Preparation process of 4-beta-sulfatoethylsulfonyl aniline-2-sulfonic acid

A technology based on sulfuric acid and ester aniline, applied in the field of preparation of dye intermediates, can solve the problems of large amount of waste acid, non-compliance, environmental pollution, etc., and achieve excellent results in energy saving and emission reduction

Inactive Publication Date: 2012-01-11
TIANJIN DEK CHEM
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Problems solved by technology

[0002] Now the general method for preparing 4-β-ethylsulfone sulfate aniline-2-sulfonic acid is to generate p-β-hydroxyethyl sulfone through chlorosulfonation, reduction reaction, and condensation reaction with ethylene oxide from acetanilide Acetanilide, then esterified and hydrolyzed to obtain p-β-hydroxyethyl sulfone sulfate aniline (para-ester), and finally sulfonated to obtain 4-β-ethylsulfone sulfate aniline-2 -sulfonic acid (abbreviated as sulfonated para-ester, hereinafter referred to as sulfonated para-ester), the three unit reactions of this preparation method: esterification, sulfonation, and hydrolysis are carried out separately, and the amount of waste acid produced is very large. Meets the current requirements of energy saving and emission reduction, causing serious pollution to the environment
Due to the constraints of environmental ecology and waste liquid treatment costs, the requirements for the amount of waste acid are getting higher and higher, and this preparation method can no longer meet the requirements of environmental protection.

Method used

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  • Preparation process of 4-beta-sulfatoethylsulfonyl aniline-2-sulfonic acid

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Embodiment 1

[0029] A preparation method of sulfonated para-ester, comprising the steps of:

[0030] a, chlorosulfonation reaction of acetanilide: in reaction tank, add 1180kg of chlorosulfonic acid, then add 275kg of acetanilide, temperature is controlled below 15 ℃, stir well, be warming up to 60 ℃, react 3 hours, obtain feed liquid (1 ). In the dilution tank, add 3000kg of crushed ice and 1000L of water, add the feed liquid (1) under stirring, and dilute the temperature at 0-10°C to obtain the feed liquid (2), filter the feed liquid (2) with a solid-liquid separator to obtain Chlorosulfonate filter cake;

[0031] b. Reduction reaction

[0032] Add the chlorosulfonate filter cake obtained in step a to the sodium bisulfite solution containing 220kg, stir evenly, control the temperature at 25-30°C, use 40% sodium hydroxide solution to maintain pH = 7-7.5, and react for 2 hours , after the reaction is completed, the reduction reaction solution is obtained;

[0033] c. Condensation react...

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Abstract

The invention relates to a preparation process of 4-beta-sulfatoethylsulfonyl aniline-2-sulfonic acid. The preparation process comprises the following steps: sulfochlorination, reduction, condensation, sulfonation, esterification and hydrolysis of acetanilide, dilution, salting-out, commercialization, and finished product packaging. In comparison of previous preparation processes, the preparation process of the present invention which has the advantages of changing three individual unit reactions of sulfonation, esterification, and hydrolysis into one unit reaction, and removing the waste acid amount of two unit reactions is excellent in energy saving and emission reduction.

Description

technical field [0001] The invention relates to a preparation method of a dye intermediate, in particular to a preparation method of 4-beta-ethylsulfone sulfate aniline-2-sulfonic acid. Background technique [0002] Now the general method for preparing 4-β-ethylsulfone sulfate aniline-2-sulfonic acid is to generate p-β-hydroxyethyl sulfone through chlorosulfonation, reduction reaction, and condensation reaction with ethylene oxide from acetanilide Acetanilide, then esterified and hydrolyzed to obtain p-β-hydroxyethyl sulfone sulfate aniline (para-ester), and finally sulfonated to obtain 4-β-ethylsulfone sulfate aniline-2 -sulfonic acid (abbreviated as sulfonated para-ester, hereinafter referred to as sulfonated para-ester), the three unit reactions of this preparation method: esterification, sulfonation, and hydrolysis are carried out separately, and the amount of waste acid produced is very large. It meets the current requirements of energy saving and emission reduction, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/36C07C315/04
Inventor 张兴华邢广文
Owner TIANJIN DEK CHEM
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