CN109414376A - 稳定的微胶囊组合物 - Google Patents
稳定的微胶囊组合物 Download PDFInfo
- Publication number
- CN109414376A CN109414376A CN201780040398.3A CN201780040398A CN109414376A CN 109414376 A CN109414376 A CN 109414376A CN 201780040398 A CN201780040398 A CN 201780040398A CN 109414376 A CN109414376 A CN 109414376A
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- polyquaternium
- agent
- microcapsule compositions
- ester
- microcapsules
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Abstract
公开了稳定的微胶囊组合物,其各自含有分散在水相中的微胶囊和稳定剂。微胶囊组合物在45℃储存时稳定至少4周,并且认为所述微胶囊组合物在(i)所述组合物的粘度为3000cP以下以及(ii)所述组合物体积的20%以下的水与所述组合物分离时是稳定的。还公开了具有这样的稳定的微胶囊组合物的消费品。
Description
背景
微胶囊可用于其中需要以时间延迟或受控的方式递送、施用或释放香精或其他活性材料的多种应用。
常规的微胶囊组合物含有分散在水相中的微胶囊。它们倾向于形成凝胶,分层,过早地释放活性材料等。参见US 2014/0287008和WO 2015/023961。已经开发特定的微胶囊组合物以通过设计更坚固耐用的微胶囊壁来改善稳定性。参见US 20140044760、WO2014011860和US20130337023。然而,这些微胶囊组合物仍面临稳定性问题,包括短的储存寿命,在严苛温度运输期间的凝胶形成,和在消费品中的不稳定性。
需要开发可以储存延长的时间段并且提供在化妆品中的长货架期的稳定的微胶囊组合物。
概述
本发明基于以下发现:带负电的粘土和阳离子聚合物的组合可以使微胶囊组合物稳定。
因此,本发明的一个方面涉及一种稳定的微胶囊组合物,所述微胶囊组合物具有分散在水相中的微胶囊和稳定剂,其中所述微胶囊组合物在45℃储存时稳定至少4周。认为所述微胶囊组合物在(i)所述组合物的粘度为3000cP以下(例如,2000cP以下)以及(ii)所述组合物体积的20%以下(例如,15%以下,和10%以下)的水与所述组合物分离时是稳定的。
本发明的另一方面涉及一种稳定的微胶囊组合物,所述微胶囊组合物包含分散在水相中的微胶囊和稳定剂,其中稳定剂是带负电的粘土和阳离子聚合物的组合。该组合物在45℃储存时稳定例如至少4周。
在一个实施方案中,微胶囊以上述稳定的微胶囊组合物重量的10%至70%(例如,20%至70%以及30%至60%)的水平存在。
在另一实施方案中,带负电的粘土以0.05%至2%(例如,0.05%至1%、0.1%至0.5%以及0.1%至0.3%)的水平存在;并且阳离子聚合物以0.05%至5%(例如,0.05%至2.5%、0.1%至2%、0.1%至1%以及0.2%至0.7%)的水平存在。一种示例性的带负电的粘土是蒙脱石粘土。合适的阳离子聚合物是阳离子聚季铵盐聚合物,如羟乙基纤维素二甲基二烯丙基氯化铵共聚物(PQ-4),丙烯酰胺和二烯丙基二甲基氯化铵的共聚物(PQ-7),丙烯酸、甲基丙烯酰胺-丙基三甲基氯化铵和丙烯酸甲酯的三元共聚物(PQ-47),及其组合。
本发明的合适的微胶囊包括但不限于各自具有微胶囊壁和被所述微胶囊壁囊封的微胶囊芯的芯-壳型微胶囊。微胶囊壁可以由选自由以下各项组成的组中的囊封聚合物形成:聚丙烯酸酯、聚脲、聚氨酯、聚丙烯酰胺、聚酯、聚醚、聚酰胺、聚(丙烯酸酯-共-丙烯酰胺)、淀粉、二氧化硅、明胶和阿拉伯树胶、藻酸盐、壳聚糖、聚丙交酯、聚(三聚氰胺-甲醛)、聚(脲-甲醛)及其组合。微胶囊芯可以含有选自由以下各项组成的组中的活性材料:香精、前香精(pro-fragrance)、香料、恶臭中和剂、维生素或其衍生物、抗炎剂、杀真菌剂、麻醉剂、止痛剂、抗微生物活性成分(antimicrobial active)、抗病毒剂、抗感染剂、祛痘剂、皮肤光亮剂、驱昆虫剂(insect repellant)、兽用驱避剂(animal repellent)、驱寄生虫剂(vermin repellent)、软化剂(emollient)、皮肤保湿剂、皱纹控制剂、UV防护剂、织物柔顺剂活性成分(fabric softener active)、硬表面清洁活性成分(hard surface cleaningactive)、皮肤或头发调理剂、阻燃剂、抗静电剂、纳米至微米尺寸的无机固体、聚合物或弹性体颗粒、味道调节剂、细胞、益生菌及其组合。
上述微胶囊组合物中的任一种还可以包含烷基萘磺酸盐/酯甲醛缩合物、聚乙烯吡咯烷酮、聚乙烯醇、聚磺苯乙烯、羧甲基纤维素、萘磺酸盐/酯缩合物的钠盐、乙烯吡咯烷酮和季铵化的甲基丙烯酸二甲基氨基乙酯的共聚物或其组合。当囊封聚合物是聚脲或聚氨酯时,所述聚脲可以是多官能异氰酸酯和多官能胺任选地在烷基萘磺酸盐/酯甲醛缩合物和聚乙烯吡咯烷酮的存在下的反应产物,并且所述聚氨酯可以是多官能异氰酸酯和作为交联剂的多官能醇任选地在烷基萘磺酸盐/酯甲醛缩合物和聚乙烯吡咯烷酮的存在下的反应产物。烷基萘磺酸盐/酯甲醛缩合物和聚乙烯吡咯烷酮中的每一种可以独立地以微胶囊组合物重量的0.1%至5%的水平存在,并且烷基萘磺酸盐/酯甲醛缩合物和聚乙烯吡咯烷酮之间的比率可以是10:1至1:10。
在一些实施方案中,多官能异氰酸酯是芳族多官能异氰酸酯、脂族多官能异氰酸酯或其组合,其中芳族多官能异氰酸酯含有苯基、甲苯基、二甲苯基、萘基或联苯基部分或者所述部分中的两种以上,并且脂族多官能异氰酸酯是六亚甲基二异氰酸酯的三聚体、异佛尔酮二异氰酸酯的三聚体、六亚甲基二异氰酸酯的缩二脲或其组合。示例性的芳族多官能异氰酸酯是聚合的亚甲基二苯基二异氰酸酯、甲苯二异氰酸酯的多异氰脲酸酯、甲苯二异氰酸酯的三羟甲基丙烷加合物、亚二甲苯基二异氰酸酯的三羟甲基丙烷加合物或其组合。合适的脂族多官能异氰酸酯包括选自由以下各项组成的组中的那些:六亚甲基二异氰酸酯的二聚体、缩二脲、对称三聚体、不对称三聚体,及其组合。
在其他实施方案中,多官能胺是六亚甲基二胺、六亚乙基二胺、乙二胺、1,3-二氨基丙烷、1,4-二氨基-丁烷、二亚乙基三胺、五亚乙基六胺、1,6-二氨基己烷、肼、1,4-二氨基环己烷、1,3-二氨基-1-甲基丙烷、双(3-氨基丙基)胺、双(六亚甲基)三胺、三(2-氨基乙基)胺、三亚乙基-四胺、N,N'-双(3-氨基丙基)-1,3-丙二胺、四亚乙基五胺、支化的聚乙烯亚胺、壳聚糖、乳酸链球菌肽(nisin)、明胶、1,3-二氨基-胍、1,1-二甲基双胍、胍、精氨酸、赖氨酸、鸟氨酸、组氨酸、氨基-2-甲基-1-丙醇或其组合。
在其他实施方案中,囊封聚合物是聚脲,所述聚脲是多官能异氰酸酯和多官能胺的反应产物,其中多官能异氰酸酯含有甲苯二异氰酸酯的三羟甲基丙烷加合物或亚二甲苯基二异氰酸酯的三羟甲基丙烷加合物,并且多官能胺是二亚乙基三胺、双(3-氨基丙基)胺、双(六亚甲基)三胺(bis(hexanethylene)triamine)、三(2-氨基乙基)胺、三亚乙基四胺、N,N'-双(3-氨基丙基)-1,3-丙二胺、四亚乙基五胺、五亚乙基六胺、支化的聚乙烯亚胺、壳聚糖、乳酸链球菌肽、明胶、1,3-二氨基-胍单盐酸盐、1,1-二甲基双胍盐酸盐或碳酸胍或其混合物。这些微胶囊组合物还可以包含聚乙烯醇、聚磺苯乙烯、羧甲基纤维素、聚乙烯吡咯烷酮、萘磺酸盐/酯缩合物的钠盐、乙烯吡咯烷酮和季铵化的甲基丙烯酸二甲基氨基乙酯的共聚物或其组合。
上述微胶囊组合物中的任一种任选地包含选自由以下各项组成的组中的沉积助剂:聚季铵盐-5、聚季铵盐-6、聚季铵盐-7、聚季铵盐-10、聚季铵盐-16、聚季铵盐-22、聚季铵盐-24、聚季铵盐-28、聚季铵盐-39、聚季铵盐-44、聚季铵盐-46、聚季铵盐-47、聚季铵盐-53、聚季铵盐-55、聚季铵盐-67、聚季铵盐-68、聚季铵盐-69、聚季铵盐-73、聚季铵盐-74、聚季铵盐-77、聚季铵盐-78、聚季铵盐-79、聚季铵盐-80、聚季铵盐-81、聚季铵盐-82、聚季铵盐-86、聚季铵盐-88、聚季铵盐-101、聚乙烯胺、聚乙烯亚胺、聚乙烯胺和乙烯基甲酰胺共聚物及其组合。其还可以含有一种或多种游离香精或者一种或多种另外的微胶囊。
上述微胶囊组合物的pH值一般为2至10(例如,3至9、4至8、5至8以及6至7.5)。可以通过添加酸或碱来调节pH值。
微胶囊组合物中的任一种可以是固体形式,例如通过喷雾干燥。
含有上述微胶囊组合物中的一种或多种的消费品也在本发明的范围内。示例性的消费品包括:洗发剂、护发剂、染发剂、头发清新剂、头发固定或定型助剂、头发漂白剂、头发染料或着色剂、肥皂、沐浴液、化妆品制备物、通用清洁剂、浴厕清洁剂、地板清洁剂、窗户清洁剂、浴巾(Bath Tissue)、纸巾、一次性擦拭巾、尿布疹乳膏/护臀膏、婴儿爽身粉、尿不湿、围嘴、婴儿擦拭巾、口腔护理产品、牙膏、漱口水、牙齿增白剂、义齿粘附剂、口香糖、口气清新剂、口腔可溶条、咀嚼糖、硬糖、洗手液、抗炎香油、抗炎软膏、抗炎喷雾剂、保健设备、牙线、牙刷、卫生棉塞、卫生巾、个人护理产品、防晒露、防晒喷雾剂、基于蜡的除臭剂、二醇型除臭剂、皂型除臭剂、面部乳液、身体乳液、手部乳液、爽身粉、剃须膏、浸浴用品、去角质磨砂膏、足霜、面巾、清洁擦拭巾、织物护理产品、织物柔顺剂、织物清新剂、熨烫水、液体衣物洗涤剂、液体碗碟洗涤剂、自动碗碟洗涤剂、单位剂量片剂或胶囊、增味剂、干衣机片板(drier sheet)、精制香精、固体香料、粉末粉底、液体粉底、眼影、唇膏或润唇膏、淡香水产品(Eau De Toilette product)、除臭剂、地毯除臭剂、蜡烛、房间除臭剂、消毒剂、气溶胶止汗剂,棒式止汗剂(stick antiperspirant),滚抹式止汗剂、乳液喷雾止汗剂、透明乳液棒式止汗剂、软固体止汗剂、乳液滚抹式止汗剂、透明乳液棒式止汗剂、不透明乳液棒式止汗剂、透明凝胶止汗剂、透明棒式除臭剂、喷雾除臭剂、烘烤产品、面包、干饼干、蛋糕、小甜饼、薯片、爆米花、椒盐脆饼、膨化零食、早餐谷物食品、燕麦坚果棒、预烹制的成品大米产品、含酒精的或不含酒精的饮料、香辛料调和物、汤、酱、炖菜、冷冻的主菜、酸奶、冰淇淋、豆腐、奶酪、大豆蛋白产品、肉制品、蛋制品、蛋黄酱、调味酱、调料、调味品制备物、水果制备物或蔬菜制备物。
除非另外指明,则在本文和在权利要求中提到的所有份、百分比和比例都是以重量计的。
本文公开的值和尺寸不应理解为严格限于所记载的精确数值。而是,除非另外详细说明,每个这样的值都旨在意指所记载的值和在该值附近的功能等同范围两者。例如,作为“50%”公开的值旨在意指“约50%”。
本文中的术语“胶囊”和“微胶囊”可互换地使用。
术语“g”、“mg”和“μg”分别是指“克”、“毫克”和“微克”。术语“L”和“mL”分别是指“升”和“毫升”。
本发明的一个或多个实施方案的细节在以下描述中说明。本发明的其他特征、目的和优点根据说明书和权利要求将会是明显的。
详述
已经发现,组合的带负电的粘土和阳离子聚合物可以出人意料地使微胶囊组合物稳定。
本发明的微胶囊组合物用于各种消费应用,例如个人护理产品,包括洗发剂、护发剂、染发剂、头发清新剂;个人洗涤用品,如条皂、沐浴露、个人清洁剂和消毒剂、水醇制剂;织物护理品,如织物清新剂、柔顺剂和干衣机片板(dryer sheets)、熨烫水、工业清洁剂、液体和粉状洗涤剂(包括单位剂量胶囊)、漂洗调理剂(rinse conditioner)和增味剂产品;精制香精;淡香水产品;除臭剂;滚抹式产品和气溶胶产品。
