PBF的合成及其复合材料的光/热固化

Synthesis and Thermo-/UV-curing Behavior of Poly(butyl fumarate)-based Composites

摘要:

以富马酸二乙酯和1,4-丁二醇为基本原料，通过两步反应成功合成聚富马酸丁二醇酯（PBF）。利用FTIR、1HNMR、GPC、TG及DSC等手段对聚合物进行了表征。依据反应机理探讨了反应时间、温度及醇的用量对聚合物产率的影响。结果表明，当反应温度为130 ℃，反应时间为8 h，n（富马酸二乙酯）：n（1,4-丁二醇）=1:3时得到适当分子质量（Mn=2773）和较高产率（61.94%）的PBF。分别采用光固化和热固化工艺制备了PBF/N-乙烯基吡咯烷酮（NVP）复合材料，并探究了引发剂用量对复合材料交联固化程度的影响。结果表明：当光引发剂（2,4,6-三甲基苯甲酰基）苯基氧化磷（BAPO）的质量分数为2.5%，热引发剂过氧化苯甲酰（BPO）的质量分数为3%〔N,N-二甲基对甲苯胺（DMT）质量分数为0.2%〕时，交联固化效果较佳。

Abstract:

Poly(butyl fumarate) (PBF) was successfully synthesized by two-step reaction with diethyl fumarate and 1,4-butanediol as basic raw material. The polymers were characterized by FTIR, 1HNMR, GPC, TG and DSC. The effects of reaction parameters on the yield of PBF were studied. Based on the polymerization mechanisms, the reaction time, temperature and doses of alcohol were investigated to achieve maximum polymer yield. The results suggested that the appropriate molecular weight (Mn=2773) and higher yield (61.94%) of PBF are obtained when the molar ratio of diethyl fumarate and 1,4-butanediol is 1:3, the reaction temperature is 130 ℃ and the reaction time is 8 h. PBF/N-Vinyl-2-pyrrolidone (NVP) composite was prepared by UV-curing and thermo-curing respectively. And the effects of initiator dosage on crosslinking and curing degree of the composite were also investigated. The results showed that crosslinking and curing effect of the composite were better, when the dosage of photoinitiator and thermal initiator were 2.5% phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide (BAPO) and 3% benzoyl peroxide (BPO) [0.2% N,N-Dimethyl-p-toluidine (DMT)], respectively.