CN1741785B - 芳香组合物 - Google Patents
芳香组合物 Download PDFInfo
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- CN1741785B CN1741785B CN2004800025677A CN200480002567A CN1741785B CN 1741785 B CN1741785 B CN 1741785B CN 2004800025677 A CN2004800025677 A CN 2004800025677A CN 200480002567 A CN200480002567 A CN 200480002567A CN 1741785 B CN1741785 B CN 1741785B
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/2003—Alcohols; Phenols
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- 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
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- C11D3/225—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin etherified, e.g. CMC
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- C—CHEMISTRY; METALLURGY
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Abstract
一种可用于给表面赋予芳香的芳香组合物，其含有水、芳香物质、含有至少一种至少22个碳原子脂肪醇的形成液晶的材料和增强材料。该组合物即使是在高温下异乎寻常地是储存稳定的。
Description
本发明涉及增香的家用和个人护理产品，例如洗涤剂和调理剂，清洁用产品和美容产品，可以将它们涂敷给待处理的表面并且赋予其长效的清新性。
对于配制者来说，给例如织物、固体表面的表面或给头发或皮肤赋予清新的芳香协香具有相当的困难。最优选，芳香物质经常是物化性能完全不同的各种成分的复杂混合物，所述物化性能如挥发性、溶解性和化学反应活性。在家用和个人护理产品中，这些成分的任何的相互作用都会干扰芳香物质的性能。例如，芳香组分可以被降解、分散于或者从这些产品中蒸发，由此在储存和使用期间可降低芳香物质的效果或者改变香调。
为解决这些问题，配制者们致力于通过提供适宜于芳香物质的传递载体，来将芳香物质与消费者用或家用产品组合物分开的机理。这种方法的典型方法是将芳香物质包胶。然而，虽然很多包胶介质在保护芳香物质免受上述有害效果方面是成功的，但经常的情况是，包胶介质干扰芳香物质的性能。例如，它可能不按所需的方式释放芳香物质，或者它可能不会实质性沉积在表面上。因此很多这样的体系在消费者调查中被认为是差的并不令人奇怪。
仍然需要提供包胶介质，其不仅保护芳香物质免受与家用和消费者用产品的成分长期接触所带来的有害影响，而且允许在室温下缓慢释放芳香以便给受到处理的表面赋予延长的清新感觉，并且还能够允许在高温下突放芳香，例如在烫熨的过程中，或者在机械作用下，例如摩擦或擦拭处理表面时的摩擦性接触。
能够形成液晶结构的表面活性剂业已在洗涤剂产品中使用。对大部分来说，这种材料是由于表面活性剂的特性而被使用的，或者由于它们的质构化或流变特性(参见US5696074或US5958431)；或者作为增稠剂使用(参见WO 97/00667)。
然而，EP 0466235A1公开了使用这种材料，以在分散的芳香液滴周围形成有序的液晶结构，由此将它们包封并且增强芳香物的性能。
尽管认识到可以使用液晶材料在织物上沉积芳香物质，但这种材料仍没有在液体消费者产品中商业化成功采用。同时，消费者对这种材料的接受性比较低，因为液晶结构是热不稳定的。当将它们分散在含水产品中时，并且特别是在含有表面活性剂的这类产品中，尤其成问题。在这类产品中，特别是在高储存温度下，例如约40℃或更高，液晶结构往往会破裂或者溶解，伴随着芳香物质损失至周围的介质中。
出于能够传递芳香物质，液晶材料仍然是让人感兴趣的介质。然而显然需要以一定的形式提供它们，致使它们在产品中是稳定的，并且能够可靠地在长时间的期限内将芳香协香传递给经过处理的表面，并且当给处理的表面施加热或施加磨擦时能够按要求快速释放芳香。
现在意想不到地发现，如果将液晶材料与某些增强剂混合，则可以获得含有液晶结构的颗粒，其具有延长的热稳定性和机械稳定性，由此使得这种材料可在家用和消费者用产品中突出地用作芳香传递载体。
因此，本发明第一个方面提供一种芳香组合物，该组合物含有水、芳香物质、形成液晶的材料和增强材料，其中所述形成液晶的材料含有至少一种具有至少22个碳原子的脂肪醇.
