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Preparation method of monolithic polysulfone bipolar membrane with side group bonded with phthalocyanine catalytic group

A technology for synthesizing phthalocyanine catalytic groups and bipolar membranes is applied in the field of preparation of monolithic polysulfone bipolar membranes with side groups bonded to phthalocyanine catalytic groups, and can solve the chemical stability and thermal stability of functional groups. It is not high, the scope of use is limited, the utilization rate of monomer is low, etc., to achieve good economic benefits and promotion value, improve stability and service life, and save the effect of film forming process

Active Publication Date: 2020-08-14
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 Patents US4024043 and US4057481 soaking the monomer solution multiple times and polymerizing), which increases the number of synthesis steps; the fifth is affected by the grafted monomers. 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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  • Preparation method of monolithic polysulfone bipolar membrane with side group bonded with phthalocyanine catalytic group
  • Preparation method of monolithic polysulfone bipolar membrane with side group bonded with phthalocyanine catalytic group
  • Preparation method of monolithic polysulfone bipolar membrane with side group bonded with phthalocyanine catalytic group

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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, dissolve 20mL of NMP solution with 6.6g of hydroxyphthalocyanine manganese and 1.0g 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 60 m...

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Abstract

The invention relates to a preparation method of a monolithic polysulfone bipolar membrane with a side group bonded with a phthalocyanine catalytic group. The preparation method comprises the following steps: taking a bromomethylated polysulfone polymer as a starting raw material, respectively synthesizing an epoxy group-containing substituent polysulfone polymer and a polysulfone side group bonded phthalocyanine polymer, mixing the epoxy group-containing substituent polysulfone polymer and the polysulfone side group bonded phthalocyanine polymer, casting on a clean glass plate, and drying toprepare a polysulfone-based membrane containing a phthalocyanine group side group and an epoxy group side group; and sulfonating, aminating and quaternizing the base membrane, and washing with deionized water to obtain the monolithic phthalocyanine group-containing polysulfone bipolar membrane. According to the bipolar membrane prepared by the method, an epoxy group is introduced into a polysulfone side group through nucleophilic substitution reaction, and anion and cation exchange membranes are introduced into a polysulfone molecular chain so that a membrane forming process is omitted, and the use of carcinogen chloromethyl ether is avoided. The prepared bipolar membrane has a self-catalysis effect, and is low in resistance and low in transmembrane voltage. And after long-term use, the problems of bubbling, cracking and the like of the middle interface layer, which are easily caused in the use process of the composite bipolar membrane, can be avoided.

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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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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