歧化松香(丙烯酸-2-羟基乙基酯)酯的合成

林明涛1， 储富祥1*， 马 丽1，2， 周道兵1，王基夫1， 王春鹏1

（1．中国林业科学研究院林产化学工业研究所；国家林业局林产化学工程重点开放性实验室，江苏南京210042； 2．南京林业大学化学工程学院，江苏南京210037）

摘 要： 通过对歧化松香（DPR）分别进行酰氯化和酯化反应成功制备了DPR（丙烯酸-2-羟基乙基酯）酯。考察了反应过程中反应温度、反应时间以及原料物质的量之比对DPR酰氯化反应的影响，确定了DPR酰氯化反应的最佳条件（DPR与三氯化磷（PCl3）的物质的量比为1∶0.33，反应温度50℃，反应时间3h)，并对DPR酰氯的酯化反应进行了研究。实验结果表明：温度对于DPR酰氯化反应的影响较小；而原料物质的量之比对反应程度的影响较大，PCl3用量的增加有利于反应程度的增加。实验结果还显示IR、13C NMR和GC-MS联用分析技术可有效地对反应过程进行跟踪。
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关键词： 歧化松香；丙烯酸-2-羟基乙基酯；酰氯；酯化

中图分类号：TQ351.471      文献标识码：A      文章编号：0253-2417(2006)04-0043-05

Study on the Synthesis of Disproportionated Rosin (2­Hydroxyethyl Acrylate) Ester

LIN Ming­tao1, CHU Fu­xiang1, MA Li1,2, ZHOU Dao­bing1, WANG Ji­fu1, WANG Chun­peng1

(1. Institute of Chemical Industry of Forest Products,CAF; Key and Open Lab. on Forest Chemical Engineering,SFA,  Nanjing 210042, China；2.College of Chemical Engineering,Nanjing Forestry University, Nanjing 210037, China)

Abstract: Disproportionated rosin (DPR) (2­hydroxyethyl acrylate) ester was synthesized by acyl chlorination and esterification of DPR acid. The influences of temperature, reaction time and molar ratio of the reaction were studied by monitoring the course of reaction.The optimum conditions of acyl chlorination and esterification were investigated as follows: molar ratio of DPR to PCl3 1∶0.33, reaction temperature  50℃ and reaction time 3 h. It was found that  temperature had no significant effect on acylation of DPR, and the increase of molar ratio of PCl33 had a positive impact on the reaction degree. The results also showed that IR,13C NMR and GC­MS were effective methods for tracking the course of acylation and esterification reaction.
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Key words: disproportionated rosin;2­hydroxyethyl acrylate;acyl chlorination;
esterification