苯并噻唑离子液体的合成及其在间氯苯甲醛乙二醇缩醛反应中的应用  

Synthesis of Benzothiazole Ionic Liquid and its Application in m-Chlorobenzaldehyde Glycol Acetal Reaction

作　　者：梁秋月 王楠 戎有明 马全红[1] 周建成 李乃旭[1,2] Liang Qiuyue;Wang Nan;Rong Youming;Ma Quanhong;Zhou Jiancheng;Li Naixu(School of Chemistry and Chemical Engineering,Southeast University,Jiangsu Nanjing 211189;Nanjing Zhongwei Nano Functional Materials Research Institute Co. Ltd, Jiangsu Nanjing 210044)

机构地区：[1]东南大学化学化工学院,江苏南京211189 [2]中微纳米功能材料研究院有限公司,江苏南京210044

出　　处：《化工时刊》2022年第6期10-15,共6页Chemical Industry Times

摘　　要：以廉价的苯并噻唑为原料,使用H_(2)SO_(4)处理后得到了酸性离子液体[HBth]-HSO_(4)。通过FT-IR、^(1)HNMR对产物的结构进行表征,并对其溶解性、酸性和热稳定性进行考察。对以自制离子液体[HBth]-HSO_(4)催化的间氯苯甲醛和乙二醇合成间氯苯甲醛乙二醇缩醛的反应进行研究,考察了催化剂用量、原料配比、带水剂用量和反应时间对产率的影响。结果表明:当[HBth]-HSO_(4)用量为间氯苯甲醛的2%,醇醛比为1.4∶1,带水剂甲苯用量为醛的2倍,反应时间为3 h时,产物收率达97.3%,与浓硫酸催化效果相当。该催化剂保持了传统酸催化剂的高催化活性,在反应后经简单处理即可回收,同时在循环五次后,仍可保持较高的催化活性(收率>95%),为缩醛合成提供了一条高效、绿色、低成本的方法,具有良好的工业化潜力。The acidic ionic liquid([HBth]-HSO_(4))was prepared from cheap benzothiazole using H_(2)SO_(4) treatment.The structure of the ionic liquid was characterized by FT-IR and ^(1)HNMR,and the solubility,acidity and thermal stability were investigated.The synthesis of m-chlorobenzaldehyde glycol acetal catalyzed by home-made ionic liquid([HBth]-HSO_(4))with m-chlorobenzaldehyde and ethylene glycol was studied to investigate the effect of catalyst dosage,feedstock ratio,amount of water-carrying agent and reaction time on the yield.The results showed that when the amount of[HBth]-HSO_(4) was 2%of m-chlorobenzaldehyde,the alcohol to aldehyde ratio was 1.4∶1,the amount of toluene was twice that of aldehyde and the reaction time was 3 h,the product yield reached 97.3%,which was comparable to the catalytic effect of concentrated sulfuric acid.The catalyst maintains the high catalytic activity of conventional acid catalysts and can be recovered by simple treatment after the reaction,while maintaining high catalytic activity(yield>95%)after five cycles,providing an efficient,green and low-cost method for acetal synthesis with good potential for industrialization.

关 键 词：离子液体 苯并噻唑 缩醛反应 催化活性 

分 类 号：O643.32[理学—物理化学]