CN115161127B - 一种含有纤维素酶的液体洗衣凝珠组合物及其制备方法 - Google Patents
一种含有纤维素酶的液体洗衣凝珠组合物及其制备方法 Download PDFInfo
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- CN115161127B CN115161127B CN202210921973.3A CN202210921973A CN115161127B CN 115161127 B CN115161127 B CN 115161127B CN 202210921973 A CN202210921973 A CN 202210921973A CN 115161127 B CN115161127 B CN 115161127B
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Classifications
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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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/83—Mixtures of non-ionic with anionic compounds
-
- 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
-
- 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
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2041—Dihydric alcohols
- C11D3/2044—Dihydric alcohols linear
-
- 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
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- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2065—Polyhydric alcohols
-
- 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
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2068—Ethers
-
- 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
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy carboxylic acids-salts thereof
-
- 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
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/30—Amines; Substituted amines ; Quaternized amines
-
- 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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- C11D3/3707—Polyethers, e.g. polyalkyleneoxides
-
- 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
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38645—Preparations containing enzymes, e.g. protease or amylase containing cellulase
-
- 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
- C11D3/43—Solvents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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Abstract
本发明公开了一种含有纤维素酶的液体洗衣凝珠组合物及其制备方法,涉及洗涤剂技术领域。按组合物总量的重量百分比计,包含:25%~45%的有机溶剂,所述有机溶剂包含主溶剂和助溶剂,主溶剂与助溶剂的重量比为(0.5~1.75):1;20%~60%的表面活性剂,表面活性剂中阴离子表面活性剂与非离子表面活性剂的重量比为(1.8~2.5):1,阴离子表面活性剂中磺酸盐型表面活性剂的重量占比为35%~50%;0.1%~2%的纤维素酶;余量的水。本发明的液体洗衣凝珠组合物,通过主溶剂和助溶剂复配,阴离子表面活性剂与非离子表面活性剂复配,使得纤维素酶在高含量磺酸盐型表面活性剂的洗涤剂组合物中,依然具有高的酶活稳定性,使液体洗衣凝珠组合物具有优异的存储稳定性。
Description
技术领域
本发明涉及洗涤剂技术领域,特别是涉及一种含有纤维素酶的液体洗衣凝珠组合物及其制备方法。
背景技术
近年来,洗衣凝珠产品广泛应用在家用洗涤剂领域。洗衣凝珠将液体洗涤剂包装在水溶性膜中,从而减少使用者手与洗涤剂之间的接触,另外,通过单位剂量的产品形式,为消费者提供了免倾倒和定量的便利。因此,受到了消费者的喜爱和洗涤业界的重视。
由于人们对绿色洗涤剂产品需求的提高,而酶制剂正是绿色化学工艺中的理想催化剂,这就为含酶洗涤剂的发展提供了契机。对于洗涤剂用酶,可以追溯到20世纪60年代,丹麦诺沃公司推出了一种来自地衣芽孢杆菌的细菌内蛋白酶,作为洗涤配方的成分,使洗涤用品的去污效果得到大大提高。初期的洗涤产品大部分都是粉末,随着包裹造粒等技术的发展,使酶与洗涤配方体系中的组分相隔绝开,减少了酶与其它组分的接触,从而使粉状的洗涤产品的酶稳定性问题得到了解决。但是随着粉状洗涤剂向液体洗涤剂的转变,酶的稳定性问题再一次成为了人们关注的焦点,成功地使用酶助剂已经成为生产具有成本效益、对环境无害的驱动力,酶制剂的加入对于各类型洗涤产品的创新发展均具有很大的助推力。但是酶制剂因为其生物属性使其在洗涤剂工业应用中特别容易受到外界影响而失去活性。所以,研究酶在洗涤剂溶液中(主要是表面活性剂溶液)的稳定性,探讨洗涤剂配方组分的表面活性剂等组分对酶的活性的影响,是一个非常重要的课题。
纤维素酶是将纤维素水解成纤维二糖和葡萄糖的一组复杂酶系的总称,又可称纤维素酶系。纤维素酶能通过3种酶的协同作用,将纤维素有效水解成葡萄糖,这3种酶分别是内切葡聚糖酶、外切葡聚糖酶和β-葡萄糖苷酶。纤维素酶常应用于纺织、动物饲料、污水处理、酿造等行业。纤维素酶去污机理不同于蛋白酶和淀粉酶的去污机理,纤维素酶用于洗涤时,作用在棉纤维上,能将污垢剥落下来,同时纤维素酶能扩大织物纤维中的空穴和毛细管,赋予织物一系列有价值的服用性能,如轻薄感、手感柔软、吸水性好、抗起球等。随着人们对天然制品的重新重视,纯棉制品越来越受到消费者的欢迎,而且人们也越来越重视环境保护,因此,将纤维素酶应用到棉织物的洗涤中得到了越来越多的关注。研究表明阴离子表面活性剂使纤维素酶中色氨酸和酪氨酸所处的微环境发生了变化,这些变化导致了纤维素酶结构的变化,从而对纤维素酶的活性产生了影响。其中,阴离子表面活性剂中带有电离度较大的磺酸基团,使得阴离子表面活性剂吸附到了纤维素酶表面,进而改变了纤维素酶的二级结构和侧链的微环境,从而使得纤维素酶失活,限制了纤维素酶在高磺酸洗涤剂中的应用。而在单剂量洗涤中,洗涤剂组合物为浓缩配方,磺酸盐型表面活性剂的含量高达10%以上,纤维素酶很难存活,因而目前市面上的单剂量洗涤剂产品的酶制剂主要采用单一的蛋白酶。
