CN116457084A - 有机化合物中或与之相关的改进 - Google Patents
有机化合物中或与之相关的改进 Download PDFInfo
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- CN116457084A CN116457084A CN202180078591.2A CN202180078591A CN116457084A CN 116457084 A CN116457084 A CN 116457084A CN 202180078591 A CN202180078591 A CN 202180078591A CN 116457084 A CN116457084 A CN 116457084A
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/10—Complex coacervation, i.e. interaction of oppositely charged particles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/11—Encapsulated compositions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q13/00—Formulations or additives for perfume preparations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/50—Perfumes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
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Abstract
公开了一种包含至少一种芯‑壳微胶囊的包封的组合物。所述至少一种芯‑壳微胶囊包含芯和围绕所述芯的壳,所述芯包含至少一种有益剂。所述壳包含第一和第二聚电解质,所述第一和第二聚电解质形成复合凝聚层。所述微胶囊包含至少一种界面使能剂。
Description
本发明涉及一种包封的组合物,制备包封的组合物的方法,通过这种方法可获得的包封的组合物,界面使能剂(interfacial enabler)在获得包封的组合物中的用途以及包封的组合物在获得消费品中的用途。
已知将包封的有益剂掺入到消费品例如家庭护理产品,个人护理产品和织物护理产品中。功能性材料包括例如香料,化妆品活性成分和生物活性成分,例如杀生物剂和药物。为避免任何疑问,“有益剂”和“功能性材料”在本文中用作同义词。
特别适合递送这种有益剂的微胶囊是芯-壳微胶囊,其中所述芯包含所述功能材料,并且所述壳对所述芯是不可渗透的或部分不可渗透的。通常,这些微胶囊用于水性介质中,并且包封的有益剂是疏水性的。可以使用宽范围选择的壳材料,只要这种壳材料对包封的功能性材料是不可渗透的或部分不可渗透的。
在这些有益剂中,因许多原因包封香料。微胶囊可以将香料与外部悬浮介质例如消费品基质隔离并保护其免受其影响,香料可能与这些介质不相容或在其中不稳定。微胶囊还用于辅助香料成分沉积在底物上,例如皮肤,头发,织物或坚硬的家用表面。它们还可以作为控制香料时空释放的方式。
含有疏水性液体芯的微胶囊被一层交联的基于明胶的简单或复合凝聚层包围,这在本领域是众所周知的。例如,US6045835公开了一种将香精或香料包封到具有包含明胶和油芯的水凝胶壳的微胶囊中的方法。在US8088403中,B2明胶由于其良好的物理化学性质而优于其他蛋白质。
然而,明胶是一种动物来源的蛋白质,其典型地从鱼类,猪肉,牛肉和/或家禽中获得。如今,消费者越来越关注使用从动物来源获得的材料,尤其是在这些材料用于身体护理应用的情况下。
因此,克服现有技术中的上述缺点是本发明的根本问题。特别地,提供由非动物来源的材料制成的上述类型的基于蛋白质的包封的组合物是本发明的根本问题。胶囊在制造和储存过程中应表现出良好的稳定性,并在应用中表现出有益的释放特性。此外,组合物应能够在操作安全,稳定和成本有效的过程中生产。
这些问题通过独立权利要求的主题来解决。
在第一方面,本发明涉及包含至少一种芯-壳微胶囊的包封的组合物。所述至少一种芯-壳微胶囊包含芯和围绕所述芯的壳,所述芯包含至少一种有益剂。所述壳包含第一和第二聚电解质,所述第一和第二聚电解质形成复合凝聚层。所述微胶囊包含至少一种界面使能剂。
在本上下文中,“界面使能剂”是指具有在芯组合物的相界面处与聚电解质的至少一种相互作用的能力以促进壳形成的物质。在不受任何理论束缚的情况下,这种相互作用可以通过分散力,静电力或氢键实现。而且共价键也包含在该术语中。
所述芯-壳微胶囊的芯由芯组合物制成。所述芯组合物特别地基本上与水不混溶。
所谓“基本上与水不混溶”是指当芯组合物与水混合时,即使在剧烈搅拌下,至少95wt.-%,优选至少99wt.-%的芯组合物相在搅拌停止后立即或逐渐地与水相分离。
优选地,芯组合物的量低于水相的量,使得当用水相乳化时,芯组合物在水相中形成分散相,通常为芯组合物液滴的形式。
所谓“凝聚层”是指与水性贫聚电解质连续相共存的富含聚电解质的液滴。液滴在界面处聚集以形成界面层。
在本发明的上下文中,凝聚层液滴在芯组合物与水相之间的界面处聚集。作为结果,形成了稳定的芯-壳胶囊,其包含被凝聚层液滴包围的芯组合物液滴。这些使组合物液滴稳定并形成胶囊壁。
所谓“复合凝聚”或“复合凝聚层”是指形成包含聚电解质混合物的界面层。
可以在光学显微镜下观察到复合凝聚的现象,其中其通过在芯组合物液滴周围出现环来标记。该环由上述富含聚电解质的相组成,该富含聚电解质的相具有与周围水相不同的折射率。
两种聚电解质的复合凝聚通常通过使两种聚电解质达到它们的等电点来诱导,这是指两种聚电解质总体的净电荷为零或接近零的点,从而诱导两种聚电解质的复合。这可以通过改变盐浓度来实现,或者在两性聚电解质例如蛋白质的情况下,通过改变介质的pH来实现。
已经发现,通过使用界面使能剂,可以显著提高两种聚电解质之间的复合凝聚的效率。特别地,这种显著的改进使得获得与基于明胶的微胶囊一样性能的基于严格素食蛋白质的微胶囊成为可能。此外,通过使用这种界面使能剂,能够获得具有体积平均直径低于25μm且甚至低于10μm的微胶囊,否则难以实现。
在本发明的特定实施方案中,芯由液体芯组合物组成。界面使能剂然后可溶于芯组合物中或衍生自可溶于芯组合物的材料。
优选地,界面使能剂为或衍生自多官能分子,优选双官能分子。已经发现多官能分子特别适合于促进壳形成。
在不受任何理论束缚的情况下,如果界面使能剂为多官能分子或衍生自多官能分子,则其可以为交联所述第一和/或第二聚电解质的交联剂。
为了进行复合凝聚,优选所述第一和第二聚电解质在给定pH下具有相反的电荷。如上所述,当两种聚电解质的总体的纯电荷为零或接近零时,发生复合凝聚。
在下文中,所述第一和第二聚电解质是可互换的,这意味着所述“第一”措辞不优先于所述“第二”措辞。
所述第一聚电解质优选为两性聚电解质。所述两性聚电解质的优点是具有可变的电荷,这取决于pH值。因此,改变pH可以控制聚合物在水(下文称为“水相”)中的状态。因此,取决于pH,聚合物可以或多或少是阳离子的,或多或少是阴离子的,乃至从阳离子聚电解质变为阴离子聚电解质,并且反之亦然。聚合物具有零电荷的pH称为等电点。
在优选的实施方案中,所述两性聚电解质的等电点低于pH 7,优选低于pH 6,更优选低于pH 5.5,甚至更优选低于pH 5.0。在这些条件下,所述两性聚电解质经历阴离子到阳离子的转变,这可以通过使用传统的布朗斯台德酸容易地触发。同时,如下文所述,所述第二聚电解质的电荷也由该区域的pH控制。这种情况特别有利于复合凝聚。
为了获得具有实际可接受量的微胶囊的浆液,优选所述第一和第二聚电解质在pH7±0.5和室温下的水中的溶解度高于5wt.-%,优选高于10wt.-%。在本发明的上下文中,术语“水”包括去离子水和自来水。
在本发明的优选实施方案中,所述两性聚电解质为蛋白质,特别是源自严格素食来源的蛋白质。蛋白质由于其化学和构象的多样性,疏水性与亲水性平衡和静电特性而成为一种用途非常广泛的两性聚电解质(polyampholite)。这样的属性对于复合凝聚特别有利。在当今的社会和伦理背景下,严格素食蛋白质并非源自动物这一事实是一个优势。
在特别优选的实施方案中,源自严格素食来源的蛋白质选自大豆蛋白,豌豆蛋白,大米蛋白和大麻蛋白,优选大豆蛋白。这些蛋白质可以直接使用或以变性的形式使用。蛋白质变性通常涉及蛋白质的二级,三级和四级结构的变化,将一种高官能和特殊的大分子转化为可用于广泛应用的材料。众所周知,变性可以由例如温度,pH,电离辐射,剪切应力,水结构破坏剂和洗涤剂的作用诱导。蛋白质可以通过已知的方法例如提取和离心从严格素食来源中分离出来。
蛋白质分离物可以包含不溶于水的物质,并且可以在包含蛋白质的水溶液中沉淀或赋予其浑浊的方面。在本发明的特定实施方案中,基于所述溶液的总重量,包含标称百分比为5wt.-%的蛋白质,特别是源自严格素食来源的蛋白质的水溶液包含小于0.1wt.-%,优选小于0.05wt.-%的不溶性材料。“标称百分比”是指在溶解过程开始时加入水相的蛋白质的称重量。
作为通常具有80至95wt.-%的蛋白质含量的蛋白质分离物的替代品,也可以使用具有较低蛋白质含量(例如约70wt.-%)的蛋白质浓缩物。然而,优选使用蛋白质分离物,以最大限度地减少包封过程中杂质干扰的可能性。如果使用蛋白质浓缩物,则基于所述溶液的总重量,包含标称百分比为5wt.-%的蛋白质,特别是源自严格素食来源的蛋白质的水溶液包含小于0.2wt.-%,优选小于0.1wt.-%的不溶性材料。
