CN111304017A - 温和低泡洗衣凝珠及其制备方法 - Google Patents
温和低泡洗衣凝珠及其制备方法 Download PDFInfo
- Publication number
- CN111304017A CN111304017A CN202010213632.1A CN202010213632A CN111304017A CN 111304017 A CN111304017 A CN 111304017A CN 202010213632 A CN202010213632 A CN 202010213632A CN 111304017 A CN111304017 A CN 111304017A
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- China
- Prior art keywords
- isomeric alcohol
- acid
- mild low
- parts
- alkyl glycoside
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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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
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/04—Detergent materials or soaps characterised by their shape or physical properties combined with or containing other objects
- C11D17/041—Compositions releasably affixed on a substrate or incorporated into a dispensing means
- C11D17/042—Water soluble or water disintegrable containers or substrates containing cleaning compositions or additives for cleaning compositions
- C11D17/043—Liquid or thixotropic (gel) compositions
-
- 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
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- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0026—Low foaming or foam regulating compositions
-
- 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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- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2041—Dihydric 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
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- 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
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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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- C11D3/2086—Hydroxy carboxylic acids-salts thereof
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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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- C11D3/16—Organic compounds
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- C11D3/349—Organic compounds containing sulfur additionally containing nitrogen atoms, e.g. nitro, nitroso, amino, imino, nitrilo, nitrile groups containing compounds or their derivatives or thio urea
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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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- C11D3/3757—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions
- C11D3/3765—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions in liquid compositions
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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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- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
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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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- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38618—Protease or amylase in liquid 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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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
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Abstract
本发明提供温和低泡洗衣凝珠及其制备方法。其原料按重量份数计包括:异构醇烷基糖苷30‑40、脂肪酸甲酯乙氧基化物8‑18、异构醇聚氧乙烯醚5‑12、脂肪酸甲酯磺酸盐3‑8、丙二醇15‑20、山梨醇5‑8、丙烯酸‑马来酸共聚物1‑2、酶0.05‑2、抗菌剂0.4‑0.6、香精0.1‑0.5、防腐剂0.03‑0.1和去离子水0‑10,其采用异构醇烷基糖苷作为主表面活性剂,使得无需加入消泡剂即可达到低泡效果,从而在温和低泡的同时,不会影响活性组分的活性及含量,从而使得洗衣凝珠兼具温和、低泡和高去污能力的优点,综合性能佳。制备方法简单易操作。
Description
技术领域
本发明属于日用化学品领域,具体涉及温和低泡洗衣凝珠及其制备方法。
背景技术
洗衣凝珠是一款新型的洗衣产品,专为机洗设计,操作简单,方便不脏手,其活性物质含量一般超过45%,远超普通洗衣液15-25%的含量,具有超强洁净力;此外由于洗衣凝珠为超浓缩洗涤剂,体积小巧,水含量低,生产过程节能节水,运输成本也大大降低,对节能减排具有重要意义,另外其外包膜为水溶性聚乙烯醇薄膜,为绿色可生物降解包材,可降低塑料包装对环境的污染。洗衣凝珠在欧美推出后备受青睐,在衣物洗涤剂市场占有率超过10%,2014年宝洁首先开始在中国推广洗衣凝珠产品,但一直处于较为冷清的状态,近年随着线上平台的推广、消费者对于日化产品在性能方面的需求提升,洗衣凝珠市场份额逐渐扩大,发展前景良好。
