CN101896517A - 制备丙烯酰胺基聚合物的反相胶乳的新方法和包含所述胶乳的组合物 - Google Patents
制备丙烯酰胺基聚合物的反相胶乳的新方法和包含所述胶乳的组合物 Download PDFInfo
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- CN101896517A CN101896517A CN2008801204901A CN200880120490A CN101896517A CN 101896517 A CN101896517 A CN 101896517A CN 2008801204901 A CN2008801204901 A CN 2008801204901A CN 200880120490 A CN200880120490 A CN 200880120490A CN 101896517 A CN101896517 A CN 101896517A
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- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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Abstract
本发明涉及制备含有20-70重量%,优选25-50重量%的支化或交联聚电解质的反相胶乳的方法,其特征在于所述聚电解质是部分或完全成盐的2-丙烯酰胺基-2-甲基丙磺酸与丙烯酰胺和任选地选自含有部分或完全成盐的弱酸官能团的单体和/或非丙烯酰胺的中性单体中的一种或多种单体形成的共聚物,所述制备方法包括控制在初始水相中的pH;还涉及包含通过所述方法直接获得的反相胶乳的化妆品组合物、皮肤药物组合物或药物组合物。
Description
本专利申请涉及油包水型反相胶乳的制备方法,以及所述反相胶乳作为增稠剂和/或乳化剂用于护肤和护发产品或用于生产化妆品制剂、皮肤化妆品制剂、皮肤药物制剂或药物制剂的用途。
用于化妆品或药物工业的增稠剂是用来增稠水相、洗液或霜-凝胶。在霜-凝胶的情况下,尤其是当需要将高含量油加入到配制剂中时,也添加乳化剂。然而,乳化剂经常是低分子量的产品,它们与聚合物相比可能皮肤耐受差。此外,使用聚合物能够在不加热的情况下制备霜-凝胶,这降低了生产成本并同时保持在这些霜-凝胶中所含的热敏性分子完整。因此,已经寻求开发既是增稠剂又是乳化剂的聚合物。在它们之中,可提及2-丙烯酰胺基-2-甲基丙磺酸(AMPS)和丙烯酰胺的用N,N-亚甲基双(丙烯酰胺)交联的共聚物的自可逆反相胶乳,其部分或完全中和为钠盐或钾盐的形式,所述聚合反相乳液公开在欧洲专利申请公开EP 0 503 853和国际公开WO 01/35922中。在这两篇文献中,制备方法包括使用按重量计50-60重量%的AMPS钠盐和丙烯酰胺的水溶液以及聚合在pH=7下进行。这种AMPS钠盐溶液可作为CIM化学品下的商品名为ATBSNa的按重量计55重量%的溶液或作为在Lubrizol下的商品名为AMPS2405和AMPS2405A的按重量计50%或58重量%的溶液而获得。丙烯酰胺可以作为50重量%的丙烯酰胺商购,或以固体形式商购。丙烯酰胺单体可以通过化学方法从丙烯腈获得,这减少了副产物3,3’,3”-次氮基三(丙酰胺)的形成。例如,作为KEMIRA生产的“丙烯酰胺50%”是根据涉及在铜催化下将丙烯腈水解的方法制备的,所以暗示着在超过100℃的温度下用碱预先处理的这种阮内铜催化剂的活化。催化反应是在高温(约100℃)和碱性pH下进行的。丙烯酰胺单体也可以通过酶催方法合成,这不会引起形成这种副产物。例如,由SNF生产的“Acrylamide 50 HST”是根据涉及在酶催化(腈水合酶)将丙烯腈水解的方法制备的,所以是在温和催化条件(20-25℃,中性pH)下进行的。此外,这种副产物是当丙烯酰胺处于碱性pH的溶液中形成的,不论生产方法如何。已经观察到,根据储存条件和储存时间,在一些最终聚合物组合物的样品中的丙烯酰胺浓度提高超过了2ppm限度,直到所述组合物在局部应用中成为不利的。
所以,根据第一实施方案,本发明涉及改进的生产丙烯酰胺基聚合物的反相胶乳的方法,该方法避免了丙烯酰胺在最终组合物中的释放。根据一个更特定的方面,本发明涉及一种制备组合物的方法,所述组合物包含油相、水相、至少一种油包水(W/O)型乳化体系、任选地至少一种水包油(O/W)型乳化体系,其是包含20-70重量%、优选25-50重量%的支化或交联聚电解质的反相胶乳形式,其特征在于所述聚电解质是部分或完全以钠盐或钾盐或铵盐形式成盐的2-丙烯酰胺基-2-甲基丙磺酸与丙烯酰胺和任选地选自含有部分或完全以钠盐或钾盐或铵盐形式成盐的弱酸官能团的单体和/或非丙烯酰胺的中性单体中的一种或多种单体的共聚物,所述制备方法包括以下步骤:
步骤a):制备水相(A),此水相含有丙烯酰胺、部分或完全以钠盐或钾盐或铵盐形式成盐的2-丙烯酰胺基-2-甲基丙磺酸、任选地选自含有部分或完全以钠盐或钾盐或铵盐形式成盐的弱酸官能团的单体和/或非丙烯酰胺的中性单体中的一种或多种单体以及可能的其它亲水性添加剂,所述制备包括将游离的2-丙烯酰胺基-2-甲基丙磺酸、任选地钠盐或钾盐或铵盐形式的2-丙烯酰胺基-2-甲基丙磺酸、丙烯酰胺、所述任选使用的亲水性添加剂和任选使用的选自氢氧化钠、氢氧化钾或氨水的碱性试剂放入水中,使得此溶液的pH保持大于1且小于5,从而获得pH大于1且小于5的第一含水混合物A1;并将所述第一含水混合物A1的pH值调节到5-6.5之间的pH,获得所述水相(A);
步骤b):在有机相中乳化所述水相(A),所述有机相含有油包水(W/O)型的表面活性剂体系、要存在于最终组合物中的油、任选地挥发油和任选地疏水性添加剂,从而形成油包水型乳液(B);
-步骤c):在所述油包水型乳液(B)中聚合单体,所述反应是通过将自由基引发剂引入所述乳液(B)中引发的,形成所述共聚物(P)的反相胶乳(L1);
-任选的步骤d):其中,所述共聚物(P)的所述反相胶乳(L1)是通过蒸馏浓缩直到所述挥发油被除去,形成所述共聚物(P)的反相胶乳(L2);和
步骤e):其中任选地,将水包油(O/W)型的乳化体系在低于50℃的温度加入所述共聚物(P)的所述反相胶乳(L1)中,或任选地加入所述共聚物(P)的所述反相胶乳(L2)中,形成所述共聚物(P)的自可逆反相胶乳(L3)。
非丙烯酰胺的中性单体尤其选自甲基丙烯酰胺、双丙酮丙烯酰胺、N-异丙基丙烯酰胺、N-[2-羟基-1,1-二[(羟基甲基)乙基]]丙烯酰胺[或还称为THAM的三(羟基甲基)丙烯酰胺基甲烷或N-三(羟基甲基)甲基丙烯酰胺]、N,N-二甲基丙烯酰胺、丙烯酸(2-羟基乙基)酯、丙烯酸(2,3-二羟基丙基)酯、甲基丙烯酸(2-羟基乙基)酯、甲基丙烯酸(2,3-二羟基丙基)酯、各个上述酯的分子量为400-1000的乙氧基化衍生物、或乙烯基吡咯烷酮。
根据上述步骤e)中定义的一个具体实施方案,水包油型的乳化体系是在低于50℃的温度引入的。
根据上述本发明方法的一个优选实施方案,步骤c)中的聚合反应是用氧化还原对在低于或等于10℃的温度引发的,例如氢氧化枯烯/偏亚硫酸氢钠对,然后以准绝热方式进行到大于或等于40℃的温度,更尤其大于或等于50℃的温度,或通过控制温度变化的方式进行。
当通过上述方法制备的组合物含有至少50重量%和不超过70重量%的聚电解质时,所述方法优选包括步骤d)。在这种情况下,适用于进行上述方法的挥发油是选自例如含有8-11个碳原子的轻质异烷属烃,例如以商品名IsoparTM G、IsoparTM L、IsoparTM H或IsoparTM J销售的那些。
当上述组合物含有小于50重量%的聚电解质时,所述方法一般不包括步骤d)。
根据此方法的一个变型,从步骤c)获得的反应介质在进行步骤步骤e)之前通过蒸馏进行浓缩。
根据上述方法的一个优选实施方案,步骤c)的聚合反应是用氧化还原对在低于或等于10℃的温度引发的,例如氢氧化枯烯/偏亚硫酸氢钠对,然后以准绝热方式进行到大于或等于40℃的温度,更尤其大于或等于50℃的温度,或通过控制温度变化的方式进行。
根据本发明的另一个具体方面,上述组合物含有不超过30重量%的聚电解质。
根据本发明方法的另一个具体实施方案,聚电解质含有60-20摩尔%的部分或完全以钠盐或钾盐或铵盐形式成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸单体和40-80摩尔%的丙烯酰胺单体。
根据本发明方法的另一个具体实施方案,在组合物中存在的聚电解质含有50-30摩尔%的部分或完全以钠盐或钾盐或铵盐形式成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸单体和50-70摩尔%的丙烯酰胺单体。
根据本发明方法的另一个具体实施方案,当在组合物中存在的上述聚电解质是丙烯酰胺、部分或完全以钠盐或钾盐或铵盐形式成盐的2-丙烯酰胺基-2-甲基丙磺酸、选自含有部分或完全以钠盐或钾盐或铵盐形式成盐的弱酸官能团的单体和/或非丙烯酰胺的中性单体中的一种或多种单体形成的共聚物(P)时,所有选自含弱酸官能团的单体和非丙烯酰胺的中性单体中的单体的摩尔比例是大于0%且小于或等于30%。根据此具体方案,丙烯酰胺与所有选自含弱酸官能团的单体和非丙烯酰胺的中性单体中的单体之间的摩尔比率是优选大于或等于1。
根据上述方法的另一个具体实施方案,在步骤(a)获得的含水混合物A1具有大于1且小于4的pH值,即小于3且更尤其小于2。
术语“支化聚合物”指的是含有侧链的非线性聚合物以便在将这种聚合物溶于水时获得在低剪切下产生很高粘度的大量缠结。
术语“交联聚合物”指的是呈水不溶性但可水溶胀的三维网络的形式从而导致产生化学凝胶的那些非线性聚合物。
根据本发明的组合物可包含含有交联单元和/或支化单元的聚电解质。
当将本发明组合物中存在的聚合物交联时,更特别地是用二烯属或多烯属化合物交联,该化合物摩尔比例相对于所用单体表示,为0.005%-1%,更特别是0.010%-0.20%,且还更特别是0.015%-0.15%。优选,交联剂和/或支化剂选自乙二醇二甲基丙烯酸酯、二甘醇二丙烯酸酯、二烯丙氧基乙酸钠、乙二醇二丙烯酸酯、二烯丙基脲、三烯丙基胺、三羟甲基丙烷三丙烯酸酯和亚甲基双(丙烯酰胺)。
在如上定义的组合物中,油包水(W/O)型乳化体系含有单一表面活性剂或含有表面活性剂的混合物,条件是所述混合物的HLB值足够低以致于产生油包水乳液。作为油包水型乳化剂,例如有:脱水山梨糖醇酯,例如脱水山梨糖醇油酸酯,例如由SEPPIC公司以MontaneTM 80销售的产品;脱水山梨糖醇异硬脂酸酯,例如由SEPPIC公司以MontaneTM 70销售的产品;或脱水山梨糖醇倍半油酸酯,例如由SEPPIC公以MontaneTM 83司销售的产品。还有某些多乙氧基化脱水山梨糖醇酯,例如五乙氧基化脱水山梨糖醇单油酸酯,例如由SEPPIC公司以MontanoxTM 81销售的产品;或五乙氧基化脱水山梨糖醇异硬脂酸酯,例如由SEPPIC公司以MontanoxTM 71销售的产品。还有一些脂肪链烷醇酰胺,例如由AKZO-NOBEL以商品名WITCAMIDETM 511销售的油基二乙醇酰胺。还有二乙氧基化油鲸蜡醇(diethoxylated oleocetyl alcohol),例如由SEPPIC公司以SimulsolTM OC 72销售的产品;四乙氧基化丙烯酸月桂酯,例如以BlemmerTM ALE 200销售的产品;或由聚(异丁烯基)琥珀酸或其酸酐与聚乙二醇缩合生产的分子量为1000-3000的聚酯,例如由Uniqema公司销售的HypermerTM 2296;或最后是分子量为2500-3500的嵌段共聚物,例如由Uniqema公司销售的HypermerTM B246或由SEPPIC公司销售的SimalineTM IE 200。
本发明组合物通常包含2-8重量%的油包水(W/O)型乳化体系。
在如上定义的组合物中,水包油(O/W)型乳化体系含有单一表面活性剂或含有表面活性剂的混合物,条件是所述混合物的HLB值足够高以致于产生水包油乳液。作为水包油型乳化剂,例如有:乙氧基化脱水山梨糖醇酯,例如用20mol氧化乙烯多乙氧基化的脱水山梨糖醇油酸酯,由SEPPIC公司以MontanoxTM 80销售;用20mol氧化乙烯多乙氧基化的脱水山梨糖醇月桂酸酯,由SEPPIC公司以MontanoxTM 20销售;用40mol氧化乙烯多乙氧基化的蓖麻油,以SimulsolTM OL50销售;十乙氧基化油癸醇(decaethoxylated oleodecyl alcohol),由SEPPIC公司以SimulsolTM OC710销售;七乙氧基化月桂醇,以SimulsolTM P7销售;或用20mol氧化乙烯多乙氧基化的脱水山梨糖醇单硬脂酸酯,由SEPPIC公司以MontanoxTM60销售。
作为本发明主题的组合物通常包含3-8重量%的水包油(O/W)型乳化体系。
在作为本发明主题的组合物中,油相包含室温下密度为0.7-0.9且沸点高于约250℃的含有饱和烃(例如链烷烃、异链烷烃或环烷烃)的商业矿物油,例如由Exxon Chemical销售的MarcolTM 52、IsoparTM M或IsoparTM L;Chemical Abstracts中编号RN=93685-80-4的异十六烷,其为含有至少97%的C16异链烷烃的C12、C16和C20异链烷烃的混合物,其中主要成分是2,2,4,4,6,8,8-七甲基壬烷(RN=4390-04-9);它在法国由Bayer公司销售,或异十二烷,在法国也由Bayer公司销售;或合成油例如氢化聚癸烯或氢化聚异丁烯,在法国由Ets B.Rossow et Cie公司以Parleam-PolysynlaneTM销售。它列于:Michel and Irene Ash;Thesaurus of Chemical Products,Chemical Publishing Co.Inc.1986第I卷,第211页(ISBN 0 7131 3603 0);或植物油,例如在法国由Sophim公司以PhytosqualaneTM销售且在Chemical Abstracts中编号RN=111-01-3的植物来源的角鲨烷;它是含有多于80重量%的2,6,10,15,19,23-六甲基二十四烷的烃混合物,或多种上述油的混合物。
油相还可包含脂肪酸酯。在本发明的范围内,术语“脂肪酸酯”是指式(I)的化合物:
R1-(C=O)-O-[[CH2-CH[O-[C(=O)]m-R2]-CH2-O]n-[C(=O)]p]q-R3 (I)
其中:
R1表示含有7-30个碳原子的饱和或不饱和、线性或支化的烃基链,
R2独立于R1,表示氢原子或含有7-30个碳原子的饱和或不饱和、线性或支化的烃基链,
R3独立于R1或R2,表示氢原子或含有1-30个碳原子的饱和或不饱和、线性或支化的烃基链,
m、n、p和q彼此独立地是等于0或1,应理解当R3表示氢原子时,q不等于0。
在如上定义的式(I)中,R1、R2和R3彼此独立特别表示选自庚基、辛基、壬基、癸基、十一烷基、十二烷基、十三烷基、十四烷基、十五烷基、十六烷基、十七烷基、十八烷基、十九烷基、二十烷基、二十一烷基、二十二烷基、十七碳烯基、二十碳烯基、二十一碳烯基、二十二碳烯基、十七碳二烯基和癸烯基的基团;基团R1-C(=O)-更特别地表示如下基团中的一个:辛酰基(辛酰基)、癸酰基、十一烷酰基、十二烷酰基(月桂酰基)、十四烷酰基(肉豆蔻酰基)、十六烷酰基(棕榈酰基)、十八烷酰基(硬脂酰基)、二十烷酰基(arachidoyl)、二十二烷酰基(山萮酰基)、8-十八碳烯酰基(油基)、二十碳烯酰基(gadoloyl)、13-二十二碳烯酰基(芥酰基)、9,12-十八碳二烯酰基(亚油酰基)、9,12,15-十八碳三烯酰基(亚麻酰基)。
油相可以更特别地包含式(Ia)的化合物或式(Ia)化合物的混合物:
R1-(C=O)-O-CH2-CH[O-[C(=O)]m-R2]-CH2-O-[C(=O)]p-R3 (Ia)
所述式(Ia)相当于其中q和n等于1的如上定义的式(I)。在这种情况下,优选:
或者是式(Ia1)的化合物:
R1-(C=O)-O-CH2-CH(OH)-CH2-OH (Ia1)
所述式(Ia1)相当于其中m和p等于0且R2和R3表示氢原子的如上定义的式(Ia),
或者是式(Ia2)的化合物:
R1-(C=O)-O-CH2-CH(OH)-CH2-O-C(=O)-R3 (Ia2)
所述式(Ia2)相当于其中p等于1、m等于0且R2表示氢原子的如上定义的式(Ia),
或者是式(Ia3)的化合物:
R1-(C=O)-O-CH2-CH[O-C(=O)-R2]-CH2-O-C(=O)-R3 (Ia3)
所述式(Ia3)相当于其中m和p等于1的如上定义的式(Ia),
或者是式(Ia1)、(Ia2)和/或(Ia3)的化合物的混合物。
作为式(Ia1)、(Ia2)或(Ia3)的化合物的实例,例如有:甘油三脂肪酸酯或脂肪酸混合物例如含有6-10个碳原子的甘油三脂肪酸酯的混合物(以SoftenolTM 3819销售)、含有8-10个碳原子的甘油三脂肪酸酯的混合物(以SoftenolTM 3108销售)、含有8-18个碳原子的甘油三脂肪酸酯的混合物(以SoftenolTM 3178销售)、含有12-18个碳原子的甘油三脂肪酸酯的混合物(以SoftenolTM 3100销售)、含有7个碳原子的甘油三脂肪酸酯的混合物(以SoftenolTM 3107销售)、含有14个碳原子的甘油三脂肪酸酯的混合物(以SoftenolTM 3114销售)、或含有18个碳原子的甘油三脂肪酸酯的混合物(以SoftenolTM 3118销售)、甘油二月桂酸酯、甘油二油酸酯、甘油异硬脂酸酯、甘油二硬脂酸酯、甘油单月桂酸酯、甘油单油酸酯、甘油单异硬脂酸酯或甘油单硬脂酸酯、或这些化合物的混合物。
油相可以更特别地包含式(Ib)的化合物或式(Ib)化合物的混合物:
R1-(C=O)-O-R3 (Ib)
所述式(Ib)相当于其中q等于0的如上定义的式(I)。
式(Ib)的化合物的实例例如有棕榈酸辛酯。
如上定义的反相胶乳通常含有4重量%-10重量%的乳化剂。其油相一般占组合物总重量的15%-40%,优选20%-25%。水相一般占组合物总重量的2%-40%。
根据本发明另一个特定的方面,其主题是通过如上定义的方法获得的组合物,其中所述共聚物选自:
-丙烯酰胺和以钠盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联共聚物;
-丙烯酰胺和以铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联共聚物;
-丙烯酰胺和以钾盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联共聚物;
-丙烯酰胺、以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸和以钠盐、钾盐或铵盐形式部分成盐的丙烯酸的交联三元共聚物;
-丙烯酰胺、N,N-二甲基丙烯酰胺、以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸和以钠盐、钾盐或铵盐形式部分成盐的丙烯酸的交联四元共聚物;
-丙烯酰胺、N,N-二甲基丙烯酰胺和以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联三元共聚物;
-丙烯酰胺、N-异丙基丙烯酰胺和以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联三元共聚物;
-丙烯酰胺、N-[2-羟基-1,1-二(羟基甲基)乙基]丙烯酰胺和以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联三元共聚物;
-丙烯酰胺、丙烯酸(2-羟基乙基)酯、以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸和以钠盐、钾盐或铵盐形式部分成盐的丙烯酸的交联四元共聚物;
-丙烯酰胺、丙烯酸(2-羟基乙基)酯和以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联三元共聚物。
本发明的主题还有化妆品组合物、皮肤药物组合物或药物组合物,其特征在于其包含至少一种通过如上定义的方法获得的反相胶乳作为增稠和/或乳化化合物。如上定义的化妆品组合物、皮肤化妆品组合物、皮肤药物组合物或药物组合物通常包含0.1重量%-10重量%、更特别是0.5重量%-5重量%的所述反相胶乳。它尤其呈油包水乳液、水包油乳液、水/油/水(water-in-oil-in-water)乳液、油/水/油(oil-in-water-in-oil)乳液、乳、洗液、凝胶、霜-凝胶、霜、皂、泡沫浴剂、香脂、香波或调理剂的形式。根据本发明的一个优选方面,如上定义的化妆品组合物、皮肤化妆品组合物、皮肤药物组合物或药物组合物是局部组合物。