在本发明的优选实施方案中,所述第二聚电解质为多糖,优选包含羧酸基团的多糖。除了多糖也是生物来源的和严格素食的事实(这是相对于本发明的一个相当大的优点)之外,包含羧基的多糖特别适合于复合凝聚介导的微囊化。一方面,这些聚合物可能具有积累到界面并作为乳化剂或共乳化剂的能力。另一方面,它们的羧基可能或多或少地被去质子化,这取决于pH,从而允许调节它们的阴离子特性以及它们与蛋白质建立静电相互作用的能力。
包含羧酸基团的多糖可以包含糖醛酸单元,特别是己糖醛酸单元。具有糖醛酸单元,特别是己糖醛酸单元的多糖在自然界中是广泛可利用的。己糖醛酸单元可以选自半乳糖醛酸单元,葡糖醛酸单元,特别是4-O-甲基-葡糖醛酸单元,古罗糖醛酸单元和甘露糖醛酸单元。
包含羧酸基团的多糖可以是支链的。包含羧酸基团的支链多糖具有比直链多糖形成更紧密网状结构的优点,因此可以有利于包封壳的不渗透性,从而减少泄漏并提高包封效率。
羧基也可以通过化学方法接枝到多糖上。例如,羧甲基纤维素可以通过纤维素与氯乙酸或其钠盐在碱性条件下反应而获得。在该反应中,C2,C3和C6羟基可以被羧基官能团取代。
在本发明的优选实施方案中,包含羧酸基团的多糖选自羧甲基纤维素,阿拉伯胶,褐藻胶,果胶,透明质酸,黄原胶,结冷胶及其与一价碱金属的盐。在本发明的上下文中,羧甲基纤维素(CMC)和羧甲基纤维素钠是特别优选的,因为与未改性的多糖相比,这些改性的纤维素不太倾向于出现质量波动。此外,CMC的取代度(DS),即羧酸或羧酸酯基团的平均数量除以CMC大分子中吡喃葡萄糖单元的数量,可以高于其他包含羧酸基团的多糖的取代度。例如,阿拉伯胶仅由15%至16%(DS=0.15-0.16)的葡糖醛酸组成,而在CMC中,一个吡喃葡萄糖单元可以包含至多3个羧基,典型地0.4至1.5之间(DS=0.4-1.5)。DS低于0.4的CMC是少量固体,而更高等级的CMC很难在工业上制造。
优选地,按照这样一种方式选择多糖的分子量,即多糖大分子足够大以形成粘性凝聚层,并且足够低以防止浆液过于粘稠。
在本发明的特别优选的实施方案中,所述羧甲基纤维素和/或羧甲基纤维素钠具有50’000至250’000g/mol,优选75’000至125’000g/mol的分子量和0.5至1.5,优选0.6至1.1的取代度。
所述第二聚电解质与所述第一聚电解质的比率由它们各自的静电荷和在复合物凝聚pH范围内形成静电中性聚合物-聚合物复合物的必要性决定。该比率典型地通过实验确定。
在所述第一聚电解质为蛋白质且所述第二聚电解质为羧甲基纤维素和/或羧甲基纤维素钠的情况下,所述羧甲基纤维素或羧甲基纤维钠与所述蛋白质,优选源自严格素食来源的蛋白质,更优选大豆蛋白的重量比为0.05至0.2,优选0.08至0.12。
优选地,所述界面使能剂为或衍生自二酸或二醛,甚至更优选地衍生自芳族二醛。然而,二酸有效地改善了包封,所得微胶囊的热稳定性低于使用二醛作为界面使能剂获得的微胶囊。
二羧酸可以选自1,3-丙二羧酸(戊二酸),1,4-丁二羧酸(己二酸),1,5-戊二羧酸(庚二酸)和1,4-环己二羧酸。
环状二醛可以选自邻苯二甲醛(1,2-苯二甲醛),间苯二甲醛(1,3-苯二甲醛),对苯二甲醛(1,4-苯二甲醛),1,2-环己烷二甲醛(1,2-cycloxanedicarbaldehyde),1,3-环己烷二甲醛(1,3-cycloxanedicarbaldehyde),1,4-环己烷二甲醛(1,4-cycloxanedicarbaldehyde),环戊烷-1,3-二甲醛,[1,1’-联苯]-3,4’-二甲醛,[1,1’-联苯]-3,3’-二甲醛,[1,1’-二苯]-3,2’-二甲醛,9,10-蒽二甲醛,4,4’-联苯二甲醛,呋喃-2,5-二甲醛和1,4-双(X-甲酰基-苯氧基)烷烃,其中X=2,3或4,且烷烃残基包括2至6个碳原子,更具体地4个碳原子,1,4二甲酰基哌嗪(1,4-diformylpyperazin)和2,2’-联吡啶-4,4’-二甲醛。更优选地,环状二醛为芳族二醛,其选自邻苯二甲醛(1,2-苯二甲醛),间苯二甲醛(1,3-苯二甲醛),对苯二甲醛(1,4-苯二甲醛),[1,1’-联苯]-3,4’-二甲醛,[1,1’-联苯]-3,3’-二甲醛,[1,1’-联苯]-3,2’-二甲醛,9,10-蒽二甲醛和4,4’-联苯二甲醛。
在优选的实施方案中,所述界面使能剂为或衍生自二醛,所述二醛选自1,3-苯二甲醛,1,3-环己烷二甲醛,环戊烷-1,3-二甲醛,呋喃-2,5-二甲醛和1,4-二甲酰基哌嗪,甚至更优选选自1,3-苯二甲醛和1,4-二甲酰基哌嗪,且仍然更优选选自1,3-苯二甲醛。这些特点的界面使能剂良好地溶于芯组合物,且由此特别有利于得到合适的本发明的微胶囊。
在本发明的优选实施方案中,基于所述芯组合物的重量,所述界面使能剂以0.1至5wt.-%,优选0.5至2.0wt.-%,仍然更优选0.75至1.5wt.-%的水平存在。如果界面使能剂的水平过低,则无法形成具有期望特性的微胶囊:获得的微胶囊过大且热不稳定。另一方面,将界面使能剂的水平增加到超过一定水平,例如2wt.-%,则无法改善微胶囊的特性,并且可能对芯组合物的质量有害。例如,如果芯成分为香料,则过量的界面使能剂可能会影响这种香料的嗅觉特性。此外,在更高的水平下,例如超过5%,可能会遇到溶解度问题。
当界面使能剂与蛋白质(优选源自严格素食来源的蛋白质,甚至更优选大豆蛋白)的重量比为0.01至0.1,优选0.02至0.08,甚至更优选0.03至0.07时,可以得到在微胶囊直径,包封效率和微胶囊稳定性方面的最佳性能。
包含在芯或芯组合物中的有益剂可以选自香料成分,化妆品成分和生物活性成分。
在本发明的特定实施方案中,所述芯组合物包含至少一种香料成分。可以根据本发明包封的香料成分的综合列表可以在香料文献例如“Perfume&Flavor Chemicals”,S.Arctander(Allured Publishing,1994)中找到。本发明的包封的香料优选包含选自以下的香料成分:乙酰基异丁香酚(乙酸(E)-2-甲氧基-4-(丙-1-烯-1-基)苯酯);阿道克醛(2,6,10-三甲基十一碳-9-烯醛);AGRUMEX(乙酸2-(叔丁基)环己酯);C10癸醛(癸醛);C11 MOA醛(2-甲基癸醛);C11十一碳烯醛(十一碳-10-烯醛);C110十一醛(十一醛);C12月桂醛(十二醛);C12 MNA醛(2-甲基十一醛);C8辛醛(辛醛);C9异壬醛(3,5,5-三甲基己醛);食品级C9壬醛(壬醛);C90壬烯醛((E)-壬-2-烯醛);ISO C11醛((E)-十一碳-9-烯醛);红桔醛((E)-十二碳-2-烯醛);戊基甘醇酸烯丙酯(2-(3-甲基丁氧基)乙酸丙-2-烯基酯);己酸烯丙酯(己酸丙-2-烯基酯);环己基丙酸烯丙酯(3-环己基丙酸丙-2-烯基酯);庚酸烯丙酯(庚酸丙-2-烯基酯);琥珀芯(1-((2-(叔丁基)环己基)氧基)丁-2-醇);龙涎缩醛(3,8,8,11a-四甲基十二氢-1H-3,5a-环氧萘并[2,1-c]氧杂环庚三烯);极品龙涎醇(1,3,4,5,6,7-六氢-β,1,1,5,5-五甲基-2H-2,4a-亚甲基萘-8-乙醇);黄葵内酯((Z)-氧杂环十七碳-10-烯-2-酮);龙涎呋喃((3aR,5aS,9aS,9bR)-3a,6,6,9a-四甲基-2,4,5,5a,7,8,9,9b-八氢-1H-苯并[e][1]苯并呋喃);丁酸戊酯(丁酸戊酯);戊基肉桂醛((Z)-2-亚苄基庚醛);水杨酸戊酯(2-羟基苯甲酸戊酯);合成茴香脑((E)-1-甲氧基-4-(丙-1-烯-1-基)苯);乙酸茴香酯(乙酸4-甲氧基苄酯);阿弗曼酯(甲酸1-(3,3-二甲基环己基)乙酯);茴香醛对甲酚(4-甲氧基苯甲醛);橙花素((E)-2-((7-羟基-3,7-二甲基亚辛基)氨基)苯甲酸甲酯);BELAMBRE((1R,2S,4R)-2’-异丙基-1,7,7-三甲基螺[双环[2.2.1]庚烷-2,4’-[1,3]二噁烷]);苯甲醛(苯甲醛);乙酸苄酯(乙酸苄酯);苄基丙酮(4-苯基丁-2-酮);苯甲酸苄酯(苯甲酸苄酯);水杨酸苄酯(2-羟基苯甲酸苄酯);百瑞福(6-乙酰氧基己酸乙酯);双环壬内酯(八氢-2H-色烯-2-酮);乙氧基环十二烷氧基甲烷((乙氧基甲氧基)环十二烷);伯斯利((1S,2R,5R)-2-乙氧基-2,6,6-三甲基-9-亚甲基双环[3.3.1]壬烷);龙脑晶体((1S,2S,4S)-1,7,7-三甲基双环[2.2.1]庚-2-醇);乙酸龙脑酯(乙酸(2S,4S)-1,7,7-三甲基双环[2.2.1]庚-2-基酯);波洁洪醛(3-(4-(叔丁基)苯基)丙醛);丁酰乳酸丁酯(丁酸1-丁氧基-1-氧代丙-2-基酯);对丁基环己基乙酸酯(乙酸4-(叔丁基)环己酯);仲丁基喹啉(2-(2-甲基丙基)喹啉);合成樟脑((1S,4S)-1,7,7-三甲基双环[2.2.1]庚-2-酮);香芹酚(5-异丙基-2-甲基苯酚);左旋香芹酮((5R)-2-甲基-5-丙-1-烯-2-基环己-2-烯-1-酮);开司米酮(1,1,2,3,3-五甲基-2,3,6,7-四氢-1H-茚-4(5H)-酮);CASSYRANE(5-叔丁基-2-甲基-5-丙基-2H-呋喃);柏木烯((1S,8aR)-1,4,4,6-四甲基-2,3,3a,4,5,8-六氢-1H-5,8a-亚甲基甘菊环);乙酸柏木酯(乙酸(1S,6R,8aR)-1,4,4,6-四甲基八氢-1H-5,8a-亚甲基甘菊环-6-基酯);柏木基甲基醚((1R,6S,8aS)-6-甲氧基-1,4,4,6-四甲基八氢-1H-5,8a-亚甲基甘菊