CN106176326A - 制造微胶囊的方法 - Google Patents
制造微胶囊的方法 Download PDFInfo
- Publication number
- CN106176326A CN106176326A CN201610824985.9A CN201610824985A CN106176326A CN 106176326 A CN106176326 A CN 106176326A CN 201610824985 A CN201610824985 A CN 201610824985A CN 106176326 A CN106176326 A CN 106176326A
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- CN
- China
- Prior art keywords
- isocyanates
- consumer products
- microcapsule
- emulsion
- diisocyanate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
本申请描述一种制造微胶囊的方法,所述微胶囊包含由聚脲制成的壳,所述壳在其内部包围香料油核,其中该壳由乳液形式的两种结构上不同的二异氰酸酯的反应获得。
Description
本申请是申请日为2011年06月24日、申请号为201180028710.X、发明名称为“制造微胶囊的方法”的中国专利申请的分案申请。
本申请涉及制造微胶囊的方法和那些微粒在消费产品中的用途。
微胶囊为由核以及包围该核的壁材料构成的粉末或颗粒,其中核为固体、液体或气体物质,其被固体的,通常为聚合物的壁材料包围。它们可以为固体,即由单一材料构成。微胶囊具有平均1至1000μm的直径。
已知许多壳材料用于制造微胶囊。壳可以由天然、半合成或合成材料构成。天然壳材料为例如阿拉伯树胶,琼脂,琼脂糖,麦芽糊精,藻酸或其盐,例如藻酸钠或藻酸钙,脂肪和脂肪酸,鲸蜡醇,胶原,壳聚糖,卵磷脂,明胶,白蛋白,虫胶,多糖,例如淀粉或葡聚糖,多肽,蛋白水解物,蔗糖和蜡。半合成壳材料特别为化学改性的纤维素,特别是纤维素酯和纤维素醚,例如醋酸纤维素,乙基纤维素,羟丙基纤维素,羟丙基甲基纤维素和羧甲基纤维素,以及淀粉衍生物,特别是淀粉醚和淀粉酯。合成壳材料为例如聚合物,例如聚丙烯酸酯,聚酰胺,聚乙烯醇或聚乙烯吡咯烷酮。
就关注的直径、粒度分布和物理和/或化学性能而言,根据壳材料的类型和制造方法,在各情况下形成具有不同性能的微胶囊。
因此持续需要研发新颖的制造方法,以能够提供具有特定性能的微胶囊。
因此本申请的第一个主题涉及制造微胶囊的方法,该微胶囊包含壳和香料油核,其中使保护性胶体的水溶液和至少两种结构上不同的至少双官能的异氰酸酯(A)和(B)的混合物在所述油中的溶液合并在一起,直到形成乳液,然后向其中加入至少双官能的胺,并然后将其加热到至少60℃的温度,直到形成微胶囊,其中该异氰酸酯(B)选自阴离子改性的异氰酸酯或含聚氧化乙烯的异氰酸酯或这些类型的混合物,并且该异氰酸酯(A)是不带电的,但是不是含聚乙烯的异氰酸酯。
该方法具有以下优点:可以以定向方式制造预定粒度或粒度分布的微胶囊,这里可能特别是制造直径为10至60μm的较小微胶囊。另外,获得具有更大机械稳定性的胶囊。这里,特别是获得其壳对液体成分仅仅具有低渗透性的那些胶囊。
原则上,总是制造保护性胶体的水溶液,为此,将异氰酸酯(A)和(B)溶于香料油中,所述香料油随后形成微胶囊的核;然后添加胺组分,并将混合物加热直到形成乳液。使异氰酸酯与胺组分反应的温度必须为至少60℃,但是更好为70℃,但是优选为75至90℃和特别是85至90℃,以确保足够快的反应进程。
这里,可以优选提高各步骤中的温度(例如在各情况下为提高10℃),直到反应完成之后,将分散体冷却至室温(21℃)。反应时间通常取决于使用的量和温度。但是通常,形成微胶囊的升高的温度确定为在大约60分钟至6小时或至多8小时之间。
