CN1964993A - 液体分散聚合物组合物、其制备及其应用 - Google Patents
液体分散聚合物组合物、其制备及其应用 Download PDFInfo
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- CN1964993A CN1964993A CNA2005800185238A CN200580018523A CN1964993A CN 1964993 A CN1964993 A CN 1964993A CN A2005800185238 A CNA2005800185238 A CN A2005800185238A CN 200580018523 A CN200580018523 A CN 200580018523A CN 1964993 A CN1964993 A CN 1964993A
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Classifications
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
- C08L101/12—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
- C08L101/14—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity the macromolecular compounds being water soluble or water swellable, e.g. aqueous gels
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- A61K8/00—Cosmetics or similar toiletry preparations
- 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
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8147—Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
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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
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- A61K8/8158—Homopolymers or copolymers of amides or imides, e.g. (meth) acrylamide; Compositions of derivatives of such polymers
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- A—HUMAN NECESSITIES
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Abstract
液体分散聚合物组合物,其包含在合适的非水流体载体中分散的中和度约25-约100%的亲水性、水溶性或水可溶胀性的聚合物、优选丙烯酸系聚合物的微粒、以及水包油表面活性剂,可用于制备微粒增稠体系以使含水组合物或含水/有机组合物增稠,特别是用于个人护理和药物制剂中。
Description
本发明涉及包含分散的聚合物相、连续的载体相和表面活性剂的液体分散聚合物组合物、其制备以及这些液体分散聚合物组合物的应用,其用于制备使含水组合物、或含水/有机组合物增稠的微粒增稠体系。更具体地,它涉及液体分散聚合物组合物,其包含中和度约25-约100%的亲水性、水溶性或水可溶胀性的聚合物的微粒、以及水包油表面活性剂,所述微粒分散在非水流体载体相中,优选在油或润肤剂酯中,以及所述聚合物组合物的制备以及这些液体分散聚合物组合物的应用,其用于制备微粒增稠体系以使含水组合物或含水/有机组合物增稠,特别是用于个人护理和药物制剂中。
增稠剂广泛用于个人护理制剂如化妆品以及药物制剂中,从而作用于美观性、产品应用以及活性原料的悬浮和递送。为此已经多年使用聚合物增稠剂。所用的聚合物增稠剂的种类从天然树胶如瓜尔胶,到改性的天然材料如羟乙基纤维素,到合成增稠剂如基于聚丙烯酸的Carbomers。
