A kind of cross-linked chitosan/nitrogen-containing phosphonic acid group polysiloxane high temperature proton exchange membrane and preparation method thereof

A technology of cross-linked chitosan and proton exchange membrane, which is applied in sealing/supporting devices, fuel cells, electrochemical generators, etc., can solve the problems of phosphotungstic acid leakage, weakened ion cross-linking effect, and decreased conductivity. Achieve the effects of reducing swelling degree, increasing mechanical properties and thermal stability, and increasing mechanical properties

Inactive Publication Date: 2017-08-25
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as the temperature increases, the ion cross-linking effect between phosphotungstic acid and chitosan weakens, and a part of phosphotungstic acid will leak out, resulting in a decrease in electrical conductivity (Cui Z, Liu C, Lu T, et al. .Polyelectrolyte complexes of chitosan and phosphotungsticacid as proton-conducting membranes for direct methanol fuel cells[J].Journal of Power Sources,2007,167(1):94-99.)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of cross-linked chitosan / nitrogen-containing phosphonic acid group polysiloxane high-temperature proton exchange membrane, the specific steps are as follows:

[0034] 1) At normal temperature, prepare 10 mL of aqueous acetic acid solution with a volume concentration of 1%, dissolve 0.1 g of chitosan powder in the aqueous acetic acid solution, stir fully to make it dissolve uniformly, and obtain a chitosan solution;

[0035] 2) Dissolve 0.4984 g of aminotrimethylene phosphonic acid in 10 mL of deionized water, and keep stirring at room temperature for 12 hours to obtain a nitrogen-containing organic phosphonic acid solution;

[0036]3) Slowly add the above-mentioned nitrogen-containing organic phosphonic acid solution into the above-mentioned chitosan solution dropwise at room temperature, continue stirring at room temperature for 12 hours to obtain a mixed solution, and then add 4.4274g of aminosiloxane (3-aminopropyltriethoxy Silane) is slowly adde...

Embodiment 2

[0041] A preparation method of cross-linked chitosan / nitrogen-containing phosphonic acid group polysiloxane high-temperature proton exchange membrane, the specific steps are as follows:

[0042] 1) At normal temperature, prepare 10 mL of aqueous acetic acid solution with a volume concentration of 2%, dissolve 0.2 g of chitosan powder in the aqueous acetic acid solution, stir fully to make it dissolve uniformly, and obtain a chitosan solution;

[0043] 2) Dissolve 0.9968 g of aminotrimethylene phosphonic acid in 10 mL of deionized water, and continue stirring at room temperature for 12 hours to obtain a nitrogen-containing organic phosphonic acid solution;

[0044] 3) Slowly add the above-mentioned nitrogen-containing organic phosphonic acid solution into the above-mentioned chitosan solution dropwise at room temperature, continue stirring at room temperature for 12 hours to obtain a mixed solution, and then add 3.5858g of aminosiloxane (3-aminopropyltrimethoxysilane ) was slow...

Embodiment 3

[0049] A preparation method of cross-linked chitosan / nitrogen-containing phosphonic acid group polysiloxane high-temperature proton exchange membrane, the specific steps are as follows:

[0050] 1) At normal temperature, prepare 10 mL of aqueous acetic acid solution with a volume concentration of 1%, dissolve 0.1 g of chitosan powder in the aqueous acetic acid solution, stir fully to make it dissolve uniformly, and obtain a chitosan solution;

[0051] 2) Dissolve 1.6350 g of ethylenediamine tetramethylene phosphonic acid in 10 mL of deionized water, and continue stirring at room temperature for 12 hours to obtain a nitrogen-containing organic phosphonic acid solution;

[0052] 3) Slowly add the above-mentioned nitrogen-containing organic phosphonic acid solution into the above-mentioned chitosan solution dropwise at room temperature, continue stirring at room temperature for 12 hours to obtain a mixed solution, and then add 4.4274g of aminosiloxane (3-aminopropyltriethoxy Sila...

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Abstract

The invention relates to a high-temperature crosslinked chitosan / nitrogenous phosphonic acid polysiloxane proton exchange membrane and a preparation method thereof. The membrane is obtained by the following steps: (1) preparing a chitosan liquid; (2) preparing an organic nitrogenous phosphonic acid liquid; (3) slowly dropwise adding the organic nitrogenous phosphonic acid liquid to the chitosan liquid, fully stirring evenly to obtain a mixed liquid, and slowly dropwise adding amino siloxane to the mixed liquid, so as to obtain a sol liquid; (4) slowly adding an aldehyde crosslinking agent to the sol liquid, and stirring evenly, so as to obtain a gel liquid; and (5) pouring the gel liquid into a polytetrafluoroethylene mold, ageing at a room temperature for 2-3 days, drying at 80 DEG C, then sequentially carrying out heat treatment at 100 DEG C, 120 DEG C and 150 DEG C for 2 hours respectively, cooling and stripping off from the polytetrafluoroethylene mold, so as to obtain the high-temperature crosslinked chitosan / nitrogenous phosphonic acid polysiloxane proton exchange membrane. The preparation method is simple, and mild in reaction condition; the prepared proton exchange membrane has the advantages of relatively high proton conductivity and good heat stability under high-temperature and anhydrous conditions.

Description

technical field [0001] The invention belongs to the technical field of fuel cells, and relates to a cross-linked chitosan / nitrogen-containing phosphonic acid group polysiloxane high-temperature proton exchange membrane and a preparation method thereof. Background technique [0002] A proton exchange membrane fuel cell (PEMFC) is a type of fuel cell system that uses a proton exchange membrane as an electrolyte. This type of fuel cell is also often referred to as a solid polymer fuel cell. The proton exchange membrane is the core component of the fuel cell, which directly affects the performance and life of the battery. Proton exchange membranes for PEMFC need to have high H + It also needs to have good proton conductivity and certain mechanical strength under high temperature and low humidity working conditions. [0003] At present, the commonly used proton exchange membrane materials include polymers such as perfluorosulfonic acid polymers, polyaryletherketones, polyethere...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M8/1041H01M8/1072H01M8/1044H01M8/1069
CPCH01M8/0284H01M8/0286H01M8/1233Y02E60/50
Inventor 高山俊尹珊珊沈春晖李伟李慧琳
Owner WUHAN UNIV OF TECH
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