相比使用现有技术组合物可达到的热稳定性，本发明的组合物显示出更大的热稳定性范围。不期望受任何理论的束缚，据信形成液晶的材料可将颗粒内部组织成层状结构，并且增强剂能够插入这些层状结构的层之间，从而提供机械和热稳定性得到增强的结构。
具体说，本发明的组合物可以在大于40℃的温度下储存，即使是含有表面活性剂的含水产品形式，也没有可感知的芳香物质的损失。此外，当在苛刻的含水环境中使用时，仍会保留高含量的芳香物质，因为液晶结构是稳定的并且基本上保持完整无损。由此确保高含量的芳香物质可以利用，以便完整无损地沉积在表面上。
当沉积在表面上后，干燥过程中的水的蒸发可以引起液晶结构中的结构性变化，例如断裂，从而允许芳香物以可受控的方式释放。按此方式，使用者可以长时间地感受明显的清新芳香协香的感觉。此外，当使用者摩擦性地接触处理过的表面时，在液晶结构中可以出现机械性破裂，从而允许芳香物突放，以便在用芳香物质处理之后一连几个小时、甚至几天地从干燥的表面中放出香气。
增强材料是一种可以溶解或分散在液体中形成粘弹性物质的化合物。向液晶结构中添加增强材料可增加储能弹性模量G′、损耗弹性模量G″和结构的各向异性至各向同性转变温度。G′和G″是流变参数，分别是粘弹性体系中的材料的劲度和粘度的量度。当处于流变测量条件下时(如下实施例所详细描述的)，被增强结构的行为既类似瞬变凝胶又类似永久凝胶。瞬变凝胶的特征在于在相对低形变幅度下的G′＞G″区域(以下称作″弹性区域″)和相对高形变幅度下的G′＜G″区域之间交叉。相反，永久凝胶的特征在于没有任何的交叉并且在所有形变幅度下持续的弹性区域，直至凝胶出现破裂为止。
本发明上下文中的增强材料是指那些能使储能弹性模量的平台区，相比含有非增强化液晶结构的组合物，增加至少一个数量级的材料。优选，被增强的芳香组合物显出储能弹性模量在25℃下高于103帕斯卡并且优选高于104帕斯卡的平台区(参见图1和实施例2的细节)。储能弹性模量的值越高，劲度越强，因此材料越被加强。此外，材料在相对高形变幅度下显示交叉点，说明相比在较低幅度下显示交叉点的材料，具有较高的弹性。
增强材料可以选自有机两亲性、疏水性、亲水性或无机材料。
两亲性增强材料可以是含有疏水性和亲水性部分的材料，两部分之比可以根据所需的特定性能而不同。适宜的两亲性材料的实例是表面活性剂、缔合聚合物，如接枝和嵌段共聚物，尤其是聚(乙烯-b-氧化乙烯)、聚(苯乙烯-b-氧化乙烯)和烷基改性的聚(二甲基硅氧烷-g-氧化乙烯)。明胶和果胶是可以表现两亲特性的生物聚合物的另一实例。
优选的两亲性材料是氧化乙烯含量优选低于80％并且最优选低于50％并且分子量优选低于2500g/mol并且最优选低于1000g/mol的聚(乙烯-b-氧化乙烯)共聚物。典型品牌的这种共聚物可以按商标Peformathox Ethoxylate(ex Baker Petrolite)来获得。
其它优选的两亲性材料是明胶，非必需地与选自甲醛、戊二醛或二琥珀酰亚氨基辛二酸酯的交联剂交联，其中将两种反应物添加至形成液晶的材料中，并且交联反应优选就地并且是在形成液晶相之后进行。优选明胶的起霜强度(Bloom strength)高于250。起霜强度在British Standard BF 757有所定义。最优选的明胶是来自猪皮的、起霜强度为300的明胶，该明胶可获得自例如Sigma Chemie。
亲水性有机增强材料包括亲水性官能单体和聚合物，非必需地与交联剂结合.实例包括丙烯酰胺、N-烷基丙烯酰胺或可以与其它反应性本体形成化学键的任何水溶性多官能本体.水溶性聚合物包括聚((甲基)丙烯酸-共-丙烯酸烷基酯)共聚物，例如，CarbopolTM，或者含有聚(丙烯酰胺)、聚(乙烯基醇)、聚(氧化亚烷基)部分的共聚物，或其混合物，及与多价金属离子如钙和铝交联的藻酸盐。
一种优选的亲水性有机增强材料是与N，N-双丙烯酰胺交联的丙烯酰胺，其中将两种反应物添加至形成液晶的材料中，并且交联反应优选就地、使用适宜的催化剂如偶氮-二-异丁腈AIBN、并且是在形成晶体相之后进行。
特别优选的亲水性增强材料是藻酸盐，其非必需地与两亲性改性淀粉或糊精掺混。优选的藻酸盐的1％溶液粘度低于50mPas，当在20℃水中用锭子数为1并且在60rpm下操作的Brookfield粘度计测定时。典型品牌的这种藻酸盐是Grindsted FD 120和Grindsted LFD1515，ex Danisco或Kelton LV，ex ISP。最优选的藻酸盐是GrinstedFD 120。适宜的两亲性改性淀粉和糊精是琥珀酸辛烯酯型的淀粉衍生物，如CapsulTM和Hi-CapTM100，可获得自National Starch。
疏水性增强材料包括单体(其非必需地与交联剂结合)，可部分结晶的聚烯烃，嵌段和接枝共聚物，如苯乙烯-丁二烯或苯乙烯-异戊二烯二嵌段和三嵌段共聚物，聚(乙烯-共-二甲基硅氧烷)嵌段和接枝共聚物，高度交联的硅氧烷树脂，聚倍半硅氧烷，疏水化改性的硅酸盐和氨基硅酸盐，或者可热或UV固化的聚合物，如带有可热或光活化交联的官能团的聚丙烯酸酯。
一种优选的疏水性增强剂是分子量低于10,000g/mol并且优选低于1000g/mol的结晶性或部分结晶性聚乙烯，如可按商标Performalene(ex Baker Petrolite)获得的那些，或者在25℃下，当按5％溶解于80/20重量的甲苯/甲醇中时的Ubbelohde溶液粘度高于50mPas的乙基纤维素，如可按商标Ethnocel NF 100(ex Dow ChemicalCompany)商购获得的乙基纤维素。
作为无机增强剂，可以提及的是含二氧化硅的化合物，如烷基和烷氧基硅烷，及与多价金属离子的盐结合的硅酸钠(可按含水溶液形式商购获得，称作″水玻璃″)，其中所述多价金属离子的盐如硫酸钙和硫酸铝。
一种优选的无机增强材料是与钙结合的硅酸钠，其中将硅酸钠添加至形成液晶的材料中，并且交联反应是在形成液晶相之后通过后加氯化钙而就地进行的。
所用的具体的增强材料取决于所需要的结构形成特性。例如，可以使用能通过范德华力缔合或者能轻度交联以便产生软质凝胶的材料。或者，可以使用高度交联的增强材料来获得硬质的玻璃状凝胶。本领域技术人员知道形成特别硬质、脆性凝胶或软质凝胶或者具有介于这些极端性质之间特性的凝胶所必需的材料。
本文上述的增强材料可提高液晶结构在高温下的稳定性，并且甚至可以增加结构在高于所用特定形成液晶的材料的各向同性/各向异性转变温度下的热稳定性。由此能够确保芳香物质可以保持被包封，在超过40℃的温度下、更特别是在超过45℃的温度下具有优越的保留性。
除此之外，意想不到地发现，通过使用无机或轻度交联的增强材料，可以获得非常脆性的液晶结构，当在经过处理的表面上干燥时，所述液晶结构在剪切力的条件下碎裂，从而以类似突放的形式释放芳香物.在此方面，特别有利的增强材料是胶体硅酸钠和硅烷衍生物，如四(烷氧基硅烷).