通过Ciba Specialty Chemicals可得到的Salcare和Tinovis系列的液体分散聚合物是在疏水载体介质中的微粒丙烯酸基聚合物增稠剂(microparticulate acrylic-based polymeric thickeners)。SalcareSC91是以PPG-1 trideceth-6(PPG-1十三烷基聚氧乙烯醚-6)作为活性表面活性剂的基于丙烯酸钠聚合物和矿物油载体的阴离子增稠剂。SalcareSC92是包含polyquaternium 32(聚季铵-32)和矿物油的阳离子共聚物增稠剂和调节剂。SalcareSC95和SalcareSC96是阳离子均聚物增稠剂和调节剂。SalcareSC95在具有PPG-1 trideceth-6的矿物油中包含polyquatemium 37。SalcareSC96在具有PPG-1 trideceth-6的丙二醇二辛酸酯二癸酸酯中包含polyquaternium 37。SalcareAST是基于具有PPG-1 trideceth-6的大豆油中的丙烯酸钠聚合物的阴离子增稠剂。
上述亲水性丙烯酸聚合物的微小球形微粒(带正电或带负电的)具有0.1-2μm的典型粒度,平均粒度为0.5-1.0μm。聚合物微粒优选通过其中采用油包水聚合路线使水溶性的乙烯基加成单体聚合的方法制成。
将任意的上述液体分散聚合物搅拌入含水体系中时,活性表面活性剂使疏水性载体转换至水包油乳液中。术语“活性表面活性剂”指的是使疏水性载体至水包油乳液中的转换活化的表面活性剂。同时亲水性聚合物在暴露于水中时膨胀,但没有溶解,导致平稳而快速的粘度增加。通常聚合物颗粒溶胀以得到包含典型粒度为直径2.5-5μm的聚合物颗粒的微粒增稠体系。由于水分子通过渗透移动至小的聚合物颗粒中,聚合物颗粒经受的渗透作用是水与体系中存在的任意电解质之间的平衡。因此高的电解质水平可减少聚合物颗粒的溶胀。
微粒增稠体系具有假塑性体流变学性质(pseudoplastic rheologicalprofile),其提供在低剪切速率(例如静置时制品所受到的剪切速率)下良好的稳定性和悬浮特性,以及在高剪切速率下低的表观粘度,它对应于优异的擦入(rub-in)特性。
令人惊讶地,已经发现使用中和度约25-约50%的聚合物产生改进的增稠体系。
中和度定义为
中和度从0%(其中没有聚合物的可中和位得到中和)直至100%(其中聚合物所有的可中和位都得到中和)。通过常规的酸碱滴定以确定经转化的可中和位%(百分比)来测量中和度。
本发明的一方面提供液体分散聚合物组合物,其包含中和度为约25%-约100%、优选约30%-约50%、更优选约30%-约45%、特别是约30%-约40%的亲水性、水溶性或水可溶胀性的聚合物、非水载体相和水包油表面活性剂(oil-in-water surfactant)。
优选地,所述亲水性、水溶性或水可溶胀性的聚合物以平均粒度为约0.1-约2μm的微粒形式使用。
通常所述液体分散聚合物组合物包含
a)35wt%-65wt%的中和度为约25%-约50%、优选约30%-约50%、更优选约30%-约45%、特别是约30%-约40%的聚合物,
b)20wt%-50wt%的非水载体,和
c)5wt%-25wt%的表面活性剂或表面活性剂混合物,
均以该组合物的总重计。
有利地,该亲水性聚合物a)是水可溶胀的,即它得到充分交联以溶胀但是不溶于水中。优选它是丙烯酸系聚合物。另外它优选是阴离子聚合物。
b)中提及的非水载体流体是化妆品工业已知的而且已经在毛发和皮肤制剂中使用多年。它们包括硅氧烷聚合物,矿物油,氢化聚癸烯,异十六烷,酯类如三羟甲基丙烷三辛酸酯/三癸酸酯、苯甲酸C12-C15烷基酯、硬脂酸乙基己酯、辛酸癸酸甘油三酯、角鲨烷、椰油酸乙基己酯、油酸癸酯、椰油酸癸酯、油酸乙酯、肉豆蔻酸异丙酯、ethylhexyl perlagonate、季戊四醇四辛酸酯/四癸酸酯、PPG-3苄基醚肉豆蔻酸酯、丙二醇二辛酸酯/二癸酸酯、异硬脂酸乙基己酯、棕榈酸乙基己酯,和天然油类如野生大豆、向日葵、希蒙得木(simmondsia chinensis)、红花、月见草和精制油菜籽油以及所有这些化合物的混合物和衍生物。
优选表面活性剂混合物c)既包含可用于制造可溶胀聚合物a)微粒的表面活性剂,也包含充当用于随后的水包油微粒增稠乳液的活化剂的至少一种表面活性剂。用于水包油增稠乳液的活化剂表面活性剂占该组合物的1.0wt%-10.0wt%,优选该组合物的2.0wt%-8.0wt%。优选该活化剂表面活性剂是HLB通常在7以上的非离子水包油乳化剂。合适的此类乳化剂是本领域技术人员已知的。优选乙氧基化的醇类。
另外所述组合物可以包含较少量的不会影响其基本特性的其他组分。通常这些其他组分可以包括至多约3wt%的水和挥发性有机溶剂之一以及从水溶性或水可溶胀的聚合物的制备中留下的少量其他组分。
有利地,组合物(A)包含
a)40wt%-60wt%的中和度为约25%-约50%、优选约30%-约50%、更优选约30%-约45%、特别是约30%-约40%的聚合物,其中该聚合物是阴离子型的以及是水可溶胀的,
b)25wt%-45wt%的非水载体流体,和
