The thermal decomposition process of 2,6-hexanitrodiphenyl-amine-3,5-dinitropyridine(PYX) was investigated by TG/DTG,TG/FTIR,TG/MS and therolysis rapid scan FTIR coupling techniques.The results show that the thermal decomposition process can be divided into two steps: the C-NO2 is omerizating to C-ONO,cyclization of-NH-and-NO2,releasing NO and forming polyacryl compounds in the first step,and polyacryl compounds decomposing and releasing HCN,CO,CO2 and H2O gases in the second step.