CN117467128A - 一种基于丁香酚的阴离子匀染剂、合成方法及应用 - Google Patents
一种基于丁香酚的阴离子匀染剂、合成方法及应用 Download PDFInfo
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- 239000005770 Eugenol Substances 0.000 title claims abstract description 84
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Abstract
本发明提供了一种基于丁香酚的阴离子匀染剂、合成方法及应用,将丁香酚与环氧乙烷在催化条件下加热回流发生聚合反应,得到丁香酚聚氧乙烯醚;将丁香酚聚氧乙烯醚与氨基磺酸反应得到丁香酚聚氧乙烯氨基硫酸酯;丁香酚聚氧乙烯氨基硫酸酯再与四甲基环四硅氧烷聚合得到所述阴离子匀染剂。该阴离子匀染剂对织物及染料均具有较高的亲和性,具有高效的匀染性能,同时制备原料中不含有环境有害物质,是一种生产过程绿色环保的阴离子匀染剂。
Description
技术领域
本发明涉及纺织工业领域,具体涉及一种基于丁香酚的阴离子匀染剂、合成方法及应用。
背景技术
在纺织工业生产中,分散染料高温高压染色时,常常出现色花现象,通用的解决方法是在染料中加入高温匀染剂来提高染色的质量。高温匀染剂一般为非离子和阴离子表面活性剂的复合物。非离子表面活性剂中含有大量的聚氧乙烯链段,对分散染料有亲和力,可有效降低染料的上染速率,提高匀染效果;阴离子表面活性剂对分散染料有较强的分散作用,可以解决因非离子表面活性剂浊点低造成染料凝聚而出现染斑的问题,在非离子表面活性剂分子结构中引入磺酸基,可在提高对染料分散力的同时,克服非离子表面活性剂对染料凝聚性的不利影响,极大地提升匀染和分散效果。如用烷基酚聚氧乙烯醚或苯乙烯基苯酚聚氧乙烯醚等通过磺酸化制备聚氧乙烯醚硫酸酯型高温匀染剂。
目前制备高温匀染剂的原料多为石油化工产品,存在APEO问题,需要寻找更加绿色环保的生物质材料制备高温匀染剂。
发明内容
发明目的:本发明的目的是提供一种绿色环保、染色性能优异的基于丁香酚的阴离子匀染剂及其合成方法。
技术方案:本发明提供一种基于丁香酚的阴离子匀染剂,所述阴离子匀染剂为环四硅氧烷丁香酚聚氧乙烯醚硫酸酯,包括如下结构:
其中n为10~20的整数。
本发明还提供一种基于丁香酚的阴离子匀染剂合成方法,包括以下步骤:
S1、制备丁香酚聚氧乙烯醚:将丁香酚投入反应釜中,在室温下加入催化剂钠;加入催化剂钠后通入非反应气体保护,升温至95℃后加入环氧乙烷恒温反应一段时间,其中丁香酚和环氧乙烷的摩尔比为1:(4~8),得到丁香酚聚氧乙烯醚;
S2、制备丁香酚聚氧乙烯醚硫酸酯:将上述丁香酚聚氧乙烯醚与催化剂尿素混合,升温至100℃后加入氨基磺酸,其中丁香酚聚氧乙烯醚与氨基磺酸的摩尔比为(7~10):1,继续升温至120℃,恒温反应一段时间后停止加热,降温后得到丁香酚聚氧乙烯醚硫酸酯;