c)8wt%-20wt%的表面活性剂或表面活性剂混合物,
均以该组合物的总重计。
特别优选的组合物(B)包含
a)45wt%-58wt%的中和度为约25%-约50%、优选约30%-约50%、更优选约30%-约45%、特别是约30%-约40%的聚合物,其中该聚合物是阴离子型的以及是水可溶胀的,
b)30wt%-40wt%的非水载体流体,和
c)10wt%-18wt%的表面活性剂混合物,
均以该组合物的总重计。
非常特别优选的组合物(C)包含
a)45wt%-58wt%的中和度为约25%-约50%、优选约30%-约50%、更优选约30%-约45%、特别是约30%-约40%的水可溶胀的聚合物,其中该聚合物是阴离子型的,
b)32wt%-38wt%的非水载体流体,和
c)12wt%-18wt%的表面活性剂混合物,
均以该组合物的总重计。
本发明的另一方面在于提供经增稠的水性的或含水组合物(D),特别是个人护理制剂,其包含
a)0.1wt%-8wt%、优选1wt%-6wt%的上述液体分散聚合物组合物(A)、(B)或(C),
b)0.1wt%-70wt%、优选2wt%-35wt%的附加成分,例如个人护理成分如化妆品成分或药物赋形剂和/或活性成分,和
c)45wt%-99wt%的水或水与水可混溶的有机溶剂如低级醇的混合物,
均以该组合物的总重计。
上述低级醇包括乙醇、异丙醇、丙二醇、二异丙醇和其他已知的低级醇。
本发明的另一方面在于提供非水液体或固体组合物,如彩色化妆品或皂,其中本发明的聚合物提供某些额外的益处如改进的耐磨性(wearproperty)。
这些组合物可以是洗液、霜(cream)、软膏(salves)、凝胶、乳剂、喷雾剂、泡沫或油膏。
所述附加组分可以是可组成水包油类型增稠含水乳液的一部分的任意成分。化妆品成分的非限制性实例包括:抗菌剂(如三氯生或法呢醇);皮肤调理剂和润肤剂如羊毛脂及其衍生物;酯类如丙酸异丙酯、油酸癸酯、异硬脂酸异丙酯、三辛酸甘油酯(trioctanoin)、三异硬脂酸甘油酯(triisostearin)、丙酸肉豆蔻酯;脂肪醇;角鲨烯;硅氧烷类如环甲基硅氧烷、聚二甲基硅氧烷、聚二甲基硅氧烷共聚醇;乙酰胺单乙醇胺;二甲聚硅氧烷;保湿剂如真芦荟(aloe vera)、防护霜(barrier cream)、润肤剂、α-和β-羟基酸如乳酸和乙醇酸;抗炎活性剂如尿囊素和红没药醇;UV防晒剂如对氨基苯甲酸、水杨酸辛酯、和甲氧基肉桂酸辛酯,“无阳光”晒黑剂(sunlesstanning agent),增白剂,驱虫剂,香精油如广藿香油、薄荷油、迷迭香油、香茅油、茶树油、橙油或柠檬油、杉木油和檀香油,维生素,染料和颜料;毛发调理剂如氨基二甲聚硅氧烷(amodimethicone)、环甲基硅氧烷、泛酰醇、月桂酰胺二乙醇胺、月桂胺氧化物和丝蛋白质;香料组分;染发剂和漂白剂以及防腐剂如对羟基苯甲酸甲酯、乙酯和丙酯及咪唑烷基脲。药物活性成分可以大不相同以及包括打算用于对皮肤或毛发局部施用的所有治疗药,特别是处理皮肤发痒、发麻、剥落(scaling)、发炎或感染、烧伤、以及人或其他哺乳动物谢顶(scalp hair loss)的物质。
本发明的另一方面在于提供制备治疗洗液、霜、软膏、凝胶或油膏的方法,其包含将0.1wt%-8wt%、优选1wt%-6wt%的上述液体分散聚合物混合入包含0.1wt%-70wt%至少一种治疗药和/或赋形剂的含水组合物或含水/有机组合物中。
本发明的另一方面在于提供皮肤或毛发局部治疗的方法,其包含将上述组合物施加至需要上述治疗的人类或其他哺乳动物的皮肤、面部、毛发或头皮上。治疗的类型将会取决于在所述组合物中溶解或悬浮的活性成分。例如组合物可以包含面霜如防护霜、保湿霜、洗液或乳剂、清洁剂或调色剂、手部或身体乳剂或洗液、包含抗UV-A和UV-B辐射的防晒剂的体用喷雾、霜、洗液或乳剂、“无阳光”晒黑霜、洗液或喷雾、皮肤漂白霜、洗液或喷雾、脱毛霜、发用调理霜、洗液或香波、染发霜或洗液、剃须前或剃须后用的霜、洗液、凝胶或香膏、消毒霜、洗液、油膏或凝胶、作为日晒后晒伤用的润肤膏、洗液或喷雾、等等。
本发明的其他方面从以下的论述和实施例将会变得明显。实施例仅仅举例说明本发明的某些方面以及并不意味着作为其限制。
本发明中所用的亲水性、水可溶胀的丙烯酸系液体分散聚合物组合物在性质上总的说来是阴离子型的。中和度为约25%-约50%的所述聚合物可以是均聚物或共聚物。它们要么是水溶性阴离子单体的一种或多种单烯键式不饱和单体形成,要么由可以包括阴离子单体与次要量的非离子单体的混合物的主要是阴离子型的单体混合物形成。中和度为约25%-约50%的聚合物可以便利地通过在疏水性液体(即具有足够低的与水混溶性以致其可在反相聚合中用作非水相的液体)中合适单体的反相乳液聚合以平均粒度0.1-2μm的微粒形式得到。该液体必须在聚合物可能得以合成的整个温度范围(例如15-100℃)内对于聚合物或者对于形成聚合物的单体基本上没有溶剂化效应,因为溶剂化介质对反相乳液聚合会是不能令人满意的。同样地,单体或单体混合物必须是水溶性的以使反相聚合能够进行。
