4,4',6,6'-四叠氮基偶氮-1,3,5-三嗪(TAAT)的合成、表征与热分解研究

Synthesis,Characterization and Thermal Decomposition Mechanism of 4,4',6,6'-Tetra(azido)azo-1,3,5-triazine(TAAT)

以4,4',6,6'-四叠氮基联氨-1,3,5-三嗪(TAHT)为原料,经三氯异氰尿酸(TCI)、二氯异氰尿酸(DCI)、二氯异氰尿酸钠(SDCI)、二溴异氰尿酸钠(SDBI)、N-氯代丁二酰亚胺(NCS)、N-溴代丁二酰亚胺(NBS)、氯气(Cl2)、液溴(Br2)、次氯酸钠(NaClO)等氧化联氨键形成偶氮键合成了4,4',6,6'-四叠氮基偶氮-1,3,5-三嗪(TAAT),产率72%～93%.通过FT-IR,13C NMR,MS,元素分析等手段对其进行了表征;考察了不同氧化剂对氧化联氨键形成偶氮键反应的影响,验证了TAHT氧化合成TAAT的机理.通过DSC、程序升温FT-IR等测试结果,提出了TAAT的热分解机理.

4,4＇,6,6＇-Tetra（azido）azo-1,3,5-triazine（TAAT） was synthesized from 4,4＇,6,6＇-tetra（azido）hydrazo-1,3,5-triazine（TAHT） by the oxidative reaction with trichloroisocyanuric acid（TCI）,dichloro-isocyanuric acid（DCI）,sodium dichloroisocyanurate（SDCI）,sodium dibromoisocyanurate（SDBI）,N-chlorosuccinide（NCS）,N-bromosuccinide（NBS）,Cl2,Br2 and sodium hypochlorite（NaClO） with the yields of 72%～93%.Its structure was characterized by FT-IR,13C NMR,MS techniques and elemental analysis.The effects of different oxidants on oxidation reaction of hydrazo group were investigated,the oxidation mechanism of TAHT was proved and a thermal decomposition mechanism of TAAT was presented based on the results of DSC and FTIR with a dynamic heating process from 50 ℃ to 600 ℃.