CN108728035B - 一种自催化型聚氨酯热熔胶及其制备方法 - Google Patents

一种自催化型聚氨酯热熔胶及其制备方法 Download PDF

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CN108728035B
CN108728035B CN201810615454.8A CN201810615454A CN108728035B CN 108728035 B CN108728035 B CN 108728035B CN 201810615454 A CN201810615454 A CN 201810615454A CN 108728035 B CN108728035 B CN 108728035B
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王泽伟
王桂荣
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Shantou Lucan Chemical Raw Material Co ltd
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Abstract

本发明涉及一种自催化型聚氨酯热熔胶及其制备方法。按质量份计包括如下组分：结晶性己二酸聚酯多元醇、邻苯二甲酸聚酯多元醇、聚醚二元醇、二异氰酸酯、自催化剂、自催化预聚物、其他助剂。制备方法包括以下步骤：将反应釜中加入结晶性己二酸聚酯多元醇、邻苯二甲酸酐一缩乙二醇酯二醇和聚醚二元醇，升温至120℃脱水2h，然后冷却至90℃；将二异氰酸酯和自催化预聚物加入反应釜中，加料完成后在110℃下反应2h；加入自催化剂继续反应1h；再加入其他助剂，抽真空至‑0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶。根据本发明的制备方法制备的聚氨酯热熔胶具有自催化的特性，能够极大地改善聚氨酯热熔胶的固化速度及粘接强度。

Description

一种自催化型聚氨酯热熔胶及其制备方法
技术领域
本发明涉及热熔胶技术领域，具体为一种自催化型聚氨酯热熔胶的制备方法。
背景技术
反应型聚氨酯热熔胶是以聚氨酯预聚体为主要成分的热熔胶。这类热熔胶具有高的拉伸强度、优良的弹性、耐磨性、耐油性和耐寒性等优点。因此，聚氨酯热熔胶被广泛的应用在手机触摸屏和机壳的结构粘接上，而且它能够点出1mm以下的胶线，可以实现窄边框手机或平板的粘接。
当前，在手机组装的流水线环节中，对提高生产效率的要求极为迫切。而传统的聚氨酯热熔胶存在许多严重的缺陷，尤其是它初始粘接强度低，使其在进行器件组装压合时需要通过固定器具进行2小时以上的保压，从而严重制约了手机触摸屏组装的生产效率。因此，研发一种初始粘接强度高并且减少保压时间的聚氨酯热熔胶，成为该领域的迫切需求。
发明内容
为了解决现有技术中聚氨酯热熔胶存在的初始粘接强度低、保压时间长的弱点，本发明提供一种自催化型聚氨酯热熔胶及其制备方法。
本发明的技术方案如下：
一种自催化型聚氨酯热熔胶，其特征在于，按质量份计包括如下组分：结晶性己二酸聚酯多元醇 20-80%；邻苯二甲酸聚酯多元醇 10-60%；聚醚二元醇 10-60%；二异氰酸酯10-25%；自催化剂 0-5%；自催化预聚物 5-40%；其他助剂 0.01-1.5%。
优选地，其中所述结晶性己二酸聚酯多元醇为分子量在1000-3000的聚己二酸己二醇酯二醇、分子量在1000-3000的聚癸二酸己二醇酯二醇中的一种或两种的混合物。
优选地，其中所述邻苯二甲酸聚酯多元醇为分子量在1000-2000的邻苯二甲酸酐一缩乙二醇酯二醇。
优选地，其中所述聚醚二元醇为分子量在1000-4000的聚丙二醇。
优选地，其中所述二异氰酸酯为甲苯二异氰酸酯TDI，4 ,4’一二苯基甲烷二异氰酸酯MDI或苯二亚甲基二异氰酸酯XDI中的一种或几种的混合物。
优选地，其中所述自催化剂为N-甲基二乙醇胺。
优选地，其中所述自催化预聚物为N-甲基二乙醇胺，聚丙二醇和4 ,4’-二苯基甲烷二异氰酸酯制备的预聚物。
优选地，其中所述其他助剂为催化剂二吗啉基二乙基醚或抗氧剂1010。
一种上述自催化型聚氨酯热熔胶的制备方法，其特征在于，包括以下步骤：
将反应釜中加入结晶性己二酸聚酯多元醇、邻苯二甲酸酐一缩乙二醇酯二醇和聚醚二元醇，升温至120℃脱水2h，然后冷却至90℃；将二异氰酸酯和自催化预聚物加入反应釜中，加料完成后在110℃下反应2h；加入自催化剂继续反应1h；再加入其他助剂，抽真空至-0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶。
一种上述自催化型聚氨酯热熔胶的制备方法，其特征在于，包括以下步骤：
将反应釜中加入结晶性己二酸聚酯多元醇、邻苯二甲酸酐一缩乙二醇酯二醇和聚醚二元醇，升温至120℃脱水2h，然后冷却至90℃；将二异氰酸酯和自催化预聚物加入反应釜中，加料完成后在110℃下反应2h；再加入其他助剂，抽真空至-0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶。
优选地，其中所述自催化预聚物的具体合成包括以下步骤：将反应釜中加入聚丙二醇和N-甲基二乙醇胺，在氮气保护下升温至110℃脱水2h，然后冷却至80℃,将二异氰酸酯加入反应釜中，加料完成后在100℃下反应2h；抽真空至-0.08MPa以下，脱除气泡30min，出料, 制得自催化型聚氨酯热熔胶的自催化预聚物，其中NCO含量为9.8-10.2%。
与现有技术相比，本发明提供的自催化型聚氨酯热熔胶及其制备方法具有以下有益效果：本发明的自催化型聚氨酯热熔胶在合成预聚物时，通过分子设计引入叔胺基团到预聚物主链上，从而使制备的聚氨酯热熔胶具有自催化的特性，能够极大地改善聚氨酯热熔胶的固化速度及粘接强度。
具体实施方式
实施例1
（1）称量96份分子量为2000的聚丙二醇和10份的N-甲基二乙醇胺加入反应釜，升温至110℃脱水2h，然后冷却至80℃；将94份4 ,4’-二苯基甲烷二异氰酸酯加入反应釜中，加料完成后在100℃下反应2h；抽真空至-0.08MPa以下，脱除气泡30min，出料, 制得自催化型聚氨酯热熔胶的自催化预聚物，其中NCO含量为10%。
（2）将反应釜中加入90份分子量为3000的聚己二酸己二醇酯二醇、60份分子量2000的邻苯二甲酸酐一缩乙二醇酯二醇，90份分子量为2000的聚丙二醇，升温至120℃脱水2h，然后冷却至90℃；将50份4 ,4’-二苯基甲烷二异氰酸酯和6份自催化预聚物加入反应釜中，加料完成后在110℃下反应2h；加入0.6份的N-甲基二乙醇胺继续反应1h；再加入0.3份抗氧剂1010，0.3份二吗啉基二乙基醚（DMDEE)，抽真空至-0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶，NCO含量为2.58%。
实施例2
将反应釜中加入90份分子量为3000的聚己二酸己二醇酯二醇、60份分子量2000的邻苯二甲酸酐一缩乙二醇酯二醇和70份分子量为2000的聚丙二醇，升温至120℃脱水2h，然后冷却至90℃；将41份4 ,4’-二苯基甲烷二异氰酸酯和实施例1的步骤（1）中制得的12份自催化预聚物加入反应釜中，加料完成后在110℃下反应2h；再加入0.3份抗氧剂1010，0.3份二吗啉基二乙基醚（DMDEE)，抽真空至-0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶，NCO含量为2.55%。
实施例3
将反应釜中加入90份分子量为3000的聚己二酸己二醇酯二醇、60份分子量2000的邻苯二甲酸酐一缩乙二醇酯二醇和70份分子量为2000的聚丙二醇，升温至120℃脱水2h，然后冷却至90℃；将39份4 ,4’-二苯基甲烷二异氰酸酯和实施例1的步骤（1）中制得的20份自催化预聚物加入反应釜中，加料完成后在110℃下反应2h；再加入0.3份抗氧剂1010，0.3份二吗啉基二乙基醚（DMDEE)，抽真空至-0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶，NCO含量为2.55%。
实施例4
将反应釜中加入90份分子量为3000的聚己二酸己二醇酯二醇、60份分子量2000的邻苯二甲酸酐一缩乙二醇酯二醇和70份分子量为2000的聚丙二醇，升温至120℃脱水2h，然后冷却至90℃；将34份4 ,4’-二苯基甲烷二异氰酸酯和实施例1的步骤（1）中制得的40份自催化预聚物加入反应釜中，加料完成后在110℃下反应2h；再加入0.3份抗氧剂1010，0.3份二吗啉基二乙基醚（DMDEE)，抽真空至-0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶，NCO含量为2.54%。
对比实施例
将反应釜中加入90份分子量为3000的聚己二酸己二醇酯二醇、60份分子量2000的邻苯二甲酸酐一缩乙二醇酯二醇和90份分子量为2000的聚丙二醇，升温至120℃脱水2h，然后冷却至90℃；将48.2份4 ,4’-二苯基甲烷二异氰酸酯加入反应釜中，加料完成后在110℃下反应2h；再加入0.3份抗氧剂1010，0.3份二吗啉基二乙基醚（DMDEE)，抽真空至-0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶，NCO含量为2.54%。
将上述实施例1-4制得的聚氨酯热熔胶与对比实施例制备的聚氨酯热熔胶按胶粘剂试验标准进行初始剪切强度、拉伸强度、断裂伸长率、最终剪切强度，双85老化等性能检测，数据结果如表1和2所示。其中初始剪切强度由涂胶后放置10min后测试，最终强度由涂胶后放置7天后测试。一般室温固化7天可以达到最高强度。
表1实施例与对比实施例机械性能测试对照
Figure DEST_PATH_IMAGE001
表2实施例与对比实施例固化速度和耐水耐老化性能测试对照
Figure 228665DEST_PATH_IMAGE002
从表1和2的性能测试对照表能够看出，本发明制备的自催化型的聚氨酯热熔胶相对于常规聚氨酯热熔胶表现出优异的综合性能，尤其具有更高的初始粘接，固化速度快等优点，能够极大地提高生产效率，降低制造成本。同时，该胶具有良好的粘度稳定性和优异的柔韧性及耐水耐老化性能，充分满足手机等电子通讯制造业封装的严苛要求。

