Preparation method of polymer nanofiber membrane containing perfluorinated sulfonic acid

A nanofiber membrane, perfluorosulfonic acid technology, applied in the direction of conjugated synthetic polymer rayon, synthetic polymer rayon chemical post-treatment, fiber treatment, etc., can solve the problem of reducing the weight ratio activity of perfluorosulfonic acid, Can not be effectively used, not easy to stretch and other problems, to achieve the effect of controllable macro size, low equipment cost, simple and easy operation

Inactive Publication Date: 2013-12-25
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since perfluorosulfonic acid is usually in the state of dense and non-porous particles in a non-polar solvent or gas phase environment, the specific surface area is less than 0.02m 2 / g, making a large number of acid centers (sulfonic acid groups: -SO 3 H) is embedded in the polymer and cannot be effectively utilized, thereby reducing the weight-specific activity of perfluorosulfonic acid. Therefore, how to increase the specific surface area of ​​perfluorosulfonic acid and improve the utilization of its acidic center is crucial to perfluorosulfonic acid. One of the hotspots of sulfonic acid research
However, perfluorosulfonic acid is mostly in the form of ion clusters in organic solvents, has low viscosity and is not easy to stretch. Therefore, it is difficult to directly use a pure perfluorosulfonic acid solution in the electrospinning process, and it is usually necessary to add other polymers to the solution. As a dispersant (also known as a carrier) (H.Chen, J.Snyder, Y.Elabd, Macromolecules.2008, 41, 128-135)
At present, there is no domestic patent literature on the preparation of perfluorosulfonic acid nanofiber membranes by electrospinning technology, and there are only a few reports in foreign literature

Method used

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  • Preparation method of polymer nanofiber membrane containing perfluorinated sulfonic acid
  • Preparation method of polymer nanofiber membrane containing perfluorinated sulfonic acid
  • Preparation method of polymer nanofiber membrane containing perfluorinated sulfonic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Preparation of perfluorosulfonic acid / polyacrylonitrile nanofiber membrane

[0047] 1) Prepare polymer solution

[0048] Weigh 2.5g of polyacrylonitrile (PAN) and dissolve it in 14.0g of N,N-dimethylacetamide (DMAc), add 2.5g of perfluorosulfonic acid (PFSA), and magnetically stir in a water bath at 60°C until uniform to obtain an organic solution ;

[0049] 2) Preparation of organic-inorganic suspension

[0050] Add 1.0 g of calcium carbonate (CaCO 3 ) nanoparticles, ultrasonic treatment for 2 hours and magnetic stirring at room temperature for 12 hours to obtain a uniform organic-inorganic suspension;

[0051] 3) Preparation of nanofibrous membranes containing inorganic particles

[0052] The above-mentioned organic-inorganic suspension was left to defoam for 12 hours, and then transferred to an electrospinning device for spinning. The conditions were: power supply voltage 15kV, feed rate 0.5ml / h, adjust receiver and spinneret (inner diameter 0.4mm) The distance be...

Embodiment 2

[0057] Preparation of perfluorosulfonic acid / polyvinyl alcohol nanofiber membrane

[0058] 1) Prepare polymer solution

[0059] Weigh 2.0g of methanol, 4.0g of n-propanol, 14.0g of deionized water, stir at room temperature to form a uniform mixed solvent; take 1.2g of polyvinyl alcohol (PVA: 1799) and 3.0g of perfluorosulfonic acid (PFSA), heat at 95°C Dissolve, magnetically stir until uniform, and obtain an organic solution;

[0060] 2) Preparation of nanofibrous membrane

[0061] The above solution is cooled to room temperature, left standing for defoaming for 24h, and transferred to an electrospinning device for spinning, the conditions are: power supply voltage 18kV, feed rate 0.3ml / h, adjust receiver and spinneret (inner diameter 0.4mm) The distance between them is 10cm, and the perfluorosulfonic acid / polyvinyl alcohol nanofibrous membrane ( figure 2 );

[0062] The obtained nanofibrous membrane has a thickness of about 50 μm and a specific surface area of ​​32 m 2 ...

Embodiment 3

[0064] Preparation of perfluorosulfonic acid / polyethersulfone nanofiber membrane

[0065] 1) Prepare polymer solution

[0066] Weigh 3.0g of polyethersulfone (PES) and dissolve it in 14.0g of N,N-dimethylacetamide (DMAc), add 1.0g of perfluorosulfonic acid (PFSA), and magnetically stir in a water bath at 60°C until uniform to obtain an organic solution ;

[0067] 2) Prepare an organic solution containing additives

[0068] Under the condition of strong stirring, slowly add 2.0 g of ethanol dropwise to the above organic solution, and after the dropwise addition is completed, keep magnetic stirring at room temperature for 12 hours to obtain a uniform organic solution containing additives;

[0069] 3) Preparation of perfluorosulfonic acid / polyethersulfone nanofiber membrane

[0070] The above-mentioned organic solution is statically defoamed, and then transferred to an electrospinning device for spinning, the conditions are: power supply voltage 16kV, feed rate 0.8ml / h, adjust...

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Abstract

The invention relates to a preparation method of a polymer nanofiber membrane containing perfluorinated sulfonic acid. The method comprises four steps: (1) preparing an organic solution containing perfluorinated sulfonic acid and dispersed polymers, by using N, N-dimethylformamide, N, N-dimethylacetamide or dimethyl sulfoxide as a solvent; (2) adding organic small molecular alcohol or an inorganic nanoparticle additive into the above organic solution to prepare an organic blend solution containing perfluorinated sulfonic acid or an organic-inorganic suspended system; (3) preparing a polymer or polymer inorganic nanofiber membrane containing perfluorinated sulfonic acid; and (4) subjecting the obtained nanofiber membrane to acid and alkali treatment to obtain a porous nanofiber membrane with rough surface. The invention has the characteristics of mature and simple preparation process; and the obtained perfluorinated sulfonic acid nanofiber membrane has uniform and controllable distribution of size, high specific surface area, high porosity, good mechanical properties, and overcomes the defects of a traditional perfluorinated sulfonic acid membrane, such as easy swelling in a wet state and easy brittle cracking in a dry state.

Description

【Technical field】 [0001] The invention belongs to the technical field of nanofiber preparation, in particular to a method for preparing a polymer nanofiber membrane containing perfluorosulfonic acid. 【Background technique】 [0002] Perfluorosulfonic acid ion exchange resin (hereinafter referred to as perfluorosulfonic acid) is a kind of perfluoropolymer with polytetrafluoroethylene structure as the backbone, alkenyl ether structure as side chain, and sulfonate group at the end. In the past 40 years, it has become a research hotspot of a large number of researchers at home and abroad because of its excellent heat resistance, mechanical properties, electrochemical properties and chemical stability. At present, perfluorosulfonic acid ion exchange membranes have been widely used in engineering fields such as chlor-alkali industry, fuel cells, organic reactions and various membrane processes. However, since perfluorosulfonic acid is usually in the state of dense and non-porous p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F8/10D01F8/08D01F8/16D01F1/10D01F11/04D01D5/00
Inventor 许振良陆培培杨虎魏永明马晓华
Owner EAST CHINA UNIV OF SCI & TECH
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