CN112074590A - 粉末洗涤剂组合物 - Google Patents
粉末洗涤剂组合物 Download PDFInfo
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- CN112074590A CN112074590A CN201980030491.5A CN201980030491A CN112074590A CN 112074590 A CN112074590 A CN 112074590A CN 201980030491 A CN201980030491 A CN 201980030491A CN 112074590 A CN112074590 A CN 112074590A
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- oil
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Images
Classifications
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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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- 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
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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
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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
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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
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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
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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
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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
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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
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- C11D3/38609—Protease or amylase in solid compositions only
-
- 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
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- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38627—Preparations containing enzymes, e.g. protease or amylase containing lipase
-
- 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
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- C11D3/16—Organic compounds
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Abstract
本发明涉及一种粉末洗涤剂组合物,其包含:‑洗涤剂活性材料,其至少包含表面活性剂体系,‑粒状粉末,其包含由以下材料制成的颗粒:a)水溶性聚合物基质,b)油相,其包含分散在所述聚合物基质中的香料,所述油至少部分包封在微胶囊中,其中,基于粉末的总重量,粒状粉末包含至多30重量%的已包封油。
Description
技术领域
本发明涉及粉末洗涤剂组合物领域。更具体而言,本发明描述了一种粉末洗涤剂组合物,其包含洗涤剂活性材料(其包含表面活性剂体系)和粒状粉末,其包含香料含量低的颗粒,即,粒状粉末包含至多30重量%的已包封油。
背景技术
芳香剂在对消费品性能的感知中起着重要作用,因此,它们通常会决定消费者对特定产品的选择。
在洗涤剂、硬表面清洁剂或者个人或身体护理产品中,芳香剂以游离油的形式掺入和/或包封在微胶囊中,以便向织物、表面或皮肤传递令人愉悦的气味。
已包封芳香剂的主要优点之一是增强了芳香性能以及在施用期间和施用后(例如在清洗和干燥皮肤或织物之后)的嗅觉感知的持久性。
然而,当使用香料微胶囊时,必须考虑其他性质以提供具有良好品质的消费品。确实,当掺入到消费品基料中时,香料微胶囊通常处于“侵蚀性”环境中,因此必须表现出良好的稳定性且香料泄漏量少。此外,取决于消费品的类型,微胶囊在与基料的混合阶段中可能经受高机械应力,因此必须表现出良好的机械性能。
因此,令人感兴趣的是提供一种粒状粉末,其不仅在稳定性和嗅觉性能方面具有良好的性能,而且还可以经受得住需要高剪切力的制造过程。
本发明的粉末洗涤剂组合物解决了这个问题,因为它包含粒状粉末,该粒状粉末包含由根据最佳相对比例的聚合物基体和已包封油制成的颗粒,从而防止了制造过程中颗粒的磨损。
发明内容
本发明的第一目的是一种粉末洗涤剂组合物,其包含:
-洗涤剂活性材料,其至少包含表面活性剂体系,
-粒状粉末,其包含由以下材料制成的颗粒:
a)水溶性聚合物基质,
b)油相,其包含分散在所述聚合物基质中的香料,所述油至少部分包封在微胶囊中,
其中
-基于粉末的总重量,粒状粉末包含至多30重量%的已包封油。
本发明的第二个目的是制备如上定义的粉末洗涤剂组合物的方法,该方法包括将如上定义的粒状粉末与洗涤剂活性材料混合的步骤。
附图说明
图1表示与直接添加的微胶囊浆料相比,根据本发明的粒状粉末(即包含已包封香料油)在粉末洗涤剂中的嗅觉性能。
具体实施方式
除非另有说明,百分比(%)是指组合物的重量百分比。
当提及“颗粒”或“粒状粉末”时,给出干燥组合物的百分比(%)。
现在,本发明已经确定了一种在粉末洗涤剂的制造过程中经受高剪切条件时改善粒状粉末的机械抗性的方法。
实际上,本发明的第一目的是一种粉末洗涤剂组合物,其包含:
-洗涤剂活性材料,其至少包含表面活性剂体系,
-粒状粉末,其包含由以下材料制成的颗粒:
a)水溶性聚合物基质,
b)油相,其包含分散在所述聚合物基质中的香料,所述油至少部分包封在微胶囊中,
其中
-基于粉末的总重量,粒状粉末包含至多30重量%的已包封油。
本发明的粉末洗涤剂组合物应理解为能够洗涤织物的包含表面活性剂体系的组合物。相反,固体增香剂(即固体已加香珠粒)没有任何表面活性剂体系,并且不被认为是根据本发明的粉末洗涤剂组合物。
根据一个实施方案,本发明中定义的粉末洗涤剂不包含固体增香剂香料珠粒。
洗涤剂活性材料
洗涤剂活性材料包含至少一种表面活性剂体系。
表面活性剂体系可包含至少一种从由阴离子表面活性剂,非离子表面活性剂,阳离子表面活性剂,两性离子表面活性剂以及它们的混合物构成的群组中选出的表面活性剂。
洗涤剂活性材料中的表面活性剂优选从由如下构成的群组中选出:直链烯烃苯磺酸盐(LABS),月桂醇聚醚硫酸酯钠,月桂基醚硫酸钠(SLES),月桂基硫酸钠(SLS),α-烯烃磺酸盐(AOS),甲酯磺酸盐(MES),烷基聚葡糖苷(APG),伯醇乙氧基化物尤其是月桂醇乙氧基化物(LAE),伯醇磺酸盐(PAS),肥皂以及它们的混合物。
洗涤剂活性材料可包含通常用于粉末洗涤剂组合物中的另一种组分,其从由如下构成的群组中选出:漂白剂,缓冲剂;助洗剂(builders);污物释放或污物悬浮聚合物;粒状酶颗粒,缓蚀剂,消泡剂,抑泡剂(sud suppressing agents);染料,填充剂(fillers),以及它们的混合物。
根据一个特定的实施方案,洗涤剂活性材料包含:
a)5至50重量%,优选5至30重量%的表面活性剂,优选从由阴离子表面活性剂和非离子表面活性剂构成的群组中选出;
b)10至50重量%的填料,优选从由硅酸钠,硫酸钠以及它们的混合物构成的群组中选出;
c)10至30重量%的助洗剂,优选从由沸石,碳酸钠以及它们的混合物构成的群组中选出;
d)0至2重量%的酶,优选从由纤维素酶,脂肪酶,蛋白酶,甘露聚糖酶,果胶酶以及它们的混合物构成的群组中选出;
e)0至2重量%的游离香料;
f)0至20重量%的过氧化氢源,优选过碳酸钠或过硼酸钠,更优选过碳酸钠,和
g)0至5重量%的漂白活化剂,优选TAED(四乙酰基乙二胺),
百分比基于组合物的总重量计。
根据另一个特定的实施方案,该洗涤剂活性材料包括:
(i)5至50重量%,优选5至30重量%的表面活性剂,优选从由阴离子表面活性剂和非离子表面活性剂构成的群组中选出;
(ii)10至50重量%的填料,优选从由硅酸钠,硫酸钠以及它们的混合物构成的群组中选出;
