摘要
采用纯度较高的VE琥珀酸单酯作为原料、对甲苯磺酸作为催化剂与聚乙二醇1 000进行酯化反应得到TPGS.通过考察初始原料比、催化剂用量、反应温度和反应时间对酯化反应的影响,发现初始原料比、催化剂用量和反应温度对酯化反应的影响比较显著,而当反应达到平衡时,反应时间对结果影响不大.因此又采用正交设计对优化TPGS的合成工艺,得到最佳工艺为反应时间为4 h、反应温度为110℃、催化剂用量为0.5 g和原料配比为2∶1.考察其重现性,得到平均转化率为95.261%、选择率为94.280%、收率为95.067%.
TPGS was synthesized with α-tocopherol succinate (VES) and polyethylene glycol 1 000 (PEG1000) by p -toluenesulfonic acid esterification. In order to improve the reaction yield, the process parameters such as convert ratio, selection rate and molar ratio of VES to PEG1000, initiation raw material configuration, amount of catalyst, reaction time and reaction temperature were studied. The results displaied the factors except for reaction time had remarkable effect. While the reaction time had little effect on esterification, when the reaction reached the balance. Synthesis process of TPGS was optimized by means of orthogonal design, the best extraction condition was as follows : reaction time 4 h, reaction temperature 110 ℃, amount of catalyst 0.5 g and initiation raw material configuration 2: 1. Finally, the average convert rate of 95. 261% ,the section rule of 94. 280% and the average yield of 95. 067% were achieved.
出处
《安徽大学学报(自然科学版)》
CAS
北大核心
2010年第5期79-84,共6页
Journal of Anhui University(Natural Science Edition)
基金
2009年浙江省高等学校青年骨干教师国内访问学者资助项目