3，4‐Bis（3'‐aminofurazan‐4'‐yl）furazan（BATF）was synthesized by reduction with stannous chloride in glycerol using 3，4‐bis（3'‐aminofurazan‐4'‐yl）furoxan（BAFF） as raw material. 3，4‐Bis（3'‐nitrofurazan‐4'‐yl）furazan（BNTF） was prepared from BAFF by using hydrogen peroxide as oxidantwith total yield of 59.0%. The structures of BATF and BNTF were characterized by 1H NMR，13C NMR，IR，MS spectra and elemental analysis，and the single crystal structure data of BNTF was obtained successfully. The crystal belongs to orthorhombic system，space group P212121 with crystal parameters a=0.71437（10） nm， b=0.96839（11）nm，c=51555（17）nm，V=1.0484（2）nm3，Z=4，Dc=1.876 g·cm-3，F（000）=592. The influence of molar ratio，reaction time，and reaction temperature on the yield of BNTF was investigated. Results show that the optimum conditions are as follows：n（BATF）∶n（35% H2O2）∶n（98% H2SO4 ）∶n（Na2WO4?2H2O）=1∶60∶40∶0.86，the reaction time is 3 h，the reaction temperature is 30 ℃ and the yield of BNTF is 93.3%. The thermal stability of BNTF was determined by DSC and TG‐DTG methods. Apparent activation energy Ea（147.83 kJ·mol-1），pre‐exponential factor A（9.33×1015 min-1）and decomposition rate constant k （2.18×10-44）of thermal decomposition reaction for BNTF were calculated by Kissinger method，Rogers method and Arrenhis method，respectively. The detonation velocity（8.3 km·s-1）and detonation pressure（31.3 GPa）of BNTF were estimated by Ka‐mlet‐Jacobs equation. Characteristic drop height of impact sensitivity（H50=43.0 cm）and friction sensitivity（36.0%）for BNTF were measured according to GJB772A-1997 methods 601.2 and 602.1，respectively.