3,3′-二硝基-5,5′-偶氮-1H-1,2,4-三唑的合成与晶体结构

Synthesis and Crystal Structure of 3,3′-Dinitro-5,5′-azo-1H-1,2,4-triazole(DNAT)

以3-氨基-5-硝基-1H-1,2,4-三唑(ANTA)为原料,经过氧化合成3,3′-二硝基-5,5′-偶氮-1H-1,2,4-三唑(DNAT),采用红外光谱、核磁共振、元素分析等鉴定了产品结构。探讨了偶氮反应的机理和关键影响因素,确定了最佳的反应条件。测试了DNAT的部分性能,H50为17.08 cm(落锤5 kg);摩擦感度60%(表压3.92、摆角90°)。培养了DNAT单晶,四元衍射分析表明:DNAT.4H2O晶体属于单斜晶系,空间群为P 2(1)/n,晶体密度为1.550 g/cm。

3,3＇-Dinitro-5,5＇-azo-1H-1, 2,4-triazole （DNAT） was synthesized by the oxidative coupling of 5-amino- 5-nitro-1, 2, 4-triazole （ANTA） as raw material. Its structure was characterized by IR, NMR and elemental analyses. The crucial factors and mechanism in the coupling reaction were explored and the synthetical conditions were optimized. Some properties of DNAT were measured. The H50of 17.08cm（drop hammer 5 kg） and friction sensitivity of 60% （pressure 3.92MPa, pendulum angle 90°）were obtained. The single crystal of DNAT · 4H2O was cultivated, and its crystal structure was determined by X-ray crystallogaphy. The crystal of DNAT·4H2O is monoclinic crystal system with space group P2（1）/n and Dc=1. 550g ·cm^-3.