微波辅助合成碱性离子液体[Bmim]OH机理探讨  

Study on the Microwave-assisted Synthesis and Mechanism of a Hydroxide 1-butyl-3-methyl-imidazole

作　　者：谢亚丽[1] 李学琴[1] 曹玲[1] 耿莉莉[1] 程建文[1] 晁群[1] Xie Yali Li Xueqin Cao Ling Geng Lili Cheng Jianwen Chao Qun(Institute of Chemistry, Changji College, Changji 831100, China)

机构地区：[1]昌吉学院化学与应用化学系,新疆昌吉831100

出　　处：《山东化工》2017年第1期1-4,共4页Shandong Chemical Industry

基　　金：新疆维吾尔自治区大学生创新创业训练计划项目(201510997010);昌吉学院科研基金资助项目(2012YJYB004)

摘　　要：本文首先通过两步合成法合成碱性离子液体[Bmim]OH。第一步制备中间体[Bmim]Br,研究了不同的辅助手段、料液比及反应条件对[Bmim]Br产率的影响。结果表明,在氮气微波辅助的条件下,温度60℃,咪唑和溴代正丁烷的物质的量比为1∶1.3,反应时间为1h时产率最高为94.0%,并从过渡态离域性对活化能的影响解释这一结果。第二步由中间体[Bmim]Br与KOH的反应制备[Bmim]OH,研究了碱化配比、碱化时间对[Bmim]OH产率的影响。结果表明碱化配比为1∶1.4、碱化时间应控制在10 h,碱性离子液体[Bmim]OH产率最高为:54.98%。并采用核磁及红外手段对产物进行结构表征。同时对其主要物理性质进行测定,结果表明:碱性离子液体[Bmim]OH密度为:1.1713 g/m L,易溶于水、甲醇等极性较大的溶剂。1 - Butyl - 3 - methylimidazolium hydroxide （ [ Bmim ] OH） basic ionic liquid were synthesized under the conditions of ultrasound with two - step method. Firstly, the main factors effected on the yield of [ Bmim ] Br were discussed including the Ultrasonic - assisted method, the reaction molar - ratio, reaction time, reaction temperature etc.. The optimal conditions were about molar - ratio 1 ： 1.3, reaction time 1 h, pH 7.5, temperature 60 %：, and the yield was 94.0%. The studies may provide a theoretical explaining from the effects of the transition state Electron delocalizability for activation energy. Finally, [ Bmim ] OH were synthesized with [ Bmim ] Br and KOH. The main factors effected on the yield of the [ Bmim ] OH were discussed such as the alkali ratio and alkalization time. The optimum synthesis conditions of alkaline ionic liquid were about [ Bmim ] Br and KOH molar - ratio 1 ： 1.4, reaction time 10 h, the intermediate production - rate can reach 54.98% ; At the same time, [ Bmim ] OH was characterized and analyzed with a FI＇IR and 1H NMR, and the main physical properties were determined,The results showed that its Density was 1. 1713 g/mL and Soluble in water, methanol and other polar solvents.

关 键 词：微波辅助 [Bmim]OH 机理 表征及性能测定 

分 类 号：TQ413.2[化学工程]