环);烯丙基紫罗兰酮((E)-1-(2,6,6-三甲基环己-2-烯-1-基)庚-1,6-二烯-3-酮);合成肉桂醇((E)-3-苯基丙-2-烯-1-醇);肉桂醛((2E)-3-苯基丙-2-烯醛);乙酸肉桂酯(乙酸(E)-3-苯基丙-2-烯-1-基酯);顺式茉莉酮((Z)-3-甲基-2-(戊-2-烯-1-基)环戊-2-烯酮);顺式-3-己烯醇((Z)-己-3-烯-1-醇);柠檬醛((E)-3,7-二甲基辛-2,6-二烯醛);柠檬二乙缩醛((Z)-1,1-二乙氧基-3,7-二甲基辛-2,6-二烯);香茅醛(3,7-二甲基辛-6-烯醛);香茅醇(3,7-二甲基辛-6-烯-1-醇);乙酸香茅酯(乙酸3,7-二甲基辛-6-烯-1-基酯);甲酸香茅酯(甲酸3,7-二甲基辛-6-烯-1-基酯);香茅腈(3,7-二甲基辛-6-烯腈);爽腈(十二腈);花冠醇(4-环己基-2-甲基丁-2-醇);天籁麝香((Z)-3-甲基环十四碳-5-烯酮);香豆素晶体(2H-色烯-2-酮);对甲酚乙酸酯(乙酸(4-甲基苯)酯);对甲酚基甲基醚(1-甲氧基-4-甲基苯);天籁麝香((Z)-3-甲基环十四碳-5-烯酮);枯茗腈(4-异丙基苯甲腈);女贞醛(2,4-二甲基环己-3-烯-1-甲醛);兔耳草醛(3-(4-异丙基苯基)-2-甲基丙醛);环格蓬酯(2-(环己基氧基)乙酸烯丙酯);环己基乙基乙酸酯(乙酸2-环己基乙酯);水杨酸环己酯(2-羟基苯甲酸环己酯);环柑青醛(8,8-二甲基-1,2,3,4,5,6,7,8-八氢萘-2-醛);伞花烃(1-甲基-4-丙-2-基苯);突厥烯酮((E)-1-(2,6,6-三甲基环己-1,3-二烯-1-基)丁-2-烯-1-酮);甲位突厥酮((E)-1-(2,6,6-三甲基环己-2-烯-1-基)丁-2-烯-1-酮);丁位突厥酮(1-(2,6,6-三甲基-1-环己-3-烯基)丁-2-烯-1-酮);丙位癸内酯(5-己基氧杂环戊烷-2-酮);反式-4-癸烯醛((E)-癸-4-烯醛);DELPHONE(2-戊基环戊酮);δ-3蒈烯((1S,6S)-3,7,7-三甲基双环[4.1.0]庚-3-烯);富马酸二己酯(二己基-丁-2-烯二酸酯);二氢茴香脑(1-甲氧基-4-丙基苯);二氢茉莉酮(3-甲基-2-戊基环己-2-烯酮);二氢月桂烯醇(2,6-二甲基辛-7-烯-2-醇);邻氨基苯甲酸二甲酯(2-(甲基氨基)苯甲酸甲酯);二甲基苄基甲醇(2-甲基-1-苯基丙-2-醇);乙酸二甲基苄基原酯(乙酸2-甲基-1-苯基丙-2-基酯);丁酸二甲基苄基原酯(丁酸2-甲基-1-苯基丙-2-基酯);二甲基辛烯酮(4,7-二甲基辛-6-烯-3-酮);二甲基庚醇(2,6-二甲基庚-2-醇);苧烯(1-甲基-4-(丙-1-烯-2-基)环己-1-烯);二苯醚(氧联二苯);丁位十二内酯(6-庚基四氢-2H-吡喃-2-酮);丙位十二内酯(5-辛基氧杂环戊烷-2-酮);十二碳烯醛((E)-十二碳-2-烯醛);道比卡尔((E)-4-((3aS,7aS)-六氢-1H-4,7-亚甲基茚-5(6H)-亚基)丁醛);黑檀醇((E)-3-甲基-5-(2,2,3-三甲基环戊-3-烯-1-基)戊-4-烯-2-醇);ESTERLY(环己基甲酸乙酯(ethylcyclohexyl carboxylate));乙酸乙酯(乙酸乙酯);乙酰乙酸乙酯(3-氧代丁酸乙酯);肉桂酸乙酯(3-苯基丙-2-烯酸乙酯);己酸乙酯(己酸乙酯);乙基芳樟醇((E)-3,7-二甲基壬-1,6-二烯-3-醇);乙基芳樟基乙酸酯(乙酸(Z)-3,7-二甲基壬-1,6-二烯-3-基酯);乙基麦芽酚(2-乙基-3-羟基-4H-吡喃-4-酮);甲基-2-丁酸乙酯(2-甲基丁酸乙酯);辛酸乙酯(辛酸乙酯);庚酸乙酯(庚酸乙酯);乙基苯基缩水甘油酸酯(3-苯基环氧乙烷-2-甲酸乙酯);藏红花酸乙酯(2,6,6-三甲基环己-1,3-二烯-1-甲酸乙酯);乙基香草醛(3-乙氧基-4-羟基苯甲醛);巴西酸亚乙酯(1,4-二氧杂环十七烷-5,17-二酮);桉叶素((1s,4s)-1,3,3-三甲基-2-氧杂双环[2.2.2]辛烷);丁香酚(4-烯丙基-2-甲氧基苯酚);合成橡苔(2,4-二羟基-3,6-二甲基苯甲酸甲酯);乙酸葑酯(乙酸(2S)-1,3,3-三甲基双环[2.2.1]庚-2-基酯);葑醇((1S,2R,4R)-1,3,3-三甲基双环[2.2.1]庚-2-醇);小茴香醛(3-(4-甲氧基苯基)-2-甲基丙醛);FIXAMBRENE(3a,6,6,9a-四甲基十二氢萘并[2,1-b]呋喃);吐纳麝香(1-(3,5,5,6,8,8-六甲基-5,6,7,8-四氢萘-2-基)乙酮);海风醛(3-(4-乙基苯基)-2,2-二甲基丙醛);花青醛(3-(3-异丙基苯基)丁醛);FLORIDILE((E)-十一碳-9-烯腈);丙酸三环癸烯醛(丙酸(3aR,6S,7aS)-3a,4,5,6,7,7a-六氢-1H-4,7-亚甲基茚-6-基酯);弗罗派(2,4,6-三甲基-4-苯基-1,3-二噁烷);铃兰吡喃HC(四氢-4-甲基-2-(2-甲基丙基)-2H-吡喃-4-醇);鲜薄荷酮(2-(仲丁基)环己酮);苹果酯(2-(2-甲基-1,3-二氧杂环戊烷-2-基)乙酸乙酯);果糖酯((3aS,4S,7R,7aS)-八氢-1H-4,7-亚甲基茚-3a-甲酸乙酯);果腈(2-甲基癸腈);格蓬酮(1-(5,5-二甲基环己-1-烯-1-基)戊-4-烯-1-酮);乙酸苏合香酯(乙酸1-苯基乙酯);异丁酸三环癸烯酯(2-甲基丙酸(3aR,6S,7aS)-3a,4,5,6,7,7a-六氢-1H-4,7-亚甲基茚-6-基酯);香叶醇((E)-3,7-二甲基辛-2,6-二烯-1-醇);乙酸香叶酯(乙酸(E)-3,7-二甲基辛-2,6-二烯-1-基酯);巴豆酸香叶酯(丁-2-烯酸(E)-3,7-二甲基辛-2,6-二烯-1-基酯);异丁酸香叶酯(2-甲基丙酸(E)-3,7-二甲基辛-2,6-二烯-1-基酯);奇华酮(2-乙基-6,6-二甲基环己-2-烯甲酸乙酯);环十五烯内酯((E)-氧杂环十六碳-12-烯-2-酮);二氢茉莉酮酸甲酯(3-氧代-2-戊基环戊烷乙酸甲酯);洋茉莉醛晶体(苯并[d][1,3]二氧杂环戊烯-5-甲醛);香波酯((2S)-3-异丙基双环[2.2.1]庚-5-烯-2-甲酸乙酯);反式-2-己烯醛((E)-己-2-烯醛);顺式-3-己烯醇((Z)-己-3-烯-1-醇);乙酸顺式-3-己烯酯(乙酸(Z)-己-3-烯-1-基酯);丁酸顺式-3-己烯酯(丁酸(Z)-己-3-烯-1-基酯);异丁酸顺式-3-己烯酯(2-甲基丙酸(Z)-己-3-烯-1-基酯);水杨酸顺式-3-己烯酯(2-羟基苯甲酸(Z)-己-3-烯-1-基酯);乙酸己酯(乙酸己酯);苯甲酸己酯(苯甲酸己酯);丁酸己酯(丁酸己酯);己基肉桂醛((E)-2-亚苄基辛醛);异丁酸己酯(2-甲基丙酸己酯);水杨酸己酯(2-羟基苯甲酸己酯);羟基香茅醛(7-羟基-3,7-二甲基辛醛);吲哚素(4,4a,5,9b-四氢茚并[1,2-d][1,3]二噁英);吲哚(1H-吲哚);吲哚烯液(8,8-二(1H-吲哚-3-基)-2,6-二甲基辛-2-醇);乙位紫罗兰酮((E)-4-(2,6,6-三甲基环己-1-烯-1-基)丁-3-烯-2-酮);芷香酮((E)-3-甲基-4-(2,6,6-三甲基环己-2-烯-1-基)丁-3-烯-2-酮);甲位紫罗兰酮((E)-4-(2,6,6-三甲基环己-2-烯-1-基)丁-3-烯-2-酮);甲位鸢尾酮((E)-4-(2,5,6,6-四甲基环己-2-烯-1-基)丁-3-烯-2-酮);龙涎酮(1-(2,3,8,8-四甲基-1,2,3,4,5,6,7,8-八氢萘-2-基)乙酮);乙酸异戊酯(乙酸3-甲基丁酯);丁酸异戊酯(丁酸3-甲基丁酯);异丁基甲氧基吡嗪(2-甲基丙基3-甲氧基吡嗪);异环柠檬醛(2,4,6-三甲基环己-3-烯甲醛);异丁香酚((E)-2-甲氧基-4-(丙-1-烯-1-基)苯酚);异茉莉酮B11(2-己基环戊-2-烯-1-酮);异薄荷酮DL(2-异丙基-5-甲基环己酮);乙酸异壬酯(乙酸3,5,5-三甲基己酯);甲基-2-丁酸异丙酯(2-甲基丁酸异丙酯);异丙基喹啉(6-异丙基喹啉);异甲基紫罗兰酮((E)-3-甲基-4-(2,6,6-三甲基环己-2-烯-1-基)丁-3-烯-2-酮);乙酸三环癸烯酯(乙酸(3aR,6S,7aS)-3a,4,5,6,7,7a-六氢-1H-4,7-亚甲基茚-6-基酯);顺式茉莉酮((Z)-3-甲基-2-(戊-2-烯-1-基)环戊-2-烯酮);茉莉酯(乙酸3-丁基-5-甲基四氢-2H-吡喃-4-基酯);茉莉吡喃(乙酸3-戊基四氢-2H-吡喃-4-基酯);爪哇檀香((1-甲基-2-((1,2,2-三甲基双环[3.1.0]环己-3-基)甲基)环丙基)甲醇);高芳烯((Z)-3,4,5,6,6-五甲基庚-3-烯-2-酮);内酯(8-异丙基-1-氧杂螺[4.5]癸-2-酮);叶醇缩醛((Z)-1-(1-乙氧基乙氧基)己-3-烯);柠檬腈((2E,6Z)-3,7-二甲基壬-2,6-二烯腈);绿花芬(碳酸(Z)-己-3-烯-1-基甲基酯);铃兰醛(3-(4-(叔丁基)苯基)-2-甲基丙醛);#N/A芳樟醇(3,7-二甲基辛-1,6-二烯-3-醇);氧化芳樟醇(2-(5-甲基-5-乙烯基四氢呋喃-2-基)丙-2-醇);乙酸芳樟酯(乙酸3,7-二甲基辛-1,6-二烯-3-基酯);MAHONIAL((4E)-9-羟基-5,9-二甲基-4-癸烯醛);麦芽酚(3-羟基-2-甲基-4H-吡喃-4-酮);异丁酸麦芽酚酯(2-甲基丙酸2-甲基-4-氧代-4H-吡喃-3-基酯);母菊酯(2-甲基戊酸乙酯);麦芽酚((4-异丙基环己基)甲醇);玫瑰花醇(3-甲基-5-苯基戊-1-醇);甜瓜醛(2,6-二甲基庚-5-烯醛);#N/A#N/A巯基-8-薄荷烷-3-酮(巯基-对薄荷烷-3-酮);邻氨基苯甲酸甲酯(2-氨基苯甲酸甲酯);苯甲酸甲酯(苯甲酸甲酯);甲基柏木基酮(1-((1S,8aS)-1,4,4,6-四甲基-2,3,3a,4,5,8-六氢-1H-5,8a-亚甲基甘菊环-7-基)乙酮);肉桂酸甲酯(3-苯基丙-2-烯酸甲酯);甲基丹提力士(2-乙氧基-4-(甲氧基甲基)苯酚);二氢异茉莉酮酸甲酯(2-己基-3-氧代环戊烷-1-甲酸甲酯);甲基庚烯酮(6-甲基庚-5-烯-2-酮);甲基内酯(8-甲基-1-氧杂螺[4.5]癸-2-酮);甲基壬基酮(十一烷-2-酮);辛炔羧酸甲酯(壬-2-炔酸甲酯);圆柚甲烷(6,6-二甲氧基-2,5,5-三甲基己-2-烯);水杨酸甲酯(2-羟基苯甲酸甲酯);麝香烯酮((Z)-3-甲基环十五碳-5-烯酮);柑青醛(4-(4-甲基戊-3-烯-1-基)环己-3-烯甲醛);月桂烯(7-甲基-3-亚甲基辛-1,6-二烯);MYSTIKAL(2-甲基十一酸);仙酒酮(2-(2-(4-甲基环己-3-烯-1-基)丙基)环戊酮);新香柠檬酯(乙酸2-甲基-6-亚甲基辛-7-烯-2-基酯);NEOCASPIRENE