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你可能喜欢Synthesis of Itaconic Ester Catalyzed by Triethylamine Ionic Liquids--《Journal of Chemical Engineering of Chinese Universities》2009年04期
Synthesis of Itaconic Ester Catalyzed by Triethylamine Ionic Liquids
WANG Guo-hua1,LI Lu 2,XIE Cong-xia1,YU Shi-tao 2,LIU Fu-sheng 2 (1. College of Chemistry and Molecular Engineering,Qingdao University of Science and Technology, Qingdao 266042,C 2. College of Chemical Engineering,Qingdao University of Science and Technology, Qingdao 266042,China)
Several Brφnsted acidic ionic liquids (ILs) were synthesized,and using these prepared ILs as catalysts,the itaconic acid esterifications were investigated. The results show that,among those various kinds of ILs prepared,the triethylamine ILs have the highest catalytic activity and reused-life,and then they were characterized by FT-IR and NMR. Using the prepared acid ionic liquid [HSO3-pTEA]pTSA as catalyst for the synthesis of the dibutyl itaconate (DBIA),and under the optimized synthesis conditions,the itaconic acid conversion of 98.8% and the DBIA ester yield of 96.7% can be reached,respectively. Moreover,the catalyst [HSO3-pTEA]pTSA is immiscible with the product and can be reused for 7 times
during the reutilizations,the itaconic acid conversion can still keep above 96.5%. Furthermore,using the prepared [HSO3-pTEA]HSO4 as catalyst for the synthesis of diisooctyl itaconate (DOIA),and under its optimized reaction conditions,the itaconic acid conversion of 98.7% and the DOIA ester yield of 96.3% can be obtained,respectively. The catalyst [HSO3-pTEA]HSO4 can also be reused for 7 times without any disposal and its itaconic acid conversion can keep above 95.2%.
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Similar Journals
(C)2006 Tsinghua Tongfang Knowledge Network Technology Co., Ltd.(Beijing)(TTKN) All rights reserved酸性离子液体和Pt/C催化体系催化邻硝基甲苯制备2-甲基-4-甲氧基苯胺--《浙江工业大学》2012年硕士论文
酸性离子液体和Pt/C催化体系催化邻硝基甲苯制备2-甲基-4-甲氧基苯胺
【摘要】：2-甲基-4-甲氧基苯胺(MMA)是一种重要的医药化工中间体。MMA可由邻硝基甲苯催化加氢重排反应制得。现有工艺在合成反应中采用硫酸作为重排催化剂,存在腐蚀设备、污染环境等问题。近年来,室温离子液体以其溶解性好、结构和功能可设计、易与产物分离、蒸汽压低不易挥发等特性,被广泛的应用于各类反应,成为一种新型的绿色溶剂和催化剂,引起国内外众多科研工作者的的广泛关注。
本论文首先合成了甲基咪唑硫酸氢盐离子液体([Hmim]HSO4)、三乙胺硫酸氢盐离子液体([(C2H5)3NH]HSO4)、咪唑丙磺酸硫酸氢盐离子液体([HSO3-pHIM]HSO4)、甲基咪唑丙磺酸硫酸氢盐离子液体([HSO3-pMIM]HSO4)、吡啶丙磺酸硫酸氢盐离子液体([HSO3-pPydin] HSO4)以及吡啶丙磺酸对甲苯磺酸盐离子液体([HSO3-pPydin]+[pTSA]-)等6种酸性离子液体,并通过FT-IR、1HNMR对离子液体进行了结构表征,创新性地将酸性离子液体与Pt/C组成共催化体系应用于邻硝基甲苯加氢重排“一锅法”合成MMA反应中。系统考察了离子液体种类及用量、3%Pt/C用量、反应温度和反应压力等对邻硝基甲苯转化率和MMA选择性的影响。结果表明,在实验考察的酸性离子液体中,离子液体[HSO3-pHIM]HSO4和[HSO3-pMIM]HSO4对邻硝基甲苯加氢重排反应具有很好的催化性能。在酸性离子液体[HSO3-pHIM]HSO4为酸催化剂(用量为4ml)、3%Pt/C催化剂用量为0.02g、反应温度为50℃、氢气压力为0.04MPa条件下,邻硝基甲苯的转化率为93%,MMA的选择性为79%。
为了使离子液体能更好的回收利用,在上述研究基础上,分别采用浸渍法、键合法、溶胶-凝胶法对酸性离子液体[HSO3-pHIM]HSO4进行了固载,并考察了各方法制备的固载离子液体3次回收利用情况。结果表明,浸渍法制备的固载离子液体流失严重；键合法制备时间较长,步骤繁多；溶胶-凝胶法制备的固载离子液体稳定性较好,且该方法制备原料易得,过程简单,是制备固载离子液体的良好方法。
在上述研究基础上,采用溶胶-凝胶法制备了固载型酸性离子液体[HSO3-pMIM]HSO4,考察了制备过程中盐酸和正硅酸乙酯(TEOS)用量对[HSO3-pMIM]HSO4固载牢度的影响。研究结果表明,在盐酸和正硅酸乙酯(TEOS)用量分别为4ml和10ml时,邻硝基甲苯的转化率为100%,MMA的选择性为38.56%,催化剂循环使用三次后仍有较高的选择性。
【学位授予单位】：浙江工业大学【学位级别】：硕士【学位授予年份】：2012【分类号】：TQ246.31
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