Method for preparing 1, 3, 5-trinitrobenzene

A kind of trinitrobenzene, a certain amount of technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of unstable chloric acid, complex process, unfavorable environment and the like, and achieve high reaction yield, Reaction process safety, the effect of simplifying the process

Active Publication Date: 2021-07-23
ZHONGBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The problems of this method: (1) The preparation process is divided into two steps, the process is complicated and the cost is high; (2) Chloric acid is unstable under high temperature conditions, and it is easy to decompose into perchloric acid and ClO 2 , the latter continues to decompose to release chlorine gas, which is not good for the environment

Method used

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  • Method for preparing 1, 3, 5-trinitrobenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Measure 50mL of methanol, pour it into the first container equipped with a thermometer and a stirring device, weigh 5g of TNT, add TNT to methanol, raise the temperature to 50°C, dissolve the TNT, and obtain a TNT alcohol solution;

[0034] (2) Measure 30mL of water, pour it into a second container equipped with a thermometer, stirring and reflux device, weigh 15g of sodium chlorite and add it to the water, dissolve the sodium chlorite at room temperature to obtain chlorite Sodium acid aqueous solution;

[0035] (3) Use 2M hydrochloric acid to adjust the pH value of the TNT alcohol solution in step (1) to 5, and then raise the temperature of the TNT alcohol solution to 55°C;

[0036] (4) Add the sodium chlorite aqueous solution in step (2) dropwise to the TNT alcohol solution in step (3), and react at constant temperature for 8 hours;

[0037] (5) Filter, wash with hot water, and recrystallize with ethanol to obtain 2.87 g of trinitrobenzene, with a yield of 61.19%...

Embodiment 2

[0039] (1) Measure 50mL of methanol, pour it into the first container equipped with a thermometer and a stirring device, weigh 5g of TNT, add TNT to methanol, raise the temperature to 60°C, dissolve the TNT, and obtain a TNT alcohol solution;

[0040] (2) Measure 10mL of water, pour it into a second container equipped with a thermometer, stirring and reflux device, weigh 5g of sodium chlorite and add it to the water, dissolve the sodium chlorite at room temperature to obtain chlorite Sodium acid aqueous solution;

[0041] (3) Use 2M hydrochloric acid to adjust the pH value of the TNT alcohol solution in step (1) to 6, and then raise the temperature of the TNT alcohol solution to 60°C;

[0042] (4) Add the sodium chlorite aqueous solution in step (2) dropwise to the TNT alcohol solution in step (3), and react at constant temperature for 4 hours;

[0043] (5) Filter, wash with hot water, and recrystallize with ethanol to obtain 3.01 g of trinitrobenzene, with a yield of 64.17%....

Embodiment 3

[0045] (1) Measure 50mL of methanol, pour it into the first container equipped with a thermometer and a stirring device, weigh 5g of TNT, add TNT to methanol, raise the temperature to 55°C, dissolve the TNT, and obtain a TNT alcohol solution;

[0046] (2) Measure 10mL of water, pour it into a second container equipped with a thermometer, stirring and reflux device, weigh 5g of sodium chlorite into the water, and dissolve the sodium chlorite at room temperature to obtain sodium chlorite aqueous solution;

[0047] (3) Use 2M hydrochloric acid to adjust the pH value of the TNT alcohol solution in step (1) to 6, and then raise the temperature of the TNT alcohol solution to 50°C;

[0048] (4) Add the sodium chlorite aqueous solution in step (2) dropwise to the TNT alcohol solution in step (3), and react at constant temperature for 3 hours;

[0049] (5) Filter, wash with hot water, and recrystallize with ethanol to obtain 2.65 g of trinitrobenzene, with a yield of 56.50%.

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Abstract

The invention relates to a method for preparing 1, 3, 5-trinitrobenzene, and belongs to the technical field of organic intermediates. The method comprises the following steps: respectively preparing a TNT alcoholic solution and a sodium chlorite aqueous solution, adjusting the pH value of the TNT alcoholic solution with hydrochloric acid, heating to a reaction temperature, dropwise adding the sodium chlorite aqueous solution into the TNT alcoholic solution, reacting at a constant temperature, and finally filtering, washing and recrystallizing to obtain the 1, 3, 5-trinitrobenzene. Sodium chlorite is adopted as an oxidizing agent, so that oxidation and decarboxylation reactions are completed in one step, the process is simplified, and the operation cost is reduced; the energy consumption required by the reaction is low, and the product purity is high; the reaction process is safer, and the reaction yield is higher.

Description

technical field [0001] The invention relates to the technical field of organic intermediates, in particular to a method for preparing 1,3,5-trinitrobenzene. Background technique [0002] 1,3,5-Trinitrobenzene, English name: 1,3,5-Trinitrobenzene, molecular formula: C 6 h 3 N 3 o 6 , the structural formula: [0003] [0004] Molecular weight 213.1, melting point 123°C, white or yellow orthorhombic crystals, can be used as explosives, and can also be used as pesticide or pharmaceutical intermediates for the synthesis of 3,5-difluoroaniline, 3,5-diarylphenylene ring ether derivatives, etc. It is also an important precursor for the synthesis of heat-resistant explosives such as 1,3,5-triamino-2,4,6-trinitrobenzene (TATB), and can also be used as a pH indicator in analytical chemistry. [0005] The existing method for preparing 1,3,5-trinitrobenzene mainly uses trinitrotoluene (TNT) as a raw material oxidation and decarboxylation two-step method: that is, potassium chlora...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C205/06
CPCC07C201/12C07C205/06
Inventor 陈丽珍张茹新赵鑫华赵林秀王建龙
Owner ZHONGBEI UNIV
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