CN101121102A - 细分散的水包油乳状液的制备方法 - Google Patents
细分散的水包油乳状液的制备方法 Download PDFInfo
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- CN101121102A CN101121102A CNA200710126370XA CN200710126370A CN101121102A CN 101121102 A CN101121102 A CN 101121102A CN A200710126370X A CNA200710126370X A CN A200710126370XA CN 200710126370 A CN200710126370 A CN 200710126370A CN 101121102 A CN101121102 A CN 101121102A
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Abstract
本发明涉及制备包含油、水和至少一种乳化剂的细分散的水包油乳状液的方法,其包括步骤A)通过将油、水、至少一种乳化剂和至少一种成序物质进行混合制备混合物2,该混合物包含油、水、至少一种乳化剂和至少一种成序物质,其中该混合物(Winsor IV体系)的相转变温度PIT2小于混合物1(Winsor IV体系)的相转变温度PIT1,该混合物1不具有成序物质而在其他方面与混合物2的组成相同,以及随后的步骤B)在混合物2中加入稀释剂将该混合物转化为乳状液3,其中选择所加入的稀释剂的量,使在预先给定的温度下得到的乳状液3不是处在该Winsor IV相的区域之内。
Description
技术领域
本发明本身涉及制备细分散的水包油乳状液的方法,特别涉及通过加入成序物质(cosmotropic substance)来影响该具体系统的相转变温度(PIT)的方法。
背景技术
在某些应用领域,水包油型(O/W)乳状液优选用于化妆品的、皮肤病的和制药的配方中,以及还用在家庭和工业领域的水溶液配方中。
常规方式制备的乳状液具有在微米范围内的液滴大小,并因此具有不稳定的缺点,即它们在不加入另外的稳定剂的情况下具有相分离的趋势。因此,利用常规方法,只能非常偶然地制备出具有长期稳定性和特别是具有低粘度的乳状液。
一种替代方案是热动力学稳定的微乳状液。尽管这些微乳状液对于分离来说是稳定的,但是它们只存在于较窄的浓度和温度范围之内,这不是对所有的应用领域均适合。
通过相转变温度法(PIT法)所制备的乳状液(K.Shinoda,H.Kunieda;Encyclopedia of Emulsion Technology;Vol.1(1983),337-367)同样是极其细分散的,即考虑到它们的液滴大小在20-200nm的范围内,它们在大的温度和浓度范围内确保具有优异的稳定性。
在本方法中,根据目前的模型概念发生了下述过程:
在室温下,油、水和乳化剂形成包含O/W型微乳状液和油相(Winsor I型,W I)的两相混合物。
为了实现单相区域(Winsor IV型,W IV),仅靠增加乳化剂的浓度是不够的;必需要求升高温度。在相转变温度(PIT)的系统决定的最低温度下,形成双连续的、均匀的混合相(Winsor IV型),其中发生了从O/W型到W/O型的相转变。
一旦进一步升高温度,该均匀的Winsor IV体系即转变为两相的Winsor II体系(W II),其中W/O微乳状液与过量的水相达到平衡。
在本领域内,现在利用的事实是,在快速冷却时可以形成该W IV型的微乳状液,这种微乳状液在到O/W的相转变之后实际上被“冻结”,这意味着不发生到该W I型的进一步转变。
这样,获得了极其稳定的细分散的乳状液浓缩物,它可用水稀释到无限制的程度。
该方法是迄今为止在工业规模上亦可制备这种乳状液的唯一方法。
在该方法中,不利之处是为了将室温下存在的该O/W型乳状液转变为W/O型乳状液并通过随后的冷却生成细分散的O/W型乳状液,必须将这些组分的混合物加热到相转变温度以上。用于加热和有效冷却所需的能量输入相当可观并且不经济。
因此需要一种成本有效的方法来制备细分散的乳状液,而这些乳状液在宽的温度和浓度范围内具有优异的稳定性。
通过一种方法实现了该目标,在该方法中:在第一阶段中,通过使用多种成序物质使所谓的相转变温度(PIT)降低到至少为室温或者应用温度水平,以及,在第二阶段中,再次升高相转变温度,优选通过加入稀释剂升高到原始水平。
