[1]汪营磊,高福磊,丁峰,等.3,4-二硝基吡唑合成放大工艺研究[J].爆破器材,2018,47(05):35-38,43.[doi:10.3969/j.issn.1001-8352.2018.05.006]
　WANG Yinglei,GAO Fulei,DING Feng,et al.Study on the Up-sizing Synthesis Technology of 3, 4-Dinitropyrazole[J].EXPLOSIVE MATERIALS,2018,47(05):35-38,43.[doi:10.3969/j.issn.1001-8352.2018.05.006]
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3,4-二硝基吡唑合成放大工艺研究()
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《爆破器材》[ISSN:1001-8352/CN:32-1163/TJ]

卷:
47
期数:
2018年05
页码:
35-38,43
栏目:
基础理论
出版日期:
2018-09-27

文章信息/Info

Title:
Study on the Up-sizing Synthesis Technology of 3, 4-Dinitropyrazole
文章编号:
5248
作者:
汪营磊; 高福磊; 丁峰; 陆婷婷; 闫峥峰
西安近代化学研究所（陕西西安，710065）
Author(s):
WANG Yinglei;  GAO Fulei;  DING Feng;  LU Tingting;  YAN Zhengfeng
Xi’an Modern Chemistry Research Institute (Shaanxi Xi’an, 710065)
关键词:
有机化学; 3; 4二硝基吡唑; 硝化; 放大合成工艺
Keywords:
organic chemistry;  3;  4-dinitropyrazole;  nitration;  up-sizing synthesis technology
分类号:
TQ564
DOI:
10.3969/j.issn.1001-8352.2018.05.006
文献标志码:
A
摘要:
以吡唑为原料，经N-硝化、热重排、C-硝化等反应合成了3,4-二硝基吡唑(DNP)。进行了DNP的放大工艺研究，优化了硝化工艺条件，考察了C-硝化的工艺稳定性及重结晶溶剂苯甲腈的循环利用。研究发现：DNP较佳反应温度为55~57 ℃，反应时间45 min，收率86.8%；DNP的放大硝化工艺具有较好的稳定性，重结晶溶剂可以循环利用5次以上，重结晶纯度99%以上。该放大合成工艺得到的DNP具有良好的物理化学性能，有望应用于混合炸药的研制。
Abstract:
3, 4-dinitropyrazole (DNP) was synthesized from pyrazole by N-nitration, thermal rearrangement and C-nitration reactions. Large scale process was studied, and nitrification process conditions were optimized. Process stability of C-nitration and the recycling of recrystallization solvent were investigated. It was found that the ideal reaction temperature and reaction time is 55-57 ℃ and 45 min, yielding DNP up to 86.8%. Up-sizing nitrification process of DNP is stable, in which the recrystallization solvent could be recycled more than 5 times, and the purity of recrystallization product is above 99%. DNP obtained from this process exhibits good physical and chemical properties, and it is expected to be applied to the development of composite explosives.

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备注/Memo

备注/Memo:
收稿日期：2018-01-23
基金项目：国家自然科学基金(21173163)
作者简介：汪营磊（1983－），男，副研究员，主要从事含能功能材料合成及性能研究。E-mail: wyl-204@163.com
更新日期/Last Update: 2018-09-27