双四唑肼的结构表征与合成工艺优化

Structural Characterization and Process Optimization of Bistetrazolohydrazine

以5,5′-偶氮四唑二钠、镁粉为原料,制得肼双四唑钠盐,再与盐酸反应得目标产物双四唑肼(HBT),利用元素分析、红外分析、核磁共振波谱、扫描电镜和热重-差示扫描量热法等手段对目标产物进行了表征。研究了反应摩尔比、反应时间、反应温度、盐酸质量分数等条件对收率的影响,得到较好的工艺条件为n(Na2ZT)∶n(Mg)=1∶6,反应时间6h,反应温度100℃,盐酸质量分数20%,目标产物最高收率达91.53%。

Disodium 5,5′-hydrazinotetrazolate was prepared with the starting materials,sodium 5,5′-azotetrazolate as well as magnesium,and the fianl product,bistetrazolohydrazine（HBT） was synthesized through hydrochloric acid and sodium 5,5′-hydrazinotetrazolate.The target product HBT was characterized by elemental analysis,IR,HNMR,SEM and TG-DSC.The factors affecting the yield,including reaction mole ratio,reaction time,reaction temperature,HCl mass fraction were investigated.The optimum reaction conditions are reactant mole ratio n（Na2ZT）∶n（Mg）=1∶6,reaction time 6 hour,reaction temperature 100℃ and HCl mass fraction,20%,the highest yield of the HBT is 91.53%.