根据本教导,胺的添加也优选与例如使用搅拌装置的能量输入一起进行。
为了形成本方法中的乳液,由本领域技术人员已知的方法将各混合物乳化,例如通过使用合适的搅拌器搅拌将能量引入混合物中,直到混合物乳化。优选使用含水碱调节pH,优选使用氢氧化钠溶液(例如5wt%浓度)。
对于本方法必要的是使用至少两种结构上不同的异氰酸酯(A)和(B)。这些可以在本方法中以混合物或彼此单独的形式加入到包含保护性胶体的含水预混物(1)中,然后乳化并与胺反应。也可以计量供给(meter)(A)和(B)的混合物,以及在不同的时间分别计量供给单独的异氰酸酯(A)和(B)。
在一个优选的实施方案中,该方法如下进行:
(a)由水和保护性胶体制备预混物(I);
(b)将该预混物调节至5至12的pH;
(c)由香料油与异氰酸酯(A)和(B)一起制备另一种预混物(II);
(d)将两种预混物(I)和(II)合并在一起,直到形成乳液和
(e)然后将至少双官能的胺计量供给到来自步骤(d)的乳液中和
(f)然后将乳液加热到至少60℃的温度,直到形成微胶囊。
可能有利的是将步骤(b)中的pH调节至8至12。这里适用的是含水碱,优选氢氧化钠水溶液。优选通过使用合适的搅拌器来确保步骤(d)中,而且还有步骤(e)中的乳液形成。
另一个同样优选的实施方案设想(envisage):
(a)由水和保护性胶体制备预混物(I);
(b)将该预混物调节至5至12的pH;
(c)由香料油与异氰酸酯(A)制备另一种预混物(II);
(d)通过搅拌由预混物(I)和(II)形成乳液,并且向其中
(e)添加第二种异氰酸酯(B),然后将乳液的pH调节至5至10的值;
(f)然后将至少双官能的胺计量供给到来自步骤(e)的乳液中和
(g)然后加热到至少60℃的温度,直到形成微胶囊。
在该方法中,在添加胺并进行制造微胶囊的反应之前将异氰酸酯(A)和(B)分别加入到保护性胶体中。如同步骤(e)中的混合的乳液形成在这里同样优选通过使用搅拌装置发生。
步骤(e)中的pH优选调节至7.5至9.0的值。对于步骤(b),该值也可以调节至8至12。对于该目的适用的特别是含水碱,优选氢氧化钠水溶液。
微胶囊
在本教导的上下文中,微胶囊具有由至少两种不同的至少双官能的异氰酸酯与胺,优选与聚胺的反应产物制成的壳。该反应为异氰酸酯与胺之间的缩聚,产生聚脲衍生物。
微胶囊可以以水分散体的形式存在,这些分散体在胶囊中的重量百分率优选为15至45wt%,并优选为20至40wt%。微胶囊具有1至500μm,并优选1至50μm或5至25μm的平均直径。
香料油的量可以为10至95wt%,基于胶囊重量,其中70至90wt%的百分率可能是有利的。作为该方法的结果,获得典型地具有20:1至1:10,优选5:1至2:1和特别是4:1至3:1的核/壳比率(w/w)的胶囊。
由本方法制造的微胶囊优选不含甲醛。
保护性胶体
在异氰酸酯与胺反应期间,必须存在保护性胶体。其优选为聚乙烯吡咯烷酮(PVP)。保护性胶体为悬浮液或分散体形式的聚合物体系,其防止乳化、悬浮或分散的物质在一起凝结成块(附聚、凝聚、絮凝)。溶剂化期间,保护性胶体结合大量的水,并在水溶液中产生高粘度,取决于浓度。在这里描述的方法的上下文中,保护性胶体也可以具有乳化性能。保护性胶体水溶液同样优选利用搅拌制备。
保护性胶体可以但并非必须为胶囊壳的成分,其量这里可以为0.1至至多15wt%,但是优选为1至5wt%和特别是1.5至3wt%,基于胶囊重量。
异氰酸酯
异氰酸酯为在游离状态与氰酸互变异构的异氰酸(HNCO)的N-取代的有机衍生物(R-N=C=O)。有机异氰酸酯为其中异氰酸酯基团(-N=C=O)与有机基团键合的化合物。多官能的异氰酸酯为在分子中具有两个或多个异氰酸酯基团的那些化合物。
根据本发明,使用至少双官能的,优选多官能的异氰酸酯,即所有的芳族、脂环族和脂族异氰酸酯都是合适的,条件是它们具有至少两个反应性异氰酸酯基团。