本发明的主题还有通过如上定义的方法获得的反相胶乳用于制备化妆品、皮肤药物或药物局部组合物的用途。用于施涂到人类或动物的皮肤或粘膜上的本发明局部组合物可由包含至少一个水相和至少一个油相的局部乳液构成。局部乳液可以是水包油型的。更特别地,该局部乳液可由流体乳液、例如乳或流体凝胶构成。局部乳液的油相可由一种或多种油的混合物构成。根据本发明的局部组合物可用于化妆品用途或用于制备治疗皮肤和粘膜疾病的药物。在后一种情况下,则局部组合物包含活性要素,所述活性要素可由例如抗炎药、肌肉松弛药、抗真菌剂或抗细菌剂构成。
本发明的组合物还可含有化妆品和皮肤药物领域中通常使用且本领域技术人员已知的成分,例如脂肪(油、黄油、蜡、脂肪酸和树胶)、乳化剂和助乳化剂、胶凝剂和/或稳定剂和/或成膜剂、填料、颜料、防晒剂、润湿剂、溶剂和助溶剂、增塑剂、螯合剂、抗氧化剂、香料、防腐剂或活性要素。作为可与本发明组合物组合的油的实例,可提及链烷烃、异链烷烃、石蜡油、植物油、动物油、合成油、硅油和氟代油(fluoro oil);且更特别是:
-植物来源的油,例如甜杏仁油、椰子油、蓖麻油、霍霍巴油、橄榄油、菜籽油、花生油、向日葵油、小麦胚芽油、玉米胚芽油、豆油、棉籽油、苜蓿油、罂粟籽油、南瓜油、月见草油、小米油、大麦油、黑麦油、红花油、烛果油、西番莲花油、榛子油、棕榈油、牛油树脂、杏仁油、胡桐叶油、蒜芥(sysymbrium)油、鳄梨油、金盏花油和花卉或荚果油;乙氧基化植物油;动物来源的油,例如角鲨烯和角鲨烷;矿物油,例如液体石蜡、液体凡士林和异链烷烃;合成油,特别是脂肪酸酯,例如肉豆蔻酸丁酯、肉豆蔻酸丙酯、肉豆蔻酸鲸蜡酯、棕榈酸异丙酯、硬脂酸丁酯、硬脂酸十六烷酯、硬脂酸异丙酯、硬脂酸辛酯、硬脂酸异鲸蜡酯、油酸十二烷酯、月桂酸己酯、丙二醇二辛酸酯,衍生自羊毛酸的酯,例如羊毛酸异丙酯或羊毛酸异鲸蜡酯,甘油单脂肪酸酯、甘油二脂肪酸酯和甘油三脂肪酸酯,例如甘油三庚酸酯,烷基苯甲酸酯,聚α-烯烃,聚烯烃,例如聚异丁烯,合成异烷烃,例如异十六烷、异十二烷,全氟油和硅油。在硅油中,更特别地是可提及二甲基聚硅氧烷、甲基苯基聚硅氧烷、胺改性的硅酮、脂肪酸改性的硅酮、醇改性的硅酮、醇和脂肪酸改性的硅酮、聚醚基团改性的硅酮、环氧改性的硅酮、氟基团改性的硅酮、环状硅酮和烷基改性的硅酮。
作为可与本发明组合物组合使用的另一脂肪物质,可以提及脂肪醇或脂肪酸。
本发明制剂的脂相还可含有蜡例如蜂蜡;巴西棕榈蜡;小烛 树蜡;小冠巴西棕蜡;野漆树蜡;软木纤维蜡或甘蔗蜡;石蜡;褐煤蜡;微晶蜡;羊毛脂蜡;地蜡;聚乙烯蜡;氢化油;硅酮蜡;植物蜡;室温下为固体的脂肪醇和脂肪酸;室温下为固体的甘油酯。
根据本发明的反相胶乳可任选地与其它增稠和/或乳化聚合物组合。可以提及的实例包括丙烯酸或丙烯酸衍生物的均聚物或共聚物、丙烯酰胺的均聚物或共聚物、丙烯酰胺衍生物的均聚物或共聚物、丙烯酰胺基甲基丙磺酸的均聚物或共聚物、乙烯基单体的均聚物或共聚物、丙烯酸三甲基氨基乙基酯氯化物,以CarbopolTM UltrezTM 10、PemulenTM TR1、PemulenTM TR2、SimulgelTM A、SimulgelTM NS、SimulgelTM EPG、SimulgelTM EG、LuvigelTM EM、SalcareTM SC91、SalcareTM SC92、SalcareTM SC95、SalcareTM SC96、FlocareTM ET100、HispagelTM、SepigelTM 305、SepigelTM 501、SepigelTM 502、Sepiplus、FlocareTM ET58和StabilezeTM 06销售;植物或生物合成来源的水解胶体,例如黄原胶、刺梧桐树胶、角叉菜胶(carrageenate)或藻酸盐;硅酸盐;纤维素及其衍生物;淀粉及其亲水衍生物;聚氨酯。
根据本发明的组合物还是由申请人以SepigelTM 305、SepigelTM 501、SimulgelTM EG、SimulgelTM NS或SimulgelTM 600销售的那些产品的有利替代物,因为它还表现出与用于制备配制物(例如乳、洗液、霜、霜-凝胶、皂、泡沫浴剂、香脂、香波或护发素)的其它赋形剂之间良好的相容性。它尤其是与国际公开文本WO 92/06778、WO 95/04592、WO 95/13863、WO 96/37285、WO 98/22207和WO 98/47610中或在FR 2 734 496中所描述和要求的浓缩物相容、与WO 93/08204中所描述的表面活性剂相容。
在根据本发明的反相胶乳的存在下可以使用的乳化剂中,可以提及的实例包括脂肪酸;乙氧基化脂肪酸;山梨糖醇的脂肪酸酯;乙氧基化脂肪酸酯;聚山梨酸酯;聚甘油酯;乙氧基化脂肪醇;蔗糖酯;烷基聚苷;硫酸化或磷酸化脂肪醇或烷基聚苷与脂肪醇的混合物,其描述于法国专利申请2 668 080、2 734 496、2 756 195、2 762 317、2 784 680、2 784 904、2 791 565、2 790 977、2 807 435和2 804 432,SensanovTM WR和FluidanovTM 20X中。
如上定义的化妆品组合物、皮肤化妆品组合物、皮肤药物组合物或药物组合物还可包含结构剂(texture agent)和/或填料,例如丙烯酸和甲基丙烯酸共聚物、淀粉、二氧化硅、硅酸钙、硅酸镁、硅酸铝或硅酸钡、磷酸钙、天然纤维例如棉纤维、纤维素纤维或壳聚糖纤维,或合成纤维例如聚酰胺纤维、人造丝纤维、粘胶纤维、乙酸纤维素纤维、聚对苯二甲酰对苯二胺纤维聚乙烯或聚丙烯纤维、玻璃纤维、碳纤维、特氟隆纤维、聚酯纤维、聚氯乙烯纤维、聚乙烯醇纤维、聚丙烯腈纤维、聚氨酯纤维或聚邻苯二甲酸乙二酯纤维、滑石、云母、绢云母、二氧化硅、氮化硼、月桂酰基赖氨酸、硅树脂粉末、碳酸钙、碳酸镁、氧化钛、氧化锌或氧化铈、钛云母、铁氧化物和其它无机或有机颜料、或这些粉末的混合物。
作为可与本发明反相胶乳组合使用的活性要素的实例,可以提及具有使色泽变淡或去色素作用、润湿作用、拉紧作用、镇静或放松作用、净化作用、皮脂调理或防脱发作用、抗老化作用、或稳固(紧致)、重构(resturcturing)作用、自由基清除作用、抗氧化作用或自晒黑(self-tanning)作用的化合物。因此本发明的组合物可与如下物质组合:活性剂例如熊果苷、曲酸、氢醌、鞣花酸、维生素C及其衍生物、Stay C、磷酸抗坏血酸酯镁及其衍生物、抗坏血酸葡糖苷、植酸、果酸、乳酸、鲁忻喏(Rucinol)或间苯二酚、壬酸、羟乙酸、葡糖酸、二羟丙酮(DHA)、赤藓酮糖、硫辛酸、VegewhiteTM、GatulineTM、SynerlightTM、BiowhiteTM、PhytolightTM、DermalightTM、ClariskinTM、MelaslowTM、DermawhiteTM、EthiolineTM、MelarestTM、GigawhiteTM、AlbatineTM、LumiskinTM、多酚提取物、葡萄提取物、松树提取物、葡萄酒提取物、橄榄提取物、茶提取物、可可提取物、亚马逊河森林植物提取物、荚果提取物、花卉提取物、水果提取物、薄荷提取物、pond提取物、N-酰基蛋白质、N-酰基肽例如MatrixylTM、N-酰氨基酸、N-酰基蛋白质的部分水解产物、氨基酸、肽、完全蛋白质水解产物、部分蛋白质水解产物、多元醇(例如甘油、丁二醇等等)、乳衍生物、AquaxylTM、脲、吡咯烷酮羧酸或所述酸的衍生物、甘草次酸或其衍生物、α-没药醇、糖或糖衍生物、多糖或其衍生物、羟基酸例如乳酸或水杨酸、维生素、维生素衍生物例如维生素A、维生素A衍生物、维生素E及其衍生物、矿物、微量元素、岩石或石料的提取物、酶或其衍生物、辅酶或其衍生物例如辅酶Q10、激素或“类激素”物质例如Phyto ageTM、大豆提取物例如RaffermineTM、小麦提取物例如TensineTM或GliadineTM、植物提取物、富含单宁的植物提取物、富含异黄酮的提取物或富含萜的提取物、淡水或海产藻类提取物、通常的海洋提取物,包括珊瑚提取物,提炼的蜡(essential wax)、细菌提取物、矿物例如GivobioTM范围内的产品且尤其是钙、镁、铜、钴、锌、锰等等的衍生物,通常的类脂、类脂例如神经酰胺或磷脂及其衍生物,具有减肥作用的活性剂例如咖啡因或其衍生物,改善皮肤毛细管循环的活性剂例如静脉紧张剂,排泄活性剂,降低充血的活性剂例如银杏、常春藤、欧洲七叶树(common horsechestnut)、竹子、假叶树(ruscus)、积雪草(centella asiatica)、墨角藻、迷迭香或鼠尾草,对油性皮肤具有抗微生物活性或净化作用的活性剂例如铜或锌的衍生物或羟甲辛吡酮(octopirox)或Sensiva SC50,具有促进或刺激特性的活性剂例如SepitonicTM M3或PhysiogenylTM,泛醇及其衍生物例如SepicapTM MP、抗老化活性剂、SepivinolTM、SepivitalTM、ManolivaTM和Phyto ageTM。本发明的组合物更通常还可与对抗光老化用抗老化活性剂、保护真皮表皮连接完整性的目标活性剂、增加细胞外基质的成分(例如胶原、弹性蛋白、糖胺聚糖等等)的合成的活性剂、对化学(细胞因子)或物理(整联蛋白)细胞间通讯起有利作用的活性剂、具有重构作用的活性剂、具有愈合作用的活性剂、具有紧致作用的活性剂、具有“类肉毒素”作用的活性剂、对表情纹起作用的活性剂、对钙通道起作用的活性剂、改善皮肤隔膜(barrier)完整性的活性剂、对特定皮肤酶起作用的活性剂、对特定细胞受体起作用的活性剂、改善细胞间通讯的活性剂、具有自由基清除或抗氧化作用的活性剂、具有“拉紧”作用的活性剂和具有去头屑、去粉刺、镇静或抗神经介质作用的活性剂组合。根据本发明含有聚合物的组合物还可与对皮肤提供加热作用的活性剂例如皮肤毛细管循环促进剂(例如烟酸盐/酯)或相反地在施涂时产生清新感觉的成分(例如薄荷醇)组合。
