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Method for synthesizing tri-amino trinitrobenzene (TATB) by trinitrotoluene (TNT)

A high-yield, concentrated nitric acid technology, applied in the preparation of amino groups replacing hydrogen atoms, organic chemistry, etc., can solve the problems of demanding reaction equipment, achieve the effects of optimizing kinetic conditions, reducing costs, and avoiding pollution

Inactive Publication Date: 2011-03-02
BEIJING INSTITUTE OF TECHNOLOGYGY
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Problems solved by technology

The nitric acid oxidation method is used in the oxidation process research related to this synthetic route, but the defect of this process is that if a higher yield (69%) is to be obtained, it must be strengthened by high temperature of 224 ° C and high pressure of about 4.5Mpa. Equipment requirements are also very demanding

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  • Method for synthesizing tri-amino trinitrobenzene (TATB) by trinitrotoluene (TNT)
  • Method for synthesizing tri-amino trinitrobenzene (TATB) by trinitrotoluene (TNT)
  • Method for synthesizing tri-amino trinitrobenzene (TATB) by trinitrotoluene (TNT)

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Effect test

Embodiment 1

[0031] 1) Dissolve 1g of TNT in 1.5mL of concentrated nitric acid, heat to 110°C, then add 1g of saturated aqueous solution of sodium chlorate, react for 3h, cool to room temperature, add ice water, filter to obtain 1.02g of trinitrobenzoic acid TNBA; Yield is 90%;

[0032] 2) Add 5mL of water to the TNBA obtained in step 1), add 1mL of 20% sodium hydroxide aqueous solution under stirring, filter, heat the filtrate to 100°C for decarboxylation reaction, the heating time is 3h, stop heating after the reaction is completed, and generate trinitrate Phenylbenzene TNB solid was suspended in the solution, cooled, filtered, and dried to obtain 0.72g TNB solid with a yield of 85%;

[0033] 3) Under nitrogen protection, mix 3mmol ATA, 6mmol sodium methoxide and 3mL DMSO to form a suspension, stir for 20min; then add 2mL of DMSO dissolved with 0.21gTNB into the suspension, heat up to 50°C, react for 6h, and the reaction is complete After cooling, pour it into 2001 mL of distilled water...

Embodiment 2

[0035] Same as Example 1, except that DMSO is DMF in step 3), and finally 0.248gTATB is obtained with a yield of 98%.

Embodiment 3

[0037] Same as Example 1, but the difference is that DMSO is THF in step 3), and finally 0.24g TATB is obtained with a yield of 95%.

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Abstract

The invention relates to a method for synthesizing tri-amino trinitrobenzene (TATB) by trinitrotoluene (TNT), belonging to the field of organic synthesis technology. The method comprises the following steps of: dissolving the TNT into the concentrated nitric acid, heating up, adding the saturated water solution of the sodium chlorate, reacting, cooling and filtering to obtain the TNBA; adding the TNBA into the water, stirring, adding the sodium hydroxide water solution, filtering, heating up the filter liquor to perform the decarboxylation reaction, cooling, filtering and drying to obtain the TNB; dissolving the TNB into reagent, adding the TNB into turbid liquid mixed by the ammoniation reagent, the sodium methylate and the reagent, and stirring; and heating up, cooling after the reaction, pouring into the distilled water, adjusting the PH value to be neutral or weakly acidic by the acetic acid, stewing, filtering in a pumping way, washing with water, and drying to obtain the TATB. The method takes the TNT as the raw material and uses the chrome-free technology in the oxidizing reaction to avoid the environment pollution, uses a small quantity of the reagent during the aminating reaction to increase the concentration of the reactant and optimize the dynamic conditions, and uses a small quantity of the ammoniation reagent and the sodium methylate to reduce the cost.

Description

technical field [0001] The invention relates to a method for synthesizing TATB from TNT, which belongs to the technical field of organic synthesis. Background technique [0002] The synthesis of triaminotrinitrobenzene (TATB) can be traced back to 1888, and it is prepared by reacting tribromotrinitrobenzene (TBTNB) with an ethanol solution of ammonia. In 1937, Backer and Vander Bann stably synthesized TATB using trichlorotrinitrobenzene (TCTNB) and ammonia as raw materials, with a yield of 80%. In 1956, Taylor of Naval Ordance Laboratory reported the excellent properties of TATB. Compared with other existing explosives, TATB has a higher density, is less sensitive to shock, and has a higher detonation velocity than TNT. Kaplan, Adelphi, and Taylor patented the method for the synthesis of TATB in 1959, and the project was funded by the US Navy. At the same time, Blais and Worman of the U.S. Army Department improved the synthesis method of TCTNB. By 1964, recognizing that ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/02
Inventor 周智明王凯孙稳稳梁丽轩吴玉凯
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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