S3、制备环四硅氧烷丁香酚聚氧乙烯醚硫酸酯:将四甲基环四硅氧烷、甲苯、Karsted催化剂投入反应釜,通入非反应气体保护,升温至80℃后滴加丁香酚聚氧乙烯醚硫酸酯,其中四甲基环四硅氧烷和丁香酚聚氧乙烯醚硫酸酯的摩尔比为3:(25~55),恒温反应一段时间,得到环四硅氧烷丁香酚聚氧乙烯醚硫酸酯。
所述步骤S1具体为:
S11、在室温下,在反应器中加入丁香酚,向丁香酚内加入催化剂钠,反应30min;
S12、向反应器中通入非反应气体保护,升温至95℃后,向反应器中加入环氧乙烷,反应4h;
S13、降温至60℃,加入醋酸中和反应体系,加入硅藻土过滤,得到丁香酚聚氧乙烯醚。
优选的,反应釜中压力保持0.2MPa。
优选的,催化剂钠在30min内缓慢加入。
所述步骤S2具体为:
S21、将丁香酚聚氧乙烯醚与催化剂尿素混合,升温至100℃,加入氨基磺酸;
S22、将S21中反应体系升温至120℃持续2h,降温后得到丁香酚聚氧乙烯醚硫酸酯粗产品;
S23、加入无水乙醇溶解丁香酚聚氧乙烯醚硫酸酯粗产品,过滤后蒸发乙醇,得到丁香酚聚氧乙烯醚硫酸酯。
所述步骤S3具体为:
S31、将四甲基环四硅氧烷、甲苯、Karsted催化剂加入反应釜,通入非反应气体保护后,搅拌并升温至80℃,其中四甲基环四硅氧烷与甲苯的摩尔比为6:5;
S32、滴加丁香酚聚氧乙烯醚硫酸酯,恒温反应12h;
S33、蒸发甲苯,得到环四硅氧烷丁香酚聚氧乙烯醚硫酸酯。
优选的,所述非反应性气体为氮气、二氧化碳、氦气或氩气。
优选的,所述催化剂钠与丁香酚的摩尔比为3:50;所述催化剂尿素与丁香酚聚氧乙烯醚的摩尔比为1:(35~50);所述Karsted催化剂与丁香酚聚氧乙烯醚硫酸酯的摩尔比为1:(2000~4400)。
有益效果:与现有技术相比,本发明的显著效果是:采用生物质材料丁香酚与聚乙烯醇类化合物反应得到的酯类物质作为主要原料,在材料和合成路线上实现了绿色环保;反应条件温和,制备过程简单易操作,具有较高的制备效率和较低的制备成本,适合大规模工业化生产;本发明匀染剂具有较好的匀染性能,使用后织物染色均匀,无染斑出现。
具体实施方式
下面结合具体实施方式,进一步阐明本发明。
实施例1
本实施例所述的基于丁香酚的阴离子匀染剂结构式如下:
其中n为10。
所述基于丁香酚的阴离子匀染剂合成方法如下:
S1、在室温下,将50份丁香酚投入反应釜中,在30min内加入3份催化剂钠,催化剂加完后再反应30min,之后通入氮气保护,升温至95℃,通入200份环氧乙烷,反应压力为0.2MPa,反应4h;将反应釜降温至60℃,加入醋酸中和,再加入硅藻土过滤,制得丁香酚聚氧乙烯醚,平均聚合度为10。
S2、将S1制得的70份丁香酚聚氧乙烯醚与2份催化剂尿素在反应釜中混合,升温至100℃,加入10份氨基磺酸粉末,继续升温至120℃保温2h,降温得到丁香酚聚氧乙烯醚硫酸酯粗产品,加入无水乙醇溶解丁香酚聚氧乙烯醚硫酸酯粗产品后过滤,加入碱性溶液调节体系pH呈弱碱性,过滤不溶于无水乙醇的杂质,旋转蒸发除去乙醇,得到丁香酚聚氧乙烯醚硫酸酯。
S3、将24份四甲基环四硅氧烷、20份甲苯、0.1份Karsted催化剂加入反应釜中,通入氮气保护,升温至80℃,缓慢滴加200份S2制得的丁香酚聚氧乙烯醚硫酸酯,反应12h后旋转蒸发除去甲苯,得到淡黄色黏稠液体状的环四硅氧烷丁香酚聚氧乙烯醚硫酸酯。