CN106906059B公开了一种低泡易漂洗洗衣凝珠及其制备方法与应用,虽然该专利申请声称加入了蛋白酶、淀粉酶、脂肪酶或纤维素酶等质量比的混合物,但并没有考察纤维素酶的酶活稳定性。CN108893212B公开了一种洗衣凝珠及其制备方法,复合酶由蛋白酶的包合物、脂肪酶、淀粉酶和纤维素酶按质量比9:6:3:1组成,样品在37℃放置4周后仍然就有良好的去污效果,但是实施例中非离子表活含量为56%,月桂酸钾10%,这个配方构成基本是非离子配方体系,与现有凝珠产品的阴离子体系差距太大。
因此,目前存在着纤维素酶在含磺酸盐型表面活性剂洗衣凝珠中的需求,而且需要达到在37℃、放置8周后仍有高的纤维素酶活保持率,从而保持产品在货架期内的酶活力值。
发明内容
为了克服上述现有技术的缺陷,实现纤维素酶在含磺酸盐型表面活性剂洗衣凝珠液体洗涤剂中货架期内的酶活力值,本发明提供一种含有纤维素酶的液体洗衣凝珠组合物,其特征在于,按组合物总量的重量百分比计,包含:
25%~45%的有机溶剂;所述有机溶剂包含主溶剂和助溶剂,主溶剂为聚乙二醇和/或二元醇,助溶剂为具有3~6个碳原子的多元醇,其中主溶剂与助溶剂的重量比为(0.5~1.75):1;
20%~60%的表面活性剂;所述表面活性剂中阴离子表面活性剂与非离子表面活性剂的重量比为(1.8~2.5):1,阴离子表面活性剂中磺酸盐型表面活性剂的重量占比为35%~50%;
0.1%~2%的纤维素酶;
余量的水。
优选的,所述聚乙二醇选自相对分子量200~600之间的聚乙二醇(PEG)。
优选的,所述二元醇选自乙二醇、丙二醇、丁二醇、戊二醇、二丙二醇、二甘醇、三甘醇或者其混合物;
优选的,所述助溶剂选自甘油、木糖醇、山梨醇、甘露醇、赤藓糖醇、半乳糖醇或其混合物。
优选的,所述的阴离子表面活性剂还包括羧酸盐型表面活性剂、硫酸盐型表面活性剂的一种或多种。
优选的,所述的非离子表面活性剂选自脂肪醇烷氧基化物、烷基多糖苷、脂肪酸烷氧基化物、脂肪酸乙氧基化物、脂肪酸烷基醇酰胺、乙氧基化失水山梨酸醇酯的一种或多种的混合物。
优选的,所述纤维素酶选自内切葡萄糖酶、外切葡萄糖酶、β-葡萄糖苷酶及其混合物。
进一步的,还包括0.02%~20%的其它酶制剂和添加剂。
优选的,所述其它酶制剂选自蛋白酶、淀粉酶、脂肪酶、果胶酶、甘露聚糖酶中的一种或多种。
优选的,所述添加剂选自碱剂、粘度调节剂、pH稳定剂、防腐剂、抗再沉积剂、功能性聚合物、螯合剂、荧光增白剂、香精或色素中的一种或多种。
上述含有纤维素酶的液体洗衣凝珠组合物的制备方法,包括如下步骤:
1)将水、主溶剂中的二元醇、助溶剂和碱剂混合;
2)加入阴离子表面活性剂,混合至溶液澄清后,采用冷冻水降温;
3)待温度降至40-50℃,加入非离子表面活性剂,混合至溶解完全;
4)加入主溶剂中的聚乙二醇混合均匀;
5)调节pH;
6)加入所述纤维素酶,搅拌均匀;
7)加入其它酶制剂、添加剂,搅拌至完全溶解;
8)加入余量去离子水,搅拌均匀。
采用上述技术方案,本发明具有如下优点和有益技术效果:
本发明制备的含有纤维素酶的液体洗衣凝珠组合物,无需使用酶制剂稳定剂,通过主溶剂和助溶剂复配,阴离子表面活性剂与非离子表面活性剂复配,使得纤维素酶在高含量磺酸盐型表面活性剂的洗涤剂组合物中,依然具有高的酶活稳定性,且纤维素酶在老化后仍可保持高的酶活稳定性,使液体洗衣凝珠组合物具有优异的存储稳定性。
具体实施方式
下面将结合本发明实施例,对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
应当理解,当在本说明书和所附权利要求书中使用时,术语“包括”和“包含”指示所描述特征、整体、步骤、操作、元素和/或组件的存在,但并不排除一个或多个其它特征、整体、步骤、操作、元素、组件和/或其集合的存在或添加。
对于本领域的技术人员来说,通过阅读本说明书所公开的内容,本发明的技术特征、有益效果将变得显而易见。
液体洗衣凝珠组合物可为含水的或非水的,并且可为各向异性的、各向同性的或它们的组合。本文所述“水”是指作为单独组分添加到洗涤剂组合物中的水,不包含原料中引入的水。所述“溶剂”不包含作为单独组分添加到洗涤剂组合物中的水。