微胶囊组合物含有在稳定剂的存在下分散在水相中的微胶囊。微胶囊组合物在45℃储存时可以稳定至少4周(例如,至少6周、至少8周、4周至两年、4周至一年以及4至26周)。
通过粘度和水分离两者来测量稳定性。已知的微胶囊组合物倾向于形成凝胶,这使它们不适合用于消费品。当变成凝胶时,组合物的粘度升高至3000厘泊(cP)或甚至6000cP。如果微胶囊不凝胶出来并且具有3000cP以下的粘度,则认为其是稳定的。
稳定性的另一种测量是水从微胶囊分离的程度。最初,微胶囊组合物是乳液状分散体(即,胶体悬浮液),其中微胶囊均匀地分散在水相中。经过一定的储存时间,微胶囊可以絮凝,并且水可以从组合物分离出来。这样的分离将需要另外的过程以将组合物变成均匀的悬浮液,在此期间不期望的微胶囊爆裂和香精泄露增加。如果组合物体积的20%以下的水与组合物分离,则认为微胶囊组合物是稳定的。
以下详细描述微胶囊组合物的组分。
粘土
在本发明中可以使用任何粘土。术语“粘土”是指层状硅酸盐家族的含水层状硅酸盐,即基于二维结构的硅酸盐片,其中基础结构单元是Si(O,OH)四面体片和M(O,OH)6(M是Al3+、Mg2+、Fe3+或Fe2+)八面体片。参见Vaccari,Catalysis Today 1998,41,53-71。基于每个所占据晶胞的八面体位点的数量,粘土可以是二八面体或三八面体,而所述数量又基本上取决于八面体片中存在的阳离子M(例如,Al3+、Mg2+、Fe3+或Fe2+)。
带负电的粘土在本发明中特别有用。这些粘土含有在它们的片的至少一个表面上具有净负静电荷的细颗粒。表面电荷通常由电荷平衡离子(有时称为可交换离子,例如,钠和钙)的存在平衡,所述电荷平衡离子通常存在于粘土的层之间以及层的边缘处。
优选的带负电的粘土是2:1层状硅酸盐,其中粘土层包括夹着一个八面体片的两个四面体。实例是具有通式Al2(Si2O5)2(OH)2.nH2O或Mg3(Si2O5)2(OH)2.nH2O的蒙皂石粘土及其衍生物,例如其中铝离子中的一部分被镁离子取代,或者镁离子中的一部分被锂离子取代,和/或氢氧根离子中的一些被氟离子取代;衍生物可以包含另外的金属离子以平衡总体电荷。
本文中的术语蒙皂石粘土包括其中氧化铝存在于硅酸盐晶格中的粘土和其中氧化镁存在于硅酸盐晶格中的粘土两者。典型的蒙皂石粘土化合物包括:二八面体矿物蒙脱石、贝得石、铬蒙脱石(volchonskoites)和绿脱石,以及三八面体矿物锂蒙脱石(hectorite)、皂石和锌蒙脱石(sauconite),特别是在晶格结构内具有碱金属离子或碱土金属离子的那些。优选的蒙皂石粘土是蒙脱石粘土。
蒙脱石粘土一般具有通式HAlSi2O6,但是具有可变的Al-Si比、可变的水量,并且通常含有可变量的可交换阳离子。这些粘土可以具有作为可交换离子的碱金属阳离子和碱土金属阳离子。实例包括钠蒙脱石和钙蒙脱石。另一种示例性蒙脱石粘土是符合经验式(OH)4Si8(Al3.34Mg0.66Na0.66)O20的组中的铝成员。膨润土和锂蒙脱石两者也是蒙脱石粘土的成员。
可商购获得的蒙脱石粘土包括德国BYK Additives&Instruments作为GELWHITE-GP、GELWHITE-H和GELWHITE-L销售的GELWHITE系列(高度纯化的蒙脱石粘土)。其他商品包括:Mineral Colloid BP、Mineral Colloid MO、Gelwhite MAS100(sc)、Gelwhite MAS101、Gelwhite MAS102、Gelwhite MAS103、Bentolite WH、Bentolite L10、Bentolite H、Bentolite L、Permont SX10A、Permont SC20和Permont HN24(Southern Clay Products,德克萨斯,USA);Bentone EW和Bentone MA(Dow Corning);Bentonite USP BL 670和Bentolite H4430(Whitaker,Clarke&Daniels);Clarit 100G1和Clarit 1100G1(来自SüdChemie AG的钙膨润土);以及Volclay 2(来自Süd Chemie AG的钠膨润土)。
可用于本发明的合成锂蒙脱石的实例包括以商品名Laponite RD、Laponite RDS、Laponite XLG、Laponite XLS、Laponite D、Laponite DF、Laponite DS、Laponite S和Laponite JS销售的那些(所有都来自Southern Clay products,德克萨斯,USA,其为Rockwood的子公司)。
在美国专利号3,862,058、3,948,790、3,954,632和4,062,647中以及在EP-A-299,575、EP-A-313,146和EP0352878B1中公开了另外的合适的蒙皂石粘土。
粘土可以如从供应商获得的那样使用,并且可以含有常规的添加剂,如例如,崩解剂(也称为胶溶剂(peptiser))和水合水。粘土可以以其天然状态或者以纯化或半纯化的形式使用,例如去除矿物杂质。
粘土的阳离子交换量(CEC)是众所周知的参数,并且可以通过完善的分析技术来确定,包括通过电渗析、通过与铵离子交换然后滴定或通过亚甲基蓝过程来确定,所有都在Grimshaw,“The Chemistry and Physics of Clays(粘土的化学和物理学)”,第264-265页,Interscience(1971)中充分描述。通常按照每100g干粘土的毫当量(meq/100g)来测量粘土的阳离子交换量。
用于本发明的优选的粘土的阳离子交换量为0.7meq/100g至150meq/100g(例如,30meq/100g至100meq/100g)。
粘土的基于体积的中值粒径(D0.5)优选为0.001μm至80μm(例如,0.01μm至50μm,0.02μm至20μm,以及0.05μm至5μm)。粒径可以使用Malvern Mastersizer(MalvernInstruments,UK)来确定。
粘土颗粒中的硅酸盐层的永久电荷来源于同晶取代。然而,取代程度在层与层之间在特定范围内变化,使得层间阳离子密度也在层间空间与层间空间之间变化,并且还可以在平行于层的方向上变化(不均匀的电荷分布)。层间阳离子密度的分布可以通过如在Mermut和Lagaly,Clays and Clay Minerals 49(2001),393–397中描述的烷基铵法容易地确定。蒙脱石粘土的平均层电荷为0.2至0.4eq/式单位(Si,Al)4O10。一些蒙脱石粘土具有在0.3eq/式单位附近的平均层电荷。表面电荷可以在0.01至2库伦/m2(“Cm-2”)(例如0.02至1Cm-2以及0.05至0.5Cm-2)的范围内。
总组合物中的粘土的水平优选为总组合物的0.01重量%至10重量%(例如,0.05重量%至2重量%,0.05%至1%,0.1%至0.5%,以及0.1%至0.3%)。
在本发明的组合物中,粘土有利地以分散体(例如溶胶或凝胶)的形式或作为悬浮液存在。
阳离子聚合物
合适的阳离子聚合物是阳离子聚季铵盐(在下文中“PQ”)聚合物,如以下表1中列出的那些。
表1
优选的阳离子聚合物包括:羟乙基纤维素二甲基二烯丙基氯化铵共聚物(PQ-4),丙烯酰胺和二烯丙基二甲基氯化铵的共聚物(PQ-7),丙烯酸、甲基丙烯酰胺基丙基三甲基氯化铵和丙烯酸甲酯的三元共聚物(PQ-47),及其组合。
微胶囊
可以按照本领域中已知的囊封过程来制备微胶囊。参见例如美国专利号2,800,457、3,870,542、3,516,941、3,415,758、3,041,288、5,112,688、6,329,057和6,261,483。
一类微胶囊含有囊封微胶囊芯的微胶囊壁,其中所述微胶囊壁由囊封聚合物形成,并且所述微胶囊芯含有活性材料。另一种类型的微胶囊是所谓的可重载的微胶囊,其中所述微胶囊芯含有牺牲溶剂并且不含活性材料。
形成壁的材料(即,囊封聚合物)包括:三聚氰胺甲醛、聚氨酯、聚硅氧烷、聚脲、聚酰胺、聚酰亚胺、聚乙烯醇、聚酐、聚烯烃、聚砜、多糖、蛋白质、多肽、聚丙交酯(PLA)、聚乙交酯(PGA)、聚原酸酯、聚磷腈、有机硅、脂质、改性纤维素、树胶、聚苯乙烯、聚酯、聚醚及这些材料的组合。起作用的其他聚合物材料是乙烯马来酸酐共聚物、苯乙烯马来酸酐共聚物、乙烯乙酸乙烯酯共聚物和丙交酯乙交酯共聚物。来源于藻酸盐、壳聚糖、胶原蛋白、糊精、明胶和淀粉的生物聚合物也可以用作囊封材料。另外,胶囊可以通过明胶的简单或复杂凝聚制成。优选的囊封壁聚合物包括由异氰酸酯、丙烯酸酯、丙烯酰胺、丙烯酸酯-共-丙烯酰胺、水凝胶单体、溶胶-凝胶前体、明胶、三聚氰胺-甲醛或脲-甲醛缩合物形成的那些,以及相似类型的氨基塑料。
作为非限制性实例,以下描述某些具体囊封聚合物。
1.1聚脲/聚氨酯胶囊
聚脲胶囊各自具有由囊封聚合物形成的微胶囊壁,该囊封聚合物是多异氰酸酯和多胺/多元醇的聚合反应产物。参见WO 2004/054362;EP 0 148149;EP 0 017 409B1;美国专利号4,417,916、4,124,526、4,285,720、4,681,806、5,583,090、6,340,653 6,566,306、6,730,635、8,299,011、WO 90/08468和WO 92/13450。另外,囊封聚合物也可以使用羰基交联剂和多胺/多元醇来制备。
1.1.1多异氰酸酯
多异氰酸酯各自含有两个以上的异氰酸酯(-NCO)基团。合适的多异氰酸酯包括,例如,1,5-萘二异氰酸酯,4,4’-二苯基甲烷二异氰酸酯(MDI),氢化MDI(H12MDI),苯二亚甲基二异氰酸酯(XDI),四甲基苯二亚甲基二异氰酸酯(TMXDI),4,4’-二苯基二甲基甲烷二异氰酸酯,二和四烷基二苯基甲烷二异氰酸酯,4,4’-二苄基二异氰酸酯,1,3-苯二异氰酸酯,1,4-苯二异氰酸酯,甲苯二异氰酸酯(TDI)的异构体,任选地在混合物中,1-甲基-2,4-二异氰酸基环己烷,1,6-二异氰酸基-2,2,4-三甲基己烷,1,6-二异氰酸基-2,4,4-三甲基己烷,1-异氰酸基甲基-3-异氰酸基-1,5,5-三甲基环己烷,氯化和溴化的二异氰酸酯,含磷的二异氰酸酯,4,4’-二异氰酸基苯基全氟乙烷,四甲氧基丁烷1,4-二异氰酸酯,丁烷1,4-二异氰酸酯,己烷1,6-二异氰酸酯(HDI),二环己基甲烷二异氰酸酯,环己烷1,4-二异氰酸酯,亚乙基二异氰酸酯,邻苯二甲酸双异氰酸基乙基酯,以及具有反应性卤原子的多异氰酸酯,如1-氯甲基苯基2,4-二异氰酸酯、1-溴甲基苯基2,6-二异氰酸酯和3,3-双氯甲基醚4,4’-联苯基二异氰酸酯。含硫多异氰酸酯例如通过使六亚甲基二异氰酸酯与硫二甘醇或二羟基二己基硫化物反应来获得。另外的合适的二异氰酸酯是三甲基六亚甲基二异氰酸酯、1,4-二异氰酸基丁烷、1,2-二异氰酸基十二烷、二聚体脂肪酸二异氰酸酯及其组合。
其他合适的可商购获得的多异氰酸酯包括:LUPRANATE M20(PMDI,可由巴斯夫(BASF)商购获得,含有31.5重量%的异氰酸酯基团“NCO”),其中平均的n是0.7;PAPI 27(可由陶氏化学(Dow Chemical)商购获得的具有340的平均分子量并且含有31.4重量%的NCO的PMDI),其中平均的n是0.7;MONDUR MR(含有31重量%以上的NCO的PMDI,可由拜耳(Bayer)商购获得),其中平均的n是0.8;MONDUR MR Light(含有31.8重量%的NCO的PMDI,可由拜耳商购获得),其中平均的n是0.8;MONDUR 489(可由拜耳商购获得的含有30-31.4重量%的NCO的PMDI),其中平均的n是1.0;聚[(苯基异氰酸酯)-共-甲醛](奥德里奇化学,密尔沃基,WI(Aldrich Chemical,Milwaukee,WI)),其他异氰酸酯单体,如DESMODUR N3200(可由拜耳商购获得的聚(六亚甲基二异氰酸酯)),和TAKENATE D110-N(可由三井化学株式会社,Rye Brook,NY(Mitsui Chemicals corporation,Rye Brook,NY)商购获得的二甲苯二异氰酸酯加成聚合物,含有11.5重量%的NCO)、DESMODUR L75(可由拜耳商购获得的基于甲苯二异氰酸酯的多异氰酸酯)和DESMODUR IL(可由拜耳商购获得的基于甲苯二异氰酸酯的另一种多异氰酸酯)。
在一些实施方案中,用于制备本发明的胶囊的多异氰酸酯是单一多异氰酸酯。在其他实施方案中,多异氰酸酯是多异氰酸酯的混合物。在一些实施方案中,多异氰酸酯的混合物包括脂族多异氰酸酯和芳族多异氰酸酯。在特别的实施方案中,多异氰酸酯的混合物是六亚甲基二异氰酸酯的缩二脲和苯二亚甲基二异氰酸酯的三羟甲基丙烷加合物。在某些实施方案中,多异氰酸酯是脂族异氰酸酯或脂族异氰酸酯的混合物,不含任何芳族异氰酸酯。换言之,在这些实施方案中,不使用芳族异氰酸酯制备作为胶囊壁材料的聚脲/聚氨酯聚合物。
某些合适的多异氰酸酯的平均分子量从250至1000Da并且优选从275至500Da变化。通常,多异氰酸酯浓度的范围从0.1%至10%、优选从0.1%至8%、更优选从0.2至5%并且甚至更优选从1.5%至3.5%变化,所有都基于胶囊递送系统的重量。
合适的多异氰酸酯的更多实例可以在WO 2004/054362;WO 2015/023961;EP 0148149;EP 0 017 409B1;美国专利号4,417,916、美国专利号4,124,526、美国专利号5,583,090、美国专利号6,566,306、美国专利号6,730,635、PCT 90/08468、PCT WO 92/13450、美国专利号4,681,806、美国专利号4,285,720和美国专利号6,340,653中得到。
1.1.2羰基交联剂
羰基交联剂各自具有至少两个官能团,例如第一官能团和第二官能团。
第一官能团是对多官能胺或多官能醇具有反应性的亲电子基团,以形成囊封聚合物的网络。实例包括甲酰基、酮基(keto)、羧基、羧酸酯基团、酰基卤基团、酰胺基团、酸酐基团、烷基卤基团、环氧基团、氮杂环丙烷(aziridine)基团、氧杂环丁烷(oxetane)基团、氮杂环丁烷(azetidine)基团、磺酰卤基团、氯磷酸酯基团、异氰酸酯基团、α,β-不饱和羰基、α,β-不饱和腈基团或α,β-不饱和甲磺酰基。优选地,第一官能团是含有羰基的羰基亲电子基团,如甲酰基、酮基、羧基、羧酸酯基团、酰基卤基团、酰胺基团、酸酐基团、α,β-不饱和羰基、三氟甲磺酸酯基和对甲苯磺酸酯基。
第二官能团是对多官能胺或多官能醇具有反应性的亲电子基团。它可以选自如上所列出的基团。
羰基交联剂的实例包括:戊二醛、丁二醛(succinic dialdehyde)和乙二醛;以及化合物如乙醛酰基三聚体和多聚甲醛、双(二甲基)缩醛、双(二乙基)缩醛、聚二醛,诸如氧化淀粉。优选地,交联剂是低分子量、双官能的醛,诸如乙二醛、1,3-丙二醛、1,4-丁二醛、1,5-戊二醛或1,6-己烷。
1.1.3多官能胺
合适的多官能胺包括WO 2015/023961中描述的那些。实例是六亚甲基二胺、六亚乙基二胺、乙二胺、1,3-二氨基丙烷、1,4-二氨基-丁烷、二亚乙基三胺、五亚乙基六胺、双(3-氨基丙基)胺、双(六亚甲基)三胺、三(2-氨基乙基)胺、三亚乙基-四胺、N,N′-双(3-氨基丙基)-1,3-丙二胺、四亚乙基五胺、氨基-2-甲基-1-丙醇、壳聚糖、1,3-二氨基-胍、1,1-二甲基双胍、胍、精氨酸、赖氨酸、组氨酸、鸟氨酸、乳酸链球菌肽、明胶及其组合。
其他合适的多胺包括聚乙烯亚胺和支化的聚乙烯亚胺(“BPEI”)。代表性的BPEI结构如下所示:
其中n为1至20,000(例如,1至10,000、2至5,000和2至1,000)的整数。用于本发明的BPEI优选地具有500至5,000,000道尔顿(例如,500至1,000,000道尔顿、750至500,000道尔顿、750至100,000道尔顿、750至50,000道尔顿和10,000至50,000)的分子量。
BPEI可从Sigma-Aldrich(St.Louis,MO;平均分子量25,000道尔顿)和Polysciences Inc.(Warrington,PA;分子量为600、1200、1800、10,000、70,000、750,000、250,000和2,000,000道尔顿的多种产品)商购获得。
1.1.4多官能醇
WO 2015/023961中还描述了合适的多官能醇。实例包括季戊四醇、二季戊四醇、甘油、聚甘油、乙二醇、聚乙二醇、三羟甲基丙烷、新戊二醇、山梨糖醇、赤藓糖醇、苏糖醇、阿拉伯糖醇、木糖醇、核糖醇、甘露糖醇、半乳糖醇、岩藻糖醇、艾杜糖醇(iditol)、肌醇、庚七醇(volemitol)、异麦芽糖醇(isomalt)、麦芽糖醇、乳糖醇、麦芽三糖醇(maltotriitol)、麦芽四糖醇(maltotetraitol)、聚葡萄糖糖醇(polyglycitol)及其组合。
1.2氨基塑料(Aminoplast)和明胶微胶囊
用于氨基塑料囊封的代表性工艺披露于US 2007/0078071,但是已意识到关于材料和工艺步骤的许多变形是可能的。另一种囊封工艺,即明胶囊封,披露于US 2,800,457。两种工艺分别在用于美国专利号4,145,184和5,112,688的消费品中的香精囊封的情形进行了讨论。聚合物系统在本领域是熟知的并且这些的非限制性实例包括:如在申请GB2006709 A中披露的氨基塑料胶囊和囊封粒子;如在US 4,396,670中披露的具有壁的微胶囊的生产,所述壁包含与三聚氰胺-甲醛预缩合物反应的苯乙烯-马来酸酐;如在US 5,089,339中披露的与三聚氰胺-甲醛树脂交联的丙烯酸-丙烯酰胺共聚物;如在US 5,401,577中披露的由阳离子三聚氰胺-甲醛缩合物构成的胶囊;如在US 3,074,845中披露的三聚氰胺甲醛微囊封;酰胺基-醛树脂原位聚合的胶囊(参见EP 0 158 449 A1);醚化的脲-甲醛聚合物(参见US 5,204,185);如描述于US4,525,520中的三聚氰胺-甲醛微胶囊;如描述于US 5,011,634中的交联的油溶性三聚氰胺-甲醛预缩合物;如在US 5,013,473中披露的由阳离子和阴离子三聚氰胺-甲醛预缩合物(其随后发生交联)的复合物形成的胶囊壁材料;如在US3,516,941中披露的由加成聚合物如缩合聚合物、酚醛、脲醛或丙烯酸聚合物制成的聚合物壳;如在EP 0 443 428 A2中披露的脲-甲醛胶囊;如在GB 2 062 570 A中披露的三聚氰胺-甲醛化学;以及如在US 4,001,140中披露的,由以酸或盐形式的苯乙烯磺酸的聚合物或共聚物构成的胶囊,和与三聚氰胺-甲醛交联的胶囊。
脲-甲醛和三聚氰胺-甲醛预缩合物微胶囊壳壁前体通过使脲或三聚氰胺与甲醛反应来制备,其中三聚氰胺或脲与甲醛的摩尔比在约10:1至约1:6、优选约1:2至约1:5的范围内。对于实施本发明的目的,所得的材料具有在156至3000范围内的分子量。所得的材料可以‘按照原样’用作用于前述取代或未取代丙烯酸聚合物或共聚物的交联剂,或者它可以进一步与C1-C6醇,例如,甲醇、乙醇、2-丙醇、3-丙醇、1-丁醇、1-戊醇或1-己醇反应,由此形成部分醚,其中三聚氰胺/脲:甲醛:醇的摩尔比在1:(0.1-6):(0.1-6)的范围内。所得的含醚部分的产物可以‘按照原样’用作用于前述取代或未取代丙烯酸聚合物或共聚物的交联剂,或者它可以自身缩合以形成二聚体、三聚体和/或四聚体,其也可以用作用于前述取代或未取代丙烯酸聚合物或共聚物的交联剂。用于形成这样的三聚氰胺-甲醛和脲-甲醛预缩合物的方法在美国专利号3,516,846和6,261,483以及Lee等(2002)J.Microencapsulation19,559-569中提出。
可用于本发明实践中的脲-甲醛预缩合物的实例是URAC 180和URAC 186,其是Wilmington,DE的Cytec Technology Corp.的商标。可用于本发明实践中的三聚氰胺-甲醛预缩合物的实例包括,但不限于,CYMEL U-60、CYMEL U-64和CYMEL U-65,其是Wilmington,DE的Cytec Technology Corp.的商标。作为用于交联的预缩合物,优选使用取代或未取代丙烯酸聚合物或共聚物。在实施本发明中,脲-甲醛预缩合物/三聚氰胺-甲醛预缩合物与取代/未取代丙烯酸聚合物/共聚物的摩尔比的范围在约9:1至约1:9、优选约5:1至约1:5并且最优选约2:1至约1:2的范围内。
在一个实施方案中,也可以使用具有由伯胺和/或仲胺反应性基团或其混合物和交联剂构成的的一种或多种聚合物的微胶囊。参见US2006/0248665。胺聚合物可以具有伯胺和/或仲胺官能度并且可以为天然或合成来源的。天然来源的含胺聚合物典型地是蛋白质如明胶和白蛋白,以及一些多糖。合成胺聚合物包括各种程度的水解的聚乙烯甲酰胺、聚乙烯胺、聚烯丙胺和具有伯胺和仲胺侧基的其他合成聚合物。合适的胺聚合物的实例有可商购得自巴斯夫的聚乙烯甲酰胺的LUPAMIN系列。这些材料的分子量可以在10,000至1,000,000道尔顿的范围内。
脲-甲醛或三聚氰胺-甲醛胶囊也可以包含甲醛清除剂,其能够结合游离甲醛。当胶囊用于在含水介质中使用时,甲醛清除剂如亚硫酸钠、三聚氰胺、甘氨酸和碳酰肼(carbohydrazine)是合适的。当胶囊旨在用于具有低pH的产品,例如,织物护理调理剂中时,甲醛清除剂优选选自β二酮,如β-酮酯或选自1,3-二醇,如丙二醇。优选的β-酮酯包括烷基-丙二酸酯、乙酰乙酸烷基酯和聚乙烯醇乙酰乙酸酯。
1.3溶胶-凝胶微胶囊
溶胶-凝胶微胶囊各自具有溶胶-凝胶聚合物作为囊封聚合物。溶胶-凝胶聚合物是溶胶-凝胶前体(一种能够形成溶胶-凝胶聚合物的化合物)的聚合产物。溶胶-凝胶前体典型地是含有硅、硼、铝、钛、锌、锆和钒的那些。优选的前体是有机硅、有机硼、有机铝,包括金属醇化物和b-二酮化物(b-diketonate)及其组合。参见US 9,532,933。
1.4水凝胶微胶囊
使用可聚合材料如单官能或多官能丙烯酸或甲基丙烯酸或其酯制备水凝胶微胶囊。参见例如WO2014/011860。下面列出了可用于制备水凝胶微胶囊的示例性材料。
1.4.1单体
