CN112608448A - 一种高弹性手感耐磨多臂型光固化树脂的制备方法 - Google Patents

一种高弹性手感耐磨多臂型光固化树脂的制备方法 Download PDF

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CN112608448A
CN112608448A CN202011598605.7A CN202011598605A CN112608448A CN 112608448 A CN112608448 A CN 112608448A CN 202011598605 A CN202011598605 A CN 202011598605A CN 112608448 A CN112608448 A CN 112608448A
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姚伯龙
王海潮
陈欢
王宇通
倪亚洲
程广鸿
张晋瑞
王利魁
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Abstract

一种高弹性手感耐磨多臂型光固化树脂的制备方法，属于功能性聚氨酯材料技术领域。本发明利用三官能团异氰酸酯、异佛尔酮二异氰酸酯IPDI、聚碳酸酯二元醇PCDL、季戊四醇三丙烯酸酯PETA和二元醇改性合成具有弹性及耐磨特性的弹性耐磨树脂。本发明方法制备的多官能团支化型聚氨酯耐磨弹性树脂，是一种优良的高分子合成材料，既具有橡胶的弹性又具有塑料的硬度，而且还具有良好的机械性能、耐磨性能和回弹性；在弹性手感材料应用领域具有良好的应用前景。

Description

一种高弹性手感耐磨多臂型光固化树脂的制备方法
技术领域
本发明涉及一种高弹性手感耐磨多臂型光固化树脂的制备方法，属于功能性聚氨酯材料技术领域。
背景技术
现有技术中，为了使得某些经常需要手触摸的部位，诸如吹风筒手柄﹑MP3外壳﹑鼠标﹑手机外壳﹑望远镜和伞柄等等，不再给人以冷冰冰﹑粗糙和生硬的感觉，而提供软绵爽滑的触感，弹性手感漆应运而生。弹性手感漆主要采用弹性树脂，具有色彩更鲜艳的外观以及温暖类似皮革的手触感，用途广，用量大，市场前景可观。
纯直链型聚酯树脂价格便宜，性价比较好，但在某些主要性能（如手感﹑耐刮伤性、耐磨等性能测试）方面较弱于改性聚酯树脂。为了解决上述问题，需要开发一种多官能团支化型聚氨酯耐磨弹性树脂。
发明内容
本发明的目的是克服上述不足之处，提供一种高弹性手感耐磨多臂型光固化树脂的制备方法，其制备的树脂既具有橡胶的弹性又具有塑料的硬度，而且还具有良好的机械性能、耐磨性能和回弹性。
本发明的技术方案，一种高弹性手感耐磨多臂型光固化树脂的制备方法，步骤为：
（1）将二异氰酸酯和二元醇加入反应容器中，滴加用乙酸乙酯稀释的催化剂，升温进行反应；添加季戊四醇三丙烯酸酯PETA和乙二醇封端，保温持续搅拌，得到组分1；
（2）将三官能团异氰酸酯和催化剂加入反应容器中并升温反应，将步骤（1）制备得到的组分1缓慢滴加到上述反应容器中，继续保温反应；
（3）将端羟基聚丁二烯HTPB加入到步骤（2）所述反应容器中继续反应，加入季戊四醇三丙烯酸酯进行封端处理得到高弹性手感耐磨多臂型光固化树脂。
进一步地，所述三官能团异氰酸酯具体为HDI的三聚体。
进一步地，所述催化剂具体为二月桂酸二丁基锡DBTDL、有机铋催化剂、二甲基环己胺或甲基二乙烯三胺中的一种。
进一步地，步骤（1）所述二异氰酸酯具体为异佛尔酮二异氰酸酯IPDI或甲苯二异氰酸酯TDI；
所述二元醇具体为聚碳酸酯二元醇PCDL或聚四氢呋喃PTMG。
进一步地，步骤（3）所述端羟基聚丁二烯HTPB是一种具有橡胶弹性的、端羟基封端的二元醇。
步骤（1）具体为：将8-25g的二异氰酸酯和13-50g二元醇加入接有搅拌器、冷凝管、氮气导管和恒压滴定漏斗的干燥的四口烧瓶中；继续加入用15-20mL乙酸乙酯稀释的1-3滴的催化剂，并升温至60-70℃，待温度达到后，继续反应2-3h；添加6-30g的季戊四醇三丙烯酸酯PETA和1-5g乙二醇进行封端，保温至60-70℃，持续搅拌4-5h，得到组分1。