在本方法中,该成序物质取代了升高温度的步骤。
通过加入足够量的稀释剂(根据本发明优选为水或者水溶液,任选醇溶液),没有达到为了降低相转变温度所要求的该成序物质(CS)的最低浓度,这意味着因此恢复到了原始温度。此处稀释发生的如此迅速(类似于快速降温),以至于未发生该乳状液向Winsor型W I的转变。
由于本方法因此是实质上基于该成序物质的一种钝化作用(“骤冷(quenching)”),根据温度控制的PIT法,可以在现在的情况中谈及PSQ法(通过骤冷进行的相转变)。
发明内容
因此本发明提供一种制备细分散的水包油乳状液的方法,其中所述乳状液包含油、水和至少一种乳化剂,并且它们优选在环境温度、加工温度或使用温度下在动力学方面是稳定的,所述方法包括以下步骤:
A)通过将油、水、至少一种乳化剂和至少一种成序物质进行混合制备混合物2,该混合物包含油、水、至少一种乳化剂和至少一种成序物质,其中该混合物(Winsor IV体系)的相转变温度PIT2低于混合物1(Winsor IV体系)的相转变温度PIT1,所述混合物1中没有成序物质但在其它方面具有与混合物2相同的组成,
以及随后的步骤
B)在混合物2中加入稀释剂将该混合物转变为乳状液3,其中选择所加入的稀释剂的量,使生成的在预设定温度下的乳状液3不处于Winsor IV相的区域内,
以及用本方法可以获得的细分散的水包油乳状液。
在根据本发明的方法中,优选制备一种细分散的水包油乳状液3,它具有小于1μm的平均粒径,优选为10-500nm,特别优选为15-300nm,以及非常特别优选为60-200nm的平均粒径。
优选在根据本发明的方法中制备微乳状液作为混合物2。
在根据本发明方法的步骤B)中,在为1重量份的该混合物2中优选加入至少为1重量份、优选至少5重量份并且特别优选至少10重量份的稀释剂。
在根据本发明的方法中,步骤B)中所加入的稀释剂的量,优选使该乳状液3转变至Winsor IV相区的转变温度高于环境温度、加工温度或使用温度至少1K,优选为10K,特别优选为40K。
例如,在步骤B)中可以使用的稀释剂是水或者水溶液。
根据本发明制备细分散的水包油乳状液的方法的一种变型的方法包括:制备一种在环境温度、加工温度或者使用温度下在动力学方面稳定的乳状液作为乳状液3,其中,在步骤A)中通过常规方法制备一种在热力学方面稳定的且宏观上均匀的水、油、至少一种乳化剂和至少一种成序物质的混合物,并且其中步骤A)是在低于未加入成序物质的混合物1的相转变温度PIT1的温度下进行。
根据本发明制备细分散的水包油乳状液的方法的另一种变型的方法包括:制备在环境温度、加工温度或者使用温度下在动力学方面稳定的乳状液作为乳状液3,其中步骤A)包含将至少一定量的至少一种成序物质与混合物1相混合,该混合物1包含油、水和至少一种乳化剂并且它具有相转变温度PIT1(Winsor IV体系),这样获得混合物2,其相转变温度(Winsor IV体系)PIT2低于PIT1。
根据本发明制备细分散的水包油乳状液的方法的另一种变型的方法包括:制备在环境温度、加工温度或者使用温度下在动力学方面稳定的乳状液作为乳状液3,其中在步骤A)中通过常规方法在不超过原始相转变温度的情况下利用水、油、至少一种乳化剂和至少一种成序物质制备W/O型微乳状液相(类型W II),所述W/O型微乳状液相与过量的水相平衡。
如所解释的,该成序物质使相转变温度降低。降低的程度取决于该成序物质的性质和用量。已经发现相转变温度的降低实质上与所用的量成比例。
因为在本方法的第二个步骤中是通过稀释特别是用水稀释使该成序物质的影响再次被减少,这就可以在每种单独的情况下通过探索性试验来确定最佳用量。根据本发明,最佳用量是指用来恰当地降低PIT的在实践中适当的量,或者是快速和有针对性的使该形成氢键的物质停止作用以便升高PIT的水在实践中适当的最小的用量。
本发明进一步提供了根据本发明用于制备乳状液的方法的用途,该用途涉及化妆品的、皮肤病的、医药的或者农用化学的制品的制备,用于面部护理和身体护理、婴儿护理、阳光防护、卸妆用品、止汗/除臭剂的浸渍湿巾或者可喷雾制品的制备,在家庭、运动、休闲和工业领域中应用中的水溶液配方的制备,用于纺织品、皮革、塑料、金属和非金属表面清洁和护理的浸渍湿巾或者可喷雾制品的制备,以及在包含油类和任选另外的活性物质如杀虫剂的农用配方的可喷雾制品的制备。
本发明的另外的主题由权利要求定义。
为了本发明的目的,依据定义,根据本发明所共用的这些成序物质是化合物,根据感胶离子序,这些化合物可以是带有亲水基团、具体是羟基或者羧基的阴离子、阳离子、盐或者有机化合物。