EXTRA(10-异丙基-2,7-二甲基-1-氧杂螺[4.5]癸-3,6-二烯);新福力酯((E)-壬-2-烯酸甲酯);NEROLEX((2Z)-3,7-二甲基辛-2,6-二烯-1-醇);橙花叔醇((Z)-3,7,11-三甲基十二碳-1,6,10-三烯-3-醇);NEROLIDYLE(乙酸(Z)-3,7,11-三甲基十二碳-1,6,10-三烯-3-基酯);乙位萘乙醚晶体(2-乙氧基萘);新橙花酮(1-(3-甲基苯并呋喃-2-基)乙酮);乙酸橙花酯((Z)-乙酸3,7-二甲基辛-2,6-二烯-1-基酯);NIRVANOLIDE((E)-13-甲基氧杂环十五碳-10-烯-2-酮);壬二烯醛((2E,6Z)-壬-2,6-二烯醛);2,6-壬二烯醇((2Z,6E)-2,6-壬二烯-1-醇);诺纳地(6,8-二甲基壬-2-醇);丙位壬内酯(5-戊基氧杂环戊烷-2-酮);顺式-6-壬烯醛((Z)-壬-6-烯醛);顺式-6-壬烯醇((Z)-壬-6-烯-1-醇);乙酸诺卜酯(乙酸2-(6,6-二甲基双环[3.1.1]庚-2-烯-2-基)乙酯);NYMPHEAL(3-(4-(2-甲基丙基)-2-甲基苯基)丙醛);丁位辛内酯(6-丙基四氢-2H-吡喃-2-酮);甲基己基酮(辛-2-酮);甜橙晶(1-(2-萘基)-乙酮);鸢尾酮(4-(叔戊基)环己酮);乙位苯乙基甲醚((2-甲氧基乙基)苯);对叔丁基环己基乙酸酯(乙酸4-(叔丁基)环己酯);水果酰胺(2-乙基-N-甲基-N-(间甲苯基)丁酰胺);桃醛(5-庚基二氢呋喃-2(3H)-酮);香叶吡喃(2-甲基-4-亚甲基-6-苯基四氢-2H-吡喃);四氢香叶醇(3,7-二甲基辛-1-醇);牡丹腈(2-亚环己基-2-苯基乙腈);PETALIA(2-亚环己基-2-(邻甲苯基)乙腈);法老酮(2-环己基庚-1,6-二烯-3-酮);苯氧基乙基异丁酸酯(2-甲基丙酸2-(苯氧基)乙酯);苯基乙醛(2-苯基-乙醛);苯基乙基乙酸酯(乙酸2-苯基乙酯);苯基乙醇(2-苯基乙醇);苯基乙基异丁酸酯(2-甲基丙酸2-苯基乙酯);苯基乙基苯基乙酸酯(2-苯基乙酸2-苯基乙酯);苯基丙醇(3-苯基丙-1-醇);甲位蒎烯(2,6,6-三甲基双环[3.1.1]庚-2-烯);乙位蒎烯(6,6-二甲基-2-亚甲基双环[3.1.1]庚烷);松乙醛(3-(6,6-二甲基双环[3.1.1]庚-2-烯-2-基)丙醛);新玫瑰酯(丙酸2,2-二甲基-2-苯基乙酯);POMAROSE((2E,5E)-5,6,7-三甲基辛-2,5-二烯-4-酮);POMELOL(2,4,7-三甲基-6-辛烯-1-醇);甲基柑青醛B(1-甲基-4-(4-甲基戊-3-烯-1-基)环己-3-烯甲醛);乙酸异戊烯酯(乙酸3-甲基丁-2-烯-1-基酯);椰子醛(5-戊基二氢呋喃-2(3H)-酮);白檀醇((E)-2-乙基-4-(2,2,3-三甲基环戊-3-烯-1-基)丁-2-烯-1-醇);覆盆子酮(4-(4-羟基苯基)丁-2-酮);环醚(2,4-二甲基-4-苯基四氢呋喃);结晶玫瑰(乙酸2,2,2-三氯-1-苯基乙酯);9-癸烯醇(癸-9-烯-1-醇);玫瑰醚(4-甲基-2-(2-甲基丙-1-烯-1-基)四氢-2H-吡喃);玫瑰醚CO(4-甲基-2-(2-甲基丙-1-烯-1-基)四氢-2H-吡喃);ROSYFOLIA(1-甲基-2-(5-甲基己-4-烯-2-基)环丙基甲醇);芳香玫瑰醚(4-甲基-2-苯基-3,6-二氢-2H-吡喃);藏花茚(2,3,3-三甲基-1-茚满酮);藏红花醛(2,6,6-三甲基环己-1,3-二烯甲醛);檀香(3-甲基-5-(2,2,3-三甲基环戊-3-烯-1-基)戊-2-醇);SCENTAURUS CLEAN((Z)-2-乙酰基-4-甲基十三碳-2-烯酸乙酯);SCENTAURUS JUICY(4-(十二烷基硫基)-4-甲基戊-2-酮);白麝香(环己烷甲酸2-(1-(3,3-二甲基环己基)乙氧基)-2-甲基丙酯);环十六内酯(环十五烷酮,十六内酯);银醛(2-甲基-3-[4-(2-甲基丙基)苯基]丙醛);螺环格蓬酮(1-(螺[4.5]癸-6-烯-7-基)戊-4-烯-1-酮);榄青酮((E)-5-甲基庚-3-酮肟);乙酸苏合香酯(乙酸1-苯基乙酯);SUPER MUGUET((E)-6-乙基-3-甲基辛-6-烯-1-醇);丝兰麝香(环己烷甲酸(E)-2-((3,5-二甲基己-3-烯-2-基)氧基)-2-甲基丙酯);甲位松油烯(1-甲基-4-丙-2-基环己-1,3-二烯);丙位松油烯(1-甲基-4-丙-2-基环己-1,4-二烯);松油醇(2-(4-甲基环己-3-烯-1-基)丙-2-醇);甲位松油醇(2-(4-甲基-1-环己-3-烯基)丙-2-醇);松油醇(2-(4-甲基环己-3-烯-1-基)丙-2-醇);萜品油烯(1-甲基-4-(丙-2-亚基)环己-1-烯);乙酸松油酯(乙酸2-(4-甲基-1-环己-3-烯基)丙-2-基酯);四氢芳樟醇(3,7-二甲基辛-3-醇);四氢月桂烯醇(2,6-二甲基辛-2-醇);西藏麝香(氧杂环十六烷-2-酮);麝香草酚(2-异丙基-5-甲基苯酚);环丙基茴香醚(1-(环丙基甲基)-4-甲氧基苯);三环萜醛(2,4-二甲基环己-3-烯甲醛);十三碳烯-2-腈((E)-十三碳-2-烯腈);新女贞醛(3-苯基丁醛);新洋茉莉醛(3-(苯并[d][1,3]二氧杂环戊烯-5-基)-2-甲基丙醛);新洋茉莉醛(3-(苯并[d][1,3]二氧杂环戊烯-5-基)-2-甲基丙醛);十一碳三烯((3E,5Z)-十一碳-1,3,5-三烯);甲基癸烯醇((E)-4-甲基癸-3-烯-5-醇);香草醛(4-羟基-3-甲氧基苯甲醛);凡路酮(2,2,5-三甲基-5-戊基环戊酮);环十六烯酮((Z)-环十六碳-5-烯酮);紫罗兰腈((2E,6Z)-壬-2,6-二烯腈);乙位萘甲醚(2-甲氧基萘);ZINARINE(2-(2,4-二甲基环己基)吡啶);BOIS CEDRE ESSCHINE(柏木油);EUCALYPTUS GLOBULUS ESS CHINA(桉叶油);GALBANUM ESS(格蓬油);GIROFLE FEUILLES ESS RECT MADAGASCAR(丁香油);LAVANDIN GROSSO OIL FRANCE ORPUR(杂薰衣草油);MANDARIN OIL WASHED COSMOS(红桔油);橙萜(ORANGE TERPENES)(橙萜);PATCHOULI ESS INDONESIE(广藿香油);和YLANG ECO ESSENCE(依兰油)。
这些香料成分由于其有利的亲脂性和嗅觉性能而特别适合于获得稳定且性能良好的微胶囊。
在本发明的特别优选的实施方案中,大于75wt.-%,优选大于80wt.-%,甚至更优选大于85wt.-%,甚至还更优选大于90wt.-%,甚至仍然更优选大于95wt.-%的香料成分为可生物降解的,并且选自乙酰基异丁香酚(乙酸(E)-2-甲氧基-4-(丙-1-烯-1-基)苯酯);阿道克醛(2,6,10-三甲基十一碳-9-烯醛);AGRUMEX(乙酸2-(叔丁基)环己酯);C10癸醛(癸醛);C11十一碳烯醛(十一碳-10-烯醛);C110十一醛(十一醛);C12月桂醛(十二醛);C12MNA醛(2-甲基十一醛);C8辛醛(辛醛);兔耳草醛(3-(4-异丙基苯基)-2-甲基丙醛);ISOC11醛((E)-十一碳-9-烯醛);戊基甘醇酸烯丙酯(2-(3-甲基丁氧基)乙酸丙-2-烯基酯);环己基丙酸烯丙酯(3-环己基丙酸丙-2-烯基酯);庚酸烯丙酯(庚酸丙-2-烯基酯);黄葵内酯((Z)-氧杂环十七碳-10-烯-2-酮);龙涎呋喃((3aR,5aS,9aS,9bR)-3a,6,6,9a-四甲基-2,4,5,5a,7,8,9,9b-八氢-1H-苯并[e][1]苯并呋喃);水杨酸戊酯(2-羟基苯甲酸戊酯);茴香醛对甲酚(4-甲氧基苯甲醛);乙酸苄酯(乙酸苄酯);水杨酸苄酯(2-羟基苯甲酸苄酯);乙酸龙脑酯(乙酸(2S,4S)-1,7,7-三甲基双环[2.2.1]庚-2-基酯);香芹酚(5-异丙基-2-甲基苯酚);柏木烯((1S,8aR)-1,4,4,6-四甲基-2,3,3a,4,5,8-六氢-1H-5,8a-亚甲基甘菊环);乙酸柏木酯(乙酸(1S,6R,8aR)-1,4,4,6-四甲基八氢-1H-5,8a-亚甲基甘菊环-6-基酯);柏木基甲基醚((1R,6S,8aS