| 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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| 引用本文： | 丁峰,陆婷婷,张丽洁,汪伟,姬月萍.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(4):18-21. |
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| 作者姓名： | 丁峰 陆婷婷 张丽洁 汪伟 姬月萍 |
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| 作者单位： | 西安近代化学研究所 陕西西安,710065;西安近代化学研究所 陕西西安,710065;西安近代化学研究所 陕西西安,710065;西安近代化学研究所 陕西西安,710065;西安近代化学研究所 陕西西安,710065 |
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| 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.4HNO_3):n(98%HNO_3):n(AC_2O)=1:24:15,反应温度为25℃,反应时间为2 h。
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| 关 键 词： | 有机化学 TNAD 成盐 硝化 HNO3/AC2 O |
Improved Synthesis Technology of 1,4,5,8-Tetranitro-1,4,5,8-Tetraazabicyclo[4. 4. 0] Decalin |
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| DING Feng,LU Tingting,ZHANG Lijie,WANG Wei,JI Yueping.Improved Synthesis Technology of 1,4,5,8-Tetranitro-1,4,5,8-Tetraazabicyclo[4. 4. 0] Decalin[J].Explosive Materials,2016,45(4):18-21. |
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| Authors: | DING Feng LU Tingting ZHANG Lijie WANG Wei JI Yueping |
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| Abstract: | A new method for the synthesis of 1,4,5,8-tetranitro-1,4,5,8-tetraazabicyclo4. 4. 0]decalin (TNAD) was studied. This compound was prepared from the raw material 1,4,5,8- tetraazabicyclo4. 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, 1 H NMR and elemental analysis. The effects of nitrification system, reactant ratio, reac-tion 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. |
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| Keywords: | organic chemistry 1 4 5 8-tetranitro-1 4 5 8-tetraazabicyclo [4 4 0]decalin (TNAD) salt-forming reaction nitrolysis HNO3/AC2 O |
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