CN107417874A - 一种封端型双组份无溶剂防水透湿聚氨酯树脂及其制备方法 - Google Patents

一种封端型双组份无溶剂防水透湿聚氨酯树脂及其制备方法 Download PDF

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CN107417874A
CN107417874A CN201710651354.6A CN201710651354A CN107417874A CN 107417874 A CN107417874 A CN 107417874A CN 201710651354 A CN201710651354 A CN 201710651354A CN 107417874 A CN107417874 A CN 107417874A
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贝文理
钱伟伟
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ZHEJIANG JOYA POLYMER TECHNOLOGY Co Ltd
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Abstract

本发明涉及聚氨酯树脂制备技术领域，特别涉及一种防水透湿聚氨酯树脂及其制备方法。本发明的一种封端型双组份无溶剂防水透湿聚氨酯树脂，由A、B两种组分组成，组分A由甲苯异氰酸酯、4,4‑二苯基甲烷二异氰酸酯、抗氧化剂、新戊二醇聚酯多元醇、聚四氢呋喃多元醇、聚氧化乙烯多元醇、有机铋催化剂、丁酮肟反应制得；组分B为二乙烯三胺和异佛尔酮二胺的混合物，其中二乙烯三胺的重量百分比为40％‑70％；A、B两种组分的重量比为1:(0.05‑0.1)。本发明的防水透湿聚氨酯树脂保存时间长、成品性能稳定，并且具有优良透湿性、耐水压和耐水洗性能。

