CN106554508A - 刺激响应性和自修复聚丙烯酸‑聚氨酯膜的制备方法 - Google Patents

刺激响应性和自修复聚丙烯酸‑聚氨酯膜的制备方法 Download PDF

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CN106554508A
CN106554508A CN201611104519.XA CN201611104519A CN106554508A CN 106554508 A CN106554508 A CN 106554508A CN 201611104519 A CN201611104519 A CN 201611104519A CN 106554508 A CN106554508 A CN 106554508A
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王耀斌
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Abstract

本发明涉及合成树脂及塑料技术领域，具体涉及一种刺激响应性和自修复聚丙烯酸‑聚氨酯膜的制备方法。刺激响应性和自修复聚丙烯酸‑聚氨酯膜的制备方法，包括如下步骤：（1）聚丙烯酸的制备。（2）聚氨酯的制备；（3）聚丙烯酸‑聚氨酯复合膜的制备。本发明采用溶液聚合法制备了聚丙烯酸，丙酮法制备了水性聚氨酯，涂覆法制备了聚丙烯酸‑聚氨酯复合膜。该聚丙烯酸‑聚氨酯复合膜的修复效率较高可达90％。

Description

刺激响应性和自修复聚丙烯酸-聚氨酯膜的制备方法
技术领域
本发明涉及合成树脂及塑料技术领域，具体涉及一种刺激响应性和自修复聚丙烯酸-聚氨酯膜的制备方法。
背景技术
复合材料在长期使用过程中会产生微裂纹，导致材料性能下降甚至报废。因此研究复合材料的自修复可以延长材料的使用寿命，提高材料的安全性。目前，具有刺激响应性与自修复性能的膜材料已经成为仿生学领域的重要研究内容。
聚丙烯酸-聚氨酯复合膜兼具聚氨酯的耐磨损、可裁剪性和聚丙烯酸可自修复的特性。当聚丙烯酸-聚氨酯复合膜在使用中出现微裂纹时，聚丙烯酸可以自动修复，从而延长了聚氨酯的使用寿命，聚丙烯酸-聚氨酯复合膜可应用于涂料、黏合剂及油墨等领域。
发明内容
本发明旨在提出一种刺激响应性和自修复聚丙烯酸-聚氨酯膜的制备方法。
本发明的技术方案在于：
刺激响应性和自修复聚丙烯酸-聚氨酯膜的制备方法，包括如下步骤：
（1）聚丙烯酸的制备
称取过硫酸钾0.40 g、亚硫酸氢钠0.09 g于50mL锥形瓶中，用移液管取丙烯酸10 mL，加入锥形瓶中，轻轻摇动，待引发剂完全溶于丙烯酸中，将溶液倒人三口烧瓶，再用50 mL的去离子水冲洗锥形瓶，并将冲洗溶液倒入三口烧瓶，再加入40 mL去离子水；维持搅拌转速恒定，升温至60℃，开始聚合，反应2.5~3.5 h后，升温至75℃继续反应0.5 h，结束反应得到聚丙烯酸；
（2）聚氨酯的制备
在带有搅拌器、冷凝管和滴液漏斗的干燥三口烧瓶中，加入脱水的聚乙二醇和异弗尔酮二异氰酸酯，n(-NC0)：n(-0H)=2：1，升温至80℃，反应2 h完成预聚合，加入丙酮降低黏度；将体系降温至70℃，加入N-甲基二乙醇胺、1，4-丁二醇以及1滴催化剂，进行扩链交联反应2 h；将体系降温至30℃，然后再加入中和试剂冰乙酸，继续搅拌30 min；然后在高速搅拌下，向体系中加入冰水进行反相乳化减压蒸出丙酮，制得半透明阳离子水性聚氨酯乳液；
（3）聚丙烯酸-聚氨酯复合膜的制备
采用涂覆法构筑聚丙烯酸-聚氨酯复合膜复合膜。
所述的涂覆法的步骤为：选取干净的玻璃片涂覆聚氨酯乳液，并在40℃烘干成膜；在烘干的聚氨酯膜上涂覆聚丙烯酸溶液，并在40℃烘干；重复上述步骤，达到目的层数，制成聚丙烯酸-聚氨酯复合膜。
所述的脱水的聚乙二醇和异弗尔酮二异氰酸酯中n(-NC0)：n(-0H)=2：1。
本发明的技术效果在于：
本发明采用溶液聚合法制备了聚丙烯酸，丙酮法制备了水性聚氨酯，涂覆法制备了聚丙烯酸-聚氨酯复合膜。该聚丙烯酸-聚氨酯复合膜的修复效率较高可达90％。
具体实施方式
刺激响应性和自修复聚丙烯酸-聚氨酯膜的制备方法，包括如下步骤：
（1）聚丙烯酸的制备
称取过硫酸钾0.40 g、亚硫酸氢钠0.09 g于50mL锥形瓶中，用移液管取丙烯酸10 mL，加入锥形瓶中，轻轻摇动，待引发剂完全溶于丙烯酸中，将溶液倒人三口烧瓶，再用50 mL的去离子水冲洗锥形瓶，并将冲洗溶液倒入三口烧瓶，再加入40 mL去离子水；维持搅拌转速恒定，升温至60℃，开始聚合，反应2.5~3.5 h后，升温至75℃继续反应0.5 h，结束反应得到聚丙烯酸；
（2）聚氨酯的制备
在带有搅拌器、冷凝管和滴液漏斗的干燥三口烧瓶中，加入脱水的聚乙二醇和异弗尔酮二异氰酸酯，n(-NC0)：n(-0H)=2：1，升温至80℃，反应2 h完成预聚合，加入丙酮降低黏度；将体系降温至70℃，加入N-甲基二乙醇胺、1，4-丁二醇以及1滴催化剂，进行扩链交联反应2 h；将体系降温至30℃，然后再加入中和试剂冰乙酸，继续搅拌30 min；然后在高速搅拌下，向体系中加入冰水进行反相乳化减压蒸出丙酮，制得半透明阳离子水性聚氨酯乳液；
（3）聚丙烯酸-聚氨酯复合膜的制备
采用涂覆法构筑聚丙烯酸-聚氨酯复合膜复合膜。
实施例2
（1）聚丙烯酸的制备
称取过硫酸钾0.40 g、亚硫酸氢钠0.09 g于50mL锥形瓶中，用移液管取丙烯酸10 mL，加入锥形瓶中，轻轻摇动，待引发剂完全溶于丙烯酸中，将溶液倒人三口烧瓶，再用50 mL的去离子水冲洗锥形瓶，并将冲洗溶液倒入三口烧瓶，再加入40 mL去离子水；维持搅拌转速恒定，升温至60℃，开始聚合，反应2.5~3.5 h后，升温至75℃继续反应0.5 h，结束反应得到聚丙烯酸；
（2）聚氨酯的制备
在带有搅拌器、冷凝管和滴液漏斗的干燥三口烧瓶中，加入脱水的聚乙二醇和异弗尔酮二异氰酸酯，n(-NC0)：n(-0H)=2：1，升温至80℃，反应2 h完成预聚合，加入丙酮降低黏度；将体系降温至70℃，加入N-甲基二乙醇胺、1，4-丁二醇以及1滴催化剂，进行扩链交联反应2 h；将体系降温至30℃，然后再加入中和试剂冰乙酸，继续搅拌30 min；然后在高速搅拌下，向体系中加入冰水进行反相乳化减压蒸出丙酮，制得半透明阳离子水性聚氨酯乳液；
（3）聚丙烯酸-聚氨酯复合膜的制备
选取干净的玻璃片涂覆聚氨酯乳液，并在40℃烘干成膜；在烘干的聚氨酯膜上涂覆聚丙烯酸溶液，并在40℃烘干；重复上述步骤，达到目的层数，制成聚丙烯酸-聚氨酯复合膜。
其中，所述的脱水的聚乙二醇和异弗尔酮二异氰酸酯中n(-NC0)：n(-0H)=2：1。