)-6-甲氧基-1,4,4,6-四甲基八氢-1H-5,8a-亚甲基甘菊环);柠檬醛((E)-3,7-二甲基辛-2,6-二烯醛);香茅醇(3,7-二甲基辛-6-烯-1-醇);乙酸香茅酯(乙酸3,7-二甲基辛-6-烯-1-基酯);天籁麝香((Z)-3-甲基环十四碳-5-烯酮);对甲酚基甲基醚(1-甲氧基-4-甲基苯);环己基乙基乙酸酯(乙酸2-环己基乙酯);水杨酸环己酯(2-羟基苯甲酸环己酯);突厥烯酮((E)-1-(2,6,6-三甲基环己-1,3-二烯-1-基)丁-2-烯-1-酮);甲位突厥酮((E)-1-(2,6,6-三甲基环己-2-烯-1-基)丁-2-烯-1-酮);丙位癸内酯(5-己基氧杂环戊烷-2-酮);反式-4-癸烯醛((E)-癸-4-烯醛);二氢月桂烯醇(2,6-二甲基辛-7-烯-2-醇);二苯醚(氧联二苯);二氢茴香脑(1-甲氧基-4-丙基苯);二氢茉莉酮(3-甲基-2-戊基环戊-2-烯酮);邻氨基苯甲酸二甲酯(2-(甲基氨基)苯甲酸甲酯);乙酸二甲基苄基原酯(乙酸2-甲基-1-苯基丙-2-基酯);丁酸二甲基苄基原酯(丁酸2-甲基-1-苯基丙-2-基酯);二甲基庚醇(2,6-二甲基庚-2-醇);丁位十二内酯(6-庚基四氢-2H-吡喃-2-酮);丙位十二内酯(5-辛基氧杂环戊烷-2-酮);十二碳烯醛((E)-十二碳-2-烯醛);黑檀醇((E)-3-甲基-5-(2,2,3-三甲基环戊-3-烯-1-基)戊-4-烯-2-醇);己酸乙酯(己酸乙酯);甲基-2-丁酸乙酯(2-甲基丁酸乙酯);乙基麦芽酚(2-乙基-3-羟基-4H-吡喃-4-酮);庚酸乙酯(庚酸乙酯);乙基香草醛(3-乙氧基-4-羟基苯甲醛);巴西酸亚乙酯(1,4-二氧杂环十七烷-5,17-二酮);桉叶素((1s,4s)-1,3,3-三甲基-2-氧杂双环[2.2.2]辛烷);丁香酚(4-烯丙基-2-甲氧基苯酚);合成橡苔(2,4-二羟基-3,6-二甲基苯甲酸甲酯);FIXAMBRENE(3a,6,6,9a-四甲基十二氢萘并[2,1-b]呋喃);花青醛(3-(3-异丙基苯基)丁醛);FLORIDILE((E)-十一碳-9-烯腈);格蓬酮(1-(5,5-二甲基环己-1-烯-1-基)戊-4-烯-1-酮);乙酸苏合香酯(乙酸1-苯基乙酯);香叶醇((E)-3,7-二甲基辛-2,6-二烯-1-醇);乙酸香叶酯(乙酸(E)-3,7-二甲基辛-2,6-二烯-1-基酯);环十五烯内酯((E)-氧杂环十六碳-12-烯-2-酮);二氢茉莉酮酸甲酯(3-氧代-2-戊基环戊烷乙酸甲酯);反式-2-己烯醛((E)-己-2-烯醛);顺式-3-己烯醇((Z)-己-3-烯-1-醇);乙酸顺式-3-己烯酯(乙酸(Z)-己-3-烯-1-基酯);水杨酸顺式-3-己烯酯(2-羟基苯甲酸(Z)-己-3-烯-1-基酯);乙酸己酯(乙酸己酯);吲哚烯液(8,8-二(1H-吲哚-3-基)-2,6-二甲基辛-2-醇);乙位紫罗兰酮((E)-4-(2,6,6-三甲基环己-1-烯-1-基)丁-3-烯-2-酮);芷香酮((E)-3-甲基-4-(2,6,6-三甲基环己-2-烯-1-基)丁-3-烯-2-酮);甲位紫罗兰酮((E)-4-(2,6,6-三甲基环己-2-烯-1-基)丁-3-烯-2-酮);乙酸异戊酯(乙酸3-甲基丁酯);丁酸异戊酯(丁酸3-甲基丁酯);异丁香酚((E)-2-甲氧基-4-(丙-1-烯-1-基)苯酚);异茉莉酮B11(2-己基环戊-2-烯-1-酮);异甲基紫罗兰酮((E)-3-甲基-4-(2,6,6-三甲基环己-2-烯-1-基)丁-3-烯-2-酮);茉莉酯(乙酸3-丁基-5-甲基四氢-2H-吡喃-4-基酯);内酯(8-异丙基-1-氧杂螺[4.5]癸-2-酮);柠檬腈((2E,6Z)-3,7-二甲基壬-2,6-二烯腈);芳樟醇(3,7-二甲基辛-1,6-二烯-3-醇);氧化芳樟醇(2-(5-甲基-5-乙烯基四氢呋喃-2-基)丙-2-醇);乙酸芳樟酯(乙酸3,7-二甲基辛-1,6-二烯-3-基酯);母菊酯(2-甲基戊酸乙酯);五月铃兰醇((4-异丙基环己基)甲醇);玫瑰花醇(3-甲基-5-苯基戊-1-醇);甜瓜醛(2,6-二甲基庚-5-烯醛);巯基-8-薄荷烷-3-酮(巯基-对薄荷烷-3-酮);邻氨基苯甲酸甲酯(2-氨基苯甲酸甲酯);苯甲酸甲酯(苯甲酸甲酯);甲基丹提力士(2-乙氧基-4-(甲氧基甲基)苯酚);甲基庚烯酮(6-甲基庚-5-烯-2-酮);甲基内酯(8-甲基-1-氧杂螺[4.5]癸-2-酮);辛炔羧酸甲酯(壬-2-炔酸甲酯);水杨酸甲酯(2-羟基苯甲酸甲酯);仙酒酮(2-(2-(4-甲基环己-3-烯-1-基)丙基)环戊酮);新福力酯((E)-壬-2-烯酸甲酯);NEROLEX((2Z)-3,7-二甲基辛-2,6-二烯-1-醇);橙花叔醇((Z)-3,7,11-三甲基十二碳-1,6,10-三烯-3-醇);乙位萘乙醚晶体(2-乙氧基萘);新橙花酮(1-(3-甲基苯并呋喃-2-基)乙酮);乙酸橙花酯(乙酸(Z)-3,7-二甲基辛-2,6-二烯-1-基酯);壬二烯醛((2E,6Z)-壬-2,6-二烯醛);顺式-6-壬烯醛((Z)-壬-6-烯醛);顺式-6-壬烯醇((Z)-壬-6-烯-1-醇);NYMPHEAL(3-(4-(2-甲基丙基)-2-甲基苯基)丙醛);丁位辛内酯(6-丙基四氢-2H-吡喃-2-酮);甜橙晶(1-(2-萘基)-乙酮);对叔丁基环己基乙酸酯(乙酸4-(叔丁基)环己酯);桃醛(5-庚基二氢呋喃-2(3H)-酮);四氢香叶醇(3,7-二甲基辛-1-醇);苯基乙基乙酸酯(乙酸2-苯基乙酯);甲位蒎烯(2,6,6-三甲基双环[3.1.1]庚-2-烯);乙位蒎烯(6,6-二甲基-2-亚甲基双环[3.1.1]庚烷);POMAROSE((2E,5E)-5,6,7-三甲基辛-2,5-二烯-4-酮);POMELOL FF(2,4,7-三甲基-6-辛烯-1-醇);乙酸异戊烯酯(乙酸3-甲基丁-2-烯-1-基酯);椰子醛(5-戊基二氢呋喃-2(3H)-酮);覆盆子酮(4-(4-羟基苯基)丁-2-酮);9-癸烯醇(癸-9-烯-1-醇);玫瑰醚CO(4-甲基-2-(2-甲基丙-1-烯-1-基)四氢-2H-吡喃);芳香玫瑰醚(4-甲基-2-苯基-3,6-二氢-2H-吡喃);藏红花醛(2,6,6-三甲基环己-1,3-二烯甲醛);SCENTAURUS JUICY(4-(十二烷基硫基)-4-甲基戊-2-酮);银醛(2-甲基-3-[4-(2-甲基丙基)苯基]丙醛);乙酸苏合香酯(乙酸1-苯基乙酯);丝兰麝香(环己烷甲酸(E)-2-((3,5-二甲基己-3-烯-2-基)氧基)-2-甲基丙酯);丙位松油烯(1-甲基-4-丙-2-基环己-1,4-二烯);松油醇(2-(4-甲基环己-3-烯-1-基)丙-2-醇);萜品油烯(1-甲基-4-(丙-2-亚基)环己-1-烯);四氢芳樟醇(3,7-二甲基辛-3-醇);环丙基茴香醚(1-(环丙基甲基)-4-甲氧基苯);十三碳烯-2-腈((E)-十三碳-2-烯腈);新女贞醛(3-苯基丁醛);新洋茉莉醛(3-(苯并[d][1,3]二氧杂环戊烯-5-基)-2-甲基丙醛);甲基癸烯醇((E)-4-甲基癸-3-烯-5-醇);乙位萘甲醚(2-甲氧基萘);BOIS CEDRE ESS CHINE(柏木油);EUCALYPTUS GLOBULUS ESS CHINA(桉叶油);GALBANUM ESS(格蓬油);GIROFLE FEUILLESESS RECT MADAGASCAR(丁香油);LAVANDIN GROSSO OIL FRANCE ORPUR(杂薰衣草油);MANDARIN OIL WASHED COSMOS(红桔油);橙萜(ORANGE TERPENES)(橙萜);PATCHOULI ESSINDONESIE(广藿香油);和YLANG ECO ESSENCE(依兰油)。这些成分具有提供微胶囊的优点,所述微胶囊不仅壳,而且芯均为可生物降解的。
在本发明的上下文中,“可生物降解成分”是在至少一项OECD生物降解研究中满足“固有可生物降解”和/或“易于生物降解”的通过标准的成分。为了避免任何歧义,这意味着如果一种成分通过一个测试但未通过一个或多个其他测试,则通过结果否决其他测试结果。
为了评估“易于生物降解”的通过标准,生物降解研究可以选自OECD方法301C,OECD方法301D,OECD方法301F和OECD方法310。这些方法适合于挥发性材料。
OECD方法301C,OECD方法301D和OECD方法301F描述在OECD Guidelines for theTesting of Chemicals,Section 3,Test No.301:Ready Biodegradability(采用:1992年7月17日;https://doi.org/10.1787/9789264070349-en)中。
OECD方法310描述在OECD Guidelines for the Testing of Chemicals,Section3,Test No.310:Ready Biodegradability-CO2 in sealed vessels(Headspace Test)(采用:2006年3月23日;修订:2014年9月26日;https://doi.org/10.1787/9789264016316-en)。
在本发明的一个特定方面,根据OECD方法301F评估“易于生物降解”的通过标准,其涉及测压呼吸测量法(manometric respirometry)。在该方法中,“易于生物降解性”的通过水平在于达到理论需氧量和/或化学需氧量的60%。该通过值必须在28-天的测试周期内的10-天窗口内达到。当生物降解程度达到理论需氧量和/或化学需氧量的10%时,10-天窗口开始,并且必须在测试的第28天之前结束。