形成液晶的材料可以选自本领域已知的能够在含有油和水的体系中形成准-结晶相或有序结构的任何组分。形成液晶的材料优选可以含有能够形成高熔融层状相的表面活性剂。高熔融层状相的特征在于存在一个或多个大于35℃、优选大于50℃并且最优选大于60℃的熔融温度，其可以通过差示扫描量热法根据本领域已知的技术来检测。
尤其是，形成液晶的材料可以含有非离子表面活性剂和具有16个或更多碳原子的长链脂肪醇，其中至少一种长链脂肪醇具有至少22个碳原子。非离子表面活性剂可以选自：
I)带有具有至少20个碳原子烷基的烷基糖苷或烷基多苷(polyolosides)；优选的烷基糖苷基形成液晶的材料是具有含至少20个碳原子的饱和或不饱和烷基残基的烷基糖苷和具有至少16个碳原子的长链脂肪醇的混合物，其中所述长链脂肪醇例如可按商标Montanov 202(ex Seppic)商购获得；
II)带有链长长于18个碳原子的烷基链的聚山梨酸烷基酯。优选的聚山梨酸烷基酯选自如EP 0466235中公开的聚乙氧基化脱水山梨醇脂肪酸酯，其引入本文作为参考，及它们与脱水山梨醇硬脂酸酯和具有14个碳原子以上的长链直链醇的掺混物。典型品牌的聚山梨酸烷基酯和脱水山梨醇硬脂酸酯分别是TweenTM60和SpanTM 60，ex Uniqema。优选的聚山梨酸烷基酯基形成液晶的成分可以是以聚山梨酸酯60和鲸蜡硬脂醇的混合物形式按商标Polawax NF(ex Croda)商购获得的；和
III)具有烷基残基的乙氧基化脂肪酯，其中所述烷基残基具有18个或更多碳原子。优选的脂肪酯乙氧基化物基形成液晶的材料是具有20个氧化乙烯单元的聚乙二醇硬脂酸酯，如可以与鲸蜡硬脂基醇的掺混物形式按商标Polawax GP 200(ex Croda)商购获得。
本发明制剂中的另一种组分是具有22个或更多碳原子的脂肪醇。优选，这种醇选自具有烷基或链烯基残基的那些脂肪醇，其中所述烷基或链烯基残基具有至少22个碳原子。更优选，脂肪醇具有窄分子量分布，即，至少90％的所用脂肪醇由具有22个或更多碳原子的单一脂肪酸残基组成。仍更优选，所用的脂肪醇不含含量高于5％的任何支链烷基残基。该醇的作用是增加所用的特定形成液晶的组分的各向同性/各向异性转变温度。优选的长链脂肪醇是1-二十二烷醇(ex Fluka)和较高的类似物。
具有22个或更多碳原子的脂肪醇的量可以是形成液晶的材料的10-90wt％，优选30-75wt％，并且最优选40-60wt％。
本发明组合物的X-射线散射强度模式可以在散射矢量区域显现一个或多个强度峰，其中所述散射矢量区域对应于范围从约30至120埃的典型周期长度。
根据本发明的一个优选的组合物，液晶结构的典型周期长度范围从40至60埃。X-射线散射技术及其对于液晶的应用可在D.M.Engelman(1985)Modern Trends of Colloid Sciences，H.-F.Eicke(编)，Bikhauser Verlag Basel中找到，其引入本文作为参考。
芳香物质可以含有选自以下的芳香组分：天然产品，如精油、净油、香树脂、树脂、香脂，及合成香料组分，如烃类、醇类、醛类、酮类、醚类、酸类、缩醛类、缩酮类和腈类，包括饱和和不饱和化合物、脂族、碳环族和杂环化合物。其它可以使用的增香组分的实例在H 1468(United States Statutory Invention Registration)中有所描述。
优选的芳香组分的实例是选自以下的任何芳香物质：Aldron，黄葵内酯，降龙涎香醚，肉桂酸苄酯，水杨酸苄酯，Boisambrene Forte，雪松醇晶体，乙酸柏木酯晶体，萨利麝香/Crysolide，Cetalox，乙草酸香茅酯，Fixal，Fixolide，加乐麝香，乙酸愈创木酯，水杨酸顺-3-己烯酯，己基肉桂醛，水杨酸己酯，Iso E Super，苯甲酸芳樟酯，肉桂酸芳樟酯，苯乙酸芳樟酯，甲基柏木基酮，Moskene，麝香，麝香酮，西藏麝香，二甲苯麝香，异己烯基四氢苯甲醇乙酸酯，乙酸橙花叔酯，Novalide，Okoumal，辛酸对-甲酚酯，苯乙酸对-甲酚酯晶体，5-乙酰基-1，1，2，3，3，6-六甲基茚满晶体，肉桂酸苯乙酯，水杨酸苯乙酯，玫瑰晶体/结晶玫瑰，Sandela(Lin)，十四腈，环十戊内酯，5-乙酰基-1，1，2，6-四甲基-3-异丙基茚满，三甲基环十二碳三烯酮O，2-甲基吡嗪，乙醛苯乙醇丙醇缩醛，苯乙酮，C6醇(在以下的符号表示中，Cn包括具有n个碳原子和一个羟基的所有物质)，C8醇，C6醛(在以下的符号表示中，Cn包括具有n个碳原子和一个醛官能团的所有异构体)，C7醛，C8醛，C9醛，壬烯醛，戊基甘醇酸烯丙酯，己酸烯丙酯，丁酸烯丙酯，Aldehyde anisique，苯甲醛，乙酸苄酯，苄基丙酮，苄醇，丁酸苄酯，甲酸苄酯，异戊酸苄酯，苄基甲基醚，丙酸苄酯，乙酸香柠檬酯，乙酸丁酯，樟脑，3-甲基-5-丙基-2-环己烯酮，肉桂醛，顺-3-己烯醇，乙酸顺-3-己烯酯，甲酸顺-3-己烯酯，异丁酸顺-3-己烯酯，丙酸顺-3-己烯酯，惕各酸顺-3-己烯酯，香茅醛，香茅醇，香茅腈，2-羟基-3-甲基-2-环戊烯-1-酮，枯茗醛，Cyclal