除非另外指明,本发明所用的百分比、比率和比例均按所述洗涤剂组合物的重量百分比计。除非另外明确指出,所有平均值均按所述组合物或其组分的重量。
溶剂体系
洗衣凝珠中的溶剂不会捕获其它配方组分溶解所需的所有水,这将有助于保持配方、膜和大气之间的水平衡。这些溶剂具有与水形成氢键的亲水基团。常见的亲水基团包括羟基、羧基、酯和胺官能团。
有机溶剂包括但不限于二元醇、多元醇和相对分子量200~600之间的聚乙二醇(PEG)聚合物。二元醇和多元醇可以是具有两个或多个羟基的直链或支链醇。因此,也可以使用两个或多个羟基与脂肪族链中不同碳原子连接的醇类溶剂。
本发明的液体洗涤剂组合物可以包含5%至75%的一种或多种溶剂,优选地7%至约50%,更优选地约25%至约45%。
液体洗衣凝珠组合物
所述洗衣凝珠包含水溶性薄膜,所述水溶性薄膜将液体组合物包封于至少一个隔室中。多隔室洗衣凝珠可分离化学不相容的成分或希望一部分成分更早或更迟释放。
液体洗衣凝珠组合物是指液体状态的洗涤剂组合物。该组合物可以由水溶膜包封制成洗衣凝珠制品,液体洗衣凝珠组合物按照一定比例稀释后,或直接与需要接触的底物(即织物制品、硬表面等)相接触,从而将底物表面的污渍去除,达到清洁底物表面的目的。所述的液体洗衣凝珠组合物一般还包含表面活性剂体系和其它常见的洗涤助剂如粘度调节剂、酶制剂、香料等等。
在一些实施方式中,该液体洗衣凝珠组合物按重量百分比计,包含15~20%的主溶剂丙二醇和PEG-400、小于8%的甘油和小于8%的山梨醇组成的助溶剂。进一步地,该液体洗涤剂组合物还包含如下成分:
20%~60%表面活性剂,所述表面活性剂选自阴离子表面活性剂、非离子表面活性剂和两性离子表面活性剂中的至少一种;5%~20%的添加剂,所述添加剂选自酶制剂、碱剂、粘度调节剂、pH稳定剂、防腐剂、抗再沉积剂、功能性聚合物、螯合剂、荧光增白剂和香精中的一种或多种;以及余量的水。
表面活性剂
本发明的洗涤剂组合物中使用的表面活性剂包括阴离子表面活性剂、非离子表面活性剂、两性表面活性剂或其混合物。
阴离子表面活性剂
阴离子表面活性剂的混合物总重量为液体洗涤剂组合物总量的0.01%~30%。
阴离子表面活性剂选自磺酸盐型表面活性剂、羧酸盐型表面活性剂、硫酸盐型表面活性剂的一种或多种的混合物;优选自烷基苯磺酸盐、C8至C18的烷基硫酸盐、C8至C18的乙氧基化脂肪醇硫酸盐、α-烯烃磺酸盐、脂肪酸烷基酯磺酸盐、乙氧基化脂肪醇醚羧酸盐的一种或几种的混合物。
在一些实施方案中,阴离子表面活性剂的混合物优选含有烷基苯磺酸盐及其衍生物。所述烷基苯磺酸盐满足如下通式:
其中,R1是碳数为6至24的烷基,M+为阳离子。R1可以是直链的烷基,也可以是支链的烷基;可以是饱和的烷基,也可以是含有一个或多个不饱和双键的烷基。更优选R1是碳数为8至18的直链烷基。
在一些实施例中,阴离子表面活性剂的混合物含有乙氧基化的脂肪醇硫酸盐。乙氧基化脂肪醇硫酸盐是乙氧基化物脂肪醇的衍生物,具有如下通式:
其中,R2是碳数为6至24的烷基;其中M+为阳离子。R2为直链或支链的饱和或含一个或多个不饱和双键的烷基,优选碳数为8至18的直链烷基。x代表平均乙氧基化程度,为1至30,优选1至10,更优选1至3。
在一些实施例中,含有α-烯烃磺酸盐,具有如下通式:
其中,y为0至2,R3是碳数为6至24的烷基,优选碳数为8至18的烷基。
所述阴离子表面活性剂还可以选自脂肪酸烷基酯硫酸盐,优选为脂肪酸甲酯硫酸盐(MES),脂肪酸碳数优选8至18。还可以包含磺基琥珀酸盐,优选为脂肪醇聚氧乙烯醚基琥珀酸单酯二钠盐,脂肪醇碳数优选8至18,平均乙氧基化程度优选2.0。
所述阴离子表面活性剂还可以包含烷基二磺酸钠或其衍生物的一种及多种混合物,优选烷基二苯醚二磺酸钠,合适例子是十二烷基二苯醚二磺酸钠盐。还可以含有脂肪酸烷基酯硫酸盐,优选为脂肪酸甲酯硫酸盐(MES),脂肪酸碳数优选8至18个。还可以包含磺基琥珀酸盐,优选为脂肪醇聚氧乙烯醚磺基琥珀酸单酯二钠盐,脂肪醇碳数优选8至18个,平均乙氧基化程度优选为2.0。
