By condensation reaction of 3,3-dinitroazetidine with phosgene and oxalyl chloride,two polynitrocompounds were obtained. Their thermal kinetic parameters were determined by DSC experiment and structure were identified by IR spectrum,NMR analysis. Quantum chemistry calculation for bis(3′,3′-dinitroazetidine)one was made by using SCF-MO-AM1 code and the optimal geometric configuration and electronic structure were obtained therefrom.