Preparation method of hexaazaisowurtzitane crystal

A technology of heteroisopentazine and hexanitrohexaazine, which is applied to the preparation of high-quality energetic material crystals and the preparation field of hexanitrohexaazaisopentzitane crystals, which can solve the problem that the product quality is difficult to control and operate. Complex process, low purity, etc., to achieve the effect of reduced mechanical sensitivity, simple preparation process and high crystal quality

Active Publication Date: 2013-07-24
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of the existing solvent / non-solvent recrystallization method of explosives, such as complicated operation process, difficult control of product quality, low yield and low purity, and provide a hexanitrohexaazaisopentazine The preparation method of alkane crystals, the preparation method is a two-step preparation technology of ordinary explosive particles through mechanical crushing and then solvothermal induction growth. By adjusting the reaction conditions, high-quality explosives with different shapes and particle sizes can be obtained. crystal material

Method used

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  • Preparation method of hexaazaisowurtzitane crystal
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  • Preparation method of hexaazaisowurtzitane crystal

Examples

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Embodiment 1

[0027] At room temperature, weigh 50g of CL-20 raw material, add 50g of water, 4 tungsten carbide balls with a diameter of 5mm and 40 tungsten carbide balls with a diameter of 2mm, grind at a speed of 350rpm for 60min, centrifuge the material liquid, wash and freeze-dry to obtain 48.3 g fine particle CL-20. Take 10g of fine particle samples, add 40g of deionized water, ultrasonically disperse at 20kHz for 1min, heat the feed solution to 90°C in a standing state, and keep it for 120min. The product was filtered, washed and dried to obtain 9.8 g of high-quality CL-20 with a yield of 98%.

[0028] The above-mentioned high-quality CL-20 was tested, analyzed and performance tested, and the results are as follows:

[0029] (1) Sample crystal characteristics

[0030] The TM-1000 scanning electron microscope (SEM) was used to characterize and analyze the surface morphology of the fine-grained explosives after wet ball milling and the final high-quality CL-20 explosive crystal produc...

Embodiment 2

[0033]At room temperature, weigh 100g of CL-20 raw material, add 150g of water, 8 tungsten carbide balls with a diameter of 5mm and 60 tungsten carbide balls with a diameter of 2mm, grind at a speed of 400rpm for 120min, centrifuge the material liquid, wash and freeze-dry to obtain 95.1 g fine particle CL-20. Carry out 2 batches of explosive wet grinding again in the same way. Take 250g of fine particle samples, add 500g of deionized water, ultrasonically disperse at 100kHz for 5min, heat the feed solution to 95°C in a static state, and keep it for 180min. The product was filtered, washed, and dried to obtain 247.9 g of high-quality CL-20 crystals, with a yield of 99.2%.

Embodiment 3

[0035] At room temperature, weigh 50g of CL-20 raw material, add 50g of water, 4 tungsten carbide balls with a diameter of 5mm and 40 tungsten carbide balls with a diameter of 2mm, grind at a speed of 350rpm for 90min, centrifuge the material liquid, wash and freeze-dry to obtain 48.8 g fine particle CL-20. Take 10g of fine particle samples, add 40g of deionized water, ultrasonically disperse at 20kHz for 2min, heat the material solution to 80°C with stirring speed at 200rpm, and keep it for 150min. The product was filtered, washed, and dried to obtain 9.8 g of high-quality CL-20 crystals, with a yield of 98%.

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Abstract

The invention discloses a preparation method of a hexaazaisowurtzitane crystal. The preparation method of the hexaazaisowurtzitane crystal comprises the following steps of: carrying out wet-crushing onto explosives until the particle dimension is 0.1 micron to 5 microns, centrifuging, washing, freezing and drying the crushed materials; placing the material in the step I to a solvent for carrying out ultrasonic treatment, heating, re-filtering, washing and drying under the standing condition or the stirring condition to obtain a hexaazaisowurtzitane explosive crystal. According to the preparation method of the hexaazaisowurtzitane crystal, the high-quality explosive crystal product, which is prepared by a preparation technology adopting a two-step process including mechanical crushing and solvent thermal-induction growing, is regular in particle shape, jewel-shaped, uniform in particle dimension, smooth in surface, less in internal defects of the crystal, and lower in mechanical sensitivity. Besides, the preparation method of the hexaazaisowurtzitane crystal is simple in process, gentle in reaction conditions, good in reproducibility, high in yield and suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of material science, and relates to a method for preparing high-quality energetic material crystals, in particular to a method for preparing hexanitrohexaazaisopentazane crystals. Background technique [0002] The purity, morphology, particle size and crystal form of crystal materials are the most important factors that determine the basic properties and application value of crystals. For high explosives, these factors determine the density, energy, sensitivity, and other properties of the explosive. The so-called high-quality explosives refer to high density, high chemical and crystal form purity, regular crystal morphology, smooth surface, high degree of spherification, good particle uniformity, few crystal defects, narrow density distribution, and reduced shock wave sensitivity and mechanical sensitivity. of dynamite crystals. Through crystallization technology, improving the crystal quality of explosive material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C06B49/00C06B21/00
Inventor 杨志剑吴鹏郝世龙丁玲徐容李金山
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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