A kind of preparation method of 4,4-dichlorodiphenyl sulfone

A technology of dichlorodiphenyl sulfone and chlorobenzene, which is applied in the field of chemical material preparation, can solve the problems of complicated reaction steps, poor product quality stability, three wastes of easily corroded equipment, etc., and achieves low comprehensive cost, short reaction period, three wastes and the like. less effect

Active Publication Date: 2017-11-21
河北旭隆化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] The purpose of the present invention is to provide a preparation method of 4,4-dichlorodiphenyl sulfone, to solve the existing preparation method has complex and complicated reaction steps, high reaction temperature, inconvenient production control, poor product quality stability, low yield low, easy to corrode equipment, and produce more three wastes, etc.

Method used

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  • A kind of preparation method of 4,4-dichlorodiphenyl sulfone
  • A kind of preparation method of 4,4-dichlorodiphenyl sulfone
  • A kind of preparation method of 4,4-dichlorodiphenyl sulfone

Examples

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Effect test

Embodiment 1

[0047] (1) Add 30Kg of dimethyl sulfoxide as a catalyst in a clean enamel kettle, add 598Kg of liquid sulfur trioxide and 470Kg of dimethyl sulfate, and esterify at 20°C for 2.5h to obtain 1098Kg of esterification material;

[0048] (2) Take a clean enamel kettle, add 837Kg of chlorobenzene, and add the esterified material obtained in step (1) to the chlorobenzene at 2800mL / min while maintaining the temperature at 25℃, and keep the temperature for 3h to obtain the condensation material ;

[0049] (3) Take another clean enamel kettle and add 534Kg of sodium hydroxide and 2432Kg of water. After fully dissolving, heat the condensate obtained in step (2) to 60°C, and slowly add dropwise to the sodium hydroxide at 7400mL / min Hydrolyzed in aqueous solution (mass percentage concentration of 18%), heated to 80°C, stirred, refluxed for 1h, cooled to 60°C, centrifuged at 3500r / min for 60min, took the filter cake and washed it with 60°C hot water to neutral (pH value 7.0), 998.7Kg of 4,4-di...

Embodiment 2

[0051] (1) Add 30.5Kg of dimethyl sulfoxide as a catalyst in a clean enamel kettle, add 611Kg of liquid sulfur trioxide and 480Kg of dimethyl sulfate, and esterify at 16℃ for 3h to obtain 1121.5Kg of Esterified material

[0052] (2) Take a clean enamel kettle, add 855Kg of chlorobenzene, and add the esterified material obtained in step (1) to the chlorobenzene at 2800mL / min while keeping the temperature at 30℃, and keep the temperature for 1h to obtain the condensation material ,

[0053] (3) Take another clean enamel kettle, add 545Kg of sodium hydroxide, add 2483Kg of water, and after fully dissolving, heat the condensate obtained in step (2) to 55℃, and slowly add dropwise to the sodium hydroxide at 7400mL / min Hydrolyzed in an aqueous solution (18% by mass), heated to 70°C, stirred, refluxed for 1h, cooled to 60°C, 3500r / min), centrifuged for 65min, and washed the filter cake with hot water at 75°C to neutral (pH value 7.0) to obtain 998.5Kg of 4,4-dichlorodiphenylsulfone.

Embodiment 3

[0055] (1) Add 30.3Kg of dimethyl sulfoxide as a catalyst in a clean enamel kettle, add 606Kg of liquid sulfur trioxide and 476Kg of dimethyl sulfate, and esterify at 10℃ for 3h to obtain 1112.3Kg of Esterified material

[0056] (2) Take a clean enamel kettle, add 848Kg of chlorobenzene, and add the esterified material obtained in step (1) to the chlorobenzene at 2800mL / min while keeping the temperature at 30℃, and keep the temperature for 1 hour to obtain the condensation material ,

[0057] (3) Take another clean enamel kettle and add 541Kg of sodium hydroxide and 2465Kg of water. After fully dissolving, heat the condensate obtained in step (2) to 50°C, and slowly add dropwise to the sodium hydroxide at 7400mL / min Hydrolyzed in an aqueous solution (18% by mass), heated to 70°C, stirred, refluxed for 1.5h, cooled to 60°C, centrifuged at 3500r / min for 60min, and the filter cake was washed with 70°C hot water to neutral (pH value 7.0), 998.8Kg of 4,4-dichlorodiphenylsulfone was ob...

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Abstract

The invention discloses a preparation method of 4,4-dichlorodiphenyl sulfone. The preparation method of the 4,4-dichlorodiphenyl sulfone comprises the following steps of adopting dimethyl sulfoxide as a catalyst, adopting liquid sulfur trioxide and dimethyl sulfate as reaction raw materials, and carrying out esterification reaction for 2 to 3h at the temperature of 10 to 50 DEG C to obtain an esterification material; dropwise adding the esterification material into chlorobenzene, stirring and reacting for 3 to 6h at the temperature of 20 to 50 DEG C to obtain a condensation material; warming the condensation material to be 50 to 70 DEG C, dropwise adding the warmed condensation material into alkali solution to hydrolyze, warming to be 70 to 100 DEG C, stirring, backflowing for 1 to 1.5h, cooling to be 10 to 60 DEG C, centrifuging, washing a filter cake to be neutral, and obtaining the 4,4-dichlorodiphenyl sulfone. The technological method provided by the invention has the comprehensive advantages of smaller raw material unit consumption, high yield, stable production quality, simple preparation process, moderate reaction condition, easiness in operation and control, less three industrial wastes, energy conservation and environmental protection and the like compared with the prior art, and is very suitable for popularization and application of the current industrial production.

Description

Technical field [0001] The invention relates to the technical field of preparation of chemical materials, in particular to a preparation method of 4,4-dichlorodiphenylsulfone. Background technique [0002] 4,4-Dichlorodiphenyl sulfone, DDS for short, is a white crystal, sublimable, soluble in benzene, chlorobenzene, DMF and other organic solvents, slightly soluble in ethanol, methanol, insoluble in water, with a flash point of 233 ℃, boiling point of 397℃, melting point of 246-251℃; it has a wide range of uses in engineering plastics and fine chemicals, and is the main raw material for the manufacture of engineering plastics such as polysulfone and polyethersulfone; it is also the synthesis of 4,4-diamino Diphenyl sulfone and intermediates of medicines, dyes and pesticides have been widely used in engineering plastics and fine chemicals. [0003] At present, the synthesis method of 4,4-dichlorodiphenyl sulfone is relatively mature, mainly including the following four: [0004] a) C...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C315/00C07C317/14
CPCC07C315/00C07C317/14
Inventor 刘军强朱叙金
Owner 河北旭隆化工有限公司
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