阴离子例如是SO4 2-、PO4 3-、柠檬酸根、酒石酸根或者乙酸根。
阳离子例如是Al3+、Mg2+、Ca2+、Ba2+、Li+、Na+或者K+。
盐例如是柠檬酸钠、Na2SO4、(NH4)2SO4、NaCl或者NH4SCN。
有机化合物例如是单羟基或多羟基醇,例如丁醇、甘油、二甘油、三甘油、糖类、糖醇类、糖酸类、羟基羧酸类如乳酸、马来酸、酒石酸、柠檬酸或者抗坏血酸。
这些化合物可以它们自己被共用或者彼此之间和/或在彼此之中结合使用。
足以用于降低该相转变温度的量取决于每种情况所用的油成分的种类和量、该乳化剂成分的种类和量以及成序物质的种类。通常,适当的量值范围是在按重量计从1%到50%,有利的是按重量计从20%到40%。每一情况下的最佳量可以通过几个简单的探索性试验来确定。
原则上,根据本发明可以使用的油类是适合用于制备清洁和护理用化妆品水性乳状液的所有化合物,或者它们的混合物,诸如单羧酸/二元羧酸以及单醇/二元醇的单酯和二酯,例如具有通式(I)、(II)和(III)
R1-COOR2 (I)
R2-OOC-R3-COOR2 (II)
R1-COO-R3-OOC-R1 (III)
其中
R1是具有8到22个碳原子的烷基基团,并且
R2是具有3到22个碳原子的烷基基团,并且
R3是具有2到16个碳原子的亚烷基基团,条件是化合物(I)到(III)中的碳原子总数至少为11。
这些化合物是熟知的化妆品和药物的油组分。在此类的单酯和二酯中,在室温下(20℃)的液体产物是最重要的。适合于作为油体(oilbody)的单酯例如是具有12到22个碳原子的脂肪酸的异丙基酯,例如豆蔻酸异丙酯、棕榈酸异丙酯、硬脂酸异丙酯、油酸异丙酯。其他适合的单酯例如是硬脂酸正丁酯、月桂酸正己酯、油酸正癸酯、硬脂酸异辛酯、棕榈酸异壬酯、异壬酸异壬酯、棕榈酸2-乙基己酯、月桂酸2-乙基己酯、硬脂酸2-己基癸酯、棕榈酸2-辛基十二烷酯、油酸油酯、芥酸油酯、油酸芥酯,以及从工业级脂肪醇混合物和工业级脂肪族羧酸获得的酯,例如具有12到22个碳原子的饱和的和不饱和的脂肪醇以及具有12到22个碳原子的饱和的和不饱和的脂肪酸的酯,正像那些可以从动物和植物脂肪获得。天然形成的单酯和蜡酯混合物也是适合的,例如象在霍霍巴油或鲸蜡油中所存在的。
适合的二羧酸酯(II)例如是己二酸二正丁酯、癸二酸二正丁酯、己二酸二(2-乙基己基)酯、琥珀酸二(2-己基癸基)酯和壬二酸二异十三烷酯。适合的二醇酯(III)例如是二油酸乙二醇酯、二异十三羧酸乙二醇酯、丙二醇二(2-乙基己酸酯)、二异硬脂酸丙二醇酯、二壬酸丙-45二醇酯(propylene-45 glycol dipelargonate)、二异硬脂酸丁二醇酯和二辛酸新戊二醇酯。
非常合适的油体也是三-和多羟基醇的酯,特别是植物甘油三酸酯,例如橄榄油、杏仁油、花生油、葵花籽油或者还有例如壬酸或油酸与季戊四醇的酯。
可以使用的脂肪酸甘油三酸酯是天然的植物油,例如橄榄油、葵花籽油、大豆油、花生油、油菜籽油、杏仁油、棕榈油,但也可是椰子油或棕榈壳油的液体部分,以及动物油例如牛骨油、牛油的液体部分,或者合成甘油三酸酯类,如那些通过甘油与具有8到22个碳原子脂肪酸的酯化作用所获得的产物,例如辛酸/癸酸混合物的甘油三酸酯,来自于工业级油酸或来自于棕榈酸/油酸混合物的甘油三酸酯。
根据本发明方法优选适合于做油成分的是那些在20℃的标准温度下为液体的单酯和二酯以及甘油三酸酯。但是,也可以使用在数量与所述式相符合的较高熔融的脂肪和酯类,这样该油成分的混合物在标准温度下保持为液态。
该油成分还可以含有次级数量最多不高于基于该油成分25重量%的烃油。适合的烃特别的是石蜡油,以及合成的烃例如液态聚烯烃,或者限定的烃类如烷基环己烷,例如1,3-二异辛基环己烷。
优选采用直链C8-C18-脂肪酸与直链或支链C6-C22-脂肪醇的酯以及支链C2-C13-羧酸与直链或支链C6-C22-脂肪醇的酯,例如,肉豆蔻酸肉豆蔻酯、棕榈酸肉豆蔻酯、硬脂酸肉豆蔻酯、异硬脂酸肉豆蔻酯、油酸肉豆蔻酯、山嵛酸肉豆蔻酯、芥酸肉豆蔻酯、肉豆蔻酸鲸蜡酯、棕榈酸鲸蜡酯、硬脂酸鲸蜡酯、异硬脂酸鲸蜡酯、油酸鲸蜡酯、山嵛酸鲸蜡酯、芥酸鲸蜡酯、肉豆蔻酸十八酯、棕榈酸十八酯、硬脂酸十八酯、异硬脂酸十八酯、油酸十八酯、山嵛酸十八酯、芥酸十八酯、肉豆蔻酸异十八酯、棕榈酸异十八酯、硬脂酸异十八酯、异硬脂酸异十八酯、油酸异十八酯、山嵛酸异十八酯、肉豆蔻酸油烯酯、棕榈酸油烯酯、硬脂酸油烯酯、异硬脂酸油烯酯、油酸油烯酯、山嵛酸油烯酯、芥酸油烯酯、肉豆蔻酸山嵛酯、棕榈酸山嵛酯、硬脂酸山嵛酯、异硬脂酸山嵛酯、油酸山嵛酯、山嵛酸山嵛酯、芥酸山嵛酯、肉豆蔻酸芥酯、棕榈酸芥酯、硬脂酸芥酯、异硬脂酸芥酯、油酸芥酯、山嵛酸芥酯和芥酸芥酯。
