Synthetic method of 5, 5'-bistetrazole-1, 1'-dioxo hydroxyl ammonium salt (TKX-50)

Abstract

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.

Description

technical field [0001] The invention relates to a synthesis method of 5,5'-bitetrazole-1,1'-dioxolamine salt (TKX-50), which belongs to the technical field of organic synthesis. Background technique [0002] In the civilian and military fields, high-energy explosives mainly belong to cyclic and caged nitramine compounds, such as RDX, HMX and CL-20, but they all have fatal shortcomings. Strategies for modern energetic materials research often allow the preservation or improvement of the detonation properties of these compounds while avoiding their existing disadvantages: toxicity, difficult and expensive synthesis (HMX, CL-20), high sensitivity to mechanical stimuli and spontaneous deterioration ( CL-20). However, the known energetic materials with the highest detonation performance are often highly sensitive due to their unprecedented energies, and the long and expensive synthetic routes make them unsuitable for practical applications. For example, the detonation velocity ...

AI Technical Summary

Problems solved by technology

Strategies for modern energetic materials research often allow the preservation or improvement of the detonation properties of these compounds while avoiding their existing disadvantages: toxicity, difficult and expensive synthesis (HMX, CL-20), high sensitivity to mechanical stimuli and spontaneous deterioration ( CL-20)

At the same time, the introduction of oxygen atoms on the nitrogen ring not only forms an interionic hydrogen bond system with the amine in the cation, but also makes the density reach 1.92g cm -3 , and has better oxygen balance and has potential application value in rocket propellants, etc., but most of its properties are unknown (including measured detonation velocity and pressure, friction sensitivity and compatibility, etc.)

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