4,5-二(1H-四唑-5-基)-1H-咪唑的合成及热性能
2013,21(4):443-448
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(H3BTI)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、1H NMR、13C NMR和元素分析对H3BTI的结构进行了表征，采用DSC和TG/DTG技术研究了H3BTI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，H3BTI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RDX的487.90 K，表明其热稳定性优于RDX；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。
关键词：应用化学; 含能材料; 4,5-二(1H-四唑-5-基)-1H-咪唑; 合成; 热性能
Synthesis and Thermal Decomposition Properties of 4,5-Bis(1H-tetrazol-5-yl)-1H-imidazole
Abstract: 4,5-Bis(1H-tetrazol-5-yl)-1H-imidazole(H3BTI) is a high-nitrogen azole compound which may be suitable as ingredient 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.
Key words:Applied chemistry; energetic material; 4,5-bis(1H-tetrazol-5-yl)-1H-imidazole; synthesis; thermal decomposition performance
投稿时间：2012-06-21
