[1]丁峰,陆婷婷,张丽洁,等.1,4,5,8-四硝基-1,4,5,8-四氮杂双环［4.4.0］癸烷合成工艺的改进[J].爆破器材,2016,45(04):18-21.[doi:10.3969/j.issn.10018352.2016.04.004]
　DING Feng,LU Tingting,ZHANG Lijie,et al.Improved Synthesis Technology of 1,4,5,8-Tetranitro-1,4,5,8-Tetraazabicyclo［4.4.0］ Decalin[J].EXPLOSIVE MATERIALS,2016,45(04):18-21.[doi:10.3969/j.issn.10018352.2016.04.004]
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1,4,5,8-四硝基-1,4,5,8-四氮杂双环［4.4.0］癸烷合成工艺的改进()
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《爆破器材》[ISSN:1001-8352/CN:32-1163/TJ]

卷:
45
期数:
2016年04
页码:
18-21
栏目:
基础理论
出版日期:
2016-07-12

文章信息/Info

Title:
Improved Synthesis Technology of 1,4,5,8-Tetranitro-1,4,5,8-Tetraazabicyclo［4.4.0］ Decalin
文章编号:
5073
作者:
丁峰; 陆婷婷; 张丽洁; 汪伟; 姬月萍
西安近代化学研究所（陕西西安,710065）
Author(s):
DING Feng;  LU Tingting;  ZHANG Lijie;  WANG Wei;  JI Yueping 
Xi’an Modern Chemistry Research Institute (Shaanxi Xi’an, 710065)
关键词:
有机化学; TNAD; 成盐; 硝化; HNO3/AC2O
Keywords:
organic chemistry;  1; 4; 5; 8-tetranitro-1; 4; 5; 8-tetraazabicyclo ［4.4.0］decalin (TNAD);  salt-forming reaction;  nitrolysis;  HNO3/AC2O
分类号:
TJ55
DOI:
10.3969/j.issn.10018352.2016.04.004
文献标志码:
A
摘要:
为了改进1,4,5,8-四硝基-1,4,5,8-四氮杂双环［4.4.0］癸烷（TNAD）的合成方法，以1,4,5,8-四氮杂双环［4.4.0］癸烷（THAD）为原料，经成盐、硝化两步反应合成出了TNAD，反应总收率为90%，纯度为98.7%。采用红外光谱、核磁共振氢谱及元素分析对产品结构进行了表征。考察了硝化体系、物料比、反应温度、反应时间对硝化反应的影响，确定了最佳的反应条件：n(THAD.4HNO3)∶n（98%HNO3）∶n（AC2O）= 1∶24∶15，反应温度为25 ℃, 反应时间为2 h。
Abstract:
A new method for the synthesis of 1,4,5,8-tetranitro-1,4,5,8-tetraazabicyclo［4.4.0］decalin (TNAD) was studied. This compound was prepared from the raw material 1,4,5,8- tetraazabicyclo［4.4.0］decalin (THAD) via saltforming reaction and nitrolysis. The total yield could reach as high as 90%, and the purity is 98.7%. Structure of the product was characterized by IR, 1H NMR and elemental analysis. The effects of nitrification system, reactant ratio, reaction temperature and reaction time on the yield have been investigated. Results show that the optimum reaction conditions of the reaction are determined as: n(THAD.4HNO3)∶n(98%HNO3)n (AC2O) = 1∶24∶15. Meanwhile, the best reaction temperature is 25 ℃ and the best reaction time is 2 h.

参考文献/References:

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备注/Memo

备注/Memo:
收稿日期：2016-03-01
作者简介：丁峰（1982－），男，工程师，主要从事功能材料的合成研究。E-mail:m-top@163.com
通信作者：张丽洁(1963－)，女，副研究员，主要从事功能材料及精细化工研究。E-mail：cui＿zhe@163.com
更新日期/Last Update: 2016-07-11