合适的多官能的异氰酸酯优选包含平均2至最多4个NCO基团。优选使用二异氰酸酯,即具有一般结构O=C=N-R-N=C=O的异氰酸的酯,其中R'这里为脂族、脂环族或芳族基团。
合适的异氰酸酯为例如1,5-亚萘基二异氰酸酯,4,4'-二苯基甲烷二异氰酸酯(MOI),氢化MDI(H12MDI),亚二甲苯基二异氰酸酯(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-亚苯基二异氰酸酯,1,4-亚苯基二异氰酸酯,甲苯二异氰酸酯(TDI)的异构体,任选地以混合物的形式,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酯,还有具有反应性卤素原子的多异氰酸酯,例如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,3,3-双氯甲醚4,4'-二苯基二异氰酸酯。含硫的多异氰酸酯例如通过使2mol六亚甲基二异氰酸酯与1mol硫二甘醇或二羟基二己基硫醚反应获得。其它合适的二异氰酸酯为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和二聚物脂肪酸二异氰酸酯。
本方法的一个必要特征为必须使用两种结构上不同的异氰酸酯(A)和(B)。
合适的(A)类的异氰酸酯为至少双官能的化合物(即包含至少两个异氰酸酯基团-N=C=O的化合物)。
典型的代表可以为六亚甲基二异氰酸酯(HDI),或其衍生物,例如HDI缩二脲(例如以Desmodur N3200市售),HDI三聚物(以Desmodur N3300市售)或另外二环己基甲烷二异氰酸酯(以Desmodur W市售)。甲苯2,4-二异氰酸酯或二苯基甲烷二异氰酸酯也是合适的。
第二种类型(B)的异氰酸酯与类型(A)的异氰酸酯在结构上不同,特别地,类型(B)的异氰酸酯必须为阴离子改性的异氰酸酯或含聚氧化乙烯的异氰酸酯(或这两种异氰酸酯类型的任何所需混合物)。
阴离子改性的异氰酸酯本身是已知的。优选地,这些类型(B)的异氰酸酯在分子中包含至少两个异氰酸酯基团。优选存在一个或多个磺酸基团作为阴离子基团。优选地,选择类型(B)的异氰酸酯,其为己烷1,6-二异氰酸酯(HDI)的低聚物,特别是三聚物。这些阴离子改性的异氰酸酯的商业产品例如以品牌Bayhydur(Bayer)已知,例如Bayhydur XP。
含聚氧化乙烯的异氰酸酯(具有至少两个异氰酸酯基团)也是已知的,并且例如在US5,342,556中描述。一些异氰酸酯在水中是自乳化的,这在本方法的上下文中可能是有利的,因为可以省去单独的乳化步骤。
两种异氰酸酯(A)和(B)的重量比优选调节为10:1至1:10,但是特别为5:1至1:5,以及特别为3:1至1:1。
也可使用不同的类型(A)和(B)的异氰酸酯的混合物。除异氰酸酯(A)和(B)之外,也可以在本发明的方法中另外使用其它异氰酸酯。
但是优选仅使用阴离子改性的异氰酸酯作为本方法中的组分(B)。
胺
至少双官能的胺,但是优选聚乙烯亚胺(PEI)用作本发明的方法中的其它组分。聚乙烯亚胺通常为在其主链中存在彼此在各情况下由两个亚甲基分隔的NH基团的聚合物:
聚乙烯亚胺属于聚电解质和络合聚合物。具有相对高百分率的伯氨基的短链线性聚乙烯亚胺,即通式H2N[CH2-CH2-NH]nH(n=2:二亚乙基三胺;n=3;三亚乙基四胺;n=4:四亚乙基五胺)的产物有时被称为聚乙烯胺或聚亚烷基聚胺(polyalkylenepolyamines)。
在本发明的方法中,优选使用具有至少500g/mol,优选600至30000或650至25000g/mol和特别是700至5000g/mol或850至2500g/mol的分子量的聚乙烯亚胺。
保护性胶体