合适的阴离子单体包括丙烯酸、甲基丙烯酸及其碱金属和铵盐,2-丙烯酰氨基-2-甲基-丙烷磺酸及其盐,苯乙烯磺酸钠等。丙烯酸是最优选的阴离子单体。优选羧酸基团20-80%、有利地30-45%,以碱金属盐或铵盐形式,特别是钠盐。
合适的非离子单体包括丙烯酰胺、甲基丙烯酰胺、N,N,-二烷基丙烯酰胺、N-乙烯基吡咯烷酮和水溶性的羟基取代的丙烯酸酯或甲基丙烯酸酯。
如果使用阴离子型混合物,阴离子单体的用量优选大于该混合物的60wt%,以及通常至少是该混合物的80wt%。优选的阴离子聚合物完全由阴离子单体形成。
液体分散聚合物组合物有利地通过将少量合适的交联剂如多官能乙烯基加成单体混入聚合混合物中而进行交联。优选使用水溶***联剂。
可以使用可溶于单体或单体混合物中的常规烯键式不饱和交联剂或多烯键式不饱和交联剂中的任意一种,包括二、三或四烯键式不饱和的物质。优选二烯键式不饱和化合物如亚甲基双丙烯酰胺、二(甲基)丙烯酰胺、三烯丙基铵盐、丙烯酸乙烯基氧乙基酯或甲基丙烯酸乙烯基氧乙基酯、二乙烯基苯;四烯丙基氯化铵;丙烯酸烯丙基酯和甲基丙烯酸烯丙基酯;二醇和聚二醇的二丙烯酸酯和二甲基丙烯酸酯;丁二烯;1,7-辛二烯;烯丙基-丙烯酰胺和烯丙基-甲基丙烯酰胺;双丙烯酰氨基乙酸;N,N’-亚甲基-双丙烯酰胺以及多元醇多烯丙基醚,如多烯丙基蔗糖和季戊四醇四烯丙基醚。
更优选的交联剂是四烯丙基氯化铵;烯丙基-丙烯酰胺和烯丙基-甲基丙烯酰胺;双丙烯酰氨基乙酸和N,N’-亚甲基-双丙烯酰胺。
最优选的交联剂是四烯丙基氯化铵和N,N’-亚甲基-双丙烯酰胺。
同样适合使用交联剂的混合物。
交联剂的用量通常是每百万份(以干重计)单体100-10,000重量份交联剂。最优选地,对于阳离子或阴离子单体,其是约500-2000ppm,特别是500-900ppm。可以通过例行试验确定最佳用量。
通过亲水性单体(优选一种或多种丙烯酸酯和/或甲基丙烯酸酯单体)在疏水液体相中的反相乳液聚合来制备亲水性聚合物。反相乳液聚合是已知技术,例如在US4,628,078中得到描述,其内容通过引用全部并入本文。
用于制备该液体分散聚合物组合物的连续相至少部分地由非水载体流体提供。由于该液体分散聚合物组合物主要想用于化妆品或药用目的,优选将化妆品和/或药用方面可接受的以及足够疏水性从而可在反相聚合中用作连续相的非水载体流体用作所述连续相。许多的这类材料是已知的而且是可购得的。上述非水载体流体包括矿物油、氢化聚癸烯、包括大豆油的天然油类、角鲨烷、包括丙二醇二癸酸酯二辛酸酯的润肤剂酯。优选的非水载体流体是矿物油。
用于聚合中的疏水性液体相的用量主要由提供令人满意的反相乳液介质的需要来决定。其一般是每重量份亲水性聚合物(干重)至少约0.5重量份的非水载体流体。为了得到具有在非水载体流体中更高微粒含量、例如在非水载体流体中1.2-约1.7重量份亲水性聚合物(干重)的液体分散聚合物组合物以及为了便于处理,有利的是采用挥发性的惰性疏水溶剂。合适的惰性疏水溶剂包括烃类和卤代烃。一种特别优选的烃混合物是IsoparG(Exxon Mobil Corporation的商标)。适宜采用以干重计的每份亲水性聚合物1-2份、优选1.3-1.9份的挥发性的惰性疏水溶剂。
所述聚合物通过常规的反相乳液工艺制备,即通过将任选包含螯合剂和烯键式不饱和交联单体的1重量份(干重)至少一种含水的烯键式不饱和单体,加入至约1-3重量份至少部分包含非水载体流体以及包含约0.1-0.2份至少一种HLB值在9.0以下的常规油包水乳化剂和任选0.5-10.0份聚合稳定表面活性剂的疏水性液体中,强烈搅拌以使得形成基本上稳定的所需精细粒度的乳液。合适的油包水乳化剂是本领域技术人员已知的。优选脱水山梨糖醇酯类。二亚乙基三胺五乙酸、其钠盐是合适的螯合剂。烯键式不饱和单体可以是二烯键式或多烯键式不饱和的。
反应混合物用氮气吹扫,而聚合通过加入常规的自由基源来引发。合适的聚合引发剂是本领域技术人员已知的。典型的自由基形成催化剂包括过氧化物如过硫酸钠、钾和铵、过氧化辛酰(caprylyl peroxide)、过氧化苯甲酰、过氧化氢、过氧化壬酰、氢过氧化异丙苯、叔丁基二过邻苯二甲酸酯(tertiary butyl diperphthalate)、过苯甲酸叔丁酯、过乙酸钠、二(2-乙基己基)过氧二碳酸酯等等,以及偶氮催化剂如偶氮二异丁腈。其他可用的催化剂是重金属活化的催化剂体系。优选的聚合引发剂类型是氧化还原引发对。引发之后保持适当的温度和搅拌条件直至单体到聚合物的转化基本上完成为止。适当的条件是本领域技术人员已知的。
然后从反相乳液中除去水和所有挥发性溶剂,例如是通过减压下蒸馏,以使得制备在非水连续相中分散的尺寸小于2μm的聚合物颗粒的基本上无水的稳定分散体。
