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Method for preparing large particle triaminotrinitrobenzene by reaction crystallization method

A technology of triaminotrinitrobenzene and reaction crystallization, which is applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc. It can solve the problems of poor safety of large-particle TATB, difficulty in obtaining TATB particles, and difficulty in expanding the scale. , to achieve the effect of improving anisotropic expansion, mild reaction conditions and good safety

Active Publication Date: 2019-03-22
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Abstract
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  • Claims
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Problems solved by technology

[0004] The present invention overcomes the deficiencies of the prior art, and provides a method for preparing large-particle triaminotrinitrobenzene by a reaction crystallization method, hoping to solve the problem of poor safety, difficulty in expanding the scale, and difficulty in obtaining large-particle TATB in the prior art. Problems with larger sized TATB particles above

Method used

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  • Method for preparing large particle triaminotrinitrobenzene by reaction crystallization method
  • Method for preparing large particle triaminotrinitrobenzene by reaction crystallization method

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Embodiment 1

[0026] At room temperature, 5 g of raw material TATB was added to 1100 ml of dimethyl sulfoxide (mass ratio: 1:242), and then heated to 100° C. to dissolve to obtain a saturated solution. Add 60ml of non-solvent water (the mass ratio of non-solvent to raw material TATB is 12:1) at a rate of 15ml / min under stirring, and drop the temperature to 40°C at a rate of 0.5°C / min according to the temperature control program to obtain TATB suspension liquid, filtered, washed with acetone, and dried to obtain TATB crystal particles as seeds.

[0027] At room temperature, 17 g of the precursor compound TETNB for the synthesis of TATB was dissolved in 170 ml of reaction solvent xylene (the mass ratio of reaction solvent to TETNB was 8.6:1), and the temperature was raised to 55 ° C to promote its dissolution, and then 1.7 g of TATB crystals were added. Seed (10% of TETNB quality), add 80ml ammoniacal liquor (72.8g) with the speed of 20ml / min under stirring state, and react 2h at this tempera...

Embodiment 2

[0029] At room temperature, 3 g of raw material TATB was added to 700 ml of N,N-dimethylformamide (mass ratio: 1:220.5), and then heated to 140° C. to dissolve to obtain a saturated solution. Add 86ml of non-solvent toluene (mass ratio of non-solvent to raw material TATB: 24.8:1) at a rate of 10ml / min under stirring, and drop the temperature to 35°C at a rate of 0.6°C / min according to the temperature control program to obtain TATB suspension solution, filtered, washed, and dried to obtain TATB crystal particles as seed crystals.

[0030] At room temperature, 17 g of the precursor compound TETNB used for the synthesis of TATB was dissolved in 85 ml of the reaction solvent dimethyl sulfoxide (the mass ratio of the reaction solvent to TETNB was 5.5:1), and the temperature was raised to 60 ° C to promote its dissolution, and then 0.85 gTATB seed crystal (5% of TETNB quality), add ammoniacal liquor (75ml) with the speed of 15ml / min under stirring state, and react at this temperatur...

Embodiment 3

[0032]At room temperature, 3 g of raw material TATB was added to 480 ml of sulfolane (mass ratio: 1:202), and then heated to 130° C. to dissolve to obtain a saturated solution. Add 40ml of non-solvent toluene (the mass ratio of non-solvent to raw material TATB is 11.5:1) at a rate of 5ml / min under stirring, and drop the temperature to 20°C at a rate of 3°C / min according to the temperature control program. The formation of crystal grains grows to obtain TATB suspension, which is filtered, washed and dried to obtain TATB crystal particles as seed crystals.

[0033] At room temperature, 17 g of the precursor compound TMTNB used for the synthesis of TATB was dissolved in the reaction solvent dimethyl sulfoxide (230 ml), and the temperature was raised to 70 ° C to promote its dissolution, and then 1.0 g of TATB seed crystals were added, and 5 g of TATB was added under stirring. Add 40 g of ammonium carbonate at a speed of 1 / min, and react at this temperature for 3 h, then naturally...

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Abstract

The invention discloses a method for preparing large-grained triamino trinitrobenzene (TATB) by a reactive crystallization method. The method comprises the steps: adding common TATB into a recrystallization solvent, increasing temperature and dissolving to obtain a saturated solution, adding an anti-solvent, cooling to room temperature according to a temperature control program and crystallizing to obtain TATB crystal grains to serve as seed crystals; and dissolving a precursor compound for synthesizing the TATB into a reaction solvent at room temperature, increasing temperature, promoting dissolution of the compound, adding the TATB seed crystals, adding an aminating reagent under the stirring condition, reacting at a certain temperature to crystallize, cooling to room temperature and performing aftertratment to obtain the large-grained TATB. The method is simple in process, convenient in operation, high in safety and easy in engineering enlargement. The large-grained TATB prepared by the method can be used for pouring and press-fitting charge, the charge solid content is obviously improved, the charge free-flowing property is improved, and the anisotropic expansion and the dimensional stability of TATB based explosive can be improved.

Description

technical field [0001] The invention relates to the field of energetic materials, more specifically, the invention relates to a method for preparing large-particle triaminotrinitrobenzene by a reaction crystallization method, and the invention has very good application prospects in explosives. Background technique [0002] Triaminotrinitrobenzene (TATB) is very insensitive to external stimuli such as heat, light, shock wave, friction and mechanical impact, and is an excellent heat-resistant explosive. It first appeared in 1887, and it was not until the early 1960s that the research on TATB developed rapidly and quickly became one of the important materials in ammunition desensitization engineering. At present, TATB is generally directly synthesized, and its particle size is about 5-20 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 an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/56C07C209/10C07C209/84
CPCC07C209/10C07C209/84C07C211/56
Inventor 李洪珍郝世龙陈东张朝阳徐容黄靖伦周小清张丽媛
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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