CN111647128A - 一种无醛纺织品固色剂的制备方法 - Google Patents
一种无醛纺织品固色剂的制备方法 Download PDFInfo
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- CN111647128A CN111647128A CN202010589262.1A CN202010589262A CN111647128A CN 111647128 A CN111647128 A CN 111647128A CN 202010589262 A CN202010589262 A CN 202010589262A CN 111647128 A CN111647128 A CN 111647128A
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
- C07F7/0872—Preparation and treatment thereof
- C07F7/0876—Reactions involving the formation of bonds to a Si atom of a Si-O-Si sequence other than a bond of the Si-O-Si linkage
- C07F7/0878—Si-C bond
- C07F7/0879—Hydrosilylation reactions
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Abstract
本发明涉及纺织助剂制备领域,本发明制备出了一种聚氨酯基无醛纺织品固色剂,并且在聚合过程中加入一种离子液改性硅烷到分子链段中,由于溶解度参数相差较大,硅氧烷与聚氨酯高分子链间存在一定的微相分离,导致硅较易集中在胶膜表面,从而使得改性后的聚氨酯胶膜耐水能力提高,最终使得高分子对染料的包裹增强,解决了水性聚氨酯材料作为织物固色剂,存在的织物耐水性差、干燥速率慢等缺陷;本发明的聚氨酯基无醛纺织品固色剂分子链中存在的软链端,可以赋予织物较好的手感,同时高分子链上的的异氰酸根可以与织物上及染料上的羟基、氨基等极性基团发生反应,形成高分子膜,从而可以改善织物的耐干/湿摩擦牢度性能,起到非常好的固色作用。
Description
技术领域
本发明涉及纺织助剂制备领域,尤其是一种无醛纺织品固色剂的制备方法。
背景技术
纺织工业是我国的传统产业,也是出口创汇、创利的重要产业,在国民经济发展中具有举足轻重的作用。为了达到色牢度要求,纺织品染色后通常需要进行固色处理。固色剂能提高染色过程中染料的固着率及湿处理牢度,对于提高产品质量,降低生产成本,减少污染十分重要。
CN103643566A公开了一种纺织品印染颜料固色剂,由如下组分组成:1~2质量份羟丙基甲基纤维素,120质量份去离子水,8~9质量份丙烯酸酯,4~6质量份聚吡咯烷酮,1~2质量份乙二醇单硬脂酸酯,5~7质量份2.2-偶氮二(2-甲基丙氧酸),1~2质量份环氧氯丙烷,7~8质量份有机硅氧烷,8~9质量份双氰胺。该发明纺织品印染颜料固色剂,其对染料染色后对纺织物具有很好的固色效果,且对织物的色光影响很小。
CN104878628A公开了一种纺织品印染固色剂,其由以下重量份数的原料制成:聚苹果酸3-6分,螯合剂12-18份,椰子油脂肪酸单乙醇酰胺4-6分,三乙醇胺1-4份,脂肪醇聚氧乙烯醚6-11份,双氰胺7-10份,丙烯酸酯4-6份,聚吡咯烷酮5-8份,六亚甲基四胺12-23份,羧甲基纤维素15-20份,甲苯11-16份,聚乙烯醚8-15份,氢氧化钾2-4份,甘油6-9份。该发明的有益效果是:该发明的纺织品印染固色剂,提高了染色牢度,提高了汗渍牢度,有效防止紫外线对染色结构的破坏,从而提高日晒牢度。