在蒸馏结束后加入以组合物重量计约1.0wt%-10.0wt%、优选2wt%-8wt%的HLB通常在7以上的非离子型水包油乳化剂。合适的此类乳化剂是本领域技术人员已知的。优选乙氧基化的醇类。
通过将单体相温度保持在30℃以下以及向单体相中添加包括但不限于氢氧化钠、氢氧化锂、氢氧化钾的金属碱、或者包括但不限于氢氧化铵或单质胺的含氮碱类以便使经由常规酸-碱滴定或由已知的pH测量体系测定的所需摩尔比率的羧酸位中和,从而调节中和度。
本发明的另一特征在于将合适的聚合稳定剂表面活性剂用作加工助剂,从而在蒸馏过程中保持乳液完整性,以及为最终的液体聚合物分散体即使当它包含高含量的水溶性或水可溶胀性分散聚合物的微粒时也可成为自由流动的液体作准备。
每重量份(干重)烯键式不饱和单体有利地采用0.5-10.0份、优选1.0-6.0份的这种聚合表面活性剂。
优选的聚合表面活性剂是(甲基)丙烯酸烷基酯单体与氨基官能单体的共聚物,其可以如下进行制备:
将(甲基)丙烯酸烷基酯、氨基官能单体和合适的油溶性热引发剂如2,2’-偶氮二(2-甲基丁腈)溶解在惰性溶剂例如脂族或芳族烃溶剂如Isopar G中。在80-90℃的反应温度下经过2-6小时将该混合物送入含有更多溶剂和热引发剂的容器中。在进行冷却和放料之前,在该温度下维持反应又2小时。
(甲基)丙烯酸烷基酯的烷基可以是任意的合适的烷基,然而优选C8-C22基团。
氨基官能单体为通式(1):
(1)CH2=CRC(=O)-X-B-NR1R2,
其中
R是氢或C1-C4烷基,
X是-O-或-NH-,
B是C1-C4亚烷基,
R1是氢或C1-C10烷基,和
R2是C1-C10烷基。
(甲基)丙烯酸烷基酯∶氨基官能单体的比例以摩尔计可以是0.5至8.0∶1。优选以摩尔计0.75至6.0∶1,以及最优选1.0至4.0∶1。
分子量可以通过本领域技术人员已知的常规的色谱技术来确定。典型的分子量可以是10,000-60,000,最常用的是15,000-40,000。
将所述液体分散体搅拌到含水体系中时,非离子表面活性剂将疏水性载体转换至水包油乳液中。同时亲水性聚合物在暴露于水中时膨胀,导致平稳而快速的粘度增加。通常聚合物颗粒溶胀以得到包含典型粒度为2.5-5.0μm的聚合物颗粒的微粒增稠体系。
本发明的液体分散组合物提供微粒增稠体系,其对浓度为0.1-8.0%的含水或含水/有机制剂提供有效的增稠。优选浓度为1wt%-6wt%。然而,另外它们将液体分散聚合物的增稠效应与通过有经验地选择合适的非水载体流体所带来的软化作用和感觉效果(sensorial effects)相结合。
已经证明降低此类丙烯酸聚合物的中和度以提高该微粒增稠体系在含水溶液中的增稠效率。当中和度从100中和%减小至30中和%时表观粘度的增加大致是线性的。在通过常规酸-碱滴定确定的约25中和%以下,聚丙烯酸的溶解性使其作为增稠剂和流变学改性剂的有效性显著降低。离子盐如氯化钠的加入已知由于渗透效应而可减小交联微粒的溶胀能力,但是已经证明离子物种的作用在中和度低于30%(通过常规酸-碱滴定)时增加。因此有利的是,选择30%-40%的中和度从而在含水体系、油/水乳液和包含低含量的离子物种(包括但不限于无机盐)、植物提取物、蛋白质和类似物种的体系中提供更有效的增稠。
所述液体分散聚合物组合物与许多个人护理活性成分和助剂是相容的。可以使用该聚合物的典型制剂实例包括:
皮肤护理制剂,其包括各种面部和身体乳液,如护理、清洁、除臭和脱毛用的霜、洗液、乳剂和喷雾,彩色化妆品如粉底液、液体眼影、液体胭脂、唇膏和水性睫毛膏;面膜、唇用香膏,皮肤护理制剂如体用洗涤用品,各种剃须制品;洗手皂,皂条和液体皂。
毛发护理制剂,其包括发用调理剂,染发剂(永久、半永久和暂时性的),定型凝胶、洗液和霜,洗发香波,卷发矫直剂(hair relaxers),烫发剂和发膜(hair masks)。
日晒制剂如日晒霜、洗液和喷雾,防晒乳,晒黑促进剂,晒后用霜、洗液和喷雾以及无日光晒黑洗液或霜。
以下的制剂实例仅仅举例说明配方设计可能性的一些典型方面,无论如何并非想要进行限制。所有的百分数是制剂的重量百分数。粘度用Brookfield RVT粘度计确定。
实施例1:合成实施例
通过将下列组分混合在一起制成水溶性组分的“水”相:
33.65份丙烯酸单体(100%浓度)
0.15份二亚乙基三胺五乙酸五钠的40%溶液
49.79份水
1.50份亚甲基双丙烯酰胺(在水中0.5%)
14.91份氢氧化钠(47%浓度)
(氢氧化钠加入过程中保持温度低于30℃)
通过将下列组分混合在一起制成“油相”:
3.99份脱水山梨糖醇三油酸酯
4.66份聚合稳定剂(100%浓度)
31.16份矿物白油(mineral white oil)
60.19份高纯度脱芳构化的烃溶剂(如Isopar G)
在高剪切下将两相以0.751份油相对1.0份水相的比例混合在一起以形成油包水乳液。
