偶氮四唑二胍的合成与性能

摘要

以5-氨基四唑（5-AT）为原料，经氧化和离子置换反应合成了富氮含能化合物偶氮四唑二胍（GZT），用红外光谱、核磁共振、元素分析、高效液相色谱、质谱和扫描电镜对目标化合物进行表征。采用DSC考察了目标化合物的热性能，并测试了其机械感度，通过实验得到最佳的合成工艺为：氢氧化钾的浓度为1．5 mol／L，5-氨基四唑、高锰酸钾与硝酸胍的摩尔比为1．0∶1．0∶1．1，氧化反应温度为60℃，氧化反应时间60 min，置换反应的温度为80℃，在最佳合成条件下产率为97．2％，纯度为99％，产物为黄色针状晶体，尺寸均一。产物的分解峰温为256．6℃，摩擦感度和撞击感度分别为4％和16％，表明该富氮含能化合物的分解温度高，机械感度低，在生产和运输过程中具有较高的安全性。%Guanidinium azotetrazolate(GZT)was synthesized by oxidation and cation replacement with 5-aminotet-razole(5-AT)as starting material.The title compound was characterized by FT-IR,1 HNMR,13 CNMR,elemental analysis,HPLC,MS and SEM.Thermodynamic properties of GZT were analyzed by DSC and its friction sensitivity and impact sensitivity were tested.The optimal conditions obtained by experiment are as follows:KOH concentra-tion 1 .5 mol/L,n(5-AT)∶n(KMnO4 )∶n(GN)= 1 .0∶1 .0∶1 .1 ,oxidation reaction temperature 60℃,oxidation reaction time 60 min,cation replacement reaction temperature 80℃.Under the optimal conditions,the yield can reach to 97.2% and the purity is higher than 99%.The product is in uniform yellow acicular crystal state.The thermal decomposition temperature of the product is 256.6℃ and the friction sensitivity and impact sensitivity are 4% and 1 6%,respectively,showing that this rich nitrogen compound with high decomposition temperature and low mechanical sensitivities has good safety in the production and transportation process.