作为可与本发明组合物合并的防晒剂,可以提及在修订的CosmeticDirective 76/768/EEC附录VII中所列的任意防晒剂。根据该优选方面,防晒剂更特别地选自亲脂性防晒剂,例如氰双苯丙烯酸辛酯(octocrylene)、氰双苯丙烯酸乙酯(etocrylene)、胡莫柳酯(homosalate),例如EusolexTM HMS、对甲氧基肉桂酸辛酯,例如ParsolTM MCX、奥西诺酯(octinoxate)、辛水杨酯(octisalate)、阿伏苯宗(avobenzone)、氧苯酮(oxybenzone)、二苯甲酮-1、二苯甲酮-2、二苯甲酮-3(例如Uvinul M-40)、二苯甲酮-8、二苯甲酮-12、乙基二羟基丙基PABA、甘油基PABA、乙基己基二甲基PABA、邻氨基苯甲酸薄荷醇酯、甲基亚苄基樟脑或异丙基二苯甲酰基甲烷。如上定义的防晒剂还可包含一种或多种疏脂防晒剂,例如二氧化钛、氧化锌、苯基苯并咪唑磺酸、二苯甲酮-4、TEA水杨酸盐、PABA和DEA甲氧基肉桂酸盐。如上定义的防晒剂还可包含一种或多种吸油剂,例如二氧化硅,不管是不是球状二氧化硅(例如SpheronTM L-1500)、多孔二氧化硅或热解法二氧化硅,交联或非交联聚甲基丙烯酸甲酯,例如MicropearlTM产品,糊精,环糊精,分子筛例如沸石,NylonTM 6或12,硅酸铝钠钙,滑石或云母。如上定义的防晒剂还包含一种或多种新戊酸与含有10-22个碳原子的异烷基醇的酯。在这种情况下,它优选包含新戊酸异癸酯、新戊酸异硬脂酯或新戊酸异花生酯。
根据本发明的一个特定方面,化妆品组合物、皮肤药物组合物或药物组合物包含有效量的二羟基丙酮,更特别地,组合物包含1重量%-8重量%的二羟基丙酮。根据本发明的一个更特别的方面,化妆品组合物、皮肤药物组合物或药物组合物包含二羟基丙酮和至少一种羟基酸例如乳酸、水杨酸、葡糖酸或曲酸,或者包含二羟基丙酮和至少一种防晒剂,或者包含二羟基丙酮和至少一种润湿剂,或者包含二羟基丙酮和至少一种减肥剂例如咖啡因。
以下实施例用来说明本发明,但并不是对其进行限制。
实施例1:根据本发明方法制备聚合物组合物
步骤1:制备水相
-在17℃的温度下将254g的以商品名“Acrylamide 50 HSTTM”由SNF生产的含有50%丙烯酰胺的商购溶液加入配备有机械搅拌器的容器中。
-然后加入247.32g的以商品名“ATBS 55%”由CIM Chemicals生产的含有55重量%2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸钠盐的水溶液,并测得pH为6.0。
然后加入123g的以商品名“ATBS G”由Toagosei生产的粉末形式的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸,作为在12.3g级分或9.54g级分的50%氢氧化钠溶液加入,在这些级分添加结束时这些50%氢氧化钠的总量是95.4g。在每次添加ATBS G级分和氢氧化钠级分之间控制pH,并记录在1.8-2.2范围内的检测值。在这种添加结束时,测得pH是2.2,然后另外加入氢氧化钠溶液以使此水相的pH值达到6.0。然后向预先制备的含水介质加入0.45g二亚乙基三胺五乙酸钠和0.107g的亚甲基二(丙烯酰胺),再次将pH控制为6.0的值。最终通过添加水将水相重量调节到682g。
步骤2:制备有机相
有机相是通过在配备有机械搅拌器的单独容器中将以下组分一起混合制备的:
-220g IsoparTM M(C13-C14异链烷烃),
-25.0g WitcamideTM 511(部分酯化的N,N-二链烷醇酰胺),
将这些组分在20℃用机械搅拌器以80转/分钟的低速混合15分钟。
步骤3:制备单体乳液
将水相逐步加入到有机相中并使用例如SilversonTM或IKATM搅拌器强烈搅拌混合物。
步骤4:制备聚合物乳液
然后将获得的乳液转入聚合反应器中,用氮气吹扫,然后冷却至约5-6℃。然后添加10g含有0.5g过硫酸钠的溶液,随后在溶液均化之后,以0.5ml/min的速度添加偏亚硫酸氢钠的水溶液(在水中2.5重量%)约60分钟,同时在聚合结束时使温度升高。然后使反应介质在该温度下保持约90分钟。然后添加偏亚硫酸氢钠以使丙烯酰胺在最终组合物中的浓度小于2ppm。然后冷却反应介质并且当所得化合物的温度达到25℃时,添加50g LaurethTM 7以获得预期的反相胶乳。
聚合物组合物的性能评价
在去离子水中2重量%的反相胶乳的粘度(Brookfield RVT):η=82800mPa.s;pH=6.1
在去离子水+0.1%NaCl中2重量%的反相胶乳的粘度(BrookfieldRVT):η=30200mPa.s;
用实施例1的聚合物组合物制备含水凝胶
将98g去离子水加入到250ml烧杯中并使用装配有锚组件的机械搅拌器在室温下以50rpm搅拌。将2g如前所述制备的反相胶乳逐渐添加到搅拌的去离子水中。含水介质稠化并形成凝胶。在室温下以80rpm搅拌该凝胶以便得到这种凝胶的均匀外观。将含有如前所述制备的含水凝胶的烧杯放入温度为75℃的调节烘箱中。对于丙烯酰胺浓度的每次测量,将5g预先制备的储存在烘箱中的凝胶与1g粉末形式的氯化钠加入到室温下的10ml量瓶中。然后将氯化钠的饱和溶液添加到量瓶中以将溶液的体积调整到10ml。手动搅拌含有稀释到氯化钠溶液中的凝胶的量瓶。然后将该搅拌的在氯化钠中的凝胶溶液过滤并通过装配有紫外检测器的高效液相色谱仪量化。在75℃下24小时后以及在75℃下48小时后,观察到恢复到起始反相胶乳的丙烯酰胺浓度保持在2ppm下并且不随时间而增加。
对比例1:根据现有技术的方法制备聚合物组合物
步骤1:制备水相
在17℃的温度下将254g的以商品名“Acrylamide 50 HST”由SNF生产的含有50%丙烯酰胺的商购溶液加入配备有机械搅拌器的容器中。然后将95.4g的50%氢氧化钠加入含有丙烯酰胺溶液的容器中并于20℃搅拌。测得pH为13.8。然后逐步加入246g的以商品名“ATBS G”由Toagosei生产的粉末形式的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸以保持容器内的温度低于25℃。在添加结束时,此水相的pH调节到6.0。然后向预先制备的含水介质加入0.45g二亚乙基三胺五乙酸钠和0.107g的亚甲基二(丙烯酰胺),再次将pH控制为6.0的值。最终通过添加水将水相重量调节到682g。
步骤2:制备有机相
有机相是通过在配备有机械搅拌器的单独容器中将以下组分一起混合制备的:
-220g IsoparTM M(C13-C14异链烷烃),
-25g WitcamideTM 511(部分酯化的N,N-二链烷醇酰胺),
将这些组分在20℃用机械搅拌器以80转/分钟的低速混合15分钟。
步骤3:制备单体乳液
将水相逐步加入到有机相中并使用例如SilversonTM或IKATM搅拌器强烈搅拌混合物。
步骤4:制备聚合物乳液
然后将获得的乳液转入聚合反应器中,用氮气吹扫,然后冷却至约5-6℃。然后添加10g的含有0.5g过硫酸钠的溶液,随后在溶液均化之后,以0.5ml/min的速度添加偏亚硫酸氢钠的水溶液(在水中2.5重量%)约60分钟,同时在聚合结束时使温度升高。然后使反应介质在该温度下保持约90分钟。然后添加偏亚硫酸氢钠以使丙烯酰胺在最终组合物中的浓度小于2ppm。然后冷却反应介质并且当所得化合物的温度达到25℃时,添加50g LaurethTM 7以获得预期的反相胶乳。
聚合物组合物的性能评价
在去离子水中2重量%的反相胶乳的粘度(Brookfield RVT):η=99000mPa.s;pH=6.3
在去离子水+0.1%NaCl中2重量%的反相胶乳的粘度(BrookfieldRVT):η=30000mPa.s;
用对比例1的聚合物组合物制备含水凝胶
将98g去离子水加入到250ml烧杯中并使用装配有锚组件的机械搅拌器在室温下以50rpm搅拌。将2g如前所述制备的反相胶乳逐渐添加到搅拌的去离子水中。含水介质稠化并形成凝胶。在室温下以80rpm搅拌该凝胶以便得到这种凝胶的均匀外观。将含有如前所述制备的含水凝胶的烧杯放入温度为75℃的调节烘箱中。对于丙烯酰胺浓度的每次测量,将5g预先制备的储存在烘箱中的凝胶与1g粉末形式的氯化钠加入到室温下的10ml量瓶中。然后将氯化钠的饱和溶液添加到量瓶中以将溶液的体积调整到10ml。手动搅拌含有稀释到氯化钠溶液中的凝胶的量瓶。然后将该搅拌的在氯化钠中的凝胶溶液过滤并通过装配有紫外检测器的高效液相色仪量化。在75℃下24小时后,观察到恢复到起始反相胶乳的丙烯酰胺浓度增加直到15ppm,并且在75℃下48小时后达到31ppm。
对比例2:根据现有技术的方法制备聚合物组合物
步骤1:制备水相
在17℃的温度下将254g的以商品名“Acrylamide 50%”由KEMIRA生产的含有50%丙烯酰胺的商购溶液加入配备有机械搅拌器的容器中。然后将95.4g的50%氢氧化钠加入含有丙烯酰胺溶液的容器中并于20℃搅拌。测得pH为13.8。然后逐步加入246g的以商品名“ATBSG”由Toagosei生产的粉末形式的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸以保持容器内的温度低于25℃。在添加结束时,此水相的pH调节到6.0。然后向预先制备的含水介质加入0.45g二亚乙基三胺五乙酸钠和0.107g的亚甲基二(丙烯酰胺),再次将pH控制为6.0的值。最终通过添加水将水相重量调节到682g。
步骤2:制备有机相
有机相是通过在配备有机械搅拌器的单独容器中将以下组分一起混合制备的:
-220g IsoparTM M(C13-C14异链烷烃),
-25g WitcamideTM 511(部分酯化的N,N-二链烷醇酰胺),
将这些组分在20℃用机械搅拌器以80转/分钟的低速混合15分钟。
步骤3:制备单体乳液
将水相逐步加入到有机相中并使用例如SilversonTM或IKATM搅拌器强烈搅拌混合物。
步骤4:制备聚合物乳液
然后将获得的乳液转入聚合反应器中,用氮气吹扫,然后冷却至约5-6℃。然后添加10g的含有0.5g过硫酸钠的溶液,随后在溶液均化之后,以0.5ml/min的速度添加偏亚硫酸氢钠的水溶液(在水中2.5重量%)约60分钟,同时在聚合结束时使温度升高。然后使反应介质在该温度下保持约90分钟。然后添加偏亚硫酸氢钠以使丙烯酰胺在最终组合物中的浓度小于2ppm。然后冷却反应介质并且当所得化合物的温度达到25℃时,添加50g LaurethTM 7以获得预期的反相胶乳。
聚合物组合物的性能评价
在去离子水中2重量%的反相胶乳的粘度(Brookfield RVT):η=95000mPa.s;pH=6.3
在去离子水+0.1%NaCl中2重量%的反相胶乳的粘度(BrookfieldRVT):η=32000mPa.s;
用对比例2的聚合物组合物制备含水凝胶