将所得到的油包水乳液转移到装有氮气喷管、搅拌器和温度计的反应器中。用氮气吹扫乳液以除去氧。通过加入偏亚硫酸氢钠和叔丁基氢过氧化物的氧化还原对而引起聚合。
放热完成以及已经通过使用热引发剂而减少游离单体之后,进行真空蒸馏以除去水和挥发性溶剂,从而提供约53.5%的最终聚合物固体。
向其中加入0.125份脂肪醇乙氧基化物。
将中和度调节至30-40%的值。
实施例2:不同中和度下的增稠效果的比较
在下表中,在水溶液和稀离子溶液中比较在一系列中和度下制得的本发明的聚合物的增稠效果。
中和% | 粘度去离子水中1%活性聚合物 | 粘度0.1%氯化钠溶液中1%活性聚合物 |
30 | 190000 | 66400 |
40 | 184000 | 69600 |
50 | 172000 | 63600 |
60 | 157000 | 48400 |
70 | 126000 | 33000 |
80 | 94900 | 11400 |
(通过Brookfield RVT粘度计,6#锭测定)
实施例3:脱毛霜
该制剂提供基于巯基醋酸钠的脱毛霜的制剂。调节所用增稠剂的量可以使制品从滚涂洗液(roll-on lotion)变成粘稠的乳霜。
成分 | 成分(商标&供应商) | 含量[wt-%] | |
1 | 实施例1的聚合物 | 6.0-8.0 | |
2 | 液状石蜡 | Kristol M14(Carless) | 5.0 |
3 | 甘油 | Glycerol | 2.0 |
4 | 苯氧基乙醇(和)对羟基苯甲酸甲酯(和)对羟基苯甲酸乙酯(和)对羟基苯甲酸异丙酯(和)对羟基苯甲酸丙酯 | Phenonip(Clariant) | 0.20 |
5 | 香料 | Fragrance | 0.7 |
6 | 凡士林油 | Vaseline(Richardson-Vicks) | 2.0 |
7 | 巯乙酸 | 3.0 | |
8 | 水 | 至100 |
另外,加入氢氧化钠以调节pH值为12-13。
方法:
1称取(6)至烧杯中并加热至40℃
2称取除(1)以外的所有成分至另一烧杯中并充分混合
3搅拌下加入(6)
4用氢氧化钠调节混合物的pH为12-13,连续搅拌
5平缓搅拌下加入所需量的(1),继续搅拌直至匀和为止
6根据需要,滴加氢氧化钠调节pH为12-13
典型性质:
外观:平滑的低粘度至高粘度乳霜
粘度:9000-45000cPs
pH:12-13
实施例4:面部保湿剂
该制剂包含轻质(light)润肤剂、角鲨烷和硅氧烷的组合以提供良好的擦入(rub-in)特性和优异的用后感觉。遮光剂的存在提供日常使用所需的低程度日晒防护。
所述聚合物作为油相的乳化剂和增稠剂而包括在内以及容许冷法乳化(cold-process emulsification)。另外矿物油载体会提供额外的保湿性能。
成分 | 成分(商标&供应商) | 含量[wt-%] | |
1 | 水 | 至100 | |
2 | 实施例1的聚合物 | 2.0 | |
3 | 椰油基辛酸酯/癸酸酯 | Cetiol LC(Cognis) | 2.5 |
4 | 角鲨烷 | Cetiol SQ(Cognis) | 2.0 |
5 | 月桂酸己基酯 | Cetiol A(Cognis) | 2.0 |
6 | 棕榈酸乙基己基酯 | Estol 1543(Uniqema) | 2.0 |
7 | 二甲聚硅氧烷 | Silicone Fluid 200 (DowCorning) | 2.5 |
8 | 甲氧基肉桂酸乙基己基酯 | Tinosorb OMC (CibaSpecialty Chemicals) | 5.0 |
9 | 苯氧基乙醇(和)对羟基苯甲酸甲酯(和)对羟基苯甲酸乙酯(和)对羟基苯甲酸异丙酯(和)对羟基苯甲酸丙酯 | Phenonip(Clariant) | 0.20 |
10 | 香料 | Fragrance | 0.20 |
方法:
称取除(2)以外的所有成分至洁净、干燥的烧杯中
启动搅拌并添加(2)
继续搅拌直至粘滞和均匀为止
典型性质:
外观:平滑的粘稠乳霜
粘度:25000-35000cPs
pH:5-6
实施例5:身体保湿剂(霜)
该制剂基于传统的包含脂肪醇和酯类的霜。所述聚合物在低含量混合下提供乳化以及提高外相的稳定性。
成分 | 成分(商标&供应商) | 含量[wt-%] | |
1 | 水 | 至100 | |
2 | 实施例1的聚合物 | 1.0 | |
3 | 硬脂醇 | Crodacol S95EP (CrodaChemicals) | 5.0 |
4 | 鲸蜡醇 | Crodacol C90EP (CrodaChemicals) | 5.0 |
5 | 二甲聚硅氧烷 | Silicone Fluid 200 (DowCorning) | 5.0 |
6 | 硬脂酸十六十八醇酯(CetearylStearate) | Estol 3709CSS(Uniqema) | 2.0 |
