Industrial Synthesis of N-Methylhydroxylamine Hydrochloride by Electrochemical Reduction of Nitromethane

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Industrial Synthesis of N-Methylhydroxylamine Hydrochloride by Electrochemical Reduction of Nitromethane

GANYongping^a,ZHANGWenkui^a; HUANGHui^a;XIAXinhui^a; CHENGYongsheng^b

^a College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310032, China

^b Zhejiang Huahai Pharmaceutical Company, Linhai 317024, China

Received:1900-01-01 Revised:1900-01-01 Online:2006-10-28 Published:2006-10-28
Contact: GAN Yongping

电化学还原硝基甲烷合成N-甲基羟胺盐酸盐的工业化试验

甘永平^a;张文魁^a; 黄辉^a; 夏新辉^a; 陈永胜^b

^aCollege of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310032, China ^b Zhejiang Huahai Pharmaceutical Company, Linhai 317024, China

通讯作者: 甘永平

Abstract

Abstract: An industrial electrolytic cell was designed for the electrochemical synthesis of N-methylhydroxylamine hydrochloride (N-MHA). Copper was used as the cathode, graphite as the anode, and a cation membrane as the separator. The results show that N-MHA with a high purity of 99% can be electrosynthesized directly from ni-tromethane in HCl solution. Under a constant current of 1000—2500A•m－2 in the temperature of 30—50℃, the av-erage yield, current efficiency, and reaction selectivity were 65%, 70%, and 99%, respectively. Graphite electrode and membrane material can be used continuously in the preparative electrolysis for 5000h. Moreover, the effects of the electrode and membrane materials, current intensity, electrolyte temperature, and other associated parameters on the electrosynthesis results were investigated. The direct current power consumption was 8151.3kW•h•(1000kg N-MHA) －1. This method is a simple separation process with limited contamination and hence, is a new green syn-thesis method for the industrial production of N-MHA.

Key words: N-methylhydroxylamine hydrochloride, electrosynthesis, nitromethane

摘要： An industrial electrolytic cell was designed for the electrochemical synthesis of N-methylhydroxylamine hydrochloride (N-MHA). Copper was used as the cathode, graphite as the anode, and a cation membrane as the separator. The results show that N-MHA with a high purity of 99% can be electrosynthesized directly from ni-tromethane in HCl solution. Under a constant current of 1000—2500A•m－2 in the temperature of 30—50℃, the av-erage yield, current efficiency, and reaction selectivity were 65%, 70%, and 99%, respectively. Graphite electrode and membrane material can be used continuously in the preparative electrolysis for 5000h. Moreover, the effects of the electrode and membrane materials, current intensity, electrolyte temperature, and other associated parameters on the electrosynthesis results were investigated. The direct current power consumption was 8151.3kW•h•(1000kg N-MHA) －1. This method is a simple separation process with limited contamination and hence, is a new green syn-thesis method for the industrial production of N-MHA.

关键词: N-methylhydroxylamine hydrochloride;electrosynthesis;nitromethane

GANYongping,ZHANGWenkui, HUANGHui,XIAXinhui, CHENGYongsheng. Industrial Synthesis of N-Methylhydroxylamine Hydrochloride by Electrochemical Reduction of Nitromethane[J]. .

甘永平,张文魁, 黄辉, 夏新辉, 陈永胜. 电化学还原硝基甲烷合成N-甲基羟胺盐酸盐的工业化试验[J]. CIESC Journal.

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