同样适合的是直链C6-C22-脂肪酸与支链醇特别是2-乙基己醇的酯,C18-C36-烷基羟基羧酸与直链或支链C6-C22-脂肪醇的酯,特别是苹果酸二辛酯,直链和/或支链脂肪酸与多元醇(例如丙二醇、二聚二元醇或三聚三元醇)和/或格尔伯特醇的酯,基于C6-C18-脂肪酸的甘油三酸酯,基于C6-C18-脂肪酸的液态甘油单/二/三酯混合物,C6-C22-脂肪醇和/或格尔伯特醇与芳香族羧酸特别是苯甲酸的酯,C2-C12-二元羧酸与具有1到22个碳原子的直链或支链醇或者与具有2到10个碳原子和2到6个羟基基团的多元醇的酯,植物油类,支链伯醇类,取代的环己烷类,直链和支链C6-C22-脂肪醇碳酸酯类,例如碳酸二辛酰酯类,基于具有6到18个、优选8到10个碳原子的脂肪醇的格尔伯特碳酸酯类,例如碳酸二乙基己基酯(TegosoftDEC,Goldschmidt GmbH),苯甲酸与直链和/或支链C6-C22-醇的酯,直链的或支链的、对称的或不对称的、每个烷基基团具有6到22个碳原子二烃基醚,例如,二辛酰醚,环氧化的脂肪酸酯与多元醇的开环产物,和/或脂肪烃或环烷烃类,例如,角鲨烷、角鲨烯或二烷基环己烷,硅油类,例如,环甲基硅酮或二甲基硅酮,还有丙氧基化的脂肪醇,例如PPG-15硬脂基醚、PPG-3-肉豆蔻基醚和PPG-14丁基醚。
原则上,合适的乳化剂是现有技术中为制备化妆品的O/W型和W/O型乳状液作为乳化剂使用的全部化合物。在此优选使用选自离子型和非离子型乳化剂中的至少一种乳化剂。
无须对完整性提出要求,从合适的乳化剂成分的已知各类中可以额外提到以下这些代表:
此处适合的非离子型乳化剂特别是含有亲脂性基团的基本分子的低烷氧基化物(oligoalkoxylate)。这些可衍生自特别是以下含有亲脂性基团的基本分子的类别:脂肪醇、脂肪酸、脂肪胺、脂肪酰胺、脂肪酸和/或脂肪醇的酯和/或醚、链烷醇酰胺、烷基酚和/或其与甲醛的反应产物,以及含有亲脂性基团的载体分子和低级醇化物的进一步反应产物。如所说明,各自的反应产物还可以至少是按比例封端的。多官能醇的偏酯和/或部分醚的实例特别是相应的与脂肪酸的偏酯,例如是丙三醇单和/或二酯型、乙二醇单酯,低聚合的多官能醇的相应偏酯、脱水山梨醇偏酯等,以及带有醚基团的相应化合物。这种偏酯和/或醚也可以特别是用于(低)烷氧基化反应的基本分子。
在该烷氧基化反应中,优选使用环氧乙烷、氧化丙烯、氧化丁烯或氧化苯乙烯。
特别优选的非离子型烷氧基化的乳化剂是:
2-30mol的环氧乙烷和/或0-5mol的氧化丙烯在具有8到22个碳原子的直链脂肪醇上、在具有12到22个碳原子的脂肪酸上、以及在具有8到15个碳原子烷基的烷基酚上的加成产物;具有6到22个碳原子的饱和的和不饱和的脂肪酸的丙三醇单酯和二酯以及脱水山梨醇单酯和二酯,及其环氧乙烷的加成产物;烷基基团中具有8到22个碳原子的烷基单-和低聚苷及其乙氧基化的类似物。
环氧乙烷和/或氧化丙烯在脂肪醇、脂肪酸、烷基酚、丙三醇单酯和二酯,以及脂肪酸的脱水山梨醇单酯和二酯之上的加成产物或蓖麻油上的加成产物是已知的、可商购的产品。这些是同系混合物,其平均烷氧基化的程度对应于环氧乙烷和/或氧化丙烯与用其进行加成反应的底物的数量之比;
梳子状或终端改性的有机硅聚醚,可以通过例如氢化硅烷化反应在已知条件下用优选2-100mol的环氧乙烷和/或氧化丙烯对烯烃官能化的聚醚的加成而获得。这种聚醚的终端羟基基团在此也可以是任选的烷基封端的(特别是甲基封端的)。
此外,可以使用的非离子型乳化剂还有:
多元醇以及特别是聚甘油酯,例如,聚甘油多聚蓖酸酯或聚甘油聚-12-羟基硬脂酸酯。同样适合的是两种或多种这些类别的化合物的混合物;
基于直链的、支链的、不饱和的或者饱和的C6/22-脂肪酸、蓖麻油酸和12-羟基硬脂酸和丙三醇、聚丙三醇、季戊四醇、二季戊四醇、糖醇(例如山梨糖醇)、烷基葡糖苷(例如甲基葡糖苷、丁基葡糖苷、月桂基葡糖苷)、以及多聚葡糖苷(例如纤维素)的偏酯;
聚硅氧烷-聚烷基-聚醚的共聚物和相应的衍生物;
C8/18-烷基单-和低聚苷、它们的制备及其作为表面活性物质的用途是已知的,例如US 3,839,318、US 3,707,535、US 3,547,828、DE-A 19 43 689、DE-A 20 36 472和DE-A1 30 01 064、以及EP-A 0 077 167。它们特别是通过将葡萄糖或者寡糖与具有8到18个碳原子的伯醇进行反应来制备的。
