Preparation Method of Monolithic Polyarylether Nitrile Bipolar Membrane Containing Corrole Hydrodissociation Catalytic Group

A technology of polyarylether nitrile and bipolar membrane, which is applied in chemical instruments and methods, membrane technology, ion exchange, etc., can solve the problems of increased synthesis steps, limited use range, poor grafting uniformity, etc., and achieves low resistance and low cost. The effect of eliminating the film formation process and low transmembrane voltage

Active Publication Date: 2022-03-15
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method also has several obvious disadvantages: first, the grafting rate is low, and the grafting uniformity is also poor; second, because the porous material is used as the base membrane, the grafted monomers on both sides avoid mutual penetration, and the bipolar membrane The middle interface layer is not clear; the third is that the method of co-radiation grafting will cause a large amount of monomers to self-polymerize, and the utilization rate of the monomers is very low, which is not suitable for industrial production; the fourth is to achieve the required grafting rate. The grafted membrane is cleaned and grafted again (similar to the above-mentioned U.S. patent soaking the monomer solution multiple times and polymerizing), so that the synthesis steps are increased; the fifth is affected by the grafted monomer, the bipolar membrane prepared in the paper, Regardless of its positive or negative side, the chemical stability and thermal stability of its functional groups with ion exchange capabilities are not high, thus greatly limiting its scope of use

Method used

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  • Preparation Method of Monolithic Polyarylether Nitrile Bipolar Membrane Containing Corrole Hydrodissociation Catalytic Group
  • Preparation Method of Monolithic Polyarylether Nitrile Bipolar Membrane Containing Corrole Hydrodissociation Catalytic Group
  • Preparation Method of Monolithic Polyarylether Nitrile Bipolar Membrane Containing Corrole Hydrodissociation Catalytic Group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] (1) In a three-necked flask, add 2,4-dimethoxyhydroquinone 8.5570g (50mmol), resorcinol 3.3030g (30mmol), 2,4-difluoroterephthalonitrile 8.2055 g (50mmol), difluorodiphenyl sulfone 7.6275g (30mmol), anhydrous potassium carbonate 13.2664g (90mmol), toluene 320mL, DMAc 400mL, react at 140°C for 3h in a nitrogen atmosphere, then raise the temperature to 165°C for 10h, and immediately The reaction solution was poured into deionized water for precipitation under stirring, and filtered. The filtered precipitate was soaked in deionized water, soaked in running water for 24 hours, filtered, and dried in a vacuum oven at 80° C. for 10 hours to obtain a product containing methoxy polyarylether nitrile.

[0052]

[0053] (2) Weigh 5.0 g of polyarylether nitrile polymer containing methoxy in a 250 mL three-neck flask, install a constant pressure dropping funnel, and protect it with a nitrogen balloon after vacuuming. Add 120mL of pre-dried dichloromethane to dissolve the polyme...

Embodiment 2

[0065] (1) In a three-necked flask, add 8.6898g (70mmol) of o-methylhydroquinone, 1.3601g (10mmol) of 3-cyanoresorcinol, 15.2749g (70mmol) of difluorobenzophenone, and Fluorodiphenyl sulfone 2.5425g (10mmol), anhydrous potassium carbonate 13.2664g (90mmol), toluene 320mL, DMAc 400mL, react at 140°C for 3h in a nitrogen atmosphere, then raise the temperature to 160°C for 8h, and immediately pour the reaction solution under stirring into deionized water, and filtered. The filtered precipitate was soaked in deionized water, soaked in running water for 24 hours, filtered, and dried in a vacuum oven at 80° C. for 10 hours to obtain a product containing methoxy polyarylether nitrile.

[0066]

[0067](2) Weigh 5.0 g of polyarylether nitrile polymer containing methoxy in a 250 mL three-neck flask, install a constant pressure dropping funnel, and protect it with a nitrogen balloon after vacuuming. Add 120mL of pre-dried dichloromethane to dissolve the polymer, and add 3.6mL of bor...

Embodiment 3

[0079] (1) Preparation of polyarylether nitrile containing methoxy: in a three-necked flask, add 5.1369g (30mmol) of 2,5-dimethoxyhydroquinone, 1.1101g (10mmol) of resorcinol, two Fluorodiphenyl sulfone 7.6275g (30mmol), difluorobenzonitrile 1.3900g (10mmol), anhydrous potassium carbonate 6.9002g (50mmol), toluene 160mL, DMAc200mL, in N 2 React at 140°C for 3 hours in the atmosphere, then raise the temperature to 175°C for 9 hours, immediately pour the reaction solution into deionized water for precipitation under stirring, and filter. The filtered precipitate was soaked in deionized water, soaked in running water for 24 hours, filtered, and dried in a vacuum oven at 80° C. for 10 hours to obtain a product containing methoxy polyarylether nitrile.

[0080]

[0081] (2) Weigh 5.0 g of methoxy-containing polyarylether nitrile polymer into a 250 mL three-neck flask, install a constant-pressure dropping funnel, vacuumize, and protect with a nitrogen balloon. Add 120mL of pre-d...

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Abstract

The invention relates to a method for preparing a monolithic polyarylether nitrile bipolar membrane containing corrole water dissociation catalytic groups. The present invention uses methoxy bisphenol, non-methoxy bisphenol, dihalocyanobenzene, dihalobenzophenone or dihalodiphenyl sulfone and mole catalyst I as starting materials to synthesize PAEN‑EG and Corrole respectively ‑PAEN polymer, blended and cast on a glass plate; after sulfonation, ammonization and quaternization, polyarylethernitrile bipolar membranes are obtained. The present invention introduces methoxy groups into the polyarylether nitrile molecular chain through polycondensation reaction, reacts with boron tribromide to obtain hydroxyl-containing polyarylether nitrile, and then reacts with epichlorohydrin to form polyarylether nitrile on the side group of polyarylether nitrile The introduction of epoxy groups saves the film-forming process and avoids the use of carcinogen chloromethyl ether. The prepared bipolar membrane has self-catalysis, low bipolar membrane resistance and low transmembrane voltage. Long-term use, there will be no problems such as bubbling and cracking in the middle interface layer that are prone to occur during the use of composite bipolar membranes.

Description

technical field [0001] The invention relates to a method for preparing a monolithic polyarylether nitrile bipolar membrane containing a corrole water dissociation catalytic group, in particular to introducing a substituent containing an epoxy group on the polyarylether nitrile main chain, corrole and ring Oxygen groups are introduced into the polyarylethernitrile molecular structure through reaction. Corrole-containing polyarylether nitrile and epoxy group-containing polyarylether nitrile are blended to form a film as a base film material, and anions and cations are introduced on both sides of the base film through the reaction of epoxy groups to synthesize a monolithic polyamide containing corrole group. The preparation method of aryl ether nitrile bipolar membrane. Background technique [0002] Bipolar membrane is a new branch developed on the basis of ion exchange membrane technology, and has rapidly developed into a research hotspot in the field of membrane technology. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/82B01D71/72B01D67/00B01J45/00
CPCB01J45/00B01D71/72B01D71/82B01D67/0006
Inventor 黄雪红李晓燕丁富传
Owner FUJIAN NORMAL UNIV
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