The invention provides a method for preparing 5, 5'-bistetrazole-1, 1'-dioxo hydroxyl
ammonium salt (TKX-50), and belongs to the technical field of
organic synthesis. The method comprises the steps as follows: step one, glyoxime is prepared, and the yield is 62%; step two, a product obtained in the step one is dissolved in water and concentrated
hydrochloric acid,
chlorine is introduced at the temperature of 0 DEG C for a reaction for a period of time, and dichloroglyoxime is obtained; and finally, a product obtained in the step two is dissolved in a
solvent, and the product and
sodium azide have a reaction at the temperature of 0 DEG C for a period of time; after that, the mixture is transferred into diethy
ether, and sealed for a reaction at the
room temperature overnight after HCl is introduced for a period of time; and after
diethyl ether and most HCl gas are volatilized, pH of an aqueous NaOH solution is regulated to be about 8,
reflux cooling is performed, filtered and separated solids are dissolved in
hydroxylamine hydrochloride to have a reaction for a period of time, and TKX-50 is obtained. According to the method,
glyoxal is adopted as a
raw material, water is adopted as a
solvent for preparation of dichloroglyoxime in the step two, and only direct
filtration is required in postprocessing, so that the tedious purification process is prevented, and the cost is reduced; and besides, a target product TKX-50 is synthetized through three steps of reactions, the total yield is up to 34%, the reaction condition is mild, the operation is simple and convenient, and the industrialization is easy to realize.