CN110699990A公开了一种纺织品印染颜料固色剂,以质量份计包括:羟丙基甲基纤维素20-30份,聚吡咯烷酮15-25份,乙二醇单硬脂酸酯30-50份,2.2-偶氮二(2-甲基丙氧酸)5-9份,有机硅氧烷8-12份,双氰胺10-15份。该发明提供的一种纺织品印染颜料固色剂,其对染料染色后对纺织物具有很好的固色效果,且对织物的色光影响很小。
以上发明以及现有专利所制备的固色剂含有游离甲醛,易导致皮肤发炎,甚至发生溃疡,因此,研制高色牢度的无醛固色剂势在必行。
发明内容
为了解决上述问题,本发明提供了一种无醛纺织品固色剂的制备方法。
一种无醛纺织品固色剂的制备方法 ,其主要方案如下:
按照质量份数,将80-160份的聚醚二元醇和35-60份的异佛尔酮二异氰酸酯加入到反应釜中,氮气保护下控温到75-90℃,然后加入0.01-0.5份的催化剂,保温反应1-4h,然后将3.8-10.6份的双羟甲基丙酸溶解到40-80份的N-甲基吡咯烷酮中,并加入到反应釜中,继续保温反应45-120min,然后加入5.2-8.8份的扩链剂,反应20-60min;完成后加入18-26份的离子液改性硅烷,控温55-75℃,反应40-90min;完成后降温到40-60℃,加入4.8-8.6份的三乙胺,保温反应30-45min,完成后加入500-600份的去离子水,快速搅拌3-6h,过滤后即可得到所述的无醛纺织品固色剂。
所述的一种离子液改性硅烷,按照以下方法制备:按照质量份数,将50-80份的二甲基二烯丙基氯化铵;20-30份的1,1,3,3-四甲基二硅氧烷;0.3-0.9份的1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐, 2-5份的2-丙烯酸铈盐,1-5份的浓度2-5%氯铂酸异丙醇溶液, 和180-300份的异丙醇中混合均匀,反应温度70-80℃,然后在氮气保护下反应3-6h,完成后加入过量碳酸钠中和,过滤后,90-110℃下减压蒸馏1-3h,即可得到所述的离子液改性硅烷。
其二甲基二烯丙基氯化铵, 1,1,3,3-四甲基二硅氧烷,1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐发生硅氢加成反应,2-丙烯酸铈盐也可以发生硅氢加成反应,其中二甲基二烯丙基氯化铵, 1,1,3,3-四甲基二硅氧烷,1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐反应机理示意为:
所述的聚醚二元醇为聚氧化丙烯-氧化乙烯二醇或聚四氢呋喃二元醇。
所述的聚醚二元醇的重均分子量为1000-3000。
所述的催化剂为二月桂酸二丁基锡或丙二酸二丁基锡或二醋酸二丁基锡。
所述的扩链剂为1,4-丁二醇或1,6-己二醇。
本发明的一种无醛纺织品固色剂的制备方法,本发明制备出了一种聚氨酯基无醛纺织品固色剂,并且在聚合过程中加入一种酸离子液改性硅烷到分子链段中,二甲基二烯丙基氯化铵, 1,1,3,3-四甲基二硅氧烷,1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐发生硅氢加成反应,2-丙烯酸铈盐也可以发生硅氢加成反应,得到的大分子离子液基硅烷,与异氰酸根相互作用,由于溶解度参数相差较大,硅氧烷与聚氨酯高分子链间存在一定的微相分离,导致硅较易集中在胶膜表面,从而使得改性后的聚氨酯胶膜耐水能力提高,最终使得高分子对染料的包裹增强,解决了水性聚氨酯材料作为织物固色剂,存在的织物耐水性差、干燥速率慢等缺陷;本发明的聚氨酯基无醛纺织品固色剂分子链中存在的软链端,可以赋予织物较好的手感,同时高分子链上的的异氰酸根可以与织物上及染料上的羟基、氨基等极性基团发生反应,形成三维高分子膜,从而可以改善织物的耐干/湿摩擦牢度性能,起到非常好的固色作用。
