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Method for preparing high-quality energetic crystal material fine particles

A crystalline material, fine particle technology, applied in offensive equipment, explosives processing equipment, explosives, etc., can solve the problems of wide particle size distribution, irregular particle shape, waste of raw materials, etc., and achieve reduced shock wave sensitivity, narrow particle size distribution, and particle shape. Good results

Active Publication Date: 2012-01-18
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Application Information

AI Technical Summary

Problems solved by technology

However, the various cooling crystallization preparation methods reported at home and abroad at present have a wide product particle size distribution. In order to obtain the required particle size for formula design, screening means are usually used to prepare products with different particle size distributions. This method not only increases the process, More importantly, it causes a lot of waste of raw materials
In addition, the programmed cooling crystallization technology is difficult to prepare fine particle products below 50 μm, which does not meet the requirements of fine particle products required for explosive formulation design
Although fine-grained products can be prepared by quickly adding poor solvents using dissolution crystallization technology, the crystal quality of the products prepared by this method is poor, the solvent is more occluded, the crystal density is low, and the particle shape is irregular, so it is impossible to obtain high-quality energetic crystal materials.

Method used

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  • Method for preparing high-quality energetic crystal material fine particles
  • Method for preparing high-quality energetic crystal material fine particles
  • Method for preparing high-quality energetic crystal material fine particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1: RDX ultrasonic dissolution crystallization

[0015] At room temperature, add 100g of DMSO into the ultrasonic crystallizer, and add 35g of ordinary RDX while stirring at room temperature of 30°C. After it is completely dissolved, start the ultrasonic field, the frequency of the ultrasonic field is 40kHz, and the power density of the ultrasonic field is 0.5W cm -3 , then quickly add 300g ethanol, continue ultrasonication, stir for 1 hour, filter, wash, and dry to obtain 30g high-quality RDX (see attached figure 1 ), crystal density 1.7980g cm -3 , density distribution 1.7976g cm -3 to 1.7982g·cm -3 , the average particle size is 20 μm, D10=10 μm, D90=30 μm, and the particle size distribution is a normal distribution.

Embodiment 2

[0016] Embodiment 2: CL-20 ultrasonic dissolution crystallization

[0017] At room temperature, add 30g of ethyl acetate into the ultrasonic crystallizer, and add 13g of ordinary CL-20 while stirring at room temperature at 30°C. After it is completely dissolved, start the ultrasonic field, the frequency of the ultrasonic field is 20kHz, and the power density of the ultrasonic field is 1W cm -3 , and then quickly add 60g of n-heptane, continue ultrasonication, stir for 1 hour, filter, wash, and dry to obtain 11g of high-quality CL-20 (see attached figure 2 ), crystal density 2.0355g cm -3 , density distribution 2.0351g cm -3 to 2.0366g·cm -3 , the average particle size is 30 μm, D10=10 μm, D90=50 μm, and the particle size distribution is a normal distribution.

Embodiment 3

[0018] Embodiment 3: HMX ultrasonic dissolution crystallization

[0019] At room temperature, add 50g of dimethyl sulfoxide into the ultrasonic crystallizer, and add 15g of ordinary HMX while stirring at 20°C to 50°C. After it is completely dissolved, start the ultrasonic field. The frequency of the ultrasonic field is 20kHz to 120kHz. Density greater than 1×10 -3 W·cm -3 , then quickly add 30g to 100g of water, continue ultrasonication, stir for 1 hour, filter, wash, and dry to obtain 14.5g of high-quality HMX fine particle product (see attached image 3 ), crystal density 1.9018g cm -3 , density distribution 1.9010g cm -3 to 1.9021g·cm -3 , the average particle size is 10 μm to 30 μm, and the particle size distribution is a normal distribution.

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Abstract

The invention relates to a method for preparing high-quality energetic crystal material fine particles. Various high-quality energetic crystal material fine particle products, such as pentaerythritol tetranitrate (PETN), cyclotrimethylene trinitramine (RDX), cyclotetramethylenetetranitramine (HMX), hexanitrohexaazaisowurtzitane (CL-20), DADNE (FOX-7), ammonium perchlorate (AP), and the like can be prepared by adopting an ultrasound solvating-out crystallization method in the traditional solvating-out crystallization process. The high-quality energetic crystal material fine particle product prepared by the preparation method disclosed by the invention has subglobular particle form, narrow granularity distribution, average particle diameter of 5-50 microns or so, transparent crystals, high particle density, crystal theoretical density of more than 99.9 percent and obviously reduced shock wave sensitivity and is used for pouring or pressing PBX (Plastic-bonded explosives). The method for preparing the high-quality energetic crystal material fine particles has the advantages of simple process flow and mild reaction conditions and is suitable for mass industrialized production.

Description

technical field [0001] The invention belongs to the field of energetic crystal materials, in particular to a preparation method of energetic crystal materials. Background technique [0002] A large number of studies have shown that the crystal quality of explosives (such as purity, density, crystal morphology, particle size and void ratio, etc.) is one of the main factors affecting the vulnerability of explosives. While improving its functional capabilities, its safety performance is improved, especially the performance of reducing shock wave sensitivity. In recent years, improving the crystal quality of elemental explosives through crystallization technology research and preparing various types of desensitizing elemental explosives has become a hot spot in the research of energetic materials at home and abroad. Many foreign units such as French SNPE Company, Australian ADI Company, Norwegian Dyno Nobel Company, and German ICT have developed various types of reduced-sensiti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C06B21/00
Inventor 徐瑞娟康彬黄辉姜燕陈娅夏云霞
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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