BrФnsted-Lewis双酸性离子液体催化合成二苯甲烷二氨基甲酸甲酯  

Synthesis of Methylene Diphenyl Dimethylcarbamate Catalyzed by BrФnsted-Lewis Acidic Ionic Liquid

作　　者：康丽娟[1] 赵新强[1] 安华良[1] 王延吉[1] 

机构地区：[1]河北工业大学化工学院绿色化工与高效节能河北省重点实验室,天津300130

出　　处：《石油学报（石油加工）》2013年第2期249-255,共7页Acta Petrolei Sinica(Petroleum Processing Section)

基　　金：国家自然科学基金(20976035,21076059);973计划前期研究专项(2010CB234602);河北省自然科学基金(B2010000019)资助

摘　　要：合成了具有不同ZnCl2摩尔分数的BrФnsted-Lewis双酸性离子液体[HO3S-(CH2)4-mim]Cl-xZnCl2,采用Hammett指示剂与紫外联用法测定了其酸强度,考察了其在苯氨基甲酸甲酯(MPC)与甲醛(HCHO)缩合制备二苯甲烷二氨基甲酸甲酯(MDC)反应中的催化性能,并考察了反应条件对MDC收率和MPC转化率的影响。结果表明,当x=0.7时该离子液体的催化活性最高。以[HO3S-(CH2)4-mim]Cl-0.7ZnCl2为催化剂兼溶剂,在反应温度70℃、反应时间60min、MPC与HCHO的摩尔比为10、离子液体与MPC的质量比为2的条件下,MDC收率最高可达99.1%。用水处理反应液并通过减压蒸馏回收的离子液体可以循环使用5次,其催化活性基本不变。Brφnslash;nsted-Lewis acidic ionic liquids [HO3S-（CH2）4-mim]Cl-xZnCl2 with different molar fractions of zinc chloride were prepared and their acid strength was determined by the Hammett method combined with UV-visible spectroscopy. The catalytic performance of [HO3S-（CH2）4 mim]Cl-xZnCl2 for the synthesis of methylene diphenyl dimethylcarbamate（MDC） from methyl N-phenyl carbamate（MPC） and formaldehyde（HCHO） was evaluated. The effects of reaction conditions on MDC yield and MPC conversion of the reaction were investigated. The results showed that [HO3S-（CH2）4-mim]Cl-0.7ZnCl2 had the highest catalytic activity. With [HO3S-（CH2）4mim]Cl-0.7ZnCl2 as catalyst and solvent under the reaction conditions of temperature 70℃, time 60 min, n（MPC）/n（HCHO）=10 and m（ILs）/m（MPC）=2, the yield of MDC was 99.1%. [HO3S（CH2）4-mim]Cl-xZnCl2 could be reused more than five times without significant loss in its catalytic performance after the removal of water by vacuum distillation.

关 键 词：Brφnslash nsted-Lewis双酸性离子液体 苯氨基甲酸甲酯 缩合反应 

分 类 号：TQ203.2[化学工程—有机化工] TQ323.8