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A preparation method of side group-bonded phthalocyanine catalytic group monolithic polysulfone bipolar membrane

A technology for combining phthalocyanine catalytic groups and bipolar membranes, which is applied in the field of preparation of side-group-bonded phthalocyanine catalytic groups monolithic polysulfone bipolar membranes, can solve the problem of increased synthesis steps, self-polymerization of monomers, grafting Poor branch uniformity and other problems, to achieve the effect of low resistance and low transmembrane voltage

Active Publication Date: 2022-01-11
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 film is cleaned and regrafted (similar to US Pat. The chemical and thermal stability of the functional groups with ion exchange capacity of the membrane, whether it is its positive side or its negative side, is not high, which greatly limits its application range

Method used

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  • A preparation method of side group-bonded phthalocyanine catalytic group monolithic polysulfone bipolar membrane
  • A preparation method of side group-bonded phthalocyanine catalytic group monolithic polysulfone bipolar membrane
  • A preparation method of side group-bonded phthalocyanine catalytic group monolithic polysulfone bipolar membrane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Add 5.0 g of bromomethylated polysulfone into a three-necked flask, dissolve with 60 mL of N-methylpyrrolidone, and set aside. Weigh again 2.39g 3,4,5-trimethoxyphenol and 0.52g NaOH, dissolve with 30mL N-methylpyrrolidone, stir at room temperature for 0.5h, add dropwise into bromomethylated polysulfone solution, and stir at room temperature 10h, 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, and the precipitate is soaked in deionized water. After 24 hours, filter and precipitate The product was vacuum-dried at 70°C to prepare a methoxy-containing polysulfone polymer.

[0045]

[0046] (2) Weigh 5.0 g of methoxy-containing polysulfone polymer into a 250 mL three-necked flask, install a constant-pressure dropping funnel, and protect it with a nitrogen balloon after vacuuming. Add 120mL of pre-dried dichlor...

Embodiment 2

[0058] (1) Synthesis of water catalyst in the middle layer of bipolar membrane-side chain bonded phthalocyanine substituent Pc-PSF polymer: In a 100mL three-necked flask, add 5.0g bromomethylated polysulfone polymer and 60mL NMP, and wait for copolymerization After the substance is fully dissolved, 20mL NMP solution dissolved with 6.6g hydroxyphthalocyanine iron and 1.0g 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 (Pc-PSF) with phthalocyanine (Pc) bonded to the side chain.

[0059]

[0060] (2) Add 5.0 g of bromomethylated polysulfone into a three-necked flask, di...

Embodiment 3

[0071] (1) Synthesis of side group-bonded phthalocyanine polysulfone polymer (Pc-PSF) bipolar membrane interlayer water dissociation catalyst: In a 100mL three-neck flask, add 5.0g bromomethylated polysulfone polymer and 60mL NMP, After the copolymer is fully dissolved, 20 mL of NMP solution dissolved with 6.6 g of hydroxyphthalocyanine manganese and 1.0 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 (Pc-PSF) with phthalocyanine (Pc) bonded to the side chain.

[0072]

[0073] (2) Add 5.0 g of bromomethylated polysulfone into a three-necked flask, dissolve with ...

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Abstract

The invention relates to a method for preparing a side group-bonded phthalocyanine catalytic group monolithic polysulfone bipolar membrane. The present invention uses bromomethylated polysulfone polymers as starting materials, respectively synthesizes polysulfone polymers containing epoxy group substituents and polysulfone side groups bonded with phthalocyanine polymers, mixes them and casts them on a clean A glass plate was dried to prepare a polysulfone-based membrane containing phthalocyanine group side groups and epoxy group side groups; after the base membrane was sulfonated, ammonized and quaternized, it was washed with deionized water to obtain a monolithic Polysulfone bipolar membranes containing phthalocyanine groups. The bipolar membrane prepared by the present invention adopts a nucleophilic substitution reaction, introduces an epoxy group on the polysulfone side group, introduces an anion and a cation exchange membrane method into the polysulfone molecular chain, and saves the film-forming process and avoids the carcinogen chlorine Use of methyl 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 preparation method of a side group-bonded phthalocyanine catalytic group monolithic polysulfone bipolar membrane. Epoxy group polysulfone is blended into a membrane as the base membrane material, and anion and cation are introduced into both sides of the base membrane through epoxy group reaction to synthesize a side chain-bonded phthalocyanine catalytic group monolithic polysulfone bipolar membrane preparation method . 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. It is usually a functional membrane with a three-layer structure composed of an anion exchange layer, a cation exchange layer and an intermediate catalytic layer that splits water rapidly. Under the action of a DC electric field, the water in the interface layer of the bipolar membrane dissociates, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/82B01D71/68B01D67/00B01J45/00
CPCB01D71/68B01J45/00B01D71/82B01D67/0006
Inventor 黄雪红贾玉婷张睫灵宁金凤李晓燕丁富传
Owner FUJIAN NORMAL UNIV
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