步骤（2）具体为：将10-35g的三官能团异氰酸酯和1-2滴催化剂加入接有搅拌器、冷凝管、氮气导管和恒压滴定漏斗的干燥的四口烧瓶中，并升温至60-70℃；将步骤（1）制备的组分1缓慢滴加到上述四口烧瓶中，并在60-70℃下反应2-3h。
步骤（3）具体为：将30-55g的端羟基聚丁二烯HTPB加入步骤（2）所述四口烧瓶中，在60-70℃继续反应2-3h，加入1-5g季戊四醇三丙烯酸酯进行封端处理；得到高弹性手感耐磨多臂型光固化树脂。
进一步地，步骤（3）中在反应过程里加入溶剂调节粘度，使得聚合物在反应中不出现爬杆现象。
进一步地，所述溶剂具体为四氢呋喃THF、丙酮ACE或二甲基甲酰胺DMF。
本发明的有益效果：本发明方法制备的多官能团支化型聚氨酯耐磨弹性树脂，是一种优良的高分子合成材料，既具有橡胶的弹性又具有塑料的硬度，而且还具有良好的机械性能、耐磨性能和回弹性；在弹性手感材料应用领域具有良好的应用前景。
附图说明
图1 硬段含量对弹性耐磨树脂力学性能的影响。
具体实施方式
实施例1
（1）将8.8g（0.04mol）的IPDI和40g（0.02mol）的PCDL加入接有搅拌器、冷凝管、氮气导管和恒压滴定漏斗的干燥的四口烧瓶中；加入用20mL乙酸乙酯稀释的3滴催化剂DBTDL，并升温至60℃，待温度达到后，继续反应2h；添加6g（0.02mol）的PETA和1.2g（0.02mol）的乙二醇封端，设定温度65℃，持续搅拌，共计4h得组分1，组分1留有0.02mol的羟基基团；
（2）将18.5g（0.02mol）的HDI的三聚体和2滴催化剂DBTDL加入接有搅拌器、冷凝管、氮气导管和恒压滴定漏斗的干燥的四口烧瓶中，并升温至65℃；将步骤（1）制备的组分1缓慢滴加到上述四口烧瓶中，并在65℃下反应2h；
（3）将36g（0.018mol）的HTPB加入所述四口烧瓶中65℃反应（期间用适当的溶剂调节粘度）2h后，加入1.2g（0.004mol）的PETA进行封端处理得到设计的六爪的高弹性手感耐磨多臂型光固化树脂。
实施例1制备所得硬段（即IPDI和HDI的三聚体反应物）占整个弹性耐磨树脂质量的26.7%。
实施例2
当硬段含量为38.6%时，反应物为：IPDI质量10g，HDT（HDI的三聚体） 28.6g，此时PCDL（设为x）+HTPB（设为y）=61.4g，x/800 +y/2000 =0.1015，0.1015是由IPDI和HDT的总摩尔数所确定。其他反应条件和参数与实施例1相同。
实施例3
当硬段含量为42.6%时，反应物为：IPDI质量12.6g，HDT 30g，此时PCDL（设为x）+HTPB（设为y）=57.4g，x/800 +y/2000 =0.1161，0.1161是由IPDI和HDT的总摩尔数所确定。其他反应条件和参数与实施例1相同。
实施例4
当硬段含量为46.6%时，反应物为：IPDI质量14.6g，HDT 32g，此时PCDL（设为x）+HTPB（设为y）=53.4g，x/800 +y/2000 =0.1290，0.1290是由IPDI和HDT的总摩尔数所确定。其他反应条件和参数与实施例1相同。
实施例5
当硬段含量为50.6%时，反应物为：IPDI质量20g，HDT 30.6g，此时PCDL（设为x）+HTPB（设为y）=49.4g，x/800 +y/2000 =0.1263，0.1263是由IPDI和HDT的总摩尔数所确定。其他反应条件和参数与实施例1相同。
实施例2-5所制备得到的弹性耐磨树脂中，硬段含量对弹性耐磨树脂力学性能的影响如图1所示。
由图1可知，当硬段含量由38.6％增加到50.6％时，PU弹性体的拉伸强度由4.68MPa增加到20.83MPa，断裂伸长率由248.32％先上升到445.31％，而后又降到207.38％。之所以产生这种现象，主要是由于硬段含量的提高，增加了硬段相在软段相中的分布，使硬度增加，同时因硬段岛区在弹性体中起物理交联的作用，交联点的增多也会促进硬段相之间形成氢键或交联，使PU弹性体的拉伸强度不断增大，断裂伸长率也会有较大变化。

