榄油、棕榈仁油、菜籽油、红花籽油、芝麻籽油、葵花籽油和大豆油等。
酯：肉豆蔻酸丁酯、棕榈酸鲸蜡酯、油酸癸酯、月桂酸甘油酯、蓖麻油酸甘油酯、硬脂酸甘油酯、异硬脂酸甘油酯、月桂酸己酯、棕榈酸异丁酯、硬脂酸异鲸蜡酯、异硬脂酸异丙酯、月桂酸异丙酯、亚油酸异丙酯、肉豆蔻酸异丙酯、棕榈酸异丙酯、硬脂酸异丙酯、单月桂酸丙二醇酯、蓖麻油酸丙二醇酯、硬脂酸丙二醇酯和异硬脂酸丙二醇酯等。
动物脂肪：乙酰化羊毛脂醇、羊毛脂、猪油、貂油和牛油等。
油润肤剂的其他例子包括矿物油、矿脂、硅油如二甲基聚硅氧烷、月桂基和肉豆蔻基乳酸盐等。
润肤剂/油的用量通常为组合物的约1-25重量％，优选1-10重量％。
阳离子调理剂
组合物包含0.01-5重量％，优选0.1-2重量％的阳离子沉积聚合物(阳离子调理剂)。
阳离子调理剂可包括LM-200、polyquaternium-24、/>plus 3330、polyquaternium-39和/>型聚合物。它们还可包括阳离子纤维素型聚合物，例如Polyquaternium 10(来自Dow的UCare Series)和合成阳离子聚合物，例如Polyquaternium 49和polyquaternium 51。(来自Lubrizol的Merquat Series)]
阳离子沉积聚合物也可包括疏水改性的阳离子纤维素聚合物，例如来自DowChemical Company的SoftCat Series。
另外，本发明的组合物可包含如下任选成分：
有机溶剂，如乙醇；辅助增稠剂、螯合剂，例如乙二胺四乙酸四钠(EDTA)、EHDP或其混合物，其量为0.01-1％，优选0.01-0.05％；以及着色剂、遮光剂和珠光剂，例如硬脂酸锌、硬脂酸镁、TiO2或EGMS(单硬脂酸乙二醇酯)；所有这些都可用于增强产品的化妆品性质的表现。
组合物可进一步包含抗微生物剂，例如2-羟基4,2’4’三氯二苯醚(DP300)；防腐剂，如二羟甲基二甲基乙内酰脲(Glydant XL1000)、对羟基苯甲酸酯、山梨酸等。
组合物还可包含作为泡沫增强剂的椰油酰基单或二乙醇酰胺。
抗氧化剂，例如丁基化的羟基甲苯(BHT)，如果合适，可以有利地以约0.01％或更高的量使用。
可加入的另一种任选成分是抗絮凝聚合物，例如1992年9月15日授予Montague的题为“Liquid Detergent Composition in the Form of Lamellar Deoplets Containinga Deflocculating Polymer”的美国专利第5,147,576号教导的，该专利通过引入并入本文。
可包含的其他成分是磨砂剂，例如聚氧乙烯珠、胡桃木片和杏仁等。
如上所述，本发明的组合物是层状组合物。特别地，层状相占总相体积的20-80％，优选30-65％。相体积可通过例如传导率测量或本领域技术人员熟知的其他测量来测量。尽管不希望受限于理论，但据信更高的相体积提供更好的润肤剂悬浮。
本发明的结构化聚合物是疏水改性的阴离子交联聚合物。这种聚合物也被称为“缔合”聚合物。
这些聚合物由亲水主链和疏水侧链构成。它们在溶液中的行为是其结构的疏水性和亲水性之间的竞争的结果。疏水单元导致在大分子链之间形成构成连接点的聚集体。从流变性的角度来看，这些通常为水溶性(例如，通常在微酸性或碱性条件下可溶)的聚合物在水中具有非常高的稠化能力，并且在盐介质中充分保持其粘度。在混合的聚合物和表面活性剂体系中，可以形成表面活性剂聚集体，其通过不同类型的相互作用(静电相互作用、偶极相互作用或氢键)而稳定化。典型的水溶性聚合物由于其疏水部分可以更特定地与表面活性剂相互作用。
