Preparation method and property of 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole diammonium salt structure

A technology of dinitro and diammonium salts, which is applied in the direction of offensive equipment, nitrated explosive components, nitrated acyclic/alicyclic/heterocyclic amine explosive compositions, etc., to achieve easy large-scale production, simple synthesis method, and mild conditions Effect

Inactive Publication Date: 2018-10-19
BEIJING INSTITUTE OF TECHNOLOGYGY
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Problems solved by technology

Salt formation can generally improve its sensitivity. Currently, only triaminoguan

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  • Preparation method and property of 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole diammonium salt structure
  • Preparation method and property of 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole diammonium salt structure
  • Preparation method and property of 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole diammonium salt structure

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[0021] Add 2.54g (10mmol) of 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole and 50ml of water to a 100ml single-neck flask equipped with magnetic stirring, and heat to Dissolve, then quickly add (3.40g, 10mmol) silver nitrate, stir for 1h in the dark, and filter to obtain a yellow solid 3,3'-dinitro-5,5'-azo-1H-1,2,4-tri Silver azole salt 4.30g, yield 92%; elemental analysis: C 4 Ag 2 N 10 O 4 (467.84) (%) Calculated value: C 10.27, H 0.00; N 29.94; measured value: C10.09, H0.08, N 29.71.

[0022] 467 mg (1 mmol) of 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole silver salt was added to 107 mg (2 mmol) of ammonium chloride aqueous solution (50 mL). Stir at 80°C for 4h, and filter off the AgCl precipitate while it is hot. The filtrate was evaporated to dryness and recrystallized with water. After drying, 219 mg of 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole diammonium salt was obtained, with a yield of 76%. Decomposition temperature: 248°C (DSC, heating rate 5°C / min). IR(neat): 3255,2962,2835,16...

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Abstract

The invention relates to a preparation method and property of a high-energy insensitive explosive 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole diammonium salt structure, and belongs to the technical fieldof energetic materials. The synthesis method comprises the following steps: heating and dissolving 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole into water, adding silver nitrate with molar equivalent of 2,reacting for 1 hour under a dark condition and at a room temperature, filtering to obtain yellow solid, washing the solid with cold water for twice, and drying to obtain 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole silver salt; and adding the synthesized silver salt into an ammonium chloride aqueous solution with molar equivalent of 2, performing stirring reaction at 80 DEG C for 4 hours, filtering out precipitate after reaction, evaporating the filtrate to dryness, and recrystallizing the obtained solid with a small amount of water to obtain the corresponding product 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole diammonium salt. The synthesis method is simple, stable in properties and easy in amplified preparation. According to the synthesized energetic compound, the decomposition temperature is248 DEG C, the density is 1.89 g/cm<3>, the detonation velocity is calculated to be 9071 m/s, and the detonation pressure is 32.9 GPa. The detonation performance and HMX are equivalent and insensitive, and the explosive is a novel high-energy insensitive explosive with application potentiality.

Description

technical field [0001] The invention relates to a preparation method and performance of a novel high-energy insensitive explosive 3,3'-dinitro-5,5'-azo-1H-1,2,4-triazole bis-ammonium salt, and belongs to the technical field of energetic materials . Background technique [0002] In recent years, high-energy-density materials (HEDM), as a new type of high-energy explosive, have become a research hotspot in the field of energetic materials. The ideal characteristics of new energetic materials include: high positive enthalpy of formation, high density, high detonation velocity and pressure, good thermal stability, and low sensitivity to external stimuli such as impact or friction. However, high performance and low sensitivity are inherently contradictory, which brings many interesting but challenging problems to the synthesis of new high-energy-density materials. People have been trying to find a balance between performance and stability, expecting to design and synthesize new...

Claims

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Application Information

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IPC IPC(8): C07D249/14C06B25/00
CPCC07D249/14C06B25/34
Inventor 周智明李川
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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