(iii)10至30重量%的助洗剂,优选从由沸石,碳酸钠以及它们的混合物构成的群组中选出;
(iv)大于0至2重量%的酶,优选从由纤维素酶,脂肪酶,蛋白酶,甘露聚糖酶,果胶酶以及它们的混合物构成的群组中选出;
(v)大于0至2重量%的游离香料;
(vi)大于0至20重量%的过氧化氢源,优选过碳酸钠或过硼酸钠,更优选过碳酸钠,和
(vii)大于0至5重量%的漂白活化剂,优选TAED,
百分比基于组合物的总重量计。
包含颗粒的粒状粉末
根据本发明,粒状粉末包含由以下材料制成的颗粒:
a)水溶性聚合物基质,
b)油相,其包含分散在所述聚合物基质中的香料,所述油至少部分包封在微胶囊中。
水溶性聚合物基质
任何水溶性聚合物均可用于本发明的目的。优选地,水溶性聚合物具有乳化性能。
为了本发明的目的,“水溶性生物聚合物”旨在涵盖在水中形成一相溶液的任何生物聚合物。优选地,当以高达20重量%,更优选甚至高达50重量%的浓度溶解于水中时,它形成一相溶液。最优选地,当以任何浓度溶于水中时,它形成一相溶液。
本发明中定义的水溶性聚合物的例子是淀粉,改性淀粉,麦芽糊精,多糖,碳水化合物,壳聚糖,阿拉伯胶,聚乙二醇,聚乙烯吡咯烷酮,聚乙烯醇,丙烯酰胺,丙烯酸酯,聚丙烯酸和相关物,马来酸酐共聚物,胺官能聚合物,乙烯基醚,苯乙烯,聚苯乙烯磺酸盐,乙烯基酸,乙二醇-丙二醇嵌段共聚物,以及它们的混合物。
根据一个特定的实施方案,所述水溶性聚合物包含麦芽糊精,所述麦芽糊精的葡萄糖当量(DE)在3至20之间,优选在10至18之间。
根据一个实施方案,水溶性聚合物包含麦芽糊精18DE和/或麦芽糊精10DE。
根据一个特定的实施方案,水溶性聚合物包含麦芽糊精10DE。
根据一个实施方案,基于粉末的总重量,粒状粉末包含至少55重量%的水溶性聚合物。
根据一个特定的实施方案,基于粉末的总重量,粒状粉末包含55至95重量%,优选60至85重量%,更优选70至80重量%的水溶性聚合物。
根据一个实施方案,粒状粉末内的水溶性聚合物与已包封油之间的重量比为2至20,优选为3.5至10。
基质可包含防火剂或抑爆剂。喷雾干燥乳液中这类试剂的类型和浓度是本领域技术人员已知的。作为这种防火剂或抑爆剂的非限制性例子,可以列举无机盐,C1-C12羧酸,C1-C12羧酸的盐以及它们的混合物。优选的抑爆剂是水杨酸,乙酸,丙酸,丁酸,异丁酸,戊酸,己酸,柠檬酸,琥珀酸,羟基琥珀酸,马来酸,富马酸,草酸(oxylic acid),乙醛酸,己二酸,乳酸,酒石酸,抗坏血酸,任何上述酸的钾、钙和/或钠盐,以及这些中的任何混合物。
包含香料的油相
根据本发明,油相包含香料。
根据一个特定的实施方案,油相包含香料与另一种成分的混合物,所述另一种成分从由营养保健品,化妆品,昆虫控制剂和杀生物剂活性成分构成的群组中选出。
根据一个特定的实施方案,油相由香料组成。
所谓“香料”(或也称为“香料油”),在这里是指在约20℃下为液体的成分或组合物。根据以上任一个实施方案,所述香料油可以是单独的加香成分或加香组合物形式的成分的混合物。作为“加香成分”,在此是指一种化合物,其主要目的是用于赋予或调节气味。换言之,要被认为是加香成分的这种成分必须被本领域技术人员认识到能够至少以主动或令人愉快的方式赋予或改变组合物的气味,而不仅仅是具有气味。为了本发明的目的,香料油还包括加香成分与共同改善、增强或改变加香成分的递送的物质的组合,例如香料前体、乳液或分散体,以及赋予除改变或赋予气味之外的其他益处的组合,所述益处例如持久、迸发、恶臭抵消、抗菌效果、微生物稳定性、昆虫防治。
油相中存在的加香成分的性质和类型在这里不保证有更详细的描述,其无论如何都不会穷尽,本领域技术人员能够基于其普通常识并根据预期使用或应用以及所需的感官效果来选择它们。一般而言,这些加香成分属于不同的化学类别,如醇类、醛类、酮类、酯类、醚类、醋酸酯类、腈类、萜类化合物、含氮或含硫杂环化合物和精油,并且所述加香助成分可以是天然来源的或合成来源的。无论如何,许多的这些助成分列于参考文献诸如S.Arctander的著作Perfume and Flavor Chemicals,1969,Montclair,New Jersey,USA或其更新的版本或类似性质的其他著作中,以及香料业领域内丰富的专利文献中。还应当可理解的是,所述成分还可以是已知的以受控方式释放各种类型加香化合物的化合物。
可以将加香成分溶解在香料工业中当前使用的溶剂中。溶剂优选不是醇。此类溶剂的例子为邻苯二甲酸二乙酯、肉豆蔻酸异丙酯、(松香树脂,可从伊士曼(Eastman)获得)、苯甲酸苄酯、柠檬酸乙酯、柠檬烯或其他萜烯或异链烷烃。优选地,该溶剂是非常疏水的和高度空间受阻的,例如或苯甲酸苄酯。
水溶性聚合物基质内的微胶囊中的已包封油
根据本发明,油相分散在水溶性聚合物基质内,并具有至少一部分包封在至少一个微胶囊中。
根据本发明,“已包封油”是指被包封在微胶囊中的油。
