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

Improved Synthesis Technology of 1,4,5,8-Tetranitro-1,4,5,8-Tetraazabicyclo [4. 4. 0] Decalin

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。

A new method for the synthesis of 1,4,5,8-tetranitro-1 ,d,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, 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 （AC20） = 1 ： 24 ： 15. Meanwhile, the best reaction temperature is 25 ℃ and the best reaction time is 2 h.