Claims (9)

1.一种自催化型聚氨酯热熔胶，其特征在于，按质量份计包括如下组分：结晶性己二酸聚酯多元醇 20-80%；邻苯二甲酸聚酯多元醇 10-60%；聚醚二元醇 10-60%；二异氰酸酯10-25%；自催化剂 0-5%；自催化预聚物 5-40%；其他助剂 0.01-1.5%；
其中所述自催化预聚物为N-甲基二乙醇胺，聚丙二醇和4 ,4’-二苯基甲烷二异氰酸酯制备的预聚物；
其中所述自催化预聚物的具体合成包括以下步骤：将反应釜中加入聚丙二醇和N-甲基二乙醇胺，在氮气保护下升温至110℃脱水2h，然后冷却至80℃,将二异氰酸酯加入反应釜中，加料完成后在100℃下反应2h；抽真空至-0.08MPa以下，脱除气泡30min，出料, 制得自催化型聚氨酯热熔胶的自催化预聚物，其中NCO含量为9.8-10.2%。
2.根据权利要求1所述的自催化型聚氨酯热熔胶，其中所述结晶性己二酸聚酯多元醇为分子量在1000-3000的聚己二酸己二醇酯二醇、分子量在1000-3000的聚癸二酸己二醇酯二醇中的一种或两种的混合物。
3.根据权利要求1所述的自催化型聚氨酯热熔胶，其中所述邻苯二甲酸聚酯多元醇为分子量在1000-2000的邻苯二甲酸酐一缩乙二醇酯二醇。
4.根据权利要求1所述的自催化型聚氨酯热熔胶，其中所述聚醚二元醇为分子量在1000-4000的聚丙二醇。
5.根据权利要求1所述的自催化型聚氨酯热熔胶，其中所述二异氰酸酯为甲苯二异氰酸酯TDI，4 ,4’-二苯基甲烷二异氰酸酯中的一种或两种的混合物。
6.根据权利要求1所述的自催化型聚氨酯热熔胶，其中所述自催化剂为N-甲基二乙醇胺。
7.根据权利要求1所述的自催化型聚氨酯热熔胶，其中所述其他助剂为催化剂二吗啉基二乙基醚或抗氧剂1010。
8.一种根据权利要求1所述的自催化型聚氨酯热熔胶的制备方法，其特征在于，包括以下步骤：
将反应釜中加入结晶性己二酸聚酯多元醇、邻苯二甲酸酐一缩乙二醇酯二醇和聚醚二元醇，升温至120℃脱水2h，然后冷却至90℃；将二异氰酸酯和自催化预聚物加入反应釜中，加料完成后在110℃下反应2h；加入自催化剂继续反应1h；再加入其他助剂，抽真空至-0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶。
9.一种根据权利要求1所述的自催化型聚氨酯热熔胶的制备方法，其特征在于，包括以下步骤：
将反应釜中加入结晶性己二酸聚酯多元醇、邻苯二甲酸酐一缩乙二醇酯二醇和聚醚二元醇，升温至120℃脱水2h，然后冷却至90℃；将二异氰酸酯和自催化预聚物加入反应釜中，加料完成后在110℃下反应2h；再加入其他助剂，抽真空至-0.08MPa以下，脱除气泡30min，出料，密闭包装，制得自催化型的聚氨酯热熔胶。
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