附图说明
图1为实施例1所制备的无醛纺织品固色剂产品的傅里叶红外光谱图:
在1120cm-1附近存在醚键的反对称伸缩吸收峰,在2927cm-1附近存在碳氢的伸缩吸收峰,说明聚醚二元醇参与了反应;在1664cm-1附近存在酰胺的羰基的伸缩吸收峰,在3390cm-1附近存在氮氢键的伸缩吸收峰,在1730cm-1附近存在酯羰基的伸缩吸收峰,说明异佛尔酮二异氰酸酯参与了反应;在1080/806cm-1附近存在硅氧的反对称/对称伸缩吸收峰,在731cm-1附近存在硅碳的伸缩吸收峰,在1256cm-1附近存在碳氟键的反对称伸缩吸收峰,说明离子液改性硅烷参与了反应;在1462/927cm-1附近存在羧基的羟基的面内/面外弯曲吸收峰,说明双羟甲基丙酸参与了反应;在962cm-1附近存在碳氮单键的吸收峰,说明三乙胺参与了反应。
具体实施方式
下面通过具体实施例对该发明作进一步说明:
将得到的固色剂制成20mm×20mm的胶膜,在真空环境中干燥24h,冷却至室温后称量,记录数据,将其浸入去离子水中24h,称量其质量,计算其胶膜吸水率,需测量三次求平均值。
固色性能测试:整理工艺采用二浸二轧法,在室温下将靛兰棉布浸入到乳液中,室温下浸泡25min,轧去多余的水分,之后再次重复操作一次,控制水量在80%-100%,放入烘箱,在60℃下烘干。织物的摩擦牢度测试:测试包括干摩擦牢度测试和湿摩擦牢度的测试,采取GB3920-2008进行测试。取长宽分别为140mm、50mm的布样,将其按照国标固定于耐磨擦牢度仪,纵向和径向分别测试干、湿摩擦,测试前需设置摩擦次数为10次,湿摩擦测试时需将摩擦布浸入蒸馏水,称重以确定摩擦布中的含水量达到95%~100%,最后取下测试布晾干与灰度比色卡比较,评定级别。
实施例1
一种无醛纺织品固色剂的制备方法,其主要方案如下:
将80g的聚醚二元醇和35g的异佛尔酮二异氰酸酯加入到反应釜中,氮气保护下控温到75℃,然后加入0.01g的催化剂,保温反应1h,然后将3.8g的双羟甲基丙酸溶解到40g的N-甲基吡咯烷酮中,并加入到反应釜中,继续保温反应45min,然后加入5.2g的扩链剂,反应20min;完成后加入18g的离子液改性硅烷,控温55℃,反应40min;完成后降温到40℃,加入4.8g的三乙胺,保温反应30min,完成后加入500g的去离子水,快速搅拌3-6h,过滤后即可得到所述的无醛纺织品固色剂。
所述的一种离子液改性硅烷,按照以下方法制备:将50g的二甲基二烯丙基氯化铵;20g的1,1,3,3-四甲基二硅氧烷;0.3g的1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐,2g的2-丙烯酸铈盐,1g的浓度2%氯铂酸异丙醇溶液, 和180g的异丙醇中混合均匀,反应温度70℃,然后在氮气保护下反应3h,完成后加入过量碳酸钠中和,过滤后,90℃下减压蒸馏1h,即可得到所述的离子液改性硅烷。
所述的聚醚二元醇为聚氧化丙烯-氧化乙烯二醇。
所述的聚醚二元醇的重均分子量为1000。
所述的催化剂为二月桂酸二丁基锡。
所述的扩链剂为1,4-丁二醇。
本实施例制备的聚氨酯胶膜的吸水率为3.57%,应用于布匹后其湿摩擦牢度为5级,干摩擦牢度为5级。
实施例2
一种无醛纺织品固色剂的制备方法 ,其主要方案如下:
将120g的聚醚二元醇和50g的异佛尔酮二异氰酸酯加入到反应釜中,氮气保护下控温到78℃,然后加入0.09g的催化剂,保温反应2h,然后将5.6g的双羟甲基丙酸溶解到50g的N-甲基吡咯烷酮中,并加入到反应釜中,继续保温反应85min,然后加入6.9g的扩链剂,反应40min;完成后加入22g的离子液改性硅烷,控温58℃,反应60min;完成后降温到50℃,加入6.2g的三乙胺,保温反应35min,完成后加入560g的去离子水,快速搅拌5h,过滤后即可得到所述的无醛纺织品固色剂。
所述的一种离子液改性硅烷,按照以下方法制备:将70g的二甲基二烯丙基氯化铵;25g的1,1,3,3-四甲基二硅氧烷;0.4g的1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐,4g的2-丙烯酸铈盐,3g的浓度3%氯铂酸异丙醇溶液, 和250g的异丙醇中混合均匀,反应温度76℃,然后在氮气保护下反应4h,完成后加入过量碳酸钠中和,过滤后,100℃下减压蒸馏1.2h,即可得到所述的离子液改性硅烷。
所述的聚醚二元醇为聚四氢呋喃二元醇。
所述的聚醚二元醇的重均分子量为2000。
所述的催化剂为丙二酸二丁基锡。
所述的扩链剂为1,6-己二醇。
本实施例制备的聚氨酯胶膜的吸水率为3.28%,应用于布匹后其湿摩擦牢度为5级,干摩擦牢度为5级。
实施例3
将160g的聚醚二元醇和60g的异佛尔酮二异氰酸酯加入到反应釜中,氮气保护下控温到90℃,然后加入0.5g的催化剂,保温反应4h,然后将10.6g的双羟甲基丙酸溶解到80g的N-甲基吡咯烷酮中,并加入到反应釜中,继续保温反应120min,然后加入8.8g的扩链剂,反应60min;完成后加入26g的离子液改性硅烷,控温75℃,反应90min;完成后降温到60℃,加入8.6g的三乙胺,保温反应45min,完成后加入600g的去离子水,快速搅拌6h,过滤后即可得到所述的无醛纺织品固色剂。
所述的一种离子液改性硅烷,按照以下方法制备:将80g的二甲基二烯丙基氯化铵;30g的1,1,3,3-四甲基二硅氧烷; 0.9g的1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐, 5g的2-丙烯酸铈盐,5g的浓度5%氯铂酸异丙醇溶液, 和300g的异丙醇中混合均匀,反应温度80℃,然后在氮气保护下反应6h,完成后加入过量碳酸钠中和,过滤后,110℃下减压蒸馏3h,即可得到所述的离子液改性硅烷。
所述的聚醚二元醇为聚氧化丙烯-氧化乙烯二醇。
所述的聚醚二元醇的重均分子量为3000。
所述的催化剂为二醋酸二丁基锡。
所述的扩链剂为1,6-己二醇。
本实施例制备的聚氨酯胶膜的吸水率为2.74%,应用于布匹后其湿摩擦牢度为5级,干摩擦牢度为5级。
对比例1
将160g的聚醚二元醇和60g的异佛尔酮二异氰酸酯加入到反应釜中,氮气保护下控温到90℃,然后加入0.5g的催化剂,保温反应4h,然后将10.6g的双羟甲基丙酸溶解到80g的N-甲基吡咯烷酮中,并加入到反应釜中,继续保温反应120min,然后加入8.8g的扩链剂,反应60min;加入8.6g的三乙胺,保温反应45min,完成后加入600g的去离子水,快速搅拌6h,过滤后即可得到所述的无醛纺织品固色剂。
所述的聚醚二元醇为聚氧化丙烯-氧化乙烯二醇。
所述的聚醚二元醇的重均分子量为3000。
所述的催化剂为二醋酸二丁基锡。
所述的扩链剂为1,6-己二醇。
本实施例制备的聚氨酯胶膜的吸水率为23.84%,应用于布匹后其湿摩擦牢度为2级,干摩擦牢度为3级。
对比例2
所述的一种离子液改性硅烷,按照以下方法制备:将80g的二甲基二烯丙基氯化铵;30g的1,1,3,3-四甲基二硅氧烷; 5g的2-丙烯酸铈盐, 5g的浓度5%氯铂酸异丙醇溶液, 和300g的异丙醇中混合均匀,反应温度80℃,然后在氮气保护下反应6h,完成后加入过量碳酸钠中和,过滤后,110℃下减压蒸馏3h,即可得到所述的离子液改性硅烷。
