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Method for preparing important monomer dihalo-disulfonic acid benzophenone of sulfonated polyetheretherketone and salt thereof

A technology of benzophenone disulfonate and benzophenone dihalide is applied in the efficient preparation of sulfonated aromatic ketones, 4 fields, can solve the problems of high acid content, environmental pollution, low utilization rate, etc., and achieves pollution reduction , The preparation process is stable and simple, and the utilization rate is improved.

Active Publication Date: 2009-10-07
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

Method used

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  • Method for preparing important monomer dihalo-disulfonic acid benzophenone of sulfonated polyetheretherketone and salt thereof
  • Method for preparing important monomer dihalo-disulfonic acid benzophenone of sulfonated polyetheretherketone and salt thereof
  • Method for preparing important monomer dihalo-disulfonic acid benzophenone of sulfonated polyetheretherketone and salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Get 95 grams of 4,4'-difluorobenzophenone and 470 grams of oleum with a weight concentration of sulfur trioxide of 20% and mix them with a liquid-sealed nitrogen system. 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 182 grams of white solid product which was 4,4'-difluoro-3,3'-sodium disulfonate benzophenone, with a yield of 99%. The utilization rate of sulfur trioxide is 73%.

Embodiment 2

[0027] Get 95 grams of 4,4'-difluorobenzophenone and 376 grams of oleum with a weight concentration of sulfur trioxide of 25% and mix them with a liquid-sealed nitrogen system. React at 150°C for 10 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. Repeat the operation of adding sodium chloride twice, combine the solids, and dry to obtain 176 grams of white solid product as 4,4'-difluoro-3,3'-sodium disulfonate benzophenone, with a yield of 96%. The utilization rate of sulfur trioxide is 71%.

Embodiment 3

[0029] Get 95 grams of 4,4'-difluorobenzophenone and 696 grams of oleum with a sulfur trioxide weight concentration of 20% and mix them with a liquid-sealed nitrogen system. Under the cooling condition of -5°C ethanol circulating cooling liquid, Heated to 130°C for 12 hours to react, naturally cooled to room temperature, and poured 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 179 grams of white solid product which was 4,4'-difluoro-3,3'-sodium disulfonate benzophenone, with a yield of 97%. ...

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Abstract

The present invention discloses a method for preparing important monomer dihalo-disulfonic acid benzophenone of sulfonated polyetheretherketone and salt thereof. According to the method, 4,4'-dihalo benzophenone and oleum with concentration of 15-25% counted by the weight of sulfur trioxide in a liquid seal nitrogen protection system. The mixture is executed with temperature reaction under the temperature of 100-150 DEG C for 6-12 hours; wherein the molar ratio between 4,4'-dihalo benzophenone and oleum is 1: 2.00-1: 1.35. The preparing method of the invention adopts a design of liquid sealed nitrogen protection, avoids the loss of sulfur trioxide along with the nitrogen and increases the usage factor. The usage factor of sulfur trioxide can be increased to 60% mostly. Simultaneously the pollution to the environment is reduced. The method of the invention is more suitable for the large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of reverse osmosis, nanofiltration membrane water treatment and preparation of fuel cell application materials, and relates to an efficient preparation method of sulfonated aromatic ketones, more specifically 4,4'-dihalogen-3,3'-di Efficient preparation method of sulfonic acid benzophenone and salt. Background technique [0002] According to literature reports, sulfonation as a material design strategy can increase the hydrophilicity of PEEK membranes. The most attractive features of sulfonated polyetherketones are their selective ion passage and their high resistance to chlorine over a wide pH range. At the same time, the presence of sulfonic acid groups provides the prerequisites for the function of the proton exchange membrane. However, the previous sulfonated polyetherketone materials were obtained by sulfonation after polymerization. The strong acid used therein, such as: sulfuric acid or chlorosulfo...

Claims

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Application Information

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IPC IPC(8): C07C303/06C07C303/32C07C309/44
Inventor 张中标宋爱茹郑勇
Owner TIANJIN NORMAL UNIVERSITY