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Preparation method of direct crosslinking proton exchange membrane

A proton exchange membrane and cross-linking technology, applied in chemical instruments and methods, membrane technology, organic membranes, etc., can solve problems such as poor controllability of sulfonation degree, complicated process, and polymer main chain breakage, etc., to avoid Molecular chain breaks, simple synthesis process, and good water stability

Inactive Publication Date: 2010-02-10
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process of this method is very complicated. Due to the post-sulfonation treatment, the controllability of the sulfonation degree is poor, and the post-sulfonation treatment easily leads to the breakage of the polymer main chain.

Method used

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  • Preparation method of direct crosslinking proton exchange membrane
  • Preparation method of direct crosslinking proton exchange membrane
  • Preparation method of direct crosslinking proton exchange membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Synthesis of SDFDPS / DFDPS-THB (5 / 5-5%) polymer, crosslinking agent THB content is 5%, IEC=2.11mmol / g

[0065] Add 2.051g (4.475mmol) SDFDPS, 1.138g (4.475mmol) DFDPS, 1.542g (8.278mmol) BP and 0.056g (0.448mmol) THB into a constant pressure Add 24ml of DMSO to the dropping funnel and the four-necked flask with nitrogen inlet and outlet, and after it is completely dissolved, add 1.422g of anhydrous potassium carbonate and 12ml of anhydrous toluene. The temperature was raised to 140° C. for 4 hours, and the water produced in the reaction was removed by constant boiling with toluene. Then the temperature was raised to 165° C., and 12 ml of anhydrous toluene was added dropwise through a constant pressure dropping funnel. React for 8 hours. After the reaction, add about 20ml of DMAc to dilute, lower the temperature, pour into about 500ml of pure water, precipitate fibrous products, wash thoroughly with water, and vacuum dry at 100°C for 24 hours to obtain a directly cross-...

Embodiment 2

[0068] Preparation of SFDFDPS / DFDPS-THB (5 / 5-5%) proton-type membrane (M1).

[0069] Weigh 2.0 g of SFDFDPS / DFDPS-THB (5 / 5-5%) polymer, add 50 ml of DMSO, and heat to dissolve. After filtration, it was poured on a glass plate. Dry at 80°C, 100°C, and 120°C for 2 hours respectively, and then rise to 140°C for 20 hours. Take it out, soak it in water and peel it off, soak it in water for 24 hours, then exchange it with 2M hydrochloric acid solution for 72 hours, take it out, and wash it with water for 48 hours. It was taken out and dried at 150° C. for 2 hours to obtain a proton type sulfonated polymer membrane.

[0070] Its performance data is shown in Table 1, and the conductivity under different relative humidity is shown in figure 2 .

Embodiment 3

[0072] Synthesis of SDFDPS / DFDPS-THB (6 / 4-5%) polymer, crosslinking agent THB content 5%, IEC=2.43mmol / g

[0073] Add 1.902g (4.149mmol) of SDFDPS, 0.703g (2.766mmol) of DFDPS, 1.192g (6.397mmol) of BP and 0.044g (0.346mmol) of THB into a tank equipped with a stirring device, an oil-water separator, a reflux condenser, and a constant pressure drop Add 19ml of DMSO to the liquid funnel and the four-neck flask with nitrogen inlet and outlet, and after it is completely dissolved, add 1.099g of anhydrous potassium carbonate and 10ml of anhydrous toluene. The temperature was raised to 140° C. for 4 hours, and the water produced in the reaction was removed by constant boiling with toluene. Then the temperature was raised to 165° C., and 10 ml of anhydrous toluene was added dropwise through a constant pressure dropping funnel. React for 8 hours. After the reaction, add about 15ml of DMAc to dilute, lower the temperature, pour into about 500ml of pure water, precipitate fibrous prod...

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Abstract

The invention discloses a preparation method of a direct crosslinking proton exchange membrane. The preparation method comprises the following steps: adding a sulfonated dihalogen compound, a non-sulfonated dihalogen compound, a dihydroxy compound and a crosslinking agent to a four-mouth flask with a stirring device, an oil-water separator, a reflux condensing tube, a constant-pressure drop funnel, a nitrogen inlet and a nitrogen outlet; adding an aprotic polar organic solvent until being fully dissolved; adding potassium carbonate and then adding anhydrous toluene; increasing temperature andreacting for 4-6 hours; removing water generated in the reaction; increasing the temperature to 150-190 DEG C and reacting for 4-30 hours; decreasing the temperature; diluting by the aprotic polar organic solvent; pouring into water, acetone or ethanol to separate out fibroid products; filtering, washing and drying to obtain a direct crosslinking sulfonated polymer product; dissolving the obtainedproduct into the aprotic polar organic solvent; casting and drying; and obtaining a proton polymer membrane after acid exchange. The method has simple process, and the prepared product has good stability and high conductivity.

Description

technical field [0001] The invention relates to a preparation method mainly used as an electrolyte membrane in a fuel cell, and can also be used as an electrolyte membrane in the salinization industry, in particular to a preparation method of a direct cross-linked proton exchange membrane. Background technique [0002] Sulfonated polymer membranes are widely used in fuel cells, chlor-alkali industry, ion exchange resins, membrane separation technology and humidity sensors. [0003] In a proton exchange membrane fuel cell, the proton exchange membrane is one of the key components. Currently commercially available proton exchange membranes are perfluorosulfonic acid polymer membranes, such as DuPont's Nafion series, which have the advantages of high electrical conductivity and excellent chemical stability. However, the high price, low working temperature, high methanol permeability and environmental problems caused by fluorine-containing materials limit its commercial applica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/22C08L71/10C08G65/40B01D71/52C25B13/08C25B1/46H01M8/02H01M2/16H01M8/1072
CPCY02E60/12Y02E60/50
Inventor 陈守文王连军毕慧平张轩王佳力孙秀云
Owner NANJING UNIV OF SCI & TECH
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