Description

一种封端型双组份无溶剂防水透湿聚氨酯树脂及其制备方法
技术领域
本发明涉及聚氨酯树脂制备技术领域，特别涉及一种防水透湿聚氨酯树脂及其制备方法。
背景技术
防水透湿布料是一种能防雨水穿透又能将汗液蒸气排出的布料，外套内并不会发生结露而导致湿冷不舒服现象。透湿性是指在剧烈运动时身体释放的蒸气会藉由体表挥发至外部而达到降温的效果及维持绝佳的舒适与干爽；防水性是指布料具有完全抵挡水分穿透的能力。这类防水透湿布料通常是在布料表面以PU、铁氟龙薄膜(PTFE)、TPU、TPE…等材料涂布或以film贴合加工而成。
目前对于防水透湿型聚氨酯织物及聚氨酯树脂的研究较多。以聚氨酯为原料的薄膜及涂层可巧妙地兼具防水和透气性这两个功能，并且保持其原有的优异性能。聚氨酯树脂一般由多异氰酸酯、多元醇以及小分子扩链剂(如水、小分子多元醇、多元胺)等为原料合成，具有独特的嵌段分子结构，可通过调节聚氨酯软硬段的成分比例改变其弹性、硬度、亲水性等，根据需要设计出性能各异的产品，其制品具有无可比拟的特性，如：独特的粘结性、润湿性、柔韧性、耐磨性、光泽性等。无溶剂防水透湿聚氨酯树脂具有安全、健康、环保、节能、高效以及低成本等诸多优势，广泛应用于防水透湿布料上。有专利报道过无溶剂双组份防水透湿组份聚氨酯树脂，其组成是带异氰酸酯聚合物的组份和带羟基的聚合物组份，通过配比混合反应制得无溶剂双组份防水透湿聚氨酯树脂膜，但其弊端是混合物保存时间短，成品性能不稳定，特别是高温天气。
发明内容
本发明的目的在于克服现有技术的不足，提供一种保存时间长、成品性能稳定，并且具有优良透湿性、耐水压和耐水洗性能的封端型双组份无溶剂防水透湿聚氨酯树脂。
为了达到上述目的，本发明的一种封端型双组份无溶剂防水透湿聚氨酯树脂，由A、B两种组分组成，组分A按重量份计由60-80份甲苯异氰酸酯、90-120份4,4-二苯基甲烷二异氰酸酯、0.1-0.2份抗氧化剂、100-300份新戊二醇聚酯多元醇、100-300份聚四氢呋喃多元醇、300-900份聚氧化乙烯多元醇、0.1-0.3份有机铋催化剂、60-80份丁酮肟反应制得；组分B为二乙烯三胺和异佛尔酮二胺的混合物，其中二乙烯三胺的重量百分比为40％-70％；A、B两种组分的重量比为1:(0.05-0.1)。
作为优选，所述新戊二醇聚酯多元醇的分子量为1500-3000。
作为优选，所述聚四氢呋喃多元醇的分子量为1500-3000。
作为优选，所述聚氧化乙烯多元醇的分子量为1500-3000。
本发明的另一目的是提供一种上述封端型双组份无溶剂防水透湿聚氨酯树脂的制备方法，包括如下步骤：
(1)组分A的制备：将计量的甲苯异氰酸酯、4,4-二苯基甲烷二异氰酸酯、抗氧化剂投入反应釜中在40℃-50℃下搅拌均匀，依次投入新戊二醇聚酯多元醇在60-70℃下反应2h-3h、投入聚四氢呋喃多元醇在60-70℃下反应2h-3h、投入聚氧化乙烯多元醇在60-70℃下反应4h-6h，然后在60-70℃下反应至残留NCO到达理论值，依次加入丁酮肟、有机铋催化剂，最后在70-80℃下反应至无残留NCO，反应结束出料。
(2)组分B的制备：将计量的二乙烯三胺和异佛尔酮二胺混合均匀即可。
(3)将A、B组分按照比例在20-40℃下混合均匀，脱泡，得产物。
本发明通过合成防水透湿聚合物预聚体，采用丁酮肟封端形成A组份；再采用反应活性高的二乙烯三胺和异佛尔酮二胺作为B组份；A、B组分在常温下混合即可，常温混合后保存时间长而稳定，涂层使用时需要在130℃-150℃高温下解封反应形成防水透湿高分子聚合物。
在组分A的合成中采用聚四氢呋喃多元醇和新戊二醇聚酯多元醇，主要提供树脂优异的耐水解性能，采用聚氧化乙烯聚醚多元醇提供树脂优异的透湿性，通过限定多元醇的分子量可进一步提高树脂的透湿度和耐水洗性；组分B采用二乙烯三胺和异佛尔酮二胺的混合物作为固化剂，交联强度高，可提供树脂优异的物性、耐水压和粘结性。同时，本发明的制备工艺简单，无溶剂环保，混合物储存稳定，可长时间保存，特别是高温天气。本发明的防水透湿聚氨酯树脂透湿度高、耐水压高、耐水洗优异，可作为涂层中的底料，即胶黏剂，适用在直涂工艺，布料上直涂底料即该胶黏剂，再涂覆一层防水透湿面料。胶黏剂成膜后就具备防水透湿性能，其涂覆在布料上后成品也具有防水透湿性能。
具体实施方式
实施例1：
(1)组分A的制备：按重量份计，将60份甲苯异氰酸酯(TDI-80)、90份4,4-二苯基甲烷二异氰酸酯MDI、抗氧化剂0.1份在40℃下投入反应釜内搅拌均匀，将140份分子量为2000的新戊二醇聚酯多元醇投入反应釜中在60-70℃下反应2小时，再将100份分子量为1500的聚四氢呋喃多元醇投入反应釜中在60-70℃下反应2小时，然后将300份分子量为2000的聚氧化乙烯多元醇投入反应釜中在60-70℃下反应4小时，反应至残留NCO到达理论值后加入65份丁酮肟和0.1份有机铋催化剂在70-80℃下反应至无残留NCO后出料。(2)组分B的制备：按重量份计，将40份二乙烯三胺和60份异佛尔酮二胺混合均匀。(3)将组分A与组分B按1:0.05的比例混合，脱泡，得产物。
实施例2：
(1)组分A的制备：按重量份计，将70份甲苯异氰酸酯(TDI-80)、85份4,4-二苯基甲烷二异氰酸酯MDI、抗氧化剂0.15份在45℃下投入反应釜内搅拌均匀，将110份分子量为1500的新戊二醇聚酯多元醇投入反应釜中在60-70℃下反应2.5小时，再将150份分子量为2000的聚四氢呋喃多元醇投入反应釜中在60-70℃下反应2.5小时，然后将380份分子量为2500的聚氧化乙烯多元醇投入反应釜中在60-70℃下反应5小时，反应至残留NCO到达理论值后加入70份丁酮肟和0.12份有机铋催化剂在70-80℃下反应至无残留NCO后出料。(2)组分B的制备：按重量份计，将60份二乙烯三胺和40份异佛尔酮二胺混合均匀。(3)将组分A与组分B按1:0.08的比例混合，脱泡，得产物。
实施例3：
(1)组分A的制备：按重量份计，将80份甲苯异氰酸酯(TDI-80)、90份4,4-二苯基甲烷二异氰酸酯MDI、抗氧化剂0.2份在50℃下投入反应釜内搅拌均匀，将250份分子量为3000的新戊二醇聚酯多元醇投入反应釜中在60-70℃下反应3小时，再将300份分子量为3000的聚四氢呋喃多元醇投入反应釜中在60-70℃下反应3小时，然后将900份分子量为3000的聚氧化乙烯多元醇投入反应釜中在60-70℃下反应6小时，反应至残留NCO到达理论值后加入80份丁酮肟和0.3份有机铋催化剂在70-80℃下反应至无残留NCO后出料。(2)组分B的制备：按重量份计，将70份二乙烯三胺和30份异佛尔酮二胺混合均匀。(3)将组分A与组分B按1:0.1的比例混合，脱泡，得产物。
对比试验例：
测试方法如下：透湿度测试标准：ASTM E96-2000材料的水蒸气渗透性标准试验方法；耐水压测试标准：ISO 811-1981纺织织物抗渗水性的测定静水压试验；耐水洗测试方法：40℃水温下加入20g洗衣粉洗一小时，水洗五次。

Claims (8)

1.一种封端型双组份无溶剂防水透湿聚氨酯树脂，其特征在于：由A、B两种组分组成，组分A按重量份计由60-80份甲苯异氰酸酯、90-120份4,4-二苯基甲烷二异氰酸酯、0.1-0.2份抗氧化剂、100-300份新戊二醇聚酯多元醇、100-300份聚四氢呋喃多元醇、300-900份聚氧化乙烯多元醇、0.1-0.3份有机铋催化剂、60-80份丁酮肟反应制得；组分B为二乙烯三胺和异佛尔酮二胺的混合物，其中二乙烯三胺的重量百分比为40％-70％；A、B两种组分的重量比为1:(0.05-0.1)。
2.根据权利要求1所述的一种封端型双组份无溶剂防水透湿聚氨酯树脂，其特征在于：所述新戊二醇聚酯多元醇的分子量为1500-3000。
3.根据权利要求1所述的一种封端型双组份无溶剂防水透湿聚氨酯树脂，其特征在于：所述聚四氢呋喃多元醇的分子量为1500-3000。
4.根据权利要求1所述的一种封端型双组份无溶剂防水透湿聚氨酯树脂，其特征在于：所述聚氧化乙烯多元醇的分子量为1500-3000。
5.一种制备权利要求1所述封端型双组份无溶剂防水透湿聚氨酯树脂的方法，，其特征在于：
(1)组分A的制备：将计量的甲苯异氰酸酯、4,4-二苯基甲烷二异氰酸酯、抗氧化剂投入反应釜中在40℃-50℃下搅拌均匀，依次投入新戊二醇聚酯多元醇在60-70℃下反应2h-3h、投入聚四氢呋喃多元醇在60-70℃下反应2h-3h、投入聚氧化乙烯多元醇在60-70℃下反应4h-6h，然后在60-70℃下反应至残留NCO到达理论值，依次加入丁酮肟、有机铋催化剂，最后在70-80℃下反应至无残留NCO，反应结束出料；
(2)组分B的制备：将计量的二乙烯三胺和异佛尔酮二胺混合均匀即可；
(3)将A、B组分按照比例在20-40℃下混合均匀，脱泡，得产物。
6.根据权利要求5所述的一种封端型双组份无溶剂防水透湿聚氨酯树脂的制备方法，其特征在于：所述新戊二醇聚酯多元醇的分子量为1500-3000。
7.根据权利要求5所述的一种封端型双组份无溶剂防水透湿聚氨酯树脂的制备方法，其特征在于：所述聚四氢呋喃多元醇的分子量为1500-3000。
8.根据权利要求5所述的一种封端型双组份无溶剂防水透湿聚氨酯树脂的制备方法，其特征在于：所述聚氧化乙烯多元醇的分子量为1500-3000。
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