具有离子特点的适合的乳化剂是阴离子型、阳离子型和两性离子型乳化剂。阴离子型乳化剂包括水溶性阴离子基团,例如,羧酸盐、硫酸盐、磺酸盐或者磷酸盐基团,以及亲脂性基团。本领域技术人员熟知大量的适合皮肤的阴离子型表面活性剂并且它们可以商购获得。这些特别的是以其碱金属、铵盐或链烷醇铵盐形式存在的烷基硫酸盐或烷基磷酸盐、烷基醚硫酸盐、烷基醚羧酸盐、酰基肌氨酸盐以及以其碱金属或铵盐形式存在的磺基琥珀酸盐和酰基谷氨酸盐。还可以使用二-和三烷基磷酸盐,以及单-、二-和/或三-PEG烷基磷酸盐及其盐类。
还可以使用阳离子型乳化剂。这样,特别的是可以使用季铵化合物,例如烷基三甲基铵卤化物,例如鲸蜡基三甲基铵氯化物或溴化物或山嵛基三甲基铵氯化物,而且还有二烷基二甲基铵卤化物,例如二硬脂基二甲基铵氯化物。此外,可以使用单烷基酰胺基季铵盐(monoalkylamidoquat),例如,棕榈酰胺基丙基三甲基铵氯化物或相应的二烷基酰胺基季铵盐。另外,可以使用易于生物降解的季铵酯化合物,其通常是基于单-、二-、或三乙醇铵的季铵化脂肪酸酯。此外,烷基胍盐可以被用作阳离子型乳化剂。
此外,两性离子表面活性剂可以用作乳化剂。两性离子表面活性剂一词是用来指那些在分子中带有至少一个季铵基团和至少一个羧酸根基团和一个磺酸根基团的表面活性的化合物。特别适合的两性离子表面活性剂是所谓的甜菜碱类,诸如N-烷基-N,N-二甲基甘氨酸铵,例如椰油烷基二甲基甘氨酸铵、N-酰基氨丙基-N,N-二甲基甘氨酸铵,例如椰油酰基氨基丙基二甲基甘氨酸铵、以及2-烷基-3-羧甲基-3-羟乙基咪唑啉,每种情况下在该烷基或酰基基团中具有8到18个碳原子,以及椰油酰基氨乙基羟乙基羧甲基甘氨酸盐。特别优选以CTFA名称椰油酰氨丙基甜菜碱为人所知的脂肪酸酰氨衍生物。同样适合的乳化剂是两性表面活性剂。两性表面活性剂理解为指那些表面活性的化合物,它们除了分子中的C8/18-烷基或酰基基团外,还含有至少一个自由氨基和至少一个-COOH或-SO3H基团且它们能够形成内盐。适合的两性表面活性剂的实例是N-烷基甘氨酸、N-烷基丙酸、N-烷基氨基丁酸、N-烷基亚氨基二丙酸、N-羟乙基-N-烷基氨丙基甘氨酸、N-烷基牛磺酸、N-烷基肌氨酸、2-烷基氨丙酸和烷基氨乙酸,每种情况下在该烷基基团中具有约8到18个碳原子。特别优选的两性表面活性剂是N-椰油烷基氨基丙酸盐、椰油酰基氨乙基氨基丙酸盐和C12-18-酰基肌氨酸。除了这些两性乳化剂外,季铵盐乳化剂也是适合的,其中那些酯化季铵盐类型是特别优选的,优选甲基-季铵化的二脂肪酸三乙醇铵酯盐。
特别优选使用至少一种烷氧基化的非离子型乳化剂。本发明的一个特别优选的实施方案中,该非离子型碱性乳化剂或两种或多种非离子型乳化剂的组合可以与离子型乳化剂的成分相结合。
共同使用的油和乳化剂的量对于本发明方法不严苛并且与相关技术领域所用的配方相对应,并且为本领域技术人员所熟知。
除了所提到的油和乳化剂外,在此方面这些乳状液可以含有本领域技术人员熟知的常规的助剂和添加剂。这些包括,例如,稠度调节剂、增稠剂、蜡、UV光保护过滤剂、抗氧化剂、助水溶剂、除臭剂、止汗活性成分、驱昆虫剂、自晒黑剂、防腐剂、芳香油、染料,以及生物的或合成的化妆品活性组分(例如,在DE 10 2005 003 164.1的申请中所描述)。
附图说明
图1是通过动态光散射确定的如实例1中的O/W型乳状液的半径分布图。
图2是通过动态光散射确定的如实例2a(实心符号,实曲线)和2b(空心符号,虚线曲线)中的O/W型乳状液的半径分布图。
图3是根据实例2a(上)和2b(下)的步骤2生成的O/W型乳状液的光显微镜图像。
具体实施方式
实施例
实施例1:喷雾型化妆品洗剂
步骤1:
将36g棕榈酸辛酯(TEGOSOFTOP,Goldschmidt GmbH)、24g平均带有8个环氧乙烷单元(C12/14E8)的具有12到14个碳原子的多元醇的混合物、10g水和30g丙三醇组合在一起并搅拌。形成均匀且透明的在室温下为单一相的微乳状液相,其单一相区域(Winsor IV体系)是处于19℃和31℃之间的温度范围内。
步骤2:
在室温下将一份该微乳状液相搅拌到五份水中。形成一种均匀的、乳状的、细分散的O/W型乳状液。按这种方法获得的乳状液在-15℃、-5℃、5℃、室温和40℃下三个月的储存试验中是稳定的。
