| N-甲基咪唑合成工艺研究 |
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| 引用本文： | 张平,汤琳,张婷,宋常春.N-甲基咪唑合成工艺研究[J].安徽科技学院学报,2016,50(2):71-75. |
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| 作者姓名： | 张平 汤琳 张婷 宋常春 |
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| 作者单位： | 安徽科技学院化学与材料工程学院,安徽凤阳,233100;皖南医学院药学院,安徽芜湖,241002 |
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| 基金项目： | 安徽科技学院重点建设学科(AKZDXK2015A01)；皖南医学院中青年研究基金项目(WK201516)。 |
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| 摘 要： | 目的:优化N-甲基咪唑合成工艺。方法:以乙二醛、甲胺、氨水、多聚甲醛为原料,"一锅法"合成N-甲基咪唑,对N-甲基咪唑转化率的影响因素-投料顺序、反应温度、反应时间等进行条件优化,通过N-甲基咪唑的标准折光率曲线法准确、快速检测反应过程中N-甲基咪唑含量。所得产品N-甲基咪唑分别用氢谱、碳谱以及气质联用GC-MS进行表征。结果:以当量的多聚甲醛、氨水、甲胺、乙二醛的投料顺序,反应温度为60℃,反应时间为4小时,N-甲基咪唑的转化率高达98%。通过减压蒸馏除水,共沸剂环己烷精制,最后减压蒸馏得到的产品N-甲基咪唑纯度可达到99.5%。结论:该合成工艺具有产品转化率高,污水处理量少,检测方法快速高效的优点,适合于大规模工业生产。
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| 关 键 词： | N-甲基咪唑 一锅法 折光率 |
Research on the Synthetic Technology of N-methylimidazole |
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| ZHANG Ping,TANG Lin,ZHANG Ting,SONG Chang-chun.Research on the Synthetic Technology of N-methylimidazole[J].Journal of Anhui Science and Technology University,2016,50(2):71-75. |
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| Authors: | ZHANG Ping TANG Lin ZHANG Ting SONG Chang-chun |
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| Abstract: | Objective:Different influential factors were optimized during the synthetic technology of N-methy-limidazole in synthesizing process. Method:N-methy-limidazole was synthesized by a one-pot reaction with using glyoxal,methylamine,ammonia and paraformaldehyde as raw materials. The influential factor including materials adding order,reaction temperature and reaction time on the conversion rate of N-methy-limidazole were optimized. The content of N-methy-limidazole in synthesizing process was also accurately and rapidly de-tected through the standard curve of refractive index for N-methy-limidazole. The chemical structure of the fi-nal product was characterized by 1H and 13C NMR spectroscopy and( GC-MS)mass spectrometry. Result:The results show that the conversion of the reaction is over 98% using the materials adding order of paraformalde-hyde,ammonia methylamine and glyoxal,reaction temperature of 60℃ and reaction time of 4 h. The water was removed under vacuum and then using cyclohexane as azeotrope,the product was finally obtained with a purity of 99. 5%. Conclusion:The synthetic technology has the advantages of high conversion,low sewage treatment, rapid and efficient detection method,which will be suitable for the industrial production. |
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| Keywords: | N-methy-limidazole One-pot reaction Refractive inde |
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