C，乙酸(环己氧基)-2-丙烯基酯，大马烯酮，二氢大马酮α，二氢大马酮β，十氢β-萘基甲酸酯，丙二酸二乙酯，二氢茉莉酮，二氢芳樟醇，二氢月桂烯醇，二氢萜品醇，N-甲基代邻氨基苯甲酸甲酯，二甲基苄基原醇，乙酸二甲基苄基原酯，二甲基辛烯酮，2，6-二甲基-2-庚醇，二聚月桂醇，蒿脑，乙酸乙酯，乙酰乙酸乙酯，苯甲酸乙酯，庚酸乙酯，乙基芳樟醇，水杨酸乙酯，2-甲基丁酸乙酯，桉叶油素，丁子香酚，乙酸葑酯，葑醇，4-苯基-2，4，6-三甲基1，3-二噁烷，2-辛炔酸甲酯，4-异丙基环己醇，2-仲-丁基环己酮，乙酸苏合香酯，香叶腈，乙酸己酯，紫罗兰香酮α，乙酸异戊酯，乙酸异丁酯，异环柠檬醛，二氢异茉莉酮，异薄荷酮，异戊炔酸酯，异蒲勒醇，顺-茉莉酮，左旋香芹酮，苯乙醛甘油缩醛，原酸3-己烯基甲基醚，1-甲基-环己-1，3-二烯，芳樟醇，氧化芳樟醇，戊酸乙酯2，6-二甲基-5-庚烯醛，薄荷醇，薄荷酮，对甲基苯乙酮，甲基戊基酮，苯甲酸甲酯，甲基肉桂醛α，甲基庚烯酮，甲基己基酮，对甲酚甲醚，苯乙酸甲酯，水杨酸甲酯，橙花醛，橙花醇，4-叔-戊基-环己酮，对甲酚，乙酸对甲酚酯，对叔丁基环己酮，对甲基苯甲醛，苯乙醛，乙酸苯乙酯，苯乙醇，丁酸苯乙酯，甲酸苯乙酯，异丁酸苯乙酯，丙酸苯乙酯，乙酸苯丙酯，苯丙醛，四氢-2，4-二甲基-4-戊基-呋喃，4-甲基-2-(2-甲基-1-丙烯基)四氢吡喃，5-甲基-3-庚酮肟，丙酸苏合香酯，苯乙烯单体，4-甲基苯乙醛，萜品醇，萜品油烯，四氢芳樟醇，四氢月桂烯醇，反-2-己烯醛，4，7-桥亚甲基-1H-3A，4，5，6，7，7A-六氢-乙酸酯和苯乙醛二甲缩醛。
也可以将芳香组分的前体提供在本发明的芳香物质中。前体是当处于例如光、酶、高温或者酸性或碱性pH值的活化条件下裂解时提供具有芳香特征的化合物的化合物。此外，可以将其它感观性物质与芳香成分掺混使用，例如，气味遮蔽剂、驱虫剂等等。
除芳香成分或前述的其它感官性物质外，芳香物质中还可以含有其它成分。例如，液滴中可以含有油、非极性聚合物、蜡或树脂，其中芳香物质或其它感官成分可以分散或溶解在其中。
适宜的油的实例包括用于分散或溶解包胶型芳香制剂中的芳香物质或其它感官成分的已知的油，并且包括植物、动物或矿物油或其混合物。
树脂包括通过将β-蒎烯、氢化松香或松香酯、谷甾醇衍生物和熔点高于50℃的饱和松香酯聚合产生的三萜烯。
蜡可以选自于那些矿物、植物、动物或合成来源的蜡。实例包括蜂蜡、氢化油、脂肪酸、酯蜡、一或二或三取代的甘油，其取代基是饱和或不饱和有机化合物、石蜡、微晶蜡、石油蜡、烷基硅氧烷及其混合物。尤其是，可以将芳香物质与烷基改性硅氧烷掺混，其中所述烷基改性硅氧烷具有含超过20个碳原子的烷基侧链，并且熔点高于70℃。意想不到地，申请人发现，使用烷基改性硅氧烷材料进一步提高本发明组合物的热稳定性，以及芳香物质中挥发性组分的保留和缓释。就此，如果使用它们的话，则烷基改性硅氧烷代表芳香液滴中的优选成分。
优选的烷基改性硅氧烷蜡具有含30个或更多碳原子的烷基残基并且可按商标名称AMS C 30蜡商购获得(ex Dow Corning)。
本发明的芳香组合物是含水组合物，例如以糊剂的形式，其可以含有10-30％芳香物质、10-50％形成液晶的材料、0.5％-10％增强材料和10-80％水。芳香组合物中可以含有水包油型体系中常用的其它油或水可分散性的辅剂，如染料、着色剂、防腐剂、抗氧化剂等等。
此外，本发明的芳香组合物可以含有阳离子化合物，其功能是增强组合物对于基底的亲合性，其中所述基底如棉织物、头发或皮肤。适宜的阳离子化合物可以选自阳离子聚碳水化合物，如阳离子纤维素、阳离子瓜耳树胶衍生物和脱乙酰壳多糖、季铵化N-杂环衍生物，如1-乙烯基-2-吡咯烷、乙烯基吡咯烷酮和1-乙烯基-3-甲基氯化咪唑鎓、季化胺和聚亚烷基亚胺。优选，阳离子化合物的存在量为液晶材料的最高5％，优选最高3％。
更优选，芳香组合物的特征还在于在高于50℃的温度下出现熔融转变，通过差示扫描量热法以1℃/分钟的加热速率测定。
还可以将本发明的芳香组合物在高剪切混合器的作用下于室温下分散在水中，其中所述高剪切混合器一般是在5000-20000rpm下操作，以便形成基本上水不溶性颗粒的分散液，其中所述颗粒一般由40-60％形成液晶的材料、1-20％增强材料和30-60％芳香物质组成，而可以预料在颗粒中可以存在少量的水，一般是最多5wt％的水，以间隙水的形式存在。
这种含水分散液具有比糊剂组合物更低的粘度，可以更容易加工，例如如果要进行进一步混合或喷雾步骤的话。
或者，可以使用本领域已知的技术，将上述形式的芳香组合物干燥，形成粉末.粉末的形成优选是通过将芳香组合物的颗粒分散在水中，与水胶体混合并且将混合物喷雾干燥，形成自由流动的粉末，其颗粒粒度分布为50-400微米之间并且由固体基质材料组成，其中所述固体基质材料具有分散在其中的微粒.优选的水胶体是选自改性淀粉、麦芽糖糊精、聚乙烯醇的多糖类，将其与糖结合.还可以通过常规技术进一步将喷雾干燥的产物附聚，所述常规技术如流化床粒化、湿法粒化和熔融粒化，以便形成颗粒粒度范围为400-1500微米或更大的粒状材料，由此使得将所述干燥形式处置和混合在粉末产品如洗衣护理用洗涤剂中更容易，并且使得将所述干燥形式控制溶解在洗液中更容易.非必需地，可以向受到喷雾干燥处理的混合物中添加附加的阴离子、两性离子、或优选阳离子表面活性剂，以便提供带电水不溶性颗粒.
还可以将上述芳香组合物混合入家用和个人护理消费者用品基料中，如洗衣护理或头发护理调理剂基料，清洁组合物，如液体皂或沐浴凝胶，液体洗涤剂，洗碗产品，漂白或硬表面清洁剂基料或者皂条基料。这种基料是本领域所公知的并且无需在这里进一步讨论，这些基料的代表实例可见EP 0466235A，其引入本文作为参考。
前述芳香物质在前述消费者用品中的添加量范围可以是消费者用品基料的0.1-3wt％。一般来说，通常添加至消费者用品的总香料的一部分可以是以本发明的芳香物质的形式添加。由此，例如，在消费者用品中所含的总芳香成分中，30％是芳香组合物的形式，并且在所含的总芳香成分中，60％是游离芳香油的形式。