通过举例说明且非限制性地,优选的二或多官能乙烯基单体包括:丙烯酸、甲基丙烯酸、丙烯酸2-羟乙酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸正丁酯、丙烯酸戊酯、丙烯酸己酯、丙烯酸2-乙基己酯、丙烯酸庚酯、丙烯酸辛酯、丙烯酸壬酯、丙烯酸癸酯、丙烯酸十二烷基酯、丙烯酸十四烷基酯、丙烯酸十六烷基酯、丙烯酸异丙酯、丙烯酸异丁酯、丙烯酸仲丁酯、丙烯酸2-乙基丁酯、丙烯酸3-甲基丁酯、丙烯酸1-乙基丙酯、丙烯酸2-甲基戊酯、丙烯酸2-乙基丁酯、丙烯酸1,3-二甲基丁酯、丙烯酸1-甲基己酯、丙烯酸2-乙基己酯、丙烯酸1-甲基庚酯、丙烯酸4-乙基-1-甲基辛酯、丙烯酸4-乙基-1,1-异丁基辛酯、丙烯酸烯丙酯、丙烯酸2-甲基烯丙酯、丙烯酸1-甲基烯丙酯、丙烯酸2-丁烯酯、丙烯酸1,3-二甲基-3-二丁烯酯、丙烯酸3,7-二甲基-7-辛烯酯、丙烯酸3,7-二甲基-2,6-辛二烯酯、丙烯酸3,7-二甲基-6-辛烯酯、丙烯酸叔丁酯、二丙烯酸三甘醇酯、二甲基丙烯酸三甘醇酯、二丙烯酸二甘醇酯、二甲基丙烯酸二甘醇酯、二丙烯酸三丙二醇酯、脂族或芳族尿烷二丙烯酸酯、二官能尿烷丙烯酸酯、乙氧基化双酚二丙烯酸酯、乙氧基化双酚二甲基丙烯酸酯、乙氧基化脂族二官能尿烷甲基丙烯酸酯、乙氧基化三羟甲基丙烷三丙烯酸酯、乙氧基化季戊四醇四丙烯酸酯、二丙二醇二丙烯酸酯、脂族或芳族尿烷二甲基丙烯酸酯、环氧丙烯酸酯、环氧甲基丙烯酸酯、二甲基丙烯酸四甘醇酯、二丙烯酸四甘醇酯、聚乙二醇二甲基丙烯酸酯、聚乙二醇二丙烯酸酯、二丙烯酸1,3-丁二醇酯、二甲基丙烯酸1,3-丁二醇酯、二甲基丙烯酸1,4-丁二醇酯、二丙烯酸1,4-丁二醇酯、二丙烯酸1,6-已二醇酯、二甲基丙烯酸1,6-已二醇酯、二丙烯酸新戊二醇酯、烷氧基化已二醇二丙烯酸酯、烷氧基化环己烷二甲醇二丙烯酸酯、丙氧基化新戊二醇二丙烯酸酯、三羟甲基丙烷三甲基丙烯酸酯、三羟甲基丙烷三丙烯酸酯、三丙烯酸季戊四醇酯、丙氧基化三羟甲基丙烷三丙烯酸酯、丙氧基化甘油三丙烯酸酯、二(三羟甲基)丙烷四丙烯酸酯、五丙烯酸二季戊四醇酯等。可以使用的甲基丙烯酸的代表性酯单体包括甲基丙烯酸2-羟乙酯、甲基丙烯酸缩水甘油酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丙酯、甲基丙烯酸异丙酯、甲基丙烯酸正丁酯、甲基丙烯酸异丁酯、甲基丙烯酸仲丁酯、甲基丙烯酸叔丁酯、甲基丙烯酸正己酯、甲基丙烯酸正辛酯、甲基丙烯酸异辛酯、甲基丙烯酸癸酯、甲基丙烯酸正十二烷基酯、甲基丙烯酸正十四烷基酯、甲基丙烯酸正十六烷基酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸烯丙酯、甲基丙烯酸油烯酯、甲基丙烯酸2-丙炔酯、甲基丙烯酸2-(二甲基氨基)乙酯、甲基丙烯酸2-(二乙基氨基)乙酯、甲基丙烯酸2-(二异丙基氨基)乙酯、N-(2-氨基乙基)甲基丙烯酰胺盐酸盐、甲基丙烯酸2-氨基乙酯盐酸盐、N-(3-氨基丙基)甲基丙烯酰胺盐酸盐、甲基丙烯酸2-(叔丁基氨基)乙酯等。
上述单体可以单独使用或以各种混合物使用。多官能丙烯酸酯和甲基丙烯酸酯的使用将导致在聚合时形成交联的网络聚合物。这样的聚合物具有所需的性能,如良好的机械强度、弹性、韧性和柔性。本发明中使用的多官能丙烯酸酯和甲基丙烯酸酯的实例包括,但不限于,二甲基丙烯酸乙二醇酯(EGDMA)、三羟甲基丙烷三甲基丙烯酸酯、三羟甲基三丙烯酸酯、三丙烯酸季戊四醇酯、四丙烯酸季戊四醇酯、二甲基丙烯酸双酚A酯、二(三羟甲基丙烷)四丙烯酸酯(DTTA)、1-(丙烯酰氧基)-3-(甲基丙烯酰氧基)-2-丙醇(AOOP),三羟甲基丙烷乙氧基化三丙烯酸酯(TPETA)、五丙烯酸二季戊四醇酯、己烷二丙烯酸酯、聚(乙二醇)二甲基丙烯酸酯(PEGDMA)和二甲基丙烯酸1,6-己二醇酯(HDDMA)、二甲基丙烯酸1,4-丁二醇酯、二甲基丙烯酸1,3-丁二醇酯、二丙烯酸1,6-己二醇酯、二丙烯酸1,4-丁二醇酯、二丙烯酸1,3-丁二醇酯。
在某些实施方案中,丙烯酸或甲基丙烯酸或其酯占油相的小于25质量%、优选5至20质量%或更优选10至15质量%。
1.4.2引发剂
引发剂通常用于使聚合反应开始。实例包括但不限于:AIBN、过硫酸钠、过氧化苯甲酰和过硫酸铵。
1.5凝聚胶囊
可用于凝聚工艺的蛋白质包括白蛋白、植物球蛋白和明胶。明胶可以是例如鱼、猪、牛和/或家禽明胶。根据一个优选实施方案,蛋白质是鱼、牛或家禽明胶。根据一个更优选实施方案,蛋白质是温水鱼明胶。
可用于复杂凝聚方法中的典型非蛋白质聚合物特别地包括带负电的聚合物。例如,它们可以选自阿拉伯树胶,黄原胶,琼脂,藻酸盐,纤维素衍生物,例如羧甲基纤维素,果胶酸盐,角叉菜胶,聚丙烯酸和甲基丙烯酸,和/或其混合物。另外的合适非蛋白质可以来源于文献,例如源自WO 2004/022221。
典型地使用交联剂来使包覆层硬化。合适的交联剂包括甲醛、乙醛、戊二醛、乙二醛、铬矾或转谷氨酰胺酶。优选地,转谷氨酰胺酶以10-100,优选30-60活性单位/克明胶使用。此酶被很好描述并且是商购可得的。
1.6微胶囊形成助剂
大多数微胶囊形成助剂用作分散剂(即乳化剂或表面活性剂)。它们有助于形成待囊封的含有纳米或微米级油滴的稳定乳液。此外,微胶囊形成助剂通过稳定胶囊和/或它们向目标区域的沉积或向环境的释放来改善微胶囊的性能。性能通过使用经历期间(如洗衣经历的揉搓前和揉搓后阶段)的香精释放的强度来测定。揉搓前阶段是微胶囊已经沉积在布上的阶段,例如在洗涤循环期间已经使用含有微胶囊的织物柔顺剂之后。揉搓后阶段是在微胶囊已经沉积并且通过摩擦或其他类似机制使微胶囊破裂之后。
这些微胶囊形成助剂的量是微胶囊的约0.1至40重量百分比、更优选0.1至约10重量百分比、更优选0.1至5重量百分比中的任何一点。
优选的微胶囊形成助剂是聚乙烯吡咯烷酮、聚乙烯醇、聚(磺苯乙烯)、羧甲基纤维素、萘磺酸盐/酯缩合物的钠盐、乙烯和马来酸酐的共聚物、藻酸盐、透明质酸、聚(丙烯酸)、羧甲基纤维素、丙烯酸和丙烯酰胺的共聚物、丙烯酰胺和丙烯酰胺基丙基三甲基氯化铵(acrylamidopropyltrimonium chloride)的共聚物、(丙烯酸、丙烯酰胺和丙烯酰胺基丙基三甲基氯化铵)的三元共聚物、部分或完全水解的聚乙酸乙烯酯聚合物(即聚乙烯醇)及其组合。
其他微胶囊形成助剂包括以下的水溶性盐:烷基硫酸盐、烷基醚硫酸盐、烷基异硫代硫酸盐(alkyl isothionates)、烷基羧酸盐、烷基磺基琥珀酸盐、烷基琥珀酰胺酸盐(alkyl succinamates)、烷基硫酸盐如十二烷基硫酸钠、烷基肌氨酸盐、蛋白质水解产物的烷基衍生物、酰基天冬氨酸盐、烷基或烷基醚或烷基芳基醚磷酸酯、十二烷基硫酸钠、磷脂或卵磷脂、或皂、硬脂酸钠、硬脂酸钾或硬脂酸铵、油酸盐或棕榈酸盐、烷基芳基磺酸盐如十二烷基苯磺酸钠、二烷基磺基琥珀酸酯钠、二辛基磺基琥珀酸盐、二月桂基磺基琥珀酸酯钠、聚(苯乙烯磺酸)钠盐、异丁烯-马来酸酐共聚物、阿拉伯树胶、藻酸钠、纤维素硫酸盐和果胶、异丁烯-马来酸酐共聚物、阿拉伯树胶、角叉菜胶、藻酸钠、果胶酸、黄蓍胶、杏仁胶和琼脂;半合成聚合物如硫酸化纤维素、硫酸化甲基纤维素、羧甲基淀粉、磷酸化淀粉、木质素磺酸;和合成聚合物如马来酸酐共聚物(包括其水解产物)、聚丙烯酸、聚甲基丙烯酸、丙烯酸-丙烯酸丁酯共聚物或巴豆酸均聚物和共聚物、乙烯基苯磺酸或2-丙烯酰胺-2-甲基丙磺酸均聚物和共聚物、以及此类聚合物和共聚物的部分酰胺或部分酯、羧基改性的聚乙烯醇、磺酸改性的聚乙烯醇和磷酸改性的聚乙烯醇、磷酸化或硫酸化的三苯乙烯基苯酚乙氧基化物。
可商购获得的表面活性剂包括,但不限于,磺化的萘-甲醛缩合物,如MORWET D425(烷基萘磺酸盐/酯甲醛缩合物的钠盐,Akzo Nobel,Fort Worth,TX);部分水解的聚乙烯醇,如MOWIOL,例如MOWIOL 3-83(Air Products)、Ultalux FP、Ultalux FA、Ultalux AD、Selvol 203(Sekisui)、OKS-8089(Sourus);环氧乙烷-环氧丙烷嵌段共聚物或泊洛沙姆,如PLURONIC、SYNPERONIC或PLURACARE材料(巴斯夫);磺化的聚苯乙烯,如FLEXAN II(AkzoNobel);乙烯-马来酸酐聚合物,如ZEMAC(Vertellus Specialties Inc.);丙烯酰胺和丙烯酰胺基丙基三甲基氯化铵的共聚物,如Salcare SC 60(巴斯夫);和聚季铵盐系列,如聚季铵盐11(“PQ11”;乙烯吡咯烷酮和季铵化的甲基丙烯酸二甲基氨基乙酯的共聚物;由巴斯夫作为LUVIQUAT PQ11AT 1销售)。表面活性剂MOWIOL 3-83的粘度为2-4mPa·S(例如,3mPa·S),水解度为80-85%(例如,83%),酯值为170-210mg KOH/g(例如,190mg KOH/g),并且残留未水解乙酰含量为13-18%(例如,15%)。
在其他实施方案中,胶囊形成助剂是加工助剂,如水胶体,其改善浆料针对凝聚、沉降和乳状分层(creaming)的胶体稳定性。术语“水胶体”是指广义类的具有阴离子的、阳离子的、两性离子的或非离子的特征的水溶性或水可分散性聚合物。可用于本发明的水胶体包括但不限于多糖,如淀粉、改性淀粉、糊精、麦芽糖糊精和纤维素衍生物、以及它们的季铵化形式;天然树胶,如藻酸酯、角叉菜胶、黄原胶(xanthanes)、琼脂、果胶(pectines)、果胶酸和天然树胶如阿拉伯树胶、黄蓍胶和刺梧桐胶、瓜尔胶和季铵化的瓜尔胶;明胶(gelatine)、蛋白质水解产物和它们的季铵化形式;合成的聚合物和共聚物,如聚(乙烯吡咯烷酮-共-乙酸乙烯酯)、聚(乙烯醇-共-乙酸乙烯酯)、聚((甲基)丙烯酸)、聚(马来酸)、聚((甲基)丙烯酸烷基酯-共-(甲基)丙烯酸)、聚(丙烯酸-共-马来酸)共聚物、聚(氧化烯烃)、聚(乙烯基甲基醚)、聚(乙烯基醚-共-马来酸酐)等,以及聚-(乙烯亚胺)、聚((甲基)丙烯酰胺)、聚(氧化烯烃-共-二甲基硅氧烷)、聚(氨基-二甲基硅氧烷)、Ultrez 20(丙烯酸酯/C10-30丙烯酸烷基酯交联聚合物)、Ultrez30(环己烷和乙酸乙酯共溶剂系统中聚合的丙烯酸的交联均聚物)、Aculyn Excel(丙烯酸酯共聚物)、Carbopol 981(卡波姆)等,以及它们的季铵化形式。
胶囊形成助剂在加工期间还可以与羧甲基纤维素(“CMC”)、聚乙烯吡咯烷酮、聚乙烯醇、烷基萘磺酸盐/酯甲醛缩合物和/或表面活性剂组合使用以促进胶囊形成。可以与胶囊形成助剂组合使用的表面活性剂的实例包括但不限于鲸蜡基三甲基氯化铵(CTAC),泊洛沙姆,如PLURONICS(例如,PLURONIC F127)、PLURAFAC(例如,PLURAFAC F127)或MIRANET-N,皂苷,如QNATURALE(National Starch Food Innovation);或阿拉伯树胶,如Seyal或Senegal。在某些实施方案中,CMC聚合物具有在约90,000道尔顿至1,500,000道尔顿之间、优选在约250,000道尔顿至750,000道尔顿之间、并且更优选在400,000道尔顿至750,000道尔顿之间的分子量范围。CMC聚合物具有在约0.1至约3之间、优选在约0.65至约1.4之间、并且更优选在约0.8至约1.0之间的取代度。CMC聚合物以约0.1%至约2%、并且优选约0.3%至约0.7%的水平存在于胶囊浆料中。在其他实施方案中,本发明中使用的聚乙烯吡咯烷酮是水溶性聚合物,并且具有1,000至10,000,000的分子量。合适的聚乙烯吡咯烷酮是聚乙烯吡咯烷酮K12、K15、K17、K25、K30、K60、K90或其混合物。聚乙烯吡咯烷酮的量为胶囊递送系统的2-50重量%、5-30重量%或10-25重量%。可商购的烷基萘磺酸盐/酯甲醛缩合物包括MORWET D-425,它是Akzo Nobel,Fort Worth,TX的萘磺酸盐/酯缩合物的钠盐。
在食品中,使用食品级分散剂。术语“食品级分散剂”是指具有适合人类食用的质量的分散剂。它们可以是天然或非天然产物。天然产物或表面活性剂是指天然存在的并且来自天然来源的产物。天然产物/表面活性剂包括它们的衍生物,其可以使用天然酶或微生物进行盐化、脱盐、去油、分级或改性。另一方面,非天然表面活性剂是通过不涉及酶改性的化学方法化学合成的表面活性剂。
天然分散剂包括皂树皂苷、卵磷脂、阿拉伯树胶、果胶、角叉菜胶、壳聚糖、硫酸软骨素、纤维素胶、改性淀粉、乳清蛋白、豌豆蛋白、卵清蛋白、丝蛋白、鱼明胶、猪源或牛源蛋白、酯树胶、脂肪酸及其组合。
非天然分散剂包括N-月桂酰基-L-精氨酸乙酯、脱水山梨糖醇酯、聚乙氧基化脱水山梨糖醇酯、聚甘油酯、脂肪酸酯及其组合。