其它同实施例1;
本实施例制备的聚氨酯胶膜的吸水率为14.82%,应用于布匹后其湿摩擦牢度为3级,干摩擦牢度为4级。
对比例3
所述的一种离子液改性硅烷,按照以下方法制备:将30g的1,1,3,3-四甲基二硅氧烷;0.9g的1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐, 5g的2-丙烯酸铈盐,5g的浓度5%氯铂酸异丙醇溶液, 和300g的异丙醇中混合均匀,反应温度80℃,然后在氮气保护下反应6h,完成后加入过量碳酸钠中和,过滤后,110℃下减压蒸馏3h,即可得到所述的离子液改性硅烷。
其它同实施例1;
本实施例制备的聚氨酯胶膜的吸水率为8.51%,应用于布匹后其湿摩擦牢度为3级,干摩擦牢度为4级。
对比例4
所述的一种离子液改性硅烷,按照以下方法制备:将80g的二甲基二烯丙基氯化铵;30g的1,1,3,3-四甲基二硅氧烷; 0.9g的1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐,5g的浓度5%氯铂酸异丙醇溶液, 和300g的异丙醇中混合均匀,反应温度80℃,然后在氮气保护下反应6h,完成后加入过量碳酸钠中和,过滤后,110℃下减压蒸馏3h,即可得到所述的离子液改性硅烷。
本实施例制备的聚氨酯胶膜的吸水率为6.96%,应用于布匹后其湿摩擦牢度为4级,干摩擦牢度为4级。
Claims (6)
1.一种无醛纺织品固色剂的制备方法 ,其特征在于,其主要方案如下:
按照质量份数,将80-160份的聚醚二元醇和35-60份的异佛尔酮二异氰酸酯加入到反应釜中,氮气保护下控温到75-90℃,然后加入0.01-0.5份的催化剂,保温反应1-4h,然后将3.8-10.6份的双羟甲基丙酸溶解到40-80份的N-甲基吡咯烷酮中,并加入到反应釜中,继续保温反应45-120min,然后加入5.2-8.8份的扩链剂,反应20-60min;完成后加入18-26份的离子液改性硅烷,控温55-75℃,反应40-90min;完成后降温到40-60℃,加入4.8-8.6份的三乙胺,保温反应30-45min,完成后加入500-600份的去离子水,快速搅拌3-6h,过滤后即可得到所述的无醛纺织品固色剂。
2.根据权利要求1所述的一种无醛纺织品固色剂的制备方法,其特征在于,所述的离子液改性硅烷,按照以下方法制备:
所述的一种离子液改性硅烷,按照以下方法制备:按照质量份数,将50-80份的二甲基二烯丙基氯化铵;20-30份的1,1,3,3-四甲基二硅氧烷;0.3-0.9份的1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐, 2-5份的2-丙烯酸铈盐,1-5份的浓度2-5%氯铂酸异丙醇溶液, 和180-300份的异丙醇中混合均匀,反应温度70-80℃,然后在氮气保护下反应3-6h,完成后加入过量碳酸钠中和,过滤后,90-110℃下减压蒸馏1-3h,即可得到所述的离子液改性硅烷。
3.根据权利要求1所述的一种无醛纺织品固色剂的制备方法,其特征在于,所述的聚醚二元醇为聚氧化丙烯-氧化乙烯二醇或聚四氢呋喃二元醇。
4.根据权利要求1所述的一种无醛纺织品固色剂的制备方法,其特征在于,所述的聚醚二元醇的重均分子量为1000-3000。
5.根据权利要求1所述的一种无醛纺织品固色剂的制备方法,其特征在于,所述的催化剂为二月桂酸二丁基锡或丙二酸二丁基锡或二醋酸二丁基锡。
6.根据权利要求1所述的一种无醛纺织品固色剂的制备方法,其特征在于,所述的扩链剂为1,4-丁二醇或1,6-己二醇。
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