本发明的芳香组合物可以是以分散在含水相中的含有液晶结构的颗粒的形式提供。颗粒的粒度范围可以优选是1-100微米之间，更优选1-50微米并且最优选1-10微米。
本发明的芳香组合物可以在各种条件下使用本领域通常已知的技术来形成。通常来说，分别单独形成含有所有油溶性成分的油相和含有水溶性成分的含水相，然后在一定的温度下用中等剪切螺旋桨混合在一起，其中所述中等剪切螺旋桨一般在20-250rpm下操作，非必需地与高剪切混合器联合使用，其中所述高剪切混合器一般在10,000-20,000rpm下操作。
更具体说，第一步，可以将所有的油溶性成分(任何油溶性交联剂和催化剂除外)与芳香物质在高于混合物熔点的温度下(例如约60-90℃)混合在一起。之后，可以在与前述温度相当的温度下制备所有水溶性成分(任何水溶性交联剂和催化剂除外)的含水溶液。最后，用低剪切螺旋桨轻微混合将所得的混合物冷却至室温，其中所述低剪切螺旋桨一般是在10-50rpm下操作，以便形成本发明的组合物。关于形成芳香组合物的更详细信息在下面的实施例中给出。
非必需地，在其中增强材料是通过交联来获得的情形中，可以在前述的混合物制成之后，于混合温度和室温之间的任何温度下，添加水溶性或油溶性的交联剂或催化剂，形成合意的增强的组合物。
也可以在将芳香组合物分散在水或消费者用品基料中之后，添加交联剂和催化剂，并且让交联反应在室温和粒状形式中存在的芳香物质的各向异性至各向同性的转变温度之间的任何温度下进行。
使用本发明的芳香组合物，以其中芳香物质可以包含在芳香组合物的形式，可以使家用和个人护理产品在高储存温度下增香数个月，所述储存温度例如是45℃的储存温度。即使是在延长期限储存之后，产品仍能够以受控方式给表面传递高强度的平衡香气，传递的期限达24小时甚至更长，例如高达5天。
下面给出一系列非限定性实施例，这些实施例起举例说明本发明的作用。
实施例1
芳香组合物的形成
按照以下方法形成一系列芳香组合物(参见下表I)：
将所有的油溶性成分与芳香油(香料)在75℃下于一封闭容器中混合，直至所有成分溶解。
将所有的水溶性成分溶解于水中，并且将含水溶液在80℃下加热，在中等剪切混合下，用家制的螺旋桨混合器(2300rpm下操作)逐滴添加至上述溶液中。
之后，让芳香组合物冷却至室温。
表I
| 样品 | #1 | #2 | #3 | #4 |
| 油溶性成分 | ||||
| 芳香油(1) | 20 | 20 | 20 | 20 |
| POLAWAX NF(ex Croda) | 25 | 12.5 | 10 | 10 |
| 1-二十二烷醇(ex Fluka) | 12.5 | 10 | 10 | |
| PERFORMALENE 400(2) | 5 | |||
| 水溶性成分 | ||||
| 水 | 55 | 55 | 55 | 55 |
| 硅酸钠 | 5 |
(1)所选的芳香油是含有基本上挥发性芳香成分的均衡试验混合物，所述挥发性芳香成分是乙酸戊酯、桉叶油素、二甲基辛烯酮、cyclalC、芳樟醇、醛C12MNA、苯乙醛二甲缩醛、萜品油、乙酸苄酯、紫罗兰酮、乙酸三环癸烯酯、苯乙醇、二苯醚、椰子醛、新铃兰醛。
(2)分子量范围为1000-4000g/mol的可结晶聚烯烃
(3)可按使用名称″水玻璃″商购获得(ex Fluka)并且具有式Na2O.3SiO2。在本发明的情形中，将氯化钙在室温下添加至芳香组合物中并且允许彻底扩散于组合物中24小时。
制剂1和2是未增强的对比实施例。制剂3和4是增强的本发明的组合物。
实施例2
增强的和未增强的芳香组合物的流变性
使用Paar Physica流变计MCR 300进行流变性的测定，其中所述流变计MCR 300装配有圆锥-板测定单元并且以振荡模式操作。圆锥-板测定单元CP25-2的特征如下：剪切速率系数：3s-1/min-1，剪切应力系数：12.223Pa，样品体积：0.16cm3，测定圆锥半径：12.5mm，测定圆锥角度：2°，圆锥切断：50微米。测定组合物的粘弹性响应(通过储能模量G′、损耗模量G″来表征)，作为形变幅度的函数。图1显示了通过添加PerformaleneTM400(一种本发明特别优选的增强剂)诱发了弹性模量的增加。
从图1中可以看出，增强的组合物的储能弹性模量大大高于未增强的组合物，说明前者是更具劲度的组合物.添加聚乙烯可使平台的储能弹性模量数值增加至少一个数量级.平台储能模量的新平均值接近于105Pa，而未增强样品的数值为103。此外，未增强组合物中的G′和G″的交叉接近于5％形变，而在增强的组合物中，交叉更接近于1％形变。这说明增强的组合物相比未增强的组合物具有更大的刚性。
实施例3
在织物调理剂中的应用
通过以下过程获得标准未增香的织物调理剂组合物：将5％二氢化牛油乙基羟乙基硫酸二乙铵(dihydrogenated tallowethylhydroxyethylmonium ethosulfate)(RewoquaTM WE 18，ex Degussa)和0.5％C9-11Pareth-8(NeodolTM 91 8E，ex Shell)溶解于65℃去离子水中，接着在2000rpm搅拌条件下冷却至室温。
使用高剪切混合器(Ultraturrax IKA T25，在10000rpm下操作)，将实施例1的芳香组合物分散在标准未增香的织物调理组合物中。最终混合物中香料的总量为1％。将调理组合物在45℃下老化1个月，然后对比新制备的调理组合物进行嗅觉评价。将1.4克增香的织物调理组合物搅拌分散在1升水中。用此溶液将干净的棉巾漂洗10分钟并且使其线干燥(line drying)。
