Method for increasing sulfonation degree of polyetheretherketone

A technology of polyether ether ketone and sulfonation degree, which is applied in the field of polymer modification to achieve the effects of good mechanical stability, simple and convenient preparation process, excellent film-forming property and anti-swelling performance

Inactive Publication Date: 2019-07-09
SHANDONG XINGHUO SCI TECH INSTITYTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

People have been trying to prepare it as a membrane material, but only a few solvents such as concentrated sulfuric acid can dissolve it, which limits its wide application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A method for improving the degree of sulfonation of polyether ether ketone, comprising the following steps:

[0018] 1) Mix polyether ether ketone and composite sulfonating agent at a mass ratio of 1:30, stir and react at 50°C for 6 hours; the composite sulfonating agent is a mixture of concentrated sulfuric acid and sulfamic acid, the mass of concentrated sulfuric acid and sulfamic acid The ratio is 5:20.

[0019] 2) Cool to room temperature after the reaction, pour the mixed solution into the ice-water mixture, and wait for the product to precipitate.

[0020] 3) After the product is aspirated, it is washed with a large amount of pure water for several times until the pH of the product is neutral, then heat-treated with pure water at 55°C for 2 hours, and then filtered.

[0021] 4) Dry in an oven at 60°C for 12 hours, and then dry in a vacuum oven at 90°C for 24 hours to obtain sulfonated polyether ether ketone. The degree of sulfonation (DS) is calculated according...

Embodiment 2

[0023] A method for improving the degree of sulfonation of polyether ether ketone, comprising the following steps:

[0024] 1) Take polyether ether ketone and compound sulfonating agent in a mass ratio of 4:60, mix them, and stir at 50°C for 8 hours; the compound sulfonating agent is a mixture of concentrated sulfuric acid, aminosulfonic acid, and chlorosulfonic acid, concentrated sulfuric acid, The mass ratio of sulfonic acid and chlorosulfonic acid is 5:7:15.

[0025] 2) Cool to room temperature after the reaction, pour the mixed solution into the ice-water mixture, and wait for the product to precipitate.

[0026] 3) After the product is aspirated, it is washed with a large amount of pure water for several times until the pH of the product is neutral, then heat-treated with pure water at 50°C for 1.5h, and filtered.

[0027] 4) Dry in an oven at 60°C for 12 hours, and then dry in a vacuum oven at 90°C for 24 hours to obtain sulfonated polyether ether ketone. The degree of...

Embodiment 3

[0029] 1) Mix polyetheretherketone and composite sulfonating agent at a mass ratio of 3:40, stir and react at 50°C for 4 hours; composite sulfonating agent is a mixture of concentrated sulfuric acid, aminosulfonic acid, and chlorosulfonic acid The mass ratio of sulfonic acid and chlorosulfonic acid is 4:10:13.

[0030] 2) Cool to room temperature after the reaction, pour the mixed solution into the ice-water mixture, and wait for the product to precipitate.

[0031] 3) After the product is aspirated, it is washed with a large amount of pure water for several times until the pH of the product is neutral, then heat-treated with pure water at 60°C for 1 hour, and then filtered.

[0032] 4) Dry in an oven at 60°C for 12 hours, and then dry in a vacuum oven at 90°C for 24 hours to obtain sulfonated polyether ether ketone. The degree of sulfonation (DS) is calculated according to IEC=1000DS / (288+80DS), and the degree of sulfonation is 50% after measurement and calculation.

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PUM

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Abstract

The invention relates to a method for increasing the sulfonation degree of polyetheretherketone. The method comprises the following steps: mixing polyetheretherketone with a composite sulfonating agent and stirring for reaction at 50 DEG C for 4-8 hours; cooling down to room temperature after the reaction is finished, and pouring the mixed solution into an ice-water mixture for separating out theproduct; washing the resulting product for multiple times with a large amount of pure water until the pH value of the product is neutral, and then subjecting the product to heat treatment for 1-2 hours with heated pure water and carrying out filtering; carrying out drying at 60 DEG C for 12 hours in a drying oven, and then drying at 90 DEG C for 24 hours in a vacuum drying oven to obtain sulfonated polyetheretherketone. The sulfonated polyetheretherketone prepared by the method disclosed in the invention has a high sulfonation degree, which ranges from 50% to 70%, and has excellent film-forming and anti-swelling properties and good mechanical stability; and the preparation process is simple and convenient.

Description

technical field [0001] The invention belongs to the field of polymer modification, and in particular relates to a method for increasing the sulfonation degree of polyether ether ketone. Background technique [0002] Proton exchange membrane fuel cell is a high-efficiency, low-pollution power generation device. Compared with other types of fuel cells, proton exchange membrane fuel cells have the advantages of high specific power, low operating temperature, low corrosion and long life. As the core of the proton exchange membrane fuel cell, the performance of the proton exchange membrane plays a key role in the performance of the fuel cell. At present, the perfluorosulfonic acid membrane is the most used. Although the membrane shows good stability, it has disadvantages such as high cost, low proton conductivity at low humidity or high temperature, and high methanol permeability. The good heat resistance and mechanical properties of polyaryletherketone polymers have attracted ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28
CPCC08G8/28
Inventor 车春玲
Owner SHANDONG XINGHUO SCI TECH INSTITYTE
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