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

A phase-transfer catalyst and phase-transfer technology, applied in 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, difficult to purchase, etc., and achieve a large-scale industrialization Large-scale production, simple reaction operation, and the effect of solving the problem of chlorine content

Active Publication Date: 2014-12-24
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 problems
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 1,3,5-triethoxy-2,4,6-trinitrobenzene and 15ml xylene into a four-necked flask, heat to 50℃ in a water bath with stirring, and add 15ml ammonia water (weight percentage 25-28%) reflux the reaction for 2h. After the reaction, the reaction solution is cooled to room temperature, filtered to obtain TATB, washed with ethanol for 2-3 times and dried to obtain 0.093g of TATB product, with a yield of 6%. The purity of TATB was 98.32% by high performance liquid chromatography, and the exothermic decomposition temperature by DSC was 386.12%.

[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.

Embodiment 2

[0030] Add 2.070g 1,3,5-triethoxy-2,4,6-trinitrobenzene, 15ml xylene and 0.040g cetyltrimethylammonium bromide into a four-neck flask, and heat in a water bath while stirring At 50°C, 15ml ammonia water (25-28% by weight) was added and refluxed for 2h. After the reaction, the reaction solution was cooled to room temperature, filtered to obtain TATB, washed with ethanol for 2-3 times and dried to obtain TATB product 0.805. The purity of TATB was 98% by high performance liquid chromatography, the yield was 52.00%, and the exothermic decomposition temperature by DSC was 378.84%.

Embodiment 3

[0032] Add 2.070g 1,3,5-triethoxy-2,4,6-trinitrobenzene, 15ml xylene and 0.40g β-cyclodextrin into a four-necked flask, stir and heat in a water bath at 50℃, add 15ml ammonia (The weight percentage is 25-28%) The reaction was refluxed for 2h. 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 0.09g of TATB product, with a yield of 5.8%. The purity of TATB was 98.15% by high performance liquid chromatography, and the exothermic decomposition temperature by DSC was 378.84%.

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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 preparation method of explosives, in particular to a method for synthesizing chlorine-free TATB under normal pressure by using phase transfer catalyst amination. The invention relates to an amination method suitable for industrial 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 weapons, propellants, and civil blasting. Therefore, it has important practical and theoretical significance for the study of TATB. [0003] The main method of producing TATB at home and abroad is to nitrate trichlorobenzene (TCB) with mixed acid of nitrosulphur to obtain intermediate 1,3,5-trichloro-2,4,6-trinitrobenzene (TCTNB), and then in toluene It is made by ammonia or liquid ammonia amination. The main problems of this route include: (1) The product contains high chlorine impurities. The chl...

Claims

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Application Information

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Patent Type & Authority Patents(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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