相反,根据本发明,“未包封油”是指被简单地截留(或分散)在聚合物基质内但是没有被包封在微胶囊中的油。
本发明的微胶囊的聚合物壳的性质可以变化。作为非限制性例子,壳可由选自以下构成的群组中的材料制成:聚脲,聚氨酯,聚酰胺,聚丙烯酸酯,聚硅氧烷,聚碳酸酯,聚磺酰胺,脲甲醛,三聚氰胺甲醛树脂,与多异氰酸酯交联的三聚氰胺甲醛树脂或芳族多元醇,三聚氰胺脲树脂,三聚氰胺乙二醛树脂,明胶/阿拉伯胶壳壁以及它们的混合物。
根据一个实施方案,微胶囊的壳基于三聚氰胺甲醛树脂或与至少一种多异氰酸酯或芳族多元醇交联的三聚氰胺甲醛树脂。
壳也可以是复合的,即有机-无机,例如由至少两种交联的无机颗粒组成的复合壳,或者是由聚烷氧基硅烷大单体组合物的水解和缩合反应产生的壳。
根据一个实施方案,壳包含氨基塑料共聚物,例如三聚氰胺-甲醛或脲-甲醛或交联的三聚氰胺甲醛或三聚氰胺乙二醛。
根据一个特定的实施方案,核-壳微胶囊是可通过包括以下步骤的方法获得的交联的三聚氰胺甲醛微胶囊:
1)将香料油与至少一种具有至少两个异氰酸酯官能团的多异氰酸酯混合以形成油相;
2)将一种或多种氨基塑料树脂和可选的稳定剂分散或溶解于水中以形成水相;
3)将油相加入到水相中通过混合油相和水相形成水包油分散体,其中平均液滴尺寸为1~100微米;
4)进行固化步骤以形成所述微胶囊的壁;和
5)可选地,干燥最终分散体,以得到干燥的核-壳微胶囊;
该方法在WO2013/092375和WO2015/110568中更详细地描述,其内容通过引用并入于此。
根据另一个实施方案,壳是聚脲基的,由例如但不限于异氰酸酯基单体和含胺交联剂如碳酸胍和/或胍唑制得。优选的聚脲基微胶囊包含:聚脲壁,其是至少一种包含至少两个异氰酸酯官能团的多异氰酸酯与至少一种选自胺(例如水溶性胍盐和胍)的反应物之间的聚合反应产物;胶体稳定剂或乳化剂;和已包封的香料。但是,可以省略胺的使用。
根据另一个实施方案,壳是聚氨酯基的,由例如但不限于多异氰酸酯和多元醇、聚酰胺、聚酯等制成。
根据一个特定的实施方案,胶体稳定剂包含0.1%至0.4%的聚乙烯醇,0.6%至1%的乙烯基吡咯烷酮和季铵化乙烯基咪唑的阳离子共聚物的水溶液(所有百分比均由相对于胶体稳定剂的总重量来定义)。根据另一个实施方案,乳化剂是阴离子或两亲生物聚合物,优选选自聚丙烯酸酯(和特别是与丙烯酰胺的共聚物)、阿拉伯胶、大豆蛋白、明胶、酪蛋白酸钠以及它们的混合物。
根据一个特定的实施方案,多异氰酸酯是芳族多异氰酸酯,优选包含苯基、甲苯酰基、二甲苯基、萘基或二苯基部分。优选的芳族多异氰酸酯是缩二脲和聚异氰脲酸酯,更优选甲苯二异氰酸酯的聚异氰脲酸酯(可从Bayer以商品名RC购得)、甲苯二异氰酸酯的三羟甲基丙烷加合物(可从Bayer以商品名L75购得)、苯二甲基二异氰酸酯的三羟甲基丙烷加合物(可从Mitsui Chemicals以商品名D-110N购得)。
核-壳微胶囊的水性分散体/浆料的制备是本领域技术人员公知的。在一个形态中,所述微胶囊壁材料可以包含任何合适的树脂并且尤其包括三聚氰胺、乙二醛、聚脲、聚氨酯、聚酰胺、聚酯等。合适的树脂包括醛与胺的反应产物,合适的醛包括甲醛和乙二醛。合适的胺包括三聚氰胺、尿素、苯并胍胺、甘脲和它们的混合物。合适的三聚氰胺包括羟甲基三聚氰胺、甲基化羟甲基三聚氰胺、亚氨基三聚氰胺及它们的混合物。合适的脲包括二羟甲基脲、甲基化二羟甲基脲、脲-间苯二酚及它们的混合物。合适的制造材料可以从SolutiaInc.(St Louis,Missouri U.S.A.)、Cytec Industries(West Paterson,New JerseyU.S.A.)、Sigma-Aldrich(St.Louis,Missouri U.S.A.)中的一个或多个获得。
根据一个特定的实施方案,核-壳微胶囊是无甲醛的胶囊。制备氨基塑料无甲醛的微胶囊浆料的典型方法包括以下步骤:
1)制备包含如下成分的反应产物的低聚组合物,或者通过将如下成分一起反应而获得的低聚组合物:
a)三聚氰胺形式的或三聚氰胺与至少一种包含两个NH2官能团的C1-C4化合物的混合物形式的多胺组分;
b)乙二醛、C4-6 2,2-二烷氧基乙醛和可选的乙醛酸盐的混合物形式的醛组分,所述混合物的乙二醛/C4-6 2,2-二烷氧基乙醇的摩尔比为1/1至10/1;和
c)质子酸催化剂;
2)制备水包油分散体,其中液滴尺寸为1~600μm,并且包含:
i.油;
ii.水介质
iii.至少一种如步骤1中获得的低聚组合物;
iv.至少一种选自如下的交联剂:
A)C4-C12芳族或脂族二或三异氰酸酯及其缩二脲、缩三脲、三聚体、三羟甲基丙烷加合物及它们的混合物;和/或
B)下式的二-或三-环氧乙烷化合物
A-(环氧乙烷-2-基甲基)n
其中n代表2或3,且l代表可选包含2~6个氮和/或氧原子的C2-C6基团;
v.可选地,包含两个NH2官能团的C1-C4化合物;
3)加热所述分散体;
4)冷却所述分散体。
在WO2013/068255中更详细地描述了该方法,其内容通过引用包含于此。
