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MDS-6制备离子液体最佳条件探索

The optimal conditions exploration of preparation of ionic liquids by MDS-6

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【作者】 周璐蒋荣立张豪非刘静王玲

【Author】 Zhou Lu Jiang Rongli Zhang Haofei Liu Jing Wang Ling(School of Chemical Engineering and Technology, China University of Mining & Technology,Xuzhou 221008)

【机构】 中国矿业大学化工学院

【摘要】 以N-甲基咪唑,溴代正丁烷,四氟硼酸钠为原料,采用两步法合成咪唑基离子液体1-丁基-3-甲基咪唑四氟硼酸盐(bmimBF4),重点对产物的最佳合成方法、最佳反应时间、最佳反应温度进行了探索。实验结果表明,使用微波消解仪(MDS-6)能快速有效地合成离子液体,且最佳的合成条件为:当微波功率400W,甲基咪唑与溴代正丁烷的摩尔比为1∶1.1,反应时间45min,微波反应温度80℃时,中间体bmimBr的合成最理想;当bmimBr与NaBF4的摩尔比1∶1.2,微波反应温度65℃,反应时间60min时,离子液体bmimBF4产率达到90%左右。试验产物用IR进行了确认。所制备的离子液体为后面制备四氧化三铁纳米空心球做准备。

【Abstract】 Ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate(bmimBF4)has been synthesized through two step methods under microwave irradiation using n-methylimidazole,1-bromobutane and sodium fluoroborate as raw materials,and the experiments were mainly explored the effects of reaction methods,reaction time and reaction temperature on the synthesis of ionic liquid.The results showed that bmimBF4 was synthesized effectively by MDS-6.The optimum synthetic conditions were obtained as follows:the molar ratio of n-methylimidazole to 1-bromobutane was 1∶1.1,reaction time was 45min,reaction temperature was 80℃,microwave power was 400W,under which the yield of bmimBr was best,while in the second step,the molar ratio of bmimBr to NaBF4 was 1∶1.2,reaction time was 60min,reaction temperature was 65℃,microwave power was 400W,under which the yield of bmimBF4 amounted to about 90%.The target product was characterized by IR.The synthetic ionic liquids would be used to the subsequent preparation of Fe3O4 hollow nanospheres.

【关键词】 离子液体微波法合成
【Key words】 ionic liquidmicrowave methodsynthesis
【基金】 高等学校博士学科点专项科研基金(20100095110009);中央高校基本科研业务费专项基金(2010LKHX05)
  • 【文献出处】 化工新型材料 ,New Chemical Materials , 编辑部邮箱 ,2012年08期
  • 【分类号】O626.23
  • 【被引频次】4
  • 【下载频次】80
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