在一些实施方案中,阴离子表面活性剂的混合物含有脂肪酸盐。脂肪酸盐为脂肪酸经碱性造化后形成的。可以选用的碱剂为单乙醇胺或三乙醇胺。本发明涉及的液体洗涤剂组合物中,所述脂肪酸盐选自碳原子为10个至20个的脂肪酸的金属盐,优选碳原子为10个至16个的直链烷基脂肪酸。
非离子表面活性剂
非离子表面活性剂的混合物总重量为液体洗涤剂组合物总重量的0.01~30%。非离子表面活性剂选自脂肪醇烷氧基化物、烷基多糖苷、脂肪酸烷氧基化物、脂肪酸乙氧基化物、脂肪酸烷基醇酰胺、乙氧基化失水山梨酸醇酯的一种或多种的混合物。在一些实施方案中,非离子表面活性剂混合物优选含有脂肪醇烷氧基化物,所述脂肪醇烷氧基化物具有以下通式:
其中,n为6至24;x为0.5至30;y为0至10。
所述脂肪醇烷氧基化物是脂肪醇和环氧烷烃在碱性催化剂作用下开环聚合的产物,因此均为混合物。脂肪醇包括直链醇或支链的异构醇。烷氧基团包括乙氧基团和丙氧基团。脂肪醇优选碳数为8至18的脂肪醇,优选的醇包括但不限于己醇、辛醇、癸醇、2-乙基已醇、3-丙基庚醇、月桂醇、异三癸醇、十三烷醇、十四烷醇、十六烷醇、棕榈油醇、硬脂醇、异硬脂醇、油醇、亚油醇、亚麻醇的一种及其混合物。平均乙氧基化程度x优选2至12。优选例子是SHELL公司NEODOL系列直链脂肪醇乙氧基化物产品,DOW公司ECOSURFEH系列乙氧基化和丙氧化2-乙基已醇产品,BASF公司LutensolXL系列乙氧基化和丙氧化3-丙基庚醇产品和BASF公司LutensolXP系列乙氧基化3-丙基庚醇产品。
非离子表面活性剂混合物可以含有脂肪酸烷氧基化物,优选自乙氧基化C8至C18脂肪酸酯,平均乙氧基化程度为2至10。可以含有乙氧基化失水山梨酸醇烷基酯,烷基碳数为6至18,平均乙氧化程度为4至20;合适的例子是Corda公司Tween系列产品。
非离子表面活性剂混合物可以含有脂肪酸烷基醇酰胺,脂肪酸的碳数为6至24,可以是直链的脂肪酸,也可以是支链的脂肪酸,可以是饱和的脂肪酸,也可以是不饱和的脂肪酸;烷基醇数目为0至2。优选脂肪酸碳数为8至18的一乙醇酰胺,二乙醇酰胺,异丙醇酰胺,合适的例子是椰子油酸二乙醇酰胺。
其它合适的表面活性剂包括两性表面活性剂。用于本文的合适的两性表面活性剂包括酰胺基丙基甜菜碱和脂肪族或杂环仲胺和叔胺的衍生物,其中脂肪族部分可以为直链或支链,并且其中脂肪族取代基之一含有8到24个碳原子和至少一个含有阴离子水溶性基团的脂肪族取代基。两性表面活性剂在存在时通常包含本发明的液体洗涤剂组合物的0.01%至20%或0.5%至10%。
纤维素酶
可包含细菌或真菌来源的纤维素酶。包括经化学修饰或蛋白质工程化的突变体。合适的纤维素酶包括来自芽孢杆菌属、假单胞菌属、腐质霉属、镰孢菌属、草根霉属、支顶孢属的纤维素酶,例如,在US4,435,307、US 5,648,263、US 5,691,178、US 5,776,757和5,691,178中所公开的由特异腐质霉(Humicola insolens)、嗜热毁丝菌(Myceliophthorathermophila)和尖孢镰孢菌(Fusarium oxysporum)制得的真菌纤维素酶。可商购获得的纤维素酶包括和Carezyme(Novozymes A/S)、和Puradax和
存储稳定性
高温稳定性:组合物瓶装密封后,置于45℃±1℃环境,恒温放置4周后,恢复至室温25℃±5℃,组合物无分层或沉淀析出,为高温稳定性合格。
低温稳定性:组合物瓶装密封后,置于0℃±2℃环境,恒温放置4周后,取出立即观察。组合物无分层或沉淀析出,为低温稳定性合格。
冻融循环稳定性:置于-15℃~-20℃环境,恒温放置24小时后取出,再置于室温25℃±5℃环境24小时为循环一次,连续循环四次,每次均观察组合物状态。组合物无分层或沉淀析出,为冻融循环稳定性合格。
常温稳定性:组合物瓶装密封后,置于室温环境(20℃~30℃),放置4周后,组合物无分层或沉淀析出,为常温稳定性合格。
纤维素酶活保持率
