Method for preparing OBSC (4,4'-oxo-bis-benzenesulfonyl chloride) from basic chemical raw materials

A chemical raw material and a basic technology, applied in the field of preparing OBSC from basic chemical raw materials, can solve the problems of low product yield and purity, excessive sulfonating agent raw materials, complicated product post-processing, etc., so as to avoid raw material consumption and yield. And the effect of excellent purity and low production cost

Inactive Publication Date: 2014-10-01
SHANDONG TIANYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, most of the current production of OBSC uses chlorosulfonic acid or concentrated sulfuric acid to sulfonate diphenyl ether, which consumes a lot of sulfonating agent raw materials and cannot be recycled, resulting in a lot of waste. A large amount of water will produce a large amount of acidic wastewater, and it is easy to cause hydrolysis of the product, resulting in a large number of isomers and sulfoxide by-products, and the product yield and purity are not high

Method used

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  • Method for preparing OBSC (4,4'-oxo-bis-benzenesulfonyl chloride) from basic chemical raw materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Under the catalysis of ferric chloride, chlorine gas is homogeneously split into chlorine free radicals by light; the dosage of catalyst ferric chloride is 1% of the mass of chlorine gas.

[0024] (2) Sulfur dioxide gas is produced by burning sulfur in the air.

[0025] (3) Put the diphenyl ether into the reaction kettle, pass the chlorine gas treated in step (1) 0.9 times the mass of diphenyl ether and the sulfur dioxide gas prepared in step (2) and 0.8 times the mass of diphenyl ether into the reaction In the kettle, react with diphenyl ether for 5 hours at a temperature of 55°C, a pressure of 0.5KPa, and a stirring rate of 100 r / min, and then keep the pressure and stirring conditions constant and react at a temperature of 30°C for 4 hours.

[0026] (4) Feed chlorine gas into the reaction kettle again, react at a temperature of 35°C and a pressure of 0.05MPa, stop feeding chlorine gas when the oxidation-reduction potential suddenly rises, and then continue to reac...

Embodiment 2

[0028] (1) Under the catalysis of ferric chloride, chlorine gas is homogeneously split into chlorine free radicals by light; the amount of catalyst ferric chloride is 2% of the mass of chlorine gas.

[0029] (2) Sulfur dioxide gas is produced by burning sulfur in the air.

[0030] (3) Put the diphenyl ether into the reactor, and pass the chlorine gas with 1.1 times the mass of diphenyl ether treated in step (1) and the sulfur dioxide gas with 0.95 times the mass of diphenyl ether prepared in step (2) into the reactor , react with diphenyl ether for 4 hours at a temperature of 70°C, a pressure of 3KPa and a stirring rate of 200 r / min, and then keep the pressure and stirring conditions constant and react at a temperature of 45°C for 3 hours.

[0031] (4) Feed chlorine gas into the reaction kettle again, react at a temperature of 45°C and a pressure of 0.09MPa, stop feeding chlorine gas when the oxidation-reduction potential suddenly rises, and then continue to react at a tempera...

Embodiment 3

[0033] (1) Under the catalysis of ferric chloride, chlorine gas is homogeneously split into chlorine free radicals by light; the amount of catalyst ferric chloride is 3% of the mass of chlorine gas.

[0034] (2) Sulfur dioxide gas is produced by burning sulfur in the air.

[0035] (3) Put the diphenyl ether into the reactor, and pass the chlorine gas with 1.2 times the mass of diphenyl ether treated in step (1) and the sulfur dioxide gas with 1.1 times the mass of diphenyl ether prepared in step (2) into the reactor , react with diphenyl ether for 3 hours at a temperature of 90°C, a pressure of 5KPa, and a stirring rate of 300 r / min, and then keep the pressure and stirring conditions constant and react at a temperature of 60°C for 2 hours.

[0036] (4) Feed chlorine gas into the reaction kettle again, react at a temperature of 50°C and a pressure of 0.15MPa, stop feeding chlorine gas when the oxidation-reduction potential suddenly rises, and then continue to react at a tempera...

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Abstract

The invention discloses a method for preparing OBSC (4,4'-oxo-bis-benzenesulfonyl chloride) from basic chemical raw materials, which comprises the following steps: (1) irradiating chlorine gas in light under the catalytic action of iron trichloride to crack into chlorine free radicals; (2) combusting sulfur in air to prepare sulfur dioxide gas; (3) adding diphenyl ether into a reaction kettle, introducing the chlorine gas treated by the step (1) and the sulfur dioxide gas prepared in the step (2) into the reaction kettle, reacting with the diphenyl ether at 55-90 DEG C for 3-5 hours, and reacting at 30-60 DEG C for 2-4 hours; and (4) introducing chlorine gas into the reaction kettle, reacting at 35-50 DEG C, stopping introducing the chlorine gas when the oxidation-reduction potential suddenly increases, and continuing the reaction at 35-50 DEG C for 1-3 hours, thereby obtaining the OBSC. The product prepared by the method has the advantages of lower production cost, high yield, high purity and no generation of waste liquids, and has higher yield and purity than that of the traditional preparation method.

Description

technical field [0001] The invention relates to a method for preparing OBSC with basic chemical raw materials. Background technique [0002] At present, OBSC is used as a raw material to prepare various products such as high, medium and low temperature foaming agents and engineering plastics, which are widely used in the fields of chemical industry, aviation, electrical insulation, etc. It is a key intermediate widely used in high-end plastic and rubber industries . [0003] The traditional process of synthesizing 4,4'-oxobisbenzenesulfonyl chloride (OBSC) is mostly liquid sulfonating agent and chlorinating agent phosphorus oxychloride. For example, most of the current production of OBSC uses chlorosulfonic acid or concentrated sulfuric acid to sulfonate diphenyl ether, which consumes a lot of sulfonating agent raw materials and cannot be recycled, resulting in a lot of waste. A large amount of water will produce a large amount of acidic waste water at the same time, and i...

Claims

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Application Information

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IPC IPC(8): C07C309/87C07C303/02
Inventor 鞠有国孙跃明邢晓华赵奔腾
Owner SHANDONG TIANYI CHEM
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