Claims (3)

1.刺激响应性和自修复聚丙烯酸-聚氨酯膜的制备方法，其特征在于：包括如下步骤：
（1）聚丙烯酸的制备
称取过硫酸钾0.40 g、亚硫酸氢钠0.09 g于50mL锥形瓶中，用移液管取丙烯酸10 mL，加入锥形瓶中，轻轻摇动，待引发剂完全溶于丙烯酸中，将溶液倒人三口烧瓶，再用50 mL的去离子水冲洗锥形瓶，并将冲洗溶液倒入三口烧瓶，再加入40 mL去离子水；维持搅拌转速恒定，升温至60℃，开始聚合，反应2.5~3.5 h后，升温至75℃继续反应0.5 h，结束反应得到聚丙烯酸；
（2）聚氨酯的制备
在带有搅拌器、冷凝管和滴液漏斗的干燥三口烧瓶中，加入脱水的聚乙二醇和异弗尔酮二异氰酸酯，n(-NC0)：n(-0H)=2：1，升温至80℃，反应2 h完成预聚合，加入丙酮降低黏度；将体系降温至70℃，加入N-甲基二乙醇胺、1，4-丁二醇以及1滴催化剂，进行扩链交联反应2 h；将体系降温至30℃，然后再加入中和试剂冰乙酸，继续搅拌30 min；然后在高速搅拌下，向体系中加入冰水进行反相乳化减压蒸出丙酮，制得半透明阳离子水性聚氨酯乳液；
（3）聚丙烯酸-聚氨酯复合膜的制备
采用涂覆法构筑聚丙烯酸-聚氨酯复合膜复合膜。
2.根据权利要求1所述的刺激响应性和自修复聚丙烯酸-聚氨酯膜的制备方法，其特征在于：所述的涂覆法的步骤为：选取干净的玻璃片涂覆聚氨酯乳液，并在40℃烘干成膜；在烘干的聚氨酯膜上涂覆聚丙烯酸溶液，并在40℃烘干；重复上述步骤，达到目的层数，制成聚丙烯酸-聚氨酯复合膜。
3.根据权利要求1所述的刺激响应性和自修复聚丙烯酸-聚氨酯膜的制备方法，其特征在于：所述的脱水的聚乙二醇和异弗尔酮二异氰酸酯中n(-NC0)：n(-0H)=2：1。
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109888286A (zh) * 2019-01-23 2019-06-14 西安交通大学 一种动态离子交联的聚丙烯酸-聚乙二醇水凝胶粘合剂及其制备方法和应用

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109888286A (zh) * 2019-01-23 2019-06-14 西安交通大学 一种动态离子交联的聚丙烯酸-聚乙二醇水凝胶粘合剂及其制备方法和应用

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