纤维素酶(例1,4-endoglucanase,EC.3.2.1.4)水解纤维素成还原性的碳水化合物(还原糖)。底物羧甲基纤维素(CMC)是纤维素的替代形式。此反应被含有PAHBAH和铋的碱性试剂终止,此试剂能与还原糖反应生成的复合物可在405nm有吸收,产生的颜色与纤维素酶的活性成正比。
为了保证洗衣凝珠产品在货架期内的纤维素酶活,将液体洗衣凝珠组合物瓶装密封后,分别置于高温(37℃±1℃)和低温(-15℃±1℃)环境,放置4周、8周后,恢复至室温测试纤维素酶活。
酶活保持率=(高温样品酶活-低温样品酶活)/低温样品酶活
其它酶
本发明涉及的液体洗衣凝珠组合物可以包含一种或更多种酶制剂,以提供清洁性能,织物护理和/或其它有益效果。酶制剂选自以下酶组成的组:
蛋白酶、α-淀粉酶,磷脂酶,酯酶,脂肪酶,过氧化物酶/氧化酶,果胶酶,裂解酶,甘露聚糖酶,角质酶,还原酶,木聚糖酶,支链淀粉酶,鞣酸酶,戊聚糖酶,麦芽聚糖,阿拉伯糖酶,β-葡聚糖酶。常用的酶制剂是蛋白酶、淀粉酶、脂肪酶、果胶酶和甘露聚糖酶。酶制剂含量为洗涤剂组合物的0.001%至5%,进一步地为0.01%至2%。
本发明的洗涤剂组合物可以包含占组合物重量0.001%至10%的酶稳定体系。酶稳定体系可以和洗涤剂组合物相容,可包含钙离子、硼酸、硼砂、丙二醇、甘油、多元醇的一种及或多种的混合物。酶稳定体系的重量和用量根据洗涤剂组合物的形式和组成以及酶制剂的类型进行调整。
添加剂
本发明涉及的液体洗衣凝珠洗涤剂组合物包含如下任选的添加剂:添加剂选自碱剂、粘度调节剂、pH稳定剂、防腐剂、抗再沉积剂、功能性聚合物、螯合剂、荧光增白剂和香精中的一种或多种。
碱剂
本发明涉及的液体洗涤剂组合物可以包含一种或多种碱剂,碱剂选自氢氧化钠、氢氧化钾、碱金属碳酸盐、碱金属的硅酸盐。碱剂在所述液体洗涤剂组合物中的重量百分含量为0.01%~30.0%,进一步的为0.05%~10.0%,更进一步地为0.05%~5.0%。
粘度调节剂
本发明涉及的液体洗涤剂组合物可以包含一种或更多种粘度调节剂,以提供合适的粘度。适宜的粘度调节剂如盐、多糖、胶料、短链脂肪醇、短链脂肪醇烷基醚。合适的例子是氯化钠、甲酸钠、乙酸钠、乙醇、丙二醇、柠檬酸钠、烷基羟烷基纤维素醚、卡拉胶、黄原胶、聚丙烯酰胺衍生物。粘度调节剂在所述液体洗涤剂组合物中的重量百分含量为0.01%~30.0%,进一步地为0.05%~10.0%,更进一步地选为0.05%~5.0%。
防腐剂
在一些实施方案中,本发明涉及的液体洗涤剂组合物优选包含防腐剂,合适的例子是苯氧基醇、苯甲酸钠;异噻唑啉酮及其衍生物,如甲基异噻唑啉酮、甲基氯异噻唑啉酮、苯并异噻唑啉酮的一种或其混合物。所述防腐剂用量为0.001%至5%,进一步地为0.01%至2%。
抗再沉积剂
从有效提高洗涤效果的观点出发,在本发明涉及的液体洗涤剂组合物可以包含抗再沉积剂。抗再沉积剂包括但不限于以下化合物组成的组:
纤维素衍生物,例如羧甲基纤维素、乙基羟乙基纤维素、甲基纤维素;乙烯基吡咯烷酮的均聚物和共聚物,例如直链聚乙烯基吡咯烷酮、乙烯基吡咯烷酮和乙酸乙烯酯的共聚物、乙烯基吡咯烷酮和乙烯基咪唑的共聚物;聚羧酸盐,例如聚丙烯酸盐、聚丙烯酸聚马来酸共聚物、丙烯酸-丙烯酸酯-磺酸盐共聚物。抗再沉积剂在液体洗涤剂组合物中含量为0.01%至5%,进一步地为0.01%~2%。
功能性聚合物
本发明涉及的洗涤剂组合物包含一种或多种功能性聚合物,其包括两亲性烷氧基化油脂清洁聚合物、羧酸酯聚合物和/或改性羧酸酯聚合物、聚羧酸盐和/或改性聚羧酸盐。
本发明涉及的洗涤剂组合物可包含两亲性烷氧基化油脂清洁聚合物,其具有平衡的亲水性能和疏水性能,使得他们从织物表面或硬表面去除油脂颗粒。该两亲性烷氧基化油脂清洁聚合物的一类实施例是包含一个或多个芯结构以及多个连接至该芯结构的烷氧基化基团,其芯结构可以但不局限于乙二胺、三亚乙基四胺、四亚乙基五胺等分子式为H2N(C2H4NH)nH的线性多胺结构或星型聚乙烯亚胺,其烷氧基化基团可以但不局限于聚氧乙烯基、聚氧丙烯基和/或它们的嵌段和/或无规则共聚基团。
本发明涉及的液体洗涤剂组合物中,两亲性烷氧基化油脂清洁聚合物在所述液体洗涤剂组合物中的重量百分含量为0~10.0%,进一步地为0.1%~5.0%,更进一步地为0.5%~2.0%。