这些聚合物的亲水主链尤其可以由包含含有随后可以在其上接枝疏水链的官能团(例如酸官能团)的亲水单体的聚合产生。这种制备聚合物的方法在“Water SolublePolymers”,ACS Symposium Series 467,ed.Shalaby W.Shalaby et al.,Am.Chem.Soc.Washington(1991),pp.82-200中具体描述。然而，也可以使用天然来源的水溶性聚合物，或通过化学改性而变为水溶性的天然聚合物。聚合物也可以通过亲水单体和疏水单体的共聚合形成。以比亲水聚合物少得多的量引入反应介质中的这些疏水聚合物通常包含脂肪族烃链。该制备方法在S.Biggs et al.,J.Phys.Chem.(1992,96,pp 1505-11)的出版物中描述。
这些聚合物的例子是丙烯酸类聚合物、聚醚和可部分取代的聚糖链。亲水主链由带有高度疏水的侧基的单体构成。带有疏水侧基的单体的摩尔百分比称为亲水链的改性百分比。疏水侧基可以是常规用于制备所述聚合物的任何疏水侧基。一方面，所使用的疏水基团包含含有至少8个碳原子、优选10至28个碳原子的主链。
这些疏水基团的具体例子是直链、支链、饱和或不饱和的烃链，其可以包含也可以不包含环。疏水基团的优选例子是含有8-28个碳原子，优选12-22个碳原子的烃链，特别是烷基链。改性单元有利地为醚、酯或酰胺的形式。当缔合聚合物的主链是丙烯酸链时尤其如此。所使用的缔合聚合物的质量平均摩尔质量可在104至107范围内。
组合物中聚合物的浓度通常为按组合物的重量计约0.01％至约5％或约0.05％至约2.0％，优选约0.1％至约1.0％或约0.1％至约0.5％。优选的缔合聚合物包括疏水改性的聚丙烯酸酯；疏水改性的多糖；疏水改性的聚氨酯。聚合物的非限制性例子包括丙烯酸酯/异癸酸乙烯酯交联聚合物(来自3V的Stabylen 30)、丙烯酸酯/丙烯酸C10-30烷基酯交联聚合物(来自Pemulen TR1和TR2)、丙烯酰二甲基牛油酸铵/山嵛醇聚醚-25甲基丙烯酸酯交联聚合物(来自Clariant的Aristoflex HMB)、丙烯酸酯/山嵛醇聚醚-25甲基丙烯酸酯共聚物(来自Rohm and Haas的Aculyn 28)；丙烯酸酯/硬脂醇聚醚-20甲基丙烯酸酯共聚物(来自Rohm and Haas的Aculyn 22)、PEG-150/癸基醇/SMDI共聚物(来自Rohm and Haas的Aculyn44)、PEG-150双硬脂酸盐(来自Rohm and Haas的Aculyn 60)、丙烯酸酯/硬脂醇聚醚-20甲基丙烯酸酯交联聚合物(来自Rohm and Haas的Aculyn 88)。
在一个实施方式中，该聚合物是交联碱性可溶胀缔合聚合物，其包含酸性单体和具有疏水端基的缔合单体，其中该聚合物包含一定百分比的疏水改性和包含具有一定长度的烷基官能团的疏水侧链。不旨在受理论限制，据信酸性单体对聚合物在酸基团中和后在水中溶胀的能力做出贡献；并且缔合单体(例如具有疏水链的单体)将聚合物锚定在结构化表面活性剂疏水域(例如片层)中，以将结构赋予表面活性剂组合物，并保持聚合物不在电解质存在下塌陷和失效。该交联缔合聚合物包含一定百分比的疏水改性，其是单体的摩尔百分比，表示为聚合物主链中的所有单体的总数的百分比，包括酸性和其他非酸性单体两者。该聚合物的疏水改性百分比(以下称％HM)可通过合成过程中加入的单体的比例或通过分析技术(如质子核磁共振(NMR))确定。烷基侧链长度可以类似地确定。出于本发明的目的，仅包含2个或更少烷基烃(例如乙基、甲基)的单体不被认为是缔合的，所有具有多于2个碳的侧链都是缔合的。缔合烷基侧链包括例如丁基、丙基、硬脂基、硬脂醇聚醚、鲸蜡基、月桂基、月桂醇聚醚、辛基、山嵛基、山嵛醇聚醚、硬脂醇聚醚或其他直链、支链、饱和或不饱和的烷基或烷基醇聚醚(alketh)烃侧链。
本发明的优选聚合物是疏水改性或非疏水改性的交联聚丙烯酸酯，而不是疏水改性的直链聚丙烯酸酯。它们的粘度通常低得多。
更具体地，2％溶液(例如在水中)的粘度(在pH 6.35和剪切速率5s-1下测量，并在25℃下使用流变仪进一步测量)在1至100厘泊，更优选10至80厘泊，最优选20至60厘泊的范围内。此外，粘度剪切速率曲线的斜率在-0.6至-1.2的范围内，更优选在-0.7至-1.1的范围内，最优选在-0.8至-1.0的范围内。