其他食品安全分散剂也可包括在本发明的微胶囊中。实例包括铵磷酯(ammoniumphosphatide)、甘油单酯和甘油二酯的乙酸酯(Acetem)、脂肪酸的甘油单酯和甘油二酯的乳酸酯(Lactem)、脂肪酸的甘油单酯和甘油二酯的柠檬酸酯(Citrem)、脂肪酸的甘油单酯和甘油二酯的单和二乙酰酒石酸酯(Datem)、脂肪酸甘油单酯的琥珀酸酯(SMG)、乙氧基化甘油单酯、脂肪酸蔗糖酯、蔗糖甘油酯(sucroglyceride)、聚蓖麻油酸聚甘油酯、脂肪酸的丙烷-1,2-二醇酯、与脂肪酸的甘油单酯或甘油二酯相互作用的热氧化大豆油、硬脂酰乳酸钠(SSL)、硬脂酰乳酸钙(CSL)、硬脂酰酒石酸酯、酯交换蓖麻油酸的聚甘油酯(E476)、硬脂酰乳酸钠(sodium stearoyllatylate)、十二烷基硫酸钠、聚氧乙烯化氢化蓖麻油(例如,以商品名CREMO-PHOR销售的)、环氧乙烷和环氧丙烷的嵌段共聚物(例如,以商品名PLURONIC或商品名POLOXAMER销售的)、聚氧乙烯脂肪醇醚和聚氧乙烯硬脂酸酯。
1.7另外的壁聚合物
囊封聚合物还可以包括一种或多种另外的壁聚合物,例如第二、第三、第四、第五或第六聚合物。另外的聚合物可以选自由以下组成的组:二氧化硅、聚丙烯酸酯、聚丙烯酰胺、聚(丙烯酸酯-共-丙烯酰胺)、聚脲、聚氨酯、淀粉、明胶和阿拉伯树胶、聚(三聚氰胺-甲醛)、聚(脲-甲醛)及其组合。
1.8囊封方法
常规囊封方法可以用于制备微胶囊。参见WO 2015/023961。
通过举例说明,为了制备具有聚脲囊封聚合物的微胶囊,首先制备含有以下的水包油乳液:(i)多胺、多元醇或其混合物,(ii)多异氰酸酯、羰基交联剂或其混合物,(iii)具有亲水性芯溶剂和疏水性芯溶剂的油相,和(iv)具有微胶囊形成助剂和水的水相。当提高反应混合物的温度或向混合物中加入催化剂(如用于催化酰胺形成的转谷氨酰胺酶)时,发生多胺/多元醇与多异氰酸酯/羰基交联剂之间的反应。
适合用于聚脲/聚氨酯形成的催化剂是转谷氨酰胺酶、金属碳酸盐、金属氢氧化物、氨基或有机金属化合物,并且包括例如碳酸钠、碳酸铯、碳酸钾、氢氧化锂、1,4-二氮杂双环[2.2.2]辛烷(即DABCO)、N,N-二甲基氨基乙醇、N,N-二甲基环己基胺、双-(2-二甲基氨基-乙基)醚、N,N二甲基乙酰胺、辛酸锡和二月桂酸二丁基锡。
然后将所得微胶囊浆料在预定温度下固化预定时间。
根据一些实施方案,根据上述方法制备的微胶囊在例如15℃至230℃(例如,55℃至90℃、55℃至75℃和90℃至130℃)的范围内的温度下固化1分钟至10小时(例如,0.1小时至5小时、0.2小时至4小时和0.5小时至3小时)。本领域技术人员无需过度实验就可以确定固化温度、持续时间和加热速率。
为了获得具有更多浸出的活性材料的微胶囊,本发明的某些实施方案提供在低温(例如,低于100℃)下的固化。在一些实施方案中,固化温度是90℃以下。在其他实施方案中,固化温度是80℃以下。
在一个实施方案中,将胶囊在1至60分钟(例如,1至30分钟)的时间段内以0.5至2℃/分钟的线性速率(例如,1至5℃/分钟、2至8℃/分钟和2至10℃/分钟)加热至目标固化温度。可以使用以下加热方法:例如通过油传导,通过红外线的蒸汽辐射,和微波,通过加热空气的对流,蒸汽注入和本领域技术人员已知的其他方法。本文中使用的目标固化温度是指胶囊可以固化以延迟浸出的最低温度(摄氏度)。
2.活性材料
本发明的微胶囊组合物在外部亲水性溶剂中具有一种或多种活性材料。非限制性实例包括WO 2016/049456中描述的那些。这些活性材料包括香料或香精成分、掩味剂、味觉感知剂(taste sensate)、恶臭中和剂、维生素、抗菌剂、遮光剂活性成分(sunscreenactive)、抗氧化剂、抗炎剂、麻醉剂、止痛剂、抗真菌剂、抗生素、抗病毒剂、抗寄生虫剂、抗感染剂和祛痘剂、皮肤活性成分、酶和辅酶、皮肤增白剂、抗组胺剂、化疗剂和驱昆虫剂。除上面列出的活性材料以外,本发明的产品还可以含有染料、着色剂或颜料:天然获得的提取物(例如辣椒粉提取物和黑胡萝卜提取物);和铝色淀。本发明的微胶囊组合物特别适用于囊封含有一种或多种醛、胺和/或醇的香精。醛/胺/醇可以与形成微胶囊壁的材料(如多异氰酸酯、硅酸盐、丙烯酸酯等)反应。
在一些实施方案中,微胶囊组合物中的活性材料的量按组合物的重量计为0.1至95%(例如,1至90%、2%至80%、4至70%和5至50%)。胶囊壁的量按胶囊的重量计为10至98%(例如,20至95%、30至90%和50至80%)。微胶囊芯的量(亲水性和疏水性芯溶剂的总和)按胶囊的重量计为2至90%(例如,5至80%、10至70%和20至50%)。
在一些微胶囊组合物中,胶囊和活性材料之间的比率为4:1至40:1(例如,5:1至30:1和6:1至20:1)。
3.辅助材料
除了活性材料之外,本发明还考虑了在由胶囊壁囊封的芯中掺入辅助材料,包括溶剂、软化剂和芯改性剂材料。其他辅助材料是纳米级固体颗粒材料、聚合物芯改性剂、溶解度调节剂、密度调节剂、稳定剂、润湿剂、粘度调节剂、pH调节剂或其任意组合。这些改性剂可以在胶囊的壁或芯中存在或者在递送系统中的胶囊外部存在。优选地,它们作为芯改性剂在芯中。
一种或多种辅助材料可以按胶囊的重量计以0.01%至25%(例如,0.5%至10%)的量添加。
合适的实例包括在WO 2016/049456和US 2016/0158121中描述的那些。
4.沉积助剂
按胶囊的重量计,可以包含0.01至25%(下限为0.01%、0.1%、0.2%、0.5%、1%、2%和5%,并且上限为25%、20%、15%、10%、8%、5%和3%)、更优选5至20%的胶囊沉积助剂。胶囊沉积助剂可以在胶囊的制备期间添加或者其可以在已经制备胶囊之后添加。
使用这些沉积助剂以有助于胶囊至表面如织物、毛发或皮肤的沉积。这些包括阴离子、阳离子、非离子或两性水溶性聚合物。合适的沉积助剂包括聚季铵盐(polyquaternium)-4、聚季铵盐-5、聚季铵盐-6、聚季铵盐-7、聚季铵盐-10、聚季铵盐-16、聚季铵盐-22、聚季铵盐-24、聚季铵盐-28、聚季铵盐-39、聚季铵盐-44、聚季铵盐-46、聚季铵盐-47、聚季铵盐-53、聚季铵盐-55、聚季铵盐-67、聚季铵盐-68、聚季铵盐-69、聚季铵盐-73、聚季铵盐-74、聚季铵盐-77、聚季铵盐-78、聚季铵盐-79、聚季铵盐-80、聚季铵盐-81、聚季铵盐-82、聚季铵盐-86、聚季铵盐-88、聚季铵盐-101、聚乙烯胺、聚乙烯亚胺、聚乙烯胺和乙烯甲酰胺(vinylformamide)共聚物、丙烯酰胺基丙基三甲基氯化铵/丙烯酰胺共聚物、甲基丙烯酰胺基丙基三甲基氯化铵/丙烯酰胺共聚物及其组合。其他合适的沉积助剂包括在WO 2016049456第13-27页中描述的那些。US 2013/0330292、US 2013/0337023和US 2014/0017278中描述了另外的沉积助剂。
5.微胶囊递送系统制剂
微胶囊可以配制成用于消费品的胶囊递送系统(例如,微胶囊组合物)。
胶囊递送系统可以是在外部亲水性溶剂(例如,水、乙醇及其组合)中含有按胶囊递送系统的重量计0.1至80%(例如,70-75%、40-55%、50-90%、1-65%和5-45%)水平的胶囊的浆料。
在一些实施方案中,随后纯化根据本发明制备的胶囊及其浆料。参见US 2014/0017287。可以通过用水洗涤胶囊浆料直至达到中性pH来实现纯化。
6.另外的组分
胶囊递送系统也可以含有一种或多种其他递送系统如聚合物辅助递送组合物(参见US 8,187,580)、纤维辅助递送组合物(US 2010/0305021)、环糊精主客体复合物(US 6,287,603和US 2002/0019369)、前香精(WO 2000/072816和EP 0 922 084),及其任意组合。胶囊递送系统还可以含有一种或多种(例如,两种、三种、四种、五种或六种以上)不同的胶囊,包括本发明的不同胶囊和其他胶囊,如氨基塑料、水凝胶、溶胶-凝胶、聚脲/聚氨酯胶囊和三聚氰胺甲醛胶囊。可以结合的更多示例性递送系统是凝聚胶囊(参见WO 2004/022221)和环糊精递送系统(参见WO 2013/109798和US 2011/03085560)。
以上讨论的任何化合物、聚合物或试剂可以是如以上所示的化合物、聚合物或试剂本身,或者其盐、前体、水合物或溶剂化物。盐可以在阴离子和化合物、聚合物或试剂上的带正电基团之间形成。合适的阴离子包括氯离子、溴离子、碘离子、硫酸根、硝酸根、磷酸根、柠檬酸根、甲磺酸根、三氟乙酸根、乙酸根、苹果酸根、甲苯磺酸根、酒石酸根、富马酸根、谷氨酸根、葡糖醛酸根、乳酸根、戊二酸根和马来酸根。同样地,盐也可以在阳离子和化合物、聚合物或试剂上的带负电基团之间形成。合适的阳离子包括钠离子、钾离子、镁离子、钙离子和铵阳离子(例如,四甲基铵离子)。前体可以是酯和另外的合适衍生物,其在制备本发明的聚脲或聚氨酯胶囊组合物的过程期间能够转化为所述化合物、聚合物或试剂并且用于制备聚脲或聚氨酯胶囊组合物。水合物是指含有水的化合物、聚合物或试剂。溶剂化物是指在化合物、聚合物或试剂和合适溶剂之间形成的复合物。合适的溶剂可以是水、乙醇、异丙醇、乙酸乙酯、乙酸和乙醇胺。
某些化合物、聚合物和试剂具有一个或多个立体中心,其每一个可以为R或S构型或混合物。此外,一些化合物、聚合物和试剂具有一个或多个双键,其中各个双键以E(反式)或Z(顺式)构型或其组合存在。所述化合物、聚合物和试剂包括所有可能的构型立体异构体、位置异构体、非对映异构体、对映异构体和差向异构体形式以及其任意混合物。这样,本文中使用的赖氨酸包括L-赖氨酸、D-赖氨酸、L-赖氨酸单盐酸盐、D-赖氨酸单盐酸盐、赖氨酸碳酸盐等。类似地,精氨酸包括L-精氨酸、D-精氨酸、L-精氨酸单盐酸盐、D-精氨酸单盐酸盐、精氨酸碳酸盐、精氨酸一水合物等。胍包括胍盐酸盐、胍碳酸盐、胍硫氰酸盐、以及其他胍盐,包括其水合物。鸟氨酸包括L-鸟氨酸及其盐/水合物(例如,单盐酸盐)和D-鸟氨酸及其盐/水合物(例如,单盐酸盐)。
7.应用
本发明的递送系统良好适合于但不限于在以下产品中使用:
a)家居产品
i.可以利用本发明的液体或粉末衣物洗涤剂包括在美国专利号5,929,022、5,916,862、5,731,278、5,565,145、5,470,507、5,466,802、5,460,752、5,458,810、5,458,809、5,288,431、5,194,639、4,968,451、4,597,898、4,561,998、4,550,862、4,537,707、4,537,706、4,515,705、4,446,042和4,318,818中描述的那些体系。
ii.单位剂量小袋、片剂和胶囊,如在EP 1 431 382 A1、US 2013/0219996 A1、US2013/0284637 A1和US 6,492,315中描述的那些。这些单位剂量制剂可以含有高浓度的功能材料(例如,5-100%织物柔软剂或洗涤剂活性成分)、香精(例如,0.5-100%、0.5-40%和0.5-15%)和香料(例如,0.1-100%、0.1-40%和1-20%)。它们可以不含有水以将水含量限制为低至小于30%(例如,小于20%,小于10%和小于5%)。
iii.增味剂(Scent Booster)如在US 7,867,968、US 7,871,976、US 8,333,289、US 2007/0269651 A1和US2014/0107010 A1中描述的那些。
iv.织物护理产品如漂洗调理剂(含有1至30重量%的织物调理活性成分),织物液体调理剂(含有1至30重量%的织物调理活性成分),滚筒式干衣机片板(Tumble DrierSheet),织物清新剂,织物清新剂喷雾剂,熨烫液体和织物柔顺剂系统如在美国专利号6,335,315、5,674,832、5,759,990、5,877,145、5,574,179、5,562,849、5,545,350、5,545,340、5,411,671、5,403,499、5,288,417、4,767,547和4,424,134中描述的那些。
