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浙江大学学报(工学版)
J4  2010, Vol. 44 Issue (6): 1169-1172    DOI: 10.3785/j.issn.1008-973X.2010.06.022
化学工程     
催化合成肟的绿色新工艺
周少东, 钱超, 陈新志
浙江大学 化学工程与生物工程学系,浙江 杭州 310027
Green route to synthesize oxime
ZHOU Shao-dong, QIAN Chao, CHEN Xin-zhi
Department of Chemical Engineering and Biochemical Engineering, Zhejiang University,
Hangzhou 310027,China
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摘要：

为降低肟合成过程中的能耗及废物排放,通过考察反应温度、反应时间、物料比等因素对反应的影响,得到了一种合成肟的新工艺,该工艺具有不添加有机溶剂、反应条件较温和等优点.本工艺以钛硅分子筛（TS1）为催化剂,在水溶液中,以酮、氨和过氧化氢为原料进行反应合成相应的酮肟.环己酮肟的较优的合成工艺条件为：双氧水连续滴加,反应温度65 ℃,反应时间1.5 h,环己酮、氨、过氧化氢的量的比为1∶2.5∶1.1.该新工艺应用于其他肟的合成仍可获得较高的收率.
Abstract:

The effects of temperature, reaction time and molar ratio of substrates on oximation were investigated to decrease the energy consumption and discharge. A new method to synthesize oxime was presented, which is facile and uses no organic solvents. The reaction media is water, in which ketones reacts with ammonia and hydrogen peroxide under the catalysis of TS1, producing oximes. The optimized reaction conditions for cyclohexanone oxime synthesis are as follow: aqueous hydrogen peroxide is fed in continuously at 65 ℃, the reaction time is 1.5 h, and the molar ratio of cyclohexanone, ammonia and hydrogen peroxide is 1:2.5:1.1. Expanded syntheses of other oximes, such as butanone oxime, butyraldehyde oxime, cyclopentanone oxime and methylisobutylketone oxime, give high yield using the above method.
出版日期: 2010-07-16
:  TQ 217  
基金资助:

浙江省科技计划资助项目(2008C010061)；国家科技支撑计划课题资助项目（2007BA134B07）；国家自然科学基金资助项目（20776127）.
通讯作者: 钱超,助理研究员.     E-mail: supmoney@163.com
作者简介: 周少东（1986—）,男,河北保定人,博士生,从事含氮有机物合成研究.E-mail:easy157@163.com.
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引用本文:

周少东, 钱超, 陈新志. 催化合成肟的绿色新工艺[J]. J4, 2010, 44(6): 1169-1172.

ZHOU Shao-Dong, JIAN Chao, CHEN Xin-Zhi. Green route to synthesize oxime. J4, 2010, 44(6): 1169-1172.

链接本文:

http://www.zjujournals.com/eng/CN/10.3785/j.issn.1008-973X.2010.06.022    或    http://www.zjujournals.com/eng/CN/Y2010/V44/I6/1169

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