根据另一个实施方案,微胶囊的壳是聚脲基或聚氨酯基的。例如在WO2007/004166、EP2300146、EP2579976中描述了制备聚脲基和聚氨酯基微胶囊浆料的方法的例子,其内容也通过引用包含于此。通常用于制备聚脲基或聚氨酯基微胶囊浆料的方法包括以下步骤:
a)将至少一种具有至少两个异氰酸酯基团的多异氰酸酯溶解在油中以形成油相;
b)制备乳化剂或胶体稳定剂的水溶液以形成水相;
c)将油相加入到水相中以形成水包油分散体,其中平均液滴尺寸为1~500μm,优选为5~50μm;
d)施加足以引发界面聚合的条件并形成浆料形式的微胶囊。
根据一个实施方案,在该方法的任何阶段均不添加胺。
根据本发明,应该理解,在包封后,无论微胶囊的性质如何,胶囊的内核仅由由香料油组成的核油制成。
本发明中定义的颗粒可含有微胶囊,其可通过其内部的核香料油和/或通过壁(不同的化学性质,或相同的化学性质但不同的工艺参数,如交联温度或持续时间)而变化。
根据本发明的一个特定的实施方案,微胶囊具有从由非离子多糖、阳离子聚合物及它们的混合物构成的群组中选出的外涂层。
这样的涂层将有助于在洗涤过程中驱动胶囊沉积和保留在基底上,使得在洗涤阶段/起泡时未被破坏的胶囊的大部分将转移到基底(皮肤、头发、织物)并且可用于当胶囊干燥后揉搓破裂时香料释放。
非离子多糖聚合物是本领域技术人员公知的。优选的非离子多糖从由刺槐豆胶、木葡聚糖、瓜尔胶、羟丙基瓜尔胶、羟丙基纤维素以及羟丙基甲基纤维素,以及它们的混合物构成的群组中选出。
阳离子聚合物也是本领域技术人员公知的。优选的阳离子聚合物的阳离子电荷密度为至少0.5meq/g,更优选至少约1.5meq/g,但也优选小于约7meq/g,更优选小于约6.2meq/g。阳离子聚合物的阳离子电荷密度可以通过凯氏定氮法(Kjeldahl method)测定,如美国药典在氮测定的化学测试中所述。优选的阳离子聚合物选自那些含有伯、仲、叔和/或季胺基团的单元,所述单元可以形成主聚合物链的一部分或可以由与其直接连接的侧取代基承载。阳离子聚合物的重均分子量(Mw)优选为10,000至3.5M道尔顿,更优选50,000至2M道尔顿。
根据一个特定的实施方案,将使用基于丙烯酰胺、甲基丙烯酰胺、N-乙烯基吡咯烷酮、季铵化的N,N-二甲基氨基甲基丙烯酸酯、二烯丙基二甲基氯化铵、季铵化的乙烯基咪唑(3-甲基-1-乙烯基-1H-咪唑-3-鎓氯化物)、乙烯基吡咯烷酮、丙烯酰胺丙基三甲基氯化铵、决明子羟丙基三甲基氯化铵、瓜尔胶羟丙基三甲基氯化铵或聚半乳甘露聚糖2-羟丙基三甲基氯化铵醚、淀粉羟丙基三甲基氯化铵和纤维素羟丙基三甲基氯化铵的阳离子聚合物。优选地,共聚物应从由聚季铵盐-5、聚季铵盐-6、聚季铵盐-7、聚季铵盐10、聚季铵盐-11、聚季铵盐-16、聚季铵盐-22、聚季铵盐-28、聚季铵盐-43、聚季铵盐-44、聚季铵盐-46、决明子羟丙基三甲基氯化铵、瓜尔胶羟丙基三甲基氯化铵或聚半乳甘露聚糖2-羟丙基三甲基氯化铵醚、淀粉羟丙基三甲基氯化铵和纤维素羟丙基三甲基氯化铵,以及它们的混合物构成的群组中选出。
作为市售产品的具体例子,可以列举SC60(丙烯酰胺丙基三甲基氯化铵和丙烯酰胺的阳离子共聚物,来源:BASF)或例如PQ 11N、FC 550或Style(聚季铵盐-11~68或乙烯基吡咯烷酮季铵化的共聚物来源:BASF),或(C13S或C17,来源Rhodia)。
基于粉末的总重量,本发明中定义的粒状粉末包含至多30重量%,优选至多25重量%,更优选至多20重量%的已包封油,以得到具有大量水溶性聚合物基质的坚固颗粒。
根据本发明,基于粉末的总重量,粒状粉末包含3至30重量%,优选5至25重量%,更优选5至20重量%的已包封油。
已经发现,基于粉末的总重量,具有至多30重量%,优选至多25重量%,更优选至多20重量%的相对低的负载量的已包封油的这样的粒状粉末最适合承受将它们与洗涤剂粉末配方混合的高剪切力工业制造过程,因为低负载量的已包封油/高负载量的水溶性聚合物基质有助于减少加工过程中的粒状物和微胶囊的破裂。
结果,由于工业加工过程中有限的破裂,所以仅需要低剂量的此类颗粒就可以以成本有效的方式使用颗粒。
因此,本发明提供了一种高效率的粉末洗涤剂,该粉末洗涤剂可以经受得住需要高剪切的制造过程。
根据一个特定的实施方案,包含在粒状粉末中的全部油相是被包封的。
水溶性聚合物基质内的可选的非包封油
根据一个实施方案,油相包含未被包封的至少一部分。
对于“未包封油”,应该理解,油相没有被包封在微胶囊中,而是被简单地截留在水溶性聚合物基质中。
根据该实施方案,基于粉末的总重量,粒状粉末占油相总量的至多45重量%,优选至多35重量%。
根据一个实施方案,基于粉末的总重量,粒状粉末占油相的3至45重量%,优选5至35重量%。
根据一个实施方案,基于粉末的总重量,粒状粉末包含0.1至40重量%,优选10至30重量%的未包封油。
根据一个特定的实施方案,该组合物包含
(i)10至99.9重量%,优选50至99.9重量%的洗涤剂活性材料,
