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Preparation method of anion exchange membrane

A technology of anion exchange membrane and base membrane, applied in the field of ion exchange membrane, can solve the problems of low reactivity, large amount of chloromethylation reagent, long reaction time, etc., achieve high ion conductivity and ion exchange capacity, and avoid carcinogenesis effect, good chemical stability

Inactive Publication Date: 2013-06-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In comparison, chloromethyl ether and bischloromethyl ether are unstable, volatile, highly irritating, corrosive, and highly toxic. They are two known carcinogenic compounds, and storage and transportation are difficult; formaldehyde / paraformaldehyde and Although hydrogen chloride or trimethylchlorosilane is cheap, convenient for storage and transportation, and less toxic, it has low reactivity, long reaction time, and low yield; chloromethyl alkyl ether has a high boiling point, low toxicity, high activity, and is easy to recycle , so far no carcinogenic effect has been found, and it is safe and effective as a chloromethylation reagent
At present, there are chloromethyl octyl ether (X.Yan et.al Journal of Membrane Science 375(2011) 204-211) and chloromethyl butyl ether, bromomethyl butyl ether, bromomethyl octyl ether (Chinese patent "polyaryl ether ketone anion exchange membrane containing phthalazinone structure and its preparation method" application number: 201010141349.9) is used to prepare anion exchange membranes, and the obtained polyarylene ether containing phthalazinone structure Alkaline electrolytes have excellent electrochemical performance and selective permeation performance, but the amount of chloromethylation reagent is relatively large and the cost is high

Method used

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  • Preparation method of anion exchange membrane
  • Preparation method of anion exchange membrane
  • Preparation method of anion exchange membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Dissolve polyaryl ether sulfone ketone (PPESK) containing phthalazine structure with molecular weight Mn≈70000 in 95%-98% concentrated sulfuric acid at 0°C, keep the temperature constant, add SnCl 4 and BCMB, PPESK with concentrated sulfuric acid, BCMB and SnCl4 The mass volume ratios are 1g: 30mL, 1g: 2.8mL and 1g: 0.28mL, react for 4 hours, pour the reacted solution into a large amount of ice water, after the polymer is precipitated, suction filter, wash with deionized water until neutral , and then dried in a vacuum oven at 40-50°C to obtain chloromethylated naphthyridine-containing polyarylethersulfoneketone (CMPPESK), whose 1H NMR spectrum is as follows figure 1 shown.

[0040] According to the dosage of BCMB being respectively 0.25, 0.4, 0.5, 0.6, 0.75 and 1.0mL BCMB / gPPESK, the above process was repeated respectively to obtain CMPPESK with different chloromethylation degrees, and its 1H NMR spectra were as follows: figure 2 shown.

[0041] Dissolve CMPPESK wit...

Embodiment 2

[0043] Dissolve polyaryl ether ketone (PPEK) containing phthalazine structure with molecular weight Mn≈50000 in 95%-98% concentrated sulfuric acid at 0°C, keep the temperature constant, add BCMB, the mass of PPEK, concentrated sulfuric acid, and BCMB The volume ratios were 1g: 30mL and 1g: 1mL, reacted for 4h, poured the reacted mixed solution into a large amount of ice water, after the polymer was precipitated, suction filtered, washed with deionized water until neutral, and then placed in a vacuum oven for 40 Dry at -50°C to obtain a chloromethylated polyaryletherketone (CMPPEK) containing a phthalazine structure with a chloromethylation degree of 1.08. 1 H NMR spectrum as Figure 5 shown. Dissolve CMPPEK in N-methylpyrrolidone to form a 3-5wt.% solution, pour the casting solution into a glass frame, put it in an oven and dry it at 70°C to obtain a CMPPEK base film, and then put the base film into In 33wt.% trimethylamine aqueous solution, quaternization treatment at 30°C ...

Embodiment 3

[0045] Dissolve polyaryl ether nitrile ketone (PPENK) containing phthalazine structure with molecular weight Mn≈65000 in 95%-98% concentrated sulfuric acid at 0°C, keep the temperature constant, add BCMB, PPENK and concentrated sulfuric acid, BCMB The mass-volume ratios are 1g: 30mL and 1g: 1mL respectively. React for 4 hours. Pour the reacted mixed solution into a large amount of ice water. After the polymer is precipitated, filter it with suction, wash it with deionized water until it is neutral, and then put it in a vacuum oven. Dry at 40-50°C to obtain a chloromethylated polyarylether nitrile ketone (CMPPENK) containing a phthalazine structure with a chloromethylation degree of 1.43. 1 H NMR spectrum as Image 6 shown. Dissolve CMPPENK in N-methylpyrrolidone to form a 3-5wt.% solution, pour the casting solution into a glass frame, put it in an oven and dry it at 70°C to obtain a CMPPENK base film, and then put the base film into In 33wt.% trimethylamine aqueous solution,...

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Abstract

The invention relates to a preparation method of an anion exchange membrane. The preparation method includes the steps of firstly utilizing 1,4-BCMB as chloromethylation reagents, leading in a functional perssad on a polymer substrate, then carrying out quaternization and alkalization to form an ion exchange perssad, and obtaining the polymer anion exchange membrane. The preparation method has the advantages that long-chain ether BCMB is used as the chloromethylation reagents, carcinogenesis of short-chain ether is avoided; at the same time, the BCMB is low in cost and high in activity; and the produced anion exchange membrane has good chemical stability, heat stability and mechanical stability, is high in ionic conductivity and ion exchange capacity, and can be used in alkaline fuel cells.

Description

technical field [0001] The invention belongs to the technical field of ion exchange membranes, and in particular relates to a high-efficiency preparation method of polymer anion exchange membranes. Background technique [0002] The use of noble metal catalyst Pt in proton exchange membrane fuel cells (PEMFC) hinders its commercialization to some extent. Alkaline membrane fuel cell (AEMFC) has become a research hotspot because of its fast oxygen reduction kinetics, the use of non-platinum catalysts, low requirements for material corrosion resistance, and low cost. [0003] Anion exchange membrane is a key part of AEMFC and plays a decisive role in improving battery performance. It is composed of polymer skeleton, cations and counter ions. Preparation of anion exchange membrane mainly includes chemical polymerization / copolymerization, chloromethylation, alkali doping and radiation grafting. Among them, chemical polymerization / copolymerization has special requirements for mon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/22C08J7/12C08L71/12C08L81/06C08L61/16C08L71/10B01J41/12H01M8/02H01M2/16B01J41/13
CPCY02E60/50Y02P70/50
Inventor 邵志刚鲁望婷张耕李进衣宝廉
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI