CN112980376A - 一种水性聚氨酯胶粘剂及其制备方法 - Google Patents

一种水性聚氨酯胶粘剂及其制备方法 Download PDF

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CN112980376A
CN112980376A CN202110123252.3A CN202110123252A CN112980376A CN 112980376 A CN112980376 A CN 112980376A CN 202110123252 A CN202110123252 A CN 202110123252A CN 112980376 A CN112980376 A CN 112980376A
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polyurethane adhesive
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郭松华
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Foshan Shangfeng Polymer Technology Co ltd
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Abstract

本发明公开了一种水性聚氨酯胶粘剂，由以下质量份的各组分组成：聚酯多元醇55～69份；聚碳多元醇15～20份；二异氰酸酯8.5～12份；交联剂0.06～0.1份；氨基羧酸盐0.1～1.0份；磺酸盐亲水扩链剂1.0～3.0份；二元胺扩链剂0.08～0.15份；有机铋催化剂0.02～0.05份。本发明还公开了一种水性聚氨酯胶粘剂的制备方法。本发明加入氨基羧酸盐，从而增强了产品的耐水解性，且在聚酯多元醇的基础上增加使用聚碳多元醇，更有利于大大提高水性聚氨酯胶粘剂的耐水解性和韧性。

Description

一种水性聚氨酯胶粘剂及其制备方法
技术领域
本发明涉及一种聚氨酯胶粘剂及其制备方法，属于胶粘剂材料技术领域，特别涉及一种水性聚氨酯胶粘剂及其制备方法。
背景技术
聚氨酯胶粘剂是目前正在迅猛发展的聚氨酯树脂中的一个重要组成部分，具有优异的性能，在许多方面都得到了广泛的应用，是八大合成胶粘剂中的重要品种之一。聚氨酯胶粘剂具备优异的抗剪切强度和抗冲击特性，适用于各种结构性粘合领域，并具备优异的柔韧特性。聚氨酯胶粘剂还具有韧性可调节、粘合工艺简便、极佳的耐低温性能以及优良的稳定性等特性。正是由于聚氨酯胶粘剂这种优良的粘接性能和对多种基材的粘接适应性，使其应用领域不断扩大，在国内外近年来成为发展最快的胶粘剂。
水性聚氨酯胶粘剂具有低VOC含量、低或无环境污染、不燃等特点，是聚氨酯胶粘剂的重点发展方向。水性聚氨酯胶粘剂是我国重点发展的合成水性胶粘剂产品。由于聚氨酯胶粘剂具有良好的粘接性能，故已广泛用于制鞋、建筑、汽车及食品包装等行业。其特点为分散液中不含或只含极少量有机溶剂，同时具有一般聚氨酯所固有的耐磨损、高强度等优点。随着国内环保意识的增强，水性聚氨酯这种环保型产品需求量剧增。
目前在水性聚氨酯合成过程中大多使用有机锡类等稀有金属有机物作为催化剂，而这些有机物为有毒类化合物，很难真正保证产品的环保、安全等性能，甚至为欧盟禁用材料。现有技术大多利用单一聚酯多元醇或者聚醚多元醇作为软段合成水性聚氨酯胶粘剂，利用聚酯多元醇为原料合成的水性聚氨酯胶粘剂的耐水解性能较利用聚醚多元醇合成的水性聚氨酯胶粘剂差，胶粘剂的粘接性能较佳，存放过程中不出现混浊、分层等现象。但目前市售水性聚氨酯的耐水解性和韧性等性能仍存在参差不齐的现象。
发明内容
为了克服现有技术的不足，本发明目的是提供一种水性聚氨酯胶粘剂及其制备方法，提高了水性聚氨酯胶粘剂的耐水解性和韧性，且更有利于环保。
为了达到上述目的，本发明采用以下技术方案：
本发明提供一种水性聚氨酯胶粘剂，由以下质量份的各组分组成：
聚酯多元醇 55～69份；
聚碳多元醇 15～20份；
二异氰酸酯 8.5～12份；
交联剂 0.06～0.1份；
氨基羧酸盐 0.1～1.0份；
磺酸盐亲水扩链剂 1.0～3.0份；
二元胺扩链剂 0.08～0.15份；
有机铋催化剂 0.02～0.05份。
进一步地，所述聚酯多元醇为聚己二酸己二醇酯或聚己内酯二元醇。
进一步地，所述聚碳多元醇为聚碳多元醇PD-1000。
进一步地，述所二异氰酸酯为异佛尔酮二异氰酸酯IPDI和六亚甲基二异氰酸酯HDI。
进一步地，所述氨基羧酸盐为乙二胺四乙酸二钠或乙二胺四乙酸四钠。
进一步地，所述有机铋催化剂为异辛酸铋或环烷酸铋。
进一步地，所述交联剂为三羟甲基丙烷。
进一步地，所述磺酸盐亲水扩链剂为乙二胺基乙磺酸钠。
进一步地，所述二元胺扩链剂为乙二胺、丙二胺或异氟尔酮二胺。
本发明提供如上所述的水性聚氨酯胶粘剂的制备方法，包括以下步骤：
A、将聚酯多元醇、聚碳多元醇进行预热处理后，与二异氰酸酯、交联剂一起在有机铋催化剂作用下进行预聚反应，得到预聚物；
B、在预聚物中加入25～30质量份的丙酮进行稀释，加入氨基羧酸盐，加入磺酸盐亲水扩链剂进行扩链反应，得到聚合物；向聚合物中加入去离子水乳化成乳液，再加入二元胺扩链剂进行进一步的扩链反应，50～60℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
进一步地，步骤A中，预聚反应条件为80～95℃进行120～180分钟。
进一步地，步骤B中，扩链反应条件为40～50℃，与磺酸盐亲水扩链剂反应10～20分钟，与二元胺扩链剂反应20～30分钟。
与现有技术相比，本发明具有以下有益效果：
本发明联用氨基羧酸盐和聚碳多元醇，从而增加所制备得到的水性聚氨酯胶粘剂的耐水解性。而在聚酯多元醇的基础上增加20％的聚碳多元醇，更有利于大大提高水性聚氨酯胶粘剂的耐水解性和韧性。本发明所制备得到的水性聚氨酯胶粘剂使用有机铋催化剂代替市面上常用的欧盟已禁用的有机锡催化剂，利用丙酮稀释预聚物将其乳化后脱去丙酮，使制备所得水性聚氨酯胶粘剂不含或只含极少量有机溶剂，脱去的丙酮可重复使用，更能保障所得水性聚氨酯胶粘剂环保、安全性能。
具体实施方式
以下通过具体较佳实施例结合效果试验例对本发明作进一步详细说明，但本发明并不仅限于以下的实施例。
本发明公开了一种水性聚氨酯胶粘剂，由以下质量份的各组分组成：
聚酯多元醇55～69份；聚碳多元醇PD-1000 15～20份；二异氰酸酯8.5～12份；交联剂0.06～0.1份；氨基羧酸盐0.1～1.0份；磺酸盐亲水扩链剂1.0～3.0份；二元胺扩链剂0.08～0.15份；有机铋催化剂0.02～0.05份。
所述聚酯多元醇为聚己二酸己二醇酯或聚己内酯二元醇。
述所二异氰酸酯为异佛尔酮二异氰酸酯IPDI和六亚甲基二异氰酸酯HDI。
所述交联剂为三羟甲基丙烷。
所述氨基羧酸盐为乙二胺四乙酸二钠或乙二胺四乙酸四钠。
所述磺酸盐亲水扩链剂为乙二胺基乙磺酸钠。
所述二元胺扩链剂为乙二胺、丙二胺或异氟尔酮二胺。
所述有机铋催化剂为异辛酸铋或环烷酸铋。
该水性聚氨酯胶粘剂的制备方法包括以下步骤：
A、将聚酯多元醇、聚碳多元醇进行预热处理后，与二异氰酸酯、交联剂一起在有机铋催化剂作用下于80～95℃进行预聚反应120～180分钟，得到预聚物；
B、在预聚物中加入25～30质量份的丙酮进行稀释，加入氨基羧酸盐，加入磺酸盐亲水扩链剂于40～50℃进行扩链反应，反应10～20分钟后得到聚合物；向聚合物中加入去离子水乳化成乳液，再加入二元胺扩链剂进行进一步的扩链反应20～30分钟后，50～60℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
现结合具体实施例对本发明作进一步说明。
实施例1
一种水性聚氨酯胶粘剂，是通过以下工艺步骤制得：
1)将55质量份的聚己二酸己二醇酯、15质量份的聚碳多元醇PD-1000预热至70～80℃后，加入2质量份的异佛尔酮二异氰酸酯IPDI和6.5质量份的六亚甲基二异氰酸酯HDI、0.06质量份的三羟甲基丙烷一起在0.02质量份的异辛酸铋作用下于80℃进行预聚反应180分钟，得到预聚物；
2)将预聚物加入25质量份的丙酮进行稀释，降温至40℃中加入1质量份的乙二胺四乙酸二钠，加入1质量份的乙二胺基乙磺酸钠于40℃进行扩链反应，反应15分钟后得到聚合物；向聚合物中加入等体积的去离子水乳化成乳液，再加入0.1质量份的异氟尔酮二胺进行搅拌，进一步的扩链反应20分钟后，50℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
实施例2
一种水性聚氨酯胶粘剂，是通过以下工艺步骤制得：
1)将69质量份的聚己二酸己二醇酯、20质量份的聚碳多元醇PD-1000预热至70～80℃后，加入2质量份的异佛尔酮二异氰酸酯IPDI和10质量份的六亚甲基二异氰酸酯HDI、0.1质量份的三羟甲基丙烷一起在0.05质量份的异辛酸铋作用下于95℃进行预聚反应180分钟，得到预聚物；
2)将预聚物加入30质量份的丙酮进行稀释，降温至50℃中加入1质量份的乙二胺四乙酸二钠，加入3质量份的乙二胺基乙磺酸钠于50℃进行扩链反应，反应15分钟后得到聚合物；向聚合物中加入等体积的去离子水乳化成乳液，再加入0.15质量份的异氟尔酮二胺进行搅拌，进一步的扩链反应20分钟后，60℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
实施例3
一种水性聚氨酯胶粘剂，是通过以下工艺步骤制得：
1)将60质量份的聚己二酸己二醇酯、16质量份的聚碳多元醇PD-1000预热至70～80℃后，加入2质量份的异佛尔酮二异氰酸酯IPDI和8质量份的六亚甲基二异氰酸酯HDI、0.1质量份的三羟甲基丙烷一起在0.04质量份的异辛酸铋作用下于90℃进行预聚反应120分钟，得到预聚物；
2)将预聚物加入28质量份的丙酮进行稀释，降温至45℃中加入1质量份的乙二胺四乙酸二钠，加入2质量份的乙二胺基乙磺酸钠于45℃进行扩链反应，反应15分钟后得到聚合物；向聚合物中加入等体积的去离子水乳化成乳液，再加入0.10质量份的异氟尔酮二胺进行搅拌，进一步的扩链反应20分钟后，55℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
实施例4
一种水性聚氨酯胶粘剂，是通过以下工艺步骤制得：
1)将64质量份的聚己内酯二元醇、18质量份的聚碳多元醇PD-1000预热至70～80℃后，加入2质量份的异佛尔酮二异氰酸酯IPDI和8质量份的六亚甲基二异氰酸酯HDI、0.1质量份的三羟甲基丙烷一起在0.04质量份的环烷酸铋作用下于90℃进行预聚反应120分钟，得到预聚物；
2)将预聚物加入28质量份的丙酮进行稀释，降温至45℃中加入1质量份的乙二胺四乙酸四钠，加入2质量份的乙二胺基乙磺酸钠于45℃进行扩链反应，反应15分钟后得到聚合物；向聚合物中加入等体积的去离子水乳化成乳液，再加入0.12质量份的异氟尔酮二胺进行搅拌，进一步的扩链反应20分钟后，55℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
实施例5
一种水性聚氨酯胶粘剂，是通过以下工艺步骤制得：
1)将68质量份的聚己内酯二元醇、20质量份的聚碳多元醇PD-1000预热至70～80℃后，加入2质量份的异佛尔酮二异氰酸酯IPDI和9质量份的六亚甲基二异氰酸酯HDI、0.1质量份的三羟甲基丙烷一起在0.05质量份的环烷酸铋作用下于95℃进行预聚反应180分钟，得到预聚物；
2)将预聚物加入30质量份的丙酮进行稀释，降温至50℃中加入1质量份的乙二胺四乙酸四钠，加入2.5质量份的乙二胺基乙磺酸钠于50℃进行扩链反应，反应15分钟后得到聚合物；向聚合物中加入等体积的去离子水乳化成乳液，再加入0.15质量份的异氟尔酮二胺进行搅拌，进一步的扩链反应20分钟后，60℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
对比例1
一种水性聚氨酯胶粘剂，是通过以下工艺步骤制得：
1)将70质量份的聚己二酸己二醇酯预热至70～80℃后，加入2质量份的异佛尔酮二异氰酸酯IPDI和6.5质量份的六亚甲基二异氰酸酯HDI、0.06质量份的三羟甲基丙烷一起在0.02质量份的异辛酸铋作用下于80℃进行预聚反应180分钟，得到预聚物；
2)将预聚物加入25质量份的丙酮进行稀释，降温至40℃中加入1质量份的乙二胺基乙磺酸钠于40℃进行扩链反应，反应15分钟后得到聚合物；向聚合物中加入等体积的去离子水乳化成乳液，再加入0.1质量份的异氟尔酮二胺进行搅拌，进一步的扩链反应20分钟后，50℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
对比例2
一种水性聚氨酯胶粘剂，是通过以下工艺步骤制得：
1)将80质量份的聚己内酯二元醇预热至70～80℃后，加入2质量份的异佛尔酮二异氰酸酯IPDI和9质量份的六亚甲基二异氰酸酯HDI、0.1质量份的三羟甲基丙烷一起在0.05质量份的环烷酸铋作用下于95℃进行预聚反应180分钟，得到预聚物；
2)将预聚物加入30质量份的丙酮进行稀释，降温至50℃中加入2.5质量份的乙二胺基乙磺酸钠于50℃进行扩链反应，反应15分钟后得到聚合物；向聚合物中加入等体积的去离子水乳化成乳液，再加入0.15质量份的异氟尔酮二胺进行搅拌，进一步的扩链反应20分钟后，60℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
效果试验例
取实施例1～5、对比例1～2的水性聚氨酯胶粘剂分别倒入聚四氟乙烯模具中，然后置于70℃烘箱中烘干24h，即可得到表面光滑的涂层，将其进行性能测试。按以下方法，分别对各水性聚氨酯胶粘剂的性能进行评价：
耐水解性：将样品置于温度70℃、湿度95％的密封环境中7天后，测量其剥离强度，作为耐水解性指标。
拉伸强度：采用GB/T13022检测标准进行测试。
断裂伸长率：采用GB/T13022检测标准进行测试。
结果如下表2所示。
表2性能评价结果
Figure BDA0002922808330000061
由如上表2中可以得出，氨基羧酸盐和聚碳多元醇的加入，能够使本发明所制得的水性聚氨酯胶粘剂于温度70℃、湿度95％的密封7天后，剥离强度大大提高，从而增强其耐水解性。而从拉伸强度和断裂伸长率数据可以看出，在聚酯多元醇的基础上增加20％的聚碳多元醇，有利于增强本发明水性聚氨酯胶粘剂的韧性和耐水解性。
本发明并不局限于上述实施方式，如果对本发明的各种改动或变型不脱离本发明的精神和范围，倘若这些改动和变型属于本发明的权利要求和等同技术范围之内，则本发明也意图包含这些改动和变动。

Claims (10)

1.一种水性聚氨酯胶粘剂，其特征在于，由以下质量份的各组分组成：
Figure FDA0002922808320000011
2.根据权利要求1所述的水性聚氨酯胶粘剂，其特征在于：所述聚酯多元醇为聚己二酸己二醇酯或聚己内酯二元醇。
3.根据权利要求1所述的水性聚氨酯胶粘剂，其特征在于：所述聚碳多元醇为聚碳多元醇PD-1000。
4.根据权利要求1所述的水性聚氨酯胶粘剂，其特征在于：所述二异氰酸酯为异佛尔酮二异氰酸酯和六亚甲基二异氰酸酯。
5.根据权利要求1所述的水性聚氨酯胶粘剂，其特征在于：所述氨基羧酸盐为乙二胺四乙酸二钠或乙二胺四乙酸四钠。
6.根据权利要求1所述的水性聚氨酯胶粘剂，其特征在于：所述有机铋催化剂为异辛酸铋或环烷酸铋。
7.根据权利要求1所述的水性聚氨酯胶粘剂，其特征在于：所述交联剂为三羟甲基丙烷；所述磺酸盐亲水扩链剂为乙二胺基乙磺酸钠；所述二元胺扩链剂为乙二胺、丙二胺或异氟尔酮二胺。
8.权利要求1～7任一项所述的水性聚氨酯胶粘剂的制备方法，其特征在于，包括以下步骤：
A、将聚酯多元醇、聚碳多元醇进行预热处理后，与二异氰酸酯、交联剂一起在有机铋催化剂作用下进行预聚反应，得到预聚物；
B、在预聚物中加入丙酮进行稀释，加入氨基羧酸盐，加入磺酸盐亲水扩链剂进行扩链反应，得到聚合物；向聚合物中加入去离子水乳化成乳液，再加入二元胺扩链剂进行进一步的扩链反应，50～60℃低压抽真空脱丙酮即得到水性聚氨酯胶粘剂。
9.根据权利要求8所述的制备方法，其特征在于：步骤A中，预聚反应条件为80～95℃进行120～180分钟。
10.根据权利要求8所述的制备方法，其特征在于：步骤B中，扩链反应条件为40～50℃，与磺酸盐亲水扩链剂反应10～20分钟，与二元胺扩链剂反应20～30分钟。
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