将98g去离子水加入到250ml烧杯中并使用装配有锚组件的机械搅拌器在室温下以50rpm搅拌。将2g如前所述制备的反相胶乳逐渐添加到搅拌的去离子水中。含水介质稠化并形成凝胶。在室温下以80rpm搅拌该凝胶以便得到这种凝胶的均匀外观。将含有如前所述制备的含水凝胶的烧杯放入温度为75℃的调节烘箱中。对于丙烯酰胺浓度的每次测量,将5g预先制备的储存在烘箱中的凝胶与1g粉末形式的氯化钠加入到室温下的10ml量瓶中。然后将氯化钠的饱和溶液添加到量瓶中以将溶液的体积调整到10ml。手动搅拌含有稀释到氯化钠溶液中的凝胶的量瓶。然后将该搅拌的在氯化钠中的凝胶溶液过滤并通过装配有紫外检测器的高效液相色谱仪量化。在75℃下24小时后,观察到恢复到起始反相胶乳的丙烯酰胺浓度增加直到60ppm,并且在75℃下48小时后达到100ppm。
对比例3:根据现有技术的方法制备聚合物组合物
步骤1:制备水相
-在17℃的温度下将254g的以商品名“Acrylamide 50%”由KEMIRA生产的含有50%丙烯酰胺的商购溶液加入配备有机械搅拌器的容器中。
-然后加入247.32g的以商品名“ATBS 55%”由CIM Chemicals生产的含有55重量%2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸钠盐的水溶液,并测得pH为1.4。
然后加入123g的以商品名“ATBS G”由Toagosei生产的粉末形式的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸,作为在12.3g级分或9.54g级分的50%氢氧化钠溶液加入,在这些级分添加结束时这些50%氢氧化钠的总量是95.4g。在每次添加ATBS G级分和氢氧化钠级分之间控制pH,并记录在1.8-2.2pH范围内的检测值。在这种添加结束时,测得pH是2.2,然后另外加入氢氧化钠溶液以使此水相的pH值达到6.0。然后向预先制备的含水介质加入0.45g二亚乙基三胺五乙酸钠和0.107g的亚甲基二(丙烯酰胺),再次将pH控制为6.0的值。最终通过添加水将水相重量调节到682g。
步骤2:制备有机相
有机相是通过在配备有机械搅拌器的单独容器中将以下组分一起混合制备的:
-220g IsoparTM M(C13-C14异链烷烃),
-25g WitcamideTM 511(部分酯化的N,N-二链烷醇酰胺),
将这些组分在20℃用机械搅拌器以80转/分钟的低速混合15分钟。
步骤3:制备单体乳液
将水相逐步加入到有机相中并使用例如SilversonTM或IKATM搅拌器强烈搅拌混合物。
步骤4:制备聚合物乳液
然后将获得的乳液转入聚合反应器中,用氮气吹扫,然后冷却至约5-6℃。然后添加10g含有0.5g过硫酸钠的溶液,随后在溶液均化之后,以0.5ml/min的速度添加偏亚硫酸氢钠的水溶液(在水中2.5重量%)约60分钟,同时在聚合结束时使温度升高。然后使反应介质在该温度下保持约90分钟。然后添加偏亚硫酸氢钠以使丙烯酰胺在最终组合物中的浓度小于2ppm。然后冷却反应介质并且当所得化合物的温度达到25℃时,添加50g LaurethTM 7以获得预期的反相胶乳。
用对比例3的聚合物组合物制备含水凝胶
将98g去离子水加入到250ml烧杯中并使用装配有锚组件的机械搅拌器在室温下以50rpm搅拌。将2g如前所述制备的反相胶乳逐渐添加到搅拌的去离子水中。含水介质稠化并形成凝胶。在室温下以80rpm搅拌该凝胶以便得到这种凝胶的均匀外观。将含有如前所述制备的含水凝胶的烧杯放入温度为75℃的调节烘箱中。对于丙烯酰胺浓度的每次测量,将5g预先制备的储存在烘箱中的凝胶与1g粉末形式的氯化钠加入到室温下的10ml量瓶中。然后将氯化钠的饱和溶液添加到量瓶中以将溶液的体积调整到10ml。手动搅拌含有稀释到氯化钠溶液中的凝胶的量瓶。然后将该搅拌的在氯化钠中的凝胶溶液过滤并通过装配有紫外检测器的高效液相色谱仪量化。在75℃下24小时后,观察到恢复到起始反相胶乳的丙烯酰胺浓度增加直到30-35ppm,并且在75℃下48小时后达到50ppm。
在所述方法的步骤a)中对水相pH的控制是防止在不友好储存条件下丙烯酰胺从最终增稠配料释放出来的关键点。实施例1与对比例3之间的比较也显示当在最终配料中需要达到最大2ppm丙烯酰胺时,在起始丙烯酰胺中不存在3,3’,3”-次氮基三(丙酰胺)(CAS号[2664-61-1]是必要的。
用本发明组合物制备的配料的实施例
实施例2:护理霜
环状聚二甲基硅氧烷: 10%
实施例1的反相胶乳: 0.8%
MontanovTM 68: 2%
硬脂醇: 1%
硬脂醇: 0.5%
防腐剂: 0.65%
赖氨酸: 0.025%
EDTA(二钠盐): 0.05%
黄原胶: 0.2%
甘油: 3%
水: 适量,100%
实施例3:须后香脂
配方
A 实施例1的反相胶乳: 1.5%
水: 适量,100%
B MicropearlTM M 100: 5.0%
SepicideTM CI: 0.50%
香料: 0.20%
95°乙醇: 10.0%
步骤
将B添加到A中。
实施例4:润体乳液(satin body emulsion)
配方
A SimulsolTM 165: 5.0%
LanolTM 1688: 8.50%
牛油树脂: 2%
液体石蜡: 6.5%
LanolTM 14M: 3%
LanolTM S: 0.6%
B 水: 66.2%
C MicropearlTM M 100: 5%
D 实施例1的反相胶乳: 3%
E SepicideTM CI: 0.3%
SepicideTM HB: 0.5%
AquaxylTM: 3%
香料: 0.20%
维生素E乙酸酯: 0.20%
吡咯烷酮羧酸钠: 1%
步骤
将C添加到B中,在70℃下使B在A中乳化,然后在60℃下添加D,随后在30℃下添加E。
实施例5:水包油霜
配方
A SimulsolTM 165: 5.0%
LanolTM 1688: 20.0%
LanolTM P: 1.0%
B 水: 适量,100%
C 实施例1的反相胶乳: 2.50%
D SepicideTM CI: 0.20%
SepicideTM HB: 0.30%
步骤
在约75℃下将B加入到A中;在约60℃下加入C,然后在约45℃下加入D。
实施例6:不油腻防晒凝胶
配方
A 实施例1的反相胶乳: 3.00%
水: 30%
B SepicideTM CI: 0.20%
SepicideTM HB: 0.30%
香料: 0.10%
C 染料: 适量
水: 30%
D MicropearlTM M 100: 3.00%
水: 适量,100%
E 硅油: 2.0%
ParsolTM MCX: 5.00%
步骤
将B加入到A中,添加C,然后添加D,然后添加E。
实施例7:防晒乳
配方
A MontanovTM S: 3.0%
芝麻油: 5.0%
ParsolTM MCX: 5.0%
角叉菜胶λ: 0.10%
B 水: 适量,100%
C 实施例1的反相胶乳: 0.80%
D 香料: 适量
防腐剂: 适量
步骤
在75℃下将B在A中乳化,然后在约60℃下添加C,然后在约30℃下添加D,并且如果需要,调节pH。
实施例8:按摩凝胶
配方
A 实施例1的反相胶乳: 3.5%
水: 20.0%
B 染料: 2滴/100g
水: 适量
C 醇: 10%
薄荷醇: 0.10%
D 硅油: 5.0%
步骤
将B添加到A中,然后向混合物中添加C,然后添加D。
实施例9:保湿无光粉底
配方
A 水: 20.0%
丁二醇: 4.0%
PEG-400: 4.0%
PecosilTM PS100: 1.0%
NaOH: 适量,pH=9
二氧化钛: 7.0%
滑石: 2.0%
黄色氧化铁: 0.8%
红色氧化铁: 0.3%
黑色氧化铁: 0.05%
B LanolTM 99: 8%
辛酸/癸酸甘油三酯: 8%
MontanovTM 202: 5.00%
C 水: 适量,100%
MicropearlTM M305: 2.0%
EDTA四钠: 0.05%
D 环状聚二甲基硅氧烷: 4.0%
黄原胶: 0.2%
实施例1的反相胶乳: 0.8%
E SepicideTM HB: 0.5%
SepicideTM CI: 0.3%
香料: 0.2%
步骤
在80℃下制备混合物B+D和A+C,然后将其混合在一起并使整体乳化。
实施例10:闪光凝胶
配方
A 实施例1的反相胶乳: 4%
水: 30%
B Elastine HPM: 5.0%
C MicropearlTM M 100: 3%
水: 5%
D SepicideTM CI: 0.2%
SepicideTM HB: 0.3%
香料: 0.06%
吡咯烷酮羧酸钠50%: 1%
水: 适量,100%
步骤
制备A;添加B,然后添加C,然后添加D。
实施例11:体乳
配方
MontanovTM S: 3.5%
LanolTM 37T: 8.0%
SolagumTM L: 0.05%
水: 适量,100%
二苯甲酮-3: 2.0%
聚二甲基硅氧烷350cPs: 0.05%
实施例1的反相胶乳: 0.8%
防腐剂: 0.2%
香料: 0.4%
实施例12:含有甜杏仁油的卸妆乳液
配方
MontanovTM 68: 5%
甜杏仁油: 5%
水: 适量,100%
实施例1的反相胶乳: 0.3%
甘油: 5%
防腐剂: 0.2%
香料: 0.3%
实施例13:油性皮肤用保湿霜
配方
MontanovTM 68: 5%
辛酸鲸蜡基硬脂基酯: 8%
棕榈酸辛酯: 2%
水: 适量,100%
实施例1的反相胶乳: 0.6%
MicropearlTM M100: 3.0%
粘多糖: 5%
SepicideTM HB: 0.8%
香料: 0.3%
实施例14:无酒精须后润肤香脂
配方
A LipacideTM PVB: 1.0%
LanolTM 99: 2.0%
甜杏仁油: 0.5%
B 实施例1的反相胶乳: 3.5%
C 水: 适量,100%
D 香料: 0.4%
SepicideTM HB: 0.4%
SepicideTM CI: 0.2%
实施例15:敏感皮肤用的含有AHA的霜
配方
月桂基氨基酸的混合物: 0.1%-5%
天冬氨酸镁钾: 0.002%-0.5%
LanolTM 99: 2%
MontanovTM 68: 5.0%
水: 适量,100%
实施例1的反相胶乳: 1.50%
葡糖酸: 1.50%
三乙胺: 0.9%
SepicideTM HB: 0.3%
SepicideTM CI: 0.2%
香料: 0.4%
实施例16:晒后润肤护理品
配方
月桂基氨基酸的混合物: 0.1%-5%
天冬氨酸镁钾: 0.002%-0.5%
LanolTM 99: 10.0%
水: 适量,100%
实施例1的反相胶乳: 2.50%
SepicideTM HB: 0.3%
SepicideTM CI: 0.2%
香料: 0.4%
染料: 0.03%
