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Method for synthesizing TATB (triamino trinitrobenzene) by normal pressure phase-transfer catalysis and amination

A technology of phase transfer and catalysis of amines, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, preparation of amino compounds, etc., can solve the problems of unfavorable large-scale industrial production, low solubility, and difficulty in purchasing, etc., and achieve large-scale industrialization Simple production and reaction operation, and the effect of solving the problem of chlorine content

Active Publication Date: 2013-11-27
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) High chlorine impurity content in the product
(2) The raw material TCB is expensive, the supply is unstable, and it is not easy to purchase, resulting in high cost of finished products, which limits the promotion and application of products
(3) Environmental pollution issues
However, the solubility of ethanol to the reaction raw materials is low, the loss of raw materials is huge, and the requirements for reaction equipment are also high, so this process is not conducive to large-scale industrial production to a certain extent.

Method used

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  • Method for synthesizing TATB (triamino trinitrobenzene) by normal pressure phase-transfer catalysis and amination
  • Method for synthesizing TATB (triamino trinitrobenzene) by normal pressure phase-transfer catalysis and amination
  • Method for synthesizing TATB (triamino trinitrobenzene) by normal pressure phase-transfer catalysis and amination

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 2.070g of 1,3,5-triethoxy-2,4,6-triaminobenzene and 15ml of xylene into a four-neck flask, heat to 50°C in a water bath while stirring, and add 15ml of ammonia water (the weight percentage is 25-28%) reflux reaction for 2 hours, after the reaction, the reaction liquid was cooled to room temperature, TATB was obtained by filtration, washed with ethanol for 2-3 times, and then dried to obtain 0.093g of TATB product with a yield of 6%. According to HPLC analysis, the purity of TATB was 98.32%, and the exothermic decomposition temperature was 386.12% according to DSC analysis.

[0028] Spectral data: MS(m / z):258.1(M + ); 1 H-NMR (DMSO-d6), δ: 3.35 (m, 6H, -NH 2 ); FT-IR(KBr), ν(cm -1 ): 3320, 3216, 1604, 1571, 1444, 1217, 1166, 781, 727, 694. Example 2

Embodiment 2

[0029] Add 2.070g of 1,3,5-triethoxy-2,4,6-triaminobenzene, 15ml of xylene and 0.040g of hexadecyltrimethylammonium bromide into a four-neck flask, stir and heat in a water bath 50°C, add 15ml of ammonia water (25-28% by weight) and reflux for 2 hours. After the reaction, cool the reaction solution to room temperature, filter to obtain TATB, wash with ethanol for 2-3 times and dry to obtain TATB product 0.805. According to HPLC analysis, the purity of TATB was 98%, and the yield was 52.00%. The exothermic decomposition temperature of DSC analysis was 378.84%.

Embodiment 3

[0031] Add 2.070g of 1,3,5-triethoxy-2,4,6-triaminobenzene, 15ml of xylene and 0.40g of β-cyclodextrin into a four-neck flask, heat in a water bath to 50°C under stirring, and add 15ml of ammonia water (25-28% by weight) reflux reaction for 2 hours. After the reaction, the reaction solution was cooled to room temperature, filtered to obtain TATB, washed with acetone for 2-3 times and dried to obtain 0.09 g of TATB product with a yield of 5.8%. According to HPLC analysis, the purity of TATB was 98.15%, and the exothermic decomposition temperature was 378.84% according to DSC analysis.

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Abstract

The invention discloses a method for synthesizing TATB (triamino trinitrobenzene) by normal pressure phase-transfer catalysis and amination. The method comprises the following steps: 1, adding 1,3,5-triethoxy-2,4,6-triaminobenzene, an organic solvent and a phase-transfer catalyst into a reactor, raising temperature and stirring, and dropwise adding ammonium hydroxide to carry out a reflux reaction; 2, after the reaction is ended, and separating a product and mother liquor, wherein the product is washed and dried to obtain TATB; and 3, analyzing and calibrating the mother liquor so as to be recycled and reused. Compared with the prior art, the method disclosed by the invention has the remarkable advantages that (1) the product TATB does not contain chlorine element, so that the chlorine-containing problem in a traditional synthesis method is solved; (2) the purity of the prepared TATB product which is not subjected to purification treatment can reach more than 98.0 percent; (3) reaction conditions are mild, the reaction operation is simple, and as the TATB is synthesized in a normal temperature phase-transfer catalysis and amination system, an airtight high pressure reaction kettle is not required, and industrial large-scale production is facilitated.

Description

technical field [0001] The invention relates to a method for preparing explosives, in particular to a method for synthesizing chlorine-free TATB by amination of a phase transfer catalyst under normal pressure conditions. The invention relates to an amination method suitable for industrialized large-scale production of chlorine-free TATB. Background technique [0002] TATB is an energetic material with high energy, good insensitivity, and good heat resistance. It has a wide range of applications in the fields of weapons, propellants, and civil blasting. Therefore, the study of TATB has important practical and theoretical significance. [0003] The method of producing TATB at home and abroad is mainly to nitrate trichlorobenzene (TCB) with nitric acid mixed acid to obtain the intermediate 1,3,5-trichloro-2,4,6-trinitrobenzene (TCTNB), and then in toluene It is made by amination of ammonia gas or liquid ammonia. The main problems of this route include: (1) The chlorine impuri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/18
Inventor 李斌栋常婷陈磊葛立波汪欢
Owner NANJING UNIV OF SCI & TECH
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