CN105199074A - 用于泡棉胶带的水性pu乳液的制备方法 - Google Patents

用于泡棉胶带的水性pu乳液的制备方法 Download PDF

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CN105199074A
CN105199074A CN201510724227.5A CN201510724227A CN105199074A CN 105199074 A CN105199074 A CN 105199074A CN 201510724227 A CN201510724227 A CN 201510724227A CN 105199074 A CN105199074 A CN 105199074A
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顾真贵
朱宏业
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SHANGHAI 3N CHEMICALS CO Ltd
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Abstract

本发明公开了一种用于泡棉胶带的水性PU乳液的制备方法，包括如下步骤：a)将大分子多元醇和多异氰酸酯混合反应，生成端基为多异氰酸根的预聚体；b)在所述预聚体中添加亲水性扩链剂进行第一次扩链，加入有机溶剂降低粘度形成聚氨酯树脂；c)以三乙胺中和树脂后，用相反转法将树脂高速分散在去离子水中；d)滴加小分子扩链剂进行第二次扩链反应后出料；e)脱除有机溶剂和部分去离子水，获得水性PU乳液。本发明利用异氰酸酯、多元醇和小分子扩链剂反应合成结晶性较好的聚氨酯树脂；并在分散过程中用小分子交联剂增加分子链的交联度，增加材料强度并改善耐水性；最后通过真空脱除提高乳液固含量，从而得到高固含量、高耐水性的水性PU乳液。

Description

用于泡棉胶带的水性PU乳液的制备方法
技术领域
本发明涉及一种涂料制备方法，尤其涉及一种用于泡棉胶带的水性PU乳液的制备方法。
背景技术
PU是英文polyurethane的缩写，化学中文名称“聚氨酯”。水性聚氨酯作为一种新型无有机溶剂的环保高分子产品，已经逐步在各种领域中取代油性聚氨酯，并随着科技的进步越来越快。水性聚氨酯真正实现了零VOC排放，无有毒气体危害，已经成为一种绿色材料。
泡棉胶带目前有PE、EVA等，但目前大部分材料力学性能都不能满足高档需求。由于PU材料力学性能优异可调节性强，因此在汽车、家居、建筑方面也应用广泛，但是目前泡棉胶带用水性PU存在耐水性差、固含量不高造成发泡时固化速度慢等问题。
发明内容
本发明所要解决的技术问题是提供一种用于泡棉胶带的水性PU乳液的制备方法，能够大大增加材料强度和耐水性，并提高PU乳液的固含量。
本发明为解决上述技术问题而采用的技术方案是提供一种用于泡棉胶带的水性PU乳液的制备方法，其中，包括如下步骤：a)将大分子多元醇和多异氰酸酯混合反应，生成端基为多异氰酸根的预聚体；b)在所述预聚体中添加亲水性扩链剂进行第一次扩链，添加有机溶剂降低粘度形成聚氨酯树脂；c)以三乙胺中和聚氨酯树脂后，用相反转法将树脂高速分散在去离子水中；d)滴加小分子扩链剂进行第二次扩链反应后出料；e)脱除有机溶剂和部分去离子水，获得水性PU乳液。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述步骤a)将大分子多元醇在80℃～110℃下真空脱水1小时后，与二异氰酸酯混合在50℃～90℃下反应3～6小时。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述大分子多元醇的分子量在500～6000之间。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述大分子多元醇为聚碳酸酯二醇、聚四氢呋喃二醇、聚己二酸乙二醇酯二醇、聚己二酸丁二醇酯二醇和聚氧化丙烯二醇中的一种或其多种的组合。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述二异氰酸酯为佛尔酮二异氰酸酯、甲基环己基二异氰酸酯、六亚甲基二异氰酸酯、二苯甲烷二异氰酸酯和二环己基二异氰酸酯中的一种或其多种的组合。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述步骤b)中第一次扩链反应时间为2～4小时，温度控制在40℃～80℃。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述亲水性扩链剂为二羟甲基丙酸和二羟甲基丁酸中的一种或其组合。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述步骤c)降温至30℃～60℃后加入三乙胺中和聚氨酯树脂。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述步骤c)的中和度介于70％～110％之间。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述小分子扩链剂为乙二醇、乙二胺、1,4-丁二醇、1,6-己二醇、异佛尔酮二胺、二乙烯三胺和三乙烯四胺的一种或其多种的组合。
上述的用于泡棉胶带的水性PU乳液的制备方法，其中，所述有机溶剂为丙酮、丁酮、N,N-二甲基甲酰胺、乙酸乙酯和醋酸丁酯中的一种或其多种的组合，所述有机溶剂的质量百分含量为树脂总质量的10～60％。
本发明对比现有技术有如下的有益效果：本发明提供的用于泡棉胶带的水性PU乳液的制备方法，利用不同结构异氰酸酯、多元醇和小分子扩链剂反应合成结晶性较好的聚氨酯树脂，增加树脂耐水性；同时在分散过程中用小分子交联剂增加分子链的交联度，增加材料强度同时也极大的改善了其耐水性；最后通过真空脱除方式提高乳液固含量，从而得到高固含量、高耐水性的水性PU乳液。
具体实施方式
下面结合实施例对本发明作进一步的描述。
本发明提供的用于泡棉胶带的水性PU乳液的制备方法包括如下步骤：
a)将大分子多元醇和多异氰酸酯混合反应，生成端基为多异氰酸根的预聚体；优先将大分子多元醇在80℃～110℃下真空脱水1小时后，与二异氰酸酯混合在50℃～90℃下反应3～6小时。较佳地，所述大分子多元醇的分子量在500～6000之间，所述大分子多元醇可以为聚碳酸酯二醇、聚四氢呋喃二醇、聚己二酸乙二醇酯二醇、聚己二酸丁二醇酯二醇和聚氧化丙烯二醇中的一种或其多种任意比例的组合；所述二异氰酸酯可以为佛尔酮二异氰酸酯、甲基环己基二异氰酸酯、六亚甲基二异氰酸酯、二苯甲烷二异氰酸酯和二环己基二异氰酸酯中的一种或其多种任意比例的组合。
b)在预聚体中添加亲水性扩链剂进行第一次扩链，添加有机溶剂降低粘度形成聚氨酯树脂；第一次扩链反应时间优选为2～4小时，温度控制在40℃～80℃；所述亲水性扩链剂可以为二羟甲基丙酸和二羟甲基丁酸中的一种或其组合。所述有机溶剂可以为丙酮、丁酮、N,N-二甲基甲酰胺、乙酸乙酯和醋酸丁酯中的一种或其多种任意比例的组合，所述有机溶剂的质量百分含量优选为树脂总质量的10～60％。
c)以三乙胺中和聚氨酯树脂后，用相反转法将树脂高速分散在去离子水中；优选降温至30℃～60℃后加入三乙胺中和聚氨酯树脂；中和度优选范围介于70％～110％之间。
d)滴加小分子扩链剂进行第二次扩链反应后出料；所述小分子扩链剂为乙二醇、乙二胺、1,4-丁二醇、1,6-己二醇、异佛尔酮二胺、二乙烯三胺和三乙烯四胺的一种或其多种任意比例的组合。
e)真空脱除有机溶剂和部分去离子水，获得水性PU乳液。
实施例1
将平均分子量2000的聚碳酸酯二醇60g，分子量2000的聚环氧丙烯二醇20g，分子量2000的聚四氢呋喃二醇20g投入三口烧瓶中，在80℃～110℃真空脱水1h后，降温至50℃～90℃加入二苯甲烷二异氰酸酯26.94g搅拌反应3～6h，降温至40℃～80℃加入二羟甲基丙酸3.9g搅拌反应2～4h，加入45g丙酮稀释，然后降温至30℃～60℃加三乙胺2.93g中和后出料。将树脂高速分散于130g去离子水中，抽真空脱除丙酮后获得水性PU乳液。
实施例2
将平均分子量2000的聚碳酸酯二醇50g，分子量2000的聚己二酸己二醇50g投入三口烧瓶中，在80℃～110℃真空脱水1h后，降温至50℃～90℃加入二苯甲烷二异氰酸酯24.13g搅拌反应3～6h，降温至40℃～80℃加入二羟甲基丙酸3.25g搅拌反应2～4h，加入45g丙酮稀释，然后降温至30℃～60℃加三乙胺2.45g中和后出料。将树脂高速分散于130g去离子水中，抽真空脱除丙酮后获得水性PU乳液。
本发明针对聚氨酯树脂分子设计的多样性来改进材料性能，解决了目前单组份水性PU的耐水性较差问题，同时也提高了固含量增加固化速度，可以广泛应用于汽车、家居、建筑等方面的泡棉胶带，改善和提高其在使用环境中的性能。本发明的水性PU乳液经过成膜后，在22℃～25℃去离子水环境下，吸水率可低至1.02％；同样温度范围内10％NAOH水溶液环境下，浸泡24h不发白不起泡；机械打泡后，1mm泡层125℃下15min内固化完全。
虽然本发明已以较佳实施例揭示如上，然其并非用以限定本发明，任何本领域技术人员，在不脱离本发明的精神和范围内，当可作些许的修改和完善，因此本发明的保护范围当以权利要求书所界定的为准。

Claims (11)

1.一种用于泡棉胶带的水性PU乳液的制备方法，其特征在于，包括如下步骤：
a)将大分子多元醇和多异氰酸酯混合反应，生成端基为多异氰酸根的预聚体；
b)在所述预聚体中添加亲水性扩链剂进行第一次扩链，加入有机溶剂降低粘度形成聚氨酯树脂；
c)以三乙胺中和聚氨酯树脂后，用相反转法将聚氨酯树脂高速分散在去离子水中；
d)滴加小分子扩链剂进行第二次扩链反应后出料；
e)脱除有机溶剂和部分去离子水，获得水性PU乳液。
2.如权利要求1所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述步骤a)将大分子多元醇在80℃～110℃下真空脱水1小时后，与二异氰酸酯混合在50℃～90℃下反应3～6小时。
3.如权利要求1所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述大分子多元醇的分子量在500～6000之间。
4.如权利要求3所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述大分子多元醇为聚碳酸酯二醇、聚四氢呋喃二醇、聚己二酸乙二醇酯二醇、聚己二酸丁二醇酯二醇和聚氧化丙烯二醇中的一种或其多种的组合。
5.如权利要求3所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述二异氰酸酯为佛尔酮二异氰酸酯、甲基环己基二异氰酸酯、六亚甲基二异氰酸酯、二苯甲烷二异氰酸酯和二环己基二异氰酸酯中的一种或其多种的组合。
6.如权利要求1所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述步骤b)中第一次扩链反应时间为2～4小时，温度控制在40℃～80℃。
7.如权利要求1所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述亲水性扩链剂为二羟甲基丙酸和二羟甲基丁酸中的一种或其组合。
8.如权利要求1所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述步骤c)降温至30℃～60℃后加入三乙胺中和聚氨酯树脂。
9.如权利要求8所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述步骤c)的中和度介于70％～110％之间。
10.如权利要求1所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述小分子扩链剂为乙二醇、乙二胺、1,4-丁二醇、1,6-己二醇、异佛尔酮二胺、二乙烯三胺和三乙烯四胺中的一种或其多种的组合。
11.如权利要求1所述的用于泡棉胶带的水性PU乳液的制备方法，其特征在于，所述有机溶剂为丙酮、丁酮、N,N-二甲基甲酰胺、乙酸乙酯和醋酸丁酯中的一种或其多种的组合，所述有机溶剂的质量百分含量为树脂总质量的10～60％。
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CN1740206A (zh) * 2005-09-22 2006-03-01 上海市合成树脂研究所 一种水性聚氨酯乳液的制备方法
CN1847277A (zh) * 2006-05-08 2006-10-18 北京科聚化工新材料有限公司 一种阴离子自乳化水性聚氨酯乳液及其制备方法
CN101724135A (zh) * 2008-10-28 2010-06-09 北京高盟化工有限公司 一种水性聚氨酯分散体的制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1740206A (zh) * 2005-09-22 2006-03-01 上海市合成树脂研究所 一种水性聚氨酯乳液的制备方法
CN1847277A (zh) * 2006-05-08 2006-10-18 北京科聚化工新材料有限公司 一种阴离子自乳化水性聚氨酯乳液及其制备方法
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