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Preparation method of cross-linked sulfonated polyarylether proton exchange membrane

A technology of proton exchange membrane and sulfonated polyarylene ether, which is applied in the field of preparation of cross-linked sulfonated polyarylene ether proton exchange membrane, can solve the problems of proton conductivity and anti-oxidative stability decrease, etc., and is conducive to proton transfer. , the synthesis process is simple, the effect of good dimensional stability and chemical stability

Active Publication Date: 2020-12-25
NANJING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Document 3 (Xu et al. Journal of Power Sources, 2015, 492, 505-517.) prepared a series of sulfonated polyarylethersulfone / sulfonated polyvinyl alcohol cross-linked membranes. The cross-linked proton exchange membrane has better Dimensional stability and mechanical properties, but the proton conductivity and anti-oxidation stability have declined. The conductivity of C-SPAEKS / SPVA-30 film (IEC=1.58mmol / g) at 80°C is only 77mS / cm, which is stable by oxidation. Mass loss reaches 11% after sex test

Method used

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  • Preparation method of cross-linked sulfonated polyarylether proton exchange membrane
  • Preparation method of cross-linked sulfonated polyarylether proton exchange membrane
  • Preparation method of cross-linked sulfonated polyarylether proton exchange membrane

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preparation example Construction

[0025] The preparation process of the cross-linked proton exchange membrane of the present invention is as follows: figure 1 , using BP, BHPF, DFBP and SDFDPS, DFDPS, BP as raw materials to prepare fluorine-containing polyarylether polymers and sulfonated polyarylether oligomers through nucleophilic polycondensation reactions, and then using sulfonated oligomers as crosslinking agents Thermal cross-linking reaction with fluorine-containing polymer to prepare cross-linked sulfonated polyarylether proton exchange membrane. Its preparation steps are as follows:

[0026] Step 1, preparation of fluorine-containing random polymer

[0027] Dissolve decafluorobiphenyl (DFBP), 4,4-biphenol (BP), 9,9'-bis(4-hydroxyphenyl)fluorene (BHPF) in N,N-dimethylacetamide ( DMA C ) to form a solution with a solid-to-liquid ratio of 20% to 25%, and add 1.2 to 1.5 times the K relative to the number of hydroxyl moles 2 CO 3 As a catalyst, cyclohexane is used as an azeotropic water-carrying agent...

Embodiment 1

[0038] Preparation of embodiment 1 fluorine-containing random polymer

[0039] In a three-necked flask equipped with a nitrogen gas guiding device, an oil-water separator and a condenser tube, 0.876g (2.5mmol) 9,9'-bis(4-hydroxyphenyl)fluorene (BHPF), 0.464g (2.5mmol) ) 4'4-dihydroxybiphenyl (BP), 1.670g (5mmol) decafluorobiphenyl (DFBP) and 12mL DMAc, after the drug was completely dissolved, add 0.829g (6.00mmol) anhydrous potassium carbonate (K 2 CO 3 ), 10mL cyclohexane, slowly heated up to 90°C for 10h under nitrogen protection, cooled naturally to room temperature, poured the reactant into deionized water to precipitate a white fibrous solid, washed several times with deionized water and ultrasonically placed at 105 °C in a vacuum oven for 24 hours to obtain a fluorine-containing random polymer main chain.

Embodiment 2

[0041] This example is basically the same as Example 1, except that the reaction temperature is 85° C., and the fluorine-containing random polymer is prepared after 12 hours of reaction.

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Abstract

The invention discloses a preparation method of cross-linking sulfonated polyarylether proton exchange membrane. The method comprises the steps of synthesizing a hydrophobic polyarylether high molecular polymer with a high fluorine content via a nucleophilic substitution reaction, synthesizing a -OK terminated hydrophilic sulfonated polyarylether oligomer via the nucleophilic substitution reaction, dissolving the hydrophilic sulfonated oligomer and the hydrophobic fluorine-containing polymer at different mass ratio, performing film formation and hot cross-linking reaction by a solvent castingmethod under a semi-closed condition, taking the sulfonated oligomer as a graft side chain and a cross-linking agent and preparing a series of cross-linking sulfonated polyarylether proton exchange membranes with different ion exchange capacities by a temperature programming method. The method is simple in technology, and controllable in sulfonation degree, and the prepared proton exchange membrane has the advantages of uniform structure, good dimensional stability, good mechanical properties, high proton electroconductivity, good antioxidation stability and the like.

Description

technical field [0001] The invention belongs to the technical field of proton exchange membrane preparation, and relates to a preparation method of a cross-linked sulfonated polyarylether proton exchange membrane. Background technique [0002] As the fifth-generation fuel cell, proton exchange membrane fuel cell (PEMFC) is widely used in mobile power supply, automobile and other fields due to its characteristics of low starting temperature, fast speed, high power density, low corrosion, no electrolyte leakage, and long life. application. The proton exchange membrane is one of the key components of PEMFC, which has the function of insulating electrons and transferring protons, and plays the role of blocking fuel and oxidant. High-quality electrolyte membrane materials should have high ionic conductivity and thermal and chemical stability, excellent mechanical properties and good water absorption and water retention, low cost and achievable preparation process. [0003] Sulf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/22C08J3/24C08L71/10C08G65/40H01M8/1025H01M8/1072B01D71/52
CPCB01D71/52C08G65/40C08J3/24C08J5/2262C08J2371/10H01M8/1025H01M8/1072Y02E60/50
Inventor 胡朝霞张虚略陈守文陆瑶严小波
Owner NANJING UNIV OF SCI & TECH
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