Channel synthesis method of m-triaminotrinitrobenzene

A technology of triaminotrinitrobenzene and trichlorotrinitrobenzene, which is applied in the channel synthesis field of m-triaminotrinitrobenzene, to achieve a wide reaction temperature, eliminate severity, and promote the effect of the reaction process

Active Publication Date: 2022-07-26
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This project is based on channel synthesis reaction technology, using m-trichlorotrinitrobenzene to synthesize m-triaminotrinitrobenzene, which has not been reported

Method used

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  • Channel synthesis method of m-triaminotrinitrobenzene
  • Channel synthesis method of m-triaminotrinitrobenzene

Examples

Experimental program
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Effect test

Embodiment 1

[0045]Weigh m-trichlorotrinitrobenzene (31.65g, 0.10mol) and toluene (316.5g, about 365.5ml) in a flask, stir and dissolve until the color is bright and there are no fine particles visible to the naked eye, as starting materials; weigh 25 % concentrated ammonia water (0.60mol, about 44.83ml) in the flask as the ammoniating reagent; start the metering pump to feed, and pump the starting material and the ammoniated reagent into the channel reactor, and the feeding rates of the two pumps are respectively set. are 2.4ml / min and 0.3ml / min, so that the molar ratio of m-trichlorotrinitrobenzene and ammonia water is approximately 1:6, and the pump pressure during operation is 0.01 to 0.95Mpa (the pump pressure threshold is set to 1.80Mpa); The residence time in the channel reactor was about 1 min, and the oil bath temperature was 70 °C; sampling was taken at the outlet of the microchannel reactor, and it was confirmed by liquid chromatography that part of the m-trichlorotrinitrobenzene...

Embodiment 2

[0047] Weigh m-trichlorotrinitrobenzene (31.65g, 0.10mol) and toluene (316.5g, about 365.5ml) in a flask, stir and dissolve until the color is bright and there are no fine particles visible to the naked eye, as starting materials; weigh 25 % concentrated ammonia water (0.90mol, about 67.25ml) in the flask, as the ammoniation reagent; start the metering pump feeding, pump the starting material and the ammoniated reagent into the channel reactor, and the feeding rates of the two pumps are respectively set to 1.6ml / min and 0.3ml / min, so that the molar ratio of m-trichlorotrinitrobenzene and ammonia water is close to 1:9, and the pump pressure during operation is 0.01-0.95Mpa (the pump pressure threshold is set to 1.80Mpa); the material is in the channel The residence time in the reactor was about 3min, and the temperature of the oil bath was 90°C; the reaction material flowed out from the channel reactor to the collector, and the reaction was continued for 0 to 5 hours; Analysis ...

Embodiment 3

[0049] Weigh m-trichlorotrinitrobenzene (31.65g, 0.10mol) and toluene (316.5g, about 365.5ml) in a flask, stir and dissolve until the color is bright and there are no fine particles visible to the naked eye, as starting materials; weigh 25 % concentrated ammonia water (0.90mol, about 67.25ml) in the flask, as the ammoniation reagent; start the metering pump feeding, pump the starting material and the ammoniated reagent into the channel reactor, and the feeding rates of the two pumps are respectively set to 4.8ml / min and 0.8ml / min, make the molar ratio of m-trichlorotrinitrobenzene and ammonia water close to 1:8, the pump pressure during operation is 1.3~1.5Mpa (the pump pressure threshold is set to 1.80Mpa, adjust the back pressure valve to maintain the material pressure in the reverse channel); the residence time of the material in the channel reactor is about 10min, the oil bath temperature is 110 °C, and ultrasonic assistance; sampling at the outlet of the channel reactor, c...

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Abstract

The invention discloses a channel synthesis method of m-triaminotrinitrobenzene, comprising the following steps: 1) preparing a toluene solution of m-trichlorotrinitrobenzene as a starting material; 2) preparing an ammoniation reagent; 3) starting The starting material and the ammoniated reagent are respectively pumped into the two inlets of the channel reactor by the metering pump synchronously; 4) The starting material and the ammoniated reagent are mixed and reacted in the channel reactor, and the reaction time is 10~1000 5) The reaction product is output from the reaction channel to the collector, and the reaction is continued for 0 to 10 hours; the mother liquor is filtered, the filter cake is washed and dried based on conventional methods to obtain the target product. The method makes full use of the high-efficiency heat and mass transfer capability of the channel reactor to achieve precise control of the synthesis process, reduces parameter fluctuations, the conversion rate is close to 100% under optimized conditions, and the particle size distribution of the obtained m-triaminotrinitrobenzene product is between 10 μm and 60 μm. In between, the peak particle size is 15 μm to 30 μm.

Description

technical field [0001] The invention relates to a method for synthesizing energetic materials, in particular to a method for channel synthesis of m-triaminotrinitrobenzene (1,3,5-triamino-2,4,6-trinitrobenzene). Background technique [0002] Meta-triaminotrinitrobenzene (1,3,5-triamino-2,4,6-trinitrobenzene, TATB for short) is an important insensitive elemental explosive, which can be used in the equipment of missiles, rockets, etc. Compared with other charges, it has the advantages of low sensitivity and good safety. [0003] The method for synthesizing m-triaminotrinitrobenzene is traditionally carried out in a reactor, using customized mes-trichlorotrinitrobenzene as a raw material, and reacting with an ammoniating reagent such as ammonia gas, ammonia water or ammonium carbonate, etc. After completion, the mother liquor is filtered, washed and dried to obtain the target product. Affected by the batch process of the reactor, the process parameters need to be constantly a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/52C07C209/10
Inventor 郁卫飞杨光成冯梅李森魏智勇张勇徐瑞娟
Owner INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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