鉴于现成生物降解性测试中的阳性结果,可以推定化学品将在环境中经历快速和最终的生物降解(Introduction to the OECD Guidelines for the Testing ofChemicals,Section 3,Part 1:Principles and Strategies Related to the Testingof Degradation of Organic Chemicals;采用:2003年7月)。
为了评估“固有可生物降解”的通过标准,生物降解研究可以是OECD方法302C,但也可以使用OECD方法301F,不过,具有不同的通过标准。这些方法也适合于挥发性材料。
OECD方法302C描述在OECD Guidelines for the Testing of Chemicals,Section 3,Test No.302C:Inherent Biodegradability:Modified MITI Test(II)(采用:1981年5月12日;修订:2009年9月8日;https://doi.org/10.1787/9789264070400-en)中。
在本发明的一个特定方面,通过OECD方法302C评估“固有可生物降解”的通过标准。在该方法中,“固有生物降解性”的通过水平达到理论需氧量的70%。对达到该水平没有时间限制。
高于70%的生物降解率可以被为视为固有的最终生物降解性的证据(OECDGuidelines for the Testing of Chemicals,Section 3,Part 1:Principles andStrategies Related to the Testing of Degradation of Organic Chemicals;采用:2003年7月)。
如果OECD方法301F用于评估“固有可生物降解”的通过标准,则通过水平为理论需氧量和/或化学需氧量的60%。该通过值可以在28-天的测试期之后达到,该测试期通常延长至60天。不适用10-天窗口。
在本发明的上下文中,如果成分为精油,则如果以≥1wt.-%的水平存在的其所有成分落入如上文所定义的“固有可生物降解”和/或“易于生物降解”的定义,则认为其是“可生物降解成分”。然而,精油也可以进行上述生物降解试验。
所述芯组合物还可以包含至少一种香料前体,即能够通过刺激手段例如温度的变化,氧化剂的存在,酶的作用或光的作用释放香料成分的材料。这样的香料前体对于本领域而言是众所周知的。
所述芯组合物还可以包含至少一种功能性化妆品成分。用于包封的组合物中的功能性化妆品成分优选是疏水性的。
特别有用的功能性化妆品成分可以选自润肤剂,平滑成分,吸水成分,舒缓和松弛成分,装饰成分,除臭剂,抗衰老成分,细胞再生成分,排水成分,重塑成分,皮肤平整成分,防腐剂,抗氧化剂,抗菌或抑菌成分,清洁成分,润滑成分,结构化成分,头发调理成分,美白成分,纹理成分,软化成分,去头屑成分和剥脱成分。
特别有用的功能性化妆品成分包括但不限于疏水性聚合物,例如烷基二甲基硅氧烷,聚甲基倍半硅氧烷,聚乙烯,聚异丁烯,苯乙烯-乙烯-苯乙烯和苯乙烯-丁烯-苯乙烯嵌段共聚物等;矿物油,例如氢化异链烷烃,硅油等;植物油,例如阿干树油,霍霍巴油,芦荟油等;脂肪酸和脂肪醇及其酯;糖脂;磷脂;鞘脂,例如神经酰胺;固醇和类固醇;萜烯,倍半萜,三萜及其衍生物;精油,例如山金车油,蒿油,树皮油,桦树叶油,金盏花油,肉桂油,松果菊油,桉树油,人参油,大枣油,向日葵油,茉莉油,杂薰衣草油,莲子油,紫苏油,迷迭香油,檀香油,茶树油,百里香油,缬草油,苦艾油,依兰油和丝兰油。
特别地,所述至少一种功能性化妆品成分可以选自檀香油,例如穗檀香仁油;泛醇三乙酸酯;生育酚乙酸酯;生育酚;柚皮苷;亚油酸乙酯;乙酸金合欢醋;金合欢醇;甲基巴豆酸香茅酯;和神经酰胺-2(1-硬脂酰-C18-鞘氨醇,CAS-No:100403-19-8)。
为了在稳定性,在底物上的沉积和性能之间提供最佳平衡,微胶囊的体积中值直径(Dv(50))可以为1至150μm,优选为5至100μm,甚至更优选为8至25μm。具有小于5μm的直径的微胶囊表现出较大的表面积与体积比,因此更倾向于浸出,而由于微胶囊的数量随着直径的增加而减少,太大的微胶囊可能数量不足以提供显著的益处。此外,大的微胶囊可能在产品中可见,或者在底物上留下可见的污渍。
本发明的一个特定方面涉及包含至少一种芯-壳微胶囊的包封的组合物。所述至少一种芯-壳微胶囊包含芯和围绕所述芯的壳,所述芯包含至少一种有益剂。所述壳包含第一和第二聚电解质,所述第一和第二聚电解质形成复合凝聚层。所述微胶囊包含至少一种交联剂,所述交联剂使所述第一和/或第二聚电解质交联。所述交联剂衍生自二醛,所述二醛选自1,3-苯二甲醛,1,3-环己烷二甲醛,环戊烷-1,3-二甲醛,呋喃-2,5-二甲醛和1,4-二甲酰基哌嗪。优选地,所述交联剂衍生自1,3-苯二甲醛。所述第一聚电解质为选自大豆蛋白,豌豆蛋白,大米蛋白和大麻蛋白的蛋白质。优选地,所述第一聚电解质为大豆蛋白。
在第二个方面,本发明提供了用于制备包封的组合物,特别是如上文所述的组合物的方法,所述方法包括以下步骤:
a)提供包含界面使能剂或可以衍生出界面使能剂的材料的芯组合物;
b)提供包含第一和第二聚电解质的水相;
c)将步骤a)中提供的芯组合物乳化到步骤b)中提供的水相中,以得到分散在所述水相中的芯组合物液滴,所述芯组合物液滴具有1至100μm,优选5至75μm,更优选8至60μm,甚至更优选7至20μm的体积中值直径;
d)降低pH,直至达到凝聚pH,由此形成芯-壳微胶囊的浆液;
e)任选地:添加交联剂(如果适用,添加另外的交联剂),并将将所述浆液保持在搅拌下,以得到交联的微胶囊的浆液。
关于步骤a),所述芯成分的混合可以在室温和搅拌下进行。
关于步骤b),可以在5至13,优选7至13,更优选9至12.5,甚至更优选11至12的pH下得到所述水相。所述聚电解质在这样的碱性条件下更好地溶解。该步骤最好在30℃或更高温度下进行,但优选低于60℃,因为经受高温和高pH的蛋白质可能倾向于水解。最佳地,溶解温度为45±5℃。
因此,在本发明的优选实施方案中,使所述蛋白质,优选源自严格素食来源的蛋白质,在45±5℃的温度下,优选在5至13,更优选7至13,仍然更优选9至12.5,甚至仍然更优选11至12的pH下溶于所述水相。
此外,在本发明的优选实施方案中,使所述多糖在45±5℃的温度下,优选在5至13,更优选7至13,仍然更优选9至12.5,甚至仍然更优选11至12的pH下溶于所述水相。
关于步骤c),可以在30至60℃,优选30至40℃的温度下得到所述乳液。在该温度范围内,预期聚合物-聚合物复合物仍然足够弱以允许芯/水界面的易于破坏以及随后芯液滴的破坏。
在复合凝聚结束时,添加水溶性或水分散性交联剂(如果适用,添加另外的交联剂),可以在微胶囊芯周围形成共价交联的网状结构,从而形成交联的包封壳。交联典型地涉及蛋白质的游离胺基,其是复合凝聚层中最具反应性的可利用基团。合适的交联剂包括1,3-丙二醛,1,4-丁二醛,1,5-戊二醛或1,6-己二醛(戊二醛),琥珀二醛,乙二醛,乙二酰三聚物,间苯二酚,多官能异氰酸酯,二酸酐,三酸酐和聚酸酐,N-羟基琥珀酰亚胺,二酯酰亚胺,碳二亚胺和二羧酸二琥珀酰亚胺。
或者,可以通过向浆液中添加转谷氨酰胺酶来有利地促进蛋白质-蛋白质交联。转谷氨酰胺酶通过在一个片段的谷氨酰胺残基与第二个片段的赖氨酸残基之间形成共价键来催化两个蛋白质(或肽)片段之间的交联。如果转谷氨酰胺酶用于蛋白质-蛋白质交联,则优选使用具有更高量的氨基酸谷氨酰胺和赖氨酸的蛋白质。这样的蛋白质是例如坚果和豆类球状蛋白质,特别是大豆蛋白。
在本发明的优选实施方案中,在步骤e)中,在10℃至50℃,更特别是15℃至40℃的温度下加入交联剂(如果适用,另外的交联剂),并且使反应进行1至20小时,优选5至15小时,例如过夜,然后将浆液在室温下冷却。
在本发明的特定实施方案中,所述交联剂(如果适用,所述另外的交联剂)选自戊二醛和转谷氨酰胺酶。
此外,步骤e)中得到的微胶囊的浆液可以通过本领域已知的任何方法例如烘箱干燥,滚筒干燥,冷冻干燥,喷雾干燥或流化床干燥进行干燥。干燥过程之前可以通过浮选将微胶囊从浆液中分离出来。
优选地,通过使用喷雾干燥或多级喷雾干燥来进行脱水。典型地,喷雾干燥通过使用喷嘴,优选双流体喷嘴,或旋转雾化器或旋转盘,在热室中喷射步骤d)或e)中得到的浆液来进行。典型地,浆液可以在喷雾干燥设备中通过喷嘴或旋转盘与并流气流一起被泵送和雾化以进行干燥。典型的入口温度可以设置在160至220℃,出口温度可以设置在60至100℃。然后,可以在干燥器出口处收集包含包裹的微胶囊且颗粒尺寸为约10至约120μm的干燥颗粒。这种干燥方法是本领域众所周知的。在多级干燥器中,使喷雾干燥的颗粒进一步团聚,以得到具有100至250μm的粒径的较大颗粒。
在本发明的替代实施方案中,可以将步骤d)或e)中得到的浆液在流化床干燥器(例如Wurster涂布设备)中喷射在具有预定平均粒径的流化载体材料上,以得到涂布有微胶囊干燥层的载体颗粒。
在本发明的进一步替代实施方案中,可以将步骤d)或e)中得到的浆液中包含的微胶囊在流化床干燥器中造粒或团聚,以得到具有150至400μm或以上的粒径的颗粒。
在本发明的其他替代实施方案中,微胶囊可以通过浮选或过滤从浆液中分离,并在流化床干燥器中在60至150℃,更特别是80至120℃的温度下干燥,以得到与步骤d)或e)中得到的浆液中包含的微胶囊具有大约相同尺寸的颗粒。
