Method for preparing high-quality fine granules of energy-containing crystal material

A crystal material and high-quality technology, applied in the field of energetic crystal material preparation, can solve the problems of not meeting the requirements of explosive fine particle products, difficulty in preparing fine particle products, increasing the process, etc., achieving high sphericity, reduced shock wave sensitivity, Effect of narrow particle size distribution

Active Publication Date: 2011-11-02
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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Problems solved by technology

However, the RDX cooling crystallization methods reported at home and abroad are difficult to produce fine particle products below 50 μm, which do not meet the requirements of fine particle products required for explosive formulation design.
In addition, the particle size distribution of the product prepared by the traditional cooling crystallization technology is wide. In order to obtain the particle size required by the formula design, the products with different particle size distribution are usually prepared by screening. This method not only increases the process, but also causes a lot of raw materials. waste of

Method used

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  • Method for preparing high-quality fine granules of energy-containing crystal material
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  • Method for preparing high-quality fine granules of energy-containing crystal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1: Ultrasonic cooling crystallization of RDX in butyrolactone solvent

[0015] At room temperature, add 50ml of butyrolactone into the ultrasonic crystallizer, add 20g of ordinary RDX under stirring, raise the temperature of the solution to 75°C, start the ultrasonic field after it is completely dissolved, the frequency of the ultrasonic field is 68kHz, and the power density of the ultrasonic field is 0.1 W·cm -3 , and then at a cooling rate of 5°C / min to a solution temperature of 30°C, filtered, washed, and dried to obtain 10.2g of high-quality RDX fine particle product (see the appendix figure 1 ), crystal density 1.7979g cm 3 , density distribution 1.7976g cm 3 to 1.7982g·cm 3 , average particle size 50.2μm, D 10 = 40μm, D 90 =60μm, the particle size distribution is a normal distribution.

Embodiment 2

[0016] Embodiment 2: Ultrasonic cooling crystallization of RDX in cyclohexanone solvent

[0017] At room temperature, add 100ml of cyclohexanone into the crystallizer, and then add 20g of ordinary hexogen under stirring, raise the temperature to 80°C, and start the ultrasonic field after it is completely dissolved. The frequency of the ultrasonic field is 28kHz, and the power density of the ultrasonic field is 0.04W·cm -3 , and then at a cooling rate of 1°C / min until the solution temperature is 30°C, filter, wash, and dry to obtain 8g of high-quality RDX fine particle product (see the appendix figure 2 ), crystal density 1.7980g cm 3 , density distribution 1.7976g cm 3 to 1.7983g·cm 3 , average particle size 30μm, D 10 = 15 μm, D 90 =60μm, the particle size distribution is a normal distribution.

Embodiment 3

[0018] Embodiment 3: Ultrasonic cooling crystallization of HMX in butyrolactone solvent

[0019] At room temperature, add 50ml of butyrolactone into the ultrasonic crystallizer, add 20g of ordinary HMX under stirring, raise the temperature of the solution to 85°C, start the ultrasonic field after it is completely dissolved, the frequency of the ultrasonic field is 28kHz, and the power density of the ultrasonic field is 0.1 W·cm -3 , and then at a cooling rate of 5 °C / min to a solution temperature of 30 °C, filtered, washed, and dried to obtain 9 g of high-quality HMX fine particle product with a crystal density of 1.9020 g cm -3 , density distribution 1.9015g cm -3 to 1.9023g·cm -3 , average particle size 10.3μm, D 10 =5μm, D 90 =25μm, the particle size distribution is a normal distribution.

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Abstract

The invention discloses a method for preparing high-quality fine granules of an energy-containing crystal material. In the core content of the method, the power ultrasound technology is introduced in the process of cooling crystallization, and a high-quality fine granular product, which has the average grain diameter of about between 10 and 50 micrometers, of the energy-containing crystal material is prepared by a method of ultrasound cooling crystallization, namely the method comprises the following steps of: (1) dissolving the ordinary energy-containing crystal material in different solvents at high temperature to form saturated crystallization solution; (2) cooling the crystallization solution according to a certain speed, and stirring and performing ultrasound processing; and (3) whenthe temperature of the crystallization solution is close to a given temperature, stopping the ultrasound processing, cooling and stirring, filtering, washing and drying to obtain the high-quality fine granular product of the energy-containing crystal material. In the method of ultrasound cooling crystallization, the high-quality fine granular product of the energy-containing crystal material has few defects and is good in appearance of the granules, high in sphericity and narrow in distribution of granularity, the apparent density of crystals reaches the theoretical density of the crystals ofmore than 99.9 percent, and the sensitivity of impact waves is reduced obviously.

Description

technical field [0001] The invention belongs to the field of preparation of energetic crystal materials, and in particular relates to a preparation method of high-quality fine particle products 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, Australian ADI, Norwegian Dyno Nobel, and German ICT have ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B30/06C30B7/06
Inventor 康彬徐瑞娟黄辉姜燕陈娅夏云霞
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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