在本发明的方法中,PVP用作保护性胶体。PVP为聚乙烯吡咯烷酮(亦称聚维酮)的缩写。根据Chemie Lexikon,Online-edition 3.6,2010,它们为[聚(1-乙烯基吡咯烷-2-酮)],即符合以下通式的聚合物(乙烯基聚合物):
标准商业化的聚乙烯吡咯烷酮具有通过说明(stating)K值表征的大约2500-750000g/mol范围内的摩尔质量,并具有取决于K值的130至175℃的玻璃化转变温度。它们以白色吸湿性粉末或水溶液的形式提供。
在本发明的方法中,优选使用具有高分子量,即大于400000g/mol并优选500000g/mol至2000000g/mol的PVPs。此外优选的是聚乙烯吡咯烷酮具有大于60,优选大于75和特别是大于80的K值。K值的优选范围为65至90。
香料油
使用如上所述方法制造的微胶囊包含香料油核。异氰酸酯应可溶于该形成核的油。
术语“香料油”表示一种或多种芳香剂组分,任选与合适的溶剂、稀释剂、载体或其它助剂的混合物,其是用来赋予消费产品所需的气味。
如本领域技术人员明了的,可以使用各种芳香剂成分,这里提供详细清单并非必要。可以用来制备这样的香料油的示例性芳香剂组分及其混合物可以包括天然产物,例如精油、净油、香膏、树脂、浸膏等,和合成芳香剂组分,例如烃类、醇类、醛类、酮类、醚类、酸类、酯类、缩醛类、缩酮类、腈类等,包括饱和与不饱和化合物,脂族、碳环和杂环化合物。这样的芳香剂组分的实例为:香叶醇,乙酸香叶酯,芳樟醇,乙酸芳樟酯,四氢化芳樟醇,香茅醇,乙酸香茅酯,二氢月桂烯醇,乙酸二氢月桂烯酯,四氢月桂烯醇,萜品醇,乙酸萜品酯,诺卜醇,乙酸诺卜酯,2-苯乙醇,乙酸2-苯基乙酯,苄醇,乙酸苄酯,水杨酸苄酯,苯甲酸苄酯,乙酸苏合香酯,水杨酸戊酯,二甲基苄基甲醇,乙酸三氯甲基苯甲酯,乙酸对-叔丁基环己酯,乙酸异壬基酯,乙酸岩兰草酯,岩兰草醇,α-正戊基肉桂醛,α-己基肉桂醛,2-甲基-3-(对-叔丁基苯基)丙醛,2-甲基-3-(对-异丙基苯基)丙醛,3-(对-叔丁基苯基)丙醛,乙酸三环癸烯基酯,丙酸三环癸烯基酯,4-(4-羟基-4-甲基戊基)-3-环己烯甲醛,4-(4-甲基-3-戊烯基)-3-环己烯甲醛,4-乙酰氧基-3-戊基四氢吡喃,二氢茉莉酮酸甲酯,2-正庚基环戊酮,3-甲基-2-戊基环戊酮,正癸醛,正十二醛,9-癸烯醇-1,异丁酸苯氧基乙酯,苯乙醛二甲缩醛,苯乙醛二乙缩醛,香叶腈,香茅腈,乙酸柏木酯,3-异莰基环己醇,柏木甲醚,异长叶烷酮,茴香醛腈,茴香醛,胡椒醛,香豆素,丁子香酚,香草醛,二苯醚,羟基香茅醛,紫罗兰酮,甲基紫罗兰酮,异甲基紫罗兰酮,鸢尾酮,顺式3-己烯醇及其酯,二氢化茚麝香香料,四氢萘麝香香料,异色满麝香香料,大环酮,大环内酯麝香香料,十三烷二酸亚乙基酯,芳族硝基麝香香料。香料油也可以包含包括以上特别提及的那些中的任一种的任何芳香剂成分的前体或前香料。
如上所述的芳香剂的合适的溶剂、稀释剂或载体为例如:乙醇,异丙醇,二乙二醇单乙醚,一缩二丙二醇,邻苯二甲酸二乙酯,柠檬酸三乙酯等。通常和香料油一起使用的载体材料、稀释剂、溶剂和其它助剂的实例可以在例如S.Arctander,‘Perfume and FlavourMaterials of Natural Origin’,Elizabeth,N.J.,1960,S.Arctander,‘Perfume andFlavour Chemicals’,Vol.I和II,Allured Publishing Corporation,Carol Stream,1994,和J.M.Nikitakis(Ed.),‘CTFA Cosmetic Ingredient Handbook’,1st ed.,TheCosmetic,Toiletry and Fragrance Association,Inc.,Washington,1988中找到。
本发明进一步提供水分散体,基于分散体总重量,其包括5至50wt%,优选15至40wt%的可以由上述方法制造的微胶囊。进一步优选的范围为20至35wt%。这些水分散体优选直接从如上所述的方法获得。