对干织物的嗅觉评价：
在24小时之后和在室温下5天之后，通过至少五名受训专家来评测干织物的嗅觉感觉，将所有的组合物与对照样品(单独的香料)进行对比。香味的强度根据以下等级来评分：
1＝几乎感觉不到
2＝弱
3＝中等
4＝强
嗅觉评价结果示于下表II。
表II
| 样品 | 新样品24h | 新样品5天 | 老化样品24h | 老化样品5天 |
| 对照 | 1 | 1 | 0 | 0 |
| #1 | 1.5 | 1 | ＜1 | 0 |
| #2 | 3 | 1.5 | 1.5 | 1 |
| #3 | 4 | 3 | 3 | 2 |
| #4 | 3.5 | 2.5 | 2 | 1.5 |
从这些数据中显然看出，本发明的组合物3和4强于无香料的对照样品，也强于未增强组合物处理过的样品。已知样品4具有脆性性质，通过摩擦毛巾来释放芳香物。
实施例4
含有疏水性增强剂的芳香组合物的其它实例
采用与实施例1相同的过程，但在制备组合物之前，将疏水性增强剂溶解于油相中(表III)
表III
| 样品 | #5 | #6 | #7 | #8 |
| 油溶性成分 | ||||
| 芳香油(如同实施例1) | 20 | 20 | 20 | 20 |
| POLAWAX NF | 10 | 10 | 10 | 10 |
| 1-二十二烷醇 | 10 | 10 | 10 | 10 |
| 乙基纤维素NF | 2 | |||
| AMS C 30(ex Dow Corning) | 5 | |||
| PERFORMALENE 2000 | 2 | |||
| PERFORMATHOX 480(3) | 5 | |||
| 水溶性成分 | ||||
| 水 | 58 | 55 | 58 | 55 |
(3)聚乙烯(C20-C40)和聚氧化乙烯(40 EO单元)的嵌段共聚物(ex Petrolite)。
含有亲水性增强剂的芳香组合物的其它实例
采用与实施例1相同的过程，但在制备组合物之前，将亲水性增强剂溶解于水相中(表IV)。
表IV
| 样品 | #9 | #10 | #11 | #12 |
| 油溶性成分 | ||||
| 芳香油(如同实施例1) | 20 | 20 | 20 | 20 |
| POLAWAX NF | 30 | 10 | 10 | 10 |
| 样品 | #9 | #10 | #11 | #12 |
| 1-二十二烷醇 | 10 | 10 | 10 | 10 |
| PERFORMALENE 400(2) | 5 | |||
| 水溶性成分 | ||||
| 水 | 30 | 53 | 57.55 | 59.10 |
| Mowiol 4/88(ex Kuraray) | 10 | |||
| 明胶型A 300起霜剂(ex Sigma) | 1 | |||
| 戊二醛 | 1 | |||
| 藻酸盐FD 120(ex Danisco) | 2.45 | |||
| 藻酸盐Kelton LV(ex ISP) | 0.4 | |||
| Capsul(ex National Starch) | 0.5 |
织物调理剂组合物的评价
采用与实施例3的相同方法，不同之处是，在此情形中，漂洗循环过程在常规的前面装载式洗衣机中进行，使用的毛巾重量440g、水体积7.4L和时间8分钟。所用温度是自来水的温度。在45℃下储存1个月后进行评价(表V)。
表V
| 样品 | 老化的对照24h | 老化的对照5天 | 老化样品24h | 老化样品5天 |
| #5 | 0 | 0 | 2.2 | 1.3 |
| #6 | 0.2 | 0 | 2.4 | 1.3 |
| #7 | 0.5 | 0.2 | 2.6 | 2.4 |
| #8 | 0.5 | 0.2 | 2.3 | 2.2 |
| #9 | 0.2 | 0 | 2.3 | 0.7 |
| #10 | 0.2 | 0 | 2 | 0.9 |
| #11 | 0.3 | 0 | 3.3 | 1.2 |
| 样品 | 老化的对照24h | 老化的对照5天 | 老化样品24h | 老化样品5天 |
| #12 | 0.3 | 0 | 3.2 | 0.8 |
实施例5
含有阳离子化合物的芳香组合物
采用与实施例1中的相同过程，但在制备芳香组合物之前向水相中添加阳离子化合物(表VI)。
表VI
| 样品 | #13 | #14 | #15 |
| 油溶性成分 | |||
| 芳香油(如同实施例1) | 20 | 20 | 20 |
| POLAWAX NF | 10 | 10 | 10 |
| 1-二十二烷醇 | 10 | 10 | 10 |
| PERFORMALENE 400(2) | 5 | 5 | 5 |
| 水溶性成分 | |||
| LUPASOL P(ex BASF) | 0.6 | 0.6 | |
| REWOQUAT RTM 50(ex Degussa) | 0.6 | ||
| 脱乙酰壳多糖SC23(ex Orffa-Pomosin) | 0.6 | ||
| 柠檬酸(ex Fluka) | 1.5 | ||
| 水 | 54.4 | 54.4 | 52.3 |
实施例6
制备喷雾干燥的芳香组合物
通过以下步骤制备含有芳香组合物的粉末：
1)按照实施例1所述的方法形成芳香组合物。
2)在一单独的容器中，将所选择的水溶性材料、表面活性剂和水胶体及非必需的香料油(参见表VI)溶解于60℃水中(进料介质)，让其在室温下冷却。
3)使用Polytron混合单元(在8500rpm下操作)，将芳香组合物分散在溶液2中.粉末的最终组成在表VII中给出.