该斜率衡量聚合物的剪切稀化性质，其中斜率越高(越负)，聚合物越剪切稀化。
本发明的组合物包含0.4％或更少，优选0.3％或更少，更优选0.2％或更少，最优选0.1％或更少的HLB为1.4-13的非离子乳化剂，例如上述Wei等的美国专利8,105,996和美国专利8,158,566中使用的那些。
本发明的进一步组合物包含2.7％或更少，优选2.5％或更少，更优选2％或更少的盐，尤其是氯化钠。
实施例
制备以下组合物。矿脂乳液如下表2所述和表2下方的制备说明而制备。
表1
制剂总结：
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*使用各种各样结构性聚合物，其浓度在0.2％至1.05％范围内变化，以获得Brookfield粘度计测得的相似制剂TA粘度，其范围为70,000-110,000cP。
**矿脂乳液的组成和制备该乳液的程序如下所述。
表2
矿脂乳液的典型组成及制备该乳液的程序
| 组分 | 重量％ |
| 椰油酰基羟乙基磺酸钠 | 6.0 |
| 月桂酸 | 3.5 |
| 矿脂 | 55.0 |
| 水 | 至100 |
| Glydant Plus Liquid | 0.158 |
程序：
| 成分 | 重量％ |
油相：
| G-2212矿脂 | 55.00 |
| 月桂酸 | 3.50 |
水相：
| 浓缩SCI(85％) | 6.000 |
| DI水 | 35.342 |
| Glydant plus liquid | 0.158 |
合计100.000
1.水相在搅拌的槽式混合器中混合和加热，油相在单独的烧杯中加热。一旦加热，将油相加入到含有该水相的搅拌的槽式混合器中。油相和水相两者被分别加热至75摄氏度并合并，或在合并它们后加热至75摄氏度。在合并相并完全覆盖后，均化器升至1000rpm。
2.加入相后，将组合物混合并在4000rpm下均化10分钟
3.将组合物在5000psi下通过(一次通过)台式超声仪Nano DeBee。
表3
使用角质表面测定测量不同制剂的温和性(参考Liu et al.,Journal ofCosmetic Science 2016,38,178-186)
使用Tukey-Kramer HSD(95％置信水平)对所有配对进行的CIM比较的平均值比较
| CIM平均值 | |
| 实施例3 | 57.65* |
| 实施例4 | 57.12* |
| 实施例1 | 56.70* |
| 比较例A | 50.38** |
标示*的值彼此之间没有显著性差异(实施例1、2和3)，标示**(比较例A)的值与标示*(再次是实施例1、2和3)的值有显著性差异。
上表3证实组合物的温和性可以根据例如表面活性剂组成而变化。
表4
矿脂沉积量(克)和2％聚合物溶液在pH 6.35和剪切速率5s-1的粘度
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讨论
从表4可以看出，沉积是所使用的结构化聚合物的类型的函数。
更具体地，从表4看出，沉积与在pH 6.35和5s-1剪切速率下测量的2％聚合物溶液的粘度成反比。该关系是线性的，置信水平超过90％，与疏水聚合物是直链的还是交联的无关。还可以看出，疏水改性或非疏水改性的交联聚合物比疏水改性的直链聚合物沉积高得多的水平的矿脂。
用于测定矿脂沉积的程序如下：
用12ml不含PJ乳液的沐浴露基制剂洗涤一块8×8英寸的丝绸。通过从经洗涤和干燥的丝绸的重量中减去未经处理的丝绸块的重量获得空白沉积值。接下来，用含有PJ乳液的沐浴露洗涤另一块丝绸。总PJ沉积测量为洗涤和干燥后的丝绸的重量减去丝绸初始重量减去空白沉积。
表5
从各种制剂沉积的聚合物量(D)，克