由本方法获得的微胶囊分散体可用于各种消费产品的芳香剂。这里不能给出消费产品的详细清单,本领域技术人员将理解这种微胶囊的应用范围。说明性的消费产品的实例包括所有洗涤用品,包括软化剂,液体洗涤剂和粉末洗涤剂;所有个人护理和毛发护理用品,包括香波,调理剂,梳理乳剂,免洗型调理剂(leave on conditioners),定型乳剂,皂,身体乳剂等;除臭剂和防汗剂;和所有家庭清洁用品。
本发明进一步优选地提供无甲醛微胶囊,其包含香料油核和至少两种不同的至少双官能的异氰酸酯(A)和(B)与至少双官能的胺的反应产物的壳,其中异氰酸酯(B)必须为阴离子改性的异氰酸酯或含聚氧化乙烯的异氰酸酯或所述类型的混合物,条件是在微胶囊制造期间,异氰酸酯(A)和(B)之间的重量比为10:1至1:10。优选地,可以调节上述重量比,其中3:1至1:1的比率可以赋予特殊的重要性。
这些微胶囊优选地具有1至50μm的直径,和优选地2至45μm的直径。它们可以以水分散体的形式存在,其中胶囊的百分率可以为1至90wt%,但是优选为5至50wt%。
现在进行一系列实施例,这些实施例起到说明本发明的作用。
实施例1-包封
当将Desmodur W(Bayer)和Bayhydur XP2547(Bayer)分别以12.6%和3.4%的水平加入到香料油中时制备油相。
以4.5%的水平向水中加入Luviskol k90(BASF),制备水相(溶液S1)。通过以0.5%添加pH=10的缓冲剂,将溶液的pH调节为10。
以20%的水平向水中加入Lupasol PR8515(BASF),制备水相(溶液S2)。
根据以下步骤制备胶囊:
在装有以1000rpm工作的MIG搅拌器的1L反应器中将300g的油相与600g的溶液S1混合形成水包油乳液。混合30分钟之后,经1分钟添加100g的溶液S2。30分钟之后,将浆料加热到至多70℃(1H),然后在70℃保持2H,然后加热到80℃并在80℃保持1H,然后加热到85℃并在85℃保持1H,然后冷却至70℃并在70℃保持1H,随后最终在25℃冷却。
实施例2-毛发护理用品
使用标准毛发规程(protocols),用0.2%的芳香剂剂量,进行假发测试(HairSwitch testing)。根据实施例1中给出的配方制备胶囊。芳香剂组合物在下表中给出。通过与无芳香剂(无包封的油)进行直接比较,评价胶囊的性能。
用于香波的规程
●使用的假发:欧洲人毛发,原生,未破坏(但是重复使用若干次)
●用温水打湿假发并放置在称重天平上
●使用注射器沿着假发挤出2.5g的香波
●将香波按摩进入假发30秒
●使起泡的假发静置吸收1分钟,随后在流动的手感热水下清洗约30秒
●在两指之间挤压假发以去除过量水分
●干燥假发;悬挂空气干燥或立刻使用毛发干燥器吹气干燥
●将空气干燥的试样悬挂在无气味的房间中24小时
●使用十点等级评价梳理前后的各假发:0=无气味,9=非常强,
用于毛发调理剂的规程:
对于调理剂按照相同的规程,除了在施加调理剂之前在无香的香波中预先清洗假发之外
实施例3-织物护理用品
根据实施例1中给出的配方制备胶囊。芳香剂组合物在下表中给出。通过基于新制备的试样和在37℃存储1个月之后,与无芳香剂(无包封的油)的直接比较,评价胶囊的性能。
用于织物洗涤剂用品的规程
洗涤条件:100g的加香的粉末洗涤剂,1kg的棉毛巾,欧洲洗衣机。以标准粉末洗涤剂基料中的0.5%的芳香剂水平制备加香的试样,使用的洗涤条件如下:
-洗涤物总重量为1kg
-欧洲机器
-揉搓前后进行评价,挂干干燥和转筒干燥的毛巾,使用5点等级:0=无气味;5=非常强
用于织物软化剂用品的规程
以0.5%的芳香剂水平,在标准织物调理剂基料中制备加香的试样,所述基料包括13%的购自Akzo的Quaternium ammonium ARQUAD 2HT75,0.3%的购自Dow Corning的Silicone Dow Corning DB110,0.6%的购自Merck的CaCl2和0.15%的购自Henkel的Bronidox,使用的洗涤条件如下:
-洗涤物总重量为0.2kg
-用未加香的洗涤粉末(90g的标准内部Givaudan洗涤粉末)洗涤,之后添加35g的加香的织物调理剂
-欧洲机器
-对揉搓前后,挂干干燥和转筒干燥的毛巾进行评价,使用5点等级:0=无气味;5=非常强
Claims (13)
1.消费产品,选自洗涤用品、个人护理和毛发护理用品和家庭清洁用品,所述洗涤用品包括软化剂、液体洗涤剂和粉末洗涤剂;所述个人护理和毛发护理用品包括香波、调理剂、梳理乳剂、免洗型调理剂、定型乳剂、皂、身体乳剂、除臭剂和防汗剂;该消费产品包含微胶囊,该微胶囊包括香料油核和至少两种不同的至少双官能的异氰酸酯(A)和(B)与至少双官能的胺的反应产物的壳,其中该异氰酸酯(B)必须为阴离子改性的异氰酸酯或含聚氧化乙烯的异氰酸酯或这些类型的混合物,条件是在制造该微胶囊期间,所述异氰酸酯(A)和(B)之间的重量比为10:1至1:10。
2.根据权利要求1的消费产品,其中该微胶囊具有1至50μm的直径。
3.根据权利要求1或权利要求2的消费产品,其中微胶囊以水分散体的形式存在。
4.根据在前权利要求任一项的消费产品,其中该微胶囊由一种方法制造,在该方法中使保护性胶体的水溶液和至少两种结构上不同的至少双官能的二异氰酸酯(A)和(B)的混合物在香料油中的溶液合并在一起,直到形成乳液,然后向其中添加至少双官能的胺,并然后将其加热到至少60℃的温度,直到形成微胶囊,其中该异氰酸酯(B)选自阴离子改性的异氰酸酯或含聚氧化乙烯的异氰酸酯,并且该异氰酸酯(A)是不带电的并且不是含聚氧化乙烯的异氰酸酯。
5.根据权利要求4的消费产品,其中聚乙烯吡咯烷酮用作保护性胶体。
6.根据权利要求4或权利要求5的消费产品,其中该异氰酸酯(A)选自己烷1,6-二异氰酸酯,己烷1,6-二异氰酸酯缩二脲或己烷1,6-二异氰酸酯的低聚物,特别是其三聚物或者二环己烷亚甲基二异氰酸酯。
7.根据权利要求4-6任一项的消费产品,其中该异氰酸酯(B)选自阴离子改性的二异氰酸酯,其在分子中包含至少一个磺酸基,优选氨基磺酸基。
8.根据权利要求4-7任一项的消费产品,其中使用的至少双官能的胺为聚乙烯亚胺。
9.根据权利要求4-8任一项的消费产品,其中所述异氰酸酯(A)和(B)的重量比为10:1至1:10,优选为5:1至1:5,特别是3:1至1:1。
10.根据权利要求4-9任一项的消费产品,其中所述微胶囊的核-壳比率(w/w)为20:1至1:10,优选为5:1至2:1,特别是4:1至3:1。
11.根据权利要求4-10任一项的消费产品,其中形成微胶囊的方法根据以下步骤进行:
(a)由水和保护性胶体制备预混物(I);
(b)将该预混物调节至5至12的pH;
(c)由香料油与异氰酸酯(A)和(B)一起制备另一种预混物(II);
(d)将两种预混物(I)和(II)合并在一起,直到形成乳液和
(e)然后将至少双官能的胺计量供给到来自步骤(d)的乳液中和
(f)然后将乳液加热到至少60℃的温度,直到形成微胶囊。
12.根据权利要求11的消费产品,其中将方法步骤(b)中的pH调节至8至12。
13.如权利要求1-12任一项中定义的微胶囊用于使消费产品发香的用途,所述消费产品选自洗涤用品、个人护理和毛发护理用品和家庭清洁用品,所述洗涤用品包括软化剂、液体洗涤剂和粉末洗涤剂;所述个人护理和毛发护理用品包括香波、调理剂、梳理乳剂、免洗型调理剂、定型乳剂、皂、身体乳剂、除臭剂和防汗剂。
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2011
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- 2011-06-24 US US13/699,419 patent/US20130089590A1/en not_active Abandoned
