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Method for preparing composite proton-conducting film from branched and sulfonated polyimide/two-dimensional layered material

A technology of sulfonated polyimide and proton conductive membrane, which is applied to fuel cell components, electrolyte holding devices, etc., can solve the problems of weak oxidation resistance and low vanadium resistance performance, and achieve low cost and strong resistance Oxidation property, effect of improving proton conductivity and chemical stability

Inactive Publication Date: 2016-10-12
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention aims to overcome the disadvantages of weak anti-oxidation ability and low vanadium resistance performance of non-fluorine polymer SPI membrane, and adds layered materials to the synthesized branched sulfonated polyimide to prepare branched sulfonated polyimide Imine / two-dimensional layered material composite proton conducting membrane, the prepared composite proton conducting membrane effectively compensates for the defect of high vanadium ion permeability of the branched membrane, and the addition of inorganic materials effectively improves the proton conductivity and chemical Stability, potential application in the field of VRFB

Method used

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  • Method for preparing composite proton-conducting film from branched and sulfonated polyimide/two-dimensional layered material
  • Method for preparing composite proton-conducting film from branched and sulfonated polyimide/two-dimensional layered material
  • Method for preparing composite proton-conducting film from branched and sulfonated polyimide/two-dimensional layered material

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Embodiment 1

[0031] A preparation method of a branched sulfonated polyimide / two-dimensional layered material composite proton conductive membrane, the steps of which are:

[0032] in N 2 Under protection, add 8.0mmol NTDA, 20mL m-cresol, and 9.8mmol benzoic acid into a 250mL three-neck flask, and stir continuously at room temperature until NTDA and benzoic acid are completely dissolved; dissolve 2.0mmol BDSA in a 50mL m- Add 5.0mmol triethylamine dropwise to cresol, wait until BDSA is completely dissolved, then add 1.0mmol ODA and 3.3mmol TAPOB into the beaker to dissolve completely, and place it in a constant pressure dropping funnel and slowly drop it into a three-necked flask. And the temperature was raised to 50°C for 15 hours to obtain a branched SPI film solution; take 750 mg of layered material and disperse it in 100 mL of NMP, ultrasonicate in a water bath for 2 hours, and the ultrasonic power was 200 W, and after centrifugal sedimentation at 1500 r / ppm for 90 minutes, take the upp...

Embodiment 2

[0037] A preparation method of a branched sulfonated polyimide / two-dimensional layered material composite proton conductive membrane, the steps of which are:

[0038] in N 2 Under protection, add 8.0mmol NTDA, 30mL m-cresol, and 9.8mmol benzoic acid into a 250mL three-neck flask, and stir continuously at room temperature until NTDA and benzoic acid are completely dissolved; Add 5.0mmol triethylamine dropwise to cresol, wait until BDSA is completely dissolved, then add 1.0mmol ODA and 2.67mmol TAPOB into the beaker to dissolve completely, and place it in a constant pressure dropping funnel and slowly drop it into a three-necked flask. And the temperature was raised to 50°C for 20 hours to obtain a branched SPI film solution; take 750 mg of layered material and disperse it in 100 mL of NMP, ultrasonicate in a water bath for 2 hours, and the ultrasonic power was 200 W, and after centrifugal sedimentation at 1500 r / ppm for 90 minutes, take the upper Clear solution, and slowly add...

Embodiment 3

[0043] A preparation method of a branched sulfonated polyimide / two-dimensional layered material composite proton conductive membrane, the steps of which are:

[0044] in N 2 Under protection, add 8.0mmol NTDA, 30mL m-cresol, and 14.7mmol benzoic acid into a 250mL three-neck flask, and stir continuously at room temperature until NTDA and benzoic acid are completely dissolved; dissolve 4.0mmol BDSA in a 70mL m- Add 5.0mmol triethylamine dropwise to cresol, wait until BDSA is completely dissolved, then add 2.0mmol ODA and 1.33mmol TAPOB into the beaker to dissolve completely, and place it in a constant pressure dropping funnel and slowly drop it into a three-necked flask. And raise the temperature to 50°C for 20 hours to obtain a branched SPI membrane solution; take 375 mg of layered material and disperse it in 50 mL of NMP, ultrasonicate in a water bath for 2 hours, and the ultrasonic power is 200 W, and then centrifugally settle at 1500 r / ppm for 90 minutes to take the upper C...

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Abstract

The invention discloses a method for preparing a composite proton-conducting film from branched and sulfonated polyimide / a two-dimensional layered material. The method is characterized in that under the protection of nitrogen, m-cresol, 1,4,5,8-naphthalenetetracarboxylic dianhydride and benzoic acid are put into a reactor; m-cresol, benzidine-2,2'-disulfonic acid and triethylamine are mixed until solids are dissolved, 1,3,5-tri(4-aminophenoxy)benzene and 4,4'-diaminodiphenyl ether are added and stirred until solids are dissolved, and the mixture is added dropwise to the reactor, heated to 40-100 DEG C and subjected to a reaction for 15-24 h; the two-dimensional layered material is dispersed in a dispersing agent, added dropwise to the reactor and subjected to a stirring reaction for 20-24 h, and a reacted material is poured to a glass plate for film casting and is dried; the film is immersed and washed, and the composite proton-conducting film is prepared. The composite proton-conducting film prepared with the method has good performance and is applicable to fields such as vanadium redox batteries, hydrogen-oxygen fuel cells, direct methanol fuel cells and the like.

Description

technical field [0001] The invention belongs to the preparation of a battery separator, and relates to a preparation method of a branched sulfonated polyimide / two-dimensional layered material composite proton conductive membrane. The branched sulfonated polyimide / two-dimensional layered material composite proton conductive membrane prepared by the invention is suitable for the fields of all-vanadium redox flow battery, hydrogen-oxygen fuel cell, direct methanol fuel cell and the like. Background technique [0002] Facing the growing population, energy shortage is an important problem facing the world today, and it is imminent to find new energy sources that can replace traditional energy sources. Therefore, vigorously developing new renewable energy sources such as solar energy, tidal energy, and wind energy has become the basic national policy of my country's energy development. However, such new renewable energy sources are easily affected by external conditions (such as ...

Claims

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Application Information

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IPC IPC(8): C08J7/02C08J7/00C08J5/22C08L79/08C08K3/30C08K3/38C08G73/10H01M8/0289
CPCC08G73/1071C08J5/2256C08J7/00C08J7/02C08J2379/08C08K3/30C08K3/38C08K2003/3009C08K2003/385C08K2201/011C08L2201/08H01M8/0289C08L79/08Y02E60/50
Inventor 张亚萍蒲阳张帅黄小东周雨芹
Owner SOUTHWEAT UNIV OF SCI & TECH
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