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Production method of disulfonated dihalogenated diphenylsulfone

A technology of disulfonated dihalogenated diphenyl sulfone and dihalogenated diphenyl sulfone, which is applied in the field of chemical synthesis and polymer material application, and can solve problems such as difficult molecular weight control, high-purity sulfonated mono To solve the problem of high bulk cost, achieve high solubility, fast reaction speed, improve the success rate of polymerization and control the effect of polymer molecular weight

Inactive Publication Date: 2018-06-05
钟卓尔 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, high-purity sulfonated dihalodiphenylsulfone monomers that can be used for polymerization have not been mass-produced for various reasons, such as the amount of sulfonating agent used, the solubility of products in the reaction, post-treatment of the reaction and The problem of purification, the impact of monosulfonated products and inorganic salt impurities on product purity, etc., have not been well resolved in the process of scale-up production
The above problems lead to high cost of high-purity sulfonated monomers, low success rate of polymerization reaction, and difficulty in molecular weight control, which restricts the wide application of sulfonated poly(phenylene ether sulfone) copolymers
[0004] Therefore, the production of high-purity polymerizable sulfonated dihalogenated diphenylsulfone monomers is a bottleneck hindering the large-scale application of sulfonated polyphenylene ether sulfone materials in the field of water treatment, which needs to be solved urgently

Method used

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  • Production method of disulfonated dihalogenated diphenylsulfone
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  • Production method of disulfonated dihalogenated diphenylsulfone

Examples

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Embodiment 1

[0031] Embodiment 1: the production of disulfonated 4,4'-dichlorodiphenyl sulfone

[0032] In a dry 20-liter airtight reactor with mechanical stirring and bubbler, add raw materials sequentially, 2872 grams of 4,4'-dichlorodiphenyl sulfone, and prepare 14% sulfur trioxide after calibration by acid-base titration Fuming concentrated sulfuric acid 12010 grams. Stir mechanically to 60 rpm, and gradually heat up the oil bath. When the temperature in the reactor rises to about 75 degrees Celsius, the 4,4'-dichlorodiphenyl sulfone is completely dissolved. Continue to increase the oil bath temperature until the temperature in the reactor is 160 degrees Celsius, increase the stirring speed to 80 rpm; keep the temperature in the reactor at 160 degrees Celsius to continue the homogeneous reaction for 4.5 hours, stop heating, and cool. After the temperature in the reactor drops to 45 degrees Celsius, add about 9000 grams of sodium hydroxide to gradually neutralize to pH ~ 8-9 under the...

Embodiment 2

[0033] Embodiment 2: the production of disulfonated 4,4'-difluorodiphenyl sulfone

[0034] In a dry 20-liter airtight reactor with mechanical stirring and bubbler, add raw materials sequentially, 2543 grams of 4,4'-difluorodiphenyl sulfone, and prepare 14% sulfur trioxide after calibration by acid-base titration Fuming concentrated sulfuric acid 12010 grams. Stir mechanically to 60 rpm, and gradually heat up the oil bath. When the temperature in the reactor rises to about 70 degrees Celsius, the 4,4'-difluorodiphenyl sulfone is completely dissolved. Continue to increase the oil bath temperature until the temperature in the reactor is 158 degrees Celsius, increase the stirring speed to 80 rpm; keep the temperature in the reactor at 158 ​​degrees Celsius to continue the homogeneous reaction for 4 hours, stop heating, and cool. After the temperature in the reactor drops to 45 degrees Celsius, about 13,000 grams of potassium hydroxide is added to gradually neutralize the pH to 8...

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Abstract

The invention discloses a production method of disulfonated dihalogenated diphenylsulfone. The method disclosed by the invention comprises the following steps: carrying out a reaction on fuming sulfuric acid with accurately calibrated sulfur trioxide concentration with dihalogenated diphenylsulfone to obtain a completely disulfonated dihalogenated diphenylsulfone product; after the reaction, omitting a salting-out process, carrying out neutralization directly, and carrying out filtering and drying; and then improving the purity of the product through recrystallization. According to the technical scheme provided by the invention, the addition amount and concentration of a sulfonating agent sulfur trioxide are accurately controlled, the reaction is ensured to be carried out always under a homogeneous phase, meanwhile the defects that the reaction cannot be carried out completely under the heterogeneous condition caused by excessive sulfonating agent can be avoided, the salting-out process is omitted, the influence of introducing excessive inorganic salt on the post-treatment is avoided, and finally the high-purity polymerization-grade product is obtained through recrystallization.

Description

technical field [0001] The invention relates to a preparation and production technology of sulfonated monomers for polymerization, in particular to a production method of disulfonated dihalogenated diphenyl sulfone, which belongs to the field of chemical synthesis and polymer material application. Background technique [0002] Hydrophilic modified poly(phenylene ether sulfone) is a new type of membrane material that can be used in water treatment and hemodialysis, and has broad application prospects. The introduction of sulfonated dihalogenated diphenyl sulfone monomers for copolymerization is a very effective way of hydrophilic modification of poly(phenylene ether sulfone). Because the degree of sulfonation can be controlled and adjusted by the amount of sulfonated monomer added, and the sulfonated functional groups are uniformly dispersed at the molecular level in the copolymer matrix, the sulfonated polymer obtained by copolymerization can be obtained more than the later ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/14C07C315/04C07C315/06
CPCC07C315/04C07C315/06C07C317/14
Inventor 钟卓尔钟禺
Owner 钟卓尔
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