(ii)0.1至90重量%,优选0.1至50重量%,更优选0.1至20重量%,甚至更优选0.1%至10重量%的粒状粉末,
百分比基于组合物的总重量计。
粒状粉末的制备方法
本发明所定义的粒状粉末的制备方法有多种选择。
实际上,只要能够获得低的芳香剂负载量,获得干燥颗粒的方式就没有限制。
在那些方法中,可以列举例如喷雾干燥,这是用于包封香料的众所周知的方法。
因此,根据一个实施方案,组合物包含喷雾干燥的颗粒。
因此,根据一个实施方案,组合物包含粒状粉末,所述粒状粉末包含通过包括以下步骤的方法获得的喷雾干燥的颗粒:
(i)制备包含水溶性聚合物的水相,
(ii)可选地,制备包含香料的油相;并将油相与水相混合以获得乳液;
(iii)将步骤(i)的水相或步骤(ii)的乳液与微胶囊浆料混合,该微胶囊浆料至少包括具有油基核和聚合物壳的微胶囊,该油基核包含香料;和
(iv)将步骤(iii)的浆料喷雾干燥以获得喷雾干燥的颗粒,
其特征在于,基于粉末的总重量,粒状粉末包含至多30重量%的已包封油。
可以在上述方法的步骤(iii)和/或步骤(iv)的过程中和/或步骤(iv)之后添加抗结块剂,如二氧化硅。
但是,也可以列举其他干燥方法,例如挤出、包覆、喷雾造粒、流化床,或者甚至在室温下干燥。
本发明的另一个目的是制备如上定义的粉末洗涤剂组合物的方法,其包括将如上定义的粒状粉末与洗涤剂活性材料混合的步骤。
在将粒状粉末与洗涤剂活性材料混合之前,所述洗涤剂活性材料优选以固体形式提供,并且可以通过喷雾干燥或通过将洗涤剂活性材料干混(最初为固体和/或液体和/或糊状形式)以获得固体混合物。
现在将通过实施例进一步描述本发明。应当理解,所要求保护的本发明无意以任何方式被这些实施例所限制。
实施例
实施例1
用于本发明组合物中的粒状粉末的制备
1.含有香料油的三聚氰胺-甲醛微胶囊(微胶囊1)的合成
表1:核-壳微胶囊1的浆料组成
成分 | [%] |
油相 | 30.9 |
香料油<sup>a)</sup> | 30.28 |
苯二甲基二异氰酸酯的三羟甲基丙烷加合物<sup>1)</sup> | 0.62 |
水相 | 69.1 |
丙烯酰胺和丙烯酸共聚物<sup>2)</sup> | 4.7 |
三聚氰胺-甲醛树脂<sup>3)</sup> | 2.45<sup>3)</sup> |
水 | 50.55 |
氢氧化钠 | 0.5 |
乙酸 | 0.2 |
丙烯酰胺基丙基三甲基氯化铵/丙烯酰胺共聚物<sup>4)</sup> | 10.7 |
总计 | 100 |
纯三聚氰胺/甲醛树脂与香料油的比<sup>5)</sup> | 0.057 |
1)见表1a)(香料A)
3)来自Ciba的Alcapsol,20%水溶液
4)来自Cytec的Cymel 385和Cymel 9370的90/10共混物,二者都为70%水溶液
5)来自Ciba的Salcare SC60,3%水溶液
6)=纯三聚氰胺/甲醛树脂(2)中用量的70%)/香料油的量
表1a):香料A的组成
1)来源:瑞士日内瓦的Firmenich SA
2)4-甲基-3-癸烯-5-醇;来源和商标:瑞士的Givaudan SA
3)3-(4-叔丁基苯基)-2-甲基丙醛;来源和商标:瑞士的Givaudan SA
通过将多异氰酸酯(苯二甲基二异氰酸酯的三羟甲基丙烷加合物,D-110N,来源:Mitsui Chemicals)与由香料油组成的核油(参见上表1a)混合来制备油相。油相由2%的D-110N和98%的核油组成。包封并使用Takenate D-110N交联三聚氰胺-甲醛壁后,核油中未反应的多异氰酸酯的残留量非常低,因此胶囊的内部核仅由核油(其由香料油组成)制成。
为了制成胶囊浆料,将丙烯酰胺和丙烯酸共聚物以及两种三聚氰胺-甲醛树脂的共混物溶解在水中以形成水相。然后将香料预混合油加入到该溶液中,并用乙酸将pH调节至5。将温度升高到90℃保持2小时以使胶囊固化。此时,胶囊形成、交联且稳定。然后在80℃下将3%的Salcare SC60(丙烯酰胺基丙基三甲基氯化铵/丙烯酰胺共聚物)在水中的溶液加入到混合物中,并使其在80℃下反应2小时。然后像往常对氨基塑料胶囊一样添加乙烯脲溶液(50重量%的水溶液)作为清除残留游离甲醛的试剂。相对于浆料的重量,最终浆料包含约3%w/w的乙烯脲,并将混合物冷却至室温。用氢氧化钠将最终pH调节至7。
2.在根据本发明的组合物中使用的粒状粉末的制备
制备具有以下成分的乳液A~E:
表2:乳液A~D的组成和喷雾干燥后的粒状粉末A~D的组成
成分 | 乳液A | 乳液B | 乳液C | 对比乳液D |
改性淀粉<sup>1)</sup> | 3.5% | 3.0% | 2.5% | 2.0% |
麦芽糊精<sup>2)</sup> | 33.5% | 28.4% | 23.9% | 19.1% |
实施例1.1中获得的微胶囊浆料 | 14.0% | 28.9% | 42.1% | 56.2% |
