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Organic covalent grafting-based heteropolyacid hybrid perfluorosulfonic acid membrane and preparation method and application thereof

A technology of perfluorosulfonic acid membrane and covalent grafting, which is applied in the field of heteropolyacid hybrid perfluorosulfonic acid membrane and its preparation, can solve the problems of reducing the overall conductivity of the membrane, heteropolyacid leakage, and reducing

Active Publication Date: 2022-01-28
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, although the heteropolyacid hybrid perfluorosulfonic acid membrane exhibits excellent performance of enhanced conductivity, the heteropolyacid will be eluted from the membrane in the presence of a solvent, resulting in the leakage of the heteropolyacid from the membrane.
However, the current strategies to reduce the elution of heteropolyacids by immobilizing them on the polymeric organic matrix in the membrane through cross-linking or grafting reactions will lead to a strong decrease in membrane hydration behavior, thereby reducing the overall conductivity of the membrane.

Method used

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  • Organic covalent grafting-based heteropolyacid hybrid perfluorosulfonic acid membrane and preparation method and application thereof
  • Organic covalent grafting-based heteropolyacid hybrid perfluorosulfonic acid membrane and preparation method and application thereof

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preparation example Construction

[0021] The invention provides a method for preparing a heteropolyacid hybrid perfluorosulfonic acid membrane, comprising the following steps:

[0022] mixing polyethylene glycol monomethyl ether, chloromethyl trimethoxysilane, sodium hydride and the first polar organic solvent, and performing a nucleophilic reaction to obtain polyethylene glycol monomethyl ether trimethoxysilane;

[0023] Mix the polyethylene glycol monomethyl ether trimethoxysilane, the deficient heteropolyacid, the acid and the second polar organic solvent, and perform a substitution reaction to obtain a potassium-type organic covalently grafted heteropolyacid; the deficient The heteropolyacid is a Keggin-type absent heteropolyacid;

[0024] Using a hydrogen-type ion exchange resin as a stationary phase and a third polar organic solvent as a mobile phase, replacing the potassium-type organic covalently grafted heteropolyacid to obtain a hydrogen-type organic covalently grafted heteropolyacid;

[0025] The s...

Embodiment 1

[0059] Add 50mL tetrahydrofuran and 5mL polyethylene glycol monomethyl ether (molecular weight 450g / mol) (12mmol) into a round bottom flask, add 0.35g (14.6mmol) sodium hydride, then add 2.2mL (14.5mmol) chloromethyltrimethyl Oxysilane, stirred and reacted at 40°C for 8h; centrifuged the reacted solution at a speed of 10,000r / min for 15min, rotated the obtained supernatant at 40°C under vacuum, and added the obtained liquid dropwise to petroleum In ether, the volume ratio of sherwood oil and liquid product is 100:1, layering, and the gained lower layer is polyethylene glycol monomethyl ether trimethoxysilane;

[0060] Add 3.3g (1mmol) vacant silicotungstic acid into a round bottom flask, add 5mmol hydrochloric acid (1mol / L), 50mL acetonitrile and 1mL (2.1mmol) polyethylene glycol monomethyl ether trimethoxysilane, and react at room temperature for 8 hours , filter the product, and remove the acetonitrile solvent by rotary evaporation at 50°C under vacuum conditions to obtain p...

Embodiment 2

[0064] Prepare hydrogen-type organic covalent grafted silicotungstic acid according to the method of Example 1;

[0065] Dissolve 0.1g Nafion film in 1.5mL DMAc solvent, stir to dissolve, then add 2mg of hydrogen-form organic covalent grafted silicotungstic acid, stir to dissolve; cast the resulting mixture at 80°C to form a film, and dry at 80°C for 12 Hours, a heteropolyacid hybrid perfluorosulfonic acid film was obtained with a film thickness of 80±3 μm, in which the hybrid mass fraction of organic covalently grafted silicotungstic acid was 2%.

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Abstract

The invention provides a heteropolyacid hybrid perfluorosulfonic acid membrane based on organic covalent grafting and a preparation method and application thereof, and belongs to the technical field of fuel cell proton exchange membranes. Polyethylene glycol monomethyl ether and chloromethyl trimethoxy silane are used as raw materials to prepare polyethylene glycol monomethyl ether trimethoxy silane, then a polymer chain is grafted on Keggin type vacancy heteropolyacid, and the polymer chain grafted on the heteropolyacid can interact with a sulfonate radical in a perfluorosulfonic acid membrane to form a hydrogen bond; the heteropoly acid can be stably immobilized in the perfluorosulfonic acid membrane through the acting force, so that the heteropoly acid cannot be eluted and leaked by a solvent while the conductivity of the membrane is enhanced, the problem that the heteropoly acid is difficult to be stably immobilized in the perfluorosulfonic acid membrane is solved, and the hybrid proton exchange membrane with high stability and high proton conductivity is obtained.

Description

technical field [0001] The invention relates to the technical field of fuel cell proton exchange membranes, in particular to a heteropolyacid hybrid perfluorosulfonic acid membrane based on organic covalent grafting and its preparation method and application. Background technique [0002] Currently, one of the most promising clean energy devices is the proton exchange membrane fuel cell (PEMFC). The proton exchange membrane (PEM) is the "heart" of the fuel cell, which determines the power of the fuel cell. Although there are various structures of proton exchange membranes, the most widely used proton exchange membranes in proton exchange membrane fuel cells are perfluorinated membranes. The Nafion series perfluorosulfonic acid membrane produced by DuPont is the most widely used and is used as a reference for all proton exchange membranes. Compared with other membranes, Nafion membrane has higher proton conductivity value and chemical stability. [0003] Currently, heterop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M8/0284H01M8/0271H01M8/1004H01M8/1067C08G65/338C08G65/336C08G65/328
CPCH01M8/0284H01M8/0271H01M8/1067H01M8/1004C08G65/338C08G65/336C08G65/328H01M2008/1095Y02E60/50
Inventor 李昊龙赫海博
Owner JILIN UNIV
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