枞酸烯丙酯的制备、表征及UV固化性能研究

The synthesis,characterization and UV curing application of allyl abietate

以枞酸为原料先制备得到枞酸钠水溶液,后在此反应液中加入一定量的十六烷基三甲基溴化铵(CTAB)为催化剂和对苯二酚为阻聚剂,在微波辅助的条件下边搅拌边滴加氯丙烯,微波功率400 W,反应温度50℃,反应时间30 min,氯丙烯与枞酸钠物质的量之比2.5∶1,催化剂用量为原料质量的4%,在此条件下得到的枞酸烯丙酯得率为94.4%。采用GC、GC-MS、FTIR、~1H NMR、^(13)C NMR和元素分析对产物结构进行了表征,所得枞酸烯丙酯GC纯度为89.5%。经过分析,证明产物的结构和目标合成物结构一致。紫外光(UV)固化反应的结果表明,枞酸烯丙酯作为聚合单体有较强的聚合活性,所得聚合物热稳定性较好,初始热分解温度和玻璃化转变温度分别为218℃和22.32℃。枞酸烯丙酯UV固化产物的数均相对分子质量为4 176,数均聚合度约为12。

Sodium abietate was synthesized through neutralization reaction by using abietic acid and sodium hydroxide. The synthesized sodium abietate can be further converted into allyl abietate by using hexadecyl trimethyl ammonium bromide as catalyst and hydroquinone as polymerization inhibitor. The optimum reaction conditions were obtained as follows： the microwave power was 400 W, the reaction temperature was 50℃, the reaction time was 30 min, the molar ratio of allyl chloride to sodium abietate was 2.5：1, and the catalyst amount was 4%. The target product was separated by phase separation with the yield of 94.4%. Chemical structure of allyl abietate was confirmed by infrared spectrum, mass spectrometry, elemental analysis, hydrogen nuclear magnetic and carbon nuclear magnetic spectroscopy. The results of the ultraviolet（UV）test indicated that the cured product exhibited excellent thermal stability. The initial decomposition temperature（Tdi）and the glass transition temperature of UV cured products were 218℃ and 22.32℃, respectively. The relative molecular mass of UV cured product was 4 176 with polymerization degree of 12.