在步骤2中获得的O/W型乳状液的液滴大小在用二十倍量的水稀释到油/表面活性剂浓度为0.5%后采用动态光散射来确定。图1表明该液滴半径的较窄分布范围存在于15nm和25nm之间,而最大值是在19nm处。
实例2a:用于制备化妆品湿巾的浸渍洗剂
步骤1:
将36g棕榈酸辛酯(TEGOSOFTOP,Goldschmidt GmbH)、27gC12/14E8、12g水、18g丙三醇、3g防腐剂(EuxylK300,Schülke&Mayr(苯氧基乙醇、甲基-、乙基-、丁基-、丙基-和异丁基对羟基苯甲酸酯))和3g三月桂醇聚醚-4磷酸酯(trilaureth-4 phosphate)(HostaphatKL 340 D,Clariant)组合在一起并搅拌。形成一种均匀且透明的在室温下为单一相的微乳状液相,其单一相区域(WinsorIV体系)是处于8℃和43℃之间的温度范围内。
步骤2:
在室温下将该微乳状液相搅拌到大于五倍量的水中。形成一种均匀的、乳状的、细分散的O/W型乳状液。
在步骤2中获得的O/W型乳状液的液滴大小在用二十倍量的水稀释到油/表面活性剂浓度约为0.5%后采用动态光散射的方式来确定。图2表明该液滴半径的较窄分布范围存在于55nm和110nm之间,而最大值是在82nm处。过量的乳化剂形成胶束,其半径在15nm和20nm之间。
为了对照,如在实例2a中那样制备了一种O/W型乳状液,但没有通过PIT法加丙三醇,如在
实例2b
步骤1:
将36g棕榈酸辛酯(TEGOSOFTOP,Goldschmidt GmbH)、27gC12/14E8、12g水、3g防腐剂(EuxylK 300,Schülke&Mayr(苯氧基乙醇、甲基-、乙基-、丁基-、丙基-和异丁基对羟基苯甲酸酯))和3g三月桂醇聚醚-4磷酸酯(HostaphatKL 340D,Clariant)组合在一起并搅拌。在室温下形成一种混浊乳状液,短时间后该乳状液分离成两相的Winsor I类型体系。经加热和搅拌高于70℃形成单相的、均匀且透明的微乳状液相,其单一相区域(Winsor IV体系)是处于70℃和85℃之间的温度范围内。
步骤2(PIT法):
在室温下该微乳状液相在水浴中骤冷。形成一种均匀的、透明的、细分散的O/W型乳状液。
在步骤2中获得的O/W型乳状液如同实例2a一样被稀释到油/表面活性剂浓度约为0.5%,并且该液滴大小通过动态光散射的方式来确定。图2表明液滴半径的较宽的分布出现在50nm和490nm之间,而最大值是在110nm处。
显微镜法:
在40倍放大率的光学显微镜下观察实例1和2的步骤2中制备的该细分散的O/W型乳状液。图3表明通过如实例2b的PIT法制备的乳状液除气泡外含有的液滴处于亚微米级范围,然而在通过如实例2a的PSQ法制备的乳状液的情况下,因为该液滴的大小低于该显微镜的分辨率而形成均匀的图像。
Claims (17)
1.一种制备包含油、水和至少一种乳化剂的细分散的水包油乳状液的方法,其包括步骤
A)通过将油、水、至少一种乳化剂和至少一种成序物质进行混合来制备混合物2,该混合物包含油、水、至少一种乳化剂和至少一种成序物质,其中该混合物(Winsor IV体系)的相转变温度PIT2小于混合物1(Winsor IV体系)的相转变温度PIT1,所述混合物1不具有成序物质而在其它方面与混合物2的组成相同,
以及随后的步骤
B)在混合物2中加入稀释剂将该混合物转化为乳状液3,其中选择所加入的稀释剂的量,使在预先给定的温度下得到的乳状液3不是处在Winsor IV相的区域之内。
2.如权利要求1的方法,其中制备一种在环境温度、加工温度或者使用温度下在动力学方面稳定的乳状液作为乳状液3。
3.如权利要求1或2的方法,其中所述细分散的乳状液3具有小于1μm的平均粒径。
4.如权利要求1到3中至少一项的方法,其中制备微乳状液作为混合物2。
5.如权利要求1到4中至少一项的方法,其中,在步骤B)中,所加入的所述稀释剂的量应使所述乳状液3转变到Winsor IV相区域的转变温度至少比环境温度、加工温度或使用温度高1 K。
6.如权利要求1到5中至少一项的方法,其中,在步骤B)中,将至少1重量份的稀释剂加入到为1重量份的所述混合物2中。
7.如权利要求1到6中至少一项的方法,其中步骤B)中所使用的稀释剂是水或者水溶液。
8.如权利要求1到7中至少一项的方法,其中制备一种在环境温度、加工温度或者使用温度下在动力学方面稳定的乳状液作为乳状液3,其中,在步骤A)中,通过常规方法制备水、油、至少一种乳化剂和至少一种成序物质的混合物,所述混合物在热动力学方面稳定的并且宏观上是均相的,并且其中步骤A)是在低于未加入所述成序物质的混合物1的相转变温度PIT1的温度下进行的。
9.如权利要求1到7中至少一项的方法,其中制备一种在环境温度、加工温度或者使用温度下在动力学方面稳定的乳状液作为乳状液3,其中步骤A)包含将至少一定量的至少一种成序物质混合到混合物1中,该混合物包含油、水和至少一种乳化剂并且具有相转变温度PIT1(Winsor IV体系),这样获得混合物2,其相转变温度(Winsor IV体系)PIT2小于PIT1。
10.如权利要求1到7中至少一项的方法,其中制备一种在环境温度、加工温度或者使用温度下在动力学方面稳定的乳状液做为乳状液3,其中,在步骤A)中,通过常规方法在不超过原始相转变温度的情况下,使用水、油、至少一种乳化剂和至少一种成序物质来制备与过量的水相平衡的W/O型微乳状液相(类型WII)。
11.如权利要求1到10中至少一项的制备乳状液的方法在制备化妆品的、皮肤病的、药学的或农用化学的制品中的用途。
12.如权利要求1到10中至少一项的制备乳状液的方法在制备用于面部护理及身体护理、婴儿护理、日晒保护、卸妆用品、止汗/除臭的浸渍湿巾或可喷雾制品中的用途。
13.如权利要求1到10中至少一项的制备乳状液的方法在制备用于家庭、运动、休闲和工业领域中的应用的水溶液配方的用途。
14.如权利要求1到10中至少一项的制备乳状液的方法在制备用于纺织品、皮革、塑料、金属和非金属表面的清洁和护理的浸渍湿巾或者可喷雾制品的用途。
15.如权利要求1到10中至少一项的制备乳状液的方法在制备包含油类和任选的其他活性物质的农用化学品配方的可喷雾制品的用途。
16.通过如权利要求1到10中至少一项的方法可获得的一种细分散的水包油乳状液。
17.如权利要求16的乳状液,所述乳状液具有小于1μm的粒径。
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US10370493B2 (en) | 2016-01-29 | 2019-08-06 | Evonik Degussa Gmbh | Polyglycerol alkoxylate esters and preparation and use thereof |
DE102016204268A1 (de) * | 2016-03-15 | 2017-09-21 | Henkel Ag & Co. Kgaa | Waschmittelzusammensetzung |
BR112019003247B1 (pt) | 2016-08-18 | 2022-01-25 | Evonik Operations Gmbh | Ésteres de poliglicerol reticulados, seu método de preparo e uso e preparações cosméticas ou farmacêuticas |
WO2019048556A1 (en) | 2017-09-06 | 2019-03-14 | Evonik Degussa Gmbh | MICROEMULSION COMPRISING A QUATERNARY AMMONIUM COMPOUND, ESPECIALLY FOR THE PRODUCTION OF SOFTENER FORMULATIONS |
WO2019057754A1 (de) | 2017-09-25 | 2019-03-28 | Evonik Degussa Gmbh | Lagerstabile konzentrate enthaltend polysiloxane und deren einsatz vorzugsweise in textil-pflegenden zusammensetzungen |
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US3547828A (en) * | 1968-09-03 | 1970-12-15 | Rohm & Haas | Alkyl oligosaccharides and their mixtures with alkyl glucosides and alkanols |
US3707535A (en) * | 1969-07-24 | 1972-12-26 | Atlas Chem Ind | Process for preparing mono- and polyglycosides |
