摘要
以简化的新合成路线合成了溴化1-丁基-3-甲基咪唑盐及1-丁基-3-甲基咪唑六氟磷酸盐室温离子液体,并对其纯度进行核磁表征,以使该室温离子液体满足电化学电解质溶剂纯度要求。采用两锅法,在50℃,反应4h,常温反应8h,惰性气体保护,较温和的方法合成中间体[BMIM]Br;常温,不用惰性气体保护,复分解反应2～4h合成离子液体;采用乙酸乙酯、二氯甲烷、二次重蒸水和无水硫酸镁作为提纯试剂,旋转蒸发仪为仪器对中间体及室温离子液体进行提纯;用循环伏安电位扫描法测试电化学窗口。产物合成产率在90%以上,电化学窗口-2.0V～+1.4V,无明显氧化还原电流,达到电化学纯度,其电化学性能稳定。该合成方法简单可行,提纯方法合理、巧妙,该离子液体可以用作电解质溶剂。
Bromination 1-butyl-3-methyl imidazole salt and room temperature ionic liquid 1-ethyl-3-methyl-imimidazolium hexafluorophosphate [BMIM]PF6 have been synthesized in two reactors by new mild simplified synthetic route. Under the inert gas protection,the intermediate [BMIM]Br was synthesized by temperate method; Metathesis reaction 2-4 h and synthesis ionic liquid at the normal temperature without the inert gas protecting at 50 ℃ responded 4 h,and at the room temperature responded 8 h; The intermediate and the room temperature ionic liquid were purified using ethyl acetate,methylene chloride,water and anhydrous magnesium sulfate as the depuration reagent. The stable potential windows were tested by cyclic voltammetry sweep on GCE glassy carbon electrode. The results showed that the yield of the production is above 90%,and the electrochemical window -2.0V—＋1.4 V. This synthesis method simple feasible achieves,the electrochemistry purity,[BMIM]PF6 may be served as electrolyte solvent.
基金
科技攻关与新产品试制资助项目(桂科攻0815005-1-17)
广西壮族自治区自然科学基金资助项目(桂科自0728229)
