Method for preparing cross-linked polyimide membrane

A sulfonated polyimide membrane and a technology of sulfonated polyimide are applied in the field of preparation of functional polymer materials to achieve the effects of low cost, improved service life and simple operation

Inactive Publication Date: 2006-05-03
SHANGHAI CHLOR ALKALI CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the water resistance of these polymers needs to be further improved from the perspective of actual use, especially in high temperature (>100°C) occasions.

Method used

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  • Method for preparing cross-linked polyimide membrane
  • Method for preparing cross-linked polyimide membrane
  • Method for preparing cross-linked polyimide membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The preparation of embodiment 1 sulfonated polyimide NTDA-ODADS / BAPF (5 / 1):

[0039] NTDA refers to 1,4,5,8-naphthalic anhydride, ODADS refers to 4,4'-diaminodiphenyl ether-2,2'-disulfonic acid, BAPF refers to 9,9-bis(4-aminophenyl) fluorene;

[0040] Add 0.7200 g (2.0 mmol) of ODADS, 0.1392 g (0.4 mmol) of BAPF, 10 mL of m-cresol and 0.68 mL of triethylamine into a dry 100 mL three-necked flask equipped with a condenser and a nitrogen inlet and outlet. After the diamine monomer was completely dissolved, 0.6432 g (2.4 mmol) of NTDA and 0.42 g of benzoic acid were added. The reaction mixture was stirred at room temperature for 0.5 hours, then heated to 80°C for 4 hours, and then heated to 180°C for 20 hours. After the reaction, the resulting highly viscous polymer solution was diluted with 10 mL of m-cresol, and then slowly poured into 200 mL of methanol / hydrochloric acid solution with a volume ratio of 3:1 to obtain a fibrous precipitate, which was filtered and used ...

Embodiment 2

[0041] Preparation of embodiment 2 cross-linked sulfonated polyimide NTDA-ODADS / BAPF (5 / 1) membrane:

[0042] 1.8 grams of dry sulfonated polyimides obtained in Example 1 were dissolved in 20 mL of dimethyl sulfoxide containing 10 wt % phosphorus pentoxide, and the resulting solution was poured onto a glass plate at 80 ° C and 150 ° C. °C for 2 hours and 10 hours, respectively, and then dried at 150 °C for 20 hours under vacuum. The sulfonated polyimide was peeled off from the pouring glass plate, washed with deionized water to neutrality, and then dried under vacuum to obtain a sulfonated polyimide NTDA-ODADS / BAPF (5 / 1) film with a thickness of is 40 μm.

Embodiment 3

[0043] The performance of embodiment 3 cross-linked sulfonated polyimide NTDA-ODADS / BAPF (5 / 1) film:

[0044] The cross-linked sulfonated polyimide NTDA-ODADS / BAPF (5 / 1) film obtained in Example 2 was put into dimethyl sulfoxide for a solubility test, and it was found that the film was completely insoluble in dimethyl sulfoxide , indicating that crosslinking has occurred. The membrane was soaked in deionized water at 100°C for one month (720 hours), and it was found that the membrane still had good mechanical strength. The proton conductivity of the membrane was 0.13 S / cm at 60°C and 100% relative humidity, and 0.20 S / cm at 130°C and 100% relative humidity.

[0045] The tensile strength of the film soaked in deionized water at 100° C. for one month was immediately measured, and the measured tensile strength was 10-12 MPa.

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Abstract

The invention relates to a new method to prepare crosslinking polysulfonimides membrane, which comprises: dissolving the material in organic solvent with phosphoric anhydride, film forming with liquid moulding, drying for 2~20h at 60~200Deg; then, drying in vacuum for 1~30h at 100~200Deg; dipping the membrane in deionized water, clearing to neutrality, and drying in vacuum. This method is simple and economical. This product has well water resistance and high proton conductivity and wide application in fuel cell, ion exchange resin and sensor.

Description

technical field [0001] The invention relates to a preparation method of a functional polymer material, in particular to a preparation method of a cross-linked sulfonated polyimide membrane. Background technique [0002] Polyimide is a class of high-performance polymers with excellent heat resistance, high mechanical strength and modulus, excellent electrical properties and good chemical resistance. It has been widely used in aerospace industry and electronics industry. Six-membered ring sulfonated polyimide is a new member of the polyimide family developed in recent years. These materials have potential application prospects in fuel cells, ion exchange resins, membrane separation and sensors. Especially in terms of fuel cells, sulfonated polyimide is considered to be one of the most promising new proton exchange membrane materials for practical use. French patent 9605707 (1996) reported the preparation method of sulfonated polyimide for the first time, and its used sulfon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08G73/10C08J3/24
CPCY02E60/50
Inventor 房建华郭晓霞陈斌武蔡华明
Owner SHANGHAI CHLOR ALKALI CHEM
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