CN105693984B - 一种含酰亚胺环水性聚氨酯的制备方法 - Google Patents

一种含酰亚胺环水性聚氨酯的制备方法 Download PDF

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CN105693984B
CN105693984B CN201610114762.3A CN201610114762A CN105693984B CN 105693984 B CN105693984 B CN 105693984B CN 201610114762 A CN201610114762 A CN 201610114762A CN 105693984 B CN105693984 B CN 105693984B
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赵艳娜
姬定西
刘雅俊
张云飞
赵玉春
李娟�
赵瑶
任贝鸽
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Jiuer Xi'an Intellectual Property Service Co ltd
Shanghai Jingtan Chemical Co ltd
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Abstract

本发明公开了一种含酰亚胺环水性聚氨酯的制备方法，制备方法如下：将聚二醇16～22份加入到干燥的反应器中，加热使反应器中的聚二醇熔融后，再将二异氰酸酯10～12份加入到反应器中在80～90℃进行聚合反应，反应时间为2～3h；接着将羧酸盐型扩链剂1～4份和交联剂三羟甲基丙烷0～1份加入反应器中，在70～80℃反应2～3h；然后再将马来酰亚胺改性剂0.3～1.5份加入到反应器中反应1～2h；再向反应器中加入有机碱调解pH值为7.0～8.0；最后高速搅拌下加入温度为0～40℃的去离子水，直至得到固含量25％的淡黄色泛蓝光乳液A，即含酰亚胺环水性聚氨酯，本发明提高了产品的耐热性能。

Description

一种含酰亚胺环水性聚氨酯的制备方法
技术领域
本发明属于精细化学品及其制备技术领域，特别涉及一种含酰亚胺环水性聚氨酯乳液及其制备方法。
背景技术
有机耐高温胶黏剂种类很多，应用较广的主要有环氧树脂类、酚醛树脂类、有机硅类以及含氮杂环聚合物，但制备过程中使用一定量的有机溶剂，造成环境污染，近年来，环保型水性聚氨酯取代溶剂型聚氨酯是聚氨酯研究领域的发展趋势，与溶剂型聚氨酯相比，水性聚氨酯胶膜的的耐溶剂性、耐热性和力学性能都不太好，因此限制了它的大规模应用。
为了扩大水性聚氨酯的应用范围，普遍认为通过交联改性的方法能显著提高水性聚氨酯的耐溶剂性、耐热性和力学性能，分子链中含有酰亚胺环状结构的环链高聚物，具有优良的耐热老化性能和化学稳定性、耐溶剂性、热膨胀系数小以及优良的力学性能和电性能，人们试图通过引入热稳定性较好的杂环结构，对水性聚氨酯分子链进行改性以提高聚氨酯的热稳定性能。
双马来酰亚胺树脂由于含有苯环、酰亚胺环及交联密度较高，其固化物有较高的耐热性，其固化反应属于加成，N-(4-羟基苯基)马来酰亚胺改性水性聚氨酯主要是利用N-(4-羟基苯基)马来酰亚胺中苯环上的-OH和-NCO发生反应，将马来酰亚胺基团引入水性聚氨酯的分子链，可以解决水性聚氨酯胶黏剂耐热性能不足、固化速度较慢、交联密度小的缺点，扩大了其在胶粘剂、涂料等领域的应用，但单纯用马来酰亚胺改性聚氨酯也存在乳化困难，酰亚胺环的引入数量有限等缺点，难以推广应用。
发明内容
本发明的目的在于提供一种含酰亚胺环聚氨酯乳液及其制备方法，以克服现有技术存在的上述问题。
为克服现有技术存在的问题，本发明采用的技术方案是：一种含酰亚胺环水性聚氨酯的制备方法，包括以下步骤：按重量份数计，将聚二醇16～22份加入到干燥的反应器中，加热使反应器中的聚二醇熔融后，再将二异氰酸酯10～12份加入到反应器中在80～90℃进行聚合反应，反应时间为2～3h；接着将羧酸盐型扩链剂1～4份和交联剂三羟甲基丙烷0～1份加入反应器中，在70～80℃反应2～3h；然后再将马来酰亚胺改性剂0.3～1.5份加入到反应器中反应1～2h；再向反应器中加入有机碱调解pH值为7.0～8.0；最后高速搅拌下加入温度为0～40℃的去离子水，直至得到固含量25％的淡黄色泛蓝光乳液A，即含酰亚胺环水性聚氨酯。
所述聚二醇为聚醚二元醇或聚酯二元醇。
所述聚醚二元醇或聚酯二元醇的相对分子质量为500，700，750，1000或2000。
所述聚醚二元醇为聚氧化丙烯二元醇或聚四氢呋喃醚二元醇；聚酯二元醇为聚己内酯二元醇、聚碳酸酯二元醇或聚己二酸丁二醇酯二元醇。
所述二异氰酸酯为异佛尔酮二异氰酸酯、甲苯二异氰酸酯、六亚甲基二异氰酸酯和二苯基甲烷二异氰酸酯中一种或多种混合。
所述羧酸盐型扩链剂为二羟甲基丙酸或二羟甲基丁酸。
所述有机碱为三甲胺、三乙胺或三乙醇胺。
所述马来酰亚胺改性剂为N-(4-羟基苯基)马来酰亚胺。
与现有技术相比，本发明至少具有以下有益效果，通过引入需要量的酰亚胺基团，提高交联密度，聚氨酯的固化速度，耐水性，尤其是耐热性到改善；因马来酰亚胺类化合物多为结晶固体，有较高的熔点，熔体粘度较高，难溶于水，因此与水性聚氨酯复合，在乳化时存在乳化困难、固化时出现宏观相分离的缺点，本发明通过N-(4-羟基苯基)马来酰亚胺分子上的羟基与聚氨酯分子链反应，将马来酰亚胺基团分子水平引入聚氨酯分子链，所得改性水性聚氨酯兼具聚氨酯和马来酰亚胺树脂的优点，提高了产品的耐热性能。
具体实施方式
下面结合具体实施实例对本发明做进一步解释说明。
实施例一：
按重量份数计，将聚氧化丙烯二元醇(相对分子质量为1000)16份加入到干燥的反应器中，加热使反应器中的聚氧化丙烯二元醇熔融后，再将异佛尔酮二异氰酸酯和六亚甲基二异氰酸酯11.1份(异佛尔酮二异氰酸酯和六亚甲基二异氰酸酯摩尔比为1:1)加入到反应器中在80℃进行聚合反应2h；接着将扩链剂二羟甲基丙酸2份和交联剂三羟甲基丙烷0.54份加入反应器中；在70℃反应2.5h；然后再将N-(4-羟基苯基)马来酰亚胺0.3份加入到反应器中反应1.5h；然后，加入三甲胺调节pH值至7.5，高速搅拌下加入25℃的去离子水直至得质量分数(固含量)为25％淡黄色泛蓝光乳液A，即含酰亚胺环水性聚氨酯。
实施例二：
将聚四氢呋喃醚二元醇(相对分子质量为750)18.4份加入到干燥的反应器中，加热使反应器中聚四氢呋喃醚二元醇的熔融后，再将甲苯二异氰酸酯10份加入到反应器中在90℃进行聚合反应2.5h；接着将扩链剂二羟甲基丁酸1份加入反应器中，在75℃反应2h；然后再将N-(4-羟基苯基)马来酰亚胺0.42份加入到体系中反应1h；加入三乙胺调节pH值为7，高速搅拌下加入0℃去离子水得质量分数为25％淡黄色泛蓝光乳液A。
实施例三：
将聚己内酯二醇(相对分子质量为2000)22份加入到干燥的反应器中，加热使反应器中的聚己内酯二醇熔融后，再将六亚甲基二异氰酸酯12份加入到反应器中在85℃进行聚合反应3h；接着将扩链剂二羟甲基丙酸4份和交联剂三羟甲基丙烷1份加入反应器中，在70℃反应3h；然后再将N-(4-羟基苯基)马来酰亚胺0.62份加入到体系中反应2h；加入三乙醇胺调节pH值为8，高速搅拌下加入40℃去离子水直至得质量分数为25％淡黄色泛蓝光乳液A，即含酰亚胺环水性聚氨酯。
实施例四：
将聚碳酸酯二元醇(相对分子质量为500)17.5份加入到干燥的反应器中，加热使反应器中的聚碳酸酯二元醇熔融后，再将二苯基甲烷二异氰酸酯10.8份加入到反应器中在85℃进行聚合反应3h；接着将扩链剂二羟甲基丁酸3份和交联剂三羟甲基丙烷1份加入反应器中，在80℃反应2h；然后再将N-(4-羟基苯基)马来酰亚胺1.5份加入到体系中反应1h；加入三乙胺调节pH值为7.5，高速搅拌下加入30～40℃去离子水直至得质量分数为25％淡黄色泛蓝光乳液A，即含酰亚胺环水性聚氨酯。
实施例五：
将聚己二酸丁二醇酯二元醇(相对分子质量为700)20份加入到干燥的反应器中，加热使反应器中的聚己二酸丁二醇酯二元醇熔融后，再将异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯和二苯基甲烷二异氰酸酯11.5份(异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯和二苯基甲烷二异氰酸酯的摩尔比为1:2:1)加入到反应器中在80℃进行聚合反应2h；接着将扩链剂二羟甲基丙酸1份和交联剂三羟甲基丙烷0.5份加入反应器中，在80℃反应3h；然后再将N-(4-羟基苯基)马来酰亚胺1.2份加入到体系中反应2h；加入三甲胺调节pH值为7，高速搅拌下加入10℃去离子水直至得质量分数为25％淡黄色泛蓝光乳液A，即含酰亚胺环水性聚氨酯。

Claims (7)

1.一种含酰亚胺环水性聚氨酯的制备方法，其特征在于，包括以下步骤：按重量份数计，将聚二醇16～22份加入到干燥的反应器中，加热使反应器中的聚二醇熔融后，再将二异氰酸酯10～12份加入到反应器中在80～90℃进行聚合反应，反应时间为2～3h；接着将羧酸盐型扩链剂1～4份和交联剂三羟甲基丙烷0～1份加入反应器中，在70～80℃反应2～3h；然后再将马来酰亚胺改性剂0.3～1.5份加入到反应器中反应1～2h；再向反应器中加入有机碱调解pH值为7.0～8.0；最后高速搅拌下加入温度为0～40℃的去离子水，直至得到固含量25％的淡黄色泛蓝光乳液A，即含酰亚胺环水性聚氨酯；所述马来酰亚胺改性剂为N-(4-羟基苯基)马来酰亚胺。
2.如权利要求1所述含酰亚胺环水性聚氨酯的制备方法，其特征在于，所述聚二醇为聚醚二元醇或聚酯二元醇。
3.如权利要求2所述含酰亚胺环水性聚氨酯的制备方法，其特征在于，所述聚醚二元醇或聚酯二元醇的相对分子质量为500，700，750，1000或2000。
4.如权利要求2所述含酰亚胺环水性聚氨酯的制备方法，其特征在于，所述聚醚二元醇为聚氧化丙烯二元醇或聚四氢呋喃醚二元醇；聚酯二元醇为聚己内酯二元醇、聚碳酸酯二元醇或聚己二酸丁二醇酯二元醇。
5.如权利要求1所述含酰亚胺环水性聚氨酯的制备方法，其特征在于，所述二异氰酸酯为异佛尔酮二异氰酸酯、甲苯二异氰酸酯、六亚甲基二异氰酸酯和二苯基甲烷二异氰酸酯中一种或多种混合。
6.如权利要求1所述含酰亚胺环水性聚氨酯的制备方法，其特征在于，所述羧酸盐型扩链剂为二羟甲基丙酸或二羟甲基丁酸。
7.如权利要求1所述含酰亚胺环水性聚氨酯的制备方法，其特征在于，所述有机碱为三甲胺、三乙胺或三乙醇胺。
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