The dihydroxylammonium 5, 5′-bistetrazole -1, 1′-diolate(TKX-50) was synthesized using solution glyoxal (40% w/w in H₂O) and hydroxylammonium as starting materials by substitution, chloration, nitrine reaction, ring formation reaction, and salt formation reaction. Its structure was characterized by elemental analysis and NMR, and its impact sensitivity and friction sensitivity were studied. The effects of reaction temperature, holding time and holding temperature on yield of 5, 5′-bistetrazole -1, 1′-diolate (BTO), and the effect of concentration of hydroxylamine on yield of TKX-50 were discussed. Results show that the impact sensitivity H₅₀ for TKX-50 is 41 cm, and its friction sensitivity is 0%.The optimal reaction condition are as following: reaction temperature 0-5 ℃, holding time 12 h, holding temperature 20-25 ℃, when the concentration of hydroxylamine is 50%(w/w in H₂O).