液体织物柔顺剂/清新剂含有至少一种织物柔软剂,所述织物柔软剂优选以1至30%(例如,4至20%,4至10%和8至15%)的浓度存在。活性材料和织物柔软剂之间的比率可以为1:500至1:2(例如,1:250至1:4和1:100至1:8)。作为实例,当织物柔软剂按织物柔顺剂的重量计为5%时,活性材料为0.01至2.5%、优选0.02至1.25%并且更优选0.1至0.63%。作为另一个实例,当织物柔软剂按织物柔顺剂的重量计为20%时,活性材料为0.04至10%,优选0.08至5%并且更优选0.4至2.5%。
活性材料是香精、恶臭中和剂或其混合物。液体织物柔顺剂可以具有0.15至15%的胶囊(例如,0.5至10%、0.7至5%和1至3%)。当以这些水平包括胶囊时,柔顺剂中的净油当量(NOE)为0.05至5%(例如,0.15至3.2%、0.25至2%和0.3至1%)。
合适的织物柔软剂包括阳离子型表面活性剂。非限制性实例有季铵化合物如烷基化季铵化合物,环或环状季铵化合物,芳族季铵化合物,二季铵化合物,烷氧基化季铵化合物,酰氨基胺季铵化合物,酯季铵化合物,及其混合物。织物柔软组合物,及其组分,一般地描述于US 2004/0204337和US 2003/0060390中。合适的柔软剂包括酯季铵盐(esterquats)如可商购得自Evonik Industries的Rewoquat WE 18和可商购得自Stepan公司的Stepantex SP-90。
v.液体碗碟洗涤剂如在美国专利号6,069,122和5,990,065中描述的那些。
vi.自动碗碟洗涤剂如在美国专利号6,020,294、6,017,871、5,968,881、5,962,386、5,939,373、5,914,307、5,902,781、5,705,464、5,703,034、5,703,030、5,679,630、5,597,936、5,581,005、5,559,261、4,515,705、5,169,552和4,714,562中描述的那些。
vii.通用清洁剂,包括桶装可稀释清洁剂和卫生间清洁剂viii.浴厕清洁剂
ix.浴巾(Bath Tissue)
x.地毯除臭剂
xi.蜡烛
xii.房间除臭剂
xiii.地板清洁剂
xiv.消毒剂
xv.窗户清洁剂
xvi.垃圾袋/垃圾桶内衬
xvii.空气清新剂,包括房间除臭剂和车辆除臭剂、香薰蜡烛、喷雾剂、香油空气清新剂、自动喷雾空气清新剂和中和凝胶珠
xviii.水分吸收剂
xix.家用装置如纸巾和一次性擦拭巾
xx.蛾丸/诱捕剂/饼(Moth balls/traps/cakes)
b)婴儿护理产品
i.尿布疹乳膏/护臀膏
ii.婴儿爽身粉
c)婴儿护理装置
i.尿不湿
ii.围嘴
iii.擦拭巾
d)口腔护理产品。牙齿护理产品(作为用于口腔护理的根据本发明的制备物的实例)通常包括磨料体系(磨料或抛光剂),例如硅酸、碳酸钙、磷酸钙、铝氧化物和/或羟磷石灰,表面活性物质,例如月桂基硫酸酯钠、月桂基肌氨酸酯钠和/或椰油酰胺基丙基甜菜碱,润湿剂,例如甘油和/或山梨糖醇,增稠剂,例如羧甲基纤维素、聚乙二醇、角叉菜胶和/或Laponite.RTM.,甜味剂,例如糖精,用于令人不愉快的味道感觉的味觉矫正剂,用于另外的通常不是令人不愉快的味道感觉的味觉矫正剂,味觉调节物质(例如肌醇磷酸酯,核苷酸如单磷酸鸟苷、单磷酸腺苷,或者其他物质如谷氨酸钠或2-苯氧丙酸),凉爽活性成分,例如薄荷醇衍生物(例如L-乳酸薄荷酯、L-薄荷基烷基碳酸酯、薄荷酮缩酮、薄荷烷羧酸酰胺)、2,2,2-三烷基乙酸酰胺(例如2,2-二异丙基丙酸甲基酰胺)、icilin和icilin衍生物,稳定剂和活性成分,例如氟化钠、单氟磷酸钠、二氟化锡、季铵氟化物、柠檬酸锌、硫酸锌、焦磷酸锡、二氯化锡、多种焦磷酸盐的混合物、三氯生、鲸蜡基吡啶鎓盐氯化物、乳酸铝、柠檬酸钾、硝酸钾、氯化钾、氯化锶、过氧化氢、调味品和/或碳酸氢钠或味觉矫正剂。
i.牙膏。一种示例性制剂如下:
1.磷酸钙40-55%
2.羧甲基纤维素0.8-1.2%
3.月桂基硫酸酯钠1.5-2.5%
4.甘油20-30%
5.糖精0.1-0.3%
6.香料油1-2.5%
7.水,足量至100%
一种用于制备该制剂的典型方法包括以下步骤:(i)通过共混机混合根据前述的制剂以提供牙膏,和(ii)添加本发明的组合物并且将所得混合物共混直至均匀。
ii.牙粉
iii.漱口水
iv.牙齿增白剂
v.义齿粘附剂
e)保健设备
i.牙线
ii.牙刷
iii.呼吸器
iv.香薰/调味避孕套
f)妇女卫生保健品如卫生棉塞、卫生巾和擦拭巾,以及护垫
g)个人护理产品:美容或药物制剂,例如,“油包水”(W/O)型乳液,“水包油”(O/W)型乳液或作为例如水包油包水(W/O/W)型的多相乳液,作为PIT乳液、皮克林乳液(Pickering emulsion)、微乳液或纳米乳液;并且特别优选的乳液是“水包油”(O/W)型或水包油包水(W/O/W)型。更具体地,
i.个人清洁剂(条皂,沐浴液和沐浴露)
ii.沐浴护理剂(In-shower conditioner)
iii.防晒和纹身护色(Sunscreen ant tattoo color protection)(喷雾剂,洗剂和棒(sticks))
iv.驱昆虫剂
v.洗手液
vi.抗炎香油、软膏和喷雾剂
vii.抗菌软膏和乳膏
viii.感知剂(Sensates)
ix.除臭剂和止汗剂,包括气溶胶和泵喷止汗剂,棒式止汗剂(stickantiperspirant),滚抹式止汗剂、乳液喷雾止汗剂、透明乳液棒式止汗剂、软固体止汗剂、乳液滚抹式止汗剂、透明乳液棒式止汗剂、不透明乳液棒式止汗剂、透明凝胶止汗剂、透明棒式除臭剂、凝胶除臭剂、喷雾除臭剂、滚抹式和乳膏除臭剂。
x.基于蜡的除臭剂。一种示例性制剂如下:
1.石蜡(Parafin Wax)10-20%
2.烃蜡5-10%
3.白矿脂10-15%
4.乙酰化的羊毛脂醇2-4%
5.己二酸二异丙酯4-8%
6.矿物油40-60%
7.防腐剂(根据需要)
该制剂通过以下制备:(i)混合上述成分,(ii)将得到的组合物加热至75℃直至熔化,(iii)在搅拌下,添加4%低温研磨的包含香精的聚合物同时保持温度为75℃,和(iv)搅拌得到的混合物以确保均匀的悬浮液同时将本发明的组合物添加至制剂。
xi.二醇/皂型除臭剂。一种示例性制剂如下:
1.丙二醇60-70%
2.硬脂酸钠5-10%
3.蒸馏水20-30%
4. 2,4,4-三氯-2'-羟基二苯基醚,由Ciba-Geigy Chemical Company制造,并且商标是Ciba-Geigy Chemical Company)0.01-0.5%
将成分合并,并在搅拌下加热至75℃直到硬脂酸钠溶解。将得到的混合物冷却至40℃,然后添加本发明的组合物。
xii.乳液,包括身体乳液、面部乳液和手部乳液
xiii.爽身粉和足粉
xiv.洗漱用品
xv.身体喷雾剂
xvi.剃须膏和男性美容产品
xvii.浸浴用品
xviii.去角质磨砂膏
h)个人护理装置
i.面巾
ii.清洁擦拭巾
i)头发护理产品
i.洗发剂(液体和干粉)
ii.护发剂(洗去型护理剂,保留型护理剂和清洁型护理剂)
iii.染发剂
iv.头发清新剂
v.头发香料
vi.头发拉直产品
vii.头发造型产品、头发固定和定型助剂
viii.头发梳理乳膏
ix.发蜡
x.头发发泡剂、发胶、非气溶胶泵喷剂
xi.头发漂白剂、染料和着色剂
xii.烫发剂
xiii.头发擦拭巾
j)美容护理
i.精制香精-含酒精的。用于将香精胶囊掺入到含酒精的精制香精中的组合物和方法在US 4,428,869中描述。含酒精的精制香精可以含有以下:
1.乙醇(1-99%)
2.水(0-99%)
3.悬浮助剂,包括但不限于:羟丙基纤维素、乙基纤维素、二氧化硅、微晶纤维素、角叉菜胶、藻酸丙二醇酯、甲基纤维素、羧甲基纤维素钠或黄原胶(0-1%)
4.任选地,乳化剂或软化剂可以被包括到但不限于以上列出的那些
ii.固体香料
iii.唇膏/润唇膏
iv.化妆清洁剂
v.护肤化妆品如粉底、面膜、防晒霜、润肤乳液、乳状乳液、润肤霜、软化剂、皮肤美白剂
vi.美容化妆品,包括美甲、睫毛膏、眼线膏、眼影、液体粉底、粉末粉底、唇膏和腮红
k)消费品包装如香味盒、香味塑料瓶/箱
l)宠物护理产品
i.猫砂
ii.跳蚤和蜱处理产品
iii.宠物美容产品
iv.宠物洗发剂
v.宠物玩具、招待物(treats)和咀嚼物
vi.宠物训练垫
vii.宠物笼和箱
m)糖果,优选地选自由巧克力、巧克力棒产品、其他棒形式的产品、水果胶质、硬和软的焦糖和口香糖组成的组
i.胶质
1.胶基(天然胶乳糖树树胶,大部分当前的口香糖基质目前还包括弹性体,如聚乙酸乙烯酯(PVA)、聚乙烯(低或中等分子量)、聚异丁烯(PIB)、聚丁二烯、异丁烯-异戊二烯共聚物(丁基橡胶)、聚乙烯基乙基醚(PVE)、聚乙烯基丁基醚、乙烯基酯和乙烯基醚的共聚物、苯乙烯-丁二烯共聚物(苯乙烯-丁二烯橡胶,SBR)或乙烯基弹性体,例如基于乙酸乙烯酯/月桂酸乙烯酯、乙酸乙烯酯/硬脂酸乙烯酯或乙烯/乙酸乙烯酯,以及所提到的弹性体的混合物,如例如在EP 0 242 325、美国专利号4,518,615、美国专利号5,093,136、美国专利号5,266,336、美国专利号5,601,858或美国专利号6,986,709中描述的。)20-25%
2.糖粉45-50%
3.葡萄糖15-17%
4.淀粉糖浆10-13%
5.增塑剂0.1%
6.香料0.8-1.2%
上述组分根据前述制剂通过捏合机来捏合以提供口香糖。
然后添加囊封的香料或感知剂,并且混合直到均匀。
ii.口气清新剂
iii.口腔可溶条
iv.咀嚼糖
v.硬糖
n)烘烤产品,优选地选自由面包、干饼干、蛋糕和其他小甜饼组成的组;
o)休闲食品,优选地选自由烘烤或油炸的马铃薯片或马铃薯团产品、面包面团产品和基于玉米或花生的挤出物组成的组;
i.马铃薯、玉米粉圆饼、蔬菜或多谷物片
ii.爆米花
iii.椒盐脆饼
iv.膨化零食
p)谷物产品,优选地选自由早餐谷物食品、燕麦坚果棒和预烹制的成品大米产品组成的组
q)含酒精的和不含酒精的饮料,优选地选自由咖啡、茶、葡萄酒、含有葡萄酒的饮料、啤酒、含有啤酒的饮料、利口酒、烈性酒、白兰地、含有水果的苏打水、等渗饮料、软饮料、未冲淡的果汁(nectar)、水果和蔬菜汁和水果或蔬菜制备物组成的组;速溶饮料,优选地选自由速溶可可饮料、速溶茶饮料和速溶咖啡饮料组成的组
i.即饮液体饮品
ii.液体饮品浓缩物
iii.粉末状饮品
iv.咖啡:速溶卡布其诺
1.糖30-40%
2.奶粉24-35%
3.可溶性咖啡20-25%
4.乳糖1-15%
5.食品级乳化剂1-3%
6.囊封的挥发性香料0.01-0.5%
v.茶
vi.含酒精的
r)香辛料调和物和消费预制食品
i.粉末状肉汁、酱混配料
ii.调味料
iii.发酵产品
s)即热食品:即食餐和汤,优选地选自由汤粉、速溶汤、预煮汤组成的组
i.汤
ii.酱
iii.炖菜
iv.冷冻的主菜
t)乳制品奶制品,优选地选自由奶制饮料、冰牛奶、酸奶、开菲尔、奶油奶酪、软奶酪、硬奶酪、奶粉、乳清、黄油、酪乳和含有部分或完全水解的奶蛋白的产品奶味饮料组成的组
i.酸奶
ii.冰淇淋
iii.豆腐
iv.奶酪
u)大豆蛋白或其他大豆级分,优选地选自由豆奶以及由其生成的产品、含有大豆卵磷脂的制备物、发酵产品如豆腐或豆豉或由其生成的产品和酱油组成的组;
v)肉制品,优选地选自由火腿、鲜或生香肠制备物和调味或卤制的鲜肉或咸肉制品组成的组
w)蛋或蛋制品,优选地选自由全蛋粉、蛋白和蛋黄组成的组
x)基于油的产品或其乳液,优选地选自由蛋黄酱、调味酱、调料和调味品制备物组成的组