水 | 49.0% | 39.7% | 31.5% | 22.7% |
微粒A | 微粒B | 微粒C | 对比微粒D | |
改性淀粉<sup>1)</sup> | 7.8% | 6.7% | 5.6% | 4.9% |
麦芽糊精<sup>2)</sup> | 77.9% | 66.3% | 56.0% | 44.7% |
实施例1.1中获得的微胶囊浆料 | 12.2% | 24.9% | 36.3% | 48.4% |
二氧化硅 | 2.1 | 2.1% | 2.1% | 2.0% |
喷雾干燥后粉末中的芳香剂负载量 | 10.1% | 20.7% | 30.0% | 40.2% |
1)CapsulTM,Ingredion
2)麦芽糊精10DE,来源:Roquette
3)麦芽糖,Lehmann&Voss
4)二氧化硅,Evonik
表3:乳液E的组成和喷雾干燥后的粒状粉末E的组成
成分 | 乳液E |
改性淀粉<sup>1)</sup> | 12.5% |
麦芽糊精<sup>2)</sup> | 0% |
麦芽糖<sup>3)</sup> | 7.9% |
柠檬酸 | 1% |
柠檬酸三钾 | 1.9% |
实施例1.1中获得的微胶囊浆料 | 8.9% |
二氧化硅<sup>4)</sup> | 0% |
游离香料C<sup>5)</sup> | 11% |
水 | 56.9% |
微粒E | |
改性淀粉<sup>1)</sup> | 31.6% |
麦芽糊精<sup>2)</sup> | 0% |
麦芽糖 | 20.9% |
柠檬酸 | 2.6% |
柠檬酸三钾 | 4.9% |
已包封香料C | 28.1% |
1.1中获得的微胶囊浆料 | 9.8% |
二氧化硅 | 2.0% |
喷雾干燥后粉末中的芳香剂负载量 | 35.8% |
1)CapsulTM,Ingredion
2)麦芽糊精10DE,来源:Roquette
3)麦芽糖,Lehmann&Voss
4)二氧化硅,Evonik
5)见表4
表4:香料C的组成
1)瑞士的Firmenich SA
2)3-(4-叔丁基苯基)-2-甲基丙醛,瑞士韦尔涅的Givaudan SA
3)1-(八氢-2,3,8,8-四甲基-2-萘基)-1-乙酮,美国的International Flavors&Fragrances
4)瑞士的Firmenich SA
5)二氢茉莉酮酸甲酯,瑞士的Firmenich SA
6)瑞士的Firmenich SA
将聚合物基质的成分(麦芽糊精和capsulTM,或capsulTM、柠檬酸和柠檬酸三钾)添加到45~50℃的水中直至完全溶解。
对于乳液E,将游离香料C加入到水相中。
将微胶囊浆料添加到所得混合物中。然后,将所得混合物在25℃(室温)下轻轻混合。
通过使用Sodeva喷雾干燥器(来源:法国)将表2或表3中公开的乳液喷雾干燥来制备粒状粉末,其进气温度设定为215℃,通过量设定为每小时500ml。出风温度为105℃。雾化之前的乳液是在环境温度下。
使用适当的校准,通过GC-MS测量喷雾干燥的造粒粉末中的芳香油含量。
实施例3
本发明中定义的粒状粉末在制备粉末洗涤剂中的性能
1.加工过程中粒状粉末A~D和微胶囊浆料1的破裂
使用具有表5中定义的组成的粉末洗涤剂进行测试。
表5:粉末洗涤剂组合物
在加工步骤之后,使用GC-MS测量产品的易碎性,以量化混合过程中有多少香料从粒状粉末胶囊中泄漏出来。
表6:包含粒状粉末的洗涤剂粉末组合物的颗粒破裂和稳定性测量。
*微胶囊浆料1(0.15%的香料油→与微粒C相同)
产品制造过程中的破裂值确定如下:
将粒状粉末香料胶囊或微胶囊浆料(对比样品F)添加到表5中详细说明的洗涤剂粉末中。使用Turbula Shaker混合器将样品混合1至15分钟。然后将已混合粉末的样品用于随后的GC-MS(日本岛津)分析。
如表6所示,与纯净微胶囊浆料(对比样品F)相比,所有微粒在制造过程中的破裂(称为混合后香料泄漏%)均显著降低。此外,粒状粉末中芳香剂负载量越低,制造过程中的破裂值就越小。
实际上,以上结果表明,当芳香剂负载量大于30%(通常芳香剂负载量为40%-对比粒状粉末D)时,制造过程中的破裂值高,并且会导致最终的洗涤剂粉末组合物中的微胶囊稳定性和性能变差。
还已经评估了与微胶囊浆料相比,粒状粉末A在粉末洗涤剂中的嗅觉性能。感观小组进行了测试,要求小组成员在揉搓之前和之后使用在1(不可感知的香料)和7(非常强的香料强度)之间的等级对干毛巾上的香料强度进行评分。
从图1可以得出结论,粒状粉末显示出与微胶囊浆料相比,在揉搓之后更高的效果。
Claims (15)
1.一种粉末洗涤剂组合物,其包含:
-洗涤剂活性材料,其至少包含表面活性剂体系,
-粒状粉末,其包含由以下材料制成的颗粒:
a)水溶性聚合物基质,
b)油相,其包含分散在所述聚合物基质中的香料,所述油至少部分包封在微胶囊中,
其中
-基于粉末的总重量,粒状粉末包含至多30重量%的已包封油。