Claims (9)

1.一种高弹性手感耐磨多臂型光固化树脂的制备方法，其特征在于步骤为：
（1）将二异氰酸酯和二元醇加入反应容器中，滴加用乙酸乙酯稀释的催化剂，升温进行反应；添加季戊四醇三丙烯酸酯PETA和乙二醇封端，保温持续搅拌，得到组分1；
（2）将三官能团异氰酸酯和催化剂加入反应容器中并升温反应，将步骤（1）制备得到的组分1缓慢滴加到上述反应容器中，继续保温反应；
（3）将端羟基聚丁二烯HTPB加入到步骤（2）所述反应容器中继续反应，加入季戊四醇三丙烯酸酯进行封端处理得到高弹性手感耐磨多臂型光固化树脂。
2.根据权利要求1所述高弹性手感耐磨多臂型光固化树脂的制备方法，其特征在于：所述三官能团异氰酸酯具体为HDI的三聚体。
3.根据权利要求1所述高弹性手感耐磨多臂型光固化树脂的制备方法，其特征在于：所述催化剂具体为二月桂酸二丁基锡DBTDL、有机铋催化剂、二甲基环己胺或甲基二乙烯三胺中的一种。
4.根据权利要求1所述高弹性手感耐磨多臂型光固化树脂的制备方法，其特征在于：步骤（1）所述二异氰酸酯具体为异佛尔酮二异氰酸酯IPDI或甲苯二异氰酸酯TDI；
所述二元醇具体为聚碳酸酯二元醇PCDL或聚四氢呋喃PTMG。
5.根据权利要求1所述高弹性手感耐磨多臂型光固化树脂的制备方法，其特征在于步骤（1）具体为：将8-25g的二异氰酸酯和13-50g二元醇加入接有搅拌器、冷凝管、氮气导管和恒压滴定漏斗的干燥的四口烧瓶中；继续加入用15-20mL乙酸乙酯稀释的1-3滴的催化剂，并升温至60-70℃，待温度达到后，继续反应2-3h；添加6-30g的季戊四醇三丙烯酸酯PETA和1-5g乙二醇进行封端，保温60-70℃，持续搅拌4-5h，得到组分1。
6.根据权利要求1所述高弹性手感耐磨多臂型光固化树脂的制备方法，其特征在于步骤（2）具体为：将10-35g的三官能团异氰酸酯和1-2滴催化剂加入接有搅拌器、冷凝管、氮气导管和恒压滴定漏斗的干燥的四口烧瓶中，并升温至60-70℃；将步骤（1）制备的组分1缓慢滴加到上述四口烧瓶中，并在60-70℃下反应2-3h。
7.根据权利要求1所述高弹性手感耐磨多臂型光固化树脂的制备方法，其特征在于步骤（3）具体为：将30-55g的端羟基聚丁二烯HTPB加入步骤（2）所述四口烧瓶中，在60-70℃继续反应2-3h，加入1-5g季戊四醇三丙烯酸酯进行封端处理；得到高弹性手感耐磨多臂型光固化树脂。
8.根据权利要求7所述高弹性手感耐磨多臂型光固化树脂的制备方法，其特征在于：步骤（3）中在反应过程中加入溶剂调节粘度，使得聚合物在反应中不出现爬杆现象。
9.根据权利要求8所述高弹性手感耐磨多臂型光固化树脂的制备方法，其特征在于：所述溶剂具体为四氢呋喃THF、丙酮ACE或二甲基甲酰胺DMF。
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