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醚基功能化离子液体催化合成乙酸正丁酯
引用本文:胡甜甜,赵地顺,武宇,张拴力,扈士海,翟建华.醚基功能化离子液体催化合成乙酸正丁酯[J].化工学报,2017,68(1):136-145.
作者姓名:胡甜甜  赵地顺  武宇  张拴力  扈士海  翟建华
作者单位: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
基金项目: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)。
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  
收稿时间:2016-07-20
修稿时间:2016-10-12

Synthesis of n-butyl acetate by ether-functionalized ionic liquid
HU Tiantian,ZHAO Dishun,WU Yu,ZHANG Shuanli,HU Shihai,ZHAI Jianhua.Synthesis of n-butyl acetate by ether-functionalized ionic liquid[J].Journal of Chemical Industry and Engineering(China),2017,68(1):136-145.
Authors:HU Tiantian  ZHAO Dishun  WU Yu  ZHANG Shuanli  HU Shihai  ZHAI Jianhua
Affiliation: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
Abstract:Five ether-functionalized ionic liquids(ILs), containingMe(OEt)1-MOR-C3SO3H]MeSO3], Me(OEt)2-MOR-C3SO3H]MeSO3], Me(OEt)3-MOR-C3SO3H]MeSO3], 2(C3SO3H-MOR)-(OEt)200]2MeSO3]and2(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 catalyst2(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.
Keywords:ether-functionalized  morpholine  ionic liquid  catalysis  esterification  RSA  
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