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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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 was...

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.

Application Domain

Sulfonic acid preparation

Technology Topic

Diphenyl etherSulfur dioxide +7

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Examples

Experimental program(3)

Example Embodiment

[0022] Example 1

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

[0024] (2) Use sulfur to burn in the air to prepare sulfur dioxide gas.

[0025] (3) Put diphenyl ether into the reaction kettle, and pass the chlorine gas treated in step (1) with 0.9 times the mass of diphenyl ether and 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 unchanged and react for 4 hours at a temperature of 30°C.

[0026] (4) Chlorine gas is then introduced into the reactor, and the reaction is carried out at a temperature of 35°C and a pressure of 0.05MPa. When the oxidation-reduction potential increases suddenly, the introduction of chlorine gas is stopped, and then the temperature is 35°C and pressure of 0.05MPa. After reacting for 3 hours, 4,4-oxobisbenzenesulfonyl chloride is obtained after the reaction is completed.

Example Embodiment

[0027] Example 2

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

[0029] (2) Use sulfur to burn in the air to prepare sulfur dioxide gas.

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

[0031] (4) Then pass chlorine into the reactor, and react at a temperature of 45°C and a pressure of 0.09MPa. When the oxidation-reduction potential suddenly rises, stop the introduction of chlorine, and then continue to a temperature of 45°C and a pressure of 0.09MPa After reacting for 2 hours, 4,4-oxobisbenzenesulfonyl chloride is obtained after the reaction is completed.

Example Embodiment

[0032] Example 3

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

[0034] (2) Use sulfur to burn in the air to prepare sulfur dioxide gas.

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

[0036] (4) Chlorine gas is then introduced into the reactor, and the reaction is carried out at a temperature of 50°C and a pressure of 0.15MPa. When the oxidation-reduction potential suddenly rises, the introduction of chlorine gas is stopped, and then the temperature is 50°C and pressure of 0.15MPa. After reacting for 1 hour, 4,4-oxobisbenzenesulfonyl chloride is obtained after the reaction is completed.

[0037] The physical property parameters of the OBSC prepared in the above embodiment are shown in Table 1.

[0038] Table 1 OBSC physical property parameter table

[0039]

[0040] Note: The appearance is determined by visual inspection; the purity is determined by liquid chromatography, and the 0.5% thermal weight loss temperature is determined by a thermal weight loss analyzer.

[0041] It can be seen from the above table that the 0.5% weight loss temperature of the OBSC obtained in the present invention is above 310°C, and its purity is above 90%; while the 0.5% weight loss temperature of the OBSC prepared by the prior art is about 290°C, Its purity is about 85%; this shows that the present invention has greater advantages compared with the prior art.

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Classification and recommendation of technical efficacy words

low cost

Method, apparatus and article for microfluidic control via electrowetting, for chemical, biochemical and biological assays and the like

InactiveUS7163612B2low cost

Owner:KECK GRADUATE INST OF APPLIED LIFE SCI

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

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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