摘要
以吉纳和叠氮化钠为起始原料,经过叠氮化、萃取、洗涤、脱色、过滤以及真空蒸馏等多个步骤合成出1,5-二叠氮基-3-硝基氮杂戊烷(DIANP);通过红外、核磁及元素分析对产物进行结构表征;并分析测试了其他相关性能;考察了料比、溶媒、温度和时间等对反应的影响。结果表明,合成的最佳条件是:反应物料的质量比为1∶0.59、溶媒DMSO、反应温度80~85℃、反应时间7~8 h,收率不小于80%,纯度不小于98%(LC)。
1,5-Diazido-3-nitrazapropant (DIANP) was synthesized from DINA and sodium azide, via azidation, extraction, washing, decolor, filtration and vacuum distillation. Its structure was characterized by IR, NMR and elemental analyses. Relative properties were analysed, The parameters affecting the yield, such as ratio, solvent, temperature and reaction time, were discussed. The results show that the optimum reaction condition of synthesizing DIANP are: the mass ratio of DINA to sodium azide, about 1 : 0. 59; solvent, DMSO; reaction temperature , 80- 85 ℃ and reaction time,7-8h. The yield of DIANP is about 80% and purity 98%.
出处
《火炸药学报》
EI
CAS
CSCD
2008年第3期44-46,共3页
Chinese Journal of Explosives & Propellants