摘要
探讨了以一水合硫酸氢钠+六水合氯化铁为复合催化剂,柠檬酸、正丁醇为原料合成柠檬酸三丁酯的绿色合成工艺条件,着重考察各因素对柠檬酸转化率的影响。通过四因素三水平的正交试验优化,确定的最佳反应条件为:当柠檬酸用量控制为0.1mol时,醇酸物质的量比为4.0:1,复合催化剂(NaHSO_4·H_2O+FeCl_3·6H_2O)配料的摩尔比为n(NaHSO_4·H_2O):n(FeCl_3·6H_2O)=1.5:1,催化剂用量为反应物总质量的2.0%,反应温度为135～145℃,反应时间为2.0h,在此条件下柠檬酸的转化率可达98.8%以上。
The green technics condition was discussed that the tributyl citrate was synthetized with citric acid and n-butyl alcohol use the NaHSO4·H2O＋FeCl3·6H2O as the composite catalyst. The effects of reaction conditions on the esterification rate were investigated. The optimum reaction conditions were obtained as follows： When the amount of citric acid was 0.10mol, The molar ratio of n-butyl alcohol to citric acid was 4.0：1.The molar ratio of the composite catalyst （NaHSO4·H2O＋FeCl3·6H2O） was, n （NaHSO4·H2O）：n （FeCl3- 6H2O）= 1.5：1, the quantity of composite catalyst was equal to 2.0% by mass of the total feed stock. ,reaction temperature 135-145℃,reaction time 2.0h,the conversion rate of citric acid was more than 98.8%.
基金
湖南省教育厅优秀青年科研基金项目(06B089)
