质子酸酸化_emim_BF_4离子液体中4_4_MDC的合成反应研究.pdf

21 3 No.3 Vol.21 2007 6 Journal of Chemical Engineering of Chinese Universities June 2007 1003-9015(2007)03-0467-04 [emim]BF 4,4’-MDC 4 , , , ( , 300130) 1--3-([emim]BF ) 4 (ILs)(MPC) 4,4’- (4,4’-MDC) 4,4’-MDC 70 n(MPC) / n(HCHO) = 4/1wt(ILs) / wt(MPC) = 4/11.5 h4,4’-MDC 71.7% 71.9% 1--3- TQ203.2 TQ323.8 A + Synthesis of 4,4’-MDC in the Presence of [emim]BF Ionic Liquid Modified with H 4 HU Li-yan, GENG Yan-lou, ZHAO Xin-qiang, WANG Yan-ji (Hebei Provincial Key Lab of Green Chemical Technology and High Efficient Energy Saving, Hebei University of Technology, Tianjin 300130, China) Abstract: The synthesis of methylene diphenyl dimethylcarbamate(4,4’-MDC) from methyl N-phenyl carbamate(MPC) and formaldehyde was investigated in the presence of [emim]BF4 ionic liquid modified with + H as both catalyst and reaction solvent. The influence of reaction temperature, molar ratio of MPC to HCHO, the amount of ionic liquid used and reaction time on 4,4’-MDC synthesis reaction was studied. Under the suitable reaction conditions of 70 , n(MPC)/n(HCHO) = 4/1, wt(ILs)/wt(MPC) = 4/1 and reaction time of 1.5 h, the yield and selectivity of 4,4’-MDC are 71.74% and 71.91%, respectively. The used ionic liquid modified with H+ was treated by ultrasonic extraction with CHCl3 and was reused in the condensation reaction, and no significant loss in catalytic activity was observed. Key words: [emim]BF4 ionic liquid; methyl N-phenyl carbam