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A preparing method of a perfluorosulfonic acid-carboxylic acid composite membrane by multilayer solution tape casting

A technology of perfluorosulfonic acid and perfluorocarboxylic acid, which is applied in the field of polymer material processing, can solve the problems of foaming and peeling of the composite film layer, the difference of the ion migration number is too large, and the resin solution is difficult to enter, so as to prolong the service life. , The effect of high process controllability and stable product quality

Inactive Publication Date: 2015-05-06
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the problem with this method is that it is difficult for the highly hydrophilic resin solution to enter the hydrophobic porous PTFE membrane; the second is the lamination method, which is to directly form the fluorine-type perfluorosulfonic acid resin into a film , and then laminated with PTFE mesh and perfluorocarboxylic acid to form a composite membrane, and then transformed into acid-type or salt-type PTFE mesh-reinforced perfluorosulfonic acid-carboxylic acid composite membrane through chemical treatment
The defect of this method is that there is a certain incompatibility between the perfluorosulfonic acid resin and the perfluorocarboxylic acid resin. When the electrochemical properties such as IEC of the two perfluorocarbon resins used do not match, the Blistering and peeling of the composite membrane layer will be caused due to the large difference in the ion migration number of the two base membranes and the imbalance of water penetration between the two base membranes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 150g of perfluorosulfonic acid resin particles, soak in 20% sodium hydroxide aqueous solution, and keep the temperature in a constant temperature drying oven at 100°C for 24h to make the -SO in the resin 2 The F group is completely converted to -SO 3 Na group. The transformed Na-type perfluorinated ion exchange resin is fully washed with deionized water to neutrality, and then the resin is dried in an oven for use. Put the dried perfluorosulfonic acid resin into an autoclave, add 1000ml of 1:1 isopropanol aqueous solution, heat up to 250°C, stir with magnetic force at 120r / min, and keep constant temperature and pressure for 4h. After stopping heating and stirring, naturally cool to room temperature. Take the material from the kettle to obtain a colorless transparent liquid; add 400ml of N-N dimethylformamide to the dissolved perfluorosulfonic acid solution, put it in an oven, remove isopropanol at high temperature, and wait for the low boiling point solvent to r...

Embodiment 2

[0032] Weigh 150g of perfluorosulfonic acid resin particles, soak in 20% sodium hydroxide aqueous solution, and keep the temperature in a constant temperature drying oven at 100°C for 24h to make the -SO in the resin 2 The F group is completely converted to -SO 3 Na group. The transformed Na-type perfluorinated ion exchange resin is fully washed with deionized water to neutrality, and then the resin is dried in an oven for use. Take the dried perfluorosulfonic acid resin and put it into an autoclave, add 1000ml of 1:1 isopropanol aqueous solution, heat up to 250°C, stir with magnetic force at 120r / min, and keep constant temperature and pressure for 4h. After stopping heating and stirring, cool down to room temperature naturally. Take the material from the kettle to obtain a colorless transparent liquid; add 400ml of dimethyl sulfoxide to the dissolved perfluorosulfonic acid solution, put it in an oven, remove isopropanol at high temperature, and wait for the low boiling poin...

Embodiment 3

[0034] Weigh 150g of perfluorosulfonic acid resin particles, soak in 20% sodium hydroxide aqueous solution, and keep the temperature in a constant temperature drying oven at 100°C for 24h to make the -SO in the resin 2 The F group is completely converted to -SO 3 Na group. The transformed Na-type perfluorinated ion exchange resin is fully washed with deionized water to neutrality, and then the resin is dried in an oven for use. Put the dried perfluorosulfonic acid resin into the autoclave, add 1000ml of 1:1 isopropanol aqueous solution, raise the temperature to 250°C2, stir with magnetic force at 120r / min, keep constant temperature and pressure for 4h. After stopping heating and stirring, cool down to room temperature naturally. Open the kettle and take the material to obtain a colorless transparent liquid; add 400ml of 1-methyl-2-11 pyrrolidone (NMP) to the dissolved perfluorosulfonic acid solution, put it in an oven, and remove it at high temperature. Isopropanol, after r...

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Abstract

The invention relates to a preparing method of a perfluorosulfonic acid-carboxylic acid composite membrane by multilayer solution tape casting. The method includes: preparing a perfluorosulfonic acid resin solution and a perfluorocarboxylic acid resin solution respectively, and repeating multi-time tape casting on a steel belt tape casting machine. The preparing method is characterized in that: the composite membrane prepared by solution multi-time tape casting is high in interlayer adhesion strength, and anti-stripping performance of an ion membrane is good. Blistering and stripping of composite membranes prepared by traditional lamination methods, which are caused by large stress generated by a large difference between ion transference numbers of two base membranes and imbalance water permeation amounts of the two base membranes in an electrolytic process, are avoided, so that the service lifetime of the composite membrane is prolonged. The preparing method is high in process automation degree, simple and convenient in operation, high in process controllability, stable in product quality and capable of achieving large-scale production.

Description

1. Technical field [0001] The invention relates to a method for preparing a perfluorosulfonic acid-carboxylic acid composite film by adopting a multilayer solution casting method, and belongs to the field of polymer material processing. 2. Background technology [0002] Soda production by ion membrane method is the earliest application of perfluorinated ion exchange membrane and the most mature field of industrial technology. Ionic membrane alkali production has the advantages of low energy consumption, no pollution, high product quality, etc., and eliminates the environmental pollution caused by the previous asbestos method and mercury method, so it has become the leading production method in the domestic chlor-alkali industry. [0003] So far, the ion exchange membrane used in chlor-alkali production is a multilayer composite membrane with an asymmetric structure, and the side facing the cathode is a perfluorocarboxylic acid membrane, which has high selectivity and can eff...

Claims

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Application Information

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IPC IPC(8): C08J7/14C08J5/22C08L101/02
Inventor 苑会林高艳林
Owner BEIJING UNIV OF CHEM TECH
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