实施例17:卸妆乳
配方
SepiperlTM N: 3%
PrimolTM 352: 8.0%
甜杏仁油: 2%
水: 适量,100%
实施例1的反相胶乳: 0.8%
防腐剂: 0.2%
实施例18:粉底液
配方
SimulsolTM 165: 5.0%
LanolTM 84D: 8.0%
LanolTM 99: 5.0%
水: 适量,100%
矿物填料和颜料: 10.0%
实施例1的反相胶乳: 1.2%
防腐剂: 0.2%
香料: 0.4%
实施例19:防晒乳
配方
SepiperlTM N: 3.5%
LanolTM 37T: 10.0%
ParsolTM MCX: 5.0%
EusolexTM 4360: 2.0%
水: 适量,100%
实施例1的反相胶乳: 1.8%
防腐剂: 0.2%
香料: 0.4%
实施例20:眼部凝胶
配方
实施例1的反相胶乳: 2.0%
香料: 0.06%
吡咯烷酮羧酸钠: 0.2%
Dow CorningTM 245Fluid: 2.0%
水: 适量,100%
实施例21:免洗(leave-in)护理组合物
配方
实施例1的反相胶乳: 1.5%
香料: 适量
防腐剂: 适量
Dow CorningTM X28360: 5.0%
Dow CorningTM Q21401: 15.0%
水: 适量,100%
实施例22:纤瘦凝胶
实施例1的反相胶乳: 5%
乙醇: 30%
薄荷醇: 0.1%
咖啡因: 2.5%
假叶树提取物: 2%
常春藤提取物: 2%
SepicideTM HB: 1%
水: 适量,100%
实施例23:超天然彩色霜-凝胶
配方
A 水: 10.0%
丁二醇: 4.0%
PEG-400: 4.0%
PecosilTM PS100: 1.5%
NaOH: 适量pH=7
二氧化钛: 2.0%
黄色氧化铁: 0.8%
红色氧化铁: 0.3%
黑色氧化铁: 0.05%
B LanolTM 99: 4.0%
辛酸/癸酸甘油三酯: 4.0%
SepifeelTM One: 1.0%
实施例1的反相胶乳: 3.0%
C 水: 适量,100%
MicropearlTM M305: 2.0%
EDTA四钠: 0.05%
环状聚二甲基硅氧烷: 4.0%
D SepicideTM HB: 0.5%
SepicideTM CI: 0.3%
香料: 0.2%
步骤
制备混合物B+C,然后添加A且然后添加D。
实施例24:油性皮肤用护肤品
配方
A MicropearlTM M310: 1.0%
实施例1的反相胶乳: 5.0%
异壬酸辛酯: 4.0%
B 水: 适量,100%
C SepicontrolTM A5: 4.0%
香料: 0.1%
SepicideTM HB: 0.3%
SepicideTM CI: 0.2%
D CapigelTM 98: 0.5%
水 10%
实施例25:含有AHA的霜
配方
A MontanovTM 68: 5.0%
LipacideTM PVB: 1.05%
LanolTM 99: 10.0%
B 水: 适量,100%
葡糖酸: 1.5%
TEA(三乙醇胺) 0.9%
C 实施例1的反相胶乳: 1.5%
D 香料: 0.4%
SepicideTM HB: 0.2%
SepicideTM CI: 0.4%
实施例26:用于面部和身体的不油腻自晒黑产品
配方
A LanolTM 2681: 3.0%
实施例1的反相胶乳: 2.5%
B 水: 适量,100%
二羟基丙酮: 3.0%
C 香料: 0.2%
SepicideTM HB: 0.8%
NaOH(氢氧化钠): 适量,pH=5
配方
LipacideTM PVB: 0.5%
实施例1的反相胶乳: 2.2%
B水: 适量,100%
C香料: 0.1%
SepicideTM HB: 0.3%
SepicideTM CI: 0.1%
ParsolTM MCX: 4.0%
实施例28:面部用防晒护理产品
配方
A 环状聚二甲基硅氧烷和聚二甲基硅氧烷: 4.0%
实施例1的反相胶乳: 3.5%
B 水: 适量,100%
C 香料: 0.1%
SepicideTM HB: 0.3%
SepicideTM CI: 0.21%
ParsolTM MCX: 5.0%
钛云母: 2.0%
乳酸: 适量,pH=6.5
实施例29:自晒黑乳液
配方
A LanolTM 99: 15%
MontanovTM 68: 5.0%
ParsolTM MCX: 3.0%
B 水: 适量,100%
二羟基丙酮: 5.0%
磷酸单钠: 0.2%
C 实施例1的反相胶乳: 0.5%
D 香料: 0.3%
SepicideTM HB: 0.8%
NaOH: 适量,pH=5
实施例30:护理霜
环状聚二甲基硅氧烷: 10%
实施例1的反相胶乳: 0.8%
MontanovTM 68: 4.5%
防腐剂: 0.65%
赖氨酸: 0.025%
EDTA(二钠盐): 0.05%
黄原胶: 0.2%
甘油 3%
水: 适量,100%
实施例31:护理霜
环状聚二甲基硅氧烷: 10%
实施例1的反相胶乳: 0.8%
MontanovTM 68: 4.5%
全氟聚甲基异丙基醚: 0.5%
防腐剂: 0.65%
赖氨酸: 0.025%
EDTA(二钠盐): 0.05%
PemulenTM TR1: 0.2%
甘油 3%
水: 适量,100%
实施例32:体乳
配方
A SimulsolTM 165: 5.0%
LanolTM 1688: 12.0%
LanolTM 14M: 2.0%
鲸蜡醇: 0.3%
SchercemolTM OP: 3%
B 水: 适量,100%
C 实施例1的反相胶乳: 0.35%
D SepicideTM CI: 0.2%
SepicideTM HB: 0.5%
香料: 0.20%
步骤
在约75℃下将B在A中乳化;在约60℃下添加C,然后在约30℃下添加D。
实施例33:按摩护理凝胶
配方
A 实施例1的反相胶乳: 3.00%
水: 30%
B SepicideTM CI: 0.20%
SepicideTM HB: 0.30%
香料: 0.05%
C 染料: 适量
水: 适量,100%
D MicropearlTM SQL: 5.0%
LanolTM 1688: 2%
步骤
制备A;添加B,然后添加C,然后添加D。
实施例34:体乳
配方
A SepiperlTM N: 3.0%
甘油三庚酸酯: 10.0%
B 水: 适量,100%
C 实施例1的反相胶乳: 1.0%
D 香料: 适量
防腐剂: 适量
步骤
在约75℃下使A熔融。在75℃下使B在A中乳化,然后在约60℃下添加C,然后添加D。
实施例35:无酒精须后润肤香脂
配方
月桂基氨基酸的混合物: 0.1%-5%
天冬氨酸镁钾: 0.002%-0.5%
LanolTM 99: 2%
甜杏仁油: 0.5%
水: 适量,100%
实施例1的反相胶乳: 3%
SepicideTM HB: 0.3%
SepicideTM CI: 0.2%
香料: 0.4%
实施例36:体乳
配方
SepiperlTM N: 3.5%
LanolTM 37T: 8.0%
SolagumTM L: 0.05%
水: 适量,100%
二苯酮-3: 2.0%
聚二甲基硅氧烷350cPs: 0.05%
实施例1的反相胶乳: 0.8%
防腐剂: 0.2%
香料: 0.4%
实施例37:无酒精须后润肤香脂
配方
A LipacideTM PVB: 1.0%
LanolTM 99: 2.0%
甜杏仁油: 0.5%
B 实施例1的反相胶乳: 3.5%
C 水: 适量,100%
D 香料: 0.4%
SepicideTM HB: 0.4%
SepicideTM CI: 0.2%
实施例38:须后清新凝胶
配方
A LipacideTM PVB: 0.5%
LanolTM 99: 5.0%
实施例1的反相胶乳: 2.5%
B 水: 适量,100%
C MicropearlTM LM 0.5%
香料: 0.2%
SepicideTM HB: 0.3%
SepicideTM CI: 0.2%
实施例39:含有AHA的霜
配方
A MontanovTM 68: 5.0%
LipacideTM PVB: 1.05%
LanolTM 99: 10.0%
B 水: 适量,100%
葡糖酸: 1.5%
TEA(三乙醇胺): 0.9%
C实施例1的反相胶乳: 1.5%
D香料: 0.4%
SepicideTM HB: 0.2%
SepicideTM CI: 0.4%
实施例40:光亮凝胶
实施例1的反相胶乳: 1.5%
挥发性硅酮: 25%
单丙二醇: 25%
软化水: 10%
甘油: 适量,100%
实施例41:纤瘦凝胶
实施例1的反相胶乳: 1.5%
异壬酸异壬酯: 2%
咖啡因: 5%
乙醇: 40%
MicropearlTM LM: 2%
软化水: 适量,100%
防腐剂、香料: 适量
实施例42:卸妆乳
SimulsolTM 165: 4%
MontanovTM 202: 1%
辛酸/癸酸甘油三酯: 15%
PecosilM DCT: 1%
软化水 适量
CapigelTM 98: 0.5%
实施例1的反相胶乳: 1%
ProteolTM APL: 2%
氢氧化钠: 适量,pH=7
实施例43:用于变形和变脆头发的重构“洗去型”霜膜
配方
KetrolTM T: 0.5%
PecosilTM SPP50: 0.75%
N-椰油基氨基酸: 0.70%
丁二醇: 3.0%
实施例1的反相胶乳: 3.0%
MontanovTM 82: 3.0%
霍霍巴油: 1.0%
LanolTM P: 6.0%
AmonylTM DM: 1.0%
LanolTM 99: 5.0%
SepicideTM HB: 0.3%
SepicideTM CI: 0.2%
香料: 0.2%
去离子水: 适量,100%
实施例44:防晒霜
SimulsolTM 165: 3%
MontanovTM 202: 2%
苯甲酸C12-C15酯: 8%
PecosilTM PS 100: 2%
聚二甲基硅氧烷: 2%
环状聚二甲基硅氧烷: 5%
对甲氧基肉桂酸辛酯: 6%
二苯甲酮-3 4%
氧化钛: 8%
黄原胶: 0.2%
丁二醇: 5%
软化水: 适量,100%
实施例1的反相胶乳: 1.5%
防腐剂、香料: 适量
实施例45:混合型皮肤用护理凝胶
实施例1的反相胶乳: 4%
植物角鲨烷: 5%
聚二甲基硅氧烷: 1.5%
SepicontrolTM A5: 4%
黄原胶: 0.3%
水: 适量,100%