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表5显示，沉积取决于实施例1至3的那些制剂使用的聚合物，其在统计学上具有相同水平的温和度(见表3)。相比之下，在实施例4的制剂中(该制剂在统计学上比其他制剂更刺激性)，沉积不受所用聚合物的影响。这证实，对沉积的影响是由CIM值定义的温和度的函数。当组合物具有例如55或更高的CIM值时，具有较低粘度的聚合物(例如，Pemulen TR1相比于Aculyn 88)增强油的沉积，但当组合物具有低于55的CIM值时，不增强粘度。
表6
US8,158,566B2表3中的发明实施例1和2，采用不同水平的非离子乳化剂Trideceth-3和盐，Stabelyn 30和Aculyn 28作为缔合聚合物，按照该专利教导的程序进行
*两周后，该样品变得不稳定，显示明显分离成两相。
在美国8,158,566B2的表3中使用Aculyn 28作为缔合聚合物的发明实施例2按照该专利中列出的程序在不同水平的Trideceth-3(非离子乳化剂)下重制。此外，重制比较例A-3。结果见表6。结果表明，与专利中显示的值90Pa相比，申请人在没有缔合聚合物的情况下获得的杨氏模量为22.4Pa。换句话说，其90的杨氏模量约等于我们的22.4的杨氏模量，因此比例因子为90除以24，等于4.1。因此我们可以证明，在我们的实施例中，低于约24.4Pa的任何值都将低于US8,158,566B2表3脚注中所示的100Pa的相应目标值，即100除以比例因子4.1等于24.4。低于该100Pa值(在我们的重制实验中相当于24.4Pa)的任何事物均因稳定性受损而失败，组合物因此是不期望的。
在US8,158,566B2表3中使用Stabylen作为缔合聚合物的发明实施例1按照该专利中列出的程序在3.3％和2.7％的两种不同盐含量下以0.35％的Trideceth-3(非离子乳化剂)重制。这些结果表明，在0.35％的非离子乳化剂和2.7％的盐含量下，杨氏模量远低于(24.4)Pa(相当于Wei专利中的100Pa)的阈值。此外，在0.35％非离子乳化剂和2.7％盐含量下的样品不稳定，在两周后显示完全相分离。
基于这些结果，低于0.4％，特别是0.35％的非离子Trideceth-3水平和2.7％的盐(氯化钠)水平定义了杨氏模量的阈值保持值。
Claims (34)
1.一种层状清洁组合物，其包含：
a)1-70重量％的阴离子表面活性剂、两性表面活性剂和/或两性离子表面活性剂以及任选的非离子和其他表面活性剂的混合物，所述阴离子表面活性剂包括酰基谷氨酸盐、酰基甘氨酸盐、酰基羟乙基磺酸盐和/或甲基酰基牛磺酸盐；所述两性表面活性剂包括两性乙酸盐，所述两性离子表面活性剂包括椰油酰胺丙基甜菜碱和/或磺基甜菜碱；
b)0.1-20重量％的C8至C14脂肪酸；
c)0.1-25重量％的保湿调理剂；
d)0.01重量％-5重量％的阳离子沉积聚合物，其包括瓜尔胶羟丙基三甲基氯化铵；
e)0.01-5重量％的疏水改性或非疏水改性的阴离子交联聚合物，当在pH 6.35和5s-1的剪切速率下测量时，所述聚合物的2重量％溶液的粘度在1-100厘泊的范围内；并且其中粘度剪切速率曲线的斜率在-0.6至-1.2的范围内，其中所述疏水改性或非疏水改性的阴离子交联聚合物选自疏水改性的聚丙烯酸酯、疏水改性的多糖、疏水改性的聚氨酯或其组合；
f)0.1-20重量％的层状结构化剂；
和
其中所述层状清洁组合物具有0-0.4重量％的水平的HLB为1.4-13的非离子乳化剂，和2.7重量％或更低的盐，所述组合物基本上不包括含硫酸盐的表面活性剂。
2.根据权利要求1所述的组合物，其中，在a)中，所述组合物包含2-30重量％的所述混合物。
3.根据权利要求1所述的组合物，其中，在a)中，所述组合物包含5-20重量％的所述混合物。
4.根据权利要求1所述的组合物，其中所述组合物包含1-10重量％的C8至C14脂肪酸。