- 2011-06-24 CN CN201610824985.9A patent/CN106176326A/zh active Pending
- 2011-06-24 BR BR112012033017-9A patent/BR112012033017B1/pt active IP Right Grant
- 2011-06-24 WO PCT/EP2011/060599 patent/WO2011161229A1/en active Application Filing
- 2011-06-24 KR KR1020137001659A patent/KR101833084B1/ko active IP Right Grant
- 2011-06-24 JP JP2013515906A patent/JP6078464B2/ja active Active
- 2011-06-24 EP EP11729951.1A patent/EP2585028B1/en active Active
- 2011-06-24 CN CN201180028710XA patent/CN102958497A/zh active Pending
- 2011-06-24 ES ES11729951.1T patent/ES2602440T3/es active Active
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2012
- 2012-12-03 ZA ZA2012/09124A patent/ZA201209124B/en unknown
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2014
- 2014-12-04 US US14/560,700 patent/US20150140050A1/en not_active Abandoned
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CN109568154A (zh) * | 2018-12-28 | 2019-04-05 | 北京航洋健康科技有限公司 | 一种胶囊壳体及由其制备的锁香软胶囊及其制备方法 |
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ES2602440T3 (es) | 2017-02-21 |
US20150140050A1 (en) | 2015-05-21 |
JP2013534952A (ja) | 2013-09-09 |
BR112012033017A2 (pt) | 2017-04-04 |
MX2012013822A (es) | 2013-01-28 |
KR101833084B1 (ko) | 2018-02-27 |
EP2585028B1 (en) | 2016-08-10 |
JP6078464B2 (ja) | 2017-02-08 |
ZA201209124B (en) | 2016-07-27 |
US20130089590A1 (en) | 2013-04-11 |
BR112012033017B1 (pt) | 2018-01-09 |
CN102958497A (zh) | 2013-03-06 |
GB201010701D0 (en) | 2010-08-11 |
KR20130122930A (ko) | 2013-11-11 |
EP2585028A1 (en) | 2013-05-01 |
WO2011161229A1 (en) | 2011-12-29 |
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