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.