5.根据权利要求1所述的组合物，其中所述组合物包含2-5重量％的C8至C14脂肪酸。
6.根据权利要求1所述的组合物，其中所述脂肪酸选自辛酸、癸酸、月桂酸、肉豆蔻酸或其混合物。
7.根据权利要求1所述的组合物，其中所述组合物包含1-15重量％的保湿调理剂。
8.根据权利要求1所述的组合物，其中所述组合物包含2-10重量％的保湿调理剂。
9.根据权利要求1所述的组合物，其中所述保湿调理剂是矿脂和/或甘油三酯油的乳液。
10.根据权利要求1所述的组合物，其中所述组合物包含0.1重量％-2重量％的阳离子沉积聚合物。
11.根据权利要求1所述的组合物，其中所述组合物包含0.2-1重量％的阳离子沉积聚合物。
12.根据权利要求1所述的组合物，其中所述组合物包含0.05-2重量％的疏水改性或非疏水改性的阴离子交联聚合物。
13.根据权利要求1所述的组合物，其中所述组合物包含0.1-1重量％的疏水改性或非疏水改性的阴离子交联聚合物。
14.根据权利要求1所述的组合物，其中，在e)中，当在pH 6.35和5s-1的剪切速率下测量时，所述聚合物的2重量％溶液的粘度在10-80厘泊的范围内。
15.根据权利要求1所述的组合物，其中，在e)中，当在pH 6.35和5s-1的剪切速率下测量时，所述聚合物的2重量％溶液的粘度在20-60厘泊的范围内。
16.根据权利要求1所述的组合物，其中，在e)中，粘度剪切速率曲线的斜率在-0.7至-1.1的范围内。
17.根据权利要求1所述的组合物，其中，在e)中，粘度剪切速率曲线的斜率在-0.8至-1.0的范围内。
18.根据权利要求1所述的组合物，其中所述层状清洁组合物具有0-0.35重量％的水平的HLB为1.4-13的非离子乳化剂。
19.根据权利要求1所述的组合物，其中所述层状清洁组合物具有0.1-0.35重量％的水平的HLB为1.4-13的非离子乳化剂。
20.根据权利要求1所述的组合物，其中所述层状清洁组合物具有0.3重量％或更低的水平的HLB为1.4-13的非离子乳化剂。
21.根据权利要求1所述的组合物，其中所述层状清洁组合物具有0.25重量％或更低的水平的HLB为1.4-13的非离子乳化剂。
22.根据权利要求1所述的组合物，其中所述层状清洁组合物具有2.5重量％或更低的盐。
23.根据权利要求1所述的组合物，其中所述层状清洁组合物具有2重量％或更低的盐。
24.根据权利要求1所述的组合物，其中所述盐是氯化钠。
25.根据权利要求1所述的组合物，其中所述组合物具有53或更高的Liu等,JournalofCosmetic Science 2016,38,178-186中定义的角质表面测定温和度量热指数CIM。
26.根据权利要求1所述的组合物，其中所述组合物具有55或更高的Liu等,JournalofCosmetic Science 2016,38,178-186中定义的角质表面测定温和度量热指数CIM。
27.根据权利要求1所述的组合物，其中所述组合物具有55至65的Liu等,JournalofCosmetic Science 2016,38,178-186中定义的角质表面测定温和度量热指数CIM。
28.根据权利要求1至27中任一项所述的组合物，其中所述保湿调理剂为亚微米矿脂乳液。
29.根据权利要求1至27中任一项所述的组合物，其中所述保湿调理剂为甘油三酯油。
30.根据权利要求29所述的组合物，其中所述甘油三酯油为葵花籽油或大豆油。
31.根据权利要求1至27中任一项所述的组合物，其中所述阳离子沉积聚合物为瓜尔胶羟丙基三甲基氯化铵。
32.根据权利要求1至27中任一项所述的组合物，其中所述阳离子沉积聚合物是阳离子取代的纤维素衍生物。
33.根据权利要求1至27中任一项所述的组合物，其中所述疏水改性或非疏水改性的阴离子交联聚合物为卡波姆、丙烯酸酯/硬脂醇聚醚-20甲基丙烯酸酯交联聚合物、丙烯酸酯/C10-30烷基丙烯酸酯交联聚合物、或丙烯酸酯/异癸酸乙烯酯交联聚合物。