本发明涉及的洗涤剂组合物可包含羧酸酯聚合物和/或改性羧酸酯聚合物,以增强组合物对油脂的清除能力。包括羧酸酯聚合物可以是聚丙烯酸酯均聚物或者马来酸酯/丙烯酸酯的无规则共聚物,以及烷氧基化聚羧酸酯即含有聚氧乙烯基侧链的聚丙烯酸酯。其分子量通常在约2000至约50000之间。本发明涉及的液体洗涤剂组合物中,羧酸酯聚合物和/或改性羧酸酯聚合物在所述液体洗涤剂组合物中的重量百分含量为0~10.0%,优选为0.1%~5.0%,更优选为0.5%~2.0%。
本发明涉及的洗涤剂组合物可包含聚羧酸盐和/或改性聚羧酸盐,以增强组合物对颗粒性污垢的清除能力以及抑制钙垢形成。包括一种或多种含双键的脂肪羧酸单体所聚合而成的均聚物和共聚物的水溶性盐,所用含双键的脂肪羧酸单体包括但不限于丙烯酸、甲基丙烯酸、马来酸、衣康酸、中康酸、富马酸、乌头酸、柠康酸和亚甲基丙二酸。
改性聚羧酸盐的侧链上含有聚氧乙烯基或烷烃基,其分子量通常在约2000至约10000之间。本发明涉及的液体洗涤剂组合物中,聚羧酸盐和/或改性聚羧酸盐在所述液体洗涤剂组合物中的重量百分含量为0~10.0%,进一步地为为0.1%~5.0%,更进一步地为0.5%~2.0%。
螯合剂
本发明所述液体洗涤剂组合物可包含一种或多种金属离子螯合剂,包括铜、铁和/或锰螯合剂以及它们的混合物。这些螯合剂可以降低液体洗涤剂中游离的金属离子的浓度,从而降低这些金属离子对酶制剂的失活作用、对其他组分的催化分解作用等。可用做螯合剂的包括氨基羧酸盐、氨基膦酸盐等,包括但不限于乙二胺四乙酸盐(EDTA)、氨三乙酸盐(NTA)、二亚乙基三胺五乙酸盐(DTPA)、丙氨酸二乙酸盐(MGDA)、谷氨酸二乙酸盐(GLDA)和/或乙二胺四(亚甲基磷酸盐)(EDTMPA)、氨三(亚甲基磷酸盐)(ATMP)、二亚乙基三胺五(亚甲基磷酸盐)(DTPMP)、羟基-乙烷二膦酸盐(HEDP)以及乙二胺二琥珀酸盐(EDDS)以及它们混合物。
本发明涉及的液体洗涤剂组合物中,螯合剂在液体洗涤剂组合物中的重量百分含量为0~20.0%,进一步的为0.1%~5.0%,更进一步的为0.5%~2.0%。
制备方法
本发明的液体洗衣凝珠组合物采用本领域技术人员所熟知的各种方法制备。所述组合物的制备可以通过常规手段进行,具体应根据组分在溶液中的状态和作用,以及组分的稳定性选择合适的加工温度和加工时间。
无需进一步详细说明,相信本领域技术人员使用以上所述即可最大限度地使用本发明。下面的实施例目的在于进一步介绍和展示在本发明范围内的具体实施方案。因此,以下实施例应理解为仅用于更详细地展示本发明,而不以任何方式限制本发明的内容。
以下实施例及对比例的液体洗衣凝珠组合物的制备方法,包括如下步骤:
1)向配制罐中加入部分去离子水、主溶剂中的二元醇、助溶剂甘油和山梨醇和碱剂单乙醇胺,搅拌5min;
2)加入油酸、十二酸与单乙醇胺中和成脂肪酸盐,搅拌至溶解完全后加入磺酸盐型表面活性剂、乙氧基化脂肪醇硫酸盐,搅拌5min待溶液澄清后,开启冷冻水降温;
3)待温度降至40-50℃,加入C12-C14醇乙氧基化物,搅拌至溶解完全;
4)加入主溶剂中的聚乙二醇;
5)加入柠檬酸钠调节pH;
6)加入所述纤维素酶Celluclean 5000L,搅拌均匀;
7)加入其它酶制剂、色素、聚乙烯亚胺乙氧基化合物、香精等添加剂,搅拌至完全溶解;
8)加入余量去离子水,搅拌均匀。
实施例和对比例
在以下实施例1-9和对比例1-9中列举说明了本发明的实施方案,尽管本发明并不旨在由这些实施例和对比例限制,但所述实施例说明了根据本发明的实施方案。
按照表1所示的配比制备液体洗衣凝珠组合物A~J。
表1液体洗衣凝珠组合物A~J
检测液体洗衣凝珠组合物A~J的酶活保持率和存储稳定性,结果如表2所示。
表2液体洗衣凝珠组合物A~J的酶活保持率和存储稳定性
以上实施例1-5和对比例1-5中选择了市售纤维素酶Celluclean 5000L,实施例1-5显示在主溶剂与助溶剂的重量比为(0.5~1.75):1,阴离子表面活性剂与非离子表面活性剂的重量比为(1.80~2.5):1,老化4周纤维素酶酶活保持率为82%~100%,老化8周的纤维素酶活保持率为69%~82%,且实施例在1-5在常温和老化存储过程中稳定无沉淀。