7 | 甘油 | Glycerol | 2.0 |
8 | 丙二醇 | Propylene Glycol | 2.0 |
9 | 苯氧基乙醇(和)对羟基苯甲酸甲酯(和)对羟基苯甲酸乙酯(和)对羟基苯甲酸异丙酯(和)对羟基苯甲酸丙酯 | Phenonip(Clariant) | 0.20 |
10 | 香料 | Fragrance | 0.20 |
称取成分(1)、(7)和(8)至洁净干燥的烧杯中并加热至80℃
称取成分(3)-(6)至另一洁净干燥的烧杯中并加热至80℃
在充分搅拌下将油相加入到水相中以及开始冷却
在<50℃下添加成分(2),在<30℃下添加成分(9)和(10)
继续搅拌直至粘滞和均匀为止
典型性质:
外观:平滑的粘稠乳霜
粘度:35000-45000cPs
pH:5-6
实施例6:晒后洗液/霜
成分 | 成分(商标&供应商) | 含量[wt-%] | |
1 | 水 | 至100 | |
2 | Prunus Dulcis | 甜杏仁油(AE Connock) | 4.50 |
3 | 可拉果提取物 | Actiphyte Kola Nut(Active | 5.00 |
Organics) | |||
4 | Aloe Barbadenis | Aloe Vera(Active Organics) | 2.00 |
5 | 实施例1的聚合物 | 3.25 | |
6 | 水&泛醇&辛酸/癸酸甘油三酯&聚山梨醇酯80&卵磷脂 | Tinoderm P(Ciba SpecialtyChemicals) | 1.25 |
7 | 苯氧基乙醇&对羟基苯甲酸甲酯&对羟基苯甲酸丙酯&2-溴-2-硝基丙烷-1,3-二醇 | Nipaguard BPX (NipaLaboratories) | 0.20 |
方法:
将1加入烧杯中,启动搅拌然后加入2、3、4、6和7,充分混合约5-10分钟
提高搅拌速度后缓慢添加5,继续缓慢搅拌约5-10分钟直至粘滞和均匀为止
典型性质:
外观:可流动的洗液
粘度:5,000-8,000cPs
pH:5.0-6.5
实施例7:硅氧烷喷雾调理剂
这是适于每天使用的轻质调理剂以及包含轻质硅氧烷和润湿剂。所述聚合物帮助香味混入至大量含水的制剂中以及提供粘度和良好的施用特性。
成分 | 成分(商标&供应商) | 含量[wt-%] | |
1 | 水 | 至100 | |
2 | 实施例1的聚合物 | 1.0 | |
3 | 氨基二甲聚硅氧烷(和)十六烷基三甲基氯化铵(和)十三烷基聚氧乙烯醚-12 | Silicone Fluid 949 Cationic(Dow Corning) | 5.0 |
4 | 环甲基硅氧烷 | Silicone Fluid 235 (DowCorning) | 1.0 |
5 | 油醇聚氧乙烯醚-20(Oleth-20) | Volpo N20 (CrodaChemicals) | 1.0 |
6 | 咪唑烷基脲 | Germall 115(ISP) | 0.2 |
7 | 香料 | Fragrance | 0.20 |
方法:
称取除(2)以外的所有成分至洁净、干燥的烧杯中
启动搅拌并添加(2)
继续搅拌直至均匀为止
典型性质:
外观:可喷雾的液体
粘度:2500-5000cPs
pH:5.0-6.0
Claims (12)
1.一种液体分散体聚合物组合物,其包含中和度为约25%-约100%的亲水性、水溶性或水可溶胀的聚合物、非水载体相和水包油表面活性剂。
2.权利要求1的液体分散体,其中所述亲水性、水溶性或水可溶胀的聚合物具有约30%-约50%的中和度。
3.权利要求1的液体分散体,其中所述亲水性、水溶性或水可溶胀的聚合物具有约30%-约45%的中和度。
4.权利要求1的液体分散体,其中所述亲水性、水溶性或水可溶胀的聚合物具有约30%-约40%的中和度。
5.权利要求1-4中任一项的液体分散体,其中所述亲水性、水溶性或水可溶胀的聚合物以平均粒度为约0.1-约2μm的微粒形式使用。
6.权利要求1-5中任一项的液体分散体,其包含
a)35wt%-65wt%的亲水性、水溶性或水可溶胀的聚合物,
b)20wt%-50wt%的非水载体,和
c)5wt%-25wt%的表面活性剂或表面活性剂混合物,
均以该组合物的总重计。
7.权利要求6的液体分散体,其包含
a)40wt%-60wt%的阴离子型的和水可溶胀的聚合物,
b)25wt%-45wt%的非水载体流体,和
c)8wt%-20wt%的表面活性剂或表面活性剂混合物,
均以该组合物的总重计。
8.权利要求1-7中任一项的液体分散体,其中所述亲水性、水溶性或水可溶胀的聚合物通过丙烯酸和甲基丙烯酸(及其盐)、2-丙烯酰氨基-2-甲基-丙烷磺酸、苯乙烯磺酸钠、丙烯酰胺、甲基丙烯酰胺和N,N-二烷基丙烯酰胺中的至少一种单体的聚合而得到。
