N-正丁基吡啶四氟硼酸盐离子液体的合成  

Synthesis of N-butyl Pyridine Tetrafluoroborate Ionic Liquid

作　　者：彭全明[1] 王磊[1] 于娜[1] 李成[1] 

机构地区：[1]上海应用技术学院化学与环境工程学院,上海201418

出　　处：《上海应用技术学院学报（自然科学版）》2014年第1期20-23,共4页Journal of Shanghai Institute of Technology: Natural Science

基　　金：上海市大学生创新项目(PE2013029)

摘　　要：以吡啶、氟硼酸钠和氯代正丁烷为反应物,采用两步法成功合成了N-正丁基吡啶四氟硼酸盐(BPyBF4)离子液体.首先氯代正丁烷和吡啶反应合成中间体氯代N-正丁基吡啶(BPyCl),应用L9(34)正交表进行条件优化,确定最佳条件为反应时间16h、反应温度80℃、n(氯代正丁烷)∶n(吡啶)=1∶1及溶剂乙腈用量20mL;然后中间体再和氟硼酸钠进行离子交换,得到目标产物BPyBF4,同样应用L9(34)正交表进行条件优化,确定最佳条件为n(NaBF4)∶n(BPyCl)=1.4∶1、溶剂丙酮用量40mL、反应温度40℃及反应时间30h.两步反应总收率达79%.BPyCl和BPyBF4的结构均经X射线能谱仪(EDX)和氢核磁共振波谱(1 H-NMR)表征.N-butyl pyridine tetrafluoroborate ionic liquid was successfully synthesized from pyridine,chlorinated N-butane and tetrafluoroboric acid in two steps.Firstly,the intermediates chlorinated N-butyl pyridine(BPyCl)was synthesized from pyridine and chlorinated N-butane.Orthogonal table L9(34)was applied into the optimization of condition,and the optimum conditions were determined as 16hreaction time,reaction temperature 80℃,n(sodium tetrafluoroborate)∶n(N-butyl pyridine chloride)=1∶1and the dosage of solvent acetonitrile 20 mL.Then intermediates and fluoboric acid sodium ion were exchanged,finally obtaining the target product BPyBF4,also orthogonal table L9(34)was applied into the optimization of condition.The optimum conditions were determined as n(NaBF4)∶n(BPyCl)=1.4∶1,the dosage of solvent acetone 40mL,reaction temperature 40℃and reaction time to 30h.The total yield of the two steps reached 79%.The structures of BPyCl and BPyBF4 were both well characterized by the EDX and 1 H-NMR.

关 键 词：正交试验 N-正丁基吡啶四氟硼酸盐离子液体 合成 

分 类 号：O645.1[理学—物理化学]