CIESC Journal ›› 2017, Vol. 68 ›› Issue (1): 136-145.DOI: 10.11949/j.issn.0438-1157.20161017

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Synthesis of n-butyl acetate by ether-functionalized ionic liquid

HU Tiantian1, ZHAO Dishun1, WU Yu1, ZHANG Shuanli2, HU Shihai2, ZHAI Jianhua1   

  1. 1 College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, Hebei, China;
    2 Shijiazhuang XinyuSanyang Industrial Co., Ltd., Shijiazhuang 051430, Hebei, China
  • Received:2016-07-20 Revised:2016-10-12 Online:2017-01-05 Published:2017-01-05
  • Contact: 10.11949/j.issn.0438-1157.20161017
  • Supported by:

    supported by the National Natural Science Foundation of China (20576026, 21106032) and the Shijiazhuang Science Technology Research and Development Program(161070251A)。

醚基功能化离子液体催化合成乙酸正丁酯

胡甜甜1, 赵地顺1, 武宇1, 张拴力2, 扈士海2, 翟建华1   

  1. 1 河北科技大学化学与制药工程学院, 河北 石家庄 050018;
    2 石家庄新宇三阳实业有限公司, 河北 石家庄 051430
  • 通讯作者: 赵地顺
  • 基金资助:

    国家自然科学基金项目(20576026,21106032);石家庄市科学技术研究与发展计划资助项目(161070251A)。

Abstract:

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.

Key words: ether-functionalized, morpholine, ionic liquid, catalysis, esterification, RSA

摘要:

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。

关键词: 醚基功能化, 吗啡啉, 离子液体, 催化, 酯化, 响应面

CLC Number: