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Side-chain sulfonic acid type polyarylether, preparation method thereof and application of polyarylether in preparation of proton exchange membrane

A technology of polyarylether and chain sulfonic acid, which is applied in the field of polymer functional materials, can solve the problems of polymers losing mechanical properties, polymer swelling rate is serious, and polymer phase separation is not obvious enough, etc.

Inactive Publication Date: 2012-07-18
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Current studies have found that there are still some problems to be solved for this kind of material, that is, the degree of hydrophilicity and hydrophobicity in the microphase structure of this kind of material is not as good as that of perfluorosulfonic acid membrane, resulting in insufficient obvious phase separation of the polymer
If the degree of sulfonation is increased to increase the concentration of sulfonic acid groups in the polymer to increase the conductivity of the polymer, the swelling rate of the polymer will be very serious at higher temperatures, resulting in the loss of mechanical properties of the polymer.

Method used

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  • Side-chain sulfonic acid type polyarylether, preparation method thereof and application of polyarylether in preparation of proton exchange membrane
  • Side-chain sulfonic acid type polyarylether, preparation method thereof and application of polyarylether in preparation of proton exchange membrane
  • Side-chain sulfonic acid type polyarylether, preparation method thereof and application of polyarylether in preparation of proton exchange membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: Preparation of 4-(3-(4-(2,6-difluorobenzoyl)phenoxy)propoxy)sodium benzenesulfonate difluorosulfonated monomer

[0024] Put 4-(2,6'-difluorophenylcarbonyl) diphenylpropyl ether (10g) into 30mL concentrated sulfuric acid solution with a mass fraction of 95-98% at 50°C, stir for 4h; then discharge in 100ml neutralized with 1 mol / l sodium hydroxide solution to pH=7, and filtered to obtain a white solid. After recrystallization, sodium 4-(3-(4-(2,6-difluorobenzoyl)phenoxy)propoxy)benzenesulfonate difluorosulfonated monomer was obtained with a yield of 40%. FT-IR (KBr: 1 034cm -1 (-SO 3 Na), 1660cm -1 (C=O), 1257cm -1 (C-O-C). 1 H NMR (300MHz, DMSO) δ7.78(d, J=8.4Hz, 2H), 7.65(d, J=7.1Hz, 1H), 7.52(d, J=8.3Hz, 2H), 7.30(t, J =8.1Hz, 2H), 7.14(d, J=8.7Hz, 2H), 6.88(d, J=8.5Hz, 2H), 4.26(t, J=5.9Hz, 2H), 4.14(t, J=5.7 Hz, 2H), 2.41-1.98 (m, 2H).

Embodiment 2

[0025] Embodiment 2: the preparation of polymer PAEK-1

[0026] In a three-neck flask equipped with a stirrer, a water dispenser and a nitrogen port, add 10 mmol of 4,4'-dihydroxydiphenyl ether, 7.36 mmol of 4-(3-(4-(2,6-difluoro Benzoyl)phenoxy)propoxy)sodium benzenesulfonate, 2.64mmol of 4,4'-difluorobenzophenone, 11mmol of anhydrous potassium carbonate, 40ml of sulfolane and 8ml of toluene were put into the three-necked flask In the process, nitrogen gas was passed, and the temperature was raised to 120°C. Reflux with water for 2 hours, steam the dehydrating agent, raise the temperature to 175°C and react for 6 hours, then pour the reaction mixture into water to obtain a polymer, then crush it into particles of about 10 mesh with a pulverizer, and then filter it with a Buchner funnel for more After washing with deionized water and ethanol, vacuum drying at 100° C. for 12 hours yielded polymer PAEK-1 with a yield of over 90%. Its sulfonation degree is 0.74 and its glass tr...

Embodiment 3

[0027] Embodiment 3: the preparation of the PAEK-2 of polymer

[0028]In a three-neck flask equipped with a stirrer, a water vessel and a nitrogen port, add 10 mmol of 4,4'-dihydroxydiphenyl ether, 8.1 mmol of 4-(3-(4-(2,6-difluoro Benzoyl)phenoxy)propoxy)sodium benzenesulfonate, 1.9mmol of 4,4'-difluorobenzophenone, 11mmol of anhydrous potassium carbonate, 45ml of sulfolane and 9ml of toluene were put into the three-necked flask In the process, nitrogen gas was passed, and the temperature was raised to 120°C. Reflux with water for 2 hours, steam the dehydrating agent, raise the temperature to 175°C and react for 6 hours, then pour the reaction mixture into water to obtain a polymer, then crush it into particles of about 10 mesh with a pulverizer, and then filter it with a Buchner funnel for more After washing with deionized water and ethanol, vacuum drying at 100° C. for 12 hours yielded polymer PAEK-2 with a yield of over 90%. Its degree of sulfonation is 0.81, and its gla...

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Abstract

The invention belongs to the technical field of high polymer materials and relates to a side-chain sulfonic acid type polyarylether polymer which has high thermal stability and is used in a proton exchange membrane of a fuel cell and a preparation method thereof. The preparation method comprises the following steps: adding a diphenol monomer, a sulfonated difluoro-monomer, a difluoro-monomer and anhydrous potassium carbonate in a three-necked bottle provided with a stirrer, a water-carrying device and a nitrogen hole, adding a solvent and an azeotropic dehydrant which accounts for 20% of the solvent by volume in the three-necked bottle, injecting nitrogen, and heating to reflux the azeotropic dehydrant; and refluxing for 2-5h to dehydrate, evaporating the azeotropic dehydrant, heating to 175-190 DEG C to react for 5-8h, then pouring the reaction mixture in water to obtain a polymer, grinding the polymer to fine particles by using a grinder, filtering by using a buchner funnel, washingwith deionized water and ethanol several times, and performing vacuum drying at 100-110 DEG C for 10-15h to obtain the side-chain sulfonic acid type polyarylether polymer with high thermal stability,good solubility and film-forming property and low water absorption rate.

Description

technical field [0001] The invention belongs to the technical field of polymer functional materials, and in particular relates to a side-chain sulfonic acid type polyarylether polymer with high thermal stability used for fuel cell proton exchange membranes and a preparation method thereof. Background technique [0002] Proton exchange membrane fuel cell, also known as polymer electrolyte membrane fuel cell, has the advantages of high energy conversion rate, low temperature start-up, no electrolyte leakage, no corrosion, and long life due to the use of polymer membrane as a solid electrolyte. It is recognized as the most promising power source for aerospace, military, electric vehicles and regional power stations. As the key part of the proton exchange membrane fuel cell, the proton exchange membrane plays the role of isolating the contact between the oxidant and the fuel, and as a proton carrier to complete the proton transfer. Its performance determines the performance of t...

Claims

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Application Information

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IPC IPC(8): C08G65/40C08J5/22C08L71/10H01M8/02H01M2/16H01M8/1016H01M8/102H01M8/1069
CPCY02E60/12Y02E60/50
Inventor 姜振华张强刘佰军庞金辉
Owner JILIN UNIV
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