[1]周心龙,刘祖亮,成健,等.2,6-二乙酰氨基吡嗪-1-氧化物硝化反应研究[J].爆破器材,2014,43(04):16-21.[doi:10.3969/j.issn.1001-8352.2014.04.004]
　ZHOU Xinlong,LIU Zuliang,CHENG Jian,et al.Study on the Nitration Reaction of 2,6-Diacetamidopyrazine-1-Oxide[J].EXPLOSIVE MATERIALS,2014,43(04):16-21.[doi:10.3969/j.issn.1001-8352.2014.04.004]
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2,6-二乙酰氨基吡嗪-1-氧化物硝化反应研究()
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《爆破器材》[ISSN:1001-8352/CN:32-1163/TJ]

卷:
43
期数:
2014年04
页码:
16-21
栏目:
基础理论
出版日期:
2014-08-20

文章信息/Info

Title:
Study on the Nitration Reaction of 2,6-Diacetamidopyrazine-1-Oxide
文章编号:
4708
作者:
周心龙; 刘祖亮; 成健; 赵晓锋
南京理工大学化工学院（江苏南京，210094）
Author(s):
ZHOU Xinlong;  LIU Zuliang;  CHENG Jian;  ZHAO Xiaofeng
School of Chemical Engineering, Nanjing University of Science & Technology (Jiangsu Nanjing, 210094)
关键词:
2; 6-二乙酰氨基吡嗪-1-氧化物; 2; 6-二氨基-3; 5-二硝基吡嗪-1-氧化物; 酸性离子液体; 硝化; 催化
Keywords:
2;  6-diacetamidopyrazine-1-oxide;  2;  6-diamino-3;  5-dinitropyrazine-1-oxide;  acidic ionic liquid;  nitration;  catalysis
分类号:
O643.3；TQ564.4
DOI:
10.3969/j.issn.1001-8352.2014.04.004
文献标志码:
A
摘要:
研究了2,6-二乙酰氨基吡嗪-1-氧化物在硝硫混酸和发烟硝酸/酸性离子液体中的硝化反应。在混酸硝化体系中，考察了混酸硝化剂类型对产物2,6-二氨基-3,5-二硝基吡嗪-1-氧化物（LLM-105)收率和纯度的影响。在发烟硝酸/N,N,N-三甲基-N-丙磺酸基-硫酸氢铵(TMPSHSO4)硝化体系中，考察了在酸性离子液体催化条件下酸性离子液体使用量、硝解反应温度、酸性离子液体重复使用次数对LLM-105收率和纯度的影响。结果表明：混酸硝化体系中，2,6-二乙酰氨基吡嗪-1-氧化物的最佳硝化剂为KNO3和质量分数20%发烟硫酸，LLM-105的收率为72.5%，质量分数为98.6%。发烟硝酸/酸性离子液体硝化体系中，最佳反应条件为：TMPSHSO4与2,6-二乙酰氨基吡嗪-1-氧化物的物质的量的比为0.05∶1.00，硝解温度为75 ℃，LLM-105收率为64.8%，质量分数为98.5%，TMPSHSO4经回收可重复使用3次。相对而言，以发烟硝酸/TMPSHSO4为硝化剂合成LLM-105更具优势。用1H NMR、IR和MS对LLM-105的结构进行了表征。
Abstract:
Nitration reactions of 2, 6-diacetamidopyrazine-1-oxide in mix acid or fuming nitric acid/acidic ionic-liquid- were researched. In the mixed acid nitration system, effects of mixed acid nitration agent types on the yield and purity of the product LLM-105 were investigated. In the fuming nitric acid and N,N,N-trimethyl-N-propanesulfonic acid -ammonium- hydrogen sulfate (TMPSHSO4) nitration system, the effects of acidic ionic liquid quantity, nitration temperature and acidic ionic liquid recycle times on the yield and purity of LLM-105 were investigated in the catalyst condition of acidic ionic liquid. The results show that, in the mixed acid nitration system, the best nitrating agent of 2, 6-diacetamidopyrazine-1-oxide are KNO3 and 20% oleum, the product yield is 72.5%, and the purity is 98.6%. In the fuming nitric acid and TMPSHSO4 nitration system, optimal reaction conditions are that molar ratio of TMPSHSO4 and 2,6-diacetamidopyrazine-1-oxide is 0.05∶1.00, reaction temperature is 75 ℃, the product yield is 64.8%, the purity is 98.5%, and TMPSHSO4 could be recovered and used repeatedly for three times. Nitration of 2,6-diacetamidopyrazine-1-oxide by fuming nitric acid and TMPSHSO4 has more advantages. The structure of LLM-105 was also characterized by1H NMR, IR and MS.

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备注/Memo

备注/Memo:
收稿日期：2013-1008
作者简介：周心龙（1980~），男，博士研究生，研究方向：低易损混合炸药。E-mail：64259695@qq.com
通信作者：刘祖亮（1951~），男，研究员，博导，研究方向：化学工艺和含能材料合成和配方。E-mail：liuzl@njust.edu.cn
更新日期/Last Update: 2014-08-25