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Phosphate siloxane high-temperature proton exchange membrane with hydrolytic stability and preparation method thereof

A technology of phosphate-based siloxane and proton exchange membrane, which is applied in the field of phosphate-based siloxane high-temperature proton exchange membrane and its preparation, can solve the problems of low hydrolytic stability and decreased proton conductivity, and achieve good hydrolytic stability , Improve the effect of proton conductivity

Inactive Publication Date: 2015-11-11
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this reaction process is simple and easy to operate, the hydrolytic stability of the formed C-O-P bond is not high, and phosphoric acid will flow away with the water generated during the operation of the fuel cell, resulting in a decrease in the proton conductivity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A hydrolytically stable phosphate-based siloxane high-temperature proton exchange membrane, prepared by the following method:

[0024] (1) According to phosphoroacetic acid: oxalyl chloride: aminosiloxane: the molar ratio of tetraethoxysilane is 1:1:2:1 and takes raw material;

[0025] (2) Dissolve 1 mmol of phosphoroacetic acid in 5 ml of dichloromethane, and put it into a four-necked flask equipped with a stirrer, reflux condenser, dropping funnel and tail gas absorption device, slowly add 1 mmol dropwise at room temperature Oxalyl chloride was stirred and reacted for 3h, and the product was obtained by distillation under reduced pressure;

[0026] (3) Dissolve 2mmol of 3-aminopropyltriethoxysilane in 10ml of dichloromethane, and put it into a four-neck flask equipped with a stirrer, reflux condenser, dropping funnel and tail gas absorption device, add 6mmol Triethylamine, the product obtained in step (2) was dissolved in dichloromethane, and slowly added dropwise in...

Embodiment 2

[0030] A hydrolytically stable phosphate-based siloxane high-temperature proton exchange membrane, prepared by the following method:

[0031] (1) Take raw materials according to the molar ratio of phosphoroacetic acid: oxalyl chloride: aminosiloxane: tetraethoxysilane is 1:1.5:2:3;

[0032] (2) Dissolve 1mmol of phosphoroacetic acid in 5ml of dichloromethane, and put it into a four-necked flask equipped with a stirrer, reflux condenser, dropping funnel and tail gas absorption device, and slowly add 1.5 mmol oxalyl chloride was stirred and reacted for 5h, and the product was obtained by distillation under reduced pressure;

[0033] (3) Dissolve 2mmol of 3-aminopropyltriethoxysilane in 10ml of dichloromethane, and put it into a four-neck flask equipped with a stirrer, reflux condenser, dropping funnel and tail gas absorption device, add 6mmol Triethylamine, the product obtained in step (2) was dissolved in dichloromethane, and slowly added dropwise in a four-necked flask, stirr...

Embodiment 3

[0037] A hydrolytically stable phosphate-based siloxane high-temperature proton exchange membrane, prepared by the following method:

[0038] (1) Take the raw material according to the molar ratio of phosphoroacetic acid: oxalyl chloride: aminosiloxane: tetraethoxysilane is 1:1.5:3:3;

[0039] (2) Dissolve 1mmol of phosphoroacetic acid in 5ml of dichloromethane, and put it into a four-necked flask equipped with a stirrer, reflux condenser, dropping funnel and tail gas absorption device, and slowly add 1.5 mmol oxalyl chloride was stirred and reacted for 4h, and the product was obtained by distillation under reduced pressure;

[0040] (3) Dissolve 3mmol of 3-aminopropyltriethoxysilane in 10ml of dichloromethane, and put it into a four-necked flask equipped with a stirrer, reflux condenser, dropping funnel and tail gas absorption device, add 3mmol 4-dimethylaminopyridine, the product obtained in step (2) was dissolved in dichloromethane, and slowly added dropwise in a four-neck...

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Abstract

The invention belongs to the technical field of fuel cells and particularly relates to a phosphate siloxane high-temperature proton exchange membrane with hydrolytic stability and a preparation method thereof. The preparation method of the proton exchange membrane comprises the following steps: firstly, carrying out acylation reaction between phosphonoacetic acid and oxalyl chloride to obtain phosphoryl chloride; then, carrying out amidation reaction between phosphoryl chloride and amino siloxane to obtain phosphate siloxane; and finally, hydrolyzing and cross-linking phosphate siloxane and tetraethoxysilane together, and preparing a membrane through a sol-gel process. According to the invention, reaction conditions are relatively mild, the preparation process is simple, phosphoric acid in the prepared proton exchange membrane exists in the membrane in a form of C-P bonds, and the hydrolytic stability is better.

Description

technical field [0001] The invention belongs to the technical field of fuel cells, and in particular relates to a hydrolytically stable phosphate-based siloxane high-temperature proton exchange membrane and a preparation method thereof. Background technique [0002] Proton exchange membrane is the key material in proton exchange membrane fuel cells, it plays an important role in blocking fuel gas and oxygen or air, conducting protons, and attaching electrocatalysts. An ideal proton exchange membrane material must have good barrier properties to fuel gas and oxygen or air, have excellent physical and chemical stability, and have high proton conductivity. [0003] At present, phosphate-based siloxane proton exchange membrane is a research hotspot. Phosphoric acid is a kind of amphoteric acid, which can be used as both a proton donor and a proton acceptor, and has a high proton self-detachment ability. group, through the formation and breaking of intermolecular dynamic hydroge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/30C08J5/22H01M8/10
CPCY02E60/50Y02P70/50
Inventor 沈春晖李伟高山俊尹珊珊李慧琳
Owner WUHAN UNIV OF TECH
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