烷基糖苷是一种温和型非离子表面活性剂,为直链脂肪醇与葡萄糖在酸性催化剂条件下缩醛反应制得,是国际公认的温和型绿色表活,其泡沫丰富,配伍性好,去污性能优良,但用于机洗洗衣凝珠,其泡沫丰富的性质会导致需要大量水进行漂洗,造成水资源的浪费。比如,CN106544179A公开了一种婴幼儿用洗衣凝珠,由以下质量百分比计的组分组成:20~30%烷基糖苷0814、15~25%椰子油脂肪酸二乙醇酰胺、15~25%椰油酰丙基甜菜碱CAB-35、1~5%十二醇聚氧乙烯醚磺基琥珀酸酯二钠、1~5%N-月桂酰基谷氨酸钠、20~30%多元醇、0.02~0.05%蛋白酶、0.03~0.08%山茶精油、0.03~0.08%天然植物提取液、余量为去离子水,该配方选用的表面活性剂泡沫丰富、去污性能优良、绿色温和,但用于机洗时泡沫太多不易漂洗。
CN 106906059 A公开了一种低泡易漂洗洗衣凝珠,由以下质量百分比计的组分组成:15~30%C12~18烷基糖苷、15~25%椰油脂肪酸二乙醇酰胺、10~20%非离子表面活性剂贝斯曼LT107、10~20%消泡型表面活性剂贝斯曼L85、20~30%多元醇、0.02~1%酶、0.02~1.5%香精、0.06~0.15%防腐剂、余量为去离子水。为了降低烷基糖苷的泡沫,加入了10~20%的消泡剂,降低了其余活性组分的含量,影响洗衣凝珠的综合性能。
因此,目前需要寻求一种温和低泡洗衣凝珠,以同时兼顾良好的去污性能和低泡性能。
发明内容
本发明的第一个目的在于提供一种温和低泡洗衣凝珠,该温和低泡洗衣凝珠去污能力强,且温和低泡,容易清洗。
本发明的第二个目的在于提供前述温和低泡洗衣凝珠的制备方法,该制备方法工艺简单易操作。
为实现发明的第一个目的,采用以下的技术方案:
一种温和低泡洗衣凝珠,采用包括以下重量份数的原料制备得到:
异构醇烷基糖苷 30-40,优选32-36,比如33、34和35;
脂肪酸甲酯乙氧基化物 8-18,优选12-16,比如13、14和15;
异构醇聚氧乙烯醚 5-12,优选7-10,比如8和9;
脂肪酸甲酯磺酸盐 3-8,优选4-6,比如5;
丙二醇 15-20,优选17-19,比如18;
山梨醇 5-8,优选5.5-7,比如6和6.5;
丙烯酸-马来酸共聚物 1-2,优选1.2-1.5,比如1.3和1.4;
酶 0.05-2,比如0.1、0.2、0.5、1.0、1.4和1.8;
抗菌剂 0.4-0.6,比如0.45、0.5和0.55;
香精 0.1-0.5,优选0.2-0.3,比如0.25;
防腐剂 0.03-0.1,比如0.05、0.07、0.08和0.09;
去离子水0-10,比如2、4、5、6和8;其中,
所述异构醇烷基糖苷的结构式如下:
本发明中,异构醇烷基糖苷作为主表面活性剂加入,其结构中作为端基的格尔伯特异构十醇基团会使得洗衣凝珠的润湿性得到提升,作为中间基团的聚环氧丙烷基团具备多支链结构,消泡性能优良,兼具润湿、低泡、温和的特性;异构醇烷基糖苷的加入,使得无需加入消泡剂即可达到低泡效果,从而在温和低泡的同时,不会影响活性组分的活性及含量,从而使得洗衣凝珠兼具温和、低泡和高去污能力的优点,综合性能佳。
本领域技术人员理解,所述异构醇烷基糖苷的分子式为C6H11O5-(C3H6O)n-C10H21O,即C16+3nH32+6nO6+n。
在一种实施方式中,前述各原料的重量份数总和为100。此时,去离子水的用量为0-10wt%,从而有助于防止凝珠表层包覆的水溶膜***甚至破裂。
本领域技术人员理解,异构醇聚氧乙烯醚是一种表面活性剂,主要分为异构十醇聚氧乙烯醚、异构十一醇聚氧乙烯醚、异构十三醇聚氧乙烯醚。在一种实施方式中,所述异构醇聚氧乙烯醚为异构十醇聚氧乙烯醚和/或异构十三醇聚氧乙烯醚,优选为异构十醇聚氧乙烯醚,即支链化十碳格尔伯特醇聚氧乙烯醚,从而提高洗衣凝珠的湿润性。
优选地,所述异构醇烷基糖苷的制备方法包括以下步骤:
(1)将格尔伯特异构十醇与环氧丙烷在碱性催化剂作用下进行开环聚合反应,然后加入有机酸进行中和,再进行抽真空脱单,得到异构醇烷氧基中间体;
(2)将步骤(1)所得异构醇烷氧基中间体与葡萄糖在酸性催化剂作用下进行缩醛化反应,然后加入无机碱进行中和至pH为7-8,得到粗反应液;
(3)对步骤(2)所得粗反应液进行减压蒸馏除去其中未反应的异构醇烷氧基中间体,得到异构醇烷基糖苷粗产品;
(4)对步骤(3)所得异构醇烷基糖苷粗产品进行漂色处理,得到异构醇烷基糖苷。
本领域技术人员理解,格尔伯特异构十醇又名二丙基庚醇,其是在第二个碳上连有支链、且总碳原子为10个的脂肪醇。
本领域技术人员理解,所述步骤(1)中,抽真空脱单主要是脱除其中游离的有机酸单体和环氧丙烷单体,从而提高异构醇烷氧基中间体的纯度,有利于后续缩醛化反应的顺利进行,提高其反应速率。
优选地,所述步骤(1)中,格尔伯特异构十醇与环氧丙烷的摩尔比为1:(1.5-2.5),优选1:(1.8-2),比如1.9,以利于开环聚合反应的顺利进行。
