1-氨基-3,5-二硝基-1,2,4-三唑的合成工艺改进及性能

Synthesis Improvement and Properties of 1-Amino-3,5-dinitro-1,2,4-triazole

以3,5-二氨基-1,2,4-三唑为原料合成出中间体3,5-二硝基-1,2,4-三唑(DNT)钠盐(Ι),用2,4,6-三甲基苯磺酰羟胺(MSH)胺化Ι,得到了目标物1-氨基-3,5-二硝基-1,2,4-三唑(ADNT),收率66%。采用红外、核磁、质谱及元素分析表征了ADNT的结构。确定了较佳的反应条件:室温,摩尔比n(DNT-Na+)∶n(MSH)=1∶1.5,反应时间12 h。采用差示扫描量热法研究了ADNT的热性能,其熔点为128.7℃,分解峰温为225.8℃。按GJB772-1997测试ADNT的撞击感度为H50大于112 cm(落锤2 kg),表明ADTN为性能良好的低感炸药。

1-Amino-3,5-dinitro-1,2,4-triazole（ ADN T） w as synthesized by amination of the sodium salt of 3,5-diamino-1,2,4-triazole（ DNT-Na^＋） with mesitylene sulfonyl hydroxylamine（ MSH） with yield of 66%,in which the DNT-Na＋w as obtained from 3,5-diamino-1,2,4-triazole. T he structure of ADN T w as characterized by IR,M S,1H N M R,13C N M R and elemental analysis,the thermal behavior w as studied by differential scanning calorimetry（ DSC）. T he factors effecting amination w ere investigated as w ell. R esults show that the optimum reaction conditions are the molar ratio DN T-N a＋to M SH is 1∶ 1. 5,reaction time 12 h at room temperature. T he melting and decomposition temperatures are 128. 7,225. 8 ℃,respectively,and the impact sensitivity（ H50） with 2 kg drop weigh is beyond 112cm,which show ing ADN T is an energetic insensitive explosive w ith good comprehensive performance.