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A kind of preparation method of dibenzo-18-crown-6 grafted polyvinyl alcohol microporous membrane

A technology of polyvinyl alcohol and microporous membranes, applied in fuel cells, electrical components, electrochemical generators, etc., can solve problems such as poor stability, unseen problems, and damage to polymer matrix properties, so as to improve thermal stability , Improve ion exchange capacity and conductivity, and inhibit excessive swelling

Active Publication Date: 2020-09-08
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the actual working process of this type of membrane, the properties of the polymer matrix are obviously damaged due to the grafting of quaternary ammonium groups, which will lead to poor stability.
Considering PVA as the polymer matrix, its hydroxyl groups undergo acetal reaction with crown ethers with aldehyde functional groups for modification to form anion-conducting films, which not only preserve the good film-forming properties and non-toxic advantages of polyvinyl alcohol, Crown ether can inhibit the excessive swelling of polyvinyl alcohol and maintain the unique excellent conductivity of crown ether. It is a high-quality material for anion exchange membranes, and such reports have not been seen in the field of fuel cells.

Method used

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  • A kind of preparation method of dibenzo-18-crown-6 grafted polyvinyl alcohol microporous membrane
  • A kind of preparation method of dibenzo-18-crown-6 grafted polyvinyl alcohol microporous membrane
  • A kind of preparation method of dibenzo-18-crown-6 grafted polyvinyl alcohol microporous membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Heat the constant-temperature heating magnetic stirrer to 95°C for later use; place dibenzo-18crown 6 (0.02mol / L) and hexamethamine (0.08mol / L) in a 100mL circular tube equipped with the above-mentioned magnetic stirrer Quickly add concentrated hydrochloric acid (10mol / L) to the three-neck flask at the bottom, and reflux for 12 hours under the protection of high-purity nitrogen to obtain a brown viscous liquid; after the reaction is completed and cooled to room temperature, add 50 mL of concentrated NaOH solution in sequence and deionized water 200mL, fully stirred until a brown solid appeared, filtered off the water phase, and spin-dried the solid to obtain the crude product 4-formyldibenzo-18-crown 6.

[0056] (2) Add 3.8g of polyvinyl alcohol and 0.2g of 4-formyl dibenzo-18 crown 6 into a 100mL three-necked flask, use 30mL of dimethylformamide (DMF) as a solvent, and heat to 90°C until they are completely dissolved. After the reaction was completed, the solution ...

Embodiment 2

[0058] (1) Heat the constant-temperature heating magnetic stirrer to 95°C for later use; place dibenzo-18crown 6 (0.02mol / L) and hexamethamine (0.08mol / L) in a 100mL circular tube equipped with the above-mentioned magnetic stirrer Quickly add concentrated hydrochloric acid (10mol / L) to the three-neck flask at the bottom, and reflux for 12 hours under the protection of high-purity nitrogen to obtain a brown viscous liquid; after the reaction is completed and cooled to room temperature, add 50 mL of concentrated NaOH solution in sequence and deionized water 200mL, fully stirred until a brown solid appeared, filtered off the water phase, and spin-dried the solid to obtain the crude product 4-formyldibenzo-18-crown 6.

[0059] (2) Add 3.6 g of polyvinyl alcohol and 0.4 g of 4-formyl dibenzo-18 crown 6 into a 100 mL three-necked flask, use 30 mL of dimethylformamide (DMF) as a solvent, and heat to 90° C. until they are completely dissolved. After the reaction was completed, the sol...

Embodiment 3

[0061] (1) Heat the constant temperature heating magnetic stirrer to 95°C for later use; put dibenzo-18crown 6 (0.02mol / L) and urotropine (0.08mol / L) in a 100mL round-bottomed three-port container equipped with mechanical stirring In the bottle, quickly add concentrated hydrochloric acid (10mol / L), and reflux for 12 hours under the protection of high-purity nitrogen to obtain a brown viscous liquid; after the reaction is completed and cooled to room temperature, add 50 mL of concentrated NaOH solution and remove 200 mL of ionic water, fully stirred until a brown solid appeared, filtered off the water phase, and spin-dried the solid to obtain the crude product 4-formyldibenzo-18-crown 6.

[0062] (2) Add 3.4 g of polyvinyl alcohol and 0.6 g of 4-formyl dibenzo-18 crown 6 into a 100 mL three-necked flask, use 30 mL of dimethylformamide (DMF) as a solvent, and heat to 90° C. until they are completely dissolved. After the reaction was completed, the solution was placed on a clean ...

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Abstract

The invention belongs to preparation technologies of membrane electrolytes of an anion-exchange membrane fuel cell, and particularly relates to a preparation method of a dibenzo-18-crown-6 grafted polyvinyl alcohol microporous membrane. The method includes steps of: 1) firstly, synthesizing 4-formyldibenzo-18-crown-6 with the dibenzo-18-crown-6, concentrated hydrochloric acid and urotropine as rawmaterials; 2) blending the 4-formyldibenzo-18-crown-6 with polyvinyl alcohol with dimethyl formamide as a solvent, mechanically stirring the mixture uniformly, and casting the mixture, as a film casting liquid, on a glass board through a tape-casting process to form the film; 3) drying the film to constant weight, and performing an aldolization reaction to obtain an F-P membrane material having micropores; 4) impregnating the F-P membrane in a KOH solution to prepare the F-P-K conductive film. The product has great thermostability, strong conductivity and high tensile strength and breaking elongation.

Description

technical field [0001] The invention relates to the technical field of fuel cells, and belongs to the membrane electrolyte preparation technology of anion exchange membrane fuel cells, in particular to a preparation method of dibenzo-18-crown-6 grafted polyvinyl alcohol microporous membrane. Background technique [0002] Fuel cells have brought new opportunities to solve problems such as energy shortage and environmental pollution because of their advantages such as rapid start-up at low temperature, no electrolyte loss, high specific power and specific energy, low emission, or even "zero" emission. Compared with anion exchange membrane (AEMS), proton exchange membrane has high alkaline chemical stability and high ion conductivity, which is the key to achieve long-term and low cost. Recently, it has received more and more attention and has been widely used. in the fuel cell. The crown ether molecule has a hydrophobic skeleton and a hydrophilic inner cavity, which can coordi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M8/083
CPCH01M8/083Y02E60/50
Inventor 王吉林郑旭莹范志鸿曲志强王璐璐赵崇峰
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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