Efficient preparation method of sulfonated polyethersulfone monomer

A technology for sulfonated polyethersulfone and monomers, which is applied in the field of nanofiltration membrane water treatment and fuel cell application materials, reverse osmosis, and can solve the problems of low product yield, high acid content, low utilization rate, etc., and achieve improvement Utilization rate, pollution reduction, pollution reduction effect

Active Publication Date: 2011-12-28
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing reaction, the structure of the blowing nitrogen protection system is adopted, and a large amount or even an excess of sulfur trioxide is required (over 115%). Environmental pollution, and product yield is low

Method used

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  • Efficient preparation method of sulfonated polyethersulfone monomer
  • Efficient preparation method of sulfonated polyethersulfone monomer
  • Efficient preparation method of sulfonated polyethersulfone monomer

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preparation example Construction

[0021] A high-efficiency preparation method for sulfonated polyethersulfone monomer is characterized in that the implementation steps include:

[0022] Dihalogenated diphenyl sulfone and oleum are used as starting materials, the fuming sulfuric acid adopts oleum with a weight concentration of sulfur trioxide of 15-25%, and the starting material is 4,4'-dihalodiphenyl sulfone The molar ratio to sulfur trioxide ranges from 1:2.00-1:1.35; the reaction temperature is 100°C-150°C, and the reaction time is 6-12 hours; the experimental device adopts a liquid-sealed type that avoids the loss of sulfur trioxide with nitrogen. Nitrogen protection system; low-temperature coolant cooling system, coolant temperature range -5°C-15°C; efficient preparation of 4,4'-dihalo-3,3'-disulfonic acid and salt diphenyl sulfone monomer.

[0023]

[0024] The above is the structure of 4,4'-dihalo-3,3'-disulfonic acid and salt diphenyl sulfone monomer (X=F or Cl; M=H, the first group of alkali metals,...

Embodiment 1

[0033] Get 133 grams of 4,4'-dichlorodiphenyl sulfone and 500 grams of sulfur trioxide weight concentration of 20% fuming sulfuric acid to mix, adopt liquid-sealed nitrogen system protection, under the cooling condition of 5 ℃ ethanol circulating cooling liquid, be heated to React at 130°C for 7 hours, cool naturally to room temperature, and pour into 1.2 liters of ice water. Add 100 g of sodium chloride, stir at room temperature for 4 hours, filter, and drain the solid. Repeat the above operation of adding sodium chloride twice; combine the obtained white solids, add 1 liter of water to dissolve, and adjust the pH value to 7 with 1 mole per liter of sodium hydroxide solution. Add 100 g of sodium chloride, stir at room temperature for 4 hours, filter, and drain the solid. The operation of adding sodium chloride was repeated twice, the solids were combined and dried to obtain 223 grams of white solid product with a yield of 98%.

Embodiment 2

[0035] Get 133 grams of 4,4'-dichlorodiphenyl sulfone and 400 grams of sulfur trioxide weight concentration to be 25% oleum and mix, adopt the protection of liquid-sealed nitrogen system, under the cooling condition of 12 ℃ of ethanol circulation coolants, be heated to React at 150°C for 7 hours, cool naturally to room temperature, and pour into 1.2 liters of ice water. Add 100 g of sodium chloride, stir at room temperature for 4 hours, filter, and drain the solid. Repeat the above operation of adding sodium chloride twice; combine the obtained white solids, add 1 liter of water to dissolve, and adjust the pH value to 7 with 1 mole per liter of sodium hydroxide solution. Add 100 g of sodium chloride, stir at room temperature for 4 hours, filter, and drain the solid. The operation of adding sodium chloride was repeated twice, the solids were combined and dried to obtain 218 grams of white solid product with a yield of 96%.

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Abstract

The invention provides a high-efficiency preparation method of sulfonated polyethersulfone monomer, the implementation steps include: using dihalogenated diphenyl sulfone and oleum as starting materials, and the oleum is made of sulfur trioxide with a weight concentration of 15 -25% oleum, the molar ratio range of the starting material 4,4'-dihalodiphenyl sulfone to sulfur trioxide is 1:2.00-1:1.35; the reaction temperature is 100°C-150°C, and the reaction time is 6-12 hours; the experimental device adopts a liquid-sealed nitrogen protection system to avoid the loss of sulfur trioxide with nitrogen; a low-temperature coolant cooling system is used, and the temperature range of the coolant is -5°C-15°C; efficient preparation obtains 4,4' - Dihalo-3,3'-disulfonic acid and salt diphenyl sulfone monomers. The invention adopts a liquid-sealed nitrogen protection design, avoids the loss of sulfur trioxide with nitrogen, improves its utilization rate, and the maximum utilization rate of sulfur trioxide is increased by 60%; at the same time, environmental pollution is reduced. The preparation method of the invention is simple and reasonable, energy-saving and high-efficiency, the preparation process is stable and convenient, pollution is reduced, and product quality and output are effectively improved.

Description

technical field [0001] The invention relates to the technical field of preparation of reverse osmosis, nanofiltration membrane water treatment and fuel cell application materials, in particular to a high-efficiency preparation method of sulfonated polyethersulfone monomer. Background technique [0002] One of the urgent needs of the development of human society in the 21st century is to have a safe and sustainable source of fresh water. Membrane-based water desalination technology is an energy-efficient, low-environmental-impact route to clean water for a range of applications. The continuous decline in membrane system investment cost, operation and maintenance costs makes it more attractive in the field of water purification applications. Membrane separation processes, such as nanofiltration and reverse osmosis, have rapidly developed into mainstream technologies for water desalination over the past three decades. Commercially available reverse osmosis membranes are mainl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/14C07C315/04
Inventor 张中标宋爱茹郑勇
Owner TIANJIN NORMAL UNIVERSITY
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