本发明的方法还可以另外包含稀释步骤,其中将干燥的颗粒与至少一种载体材料混合,所述至少一种载体材料选自脲,氯化钠,硫酸钠,乙酸钠,沸石,碳酸钠,碳酸氢钠,粘土,滑石,碳酸钙,硫酸镁,石膏,硫酸钙,氧化镁,氧化锌,二氧化钛,氯化钙,氯化钾,氯化镁,氯化锌,糖类,聚乙二醇,聚乙烯吡咯烷酮,柠檬酸或任何水溶性固体酸,脂肪醇,脂肪酸。
将干燥的微胶囊与至少一种载体材料混合可以通过本领域已知的任何方式进行,所述方式包括对流共混,叶片共混,流化共混,翻滚拌合和涡流共混。在第三个方面,本发明提供了可通过上文所述方法获得的包封的组合物。
在第四个方面,本发明提供了界面使能剂在获得包封的组合物,特别是如上文所述的包封的组合物中的用途。
此外,本发明提供了包含如上文所述的包封的组合物的消费品,所述消费品优选为织物护理产品,家庭护理产品或个人护理产品。
本发明的胶囊化组合物可用于对所有形式的消费品进行加香,所述消费品包括洗衣护理洗涤剂,洗衣护理调理剂,织物清新剂,个人护理清洁组合物(例如洗发水,沐浴凝胶和沐浴露),液体肥皂,皂条,个人护理调理组合物(例如护发素),沐浴露,除臭剂组合物,止汗剂组合物,家庭护理组合物(例如硬表面清洁剂和重垢洗涤剂)。
本发明的消费品可以用于处理底物,例如织物,皮肤,毛发,有生命和无生命的表面,硬表面,其中处理底物的作用包括对底物进行洗涤,清洁,软化,护理,整理,增香和/或除臭。
在本发明的一个方面,所述消费品包含如上文所述的组合物,优选占所述消费品0.005至5wt.-%,更优选0.01至1wt.-%且仍然更优选0.02至0.5wt.-%的水平。
在许多情况下,本发明的消费品包含表面活性剂,例如阴离子型表面活性剂,阳离子型表面活性剂,两性表面活性剂或非离子型表面活性剂。
本发明的消费品可以包含酸或碱,或提供酸度或碱度的物质,也称作酸度源或碱度源。
本发明的消费品可以包含用于降低水硬度的增效助剂,例如磷酸盐,多磷酸盐,聚羧酸盐,柠檬酸钠,碳酸钠,硅酸钠,铝硅酸钠(沸石)。
在许多情况下,本发明的消费品为液体,并且可以包含另外的添加剂,例如溶剂,填料,结构改进剂例如增稠剂和流变助剂,分布助剂,抗再沉积剂,防腐剂,除臭剂,化妆品成分和表面增强剂。
本发明的包含微胶囊的消费品可以包含至少一种溶剂,所述溶剂选自水溶性溶剂,或水不溶性或部分水溶性的溶剂。
包含本发明微胶囊的消费品可以包含至少一种结构改进剂和/或胶体稳定剂,其选自流变调节剂,增稠剂,胶凝剂,触变剂和分散剂。
本发明的包含微胶囊的消费品可以包含至少一种硅氧烷,其选自但不限于二甲基硅氧烷,聚(二甲基硅氧烷化二甲基硅氧烷),氨基-硅氧烷,例如氨端聚二甲基硅氧烷,三烷基铵-硅氧烷盐,乙氧基化硅氧烷。
本发明的包含微胶囊的消费品可以包含至少一种化妆品成分,所述化妆品成分选自但不限于润肤剂,保湿剂,防皱剂,剥脱剂,防晒剂,染料,颜料,滑石,调理剂,头发定型剂和去头屑剂。
本发明的包含微胶囊的消费品可以包含至少一种织物增强剂,所述织物增强试剂选自但不限于柔软剂,光学增白剂和抗静电剂。
在本发明的特定实施方案中,消费品为个人护理除臭剂或止汗剂组合物,其可以为可喷雾组合物的形式,或者可以为可以通过滚涂装置,棒,霜或粉末直接施加在皮肤上的组合物。本发明的包封的组合物可以作为通过上文所述方法获得的微胶囊的浆液或以干燥形式掺入到除臭剂或止汗剂组合物中。
可喷洒的除臭剂和止汗剂组合物可以包含冷凝的推进剂气体,例如异丁烷;助悬剂,例如二氧化硅和疏水性膨润土;一种或多种溶剂,例如水和乙醇;脂质,例如肉豆蔻酸异丙酯;表面活性剂;多元醇,例如甘油;止汗剂化合物,例如氯化铝水合物;除臭化合物,例如碳酸锌,环糊精,以及不饱和脂族羟基羧酸的钙,铝,镁或锌盐,例如蓖麻油酸锌;和香料。
除臭剂和止汗剂滚涂组合物可以为凝胶或液体的形式,其包含胶凝剂,例如脂肪酸的钠盐,例如硬脂酸钠,聚酰胺和基于硅氧烷的胶凝剂;助悬剂,例如疏水性膨润土;乳化剂,例如脂肪酸聚乙二醇酯,例如硬脂醇聚醚-2,硬脂醇聚醚-4,硬脂醇聚醚-6,硬脂醇聚醚-7,硬脂醇聚醚-10,硬脂醇聚醚-11,硬脂醇聚醚-13,硬脂醇聚醚-15,硬脂醇聚醚-20和甘油酯和醚;脂肪醇,例如鲸蜡醇和硬脂醇;止汗剂化合物,例如氯化铝水合物,脂质,例如肉豆蔻酸异丙酯和植物油;脂肪酸,例如硬脂酸;醇和多元醇,例如乙醇和甘油;和水。
除臭剂棒和霜可以包含止汗剂复合物,例如铝和铝锆多氯水合物(aluminumzirconium polychlorohydrate)蜡质材料,例如硬脂醇,鲸蜡醇,与氢化油,例如氢化蓖麻油混合;乳化剂,如硬脂酸甘油酯;润肤剂,如环聚二甲基硅氧烷(cyclodimeticone);以及例如滑石和淀粉这样的粉末材料。
在第四个方面,本发明涉及如上文所述的包封的组合物在获得消费品中的用途。
本发明的其他特征和特定优点从以下实施例中变得显而易见。
实施例1:微胶囊的制备
在实施例1.1中,本发明的微胶囊通过进行以下步骤制备:
a)通过将0.25g间苯二甲醛(1,3-苯二甲醛)和0.004g溶剂黄98荧光染料溶于19.75g香料组合物得到芯组合物;
b)提供第一水相,其通过在45℃温度下将4.55g固体大豆蛋白分离物(Clarisoy170,ex Arthur Daniel Midland Company)溶于41.7g0.43wt.-%氢氧化钠的去离子水溶液(pH 11.5)并且使该溶液冷却至室温制备;
c)提供第二水相,其通过在45℃温度下将0.45g羧甲基纤维素溶于19.3g0.6wt.-%氢氧化钠的去离子水溶液(pH为11.5)并且使该溶液冷却至室温制备;
d)提供第三水相,其由pH 11.5的氢氧化钠的去离子水溶液组成;
e)在400ml反应器容器中通过使用搅拌桨在搅拌下将所述第一水相加热至35℃;
f)在搅拌下通过滴液漏斗将所述第二水相滴加至所述第一水相中,历时15分钟;
g)用约1g的所述第三水相冲洗滴液漏斗并且将该冲洗水收集在反应器中;
h)使搅拌速率增加至300rpm并且通过滴液漏斗滴加所述芯组合物,历时24分钟,以得到乳液;
i)用约1g的所述第三水相冲洗滴液漏斗并且将该冲洗水收集在反应器中;
j)使搅拌速率降至180rpm并且通过滴液漏斗添加其余的第三水相,历时13分钟,同时将步骤i)中得到的乳液保持在搅拌下;
k)将22.5wt.-%柠檬酸水溶液以1.3ml/小时的速率连续添加至步骤j)中得到的乳液中,直至达到5.2±0.2的凝聚pH,由此形成芯-壳微胶囊的浆液;
l)缓慢地添加1.3ml的25wt.-%的戊二醛水溶液;
m)将步骤l)中形成的浆液在35℃保持在搅拌下60分钟,且然后使浆液冷却至室温过夜(约15小时),以得到交联的微胶囊的浆液。
在干燥引起的重量变化速率降至低于0.1wt.-%/min时,取固体含量,表示为沉积在120℃下操作的热天平上的初始浆液的重量百分比。将测量的固体含量与基于所用香料组合物和包封材料的重量计算的理论固体含量的比率作为包封效率的测量值,表示为wt.-%。
使用Beckman-Coulter LS 13 320激光粒径分析仪测量微胶囊尺寸分布。
浆液不含聚集物,所得浆液的固体含量为20.2wt.-%,体积中值尺寸Dv(50)为9μm,Dv(90)为15μm,且包封效率为95wt.-%。
在实施例1.2中,本发明的微胶囊通过与实施例1.1中相同的方法制备,但是在步骤l)中用溶解在3.6ml去离子水中的0.4g转谷氨酰胺酶(Activa TI,ex Ajinomoto)替代戊二醛。在这种情况下,在步骤m)中,将浆液的温度升至50℃持续1小时,然后降低至35℃并在后一温度下维持过夜(约16至17小时),然后使交联的微胶囊的浆液冷却至室温。
浆液不含聚集物,所得浆液的固体含量为20.6wt.-%,体积中值尺寸Dv(50)为6μm,Dv(90)为10μm,且包封效率为96wt.-%。
实施例2:使能剂的变化
在实施例2.1至2.16中,本发明的微胶囊通过进行1.1或1.2中所述的步骤制备,但是使用各种使能剂和使能剂浓度。对于用戊二醛交联的微胶囊样品,这些实验的细节报告在表1中,对于用转谷氨酰胺酶交联的微胶囊样品,这些实验的细节报告在表2中,连同微胶囊尺寸、包封效率和庚烷可提取油。使能剂的百分比涉及的是芯组合物的总重量。
庚烷可提取油的测定如下:1.5g浆液用5.5ml庚烷在30-40rpm下翻滚提取2小时。然后将该混合物在3150rpm下离心5分钟。虹吸出上层庚烷相,记录其在350nm至650nm之间的VIS光谱。基于线性校准曲线,根据在449nm波长处的吸光度计算提取油的百分比。
表1:用戊二醛交联的样品
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1还存在50至100μm的较大的胶囊。
表2:用转谷氨酰胺酶交联的样品
表1和表2的结果表明,在0.25wt.-%和以上的使能剂存在下获得的微胶囊比不存在使能剂时更好。在0.5wt.-%和以上时,不仅改善了微胶囊的包封效率,而且微胶囊的尺寸也在优选的范围内。
结果还表明,在界面使能剂浓度为1.25wt.-%(基于所述芯组合物的总重量)时,满足了用戊二醛和转谷氨酰胺酶交联的微胶囊的最佳条件。在这些特定条件下,两种交联剂的作用之间无显著性差异,如在两种情况下测定的庚烷中可提取油的类似量所示。
与低包封效率相比样品2.8中庚烷可提取油的低水平启示,用庚二酸作为使能剂获得的微胶囊的热稳定性低于用邻苯二甲酸作为使能剂获得的微胶囊。
实施例3:对比例
在实施例4.1中,通过进行以下步骤制备对比微胶囊:
a)提供由中链甘油三酯Miglyol 812(ex Oleo)组成的165g的芯组合物;
b)通过在40℃温度下将16.5g B型鱼明胶溶于148.5g的去离子水提供第一水相;
c)通过在40℃温度下将1.6g的羧甲基纤维素溶于77.9g去离子水提供第二水相;
