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Preparation method of cross-linked polyfluorene piperidine anion exchange membrane

A technology of anion exchange membrane and polyfluorene piperidine, which is applied in the field of preparation of cross-linked polyfluorene piperidine anion exchange membrane, and can solve problems such as battery performance decline.

Active Publication Date: 2021-06-08
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to the recent results of Maurya et al. exploring polyphenylpiperidinyl AEMFC, polyphenylpiperidine will be oxidized to phenol in a strong oxidative environment, resulting in a decrease in battery performance.

Method used

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  • Preparation method of cross-linked polyfluorene piperidine anion exchange membrane

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Experimental program
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Embodiment 1

[0037] A cross-linked polyfluorene piperidine anion exchange membrane, the preparation method steps are as follows:

[0038] In a 50ml flask, 1.56g of 9,9-dimethylfluorene was added, 0.768ml of N-methylpiperidone and 0.394ml of trifluoroacetone were added. Add 2ml dichloromethane, 0.65ml trifluoroacetic acid, 8ml trifluoromethanesulfonic acid, N 2 Protect. Speed ​​up the rotor speed and react at 0°C for 36h. Pour the reaction solution into 1mol / L K 2 CO 3 The aqueous solution was precipitated, and the precipitate was washed 3-5 times with deionized water to obtain a light yellow solid named PBBP-2 (molecular weight 289). Weigh a certain amount of fully dried 1.22g of 1,6-dibromohexane and dissolve it in 15mL of dimethyl sulfoxide, and wait until it is completely dissolved. Slowly add 0.586ml of 3-aminopropyltriethoxysilane (APTES) dropwise under ice-water bath environment, continue to 2 Stirring and reacting at room temperature under atmosphere for 12 hours. A colorless...

Embodiment 2

[0040] A cross-linked polyfluorene piperidine anion exchange membrane, the preparation method steps are as follows:

[0041] In a 50ml flask, 1.56g of 9,9-dimethylfluorene was added, 0.768ml of N-methylpiperidone and 0.394ml of trifluoroacetone were added. Add 2ml dichloromethane, 0.65ml trifluoroacetic acid, 8ml trifluoromethanesulfonic acid, N 2 Protect. Speed ​​up the rotor speed and react at 0°C for 36h. Pour the reaction solution into 1mol L -1 K 2 CO 3 The aqueous solution was precipitated, and the precipitate was washed 3-5 times with deionized water to obtain a light yellow solid named PBBP-2 (molecular weight 289). Weigh a certain amount of fully dried 1.22g of 1,6-dibromohexane and dissolve it in 15mL of dimethyl sulfoxide, and wait until it is completely dissolved. Slowly add 0.586ml of 3-aminopropyltriethoxysilane (APTES) dropwise under ice-water bath environment, continue to 2 Stirring and reacting at room temperature under atmosphere for 12 hours. A color...

Embodiment 3

[0043] A cross-linked polyfluorene piperidine anion exchange membrane, the preparation method steps are as follows:

[0044] In a 50ml flask, 1.56g of 9,9-dimethylfluorene was added, 0.768ml of N-methylpiperidone and 0.394ml of trifluoroacetone were added. Add 2ml dichloromethane, 0.65ml trifluoroacetic acid, 8ml trifluoromethanesulfonic acid, N 2 Protect. Speed ​​up the rotor speed and react at 0°C for 36h. Pour the reaction solution into 1mol / L K 2 CO 3 The aqueous solution was precipitated, and the precipitate was washed 3-5 times with deionized water to obtain a light yellow solid named PBBP-2 (molecular weight 289). Weigh a certain amount of fully dried 1.22g of 1,6-dibromohexane and dissolve it in 15mL of dimethyl sulfoxide, and wait until it is completely dissolved. Slowly add 0.586ml of 3-aminopropyltriethoxysilane (APTES) dropwise under ice-water bath environment, continue to 2 Stirring and reacting at room temperature under atmosphere for 12 hours. A colorless...

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Abstract

The invention discloses a preparation method of a cross-linked polyfluorene piperidine anion exchange membrane. The method comprises the following steps: dissolving 9,9-dimethyl fluorene, N-methyl piperidone and trifluoroacetone in dichloromethane to obtain a homogeneous solution, adding trifluoroacetic acid and trifluoromethanesulfonic acid as catalysts, performing reacting for 24-36 hours at 0-10 DEG C in a nitrogen atmosphere, performing precipitating with a K2CO3 aqueous solution, and performing washing with deionized water to obtain light yellow solid polyfluorene piperidine polymer powder; dissolving the obtained polyfluorene piperidine and iodomethane in chloroform, performing heating and refluxing for 24-36 hours under a dark condition and a nitrogen atmosphere, then pouring a reaction solution into diethyl ether to precipitate, and performing washing with deionized water to obtain a quaternized polyfluorene piperidine polymer; and dissolving the obtained solution in dimethyl sulfoxide, adding a brominated amino siloxane cross-linking agent solution, performing reacting for 12-24 hours at 50-60 DEG C, adding iodomethane, performing reacting for 24-48 hours at 30-40 DEG C in a dark nitrogen atmosphere, adding ethanol, performing standing for 24-36 hours at room temperature, performing standing for 12-24 hours at 80 DEG C, standing for 3-6 hours at 100 DEG C, and performing standing for 1-3 hours at 120 DEG C to obtain the cross-linking type polyfluorene piperidine anion exchange membrane.

Description

technical field [0001] The invention belongs to the technical field of fuel cells, and in particular relates to a preparation method of a cross-linked polyfluorene piperidine anion exchange membrane. Background technique [0002] Anion exchange membrane (AEM) is a high molecular polymer membrane containing cationic functional groups, which is selectively permeable to anions. The anion exchange membrane fuel cell is in an alkaline environment, through the oxidation of fuel at the anode and the reduction of oxygen at the cathode, the anion exchange membrane isolates the anode and cathode and conducts OH- ions, and the external collector collects electrons to realize the conversion of chemical energy and electrical energy. Alkaline anion exchange membrane fuel cell (AAEMFC) has the advantages of high specific power, environmental friendliness, and good power generation efficiency. Compared with cation exchange membrane fuel cell (PEMFC), it can avoid the use of platinum and oth...

Claims

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Application Information

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IPC IPC(8): C08J5/22C08L65/00H01M8/1072
CPCC08J5/2262H01M8/1072C08J2365/00Y02E60/50
Inventor 沈春晖丁傲吴志辉张铭亮高山俊
Owner WUHAN UNIV OF TECH
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