合成了5种醚基功能化酸性离子液体[Me(OEt)1-MOR-C3SO3H][MeSO3]、[Me(OEt)2-MOR-C3SO3H][MeSO3]、[Me(OEt)3-MOR-C3SO3H][MeSO3]、[2(C3SO3H-MOR)-(OEt)(200)][2MeSO3]、[2(C3SO3H-MOR)-(OEt)(400)][2MeSO3],使用红外光谱和核磁共振氢谱对合成的离子液体结构进行表征,考察离子液体的黏度、溶解性和腐蚀性。以正丁醇和乙酸的酯化反应考察了离子液体的催化活性,并使用响应面分析法优化反应工艺。结果表明,当酸醇摩尔比为1.2:1、催化剂[2(C3SO3H-MOR)-(OEt)(400)][2MeSO3]用量为醇质量的5%、带水剂用量为醇质量的16%时,在90℃下反应5 h,酯收率可达97.8%,离子液体经回收干燥重复使用8次催化活性没有明显的降低。
Five ether-functionalized ionic liquids(ILs), containing [Me(OEt)1-MOR-C3SO3H][MeSO3], [Me(OEt)2-MOR-C3SO3H][MeSO3], [Me(OEt)3-MOR-C3SO3H][MeSO3], [2(C3SO3H-MOR)-(OEt)(200)][2MeSO3] and [2(C3SO3H-MOR)-(OEt)(400)][2MeSO3] were synthesized and characterized by the Fourier transform infrared spectrometer and nuclear magnetic resonance spectrometer. The ionic liquid viscosity, solubility and corrosion were investigated.The promotion effect of ether-functionalized ILs in esterification of acetic acid with butyl alcohol was investigated and the reaction process was optimized using response surface analysis. The yield of n-butyl acetate was up to 97.8% under the optimized conditions: response surface analysis(RSA) of n(CH3COOH):n(C4H9OH)= 1.2:1, the mass of catalyst [2(C3SO3H-MOR)-(OEt)(400)][2MeSO3] was 5% of the quality of butyl alcohol, the mass of water carrying agent was 30% of the quality of butyl alcohol, temperature was 90℃, and reaction time was 5 h. The catalysts could be recycled for 8 times without obviously decline of catalytic activity.