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作 者:邓运泉[1] 方岩雄[1] 任清刚[1] 张金玲[1] 徐学涛[1]
出 处:《应用化学》2008年第10期1138-1141,共4页Chinese Journal of Applied Chemistry
基 金:国家自然科学基金(20376015);广东省基金(32491);广州市科技计划(2004J1-C0151)资助项目
摘 要:制备了8种不同链长的溴化烷基咪唑盐和4种丁基类甲基咪唑六氟磷酸盐、四氟硼酸盐、全氟丁基磺酸盐及氯化盐离子液体,研究了咪唑盐类离子液体催化邻二甲苯、氯化氢、多聚甲醛为起始原料的氯甲基化反应。考察了离子液体类型、催化剂用量、反应温度及反应时间对反应的影响。反应产物采用气相色谱法进行定量分析;采用GC-MS测试技术进行了定性分析。结果表明,[C12mim]Br(溴化1-十二烷基-3-甲基咪唑盐)是最适合的催化剂。其最佳反应条件是:离子液体摩尔分数为4%(与邻二甲苯的摩尔比),温度70℃,反应时间10 h,产物收率可达89.8%,TON数达到22.4。1-Butyl-3-methyl imidazolium salts with hexafluorophosphate,tetrafluoroborate,perfluorobutyl sulphonate,and chloride anions and eight kinds of alkylimidazolium bromide salts with different alkyl chain length were prepared.The Blanc chloromethylation of o-xylene with hydrogen chloride and paraformaldehyde was investigated in the presence of the above ionic liquids as catalysts.The influence of the type and the amount of the ionic liquid,reaction temperature,and reaction time on the chloromethylation was investigated.The products were analyzed by GC-MS.The results showed that 1-dodecyl-3-methylimidazolium bromide([C12mim]Br) was the best one among the catalysts for the reaction.The optimum reaction conditions were 4%(the molar ratio of ionic liquid to o-xylene) ionic liquid,70 ℃ reaction temperature and 10 h reaction time.Under the above reaction conditions,the yield was 89.8%,and the turnover number was 22.4.
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