Method for preparing special 3-nitro-1,2,4-triazole-5-ketone

A nitro, special technology, applied in the field of explosives, can solve the problems of poor molding performance, many crystal defects, difficult molding and other problems

Active Publication Date: 2016-03-23
SHANXI BEIHUA GUANLYU CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are two crystal forms of 3-nitro-1,2,4-triazol-5-one: α and β. The α crystal form is a stable triclinic crystal system, and the α crystal form is an unstable triclinic crystal system. Typical crystals are rod-shaped and easy to agglomerate. The product has a large particle size and many crystal defects, which lead to increased sensitivity and limit the scope of use.
[0004] The 3-nitro-1,2,4-triazol-5-one obtained directly during the synthesis reaction has a typical rod-like structure with an aspect ratio of about 3:1, is sensitive to shock waves, and has poor formability. It will lead to increased viscosity when charging, which is not conducive to casting. In the use of 3-nitro-1,2,4-triazol-5-one, it must be solved due to 3-nitro-1,2,4- Difficulty in forming due to crystal morphology of triazol-5-one

Method used

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  • Method for preparing special 3-nitro-1,2,4-triazole-5-ketone

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preparation example Construction

[0022] The invention provides a method for preparing special 3-nitro-1,2,4-triazol-5-one, comprising the following steps:

[0023] Provide 3-nitro-1,2,4-triazol-5-one solution;

[0024] The 3-nitro-1,2,4-triazol-5-one solution is cooled and crystallized by a cooling medium to obtain the specific 3-nitro-1,2,4-triazol-5-one. .

[0025] In the method provided by the invention, the 3-nitro-1,2,4-triazol-5-one solution is cooled and crystallized through a cooling medium, and the recrystallization technology is used to increase the crystal density of the simple explosive, reduce internal defects of the crystal, and eliminate surface defects , the surface is smooth and dense, and the crystal shape and particle size are controlled, thereby improving the quality of the simple explosive and satisfying the molding performance.

[0026] The invention uses a cooling medium to cool and crystallize the 3-nitro-1,2,4-triazol-5-one solution. In the present invention, the solvent in the 3-n...

Embodiment 1

[0040] Put 170L of ethylene glycol in the cooling medium in advance, set the temperature difference of the cooling equipment through the SL-20L cooling device to control the temperature of the cooling medium -25°C±2°C; use a double-layer coil crystallization kettle with a capacity of 200L, at room temperature Add 9.3L of water and 3.1L of N-methylpyrrolidone into the crystallization kettle of the double-layer coiled tube crystallization kettle, and dissolve at 65°C; under stirring conditions, add 1kg of NTO (microstructure such as figure 1 As shown, the raw material 3-nitro-1,2,4-triazol-5-one is a typical rod-shaped structure, and its length-to-diameter ratio is about 3: 1), and the NTO is completely dissolved and drained in the jacket of the crystallization kettle Hot water; immediately pour the cooling medium into the inner cooling coil of the double-layer coiled tube crystallization kettle and the jacket of the double-layer coiled tube crystallization tank for cooling and c...

Embodiment 2

[0043] The special 3-nitro-1,2,4-triazol-5-one was prepared by adopting the technical scheme of Example 1. The difference is that in this example, the cooling medium is ethanol, and the temperature of the cooling medium is 23°C± At 2°C, the mass fraction of the 3-nitro-1,2,4-triazol-5-one solution is 8%.

[0044] The characteristic 3-nitro-1,2,4-triazol-5-one crystal obtained in this example is nearly spherical, with a smooth and dense surface; the obtained 3-nitro-1,2,4-triazole-5- The crystallization of ketone is up to 180 microns, the shape is spherical, the roundness value is 0.9, the shock wave sensitivity is reduced, the ratio of the long and short axis is 1.05-1.1, the crystal surface is smooth, the edges and corners are few, and the spherical shape is beneficial to reduce the sensitivity of explosives.

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Abstract

The invention discloses a method for preparing special 3-nitro-1,2,4-triazole-5-ketone. The method comprises the following steps: providing a 3-nitro-1,2,4-triazole-5-ketone solution; and cooling the 3-nitro-1,2,4-triazole-5-ketone solution with a cooling medium and crystallizing to obtain the special 3-nitro-1,2,4-triazole-5-ketone. According to the provided method, a recrystallization technology is employed for increasing crystal density of a single-compound explosive, reducing internal defect of the crystal, and eliminating surface defects, so that the surface is smooth and dense, crystal shape and granularity can be controlled, quality of the single-compound explosive is enhanced, and moulding performance can be satisfied.

Description

technical field [0001] The invention relates to the field of explosives, in particular to a preparation method of special 3-nitro-1,2,4-triazol-5-one. Background technique [0002] 3-nitro-1,2,4-triazol-5-one (NTO) is a high-energy insensitive explosive with energy close to cyclotrimethylene trinitramine and sensitivity close to triaminotrinitrobenzene. Since the 1980s, extensive research has been carried out at home and abroad on the synthesis, properties, structure and mixed explosive formulations of 3-nitro-1,2,4-triazol-5-one. The research shows that 3-nitro-1 , The detonation performance and sensitivity of 2,4-triazol-5-one are closely related to the crystal morphology. [0003] There are two crystal forms of 3-nitro-1,2,4-triazol-5-one: α and β. The α crystal form is a stable triclinic crystal system, and the α crystal form is an unstable triclinic crystal system. Typical crystals are rod-shaped and easy to agglomerate. The product has a large particle size and many ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/14
CPCC07B2200/13C07D249/14
Inventor 毋文莉刘波贾宏选刘小社侯鹤卫涌闫华
Owner SHANXI BEIHUA GUANLYU CHEM IND
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