Process Optimization of the Preparation of 3-Nitropyrazole by Hydrothermal Method

被引：0

作者：

Tong Z.-K. ^{[1
]}

Wang M.-Y. ^{[1
]}

Chen J. ^{[2
]}

Hou L. ^{[3
]}

Ding Q.-N. ^{[1
]}

Shen F.-F. ^{[1
]}

Pan H.-X. ^{[2
]}

Li Y.-X. ^{[1
]}

Cao D.-L. ^{[1
]}

机构：

[1] School of Chemistry and Chemical Engineering, North University of China, Taiyuan

[2] Hubei Dongfang Chemical Co., Ltd, Hubei, Xiangyang

[3] Shanxi Jiangyang Chemical Co., Ltd., Taiyuan

来源：

Huozhayao Xuebao/Chinese Journal of Explosives and Propellants | 2023年 / 46卷 / 11期

关键词：

3-nitropyrazole; hydrothermal method; melt-cast carrier explosive; nitrogen heterocyclic compounds; organic chemistry; thermal rearrangement;

D O I：

10.14077/j.issn.1007-7812.202304016

中图分类号：

学科分类号：

摘要：

In order to solve the problems of long rearrangement time, high toxicity of rearrangement reagents and easy sublimation of N-nitropyrazole （N-NP） in the synthesis of 3-nitropyrazole （3-NP）, N-nitropyrazole was used as raw material to prepare 3-NP by the hydrothermal method using xylene as the rearrangement solvent, and the structures were characterized by microscope and IR spectrum. The reaction temperature, reaction time, filling degree and other factors were optimized. The results show that the optimal reaction conditions are as follows: reaction temperature of 180℃, holding time of 3h, filling degree of 15%, and the yield of 3-NP at corresponding theoretical pressure of 6. 130MPa is 100%. The product purity is stabilized above 99%, showing that the product obtained by this process can be directly used without post-treatment. The product yield is high when the solid-to-liquid ratio （N-NP: xylene） is 1 : 3 in the hydrothermal method. Due to the low consumption, low cost, and low toxicity of rearrangement solvent, the hydrothermal method is expected to replace the traditional synthetic process of 3-NP. © 2023 China Ordnance Industry Corporation. All rights reserved.

引用

页码：965 / 970

页数：5

共 19 条

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