d)通过使用搅拌桨在300rpm搅拌下将芯组合物添加至所述第一水相,并且维持搅拌30分钟以提供乳液;
e)将所述第二水相在搅拌下添加至步骤d)中得到的乳液中;
f)添加预热至40℃的475g去离子水,同时维持搅拌;
g)通过使用50wt.-%柠檬酸溶液将乳液的pH调剂至5.2±0.5的凝聚pH,并且以1℃/5min的速率将乳液冷却至28±1℃,以形成芯-壳微胶囊的浆液;
h)将g)中形成的浆液冷却至20±5℃的温度;
i)添加0.26g的戊二醛并且使浆液在搅拌下过夜(约15小时),以提供交联芯-壳微胶囊的浆液;
j)通过浮选使步骤j)中得到的微胶囊与水相分离,以得到微胶囊的饼状物;
k)在约80℃下在真空烘箱干燥器中或在约70℃下在流化床干燥器中干燥步骤j)中得到的饼状物,以得到自由流动的所谓“空白”微胶囊,其包含中链甘油三酯作为芯组合物,但不含香料;
l)将56.8g的空白微胶囊转移到低剪切混合器,例如带式搅拌机中;
m)在空白微胶囊的整个表面上加入5g去离子水;
n)以60±5rpm打开共混机并保持混合10-15分钟,直至混合物均匀,以得到水化的空白微胶囊;
o)关闭混合器并在步骤n)中得到的水化空白微胶囊的整个表面上添加38.2g的香料组合物;
p)以60±5rpm打开共混机并保持混合10-15分钟;
q)关闭共混器,关闭床(lit)并使微胶囊吸收香料油,直至得到加香的微胶囊的干燥粉末,以形成加香的微胶囊的干燥粉末;
通过将步骤q)中得到的粉末通过150微米筛网筛分来限制微胶囊的尺寸。微胶囊的实际香料含量为50wt.-%,基于所述微胶囊的总重量。
实施例4:腋下的嗅觉评估
将在实施例1.1和实施例3.1中得到的微胶囊浆液掺入到标准的未加香除臭剂滚涂制品中,使得基于所述制品的总重量,所述制品中香料的水平为0.1wt.-%。将该制品浸渍2天。
嗅觉评估由一组未经培训的女性评估员直接从腋下进行。在刚施用除臭剂时进行评估,然后在2小时,6小时和10小时后通过一层布进行评估。10小时后,参与者被要求以一个动作前后移动双臂,然后对香味强度进行分级,首先是通过一层布,其次是直接从皮肤上。
根据预先确定的随机分组,对哪个样品施用于哪个手臂(左或右)进行分配,并且始终要求评估员首先评估他们的左腋下。
未经培训的评估员使用0-10分制对香料的感知强度进行评估。评估员被告知0=非常弱,且10=非常强。
每个样品由56名未经培训的女性评估员进行评估。
使用配对样品t-检验对数据进行分析,其中将置信水平设置为95%。对每个时间点进行单独配对t-检验。将结果报告在表3中。在“差异的显著性”栏中显示相同的字母时,在95%的置信水平下,相关数字之间无统计学显著性差异。
表3:腋下的香味强度评分
正如从表3中显而易见的,在评估过程的所有阶段,本发明的微胶囊具有倾向于优于对比的非严格素食微胶囊或至少与之相当的性能。
实施例5:垫子上的嗅觉评估
将实施例1.1和实施例1.2中得到的微胶囊的浆液掺入标准的未加香除臭剂滚涂制品中,使得基于所述制品的总重量,所述制品中香料的水平为0.1wt.-%。将该制品浸渍2天。
将0.6g的每种制品用移液管涂覆在棉垫上。10名专家小组成员对新鲜样品和6小时前涂覆的样品评估嗅觉强度。
在垫子的一个部分相对于垫子的另一个部分摩擦之前和之后,评估6小时样品的每一个,其中进行第一次评估以对摩擦前强度进行评分,并且进行第二次评估以对摩擦后强度进行评分,评分以5个单位的等级给出(0=无强度,1=非常低,2=低,3=平均,4=强,切5=非常强的强度)。将结果报道在表4上。
表4:垫子上的香味强度评分
结果表明,用转谷氨酰胺酶交联的微胶囊的性能与用戊二醛交联的微胶囊相当。
Claims (31)
1.包封的组合物,包含至少一种芯-壳微胶囊,其中所述至少一种芯-壳微胶囊包含芯和围绕所述芯的壳,所述芯包含至少一种有益剂,其中所述壳包含第一和第二聚电解质,所述第一和第二聚电解质形成复合凝聚层,且其中所述微胶囊包含至少一种界面使能剂。
2.权利要求1的包封的组合物,其中所述芯由液体芯组合物组成,且所述界面使能剂可溶于所述芯组合物或衍生自可溶于所述芯组合物的材料。
3.权利要求1或2的包封的组合物,其中所述界面使能剂为或衍生自多官能分子,优选双官能分子。
4.权利要求3的包封的组合物,其中所述界面使能剂为交联剂,其交联所述第一和/或第二聚电解质。
5.权利要求1至4任一项的包封的组合物,其中所述第一聚电解质为两性聚电解质。
6.权利要求5的包封的组合物,其中所述两性聚电解质的等电点低于pH 7,优选低于pH6,更优选低于pH 5.5,甚至更优选低于pH5.0。
7.权利要求1至6任一项的包封的组合物,其中所述第一和第二聚电解质在水中的溶解度在pH 7±0.5和室温下高于5wt.-%,优选高于10wt.-%。
8.权利要求5至7之一的包封的组合物,其中所述两性聚电解质为蛋白质,特别是源自严格素食来源的蛋白质。
9.权利要求8的包封的组合物,其中所述源自严格素食来源的蛋白质选自大豆蛋白,豌豆蛋白,大米蛋白和大麻蛋白,优选大豆蛋白。
10.权利要求8或9的包封的组合物,包含标称百分比为5wt.-%的蛋白质,特别是源自严格素食来源的蛋白质的水溶液包含小于0.1wt.-%,优选小于0.05wt.-%的不溶性材料,其中基于溶液的总重量。
11.权利要求1至10任一项的包封的组合物,其中所述第二聚电解质为多糖,优选包含羧酸基团的多糖。
12.权利要求11的包封的组合物,其中所述包含羧酸基团的多糖选自羧甲基纤维素,阿拉伯胶,褐藻胶,果胶,透明质酸,黄原胶,结冷胶及其与一价碱金属的盐,优选羧甲基纤维素和羧甲基纤维素钠。
13.权利要求12的包封的组合物,其中所述羧甲基纤维素和/或羧甲基纤维素钠具有50’000至250’000g/mol,优选75’000至125’000g/mol的分子量和0.5至1.5,优选0.6至1.1的取代度。
14.权利要求1至13任一项的包封的组合物,其中所述羧甲基纤维素和/或羧甲基纤维素钠与所述蛋白质,优选源自严格素食来源的蛋白质,更优选大豆蛋白的重量比为0.05至0.2,优选0.08至0.12。
15.权利要求3的包封的组合物,其中所述界面使能剂为或衍生自二酸或二醛,优选衍生自芳族二醛。
16.权利要求15的包封的组合物,其中所述界面使能剂为或衍生自二醛,其选自1,3-苯二甲醛,1,3-环己烷二甲醛,环戊烷-1,3-二甲醛,呋喃-2,5-二甲醛和1,4-二甲酰基哌嗪,优选自1,3-苯二甲醛和1,4-二甲酰基哌嗪,且更优选自1,3-苯二甲醛。
17.权利要求1至16任一项的包封的组合物,其中基于所述芯组合物的重量,所述界面使能剂以0.1至5wt.-%,优选0.5至2.0wt.-%,仍然更优选0.75至1.5wt.-%的水平存在。
18.权利要求1至17任一项的包封的组合物,其中所述界面使能剂与所述蛋白质,优选源自严格素食来源的蛋白质,甚至更优选大豆蛋白的重量比为0.01至0.1,优选0.02至0.08,更优选0.03至0.07。
19.权利要求1至18任一项的包封的组合物,其中包含在所述芯或芯组合物中的有益剂选自香料成分,化妆品成分和生物活性成分。
20.权利要求1至19任一项的包封的组合物,包含多个芯-壳微胶囊,其中所述微胶囊的体积中值直径(Dv(50))为1至150μm,优选5至100μm,甚至更优选8至25μm。
21.用于制备包封的组合物,特别是权利要求1至20之一的组合物的方法,所述方法包括以下步骤:
a)提供包含界面使能剂或可以衍生出界面使能剂的材料的芯组合物;
b)提供包含第一和第二聚电解质的水相;
c)将步骤a)中提供的芯组合物乳化到步骤b)中提供的水相中,以得到分散在所述水相中的芯组合物液滴,所述芯组合物液滴具有1至100μm,优选5至75μm,更优选8至60μm,甚至更优选7至20μm的体积中值直径;
d)降低pH,直至达到凝聚pH,由此形成芯-壳微胶囊的浆液;
e)任选地:添加交联剂,如果适用,添加另外的交联剂,并且将所述浆液保持在搅拌下,以得到交联的微胶囊的浆液。
22.权利要求21的方法,其中在步骤b)中,在5至13,优选7至13,更优选9至12.5,甚至更优选11至12的pH下提供所述水相。
23.权利要求21或22之一的方法,其中在步骤b)中,在45±5℃的温度下,优选在5至13,更优选7至13,仍然更优选9至12.5,甚至仍然更优选11至12的pH下,将所述蛋白质,优选源自严格素食来源的蛋白质溶于所述水相。
24.权利要求21至23之一的方法,其中在步骤b)中,在45±5℃的温度下,优选在5至13,更优选7至13,仍然更优选9至12.5,甚至仍然更优选11至12的pH下,将所述多糖溶于所述水相。
25.权利要求21或24之一的方法,其中在步骤c)中,在30至60℃,优选30至40℃的温度下得到所述乳液。
26.权利要求21至25之一的方法,其中在步骤e)中,在30至60℃,优选30至40℃的温度下添加所述交联剂,如果适用,添加所述另外的交联剂,并且反应进行1至20小时,优选5至15小时。
27.权利要求21至26之一的方法,其中在步骤e)中,所述交联剂,如果适用,所述另外的交联剂选自戊二醛和转谷氨酰胺酶。
28.可通过权利要求21至27之一的方法得到的包封的组合物。
29.界面使能剂在获得包封的组合物,特别是权利要求1至20或28之一的组合物中的用途。
30.消费品,包含权利要求1至20或28之一的包封的组合物,所述消费品优选为织物护理产品,家庭护理产品或个人护理产品。
31.权利要求1至20或28之一的包封的组合物在获得消费品中的用途。
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