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Novel synthesis process of 2, 4, 6-trinitrobenzoic acid

A technology of trinitrobenzoic acid and trinitrotoluene, which is applied in the field of new synthesis technology of 2,4,6-trinitrobenzoic acid, can solve the problems of serious environmental pollution, low process safety and high production cost, To achieve the effect of good safety, simple process, and little environmental pollution

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

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Problems solved by technology

[0008] The purpose of the present invention is to solve the problems of high toxicity, serious environmental pollution, low process safety, large equipment corrosion and high production cost in the existing process for synthesizing 2,4,6-trinitrobenzoic acid, and provide a 2 , A new process for the synthesis of 4,6-trinitrobenzoic acid

Method used

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  • Novel synthesis process of 2, 4, 6-trinitrobenzoic acid
  • Novel synthesis process of 2, 4, 6-trinitrobenzoic acid

Examples

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Comparison scheme
Effect test

Embodiment 1

[0032] A kind of synthetic new technology of 2,4,6-trinitrobenzoic acid, comprises the steps:

[0033] (1) Weigh 2g of 2,4,6-trinitrotoluene and 20mL of ethanol, add 2,4,6-trinitrotoluene to ethanol at 60°C to make 2,4,6 - Trinitrotoluene is completely dissolved to obtain an alcoholic solution of 2,4,6-trinitrotoluene;

[0034] (2) Measure 20mL of ethanol, weigh 1.409g of sodium hydroxide and 0.1401g of copper oxide, add ethanol, sodium hydroxide and copper oxide into the reactor in turn, raise the temperature to 55°C, and wait until the sodium hydroxide is completely dissolved, Oxygen is introduced, and the oxygen flow rate is 0.2L / min;

[0035] (3) Add the alcohol solution of 2,4,6-trinitrotoluene obtained in step (1) dropwise into the reactor within 3 hours, and mature for 4 hours;

[0036] (4) After the dropwise addition, filter the reaction solution, wash the filter cake three times with 12mL ethanol, and dry at 40°C to constant weight after washing;

[0037] (5) Disso...

Embodiment 2

[0046] A kind of synthetic new technology of 2,4,6-trinitrobenzoic acid, comprises the steps:

[0047] (1) Weigh 2g of 2,4,6-trinitrotoluene and 15mL of ethanol, add 2,4,6-trinitrotoluene to ethanol at 60°C to make 2,4,6 - Trinitrotoluene is completely dissolved to obtain an alcoholic solution of 2,4,6-trinitrotoluene;

[0048] (2) Measure 15mL of ethanol, weigh 1.409g of sodium hydroxide and 0.1401g of copper oxide, add ethanol, sodium hydroxide and copper oxide into the reactor in sequence, raise the temperature to 70°C, and wait until the sodium hydroxide is completely dissolved, Introduce oxygen, the oxygen flow rate is 0.12L / min;

[0049] (3) Add the alcohol solution of 2,4,6-trinitrotoluene obtained in step (1) dropwise into the reactor within 2 hours, and mature for 5 hours;

[0050] (4) After the dropwise addition, filter the reaction solution, wash the filter cake three times with 10 mL of ethanol, and dry at 40°C to constant weight after washing;

[0051] (5) Diss...

Embodiment 3

[0056] A kind of synthetic new technology of 2,4,6-trinitrobenzoic acid, comprises the steps:

[0057] (1) Weigh 2g of 2,4,6-trinitrotoluene and 26mL of ethanol, add 2,4,6-trinitrotoluene to ethanol at 60°C to make 2,4,6 - Trinitrotoluene is completely dissolved to obtain an alcoholic solution of 2,4,6-trinitrotoluene;

[0058] (2) Measure 26mL of ethanol, weigh 1.409g of sodium hydroxide and 0.1401g of copper oxide, add ethanol, sodium hydroxide and copper oxide to the reactor in turn, raise the temperature to 50°C, and wait until the sodium hydroxide is completely dissolved, Oxygen is introduced, and the oxygen flow rate is 0.24L / min;

[0059] (3) Add the alcohol solution of 2,4,6-trinitrotoluene obtained in step (1) dropwise into the reactor within 4 hours, and mature for 3 hours;

[0060] (4) After the dropwise addition, filter the reaction solution, wash the filter cake three times with 13mL ethanol, and dry at 40°C to constant weight after washing;

[0061] (5) Dissol...

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Abstract

The invention relates to a novel synthesis process of 2, 4, 6-trinitrobenzoic acid, which comprises the following steps: firstly preparing an alcoholic solution of 2, 4, 6-trinitrotoluene, then mixing the alcoholic solution of 2, 4, 6-trinitrotoluene, sodium hydroxide, a catalyst and an oxidizing agent for reaction, filtering, washing and drying the obtained filter cake, dissolving the filter cake in water, adjusting the pH value, standing, filtering, extracting the filtrate with an organic solvent, and finally, evaporating the extract liquor, and naturally drying at normal temperature to obtain the 2, 4, 6-trinitrobenzoic acid. The method provided by the invention has the advantages of good safety, small environmental pollution, simple process, low cost and the like, avoids the use of toxic and harmful substances such as potassium / sodium dichromate, potassium perchlorate, potassium chlorate and the like, and solves the problems of high toxicity, serious environmental pollution, low process safety, high equipment corrosion, high production cost and the like in the existing process.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a new synthesis process of 2,4,6-trinitrobenzoic acid. Background technique [0002] 2,4,6-Trinitrobenzoic acid (TNBA) is an important organic chemical intermediate, widely used in the production of dyes, spices, explosives and other organic synthesis industries. The traditional synthesis process uses 2,4,6-trinitrotoluene (TNT) as raw material, 2 Cr 2 o 7 or K 2 Cr 2 o 7 One-step oxidation to 2,4,6-trinitrobenzoic acid, due to the use of Na in the oxidation process of 2,4,6-trinitrotoluene 2 Cr 2 o 7 or K 2 Cr 2 o 7 , the post-treatment of the carcinogenic wastewater produced is difficult, the pollution problem is serious, and the yield is low. The synthesis techniques of 2,4,6-trinitrobenzoic acid reported in existing literature mainly include: [0003] Literature (Wang Hongjun et al. Synthesis of trinitrobenzoic acid and its preliminary explo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C205/57
CPCC07C201/12C07C205/57
Inventor 陈丽珍张茹新赵鑫华赵嘉翔何佳远王建龙
Owner ZHONGBEI UNIV
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