溶剂法合成脱氢枞酸/甲基丙烯酸缩水甘油酯酯化物  

Synthesis of ester of dehydroabietic acid and glycidyl methacrylate by solvent

作　　者：许建本 郑燕菲 钟昌玲 农克良 XU Jian-ben;ZHENG Yan-fei;ZHONG Chang-ling;NONG Ke-liang(College of Chemistry and Chemical Engineering,Guangxi Normal University for Nationalities,Chongzuo 532200,China;Guangxi Colleges and Universities Key Laboratory Breeding Base of Chemistry of Guangxi Southwest Plant Resources,Chongzuo 532200,China)

机构地区：[1]广西民族师范学院化学化工学院,广西崇左532200 [2]广西高校桂西南特色植物资源化学重点实验室培育基地,广西崇左532200

出　　处：《分子科学学报》2020年第5期422-427,I0005,共7页Journal of Molecular Science

基　　金：广西民族师范学院科研经费资助项目(2018YB018);广西高校中青年教师基础能力提升项目(2018KY0637);大学生创新创业训练计划项目(201810604076)。

摘　　要：以脱氢枞酸(DHR)和甲基丙烯酸缩水甘油酯(GMA)为原料,对苯二酚(HQ)为阻聚剂,三乙胺为催化剂,采用溶剂法研究了合成脱氢枞酸/GMA酯化物(DG)的过程中反应温度、单体配比[n(GMA)∶n(DHR)]、催化剂用量和反应时间对酯化反应的影响.在单因素实验的基础上,利用正交实验对合成条件进行了优化.采用红外光谱、核磁氢谱和热重对DG进行表征.结果表明:成功合成了含羟基的DG,其热稳定性较好;酯化反应的较优条件为反应温度120℃,n(GMA)∶n(DHR)=1.2∶1,三乙胺用量为DHR质量分数的0.5%,反应时间为4 h,该条件下合成的DG酯化率达到99.4%.By using dehydroabietic acid(DHR) and glycidyl methacrylate(GMA) as raw materials, hydroquinone as polymerization inhibitor, and triethylamine as catalyst, a dehydroabietic acid derived GMA ester(DG) was prepared by solvent method. The effects of reaction temperature, monomer ratio, catalyst dosage and reaction time on the esterification reaction were investigated by single-factor test, and the experimental conditions were optimized by orthogonal experiment. The DG was characterized by FT-IR, ~1H NMR and TG. The results showed that DG with good thermal stability were successfully prepared and containing a hydroxyl group. The optimum conditions for the reaction were as following: reaction temperature of 120 ℃, molar ratio of GMA and DHR at 1.2∶1, triethylamine mass of 0.5%(based on DHR weight), and reaction time of 4 h. Under these conditions, the esterification rate of the DG was up to 99.4%.

关 键 词：脱氢枞酸 甲基丙烯酸缩水甘油酯 溶剂法 酯化物 

分 类 号：O636[理学—高分子化学]