防腐剂、香料: 适量,
实施例46:美发液
配方
丁二醇: 3.0%
实施例1的反相胶乳: 3%
SimulsolTM 1293: 3.0%
乳酸: 适量,pH=6
SepicideTM HB: 0.2%
SepicideTM CI: 0.3%
香料: 0.3%
水: 适量,100%
实施例47:防护和松弛香波
配方
AmonylTM 675SB: 5.0%
28%月桂基醚硫酸钠: 35.0%
实施例1的反相胶乳: 3.0%
SepicideTM HB: 0.5%
SepicideTM CI: 0.3%
氢氧化钠: 适量,pH=7.2
香料: 0.3%
染料(FDC Blue 1/Yellow 5): 适量
水: 适量,100%
实施例48:“留置型(leave-on)”保护产品;防变形护发用品
配方
KetrolTM T: 0.5%
椰油基氨基酸的混合物: 3.0%
丁二醇: 5.0%
DC 1501 5.0%
实施例1的组合物: 4.0%
SepicideTM HB: 0.5%
SepicideTM CI: 0.3%
香料: 0.3%
水: 适量,100%
实施例49:含有维生素的霜
SimulsolTM 165: 5%
MontanovTM 202: 1%
辛酸/癸酸甘油三酯: 20%
维生素A棕榈酸酯: 0.2%
维生素E乙酸酯: 1%
MicropearlTM M305: 1.5%
实施例1的反相胶乳: 2%
水: 适量,100%
防腐剂、香料: 适量
实施例50:防晒凝胶
配方
实施例1的反相胶乳: 3.00%
SepicideTM CI: 0.20%
SepicideTM HB: 0.30%
香料: 0.10%
染料: 适量
二氧化硅: 3.00%
水: 适量,100%
硅油: 2.0%
二苯甲酮-3 5.00%
实施例51:润唇膏
配方
实施例1的反相胶乳: 1.50%
SchercemolTM TISC: 15.00%
VistanolTM NPGC: 15.00%
Candurin Paprika: 0.50%
MontanoxTM 80: 1.00%
AntaronTM V216: 0.90%
杏香料(Apricot flavouring): 0.20%
SepicideTM HB: 0.50%
C MaltideXTM H 16322: 适量,100%
实施例52:阳光充足气候用粉饼
配方
实施例1的反相胶乳: 2.00%
LanolTM 99: 12.00%
SepiwhiteTM MSH: 1.00%
滑石: 33.00%
MicropearlTM M310: 3.00%
黄色氧化铁: 0.80%
红色氧化铁: 0.30%
黑色氧化铁: 0.05%
云母: 适量,100%
实施例53:特应性皮肤用乳液
配方
ArlacelTM P135: 2.00%
实施例1的反相胶乳: 1.00%
LanolTM 1688: 14.00%
PrimolTM 352: 8.00%
甘油: 5.00%
水: 适量,100%
硫酸镁: 0.70%
SepicideTM HB: 0.30%
SepicideTM CI: 0.20%
MicropearlTM M310 5.00%
实施例54:防晒护肤品(硅酮包水)
配方
实施例1的反相胶乳: 2.00%
DC5225C: 20.00%
DC345: 10.00%
SepicalmTM VG: 3.00%
二氧化钛MT100T: 5.00%
氧化锌Z-Cote HP1: 5.00%
SepicideTM HB: 0.30%
香料: 0.05%
SepicideTM CI: 0.20%
甘油: 5.00%
氯化钠: 2.00%
水: 适量,100%
实施例55:多相护理品
配方
实施例1的反相胶乳: 3.00%
苯甲酸C12-15烷基酯: 25.00%
AquaxylTM: 3.00%
SepitonicTM M3: 1.00%
SepicideTM HB: 0.50%
SepicideTM CI: 0.30%
水: 适量,100%
实施例56:自晒黑凝胶
实施例1的反相胶乳: 5%
乙醇: 30%
二羟基丙酮: 4%
赤藓酮糖: 1%
薄荷醇: 0.1%
咖啡因: 2.5%
常春藤提取物: 2%
SepicideTM HB: 1%
水: 适量,100%
实施例57:自晒黑防晒乳
配方
A SepiperlTM N: 3.0%
甘油三庚酸酯: 10.0%
LipacideTM PVB: 0.5%
实施例1的反相胶乳: 2.0%
B 水: 适量,100%
二羟基丙酮: 5.0%
C 香料: 0.1%
SepicideTM HB: 0.3%
SepicideTM CI: 0.1%
ParsolTM MCX: 4.0%
实施例58:含有AHA的自晒黑霜
配方
A MontanovTM 68: 5.0%
LipacideTM PVB: 1.05%
LanolTM 99: 10.0%
B 水: 适量,100%
葡糖酸: 1.5%
二羟基丙酮: 3.0%
TEA(三乙醇胺): 0.9%
C 实施例1的反相胶乳: 1.5%
D 香料: 0.4%
SepicideTM HB: 0.2%
SepicideTM CI: 0.4%
实施例59:敏感皮肤用的含有AHA的自晒黑霜
配方
月桂基氨基酸的混合物: 0.1%-5%
天冬氨酸镁钾: 0.002%-0.5%
LanolTM 99: 2%
MontanovTM 68: 5.0%
水: 适量,100%
实施例1的反相胶乳: 1.50%
乳酸: 1.50%
二羟基丙酮: 3.5%
三乙胺: 0.9%
SepicideTM HB: 0.3%
SepicideTM CI: 0.2%
香料: 0.4%
实施例60:丝光(Satin)自晒黑保湿乳
配方
A SimulsolTM 165: 5.0%
LanolTM 1688: 8.50%
牛油树脂: 2%
液体石蜡: 6.5%
LanolTM 14M: 3%
LanolTM S: 0.6%
B水: 66.2%
二羟基丙酮: 3%
C MicropearlTM M 100: 5%
D实施例1的反相胶乳: 3%
E SepicideTM CI: 0.3%
SepicideTM HB: 0.5%
AquaxylTM: 5%
香料: 0.20%
维生素E乙酸酯: 0.20%
吡咯烷酮羧酸钠: 1%
实施例中使用的市售产品的说明如下:
SimulsolTM 1293是乙氧基化指数等于40的氢化和乙氧基化的蓖麻油,由SEPPIC公司销售。
CapigelTM 98是基于丙烯酸酯共聚物的液体增稠剂,由SEPPIC公司销售。
KetrolTM T是由Kelco公司销售的黄原胶。
LanolTM 99是由SEPPIC公司销售的异壬酸异壬酯。
DC1501是由Dow Chemical公司销售的环五硅氧烷和聚二甲基硅氧烷的混合物。
MantanovTM 82是基于十六/十八醇和椰油基葡糖苷的乳化剂。
MontanovTM 68(十六/十八烷基葡糖苷)是WO 92/06778中所述的自乳化组合物,由SEPPIC公司销售。
MicropearlTM M100是具有很柔软触感和消光作用的超微粉末,由Matsumo公司销售。
SepicideTM CI,咪唑烷脲,是由SEPPIC公司销售的防腐剂。
PemulenTM TR1是由Goodrich销售的丙烯酸类聚合物。
SimulsolTM 165是由SEPPIC公司销售的自乳化硬脂酸甘油酯。
LanolTM 1688是由SEPPIC公司销售的具有不油腻效果的柔润酯。
SepicideTM HB是由SEPPIC公司销售的防腐剂,其为苯氧基乙醇、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯的混合物。
AquaxylTM是由SEPPIC公司销售的润湿剂。
SchercemolTM OP是具有不油腻效果的柔润酯。
LanolTM P是由SEPPIC公司销售的具有稳定作用的添加剂。
ParsolTM MCX是对甲氧基肉桂酸辛酯;由Givaudan公司销售。
SepiperlTM N是由SEPPIC公司销售的珠光试剂,例如如WO 95/13863中所述基于烷基聚葡糖苷的混合物。
MicropearlTM SQL是通过按摩作用释放出来的含有角鲨烷微粒的混合物;其由Matsumo公司销售。
LanolTM 99是由SEPPIC公司销售的异壬酸异壬酯。
LanolTM 37T是由SEPPIC公司销售的甘油三庚酸酯。
SolagumTM L是由SEPPIC公司销售的角叉菜胶。
MarcolTM 82是由Exxon公司销售的液体石蜡。
LanolTM 84D是由SEPPIC公司销售的苹果酸二辛酯。
Parsol NOXTM是由Givandan公司销售的防晒剂。
EusolexTM 4360是由Merck公司销售的防晒剂。
Dow CorningTM 245 Fluid是环状聚二甲基硅氧烷,由Dow Corning公司销售。
LipacideTM PVB是由SEPPIC公司销售的酰化小麦蛋白质水解物。
MicropearlTM LM是角鲨烷、聚甲基丙烯酸甲酯和薄荷醇的混合物,由SEPPIC公司销售。
SepicontrolTM A5是由SEPPIC公司销售的辛酰基甘氨酸、肌氨酸和Cinnamon zylanicum的提取物的混合物,例如1998年6月23日提交的国际专利申请PCT/FR98/01313所述的那些。
LanolTM 2681是由SEPPIC公司销售的椰子辛酸酯/癸酸酯混合物。
MontanovTM 202是如WO 98/47610中所述的APG/脂肪醇组合物,由SEPPIC公司销售。
ProteolTM APL是由SEPPIC公司销售的发泡表面活性剂。
SchercemolTM TISC是由Scher公司销售的酯(柠檬酸三异硬脂基酯)。
VistanolTM NPGC是由Sewa Kasei公司销售的酯(新戊二醇二癸酸酯)。
AntaronTM V216是由Univar公司销售的合成聚合物(PVP/十六碳烯共聚物)。
C MaltidexTM H16322是由Cerestar公司销售的多元醇(麦芽糖醇糖浆)。
SepiwhiteTM MSH是由SEPPIC公司销售的脱色素活性剂(十一碳烯酰基苯丙氨酸)。
DC 345是由Dow Corning公司销售的环状聚二甲基硅氧烷。
DC 5225C是由Dow Corning公司销售的环五硅氧烷和聚二甲基硅氧烷共聚多元醇(dimethiconecopolyol)的混合物。
SepicalmTM VG是由SEPPIC公司销售的安抚剂(棕榈酰基脯氨酸钠)。
