Nitropyrazole energetic compound and synthesis method thereof

A technology of nitropyrazole and synthetic method, applied in the direction of nitrated acyclic/alicyclic/heterocyclic amine explosive composition, organic chemistry, etc., can solve the problems of high sensitivity, low yield, high cost, etc., and achieve improved detonation The effect of high performance, simple synthesis, and low cost

Active Publication Date: 2022-03-08
HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0009] Trinitromethyl (nitroform) has very high energy. As early as the last century, a large number of scientific and technological workers designed and synthesized a large number of nitroform-based compounds, but the sensitivity is very high, which affects the practical application of this type of energetic compounds.
However, there are many ways to prepare the key intermediate trinitropyrazole, one of which is to use pyrazole as a raw material through nitration or multi-step nitration. The yield is low and the cost is high, which is not suitable for further engineering and amplification synthesis.

Method used

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  • Nitropyrazole energetic compound and synthesis method thereof
  • Nitropyrazole energetic compound and synthesis method thereof
  • Nitropyrazole energetic compound and synthesis method thereof

Examples

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Embodiment 1

[0068] Step (1) Add 2.05g (20mmol) 4-chloropyrazole to 25mL concentrated sulfuric acid in batches under ice bath. After it is completely dissolved, slowly add 2.6mL fuming nitric acid dropwise to the reaction system, and remove the In an ice bath, heat the mixture to 105°C, continue the reaction for 5 hours, cool, pour the reaction solution into the ice-water mixture under vigorous stirring, extract three times with ethyl acetate, combine the organic phases and wash with a small amount of saturated saline , dried over anhydrous magnesium sulfate, filtered, the organic phase was distilled off under reduced pressure to remove the solvent, and 2.93 g of a white solid was obtained, which was 3,5-dinitro-4-chloropyrazole (intermediate 1), and the yield of this step was 76 %.

[0069] Step (2) Add 15.4g (80mmol) 3,5-dinitro-4-chloropyrazole and 144mL 25% ammonia water to a 900mL pressure reactor, heat up to 150°C for 10 hours, cool to room temperature, and A large number of bright ...

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Abstract

The invention discloses a synthesis method of a nitropyrazole energetic compound, which comprises the following steps: by taking 4-chloropyrazole as a raw material, carrying out nitration, ammonification and oxidation to prepare an important intermediate trinitropyrazole, and reacting the trinitropyrazole with bromoacetone for nitration to obtain the nitropyrazole energetic compound, thereby effectively lowering the synthesis cost and enhancing the yield. The invention further discloses the nitropyrazole energetic compound obtained on the basis of the method, and the energetic compound is high in oxygen content and theoretical energy and can serve as an energetic material to be applied to the fields of explosives, propellants, initiating explosive devices and the like.

Description

technical field [0001] The invention belongs to the field of energetic materials and their synthesis, in particular to a nitropyrazole energetic compound and its synthesis method. Background technique [0002] Energetic materials, including simple explosives and mixed explosives, are the foundation for the development of advanced weapons and equipment. High energy density materials are energetic materials mainly used in propellants and explosives, which means that energetic compound molecules only store and release their energy by forming and breaking bonds, and their energy density performance is higher than that of ordinary energetic materials. [0003] Improving the energy level is an eternal theme in the development of energetic material technology. In order to improve the combat effectiveness of weapons and ammunition, energetic materials must have higher energy in the future. The application of high-energy-density materials has a major impact on the damage effects of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/16C06B25/34
CPCC07D231/16C06B25/34
Inventor 张思王发迅黎小平余凯伦邱贤平朱朝阳周智明
Owner HUBEI INST OF AEROSPACE CHEMOTECHNOLOGY
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