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Production method of 2,

A diaminobenzenesulfonic acid and production method technology, applied in the direction of sulfonic acid preparation, organic chemistry, etc., can solve the problems of secondary pollution of acid-containing wastewater, high sulfonation temperature, low reaction yield, etc., to reduce production costs, The effect of increasing product yield and improving product quality

Inactive Publication Date: 2012-06-27
JIANGSU YUANZHENG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a new production method of 2,4-diaminobenzenesulfonic acid to solve the problem of low reaction yield, high sulfonation temperature and the use of organic Problems such as secondary pollution caused by solvents and treatment of acid-containing wastewater

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Examples

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Effect test

Embodiment 1

[0024] Embodiment 1, a kind of production method of 2,4-diaminobenzenesulfonic acid, its steps are as follows:

[0025] (1) Add 98% sulfuric acid and 104.5% sulfuric acid to the reaction kettle, turn on the jacket cooling water, slowly and evenly add molten m-phenylenediamine, and add m-phenylenediamine after 1.5 hours; 98% sulfuric acid, 104.5% sulfuric acid and The weight ratio of m-phenylenediamine is 1.80:0.93:0.5;

[0026] (2) Slowly add 104.5% sulfuric acid and m-phenylenediamine; after the addition, heat up to 60°C and keep stirring for 20 minutes; the weight ratio of 104.5% sulfuric acid and m-phenylenediamine is 1.70:0.5; step (2) add The m-phenylenediamine is 0.9 times of the m-phenylenediamine added in step (1);

[0027] (3) Slowly add 104.5% sulfuric acid. After the addition, slowly raise the temperature to 100°C within 1 hour, turn off the steam, let the temperature rise slowly to 130°C, stir and react for 3 hours, and take samples for analysis. Diamine HPLC con...

Embodiment 2

[0030] Embodiment 2, a kind of production method of 2,4-diaminobenzenesulfonic acid, its steps are as follows:

[0031] (1) Add 98% sulfuric acid and 104.5% sulfuric acid to the reaction kettle, turn on the jacket cooling water, slowly and evenly add molten m-phenylenediamine, and add m-phenylenediamine after 2.5 hours; 98% sulfuric acid, 104.5% sulfuric acid and The weight ratio of m-phenylenediamine is 1.85: 0.96: 0.5;

[0032] (2) Slowly add 104.5% sulfuric acid and m-phenylenediamine; after the addition, heat up to 90°C and keep stirring for 40 minutes; the weight ratio of 104.5% sulfuric acid and m-phenylenediamine is 1.80:0.5; step (2) add The m-phenylenediamine is 1.1 times of the m-phenylenediamine added in step (1);

[0033] (3) Slowly add 104.5% sulfuric acid. After the addition, slowly raise the temperature to 130°C within 2 hours, turn off the steam, let the temperature rise slowly to 140°C, stir and react for 5 hours, and take samples for analysis. Diamine HPLC ...

Embodiment 3

[0036] Example 3, in the step (1) of the production method described in Example 1, the acidity is controlled at 100.0%.

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Abstract

4-diaminobezene sulfonic acid and salt thereof The invention relates to a production method of a dye intermediate 2,4-diaminobezene sulfonic acid. The method is characterized by using m-phenylenediamine as a main raw material and comprising operations of sulfonation, hydrolysis and refining to prepare the 2,4-diaminobezene sulfonic acid. The invention also provides a preparation method of 2,4-diaminobezene sulfonic acid ammonium salt or sodium salt by using the 2,4-diaminobezene sulfonic acid prepared by the above method, so as to solve problems of low reaction efficiency, high sulfonation temperature, secondary pollution caused by usage of organic solvent and acid-containing processing in the production process. The method of the invention employs addition of fusing m-phenylenediamine to increase solubility of the m-phenylenediamine in the sulfuric acid and reduce generation of side reaction; m-phenylenediamine and sulfuric acid are added respectively to control the acidity of the reaction system at a required acidity, control generation of side reaction and increase product quality and product yield; grading control of acidity and temperature maintains stable proceeding of reaction; and addition of hydrolysis increases yield of the product, improves product quality and reduces production cost.

Description

technical field [0001] The invention relates to a production method of a dye intermediate, in particular to a production method of 2,4-diaminobenzenesulfonic acid and its salt. The present invention also relates to a method for preparing sodium salt or ammonium salt of 2,4-diaminobenzenesulfonic acid prepared by the aforementioned method. Background technique [0002] 2,4-diaminobenzenesulfonic acid, also known as m-phenylenediamine-4-sulfonic acid, has the following structural formula: [0003] [0004] It is mainly used as an important intermediate for the synthesis of dyes, and its derivative products have been widely used in our production and life. The conventional preparation method is to obtain 2,4-dinitrochlorobenzene as raw material, react with sodium bisulfite and then reduce it. The disadvantages of this method are low reaction yield, poor product quality and low production efficiency. Chinese published invention patent document 200610029051.2 discloses the p...

Claims

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Application Information

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IPC IPC(8): C07C309/46C07C303/20C07C303/06
Inventor 彭炫王海民叶丽丽程燕明杨洋
Owner JIANGSU YUANZHENG CHEM
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