在一种实施方式中,所述步骤(1)中,碱性催化剂为氢氧化钾、氢氧化钠和甲醇钾中的任一种或多种的组合,比如氢氧化钾;优选碱性催化剂的用量为格尔伯特异构十醇质量的0.45-0.6wt%,比如0.5wt%和0.55wt%,从而有效催化开环聚合反应,提高开环聚合反应的反应速率。
在一种实施方式中,所述步骤(1)中,有机酸为乙酸和/或乳酸,比如乙酸;有机酸的用量与碱性催化剂的用量形成化学计量比,以充分中和碱性催化剂,且尽可能不残留有机酸,从而提高开环聚合反应的产物-异构醇烷氧基中间体的纯度。
化学计量比是根据化学平衡将化学方程式配平后各物质化学式前面的系数之比,也是其物质的量之比。比如本发明中,若有机酸与碱性催化剂反应的方程式配平后为:n1有机酸+n2碱性催化剂=n3水+n4M;其中,M代表该反应的反应产物中,除水之外的另一种产物;n1、n2、n3和n4分别代表有机酸、碱性催化剂、水和M前面的系数,则有机酸的用量与所述碱性催化剂的用量形成化学计量比的意思就是有机酸与碱性催化剂的物质的量之比为n1/n2,即二者的摩尔比为n1/n2。
优选地,所述步骤(1)中,反应温度为125-130℃,比如126℃、127℃、128℃和129℃;反应时间为1.5-2h,比如1.6h、1.7h、1.8h和1.9h,从而有利于开环聚合反应的顺利进行,提高开环聚合反应的反应速率和产率。
优选地,所述步骤(2)中,异构醇烷氧基中间体与葡萄糖的摩尔比为(3-5):1,比如3.5:1、4:1和4.5:1,从而有利于缩醛化反应的顺利进行。
在一种实施方式中,所述步骤(2)中,酸性催化剂为十二烷基苯磺酸、对甲苯磺酸和甲基二磺酸中的任一种或多种的组合,比如十二烷基苯磺酸;优选酸性催化剂的用量为葡萄糖质量的1.5-2wt%,比如1.6wt%、1.7wt%、1.8wt%和1.9wt%,从而有效催化缩醛化反应,提高缩醛化反应的反应速率。
本领域技术人员理解,所述步骤(2)中,所述无机碱可以为本领域常用的无机碱。在一种实施方式中,所述步骤(2)中,所述无机碱为氢氧化钠/或氢氧化钾,比如氢氧化钠。
优选地,所述步骤(2)中,反应温度为120-130℃,比如122℃、124℃、126℃和128℃;反应时间为5-8h,比如5.5h、6h、6.5h和7.5h,从而有利于缩醛化反应的顺利进行,提高缩醛化反应的反应速率和产率。
优选地,所述步骤(3)中,减压蒸馏条件如下:温度为190-195℃,比如191℃、192℃、193℃和194℃;绝对压力为0.02-0.1kPa,比如0.04kPa、0.06kPa和0.08kPa,从而提高减压蒸馏的效果,以尽可能完全除去其中未反应的异构醇烷氧基中间体,进而提高后续产品的纯度。
由于异构醇烷基糖苷为热敏性物质,高温容易炭化而产生有色基团,因此,异构醇烷基糖苷粗产品带有颜色。为获得合格的异构醇烷基糖苷产品,需要除去有色基团,脱除颜色。
在一种实施方式中,所述步骤(4)中,漂色剂为双氧水,其用量为异构醇烷基糖苷粗产品质量的2.5-3.5wt%,比如2.75wt%、3wt%和3.25wt%,以对异构醇烷基糖苷粗产品充分漂色,得到合格的异构醇烷基糖苷产品。
本领域技术人员可以理解,所述酶为本领域常用的酶。在一种实施方式中,所述酶为蛋白酶、脂肪酶、淀粉酶和纤维素酶中的任一种或多种的组合。
本领域技术人员可以理解,所述抗菌剂为本领域常用的抗菌剂。在一种实施方式中,所述抗菌剂为4,4-二氯-2-羟基联苯醚和/或三氯羟基二苯醚。
本领域技术人员可以理解,所述香精为本领域常用的香精。在一种实施方式中,所述香精为茉莉精油、薄荷精油、广藿香精油和茶树精油中的任一种或多种的组合。
本领域技术人员可以理解,所述防腐剂为本领域常用的防腐剂。在一种实施方式中,所述防腐剂为苯甲酸钠、山梨酸和山梨醇钾中的任一种或多种的组合。
在一种实施方式中,所述防腐剂为5-氯-2-甲基-4-异噻唑啉-3-酮和2-甲基-4-异噻唑啉-3-酮的混合物,优选5-氯-2-甲基-4-异噻唑啉-3-酮和2-甲基-4-异噻唑啉-3-酮的质量比为(2-4):1,比如3:1。
为实现本发明的第二个目的,本发明提供一种前述温和低泡洗衣凝珠的制备方法,包括如下步骤:
(1)按照重量份数准备各原料;
(2)将异构醇烷基糖苷、脂肪酸甲酯乙氧基化物、异构醇聚氧乙烯醚、脂肪酸甲酯磺酸盐、丙二醇、山梨醇、丙烯酸-马来酸共聚物和去离子水混合均匀,得混合溶液;优选混合温度为45-50℃,比如46℃、47℃、48℃和49℃;
(3)将步骤(2)所得混合溶液冷却至室温(比如25±5℃),然后向其中加入酶、抗菌剂、香精和防腐剂,混合均匀,得料液;
(4)将步骤(3)所得料液加入洗衣凝珠自动包装机中进行包装,并采用聚乙烯醇水溶性膜进行封包,得到温和低泡洗衣凝珠。