y)水果制备物,优选地选自由果酱、果汁冰糕、水果沙司和水果馅料组成的组;蔬菜制备物,优选地选自由番茄酱、沙司、干菜、深度冷冻的蔬菜、预烹制的蔬菜、在醋中的蔬菜和泡菜组成的组。
z)调味宠物食品。
以上列出的应用都是本领域中众所周知的。例如,美国专利号6,335,315、5,674,832、5,759,990、5,877,145、5,574,179;5,562,849、5,545,350、5,545,340、5,411,671、5,403,499、5,288,417和4,767,547、4,424,134中描述了织物柔顺剂系统。液体衣物洗涤剂包括美国专利号5,929,022、5,916,862、5,731,278、5,565,145、5,470,507、5,466,802、5,460,752、5,458,810、5,458,809、5,288,431、5,194,639、4,968,451、4,597,898、4,561,998、4,550,862、4,537,707、4,537,706、4,515,705、4,446,042和4,318,818中描述的那些系统。美国专利号6,069,122和5,990,065中描述了液体碗碟洗涤剂。可以采用本发明的洗发剂和调理剂包括美国专利号6,162,423、5,968,286、5,935,561、5,932,203、5,837,661、5,776,443、5,756,436、5,661,118、5,618,523、5,275,755、5,085,857、4,673,568、4,387,090和4,705,681中描述的那些。美国专利号6,020,294、6,017,871、5,968,881、5,962,386、5,939,373、5,914,307、5,902,781、5,705,464、5,703,034、5,703,030、5,679,630、5,597,936、5,581,005、5,559,261、4,515,705、5,169,552和4,714,562中描述了自动碗碟洗涤剂。
术语“多官能异氰酸酯(polyfunctional isocyanate)”、“多官能异氰酸酯(multifunctional isocyanate)”和“多异氰酸酯”都是指具有两个以上异氰酸酯(-NCO)基团的化合物。
术语“多官能胺(polyfunctional amine)”、“多官能胺(multifunctionalamine)”和“多胺”是指含有两个以上伯或仲胺基团的化合物。这些术语还指包含一个或多个伯/仲胺基团和一个或多个羟基(-OH)的化合物。
术语“多官能醇(polyfunctional alcohol)”“多官能醇(multifunctionalalcohol)”“多醇(poly alcohol)”和“多元醇(polyol)”是指具有两个以上羟基的化合物。
通过以下非限制性实例更详细地描述本发明。在没有进一步阐释的情况下,据信基于本文中的描述,本领域技术人员可以利用本发明至其最充分程度。本文中引用的所有出版物以其整体通过引用并入。
实施例1:胶囊1(BPEI以及聚磺苯乙烯和CMC的混合物)
在烧杯中,将96克(“g”)的香精谐香剂(fragrance accord)(InternationalFlavors and Fragrance,Union Beach,NJ)与24g的NEOBEE油M-5(辛酸/癸酸甘油三酯,Stepan,Chicago,IL)和9.6g的异氰酸酯单体TAKENATE D110-N(亚二甲苯基二异氰酸酯的三羟甲基丙烷加合物,Mitsui Chemicals Corporation,Rye Brook,NY)合并,形成油相。在单独的烧杯中,将含有1%的FLEXAN II(聚磺苯乙烯,Akzo Nobel,Bridgewater,NJ)的水溶液(130g)与1%羧甲基纤维素(“CMC”,WALOCEL CRT 50000PA 07,Dow,Midland,MI)的水溶液(30g)混合,形成水相。然后在以6500rpm剪切(ULTRA TURRAX,T25 Basic,IKA WERKE)两分钟下将油相乳化到水相中,形成香精乳液。
在利用顶置式混合器的持续搅拌下向香精乳液加入10.4g的49%支化聚乙烯亚胺水溶液(“BPEI”,Sigma-Aldrich,St.Louis,MO)。胶囊的形成通过光学显微镜直接可见。在完成支化聚乙烯亚胺的添加后降低混合器速度。将胶囊浆料在55℃固化两小时,得到胶囊1。
实施例2:胶囊2(BPEI以及PVP和PQ-11的混合物)
在烧杯中,将96g的香精谐香剂(International Flavors and Fragrance,UnionBeach,NJ)与24g的NEOBEE油M-5和9.6g的TAKENATE D110-N合并,形成油相。在单独的烧杯中,将含有1.1%的PVP(聚乙烯吡咯烷酮,K 90Pulver,BASF,Ludwigshafen,德国)的水溶液(130g)与20%聚季铵盐-11(PQ11,乙烯吡咯烷酮/甲基丙烯酸二甲基氨基乙酯共聚物,阳离子聚合物,LUVIQUAT PQ11AT 1,Ludwigshafen,德国)的水溶液(30g)混合,形成水相。然后在以9500rpm剪切(ULTRA TURRAX,T25Basic,IKA WERKE)两分钟下将油相乳化到水相中,形成香精乳液。
在利用顶置式混合器的持续搅拌下向香精乳液加入10.4g的49%BPEI水溶液。在完成交联剂的添加后降低混合器速度。将胶囊浆料在55℃固化两小时,得到胶囊2。
实施例3:胶囊3(HMDA以及PVP和PQ-11的混合物)
在烧杯中,将96g的香精谐香剂(International Flavors and Fragrance,UnionBeach,NJ)与24g的Neobee油和9.6g的异氰酸酯单体 M20(聚合的亚甲基二苯基二异氰酸酯,可由BASF corporation,Wyandotte,MI,USA商购获得)合并,形成油相。在单独的烧杯中,使用含有1%聚乙烯吡咯烷酮(K90,BASF,Ludwigshafen,德国)和4%聚季铵盐-11的水溶液(160g)作为水相。然后在以12500rpm剪切(UltraT25Basic,WERKE)两分钟下将油相乳化到水相中,形成香精乳液。
将香精乳液在圆底容器中加热至35℃,并且在利用顶置式混合器的持续搅拌下向其加入10.8g的40%六亚甲基二胺(HMDA)(INVISTA,Wichita,KS,USA)。胶囊的形成通过光学显微镜直接可见。在完成HMDA的添加后降低混合器速度。将胶囊浆料在55℃固化两小时,得到胶囊3。
实施例4:胶囊4(HMDA以及Flexan II和CMC的混合物)
在烧杯中,将96g的香精谐香剂(International Flavors and Fragrance,UnionBeach,NJ)与24g的Neobee油和9.6g的M20合并,形成油相。在单独的烧杯中,将含有1.0%的FLEXAN II的水溶液(130g)与2%CMC的水溶液(30g)混合,形成水相。然后在以9500rpm剪切(UltraT25Basic,WERKE)两分钟下将油相乳化到水相中,形成香精乳液。
将香精乳液在圆底容器中加热至35℃,并且在利用顶置式混合器的持续搅拌下向其加入10.8g的40%HMDA水溶液。胶囊的形成通过光学显微镜直接可见。在完成HMDA的添加后降低混合器速度。将胶囊浆料在55℃固化两小时,得到胶囊4。
实施例5:胶囊5(Morwet D-425和PVP的混合物)
在烧杯中,将96g的香精谐香剂(International Flavors and Fragrance,UnionBeach,NJ)与24g的Neobee油和9.6g的M20合并,形成油相。在单独的烧杯中,使用含有1%Morwet D-425(萘磺酸盐/酯缩合物的钠盐,可由Akzo Nobel,Fort Worth,TX,USA商购获得)和1%聚乙烯吡咯烷酮(K90,BASF,Ludwigshafen,德国)的水溶液(160g)作为水相。然后在以9500rpm剪切(UltraT25Basic,WERKE)两分钟下将油相乳化到水相中,形成香精乳液。
将香精乳液在圆底容器中加热至35℃,并且在利用顶置式混合器的持续搅拌下向其加入10.8g的40%HMDA水溶液。胶囊的形成通过光学显微镜直接可见。在完成HMDA的添加后降低混合器速度。将胶囊浆料在55℃固化两小时,得到胶囊5。
实施例6:组合物A的制备
通过将264g的胶囊1、6g的10重量%GELWHITE GP(一种蒙脱石粘土)水溶液和30g的5重量%聚季铵盐-11水溶液混合来制备本发明的组合物(即组合物A)。将所得混合物通过顶置式IKA实验室混合器搅拌30分钟直到聚合物溶液完全溶解。
还制备了两种比较组合物,即比较A1’和A2’。除了没有使用聚季铵盐-11以外,按照与组合物1完全相同的过程制备比较A1’。除了没有使用GELWHITE GP以外,还按照与组合物A完全相同的过程制备比较A2’。
组合物稳定性通过使组合物A以及比较A1’和A2’在45℃老化4周的时间来评价。使用胶囊1作为对照样品。拍摄照片以说明样品的稳定性。结果表明,对于组合物A没有看到分离,而胶囊1、比较A1’和A2’各自表现出明显的分离,证明带负电的粘土和聚季铵盐-11的组合的益处。
实施例7-9:组合物B1-B3的制备
通过将胶囊1与带负电的粘土和阳离子聚合物组合来制备本发明的三种组合物。粘土作为10重量%水溶液加入,并且阳离子聚合物作为5重量%水溶液加入。在下表2中示出它们的水平。
还通过将胶囊1与下表2中所示水平的辅料组合来制备二十种比较组合物,即比较B1’-B20’。
表2
稳定性评价
为了评价组合物B1-B3和比较B1’-B20’的储存稳定性,将各个样品分到2个小瓶中。将一个小瓶置于室温,并且将另一个置于45℃。定期检查样品的乳液分层和凝胶化。在4周后使用量筒测量分离的量。使用胶囊1作为对照。在下表3中给出结果。
表3
结果显示,组合物B1-B2在室温和45℃储存时各自具有良好的稳定性。通过Brookfield DV-111Ultra可编程粘度计(Brookfield Engineering Laboratories,Inc.,Middleboro,MA,USA)测量组合物B1-B2的粘度。在下表4中给出结果。
在45℃储存4周后,各个比较组合物的粘度大于6666cP(仪器的检测限)。
表4
实施例10-12
通过按照以上实施例7-9中所述的过程使用胶囊1制备本发明的另外五种微胶囊组合物,即组合物C1-C5。还制备了比较组合物C1’、C2’和C3’。在下表6中示出阳离子聚合物(PQ-4或PQ-47)和Gelwhite GP的水平。在室温储存4周后,测量各个样品的粘度(参见表5)。
表5
使用实施例5中所示的胶囊5连同PQ-4和Gelwhite来制备本发明的另外三种微胶囊组合物,即组合D1-D3。按照实施例7-9中所述的过程。还制备了比较组合物D1’和D2’。在下表6中示出阳离子聚合物(PQ-4)和Gelwhite GP的水平。在室温储存4周后,测量各个样品的粘度(参见表6)。
表6
实施例13:稳定化的胶囊制剂的感官性能
评价了在滚抹式基质中的辅料稳定化的聚脲胶囊制剂的感官性能。在表7中示出滚抹式制剂。
表7
指示小组成员(30-35名,男性和女性的混合)在评价当天用未加香精的肥皂沐浴。对于比较分析,对一侧腋下施用测试样品,对另一侧腋下施用对照样品。样品由0.35g的滚抹式基质(在塑料注射器中预先测量用于简单施用到皮肤上)组成。在腋下上平衡样品的施用。在0-10的强度等级上,在施用后的第0、8、12和24小时评价香精强度。在指定时间,由小组成员将强度评分输入到自动化数据输入系统(在手边的COMPUSENSE)中。对于各个样品,将小组成员之间的强度分数平均,并且通过Two-Way ANOVA分析(p<0.1/90%CI)。