2.根据权利要求1所述的粉末洗涤剂组合物,其中该表面活性剂体系包含至少一种从由阴离子表面活性剂,非离子表面活性剂,阳离子表面活性剂,两性离子表面活性剂以及它们的混合物构成的群组中选出的表面活性剂。
3.根据权利要求1或2所述的粉末洗涤剂组合物,其中该表面活性剂从由如下构成的群组中选出:直链烯烃苯磺酸盐(LABS),月桂醇聚醚硫酸酯钠,月桂基醚硫酸钠(SLES),月桂基硫酸钠(SLS),α-烯烃磺酸盐(AOS),甲酯磺酸盐(MES),烷基聚葡糖苷(APG),月桂醇乙氧基化物(LAE),伯醇磺酸盐(PAS),肥皂以及它们的混合物。
4.根据前述权利要求中任一项所述的粉末洗涤剂组合物,其中该洗涤剂活性材料还包含至少一种从由如下构成的群组中选出的组分:漂白剂,缓冲剂;助洗剂;污物释放或污物悬浮聚合物;粒状酶颗粒,缓蚀剂,消泡剂,抑泡剂;染料,填充剂,以及它们的混合物。
5.根据前述权利要求中任一项所述的粉末状组合物,其中该洗涤剂活性材料包含:
a)5至50重量%,优选5至30重量%的表面活性剂,优选从由阴离子表面活性剂和非离子表面活性剂构成的群组中选出;
b)10至50重量%的填料,优选从由硅酸钠,硫酸钠以及它们的混合物构成的群组中选出;
c)10至30重量%的助洗剂,优选从由沸石,碳酸钠以及它们的混合物构成的群组中选出;
d)0至2重量%的酶,优选从由纤维素酶,脂肪酶,蛋白酶,甘露聚糖酶,果胶酶以及它们的混合物构成的群组中选出;
e)0至2重量%的游离香料;
f)0至20重量%的过氧化氢源,优选过碳酸钠或过硼酸钠,更优选过碳酸钠,和
g)0至5重量%的漂白活化剂,优选TAED,
百分比基于组合物的总重量计。
6.根据前述权利要求中任一项所述的粉末洗涤剂组合物,其中它包含:
a)10至99.9重量%,优选50至99.9重量%的至少一种洗涤剂活性材料,和
b)0.1至90重量%,优选0.1至50重量%,更优选0.2至20重量%,甚至更优选0.2%至10重量%的粒状粉末,
百分比基于组合物的总重量计。
7.根据前述权利要求中任一项所述的粉末洗涤剂组合物,其中基于粉末的总重量,粒状粉末包含至多25重量%的已包封油。
8.根据前述权利要求中任一项所述的粉末洗涤剂组合物,其中基于粉末的总重量,粒状粉末包含至多20重量%的已包封油。
9.根据前述权利要求中任一项所述的粉末洗涤剂组合物,其中全部油相被包封。
10.根据权利要求1至8中任一项所述的粉末洗涤剂组合物,其中该油相包含未被包封的至少一部分,并且其中基于粉末的总重量,该粒状粉末占该油相总量的至多45重量%。
11.根据权利要求10所述的粉末洗涤剂组合物,其中该油相包含未被包封的至少一部分,并且其中基于粉末的总重量,该粒状粉末占该油相总量的至多35重量%。
12.根据前述权利要求中任一项所述的粉末洗涤剂组合物,其中被包封的油的部分被包封在至少一个具有核-壳结构的微胶囊中,其中该核包含已包封油并且其中该聚合物壳由从由以下构成的群组中选出的材料制成:聚脲,聚氨酯,聚酰胺,聚丙烯酸酯,聚硅氧烷,聚碳酸酯,聚磺酰胺,脲甲醛,三聚氰胺甲醛树脂,与多异氰酸酯或芳族多元醇交联的三聚氰胺甲醛树脂,三聚氰胺脲树脂,三聚氰胺乙二醛树脂,明胶/阿拉伯胶壳壁以及它们的混合物。
13.根据权利要求12所述的粉末洗涤剂组合物,其中该微胶囊的壳基于三聚氰胺甲醛树脂或与至少一种多异氰酸酯或芳族多元醇交联的三聚氰胺甲醛树脂。
14.根据前述权利要求中任一项所述的粉末洗涤剂组合物,其中该微胶囊包含从由非离子多糖和/或阳离子聚合物构成的群组中选出的外涂层。
15.根据前述权利要求中任一项所述的粉末洗涤剂组合物,其中该水溶性聚合物从由以下构成的群组中选出:淀粉,麦芽糊精,多糖,碳水化合物,壳聚糖,阿拉伯胶,聚乙二醇,聚乙烯吡咯烷酮,聚乙烯醇,丙烯酰胺,丙烯酸酯,聚丙烯酸和相关物,马来酸酐共聚物,胺官能聚合物,乙烯基醚,苯乙烯,聚苯乙烯磺酸盐,乙烯基酸,乙二醇-丙二醇嵌段共聚物,以及它们的混合物。
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GB202011735D0 (en) | 2020-07-29 | 2020-09-09 | Givaudan Sa | Improvements in or relating to organic conpounds |
GB202018435D0 (en) | 2020-11-24 | 2021-01-06 | Givaudan Sa | Improvements in or relating to organic compounds |
EP4123005B1 (en) * | 2021-07-19 | 2024-03-06 | The Procter & Gamble Company | Cleaning composition comprising bacterial spores |
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