稀土固体超强酸S_2O_8^(2-)/ZrO_2-La_2O_3催化合成柠檬酸三丁酯  

Synthesis of Tributyl Citrate Catalyzed by Rare Earth Solid Superacid S_2O_8^(2-)/ZrO_2-La_2O_3

作　　者：刘建平[1] 吴丽丽[1] 张俊俊[1] 徐培飞[1] 

机构地区：[1]华东交通大学化学化工系,江西南昌330013

出　　处：《华东交通大学学报》2015年第3期108-113,共6页Journal of East China Jiaotong University

摘　　要：以柠檬酸和正丁醇为原料,在稀土超强酸S2O82-/Zr O2-La2O3的催化下合成柠檬酸三丁酯。通过XRD和红外光谱确定了稀土元素La的掺量对催化剂结构的影响,用正交优化实验优化了催化剂用量、酸醇摩尔比、反应时间等对酯化率的影响。实验结果表明:La掺量为0.07 mol·L-1所得催化剂性能最佳,柠檬酸三丁酯最优催化合成条件为反应温度175℃,醇酸摩尔比4.0∶1,催化剂用量为柠檬酸质量的2.0%,反应时间180 min,酯化率可达98.27%。催化剂可循环使用5次而不会明显降低活性。经折光率、红外光谱、核磁共振氢谱和碳谱测定,所合成产物为柠檬酸三丁酯。Tributyl citrate（TBC） was synthesized by reaction of citric acid with n-butanol using rare earth solid su- peracid S2O8（2-）/ZrO2-La2O3 as the catalyst. Effects of La content on the catalyst structures were determined by using XRD and FT-IR. Effects of catalyst dosage, molar ratio of n-butanol to citric acid, reaction time on the esterifica- tion rates were explored by orthogonal experiment. Results show that the catalyst can present the best behavior under concentration of the La content of 0.07 mol·L-1. The optimum synthesis condition of TBC adds 4 times of n-bu- tanol to citric acid, under the condition of temperature 175℃ for 180 min using 2.0 wt% catalyst, with the yield of ester reaching 98.27%. The catalyst can be reused for 5 times without significant decline in its behavior. The structure of the product was qualitatively analyzed by refractive index, FT-IR, tH-NMR, and 13C-NMR.

关 键 词：柠檬酸三丁酯 稀土固体超强酸 S2O82-/ZrO2-La2O3 酯化率 

分 类 号：TQ225.2[化学工程—有机化工] TQ414