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Method for recrystallizing TATB

A recrystallization and crystal form technology, applied in organic chemistry, amino compound purification/separation, etc., can solve the problems of high sulfuric acid impurity content, danger, difficult control of crystal shape and particle size, etc., and achieve simple reaction operation and mild reaction conditions , the effect of controllable particle size distribution

Inactive Publication Date: 2016-10-05
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main problems of this route include: (1) Concentrated sulfuric acid itself is extremely corrosive
This puts forward higher requirements on the anti-corrosion of the generating equipment, increases the cost of industrial production, and causes great pollution to the environment
(2) High content of sulfuric acid impurities in the product
(3) The adjustable range of TATB particle size is small
Although the particle size distribution of the particles can be controlled by controlling the reaction conditions, due to the rapid precipitation of crystals in the concentrated sulfuric acid-water precipitation process and the short growth time of TATB crystals, the particle size of the obtained particles is generally less than 10 μm, which cannot fully meet the application of TATB
(4) The crystal morphology of TATB is uncontrollable
However, the operation of adding water to the solution under high temperature conditions (145°C) in this process has certain risks; and the crystal morphology and particle size precipitated by adding water are not easy to control, so this process is not conducive to the regulation of TATB to a certain extent. Crystal appearance and particle size

Method used

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  • Method for recrystallizing TATB
  • Method for recrystallizing TATB
  • Method for recrystallizing TATB

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 0.200 g TATB, 50ml DMSO and 0.496% TW-20 into a four-neck flask, heat it in an oil bath to 125°C under constant stirring, TATB is completely dissolved, and keep it warm for 10 minutes. Cool down to 75°C at 1°C / min, then cool naturally to room temperature, filter to obtain TATB, wash with water and ethanol for 2-3 times in turn, and then dry at 110°C to obtain TATB product. The purity of TATB was 99.82% by HPLC analysis, and the exothermic decomposition temperature was 378.93°C by DSC analysis. The particle size of TATB measured by micron particle size tester was 10.64 μm. Scanning electron microscope SEM shows that the crystal shape of TATB is relatively regular and the surface is relatively smooth, such as figure 1 shown.

Embodiment 2

[0023] Add 0.200 g TATB, 50ml DMSO and 0.514% SPAN-85 into a four-neck flask, heat it in an oil bath to 125°C under constant stirring, TATB is completely dissolved, and keep it warm for 20 minutes. Cool down to 75°C at 1°C / min, then cool naturally to room temperature, filter to obtain TATB, wash with ethanol 2-3 times, and dry at 110°C to obtain TATB product. The purity of TATB was 99.79% by HPLC analysis, and the exothermic decomposition temperature was 379.62°C by DSC analysis. The particle size of TATB measured by micron particle size tester was 11.38 μm. Scanning electron microscope (SEM) showed that the crystal shape of TATB was relatively regular, the surface was relatively smooth, and a small amount of small grains adhered.

Embodiment 3

[0025] Add 0.150 g TATB, 50 ml DMSO and 0.478% benzyltriethylammonium chloride into a four-neck flask, heat to 115°C in an oil bath with constant stirring, TATB is completely dissolved, and keep the reaction for 10 min. Stir continuously at a speed of 1 min, cool down to room temperature at 1°C / min, filter to obtain TATB, wash with water and ethanol for 2-3 times in turn, and dry at 100°C to obtain TATB product. The purity of TATB was 99.84% by HPLC analysis, and the exothermic decomposition temperature was 381.96°C by DSC analysis. Scanning electron microscope SEM shows that the crystal form of TATB is relatively regular flake, and the surface is relatively smooth, such as figure 2 shown.

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Abstract

The invention discloses a method for recrystallizing TATB, which comprises the following steps: (1) adding raw material TATB, reaction medium DMSO and crystal modifier into a container; (2) constantly stirring and raising the temperature to completely dissolve TATB to obtain a yellow transparent Solution, heat preservation; (3) After the heat preservation is over, adjust the stirring speed, and cool the above yellow transparent solution. When the temperature of the solution drops to 115-125°C, add TATB seed crystals, grow the crystals, and then cool to room temperature; (4) After the reaction, the product and the mother liquor were separated by vacuum filtration, and the precipitate was washed and dried to make a finished product, and yellow TATB crystals were obtained. Compared with the prior art, the present invention has the following remarkable points: (1) The crystal form and particle size distribution of the product TATB are controllable, which meets different application requirements; (2) The purity of the recrystallized TATB product can reach more than 99.50%; (3) ) The reaction conditions are mild, the reaction operation is simple, and the crystallization solvent can be used many times without affecting the product quality.

Description

technical field [0001] The invention relates to a method for recrystallization of explosives, in particular to a method for introducing a crystal form modifier and seed crystal technology into a cooling method for recrystallization of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) . The present invention relates to a method suitable for recrystallizing TATB. Background technique [0002] TATB is currently the only single substance insensitive explosive approved by the U.S. Department of Energy. It is very insensitive to external stimuli such as light, heat, shock wave, friction and mechanical impact, and is an excellent heat-resistant explosive. TATB has been more and more widely used in mixed explosives, propellants, solid propellants and boosters. Different applications have different requirements for the spheroidization and particle size distribution of TATB. Therefore, the research on the recrystallization technology of TATB It has important practical and theoretical sign...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/86
Inventor 李斌栋陈磊常婷葛立波
Owner NANJING UNIV OF SCI & TECH
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