将分散液在常规喷雾干燥塔中(Niro Mobile Minor Atomizer)经由两个流体喷嘴进行喷雾，使用以下加工参数：
入口温度：180℃
出口温度：80℃
进料速率：34.8g/min
雾化速度：18000rpm
下表VII显示了干材料的组成。
表VII
| 样品 | #13 | #14 | #15 |
| 芳香组合物 | |||
| 从实施例#1-12选择的组合物(无水) | 68.3 | ||
| 芳香油 | 15.47 | 13.32 | |
| POLAWAX NF | 30.99 | 26.65 | |
| CAPSUL | 5.75 | 4.93 | |
| KELTON | 3.25 | 2.81 | |
| 进料介质 | |||
| MALDOTEXTRIN IT-6 | 28.19 | 44.50 | |
| CAPSUL | 3.51 | ||
| 芳香油 | 28.65 | ||
| MOWIOL 3-83(ex Clariant) | |||
| MOWIOL 3-96(ex Clariant) | 20.56 | ||
| GAFQUAT HS-100(ex ISP) | 1.32 | ||
| REWOQUAT W-3690(ex Degussa) | 1.32 | ||
| (ISOPROPANOL) | (0.44) |
Claims (9)
1.一种用于家用产品和个人护理产品的包封在液晶结构中的芳香组合物，其含有按组合物的重量计
10-80％的水，
10-30％的芳香物质，
10-50％的形成液晶的材料，其中所述形成液晶的材料含有非离子表面活性剂和至少一种具有至少22个碳原子的脂肪醇，和
0.5-10％的增强材料，和所述增强材料是使得被包封的芳香组合物显出储能弹性模量在25℃下高于103Pa的平台区，这通过在PaarPhysica流变计MCR 300上测定，其中所述流变计MCR 300装配有圆锥-板测定单元并且以振荡模式操作，圆锥-板测定单元CP25-2具有如下特征：剪切速率系数：3s-1/min-1，剪切应力系数：12.223Pa，样品体积：0.16cm3，测定圆锥半径：12.5mm，测定圆锥角度：2°，圆锥切断：50微米，并且
所述增强材料选自
-分子量低于10,000g/mol的结晶性或部分结晶性聚乙烯，
-氧化乙烯含量低于80％且分子量低于2500g/mol的聚(乙烯-b-氧化乙烯)，
-藻酸盐，其非必需地与两亲性改性淀粉或糊精掺混，并且当在20℃水中用锭子数为1并且在60rpm下操作的Brookfield粘度计测定时具有低于50mPas的1％溶液粘度，和
-与钙结合的硅酸钠，其中将硅酸钠添加至形成液晶的材料中，并且交联反应是在形成液晶相之后通过后加氯化钙而就地进行的。
2.权利要求1的芳香组合物，其中非离子表面活性剂选自：
I)带有含至少20个碳原子的烷基链的烷基糖苷；
II)带有链长长于18个碳原子的烷基链的烷基聚山梨酸酯；和
III)具有烷基残基的乙氧基化脂肪酯，其中所述烷基残基具有至少18个碳原子。
3.权利要求1或2的芳香组合物，其中具有至少22个碳原子的所述醇选自具有窄分子量分布的脂肪醇，致使至少90％的这种脂肪醇由单一脂肪酸残基组成。
4.权利要求1或2的芳香组合物，呈颗粒的含水分散液形式，所述颗粒含有液晶结构。
5.权利要求1或2的芳香组合物，其中组合物具有周期长度在30-120埃之间的液晶相，所述周期长度通过X-射线衍射测定。
6.权利要求5的芳香组合物，其中周期长度在40-60埃之间。
7.权利要求1的芳香组合物，其中组合物在高于50℃的温度下显示至少一个熔融转变。
8.含有权利要求1-7任一项所述组合物的家用产品。
9.含有权利要求1-7任一项所述组合物的个人护理产品。
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| PCT/CH2004/000039 WO2004064790A1 (en) | 2003-01-24 | 2004-01-26 | Fragrance compositions |
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| US20080300314A1 (en) * | 2003-11-21 | 2008-12-04 | Givaudan Sa | Cooling Compounds |
| US20050238680A1 (en) | 2004-04-21 | 2005-10-27 | Qing Stella | Personal care compositions that deposit hydrophilic benefit agents |
| JP2008521942A (ja) * | 2004-11-29 | 2008-06-26 | ジボダン エス エー | 基材ケア製品 |
| WO2007019719A1 (en) * | 2005-08-15 | 2007-02-22 | Givaudan Sa | Cooling compounds |
| US20090098066A1 (en) * | 2005-08-22 | 2009-04-16 | Galopin Christophe C | Substituted bicyclo [2.2.2] oct/5-ene compounds and their use as cooling agents |
