4,5-二(1H-四唑-5-基)-1H-咪唑的合成及热性能  

Synthesis and Thermal Decomposition Properties of 4,5-Bis( 1H-tetrazol-5-yl)-1H-imidazole

作　　者：毕福强[1] 李吉祯[1] 许诚[1] 樊学忠[1] 高红旭[1] 康冰[1] 葛忠学[1] 刘庆[1] 

机构地区：[1]西安近代化学研究所,陕西西安710065

出　　处：《含能材料》2013年第4期443-448,共6页Chinese Journal of Energetic Materials

摘　　要：以N,N-二甲基甲酰胺(DMF)为溶剂,优化了4,5-二(1H-四唑-5-基)-1H-咪唑(H3BT I)的合成工艺:4,5-二氰基咪唑、叠氮化钠和氯化铵的摩尔比为1:2.2:2.2,反应温度90℃,反应时间8 h,收率为94.6%。通过红外光谱、1HNMR、13C N M R和元素分析对H3BTI的结构进行了表征,采用DSC和T G/DT G技术研究了H3BT I的热分解性能,用非等温DSC技术研究了热分解反应动力学。研究结果表明,H3BT I的活化能为197.62 kJ·mol-1,指前因子为16.16;H3BTI的临界爆炸温度为556.38 K,大于R DX的487.90 K,表明其热稳定性优于R DX;热分解反应的活化熵、活化焓和活化自由能分别为35.72 J·mol-1·K-1、193.66 kJ·mol-1和173.33 kJ·mol-1。4,5-Bis（1H-tetrazol-5-yl）-1H-imidazole（H3BTI）is a high-nitrogen azole compound which may be suitable as ingredi-ent for low signal propellant and gas generator. The synthetic technology of H3BTI was optimized with the yield of 94. 6% as following：the molar ratio of 4,5-dicyanoimidazole,sodium azide and ammonium chloride,2. 22. 21,solvent DMF,reaction temperature 90 ℃,and reaction time 8 h. The thermal behavior and non-isothermal decomposition kinetics of H3BTI were studied with DSC and TG/DTG method. Results show that the kinetic parameters of thermal decomposition reaction,are the activation energy and pre-exponential factor are 197. 62 kJ·mol -1 and 16. 16,respectively,and the critical temperature of thermal explosion of H3BTI is 556.38 K,which indicates that H3BTI has better thermal stability than that of RDX,and activation entropy,activation enthalpy and activation Gibbs free energy of the thermal decomposition are 35. 72 J·mol -1 ·K -1,193.66 kJ·mol -1 and 173. 33 kJ·mol -1 ,respectively.

关 键 词：应用化学 含能材料 4 5-二（1 H-四唑-5-基）-1 H-咪唑 合成 热性能 

分 类 号：O626.23[理学—有机化学]