桐油基光引发剂的制备及性能图45彩印李翠华周宏勇王家喜.DOCVIP

收稿日期：2017-00-00; 定用日期：2017-00-00; DOI: 10.13550/j.jxhg作者简介：李翠华（1991-），女，硕士生。联系人：王家喜（1965-），男，教授，博士生导师，电话：022E-mail：wangjiaxi@hebut.edu.cn 桐油基光引发剂的制备及性能（图4、5彩印） 李翠华，周宏勇，王家喜* （河北工业大学 化工学院，天津，300130） 摘要：以桐油（TO）、桐酸（TA）和马来酸酐(MA)为原料，经Diels-Alder反应，得到桐油酸酐（TOM1~3）及桐酸酸酐（TAM）。在三乙胺催化下，TOM、TAM分子中酸酐分别与Irgacure2959〔2-羟基-4-（2-羟乙氧基）-2-甲基苯丙酮〕的羟基反应，合成了4种裂解型光引发剂（TOMG1~3，TAMG）。用FTIR、1HNMR及HRMS表征了其结构，利用UV-vis考察了引发剂的光分解过程，用实时红外光谱探究了引发剂引发1,6-己二醇二丙烯酸酯(HDDA）的聚合过程。结果表明，在Irgacure2959和桐油改性的几种光引发剂中，TOMG3光引发性能最优。在紫外光强度为28 mW/cm2 的光照下，以HDDA、PUA（聚氨酯丙烯酸酯）及TOMG3按质量比46:46:8复配的胶液的光固化表干时间为60 s，凝胶率为96%，固化膜的硬度及柔韧性分别为6 H和5 mm，对玻璃的附着力为0级。 关键字：桐油；Diels-Alder；光引发剂；自由基聚合；紫外光固化中图分类号：O632.12 文献标识码：A Preparation and Properties of Tung Oil-based Photoinitiators LI Cui-hua, ZHOU Hong-yong, WANG Jia-xi* (School of Chemical Engineering and Technology, Hebei University of Technology, Tianjin 300130, China) Abstract: Tung oil anhydrides（TOM1~TOM3）and tung acid anhydride (TAM) were synthesized from tung oil (TO) and tung acid (TA) with maleic anhydride (MA) via the Diels-Alder reaction. Then the obtained compounds reacted with the hydroxyl groups of 2-hydroxy-4-(2-hydroxyethoxy)-2-methylpropiophenone (Irgacure2959) to produce four cleavage photoinitiators (TOMG1~TOMG3, TAMG) in the presence of catalytic amount of triethylamine. Theses initiators were characterized by FTIR, 1HNMR and HRMS spectroscopy. Their decomposition processes were investigated by UV visible spectroscopy. The photopolymerization dynamics of 1, 6-hexanediol diacrylate (HDDA) initiated photoinitiators were studied using real-time FTIR technology. The results showed that initator TOMG3 had the best photoinitiation performance among Irgacure 2959 and the tung oil modified photoinitiators. The mixture of HDDA, PUA (polyurethane acrylate) and TOMG3 in a mass ratio of 46:46:8 could be cured within 60 s under ultraviolet light irradiation with an intensity of 28 mW/cm2, and the gelation rate reached 96%. The hardness, flexibility and