Preparation method of 4, 4 '-dichlorodiphenyl sulfone

A technology of dichlorodiphenyl sulfone and dichlorodiphenyl sulfoxide, which is applied in the field of preparation of 4,4´-dichlorodiphenyl sulfone, can solve complex catalyst preparation process, equipment corrosion, special quaternary ammonium salt phase transfer agent Expensive and other issues

Active Publication Date: 2021-09-14
FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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Problems solved by technology

[0003] Hydrogen peroxide is used as an oxidant in the traditional sulfoxide oxidation method, but the purity of the obtained 4,4´-dichlorodiphenyl sulfone is low; after further improvement, many industrial productions use a large amount of sulfuric acid to enhance the acidity of the system, mixed with acetic acid or Peroxyacid has an oxidation effect, but a large amount of mixed acid is used, which has a high degree of corrosion to equipment, and it is difficult to treat the mixed waste liquid of mixed acid and solvent, and the separation of acid and solvent is relatively difficult. The separation cost is high, and the prepared 4 ,4´-dichlorodiphenyl sulfone post-treatment steps are more cumbersome, the process is more complicated, which virtually increases the production cost of the enterprise
[0004] As a further improvement, the quaternary ammonium phosphotungstic acid catalyst was used in the research, but the matching special quaternary ammonium salt phase transfer agent is expensive. As a cost consideration, enterprises are limited in its promotion and application
[0005] CN107540581A adopts formic acid or glacial acetic acid, and corresponding peroxyacid as medium reaction, but obtains lower purity
[0006] CN106349126A adopts concentrated sulfuric acid catalyst, chlorobenzene and glacial ac

Method used

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  • Preparation method of 4, 4 '-dichlorodiphenyl sulfone
  • Preparation method of 4, 4 '-dichlorodiphenyl sulfone
  • Preparation method of 4, 4 '-dichlorodiphenyl sulfone

Examples

Experimental program
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Effect test

Embodiment 1

[0043] The preparation method of described 4,4'-dichlorodiphenylsulfone comprises the following steps:

[0044] (1) Mix 0.40g ammonium molybdate, 0.37g oxalic acid, and 24.75g 27.5% hydrogen peroxide for 1 hour at room temperature to obtain a mixed solution;

[0045] (2) Add the above mixed solution dropwise into a four-neck flask containing 54.50g of 4,4´-dichlorodiphenylsulfoxide and 110.00g of dichloropropane, raise the temperature to 80°C, and react for 5 hours;

[0046] (3) After the reaction, add 0.17g of activated carbon to the reaction liquid to react for 0.5 hours, remove impurities and decolorize, filter out the activated carbon while it is hot, cool the resulting solution to 5°C, cool and crystallize for 1.5 hours, and filter again to obtain filter cake and remaining Filtrate, the filter cake was dried at 85°C for 7 hours to obtain high-purity 4,4´-dichlorodiphenylsulfone; the yield of the obtained 4,4´-dichlorodiphenylsulfone was 97.2%, and the purity was tested by...

Embodiment 2

[0049] The preparation method of described 4,4'-dichlorodiphenylsulfone comprises the following steps:

[0050] (1) Mix 0.40g ammonium molybdate, 0.37g oxalic acid, and 24.75g 27.5% hydrogen peroxide for 1 hour at room temperature to obtain a mixed solution;

[0051] (2) Add the above mixed solution dropwise into a four-neck flask containing 54.50g of 4,4´-dichlorodiphenyl sulfoxide and 110.00g of chlorobenzene, raise the temperature to 80°C, and react for 5 hours;

[0052] (3) After the reaction, add 1.00g of activated carbon to the reaction liquid to react for 0.5 hours, remove impurities and decolorize, filter out the activated carbon while it is hot, cool the resulting solution to 5°C, cool and crystallize for 1.5 hours, and filter again to obtain filter cake and remaining Filtrate, the filter cake was dried at 85°C for 7 hours to obtain high-purity 4,4´-dichlorodiphenylsulfone; the yield of the obtained 4,4´-dichlorodiphenylsulfone was 97.8%, and the purity was tested by ...

Embodiment 3

[0055]The preparation method of described 4,4'-dichlorodiphenylsulfone comprises the following steps:

[0056] (1) Mix 0.40g ammonium molybdate, 0.42g malonic acid, and 24.75g 27.5% hydrogen peroxide for 1 hour at room temperature to obtain a mixed solution;

[0057] (2) Add the above mixed solution dropwise into a four-neck flask containing 54.50g of 4,4´-dichlorodiphenyl sulfoxide and 110.00g of chlorobenzene, raise the temperature to 80°C, and react for 5 hours;

[0058] (3) After the reaction, add 1.00g of activated carbon to the reaction liquid to react for 0.5 hours, remove impurities and decolorize, filter out the activated carbon while it is hot, cool the resulting solution to 5°C, cool and crystallize for 1.5 hours, and filter again to obtain filter cake and remaining Filtrate, the filter cake was dried at 85°C for 7 hours to obtain high-purity 4,4´-dichlorodiphenylsulfone; the yield of the obtained 4,4´-dichlorodiphenylsulfone was 97.3%, and the purity was tested by ...

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of high-purity 4, 4-dichlorodiphenyl sulfone. The preparation method of the high-purity 4, 4-dichlorodiphenyl sulfone comprises the following steps: firstly, mixing molybdate, organic dicarboxylic acid and hydrogen peroxide, dropwise adding the mixture into a mixed solution of 4, 4-dichlorodiphenyl sulfoxide and a solvent for reaction, and after the reaction is completed, performing post-treatment to obtain the high-purity 4, 4-dichlorodiphenyl sulfone and residual filtrate; the residual filtrate is directly used for the next round of reaction after being layered; the molar ratio of the 4, 4-dichlorodiphenyl sulfoxide to the molybdate to the organic dicarboxylic acid to the hydrogen peroxide is 1: (0.01-0.05): (0.02-0.1): (1-3). The invention provides the preparation method of the high-purity 4, 4-dichlorodiphenyl sulfone, the catalyst is low in cost, the preparation steps are simple, the post-treatment steps are simple, the reaction residual filtrate is circularly and efficiently utilized, the purity is high, and the yield is high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of 4,4'-dichlorodiphenyl sulfone. Background technique [0002] 4,4´-dichlorodiphenyl sulfone is an important chemical raw material. There are many methods for industrial production of 4,4´-dichlorodiphenyl sulfone. Regarding the preparation of 4,4´-dichlorodiphenyl sulfone by sulfoxide oxidation There are also many reports on chlorodiphenyl sulfone. [0003] Hydrogen peroxide is used as an oxidant in the traditional sulfoxide oxidation method, but the purity of the obtained 4,4´-dichlorodiphenyl sulfone is low; after further improvement, many industrial productions use a large amount of sulfuric acid to enhance the acidity of the system, mixed with acetic acid or Peroxyacid has an oxidation effect, but a large amount of mixed acid is used, which has a high degree of corrosion to equipment, and it is difficult to treat the mixed waste l...

Claims

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Application Information

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IPC IPC(8): C07C315/00C07C317/14
CPCC07C315/00C07C317/14
Inventor 周玉有黄森彪王敏廖广明
Owner FUHAI (DONGYING) ADVANCED MATERIAL TECH CO LTD
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