摘要
以KOH或NaOH作碱试剂,考察了溶剂对1-丁基-3-甲基咪唑溴鎓([bmim]Br)合成1-丁基-3-甲基咪唑锚氢氧化物([bmim]OH)碱性离子液体的影响,并采用强碱性阴离子交换树脂法合成[bmim]OH。结果表明:在室温下,溶剂10mL,[bmim]Br和KOH的物质的量之比为1:1.1的条件下,以乙醇为溶剂反应2h和以异丙醇为溶剂反应0.5h,[bmim]Br的转化牢分别为96%和98%,[bmim]OH的产率分别为95%和97%,且没有副产物生成;1 mmol[bmim]Br和1.1~1.4g717。强碱性例离子交换树脂,分别以10mL水、甲醇和异丙醇为溶剂,并采用层析牲中静态反应和烧瓶中动态反应方式在室温下反应,反应时间分别为0.25和0.5h,[bmim]Br的转化率达到100%,[bmim]OH的产率为96%以上,且没有副产物生成;717^#强碱性阴离子交换树脂重复使用性能较好,重复使用3次后,反应的转化率和产牢分别达到100%;N96.4%。在同样条件下,利用强碱性阴离子交换树脂法以层析柱中静态反应方式合成1-乙赫-3-甲基咪唑鎓氯氧化物[emim]OH、乙基吡啶黠氢氧化物[epy]OH和丁基吡啶锚氢氧化物[bpy]OH碱杜离子液体,反应转化率为100%,产率为97%以上。
The effects of different solvents on synthesis of base functional ionic liquid l-butyl-3-methyl imidazolium hydroxide([bmim]OH) from 1-butyl-3-methyl imidazolium bromine ([bmim]Br) using KOH or NaOH as base agent were investigated and strong-base anion exchange resin was used to prepare [bmim]OH. The results showed that under the conditions of room temperature, molar ratio of [bmim]Br to KOH 1: 1.1, solvent 10 mL, the conversion of [bmim]Br and the yield of [bmim]OH could reach 96% and 95%, respectively, when the solvent was alcohol and reaction time was 2 h, while the conversion and the yield could reach 98% and 95%, respectively, when the solvent was isopropanol and reaction time was 0.5 h, and there was no byproduct. The conversion of 100% and the yield of 97% were obtained and there was no byproducts by using 717# strong-base anion exchange resin instead of KOH in column chromatography static reaction for 0.25 h or in flask dynamic reaction after reaction for 0.5 h, respectively, in l0 ml water, methanol and ethanol at room temperature when solvent was 10 mL, [bmim]Br l mmol and resin 1.1-1.4 g. And the conversion of [bmim]Br and yield of [bmim]OH could reach 100% and 96.4% after the 717# strong-base anion exchange resin was used 3 times. Under the same conditions, 1-ethyl-3-methylimidazolium hydroxide ([emim]OH), ethyl pyridinium hydroxide([epy]OH), and butyl pyridinium hydroxide([bpy]OH) were synthesized using the resin static reaction pattern, and the conversion was 100% and the yield was above 97%.
出处
《化学反应工程与工艺》
CAS
CSCD
北大核心
2011年第4期316-321,共6页
Chemical Reaction Engineering and Technology
基金
贵州省科技基金(黔科合J字[2008]2022)
贵州大学引进人才基金(贵大基合字20071051)