Channel synthesis method of m-triamino trinitrobenzene

A technology of triaminotrinitrobenzene and trichlorotrinitrobenzene is applied in the field of channel synthesis of m-triaminotrinitrobenzene to achieve the effects of promoting the reaction process, being easy to be continuous, and preventing seriousness

Active Publication Date: 2019-05-31
INST OF CHEM MATERIAL CHINA ACADEMY OF ENG PHYSICS
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  • Abstract
  • Description
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  • 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-triamino trinitrobenzene
  • Channel synthesis method of m-triamino trinitrobenzene

Examples

Experimental program
Comparison scheme
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, without visible fine particles, as starting materials; weigh 25 % thick ammonia water (0.60mol, about 44.83ml) is in the flask, as ammoniation reagent; Start metering pump feeding, starting material and ammoniation reagent are pumped into tunnel reactor, and the feeding rate of two pumps is set respectively 2.4ml / min and 0.3ml / min, so that the molar ratio of m-trichlorotrinitrobenzene to ammonia water is approximately 1:6, and the pump pressure in operation is 0.01~0.95Mpa (the pump pressure threshold is set to 1.80Mpa); The residence time in the channel reactor is about 1min, and the oil bath temperature is 70°C; samples are taken at the outlet of the microchannel reactor, and it is confirmed by liquid chromatography that part of m-trichlorotrinitrobenzene is converted into the product m-triaminotrinitrobenzene Nitrobenzene, the...

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, without visible fine particles, as starting materials; weigh 25 % strong ammoniacal liquor (0.90mol, about 67.25ml) is in flask, as ammoniation reagent; Start metering pump feeding, starting material and ammoniation reagent are pumped into channel reactor, and the feed rate of two pumps is 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, the pump pressure during operation is 0.01~0.95Mpa (the pump pressure threshold is set to 1.80Mpa); the material in the channel The residence time in the channel reactor is about 3min, and the temperature of the oil bath is 90°C; the reaction material flows out from the channel reactor to the collector, and continues to keep warm for 0 to 5 hours; the sample is taken at the outlet of the channel reactor and analy...

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, without visible fine particles, as starting materials; weigh 25 % strong ammoniacal liquor (0.90mol, about 67.25ml) is in flask, as ammoniation reagent; Start metering pump feeding, starting material and ammoniation reagent are pumped into channel reactor, and the feed rate of two pumps is respectively set to 4.8ml / min and 0.8ml / min, so that the molar ratio of m-trichlorotrinitrobenzene and ammonia water is 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 pressure of the material 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 is used; samples are taken at the outlet of the channel reactor and confirmed by liqu...

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Abstract

The invention discloses a channel synthesis method of m-triamino trinitrobenzene. The channel synthesis method of m-triamino trinitrobenzene comprises following steps: 1, a toluene solution of m-trichloro trinitrobenzene is prepared as an initial material; 2, an ammonification reagent is prepared; 3, the initial material and the ammonification reagent are pumped into a channel type reactor throughtwo inlets of the channel type reactor using metering pumps synchronously; 4, the initial material and the ammonification reagent are mixed and reacted in the channel type reactor, wherein reaction time retention time is controlled to be 10 to 1000s; 5, an obtained reaction product is delivered into a collector through a reaction channel, thermal insulation reaction is carried out for 0 to 10h, and mother liquor filtering, filter cake washing and drying are carried out based on routine methods so as to obtain a target product. According to the channel synthesis method, utilization of the highefficiency heat and mass transfer capacity of the channel type reactor is adopted to realize synthesis technology accurate control, parameter fluctuation is reduced, conversion rate is close to 100%under optimized conditions, the particle size of the obtained m-triamino trinitrobenzene product ranges from 10 to 60<mu>m, and the peak value particle size ranges from 15 to 30<mu>m.

Description

technical field [0001] The invention relates to a method for synthesizing energetic materials, in particular to a channel synthesis method for m-triaminotrinitrobenzene (1,3,5-triamino-2,4,6-trinitrobenzene). Background technique [0002] m-triaminotrinitrobenzene (1,3,5-triamino-2,4,6-trinitrobenzene, abbreviated as TATB) is an important insensitive single-substance explosive, which can be used in missiles, rockets, etc. Compared with other powders, it has the advantages of low sensitivity and good safety. [0003] The synthesis method of m-triaminotrinitrobenzene is traditionally carried out in a reaction kettle, using custom-made s-trichlorotrinitrobenzene as raw material, reacting with ammoniating reagents such as ammonia gas, ammonia water or ammonium carbonate, etc., the reaction 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 continuously a...

Claims

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Application Information

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Patent Type & Authority Applications(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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