| 醚基功能化离子液体催化合成乙酸正丁酯 |
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| 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. DOI: 10.11949/j.issn.0438-1157.20161017 |
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| 作者姓名： | 胡甜甜 赵地顺 武宇 张拴力 扈士海 翟建华 |
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| 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 |
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| 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）。 |
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| 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。
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| 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 |
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| 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. DOI: 10.11949/j.issn.0438-1157.20161017 |
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| Authors: | HU Tiantian ZHAO Dishun WU Yu ZHANG Shuanli HU Shihai ZHAI Jianhua |
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| 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 |
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| 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. |
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| Keywords: | ether-functionalized morpholine ionic liquid catalysis esterification RSA |
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