Method for synthesizing 5,5'-dinitroamino-3,3'-co-1,2,4-triazole carbohydrazide

Abstract

The invention discloses a method for synthesizing 5,5'-dinitroamino-3,3'-co-1,2,4-triazole carbohydrazide. The carbohydrazide has the following structural formula, wherein the structural formula is as shown in the specification. In the method, 5,5'-diamino-3,3'-co-1,2,4-triazole serves as a raw material, and the method comprises the following steps: (1) adding the 5,5'-diamino-3,3'-co-1,2,4-triazole into a nitric acid and ammonium nitrate system in batches at the temperature of 0 DEG C, wherein a molar ratio of the 5,5'-diamino-3,3'-co-1,2,4-triazole, nitric acid to ammonium nitrate is 1:40: (4-8), stirring for 15 minutes, raising the temperature to 25 DEG C, reacting for 1.5 hours, pouring the reaction liquid into ice water, filtering, washing and drying to obtain 5,5'-dinitroamino-3,3'-co-1,2,4-triazole; and (2) adding the 5,5'-dinitroamino-3,3'-co-1,2,4-triazole, an aqueous liquid of sodium hydroxide and carbohydrazide into a reaction bottle under the temperature of 60 DEG C, wherein a molar ratio of the 5,5'-dinitroamino-3,3'-co-1,2,4-triazole, sodium hydroxide to carbohydrazide is 1:3:2.05, stirring for 20 minutes, dropwise adding 35 mass percent of hydrochloric acid until the pH value is 4-7, reducing the temperature to 25 DEG C, separating out a white product 5,5'-dinitroamino-3,3'-co-1,2,4-triazole carbohydrazide in the system. The method is mainly used for preparing the5,5'-dinitroamino-3,3'-co-1,2,4-triazole carbohydrazide.

Description

technical field [0001] The invention relates to a method for synthesizing energetic ion salts of bitriazoles, in particular to a synthesis method of 5,5'-dinitroamino-3,3'-bi-1,2,4-triazole carbohydrazide salts resolve resolution. Background technique [0002] Bitriazoles are an important class of energetic compounds. Due to their high nitrogen content, high density, high enthalpy of formation, high gas production and clean detonation products, they have gradually become a research hotspot in the field of energetic materials. Experiments have shown that most bitriazole compounds are insensitive to static electricity, friction and impact. This is because triazole compounds have small dipole moments and tight molecular space arrangements, and two triazoles connected by C-C bonds The azole ring can form a large delocalized π bond, which is insensitive and thermally stable. [0003] 5,5'-Dinitroamino-3,3'-bi-1,2,4-triazole carbohydrazide salt is a bitriazole energetic ion salt...

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Problems solved by technology

[0008] The synthesis method is calculated based on 5,5'-diamino-3,3'-bi-1,2,4-triazole, and the reaction yield is 68%, but this method uses concentrated sulfuric acid to dissolve 5,5'-di The process of amino-3,3'-bi-1,2,4-triazole has severe heat release and is difficult to control, and the use of concentrated sulfuric acid is not conducive to the treatment and recovery of waste liquid in the later stage, which will bring inconvenience to future production ; In addition, the process of salting 5,5'-dinitroamino-3,3'-linked-1,2,4-triazole and carbohydrazide needs to prepare 5,5'-dinitroamino- 3,3'-bi-1,2,4-triazole sodium salt and sulfate salt of carbohydrazide, the steps are more complicated, so that the overall yield of the method is low

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