MT100VT是由Unipex公司销售的已进行表面处理(氢氧化铝/硬脂酸)的微米化二氧化钛。
Z-Cote HP1是由Gattefosse销售的已进行表面处理的微米化氧化锌。
Candurin Paprika是硅酸铝钾与氧化铁的混合物。
Claims (10)
1.一种制备组合物的方法,所述组合物包含油相、水相、至少一种油包水(W/O)型乳化体系、任选地至少一种水包油(O/W)型乳化体系,其是包含20-70重量%、优选25-50重量%的支化或交联聚电解质的反相胶乳形式,其特征在于所述聚电解质是部分或完全以钠盐或钾盐或铵盐形式成盐的2-丙烯酰胺基-2-甲基丙磺酸与丙烯酰胺和任选地选自含有部分或完全以钠盐或钾盐或铵盐形式成盐的弱酸官能团的单体和/或非丙烯酰胺的中性单体中的一种或多种单体的共聚物,所述制备方法包括以下步骤:
步骤a):制备水相(A),此水相含有丙烯酰胺、部分或完全以钠盐或钾盐或铵盐形式成盐的2-丙烯酰胺基-2-甲基丙磺酸、任选地选自含有部分或完全以钠盐或钾盐或铵盐形式成盐的弱酸官能团的单体和/或非丙烯酰胺的中性单体中的一种或多种单体以及可能的其它亲水性添加剂,所述制备包括将游离的2-丙烯酰胺基-2-甲基丙磺酸、任选地钠盐或钾盐或铵盐形式的2-丙烯酰胺基-2-甲基丙磺酸、丙烯酰胺、所述任选使用的亲水性添加剂和任选使用的选自氢氧化钠、氢氧化钾或氨水的碱性试剂放入水中,使得此溶液的pH保持大于1且小于5,从而获得pH大于1且小于5的第一含水混合物A1;并将所述第一含水混合物A1的pH值调节到5-6.5之间的pH,获得所述水相(A);
步骤b):在有机相中乳化所述水相(A),所述有机相含有油包水(W/O)型的表面活性剂体系、要存在于最终组合物中的油、任选地挥发油和任选地疏水性添加剂,从而形成油包水型乳液(B);
步骤c):在所述油包水型乳液(B)中聚合单体,所述反应是通过将自由基引发剂引入所述乳液(B)中引发的,形成所述共聚物(P)的反相胶乳(L1);
-任选的步骤d):其中,所述共聚物(P)的所述反相胶乳(L1)是通过蒸馏浓缩直到所述挥发油被除去,形成所述共聚物(P)的反相胶乳(L2);和
步骤e):其中任选地,将水包油(O/W)型的乳化体系在低于50℃的温度加入所述共聚物(P)的所述反相胶乳(L1)中,或任选地加入所述共聚物(P)的所述反相胶乳(L2)中,形成所述共聚物(P)的自可逆反相胶乳(L3)。
2.权利要求1所述的制备组合物的方法,其中聚电解质含有60-20摩尔%的部分或完全以钠盐或钾盐或铵盐形式成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸单体和40-80摩尔%的丙烯酰胺单体。
3.权利要求2所述的制备组合物的方法,其中聚电解质含有50-30摩尔%的部分或完全以钠盐或钾盐或铵盐形式成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸单体和50-70摩尔%的丙烯酰胺单体。
4.权利要求1-3所述的制备组合物的方法,其中在组合物中存在的聚电解质是丙烯酰胺、部分或完全以钠盐或钾盐或铵盐形式成盐的2-丙烯酰胺基-2-甲基丙磺酸、以及选自含有部分或完全以钠盐或钾盐或铵盐形式成盐的弱酸官能团的单体和/或非丙烯酰胺的中性单体中的一种或多种单体形成的共聚物(P),所有选自含弱酸官能团的单体和非丙烯酰胺的中性单体中的单体的摩尔比例是大于0%且小于或等于30%。
5.权利要求4所述的制备组合物的方法,其中在所述共聚物(P)中,丙烯酰胺与所有选自含弱酸官能团的单体和非丙烯酰胺的中性单体中的单体之间的摩尔比率是大于或等于1。
6.权利要求1-5中任一项所述的制备组合物的方法,其中在步骤(A)获得的含水混合物A1具有大于1且小于4的pH值,即小于3且更尤其小于2。
7.权利要求1-6所述的制备组合物的方法,其特征在于所述聚电解质选自:
-丙烯酰胺和以钠盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联共聚物;
-丙烯酰胺和以铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联共聚物;
-丙烯酰胺和以钾盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联共聚物;
-丙烯酰胺、以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸和以钠盐、钾盐或铵盐形式部分成盐的丙烯酸的交联三元共聚物;
-丙烯酰胺、N,N-二甲基丙烯酰胺、以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸和以钠盐、钾盐或铵盐形式部分成盐的丙烯酸的交联四元共聚物;
-丙烯酰胺、N,N-二甲基丙烯酰胺和以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联三元共聚物;
-丙烯酰胺、N-异丙基丙烯酰胺和以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联三元共聚物;
-丙烯酰胺、N-[2-羟基-1,1-二(羟基甲基)乙基]丙烯酰胺和以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联三元共聚物;
-丙烯酰胺、丙烯酸(2-羟基乙基)酯、以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸和以钠盐、钾盐或铵盐形式部分成盐的丙烯酸的交联四元共聚物;
-丙烯酰胺、丙烯酸(2-羟基乙基)酯和以钠盐、钾盐或铵盐形式部分成盐的2-甲基-2-[(1-氧代-2-丙烯基)氨基]-1-丙磺酸的交联三元共聚物。
8.化妆品组合物、皮肤药物组合物或药物组合物,其特征在于所述组合物包含至少一种通过权利要求1-7中任一项定义的方法直接获得的反相胶乳作为增稠和/或乳化化合物。
9.化妆品防晒组合物、皮肤化妆品防晒组合物或药物防晒组合物,其特征在于所述组合物包含至少一种防晒剂和通过权利要求1-7中任一项定义的方法直接获得的反相胶乳。
10.如权利要求8中定义的化妆品组合物、皮肤药物组合物或药物组合物,其包含二羟基丙酮和乳酸或葡糖酸,或者包含二羟基丙酮和至少一种防晒剂,或者包含二羟基丙酮和至少一种润湿剂,或者包含二羟基丙酮和咖啡因。
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EP07301660A EP2070958A1 (en) | 2007-12-11 | 2007-12-11 | New process for the preparation of inverse latex of acrylamide-based polymers and composition comprising said latex |
EP07301660.2 | 2007-12-11 | ||
PCT/EP2008/066863 WO2009074513A1 (en) | 2007-12-11 | 2008-12-05 | New process for the preparation of inverse latex of acrylamide-based polymers and composition comprising said latex |
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CN101896517A true CN101896517A (zh) | 2010-11-24 |
CN101896517B CN101896517B (zh) | 2013-04-03 |
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US (2) | US8668915B2 (zh) |
EP (3) | EP2070958A1 (zh) |
CN (1) | CN101896517B (zh) |
ES (1) | ES2535444T3 (zh) |
PL (1) | PL2222738T3 (zh) |
WO (1) | WO2009074513A1 (zh) |
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CN111040075A (zh) * | 2019-07-10 | 2020-04-21 | 中国科学院宁波材料技术与工程研究所 | 一种纳米凝胶的制备方法及其制备得到的纳米凝胶和应用 |
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US8961942B2 (en) | 2011-12-13 | 2015-02-24 | Conopco, Inc. | Sunless tanning compositions with adjuvants comprising sulfur comprising moieties |
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CN106279523B (zh) * | 2015-06-25 | 2019-03-15 | 中国石油天然气股份有限公司 | 一种增稠剂及其制备方法和应用 |
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EP2222738B1 (en) | 2015-02-11 |
EP2708563A1 (en) | 2014-03-19 |
US20140127150A1 (en) | 2014-05-08 |
CN101896517B (zh) | 2013-04-03 |
PL2222738T3 (pl) | 2015-11-30 |
EP2070958A1 (en) | 2009-06-17 |
US8668915B2 (en) | 2014-03-11 |
US20100272661A1 (en) | 2010-10-28 |
WO2009074513A1 (en) | 2009-06-18 |
EP2222738A1 (en) | 2010-09-01 |
ES2535444T3 (es) | 2015-05-11 |
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