响应曲面法优化(salen)Co(Ⅲ)(OAc)拆分手性环氧氯丙烷的制备工艺  

Optimization via response surface method for (salen)Co(III)(OAc) catalyzed preparation of chiral epichlorohydrin

作　　者：卢定强[1,2] 涂清波[1] 凌岫泉[1] 王俊[1] 梅巧婷[1] 

机构地区：[1]南京工业大学药学院,江苏南京210009 [2]江苏省药物研究所,江苏南京210009

出　　处：《化工进展》2010年第2期313-318,共6页Chemical Industry and Engineering Progress

基　　金：国家自然科学基金(20676060);国家重点基础研究发展计划(2009CB724700)资助项目

摘　　要：以(salen)Co(Ⅲ)(Oac)为催化剂不对称选择性水解制备手性环氧氯丙烷,采用响应曲面法中的Box-Behnken设计对影响手性环氧氯丙烷光学纯度的4个主要因素(反应温度、水用量、催化剂用量、反应时间)进行优化,建立手性环氧氯丙烷光学纯度的二次多项回归模型方程,并对回归系数进行显著性检验和方差分析。实验结果表明,当反应温度为46.02℃、水与环氧氯丙烷的摩尔比为61.10、催化剂与环氧氯丙烷的摩尔比为0.003937、反应时间为18h时手性环氧氯丙烷的光学纯度最高,最高光学纯度预测值为102.18%,与实测平均值99.61%基本相符,优化模型有效可靠。The preparation of chiral epichlorohydrin was studied by using asymmetric hydrolysis with （salen）Co（III）（OAc） catalyst. The influences of temperature,catalyst and water amount and reaction time on the optical purity of the produced epichlorohydrin were optimized with Box-Behnken mode of response surface method. A mathematical regression model for the optical purity of chiral epichlorohydrin was established,and the significance test and variance analysis for the regression equation were also analyzed. Results showed that the optimum conditions for the optical purity of chiral epichlorohydrin are：the temperature is 46.02 ℃,the molar ratio of water to epichlorohydrin is 61.10, the molar ratio of catalyst to epichlorohydrin is 0.003937 and the reaction time is 18 h. The predicted optimum optical purity of chiral epichlorohydrin is 102.18%,which is in consistent with the average measured value of 99.61%. Therefore,the regression equation is valid and reliable.

关 键 词：手性 环氧氯丙烷 (salen)Co(Ⅲ)(Oac) 响应曲面法 

分 类 号：TQ231.1[化学工程—有机化工]