脱氢枞酸基甲基丙烯酸酯单体的合成和表征

Synthesis and Characterization of 2-Methacryloyloxyisopro-panol Ester of Dehydroabietic Acid

以脱氢枞酸(DA)和甲基丙烯酸缩水甘油酯(GMA)为原料,通过酯化反应合成了脱氢枞酸(2-甲基丙烯酰氧基异丙醇基)酯(DAGMA),探讨了反应时间、反应温度、催化剂种类及催化剂用量对合成DAGMA的影响,对DAGMA的结构和性能分别采用FT-IR、~1H NMR、^(13)C NMR、DSC、和GPC进行表征。研究结果表明:DAGMA较适合的合成条件为n(AD)∶n(GMA)1∶1,以三乙胺作催化剂,用量为脱氢枞酸质量的2%,反应时间5 h,反应温度120℃,酯化率约为85%。DSC分析显示,在引发剂AIBN存在下,DAGMA可发生聚合反应,得到均聚物的重均相对分子质量(M_w)23 900,数均相对分质量(M_n)12 254,玻璃化转变温度(T_g)为62.61℃。

2-Methacryloyloxyisopropanol ester of dehydroabietic acid （DAGMA） was synthesized by esterification of dehydroabietic acid and glycidyl methacrylate. The effects of reaction time, reaction temperature, amount and type of catalyst on the yield of dehydroabietie acid derived monomer were investigated. The resulting product was then characterized by FT-IR, 1^H NMR, 13^C NMR, DSC and GPC respectively. The results showed that the optimal conditions for the reaction were as follows： triethylamine as catalyst at an amount of 2% of dehydroabietic acid, reaction time 5 h, reaction temperature 120 ℃, and the esterification rate was about 85%. DSC test showed that in the presence of initiator AIBN, the suitable conditions for synthesis of DAGMA was n（ DA）： n（GMA） 1： 1. It showed that DAGMA could be polymerized in the presence of initiator. The weight average molecular weight （ Mn ） of the asprepared homopolymer was 23 900, the number average molecular weight （ Mn） was 12 254, and its glass transition temperature was around 62. 61 ℃.