CN103923297A - 一种用于增韧淀粉浆膜的水性聚氨酯及其制备方法和应用 - Google Patents

一种用于增韧淀粉浆膜的水性聚氨酯及其制备方法和应用 Download PDF

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CN103923297A
CN103923297A CN201410155901.8A CN201410155901A CN103923297A CN 103923297 A CN103923297 A CN 103923297A CN 201410155901 A CN201410155901 A CN 201410155901A CN 103923297 A CN103923297 A CN 103923297A
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田培善
林源杰
吕福菊
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West (wuxi) Biotechnology Co Ltd
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Abstract

本发明涉及化学领域，公开了一种用于增韧淀粉浆膜的水性聚氨酯及其制备方法和应用。第一步，将二异氰酸酯、聚丙二醇在60-80℃下反应1-2小时；第二步，加入催化剂二桂酸二丁基锡和亲水单体在60-80℃下反应1-2小时；第三步，加入小分子扩链剂在60-80℃下进行扩链反应1-3小时；第四步，加入去离子水搅拌20-60分钟，然后自然降温至30-40℃，加入三乙胺反应20-50分钟。所述的各原料重量为：二异氰酸酯175-180份、聚丙二醇300-400份、亲水单体25-40份、小分子扩链剂24-35份、丙酮20-25份、三乙胺30-40份、去离子水1375-1425份、二桂酸二丁基锡1份。本方法获得的水性聚氨酯能有效解决淀粉浆料上浆成膜后，浆膜硬脆、容易龟裂脱落的技术问题。

Description

一种用于增韧淀粉浆膜的水性聚氨酯及其制备方法和应用
技术领域
本发明涉及化学领域，具体为一种用于增韧淀粉浆膜的水性聚氨酯及其制备方法和应用。 
背景技术
在纺织领域，浆纱是经纱准备工程的重要工序。浆纱可以赋予经纱抵御复杂机械外力作用的能力，提高经纱的可织性，保证织造过程顺利进行。在浆纱过程中，一部分浆液留在经纱的表面，当被烘干之后，便在经纱表面形成浆膜。浆膜可以在织造过程中抵抗外部机械作用对纱体的磨损，起到保护纱体的作用。 
淀粉浆料是目前用于浆纱的主流浆料之一，淀粉用于经纱上浆有着其他浆料难以取代的优势，它的资源丰富、价格低廉、环境污染性低，因而早已在纺织经纱上浆中广为应用。但由于淀粉高分子重复单元为葡萄糖环状结构，分子之间由于强烈的氢键作用使淀粉浆成膜后表现出硬脆性，浆膜容易龟裂脱落，不仅破坏了原有表面浆膜的完整性，降低了经纱的耐磨性，还会产生大量的二次毛羽，使相邻经纱的毛羽互相纠缠，造成经纱开口不清和断头，严重影响了织机效率。 
发明内容
鉴于以上所述现有技术的缺点，本发明的目的在于提供一种用于增韧淀粉浆膜的水性聚氨酯制备方法及所得到增韧淀粉浆膜的水性聚氨酯，用于解决上述淀粉浆料上浆成膜后出现浆膜硬脆性，容易龟裂脱落的技术问题。 
制备方法包括以下步骤： 
（1）将二异氰酸酯、聚丙二醇在60-80℃下反应1-2小时； 
（2）加入催化剂二月桂酸二丁基锡和亲水单体在60-80℃下反应1-2小时； 
（3）加入小分子扩链剂与丙酮的混合溶液，在60-80℃下进行扩链反应1-3小时； 
（4）加入去离子水搅拌20-60分钟，自然降温至30-40℃，加入三乙胺反应20-50分钟； 
（5）减压蒸馏去除有丙酮。 
所述的各原料重量为：二异氰酸酯175-180份、聚丙二醇300-400份、亲水单体25-40份、小分子扩链剂24-35份、丙酮20-25份、三乙胺30-40份、去离子水1375-1425份、二桂酸二丁基锡1份。 
优选的，二异氰酸酯为六亚甲基二异氰酸酯或甲苯二异氰酸酯。。 
优选的，亲水单体在80℃的真空箱中脱水1-2小时。 
优选的，亲水单体为二羟甲基丙酸或二羟甲基丁酸。 
优选的，小分子扩链剂用4A分子筛进行浸泡2-7天。 
优选的，小分子扩链剂包括：碳原子为2～4的二醇、碳原子为2～4的二胺、碳原子为2～4的醇胺、碳原子为2～4的巯醇、碳原子为2～4的巯胺中的任一种。 
优选的，小分子扩链剂为乙二胺、丁二醇或乙醇胺中的任一种。 
优选的，搅拌速度为40-60rpm。 
通过上述方法制备的用于增韧淀粉浆膜的水性聚氨酯，PH值为7.0-8.0，粘度为1.0-1.4mPa.S，可应用于淀粉浆膜的改性，增强浆膜韧性。 
本发明提供了一种用于增韧淀粉浆膜的水性聚氨酯的制备方法，反应体系中的甲苯二异氰酸酯使得水性聚氨酯分子链中含有苯环，提高了水性聚氨酯的刚性；反应体系中的聚丙二醇使得水性聚氨酯具有较好的柔顺性，刚柔链段交替嵌段增强了供水性聚氨酯弹性。同时在反应体系中选用了含有羧基和磺酸基的氨基酸或二羟甲基丙酸作为亲水性单体使用，有利于合成的水性聚氨酯的生物降解性和抗离子性。 
具体实施方式
实施例1 
在装有搅拌器、回流冷凝管、温度计和氮气导管的500mL四口烧瓶中，加入35g的六亚甲基二异氰酸酯、80g的聚丙二醇，混合均匀后升温至70℃，反应2h后，加入0.2g催化剂二桂酸二丁基锡和5g亲水单体二羟甲基丙酸继续反应1h得到预聚体后，通过滴液漏斗缓慢滴入7g小分子扩链剂1,4-丁二醇与4g丙酮的混合溶液，控制滴加速度，使之2h滴加完成，然后加入275ml的去离子水搅拌50min，当反应体系温度达到40℃再加入6g三乙胺进行中和反应20min，最后减压蒸馏去除有机溶剂。 
准确称取200g的酸解淀粉与水性聚氨酯的混合浆料（水性聚氨酯占总质量3%），配制成6%的混合浆液，移入500ml的三口烧瓶中，三口烧瓶上装有机械搅拌器，冷凝器和温度计，将烧瓶置于水浴中开始升温，瓶内温度达到95℃后保温1h，然后浇注成膜。将干燥成型后的浆膜裁成所需尺寸在相对湿度65%、20℃的条件下平衡24h。测得浆膜数据如下： 
注：Q为断裂强度；CV为变异系数；ε为断裂伸长率；W为断裂功 
实施例2 
在装有搅拌器、回流冷凝管、温度计和氮气导管的500mL四口烧瓶中，加入36的甲苯二异氰酸酯、60g的聚丙二醇，混合均匀后升温至70℃，反应2h后，加入0.2g催化剂二桂酸二丁基锡和8g亲水单体二羟甲基丙酸继续反应1h得到预聚体后，降低反应体系温度到65℃，通过滴液漏斗缓慢滴入的4.8g小分子扩链剂乙二胺和5g丙酮的混合溶液，控制滴加速度，使之2h滴加完成，然后加入285ml的去离子水搅拌30min，当反应体系温度再降至40℃再加入8g的三乙胺反应30min。最后减压蒸馏去除有机溶剂。 
准确称取200g的酸解淀粉与水性聚氨酯的混合浆料（水性聚氨酯占总质量3%），配制成6%的混合浆液，移入500ml的三口烧瓶中，三口烧瓶上装有机械搅拌器，冷凝器和温度计，将烧瓶置于水浴中开始升温，瓶内温度达到95℃后保温1h，然后浇注成膜。将干燥成型后的浆膜（一般为48h）裁成所需尺寸在相对湿度65%、20℃的条件下平衡24h。测得浆膜数据如下： 
注：Q为断裂强度；CV为变异系数；ε为断裂伸长率；W为断裂功。 

Claims (10)

1.一种用于增韧淀粉浆膜的水性聚氨酯的制备方法，其特征在于，包括如下步骤：
（1）将二异氰酸酯、聚丙二醇在60-80℃下反应1-2小时；
（2）加入催化剂二桂酸二丁基锡和亲水单体在60-80℃下反应1-2小时；
（3）加入小分子扩链剂与丙酮的混合溶液，在60-80℃下进行扩链反应1-3小时；
（4）加入去离子水搅拌20-60分钟，自然降温至30-40℃，加入三乙胺反应20-50分钟；
（5）减压蒸馏去除有丙酮。
所述的各原料重量为：二异氰酸酯175-180份、聚丙二醇300-400份、亲水单体25-40份、小分子扩链剂24-35份、丙酮20-25份、三乙胺30-40份、去离子水1375-1425份、二桂酸二丁基锡1份。
2.根据权利要求1所述的水性聚氨酯的制备方法，其特征在于，所述二异氰酸酯为六亚甲基二异氰酸酯或甲苯二异氰酸酯。
3.根据权利要求1所述的水性聚氨酯的制备方法，其特征在于，所述亲水单体在80℃的真空箱中脱水1-2小时。
4.根据权利要求1或3所述的水性聚氨酯的制备方法，其特征在于，所述亲水单体为二羟甲基丙酸或二羟甲基丁酸。
5.根据权利要求1所述的水性聚氨酯的制备方法，其特征在于，所述小分子扩链剂用4A分子筛进行浸泡2-7天。
6.根据权利要求1或5所述的水性聚氨酯的制备方法，其特征在于，所述小分子扩链剂包括：碳原子为2～4的二醇、碳原子为2～4的二胺、碳原子为2～4的醇胺、碳原子为2～4的巯醇、碳原子为2～4的巯胺中的任一种。
7.根据权利要求6所述的水性聚氨酯的制备方法，其特征在于，所述小分子扩链剂为乙二胺、丁二醇或乙醇胺中的任一种。
8.根据权利要求1所述的水性聚氨酯的制备方法，其特征在于，步骤（4）中所述搅拌速度为40-60rpm。
9.一种用于增韧淀粉浆膜的水性聚氨酯，其特征在于，通过权利要求1-8任一项所述的方法制备，PH值为7.0-8.0，粘度为1.0-1.4mPa.S。
10.权利要求9所述水性聚氨酯应用于淀粉浆膜的改性。
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CN111333815A (zh) * 2020-03-30 2020-06-26 杭州鹿扬科技有限公司 兼具生物粘合剂和生物可降解成分的材料、制备方法及其用途

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