本领域技术人员理解,温和低泡洗衣凝珠的制备方法为本领域的常用方法。
本发明的有益效果在于:
(1)本发明的温和低泡洗衣凝珠,其制备原料中使用了异构醇烷基糖苷,并将其作为主表面活性剂加入,其结构中作为端基的格尔伯特异构十醇基团会使得洗衣凝珠的润湿性得到提升,作为中间基团的聚环氧丙烷基团具备多支链结构,消泡性能优良,兼具润湿、低泡、温和的特性;异构醇烷基糖苷的加入,使得无需加入消泡剂即可达到低泡效果,从而在温和低泡的同时,不会影响活性组分的活性及含量,从而使得洗衣凝珠兼具温和、低泡、湿润和高去污能力的优点,易于漂洗,综合性能佳,在保证去污效果的同时能够大大节省水资源;
(2)本发明的温和低泡洗衣凝珠,其所用的原料异构醇烷基糖苷是利用本发明的制备方法制备得到,其纯度高,质量好,用于制备洗衣凝珠时,有助于进一步提高洗衣凝珠的综合性能;
(3)本发明的温和低泡洗衣凝珠的制备方法,使用异构醇烷基糖苷作为主表面活性剂,能够使洗衣凝珠兼具温和、低泡、湿润和高去污能力的优点,综合性能佳;工艺简单,易操作。
具体实施方式
以下通过具体实施例对本发明技术方案及其效果做进一步说明。以下实施例仅用于说明本发明的内容,并不用于限制本发明的保护范围。应用本发明的构思对本发明进行的简单改变都在本发明要求保护的范围内。
以下实施例和对比例中用到的原料来源如下:
格尔伯特异构十醇:纯度>99%,神华包头煤化工有限公司;
环氧丙烷:纯度>99%,万华化学股份有限公司;
氢氧化钾:纯度>96%,科密欧化学试剂有限公司;
氢氧化钠:纯度>96%,科密欧化学试剂有限公司;
甲醇钾:纯度>95%,阿拉丁试剂有限公司;
乙酸:纯度>99%,科密欧化学试剂有限公司;
乳酸:纯度>90%,西陇科学有限公司;
十二烷基苯磺酸:纯度>90%,阿拉丁试剂有限公司;
对甲苯磺酸:纯度>99%,科密欧化学试剂有限公司;
甲基二磺酸:纯度>99%,上海沪旦生物科技有限公司;
葡萄糖:纯度>99%,科密欧化学试剂有限公司;
双氧水:纯度30%,科密欧化学试剂有限公司;
脂肪酸甲酯乙氧基化物:FMEE-Ⅱ,活性物含量≥98%,pH(1%水溶液)为6-8,中轻日化科技集团有限公司;
异构醇聚氧乙烯醚:LutensolXP50,是一种异构十醇聚氧乙烯醚,活性物含量为100%,羟值为150mgKOH/g,浊点(1%水溶液)为56℃,巴斯夫股份公司;
丙烯酸-马来酸共聚物:Acusol 479N,活性物含量为40%,陶氏化学;
脂肪酸甲酯磺酸盐:活性物含量≥80%,赞宇科技股份有限公司;
丙二醇:纯度>99%,阿拉丁试剂有限公司;
山梨醇:纯度>99%,国药集团试剂有限公司;
蛋白酶:型号PRO-03L,上海丹尼悦生物科技有限公司;
脂肪酶:型号LIP-1A,上海丹尼悦生物科技有限公司;
淀粉酶:型号AMSL,上海丹尼悦生物科技有限公司;
纤维素酶:型号80L,上海丹尼悦生物科技有限公司;
4,4-二氯-2-羟基联苯醚:型号HP100,活性物含量30%,巴斯夫股份公司;
三氯羟基二苯醚:型号DP300,活性物含量100%,巴斯夫股份公司;
茉莉精油:型号JB007,华天宝中草药生物制品厂;
薄荷精油:型号JB032,华天宝中草药生物制品厂;
广藿香精油:型号JB100,华天宝中草药生物制品厂;
茶树精油:型号JB038,华天宝中草药生物制品厂;
山梨酸:纯度≥99%,苏州甫路生物科技有限公司;
苯甲酸钠:纯度≥99%,本溪黑马化工有限公司;
山梨醇钾,纯度≥99%,本溪黑马化工有限公司。
测试方法如下:
羟值:根据GB/T 7383-2007乙酐法测定异构醇烷氧基中间体的羟值;
泡沫高度:根据GB/T13173-2008洗涤剂发泡力测试方法(Ross-Miles法)测定洗衣凝珠的泡沫高度;
去污力:根据QB/T 1224-2012《衣料用液体洗涤剂》规定的方法和污布,同机测定实施例5-8及对比例1制备的洗衣凝珠及标准洗衣液的去污力。
实施例1-4(S1-4)
根据以下步骤制备异构醇烷基糖苷A1-4,其中,原料及其用量、反应条件见表1。
制备步骤如下:
(1)将格尔伯特异构十醇与环氧丙烷在碱性催化剂作用下进行开环聚合反应,然后加入有机酸进行中和,再进行抽真空脱单,得到异构醇烷氧基中间体;
(2)将步骤(1)所得异构醇烷氧基中间体与葡萄糖在酸性催化剂作用下进行缩醛化反应,然后加入无机碱进行中和至pH为7-8,得到粗反应液;
(3)对步骤(2)所得粗反应液进行减压蒸馏除去其中未反应的异构醇烷氧基中间体,得到异构醇烷基糖苷粗产品;
(4)对步骤(3)所得异构醇烷基糖苷粗产品进行漂色处理,得到异构醇烷基糖苷。
表1 S1-4中原料及其用量、反应条件