实施例2
本实施例所述的基于丁香酚的阴离子匀染剂结构式如下:
其中n为15。
所述基于丁香酚的阴离子匀染剂合成方法如下:
S1、在室温下,将50份丁香酚投入反应釜中,在30min内加入3份催化剂钠,催化剂加完后再反应30min,之后通入氮气保护,升温至95℃,通入300份环氧乙烷,反应压力为0.2MPa,反应4h;将反应釜降温至60℃,加入醋酸中和,再加入硅藻土过滤,制得丁香酚聚氧乙烯醚,平均聚合度为15。
S2、将S1制得的85份丁香酚聚氧乙烯醚与2份催化剂尿素在反应釜中混合,升温至100℃,加入10份氨基磺酸粉末,继续升温至120℃保温2h,降温得到丁香酚聚氧乙烯醚硫酸酯粗产品,加入无水乙醇溶解丁香酚聚氧乙烯醚硫酸酯粗产品后过滤,加入碱性溶液调节体系pH呈弱碱性,过滤不溶于无水乙醇的杂质,旋转蒸发除去乙醇,得到丁香酚聚氧乙烯醚硫酸酯。
S3、将24份四甲基环四硅氧烷、20份甲苯、0.1份Karsted催化剂加入反应釜中,通入氮气保护,升温至80℃,缓慢滴加440份S2制得的丁香酚聚氧乙烯醚硫酸酯,反应12h后旋转蒸发除去甲苯,得到淡黄色黏稠液体状的环四硅氧烷丁香酚聚氧乙烯醚硫酸酯。
实施例3
本实施例所述的基于丁香酚的阴离子匀染剂结构式如下:
其中n为20。
所述基于丁香酚的阴离子匀染剂合成方法如下:
S1、在室温下,将50份丁香酚投入反应釜中,在30min内加入3份催化剂钠,催化剂加完后再反应30min,之后通入氮气保护,升温至95℃,通入400份环氧乙烷,反应压力为0.2MPa,反应4h;将反应釜降温至60℃,加入醋酸中和,再加入硅藻土过滤,制得丁香酚聚氧乙烯醚,平均聚合度为20。
S2、将S1制得的100份丁香酚聚氧乙烯醚与2份催化剂尿素在反应釜中混合,升温至100℃,加入10份氨基磺酸粉末,继续升温至120℃保温2h,降温得到丁香酚聚氧乙烯醚硫酸酯粗产品,加入无水乙醇溶解丁香酚聚氧乙烯醚硫酸酯粗产品后过滤,加入碱性溶液调节体系pH呈弱碱性,过滤不溶于无水乙醇的杂质,旋转蒸发除去乙醇,得到丁香酚聚氧乙烯醚硫酸酯。
S3、将24份四甲基环四硅氧烷、20份甲苯、0.1份Karsted催化剂加入反应釜中,通入氮气保护,升温至80℃,缓慢滴加440份S2制得的丁香酚聚氧乙烯醚硫酸酯,反应12h后旋转蒸发除去甲苯,得到淡黄色黏稠液体状的环四硅氧烷丁香酚聚氧乙烯醚硫酸酯。
对上述实施例1~3制得的阴离子匀染剂环四硅氧烷丁香酚聚氧乙烯醚硫酸脂进行匀染效果测试,并选取常用的高温匀染剂A-840作为对比,在相同添加量(2.5g/L)条件下,所得染色效果测试数据如下表1。
表1实施例所合成的阴离子匀染剂与A-840型高温匀染剂染色效果测试数据
从上表中数据可以看出,本实施例所制得的阴离子匀染剂相比A-840型高温匀染剂,在分散染料方面具有相同级别的高温分散能力、更加优良的匀染性和移染率,染料利用率较高。
Claims (10)
1.一种基于丁香酚的阴离子匀染剂,其特征在于,所述阴离子匀染剂为环四硅氧烷丁香酚聚氧乙烯醚硫酸酯,包括如下结构:
其中n为10~20的整数。
2.一种如权利要求1所述基于丁香酚的阴离子匀染剂的合成方法,其特征在于,包括以下步骤:
S1、制备丁香酚聚氧乙烯醚:将丁香酚投入反应釜中,在室温下加入催化剂钠;加入催化剂钠后通入非反应气体保护,升温至95℃后加入环氧乙烷恒温反应一段时间,其中丁香酚和环氧乙烷的摩尔比为1:(4~8),得到丁香酚聚氧乙烯醚;
S2、制备丁香酚聚氧乙烯醚硫酸酯:将上述丁香酚聚氧乙烯醚与催化剂尿素混合,升温至100℃后加入氨基磺酸,其中丁香酚聚氧乙烯醚与氨基磺酸的摩尔比为(7~10):1,继续升温至120℃,恒温反应一段时间后停止加热,降温后得到丁香酚聚氧乙烯醚硫酸酯;
S3、制备环四硅氧烷丁香酚聚氧乙烯醚硫酸酯:将四甲基环四硅氧烷、甲苯、Karsted催化剂投入反应釜,通入非反应气体保护,升温至80℃后滴加丁香酚聚氧乙烯醚硫酸酯,其中四甲基环四硅氧烷和丁香酚聚氧乙烯醚硫酸酯的摩尔比为3:(25~55),恒温反应一段时间,得到环四硅氧烷丁香酚聚氧乙烯醚硫酸酯。
3.根据权利要求2所述的阴离子匀染剂合成方法,其特征在于:所述步骤S1具体为:
S11、在室温下,在反应器中加入丁香酚,向丁香酚内加入催化剂钠,反应30min;
S12、向反应器中通入非反应气体保护,升温至95℃后,向反应器中加入环氧乙烷,反应4h;
S13、降温至60℃,加入醋酸中和反应体系,加入硅藻土过滤,得到丁香酚聚氧乙烯醚。
4.根据权利要求3所述的阴离子匀染剂合成方法,其特征在于:所述步骤S11中,催化剂钠在30min内缓慢加入。
5.根据权利要求2所述的阴离子匀染剂合成方法,其特征在于:所述步骤S2具体为:
S21、将丁香酚聚氧乙烯醚与催化剂尿素混合,升温至100℃,加入氨基磺酸;
S22、将S21中反应体系升温至120℃持续2h,降温后得到丁香酚聚氧乙烯醚硫酸酯粗产品;
S23、加入无水乙醇溶解丁香酚聚氧乙烯醚硫酸酯粗产品,过滤后蒸发乙醇,得到丁香酚聚氧乙烯醚硫酸酯。
6.根据权利要求2所述的阴离子匀染剂合成方法,其特征在于:所述步骤S3具体为:
S31、将四甲基环四硅氧烷、甲苯、Karsted催化剂加入反应釜,通入非反应气体保护后,搅拌并升温至80℃,其中四甲基环四硅氧烷与甲苯的摩尔比为6:5;
S32、滴加丁香酚聚氧乙烯醚硫酸酯,恒温反应12h;
S33、蒸发甲苯,得到环四硅氧烷丁香酚聚氧乙烯醚硫酸酯。
7.根据权利要求2所述的阴离子匀染剂合成方法,其特征在于:所述非反应性气体为氮气、二氧化碳、氦气或氩气。
8.根据权利要求2所述的阴离子匀染剂合成方法,其特征在于:所述催化剂钠与丁香酚的摩尔比为3:50;所述催化剂尿素与丁香酚聚氧乙烯醚的摩尔比为1:(35~50);所述Karsted催化剂与丁香酚聚氧乙烯醚硫酸酯的摩尔比为1:(2000~4400)。
9.根据权利要求2所述的阴离子匀染剂合成方法,其特征在于:所述步骤S1中,反应釜中压力保持0.2MPa。
10.根据权利要求1所述的阴离子匀染剂在纺织工业或印刷工业领域的应用。
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