Preparation method of monolithic polyaryletherketone bipolar membrane containing porphyrin catalytic group in side group

A technology of porphyrin catalytic group and bromomethylated polyaryletherketone, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problem of increased synthesis steps, poor grafting uniformity, bipolar membrane The middle interface layer is not clear and other problems, to achieve the effect of low resistance and low transmembrane voltage

Active Publication Date: 2022-05-10
FUJIAN NORMAL UNIV
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  • 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 polyaryletherketone bipolar membrane containing porphyrin catalytic group in side group
  • Preparation method of monolithic polyaryletherketone bipolar membrane containing porphyrin catalytic group in side group
  • Preparation method of monolithic polyaryletherketone bipolar membrane containing porphyrin catalytic group in side group

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] (1) Add 5.0 g of bromomethylated polyaryletherketone into a three-necked flask, dissolve it with 60 mL of N-methylpyrrolidone, and set aside. Weigh again 1.11g 3,4,5-trimethoxyphenol and 0.24g NaOH, dissolve with 15mL N-methylpyrrolidone, stir at room temperature for 0.5h, add dropwise to bromomethylated polyaryletherketone solution, and Stir for 10 hours. After the reaction is over, use a mixed solvent precipitant with a volume ratio of water and ethanol of 1:1 to precipitate the product. After filtering, the precipitate is rinsed with ethanol several times, soaked in deionized water, and filtered after 24 hours. , and the precipitate was vacuum-dried at 70° C. to prepare a methoxy-containing polyaryletherketone polymer.

[0059]

[0060] (2) Weigh 5.0g of methoxy-containing polyaryletherketone polymer into a 250mL three-necked flask, install a constant pressure dropping funnel, vacuumize, and protect with a nitrogen balloon. Add 120mL of pre-dried dichloromethane ...

Embodiment 2

[0075] (1) Synthesis of water catalyst in the middle layer of bipolar membrane-side chain bonded porphyrin substituent PL-PAEK polymer: In a 100mL three-necked flask, add 5.0g bromomethylated polyaryletherketone polymer and 60mL DMAc, After the copolymer is fully dissolved, 30 mL of DMAc solution and 1.2 g of NaHCO 3 , put them into a three-necked flask, raise the temperature to 50°C under the protection of nitrogen, and react at a constant temperature for 5 hours. After the reaction, immediately cool the system to room temperature with an ice-water bath, and use a mixture of distilled water and methanol as a precipitant to precipitate the product polymerization The product was washed with the mixed solution several times, and dried in vacuum to obtain a polymer (PL-PAEK) with porphyrin (PL) bonded to the side chain.

[0076]

[0077] (2) Add 5.0 g of bromomethylated polyaryletherketone into a three-necked flask, dissolve it with 60 mL of N-methylpyrrolidone, and set aside....

Embodiment 3

[0087] (1) Synthesis of water catalyst in the middle layer of bipolar membrane-side chain bonded porphyrin substituent PL-PAEK polymer: In a 100mL three-necked flask, add 5.0g bromomethylated polyaryletherketone polymer and 60mL DMAc, After the copolymer is fully dissolved, 30mL DMAc solution and 1.2g NaHCO 3 , put them into a three-necked flask, raise the temperature to 50°C under the protection of nitrogen, and react at a constant temperature for 5 hours. After the reaction, immediately cool the system to room temperature with an ice-water bath, and use a mixture of distilled water and methanol as a precipitant to precipitate the product polymerization The product was washed with the mixed solution several times, and dried in vacuum to obtain a polymer (PL-PAEK) with porphyrin (PL) bonded to the side chain.

[0088]

[0089] (2) Add 5.0 g of bromomethylated polyaryletherketone into a three-necked flask, dissolve it with 60 mL of N-methylpyrrolidone, and set aside. Weigh ...

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Abstract

The invention relates to a preparation method of a monolithic polyaryletherketone bipolar membrane containing a porphyrin group in a side group. Its scheme: bromomethylated polyaryl ether ketone and methoxy-containing phenol are reacted to obtain methoxy-phenol-containing poly-aryl-ether-ketone polymer; methoxy-phenol-containing polyaryl ether ketone polymer and boron tribromide solution Reaction to obtain hydroxyl-containing polyaryletherketone polymer; hydroxyl-containing polyaryletherketone polymer adding epichlorohydrin to react to obtain epoxy group-substituted polyaryletherketone polymer; bromomethylated polyaryletherketone polymer Compounds with hydroxyl-substituted porphyrins, NaHCO 3 The reaction is to obtain a polymer in which porphyrins are bonded to the side groups of poly(aryl ether ketone); PAEK-EG and Pc-PAEK are mixed and then cast and dried, and then the poly(aryl ether ketone-based membrane) is subjected to sulfonation reaction and amination reaction, The monolithic polyaryletherketone bipolar membrane containing porphyrin catalytic group was obtained by quaternary amination reaction. The monolithic bipolar membrane of the present invention does not produce a "bubbling" phenomenon during use, which is beneficial to improving stability and service life.

Description

technical field [0001] The invention relates to a method for preparing a monolithic poly(aryl ether ketone) bipolar membrane whose side group contains a porphyrin catalytic group, in particular to introducing a substituent containing an epoxy group into the polyarylether ketone molecular chain, which will have a catalytic The porphyrin with water dissociation function is bonded to the polyaryletherketone side group. A porphyrin-containing polyaryletherketone blended with epoxy-containing polyaryletherketone is used as the 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 porphyrin-containing monolithic film. Preparation method of polyaryletherketone 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): B01D71/70B01D71/82B01J45/00B01D67/00
CPCB01D71/72B01D71/82B01J45/00B01D67/0006
Inventor 黄雪红李晓燕丁富传
Owner FUJIAN NORMAL UNIV
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