实施例14:透明除臭剂棒式制剂
在表8中提供示例性的透明除臭剂棒式制剂。
表8
实施例15:止汗剂乳液喷雾制剂
在表9中提供示例性的止汗剂乳液喷雾制剂。
表9
实施例16:止汗剂乳液滚抹式制剂
在表10中提供示例性的止汗剂乳液滚抹式制剂。
表10
实施例17:止汗剂透明乳液棒式制剂
在表11中提供示例性的止汗剂透明乳液棒式制剂。
表11
实施例18:止汗剂不透明乳液棒式制剂
在下表12中提供示例性的止汗剂不透明乳液棒式制剂。
表12
实施例19:除臭剂喷雾制剂
在表13中提供示例性的除臭剂喷雾制剂。
表13
实施例20:止汗剂透明凝胶制剂
在表14中提供示例性的止汗剂透明凝胶制剂。
表14
其他实施方案
本说明书中公开的所有特征都可以以任意组合合并。本说明书中公开的每个特征都可以被用作相同、等同或相似目的的备选特征替换。因此,除非另外明确说明,公开的每个特征都仅是等同或相似特征的通用系列的实例。
实际上,为了实现制备稳定的微胶囊组合物的目的,本领域技术人员可以选择胶囊、粘土和阳离子聚合物。另外,胶囊、粘土和阳离子聚合物之间的比例也可以由技术人员确定而无需过度实验。
根据以上描述,技术人员可以容易地确定本发明的必要特征,并且在不脱离其精神和范围的情况下,可以对本发明进行多种变化和改变以使其适合于多种使用和条件。因此,其他实施方案也在权利要求内。
Claims (20)
1.一种稳定的微胶囊组合物,所述微胶囊组合物包含分散在水相中的微胶囊和稳定剂,其中所述微胶囊组合物在45℃储存时稳定至少4周,并且认为所述微胶囊组合物在(i)所述组合物的粘度为3000cP以下以及(ii)所述组合物体积的20%以下的水与所述组合物分离时是稳定的。
2.一种稳定的微胶囊组合物,所述微胶囊组合物包含分散在水相中的微胶囊和稳定剂,其中稳定剂是带负电的粘土和阳离子聚合物的组合。
3.权利要求1或2所述的稳定的微胶囊组合物,其中所述微胶囊以20重量%至70重量%的水平存在。
4.权利要求2或3所述的稳定的微胶囊组合物,其中所述带负电的粘土以0.05%至2%、优选0.05%至1%并且更优选0.1%至0.5%的水平存在;并且所述阳离子聚合物以0.05%至5%、优选0.1%至2%并且更优选0.2%至0.7%的水平存在。
5.权利要求2至4中任一项所述的稳定的微胶囊组合物,其中所述带负电的粘土是蒙脱石粘土。
6.权利要求2至5中任一项所述的稳定的微胶囊组合物,其中所述阳离子聚合物是阳离子聚季铵盐聚合物。
7.权利要求6所述的稳定的微胶囊组合物,其中所述阳离子聚季铵盐聚合物是羟乙基纤维素二甲基二烯丙基氯化铵共聚物(PQ-4),丙烯酰胺和二烯丙基二甲基氯化铵的共聚物(PQ-7),丙烯酸、甲基丙烯酰胺基丙基三甲基氯化铵和丙烯酸甲酯的三元共聚物(PQ-47),或其组合。
8.权利要求1至7中任一项所述的稳定的微胶囊组合物,其中所述微胶囊是具有微胶囊壁和被所述微胶囊壁囊封的微胶囊芯的芯壳型微胶囊;所述微胶囊壁由选自由以下各项组成的组中的囊封聚合物形成:聚丙烯酸酯、聚脲、聚氨酯、聚丙烯酰胺、聚酯、聚醚、聚酰胺、聚(丙烯酸酯-共-丙烯酰胺)、淀粉、二氧化硅、明胶和阿拉伯树胶、藻酸盐、壳聚糖、聚丙交酯、聚(三聚氰胺-甲醛)、聚(脲-甲醛)及其组合;并且所述微胶囊芯含有选自由以下各项组成的组中的活性材料:香精、前香精、香料、恶臭中和剂、维生素或其衍生物、抗炎剂、杀真菌剂、麻醉剂、止痛剂、抗微生物活性成分、抗病毒剂、抗感染剂、祛痘剂、皮肤光亮剂、驱昆虫剂、兽用驱避剂、驱寄生虫剂、软化剂、皮肤保湿剂、皱纹控制剂、UV防护剂、织物柔顺剂活性成分、硬表面清洁活性成分、皮肤或头发调理剂、阻燃剂、抗静电剂、纳米至微米尺寸的无机固体、聚合物或弹性体颗粒、味道调节剂、细胞、益生菌及其组合。
9.权利要求1至8中任一项所述的稳定的微胶囊组合物,其中所述组合物的pH值为4至8。
10.权利要求8所述的稳定的微胶囊组合物,所述微胶囊组合物还包含烷基萘磺酸盐/酯甲醛缩合物、聚乙烯吡咯烷酮、聚乙烯醇、聚磺苯乙烯、羧甲基纤维素、聚乙烯吡咯烷酮、萘磺酸盐/酯缩合物的钠盐、乙烯吡咯烷酮和季铵化的甲基丙烯酸二甲基氨基乙酯的共聚物或其组合;其中所述囊封聚合物是聚脲、聚氨酯或其组合;所述聚脲是多官能异氰酸酯和多官能胺的反应产物;并且所述聚氨酯是多官能异氰酸酯和作为交联剂的多官能醇的反应产物。
11.权利要求10所述的稳定的微胶囊组合物,其中所述多官能异氰酸酯是芳族多官能异氰酸酯、脂族多官能异氰酸酯或其组合;所述芳族多官能异氰酸酯含有苯基、甲苯基、二甲苯基、萘基、联苯基部分或其组合;并且所述脂族多官能异氰酸酯是六亚甲基二异氰酸酯的三聚体、异佛尔酮二异氰酸酯的三聚体、六亚甲基二异氰酸酯的缩二脲或其组合。
12.权利要求11所述的稳定的微胶囊组合物,其中所述芳族多官能异氰酸酯选自由以下各项组成的组:聚合的亚甲基二苯基二异氰酸酯、甲苯二异氰酸酯的多异氰脲酸酯、甲苯二异氰酸酯的三羟甲基丙烷加合物、亚二甲苯基二异氰酸酯的三羟甲基丙烷加合物及其组合;并且所述脂族多官能异氰酸酯选自由以下各项组成的组:六亚甲基二异氰酸酯的二聚体、缩二脲、对称三聚体、不对称三聚体,及其组合。
13.权利要求10所述的稳定的微胶囊组合物,其中所述多官能胺是六亚甲基二胺、六亚乙基二胺、乙二胺、1,3-二氨基丙烷、1,4-二氨基-丁烷、二亚乙基三胺、五亚乙基六胺、1,6-二氨基己烷、肼、1,4-二氨基环己烷、1,3-二氨基-1-甲基丙烷、双(3-氨基丙基)胺、双(六亚甲基)三胺、三(2-氨基乙基)胺、三亚乙基-四胺、N,N'-双(3-氨基丙基)-1,3-丙二胺、四亚乙基五胺、支化的聚乙烯亚胺、壳聚糖、乳酸链球菌肽、明胶、1,3-二氨基-胍、1,1-二甲基双胍、胍、精氨酸、赖氨酸、鸟氨酸、组氨酸、氨基-2-甲基-1-丙醇或其组合。
14.权利要求10所述的稳定的微胶囊组合物,其中所述微胶囊组合物含有烷基萘磺酸盐/酯甲醛缩合物和聚乙烯吡咯烷酮,其中的每一种独立地以所述微胶囊组合物重量的0.1%至5%的水平存在,并且所述烷基萘磺酸盐/酯甲醛缩合物和聚乙烯吡咯烷酮之间的比率为10:1至1:10。
15.权利要求14所述的稳定的微胶囊组合物,其中所述囊封聚合物是聚脲,所述聚脲是多官能异氰酸酯和多官能胺的反应产物,所述多官能异氰酸酯含有甲苯二异氰酸酯的三羟甲基丙烷加合物或亚二甲苯基二异氰酸酯的三羟甲基丙烷加合物,并且所述多官能胺是二亚乙基三胺、双(3-氨基丙基)胺、双(六亚甲基)三胺、三(2-氨基乙基)胺、三亚乙基四胺、N,N'-双(3-氨基丙基)-1,3-丙二胺、四亚乙基五胺、五亚乙基六胺、支化的聚乙烯亚胺、壳聚糖、乳酸链球菌肽、明胶、1,3-二氨基胍单盐酸盐、1,1-二甲基双胍盐酸盐或碳酸胍或其混合物。
16.权利要求15所述的稳定的微胶囊组合物,所述组合物还包含聚乙烯醇、聚磺苯乙烯、羧甲基纤维素、聚乙烯吡咯烷酮、萘磺酸盐/酯缩合物的钠盐、乙烯吡咯烷酮和季铵化的甲基丙烯酸二甲基氨基乙酯的共聚物或其组合。
17.权利要求1至16中任一项所述的稳定的微胶囊组合物,所述组合物还包含选自由以下各项组成的组中的沉积助剂:聚季铵盐-5、聚季铵盐-6、聚季铵盐-7、聚季铵盐-10、聚季铵盐-16、聚季铵盐-22、聚季铵盐-24、聚季铵盐-28、聚季铵盐-39、聚季铵盐-44、聚季铵盐-46、聚季铵盐-47、聚季铵盐-53、聚季铵盐-55、聚季铵盐-67、聚季铵盐-68、聚季铵盐-69、聚季铵盐-73、聚季铵盐-74、聚季铵盐-77、聚季铵盐-78、聚季铵盐-79、聚季铵盐-80、聚季铵盐-81、聚季铵盐-82、聚季铵盐-86、聚季铵盐-88、聚季铵盐-101、聚乙烯胺、聚乙烯亚胺、聚乙烯胺和乙烯基甲酰胺共聚物及其组合。
18.权利要求1至17中任一项所述的稳定的微胶囊组合物,所述组合物还包含一种或多种游离香精或者一种或多种另外的微胶囊。
19.一种包含前述权利要求中任一项所述的稳定的微胶囊组合物的消费品。
20.权利要求19所述的消费品,其中所述消费品是洗发剂、护发剂、染发剂、头发清新剂、头发固定或定型助剂、头发漂白剂、头发染料或着色剂、肥皂、沐浴液、化妆品制备物、通用清洁剂、浴厕清洁剂、地板清洁剂、窗户清洁剂、浴巾、纸巾、一次性擦拭巾、尿布疹乳膏/护臀膏、婴儿爽身粉、尿不湿、围嘴、婴儿擦拭巾、口腔护理产品、牙膏、漱口水、牙齿增白剂、义齿粘附剂、口香糖、口气清新剂、口腔可溶条、咀嚼糖、硬糖、洗手液、抗炎香油、抗炎软膏、抗炎喷雾剂、保健设备、牙线、牙刷、卫生棉塞、卫生巾、个人护理产品、防晒露、防晒喷雾剂、基于蜡的除臭剂、二醇型除臭剂、皂型除臭剂、面部乳液、身体乳液、手部乳液、爽身粉、剃须膏、浸浴用品、去角质磨砂膏、足霜、面巾、清洁擦拭巾、织物护理产品、织物柔顺剂、织物清新剂、熨烫水、液体衣物洗涤剂、液体碗碟洗涤剂、自动碗碟洗涤剂、单位剂量片剂或胶囊、增味剂、干衣机片板、精制香精、固体香料、粉末粉底、液体粉底、眼影、唇膏或润唇膏、淡香水产品、除臭剂、地毯除臭剂、蜡烛、房间除臭剂、消毒剂、气溶胶止汗剂,棒式止汗剂,滚抹式止汗剂、乳液喷雾止汗剂、透明乳液棒式止汗剂、软固体止汗剂、乳液滚抹式止汗剂、透明乳液棒式止汗剂、不透明乳液棒式止汗剂、透明凝胶止汗剂、透明棒式除臭剂、喷雾除臭剂、烘烤产品、面包、干饼干、蛋糕、小甜饼、薯片、爆米花、椒盐脆饼、膨化零食、早餐谷物食品、燕麦坚果棒、预烹制的成品大米产品、含酒精的或不含酒精的饮料、香辛料调和物、汤、酱、炖菜、冷冻的主菜、酸奶、冰淇淋、豆腐、奶酪、大豆蛋白产品、肉制品、蛋制品、蛋黄酱、调味酱、调料、调味品制备物、水果制备物或蔬菜制备物。
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CN111304961A (zh) * | 2020-02-25 | 2020-06-19 | 金华盛纸业(苏州工业园区)有限公司 | 无碳复写纸用微胶囊及其制备方法、无碳复写纸及其涂料 |
CN114025737A (zh) * | 2019-06-25 | 2022-02-08 | 莱雅公司 | 包含生物表面活性剂和羧基甜菜碱聚合物的组合物 |
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CN116322326A (zh) * | 2020-08-06 | 2023-06-23 | 西姆莱斯股份公司 | 聚脲/聚氨酯微胶囊 |
CN116367720A (zh) * | 2020-08-06 | 2023-06-30 | 西姆莱斯股份公司 | 可生物降解的聚脲/聚氨酯微胶囊 |
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EP3478249A1 (en) | 2019-05-08 |
BR112018076803A2 (pt) | 2019-04-02 |
WO2018006089A1 (en) | 2018-01-04 |
MX2019000150A (es) | 2019-05-30 |
US20190231658A1 (en) | 2019-08-01 |
EP3478249A4 (en) | 2020-03-04 |
US11540985B2 (en) | 2023-01-03 |
EP3478249B1 (en) | 2024-09-11 |
US20240004145A1 (en) | 2024-01-04 |
US12013574B2 (en) | 2024-06-18 |
US20230046103A1 (en) | 2023-02-16 |
BR112018076803B1 (pt) | 2022-05-03 |
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