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Method for preparing large-granule triaminotrinitrobenzene through circular heating and cooling

A technology of triaminotrinitrobenzene and large particles, which is applied in organic chemical methods, purification/separation of amino compounds, organic chemistry, etc., can solve problems such as large safety risks, limited production scale, and failure to meet application requirements, and achieve safety Good performance, increased mechanical strength, and improved charge fluidity

Active Publication Date: 2017-03-15
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

However, due to the high temperature and high pressure operation, there are not only large safety risks, but also the preparation scale is greatly limited, which is far from meeting the application requirements; in addition, the preparation technology of TATB particles with a larger size above 100 μm has not yet been industrialized. Production technology

Method used

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  • Method for preparing large-granule triaminotrinitrobenzene through circular heating and cooling
  • Method for preparing large-granule triaminotrinitrobenzene through circular heating and cooling

Examples

Experimental program
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Effect test

Embodiment 1

[0025] At room temperature, the raw material TATB (5g) with an average particle size of 10μm was added to dimethyl sulfoxide (100ml), the stirring speed was 100-300rpm, the temperature was raised to 120°C at a speed of 3°C / min and kept for 30 minutes, the TATB part Dissolve to obtain a TATB suspension, then lower the temperature to 20°C at a rate of 3°C / min according to the temperature control program, and keep at this temperature for 10 minutes to obtain a larger particle TATB suspension, filter, wash with water, and dry. TATB crystal particles with an average particle size of about 60 μm were obtained, and the appearance of large TATB particles was as follows figure 2 shown.

Embodiment 2

[0027] At room temperature, the submicron TATB (5g) with an average particle size of 500nm was added to dimethyl sulfoxide (300ml), the stirring speed was 200-400rpm, and the temperature was raised to 120°C at a speed of 3°C / min and maintained for 30 minutes. TATB is partially dissolved to obtain a TATB suspension, and then the temperature is lowered to 20°C at a rate of 1°C / min according to the temperature control program, and kept at this temperature for 10 minutes to obtain a larger particle TATB suspension, and then repeat the temperature rise and fall for 1 times, filtered, washed with water, and dried to obtain TATB crystal particles with an average particle size of about 80 μm.

Embodiment 3

[0029] At room temperature, TATB (5 g) with an average particle size of 10 μm was added to N,N-dimethylformamide (500 ml), the stirring speed was 100-300 rpm, and the temperature was raised to 100 ° C at a speed of 3 ° C / min and kept After 10 minutes, TATB was partially dissolved to obtain a TATB suspension, and then the temperature was lowered to 20°C at a rate of 1°C / min according to the temperature control program, and kept at this temperature for 10 minutes to obtain a larger particle TATB suspension, and then repeat The temperature was raised and lowered twice, filtered, washed with water, and dried to obtain TATB crystal particles with an average particle size of about 60 μm.

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Abstract

The invention discloses a method for preparing large-granule triaminotrinitrobenzene (TATB) through circular heating and cooling. The method comprises the following steps: adding a TATB raw material with different granularities into a certain amount of a re-crystallization solvent under a stirring condition, rising the temperature to dissolve parts of the TATB in order to obtain a suspension, and cooling the suspension to room temperature according to a temperature control program in order to make granules gradually grow; and repeating the above heating and cooling process until the dimension of the TATB granules reach 50 [mu]m or above, filtering the granules, washing the filtered granules, and drying the washed granules to obtain the large-granule TATB. The large-granule TATB has regular morphology and good granule dispersibility, has far higher crystal apparent density than the raw material TATB, and has substantially increased mechanical strength. The method has the advantages of simple process, convenience in operation, good safety, easiness in engineering amplification, and realization of great reduction of the use amount and cycle use of the re-crystallization solvent. The obtained large-granule TATB can be used for casting and press-loading charges, obviously increases the solid content of the charges, improves the fluidity of the charges, and improves the anisotropy expansion and the shape stability of TATB-based explosives.

Description

technical field [0001] The invention belongs to the field of energetic materials, and in particular relates to a method for preparing large particles of triaminotrinitrobenzene (TATB) (50 μm-200 μm). The invention has very good application prospects in military explosives. Background technique [0002] Triaminotrinitrobenzene (TATB) is the only elemental insensitive explosive currently approved. It is very insensitive to external stimuli such as heat, light, shock wave, friction and mechanical impact, and is an excellent heat-resistant explosive. The extremely strong stability of TATB makes it favored in the military field where insensitive explosives are required. At present, the TATB used for charging medicine is generally directly synthesized, and its particle size is about 5 μm to 20 μm, and most of them are irregular shapes such as flakes. Due to the small particle size, it is mainly used for press-packing PBX. It has disadvantages such as poor fluidity, high viscosity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/84C07C211/52
CPCC07B2200/13C07C209/84C07C211/52
Inventor 李洪珍郝世龙徐容陈东周小清杨宗伟张祺
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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