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P-aminobenzene sulfonic acid graphene oxide grafted sulfonated polyetheretherketone proton exchange membrane material and preparation method thereof

A technology for sulfonating polyether ether ketone and p-aminobenzenesulfonic acid, which is applied in the field of p-aminobenzenesulfonic acid grafted sulfonated polyether ether ketone proton exchange membrane material and its preparation, can solve the problem of alcohol permeability coefficient and High water swelling rate, unusable for astronauts, polluting water generated by batteries, etc., to achieve low preparation cost, increase water swelling resistance, and avoid physical loss

Inactive Publication Date: 2015-03-25
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the late 1960s, polystyrene sulfonic acid membrane was first used in PEMFC, but styrene sulfonic acid material has some fatal defects as a proton exchange membrane. It is prone to degradation during use, which not only shortens the battery life , The power density is low, and it also pollutes the generated water of the battery, making it impossible for astronauts to use
However, the SPEEK membrane with high sulfonation degree (DS>90%) has higher proton conductivity, alcohol permeability coefficient and water swelling rate are higher, and even fails due to excessive swelling; while low sulfonation degree (DS<40% ) SPEEK membrane has excellent alcohol resistance and water swelling resistance, but the proton conductivity is low, far inferior to Nafion membrane

Method used

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  • P-aminobenzene sulfonic acid graphene oxide grafted sulfonated polyetheretherketone proton exchange membrane material and preparation method thereof
  • P-aminobenzene sulfonic acid graphene oxide grafted sulfonated polyetheretherketone proton exchange membrane material and preparation method thereof
  • P-aminobenzene sulfonic acid graphene oxide grafted sulfonated polyetheretherketone proton exchange membrane material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Dissolve (1.7000g, 0.0050mol) SPEEK (65% sulfonation degree) in 30 mL of DMAc solvent in a 100 mL three-neck flask equipped with magnetic rotor stirring, condenser, and thermometer, and turn on the magnetic force Stir, and heat the oil bath to 60°C to prepare a film-forming solution;

[0029] (2) Under nitrogen protection, add (0.1892g, 0.0050mol) NaBH at one time to the film-forming solution obtained in step (1) 4 , heated to 100°C for reflux reaction for 12 hours, centrifuged and purified to obtain the supernatant;

[0030] (3) Add graphene oxide (0.08825g) and coupling agent (3.10g, 1.5ml) into toluene (7g, 8ml), and stir mechanically for 12 hours at 100°C under inert gas protection.

[0031] (4) In a 500mL three-neck flask equipped with a magnetic rotor stirring, condenser, and HCl absorption device, put the solution of (3) in DMAc solvent, add the supernatant obtained in step (2) dropwise, and stir in an ice-water bath React for 24 hours.

[0032] (5) In a 5...

Embodiment 2

[0058] (1) Dissolve (3.4000g, 0.0100mol) SPEEK (sulfonation degree 75) in 30 mL of DMAc solvent in a 100 mL three-neck flask equipped with magnetic rotor stirring, condenser, and thermometer, and turn on the magnetic stirring , heat the oil bath to 100°C, and prepare a film-forming solution;

[0059] (2) Under the protection of nitrogen, add (0.3783g, 0.0100mol) NaBH4 to the membrane-forming solution obtained in step (1) at one time, raise the temperature to 90°C for reflux reaction for 18 hours, centrifuge and purify, and obtain the supernatant;

[0060] (3) Add graphene oxide (0.1765g) and coupling agent (6.20g, 0.31ml) into toluene (14g, 16ml), and stir mechanically for 12 hours at 100°C under inert gas protection.

[0061] (4) In a 500mL three-neck flask equipped with a magnetic rotor stirring, condenser, and HCl absorption device, put the solution of (3) in DMAc solvent, add the supernatant obtained in step (2) dropwise, and stir in an ice-water bath React for 24 hours. ...

Embodiment 3

[0073] (1) Dissolve (2.0400g, 0.0060mol) SPEEK (68% sulfonation degree) in 30 mL of DMAc solvent in a 100 mL three-neck flask equipped with magnetic rotor stirring, condenser, and thermometer, and turn on the magnetic stirring , heat the oil bath to 100°C, and prepare a film-forming solution;

[0074] (2) Under the protection of nitrogen, add (0.2270g, 0.0060mol) NaBH4 to the membrane-forming solution obtained in step (1) at one time, heat up to 120°C for reflux reaction for 10 hours, centrifuge and purify, and obtain the supernatant;

[0075] (3) Add graphene oxide (0.26475g) and coupling agent (9.3g, 9ml) into toluene (21g, 24ml), and stir mechanically for 12 hours at 100°C under inert gas protection.

[0076] (4) In a 500mL three-neck flask equipped with a magnetic rotor stirring, condenser, and HCl absorption device, put the solution of (3) in DMAc solvent, add the supernatant obtained in step (2) dropwise, and stir in an ice-water bath React for 24 hours.

[0077] (5) I...

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Abstract

The invention relates to a p-aminobenzene sulfonic acid graphene oxide grafted sulfonated polyetheretherketone proton exchange membrane material. The proton exchange membrane material is characterized by being formed by penetrating p-aminobenzene sulfonic acid graphene oxide grafted-modified sulfonated polyetheretherketone serving as straight chains through epoxy resin cross-linked networks as a main body, wherein the mass ratio of epoxy resin to p-aminobenzene sulfonic acid graphene oxide grafted-modified sulfonated polyetheretherketone is (0.2-1.5): 1. The epoxy resin semi-interpenetrating network p-aminobenzene sulfonic acid graphene oxide grafted sulfonated polyetheretherketone proton exchange membrane material disclosed by the invention has the characteristics of low preparation cost, high electrical conductivity, good methanol diffusion resistance and good heat resistance. At 20 DEG C-90 DEG C, the electrical conductivity is 2.90*10<-3>-5.30*10<-1>S.cm<-1>, methanol-diffusion-resistant coefficient reaches 2.00*10<-7>- 9.00*10<-7>cm<2>.s<-1> and the water absorption rate is 12-100%.

Description

technical field [0001] The invention relates to an epoxy resin semi-interpenetrating network p-aminobenzenesulfonic acid graphene oxide grafted sulfonated polyether ether ketone proton exchange membrane material and a preparation method thereof. Background technique [0002] Today, when the main task is to promote green development, circular development, and low-carbon development, it has become an inevitable trend of scientific research to improve energy utilization efficiency and develop clean energy. Fuel cell (DMFC) has been developed and applied in many fields due to its environmental protection, energy saving, high efficiency, and convenient use. [0003] In the fuel cell, the proton exchange membrane is the core component of the MEA. In terms of the selection of materials used, the research is mainly carried out from the aspects of proton conductivity, chemical stability, and mechanical properties. In the late 1960s, polystyrene sulfonic acid membrane was first used ...

Claims

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Application Information

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IPC IPC(8): C08L71/08C08L63/00C08J5/22C08G59/50C08G65/48C08K3/38
Inventor 郭强张天骄毕宸洋余舟尹泽辉张豪东
Owner SHANGHAI UNIV
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