34.根据权利要求1至27中任一项所述的组合物，其中存在非离子表面活性剂并且为CMEA。
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| EP18186321 | 2018-07-30 | ||
| EP18186321.8 | 2018-07-30 | ||
| PCT/EP2019/068536 WO2020025275A1 (en) | 2018-07-30 | 2019-07-10 | Enhanced moisturizer deposition in cleansing liquids containing hydrophobically or non-hydrophobically modified anionic polymers |
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| CN112533575B true CN112533575B (zh) | 2023-12-01 |
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| EP (1) | EP3829528B1 (zh) |
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| MX2022008876A (es) * | 2020-01-21 | 2022-08-11 | Unilever Ip Holdings B V | Composicion del tensoactivo concentrado hidratable. |
| WO2021148428A1 (en) | 2020-01-21 | 2021-07-29 | Unilever Ip Holdings B.V. | Isotropic concentrate and wash compositions |
| JP2022171305A (ja) * | 2021-04-30 | 2022-11-11 | 花王株式会社 | 毛髪化粧料 |
| JP2022171640A (ja) * | 2021-04-30 | 2022-11-11 | 花王株式会社 | 毛髪化粧料 |
| WO2024002646A1 (en) * | 2022-06-30 | 2024-01-04 | Unilever Ip Holdings B.V. | Stable wash composition with biodegradable thickener |
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| CA3107160A1 (en) | 2020-02-06 |
| CN112533575A (zh) | 2021-03-19 |
| BR112021000979A2 (pt) | 2021-04-20 |
| WO2020025275A1 (en) | 2020-02-06 |
| JP7459053B2 (ja) | 2024-04-01 |
| JP2021533137A (ja) | 2021-12-02 |
| EP3829528A1 (en) | 2021-06-09 |
| EP3829528B1 (en) | 2024-03-20 |
| US20210290517A1 (en) | 2021-09-23 |
| EA202190037A1 (ru) | 2021-09-24 |
| MX2021001175A (es) | 2021-04-19 |
| ZA202100603B (en) | 2022-08-31 |
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