而对比例1-5中主溶剂与助溶剂的重量比为(1.92~2.93):1,阴离子表面活性剂与非离子表面活性剂的重量比为(1.82~2.46):1。老化4周纤维素酶的酶活保持率为49%~71%,老化8周的纤维素酶活保持率为37%~58%。而且对比例1、4、5在常温和老化存储过程中出现了沉淀。
按照表3所示的配比制备液体洗衣凝珠组合物K~R。
表3液体洗衣凝珠组合物K~R
检测液体洗衣凝珠组合物K~R的酶活保持率和存储稳定性,结果如表4所示。
表4液体洗衣凝珠组合物K~R的酶活保持率和存储稳定性
以上实施例6-9和对比例6-9中选择了市售纤维素酶Carezyme 4500L,实施例6-9显示在主溶剂与助溶剂的重量比为(0.5~1.34):1,阴离子表面活性剂与非离子表面活性剂的比率为(1.8~2.29):1,老化4周纤维素酶酶活保持率为88%~100%,老化8周的纤维素酶活保持率为71%~82%,且实施例在6-9在常温和老化存储过程中稳定无沉淀。
而对比例6-9中主溶剂与助溶剂的重量比为(1.15~1.68):1,阴离子表面活性剂与非离子表面活性剂的重量比为(2.52~2.65):1。老化4周纤维素酶的酶活保持率为49%~71%,老化8周的纤维素酶活保持率为39%~58%。而且对比例6、7、9在常温和老化存储过程中出现了沉淀。
以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (8)
1.一种含有纤维素酶的液体洗衣凝珠组合物,其特征在于,按组合物总量的重量百分比计,包含:
25%~45%的有机溶剂;所述有机溶剂包含主溶剂和助溶剂,主溶剂为聚乙二醇和/或二元醇,助溶剂为具有3~6个碳原子的多元醇,其中主溶剂与助溶剂的重量比为(0.5~1.75):1;
20%~60%的表面活性剂;所述表面活性剂中阴离子表面活性剂与非离子表面活性剂的重量比为(1.8~2.5):1,阴离子表面活性剂中磺酸盐型表面活性剂的重量占比为35%~50%;
0.1%~2%的纤维素酶;
余量的水;
所述二元醇选自乙二醇、丙二醇、丁二醇、戊二醇、二丙二醇、二甘醇、三甘醇或者其混合物;
所述助溶剂选自甘油、木糖醇、山梨醇、甘露醇、赤藓糖醇、半乳糖醇或其混合物;
所述的阴离子表面活性剂还包括羧酸盐型表面活性剂、硫酸盐型表面活性剂的一种或多种;
所述的非离子表面活性剂选自脂肪醇烷氧基化物、烷基多糖苷、脂肪酸烷氧基化物、脂肪酸烷基醇酰胺、乙氧基化失水山梨酸醇酯的一种或多种的混合物。
2.如权利要求1所述的含有纤维素酶的液体洗衣凝珠组合物,其特征在于:所述聚乙二醇选自相对分子量200~600之间的聚乙二醇。
3.如权利要求1所述的含有纤维素酶的液体洗衣凝珠组合物,其特征在于:所述的脂肪酸烷氧基化物为脂肪酸乙氧基化物。
4.如权利要求1所述的含有纤维素酶的液体洗衣凝珠组合物,其特征在于:还包括其它酶制剂和添加剂,所述其它酶制剂和添加剂的总量为0.02%~20%。
5.如权利要求4所述的含有纤维素酶的液体洗衣凝珠组合物,其特征在于:所述其它酶制剂选自蛋白酶、淀粉酶、脂肪酶、果胶酶、甘露聚糖酶中的一种或多种。
6.如权利要求5所述的含有纤维素酶的液体洗衣凝珠组合物,其特征在于:所述添加剂选自碱剂、粘度调节剂、pH稳定剂、防腐剂、抗再沉积剂、功能性聚合物、螯合剂、香精或色素中的一种或多种。
7.如权利要求4所述的含有纤维素酶的液体洗衣凝珠组合物,其特征在于:所述添加剂选自碱剂。
8.如权利要求7所述的含有纤维素酶的液体洗衣凝珠组合物的制备方法,其特征在于,包括如下步骤:
将水、主溶剂中的二元醇、助溶剂和碱剂混合;加入阴离子表面活性剂,混合至溶液澄清后,采用冷冻水降温;
待温度降至40-50℃,加入非离子表面活性剂,混合至溶解完全;
加入主溶剂中的聚乙二醇混合均匀;
加入所述纤维素酶,搅拌均匀;
加入余量去离子水,搅拌均匀。
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