经测定,实施例1-4中步骤(1)所得异构醇烷氧基中间体的羟值分别为228.7mgKOH/g、185.3mgKOH/g、208.7mgKOH/g和204.9mgKOH/g;通过羟值计算其分子量分别为245.3g/mol、302.8g/mol、268.8g/mol和273.8g/mol,对应产物异构醇烷基糖苷中的n值分别为1.5、2.5、1.9和2。
实施例5-8(S5-8)和对比例1(D1)
根据以下步骤制备温和低泡洗衣凝珠B1-4和洗衣凝珠B1’,其中,原料及其用量、反应条件见表2。
制备步骤如下:
(1)将异构醇烷基糖苷、脂肪酸甲酯乙氧基化物、异构醇聚氧乙烯醚、脂肪酸甲酯磺酸盐、丙二醇、山梨醇、丙烯酸-马来酸共聚物和去离子水混合均匀,得混合溶液;
(2)将步骤(1)所得混合溶液冷却至室温,然后向其中加入酶、抗菌剂、香精和防腐剂,混合均匀,得料液;
(3)将步骤(2)所得料液加入洗衣凝珠自动包装机中进行包装,并采用聚乙烯醇水溶性膜进行封包,得到洗衣凝珠。
表2 S5-8及D1中原料及其用量、反应条件
洗衣凝珠性能测试:
实施例5-8及对比例1中所制得洗衣凝珠,以及标准洗衣液的性能测试结果见表3。
表3 S5-8和D1中洗衣凝珠及标准洗衣液的性测试结果
根据实施例5-8和对比例1及标准洗衣液的比较可知,本发明制得的洗衣凝珠相对于标准洗衣液及选用C12-C14烷基糖苷做主表面活性剂的对比例1,其初始泡沫高度较低且消泡性能良好,具备低泡易漂洗特性,且其去污力强,清洁能力有较大提高。
Claims (10)
2.根据权利要求1所述的温和低泡洗衣凝珠,其特征在于,所述异构醇烷基糖苷的制备方法包括以下步骤:
(1)将格尔伯特异构十醇与环氧丙烷在碱性催化剂作用下进行开环聚合反应,然后加入有机酸进行中和,再进行抽真空脱单,得到异构醇烷氧基中间体;
(2)将步骤(1)所得异构醇烷氧基中间体与葡萄糖在酸性催化剂作用下进行缩醛化反应,然后加入无机碱进行中和至pH为7-8,得到粗反应液;
(3)对步骤(2)所得粗反应液进行减压蒸馏除去其中未反应的异构醇烷氧基中间体,得到异构醇烷基糖苷粗产品;
(4)对步骤(3)所得异构醇烷基糖苷粗产品进行漂色处理,得到异构醇烷基糖苷。
3.根据权利要求2所述的温和低泡洗衣凝珠,其特征在于,所述步骤(1)中,格尔伯特异构十醇与环氧丙烷的摩尔比为1:(1.5-2.5);
优选地,所述步骤(1)中,反应温度为125-130℃,反应时间为1.5-2h。
4.根据权利要求2或3所述的温和低泡洗衣凝珠,其特征在于,所述步骤(1)中,碱性催化剂为氢氧化钾、氢氧化钠和甲醇钾中的任一种或多种的组合;优选碱性催化剂的用量为格尔伯特异构十醇质量的0.45-0.6wt%;
优选地,所述步骤(1)中,有机酸为乙酸和/或乳酸;优选有机酸的用量与碱性催化剂的用量形成化学计量比。
5.根据权利要求2-4中任一项所述的温和低泡洗衣凝珠,其特征在于,所述步骤(2)中,异构醇烷氧基中间体与葡萄糖的摩尔比为(3-5):1;
优选地,所述步骤(2)中,反应温度为120-130℃,反应时间为5-8h。
6.根据权利要求2-5中任一项所述的温和低泡洗衣凝珠,其特征在于,所述步骤(2)中,酸性催化剂为十二烷基苯磺酸、对甲苯磺酸和甲基二磺酸中的任一种或多种的组合;优选酸性催化剂的用量为葡萄糖质量的1.5-2wt%。
7.根据权利要求2-6中任一项所述的温和低泡洗衣凝珠,其特征在于,所述步骤(3)中,减压蒸馏条件如下:温度为190-195℃,绝对压力为0.02-0.1kPa。
8.根据权利要求2-7中任一项所述的温和低泡洗衣凝珠,其特征在于,所述步骤(4)中,漂色剂为双氧水,其用量为异构醇烷基糖苷粗产品质量的2.5-3.5wt%。
9.根据权利要求1-8中任一项所述的温和低泡洗衣凝珠,其特征在于,所述酶为蛋白酶、脂肪酶、淀粉酶和纤维素酶中的任一种或多种的组合;
优选地,所述抗菌剂为4,4-二氯-2-羟基联苯醚和/或三氯羟基二苯醚;
优选地,所述香精为茉莉精油、薄荷精油、广藿香精油和茶树精油中的任一种或多种的组合
优选地,所述防腐剂为苯甲酸钠、山梨酸和山梨醇钾中的任一种或多种的组合。
10.一种如权利要求1-9中任一项所述温和低泡洗衣凝珠的制备方法,其特征在于,所述制备方法包括如下步骤:
(1)按照重量份数准备各原料;
(2)将异构醇烷基糖苷、脂肪酸甲酯乙氧基化物、异构醇聚氧乙烯醚、脂肪酸甲酯磺酸盐、丙二醇、山梨醇、丙烯酸-马来酸共聚物和去离子水混合均匀,得混合溶液;优选混合温度为45-50℃;
(3)将步骤(2)所得混合溶液冷却至室温,然后向其中加入酶、抗菌剂、香精和防腐剂,混合均匀,得料液;
(4)将步骤(3)所得料液加入洗衣凝珠自动包装机中进行包装,并采用聚乙烯醇水溶性膜进行封包,得到温和低泡洗衣凝珠。
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