9.权利要求1-7中任一项的液体分散体,其中所述亲水性、水溶性或水可溶胀的聚合物通过丙烯酸和甲基丙烯酸(及其盐)、2-丙烯酰氨基-2-甲基-丙烷磺酸和苯乙烯磺酸钠中的至少一种单体的聚合而得到。
10.权利要求1-9中任一项的液体分散体,其中选择中和度以使所述体系在含水的、油/水、非水体系和包含离子物种的制剂中的增稠效率最佳。
11.一种个人护理制剂,其包含
a)0.1wt%-8wt%、优选1wt%-6wt%的权利要求6或7的液体分散体聚合物组合物,
b)0.1wt%-70wt%、优选2wt%-35wt%的附加成分,例如个人护理成分如化妆品或药物赋形剂和/或活性成分,和
c)45%-99%的水或水与水可混溶的有机溶剂如低级醇的混合物,
均以该组合物的总重计。
12.一种制备治疗洗液、霜、软膏、凝胶或油膏的方法,其包含将0.1wt%-8wt%、优选1wt%-6wt%的权利要求1-5的液体分散聚合物混合入包含0.1wt%-70wt%的至少一种治疗剂和/或赋形剂的含水组合物或含水/有机组合物中。
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CN (2) | CN101671407B (zh) |
AT (1) | ATE437896T1 (zh) |
BR (1) | BRPI0509659B8 (zh) |
DE (1) | DE602005015704D1 (zh) |
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CN104334586A (zh) * | 2012-05-21 | 2015-02-04 | 巴斯夫欧洲公司 | 含有阳离子聚合物和稳定剂的反相分散体 |
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2005
- 2005-03-30 CN CN200910158675.8A patent/CN101671407B/zh active Active
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104321349A (zh) * | 2012-05-21 | 2015-01-28 | 巴斯夫欧洲公司 | 含有阴离子性或非离子性聚合物和稳定剂的反相分散体 |
CN104334586A (zh) * | 2012-05-21 | 2015-02-04 | 巴斯夫欧洲公司 | 含有阳离子聚合物和稳定剂的反相分散体 |
CN104797679A (zh) * | 2012-11-14 | 2015-07-22 | 巴斯夫欧洲公司 | 三次矿物油开采方法 |
CN104797679B (zh) * | 2012-11-14 | 2018-04-13 | 巴斯夫欧洲公司 | 三次矿物油开采方法 |
Also Published As
Publication number | Publication date |
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JP4989458B2 (ja) | 2012-08-01 |
DE602005015704D1 (de) | 2009-09-10 |
US20080275138A1 (en) | 2008-11-06 |
ES2329488T3 (es) | 2009-11-26 |
BRPI0509659B1 (pt) | 2019-01-29 |
CN101671407A (zh) | 2010-03-17 |
CN101671407B (zh) | 2014-04-30 |
ATE437896T1 (de) | 2009-08-15 |
EP1756168B1 (en) | 2009-07-29 |
BRPI0509659A (pt) | 2007-10-09 |
JP2012102339A (ja) | 2012-05-31 |
JP2007531811A (ja) | 2007-11-08 |
EP1756168A2 (en) | 2007-02-28 |
WO2005097834A2 (en) | 2005-10-20 |
KR101239147B1 (ko) | 2013-03-07 |
BRPI0509659A8 (pt) | 2018-02-06 |
BRPI0509659B8 (pt) | 2021-05-25 |
WO2005097834A3 (en) | 2006-03-02 |
KR20070004813A (ko) | 2007-01-09 |
US20160367466A1 (en) | 2016-12-22 |
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