US3839318A (en) * | 1970-09-27 | 1974-10-01 | Rohm & Haas | Process for preparation of alkyl glucosides and alkyl oligosaccharides |
DE19530220A1 (de) * | 1995-08-17 | 1997-02-20 | Henkel Kgaa | Translucente Antitranspirantien/Deodorantien |
US6984269B2 (en) * | 2000-05-24 | 2006-01-10 | Imperial Chemical Industries Plc | Cleaning surfaces |
US7182950B2 (en) * | 2002-06-12 | 2007-02-27 | Nutralease Ltd. | Nano-sized self-assembled liquid dilutable vehicles |
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2006
- 2006-07-01 DE DE102006030532A patent/DE102006030532A1/de not_active Withdrawn
-
2007
- 2007-05-21 IL IL183355A patent/IL183355A0/en unknown
- 2007-05-30 EP EP07010663A patent/EP1882516A3/de not_active Withdrawn
- 2007-05-31 CA CA002590723A patent/CA2590723A1/en not_active Abandoned
- 2007-06-20 US US11/820,649 patent/US20080004357A1/en not_active Abandoned
- 2007-06-25 JP JP2007166647A patent/JP2008013554A/ja not_active Withdrawn
- 2007-06-29 CN CNA200710126370XA patent/CN101121102A/zh active Pending
Cited By (5)
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CN101683593B (zh) * | 2008-08-15 | 2014-10-08 | 赢创戈尔德施米特有限公司 | 纳米乳液、其制备方法及其用途 |
CN105686973A (zh) * | 2014-11-25 | 2016-06-22 | 金红叶纸业集团有限公司 | 一种卸妆乳液及湿巾 |
CN105686973B (zh) * | 2014-11-25 | 2020-10-23 | 金红叶纸业集团有限公司 | 一种卸妆乳液及湿巾 |
WO2017085508A1 (en) | 2015-11-19 | 2017-05-26 | Sofia University "St. Kliment Ohridski" | A method for the preparation of particles with controlled shape and/or size |
CN114867467A (zh) * | 2019-12-20 | 2022-08-05 | 费森尤斯卡比奥地利有限公司 | 用于产生水包油乳剂的方法 |
Also Published As
Publication number | Publication date |
---|---|
US20080004357A1 (en) | 2008-01-03 |
EP1882516A2 (de) | 2008-01-30 |
DE102006030532A1 (de) | 2008-01-03 |
JP2008013554A (ja) | 2008-01-24 |
EP1882516A3 (de) | 2010-12-22 |
IL183355A0 (en) | 2007-09-20 |
CA2590723A1 (en) | 2008-01-01 |
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