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
CN105985249AInactive Publication Date: 2016-10-05NANJING UNIV OF SCI & TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
NANJING UNIV OF SCI & TECH
Publication Date
2016-10-05
Estimated Expiration
Not applicable · inactive patent

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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.
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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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