| US8263046B2 (en) * | 2005-10-25 | 2012-09-11 | Givaudan S.A. | N-phenyl-N-pyridinyl-benzamides and benzenesulfonomides having cooling properties |
| EP1996535A2 (en) * | 2006-03-15 | 2008-12-03 | Givaudan SA | Para-substituted 2-alkoxyphenol compounds |
| WO2008061384A1 (en) * | 2006-11-20 | 2008-05-29 | Givaudan Sa | Preparation of an emulsion comprising lamellar liquid crystal (llc) particles containing fragrance |
| WO2008134908A1 (en) * | 2007-05-08 | 2008-11-13 | Givaudan Sa | Wax encapsulation |
| EP2167024B1 (en) | 2007-06-13 | 2012-01-11 | Givaudan SA | Cooling compounds |
| US7880011B2 (en) | 2007-07-23 | 2011-02-01 | Givandan, S.A. | Amide addition reaction |
| EP2250154A1 (en) * | 2008-01-17 | 2010-11-17 | Givaudan SA | Benzimidazole derivatives and their use as cooling agents |
| EP2204155A1 (en) * | 2008-12-30 | 2010-07-07 | Takasago International Corporation | Fragrance composition for core shell microcapsules |
| US9993019B2 (en) * | 2010-03-26 | 2018-06-12 | Philip Morris Usa Inc. | Method for making particle of a hydrophobic additive and a polysaccharide coating and tobacco products containing particle of a hydrophobic additive and a polysaccharide coating |
| JP2014105164A (ja) * | 2012-11-26 | 2014-06-09 | Kao Corp | 香料放出用組成物 |
| US9655837B2 (en) | 2012-11-27 | 2017-05-23 | International Flavors & Fragances Inc. | Oil-continuous liquid crystalline phase formulation and use of the same |
| CN105792806A (zh) * | 2013-11-29 | 2016-07-20 | 株式会社爱茉莉太平洋 | 具有层状液晶结构的毛发用化妆品组合物 |
| UA120260C2 (uk) * | 2013-12-31 | 2019-11-11 | Філіп Морріс Продактс С.А. | Курильний виріб з компонентом вивільнення рідини |
| JP6576315B2 (ja) * | 2016-09-12 | 2019-09-18 | 玉理化学株式会社 | 疎水性固形組成物を含有する化粧料及びその製造方法 |
| CN108498364A (zh) * | 2017-02-24 | 2018-09-07 | 上海凡因生物科技有限公司 | 液晶体透皮吸收剂及其制备和在抗衰老化妆品中的应用 |
| CN108264642B (zh) * | 2018-02-12 | 2020-11-13 | 华东理工大学 | 一类基于2-羰基乙酸酯的纳米香料前体及其应用 |
| CA3200550A1 (en) * | 2020-12-16 | 2022-06-23 | Mattia Collu | Treatment compositions comprising plant rosin materials |
| CN113470756B (zh) * | 2021-07-05 | 2023-11-28 | 中国科学院化学研究所 | 芳香环化合物与脂肪族化合物交联模型及其构建方法 |
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| EP1166769B1 (en) * | 2000-06-06 | 2006-10-18 | Takasago International Corporation | Lipid composition having liquid crystal structure |
| CN1334073A (zh) * | 2000-07-21 | 2002-02-06 | 花王株式会社 | 发用化妆品组合物 |
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