Microporous-film-and-fiber-reinforced multilayer fluorine-containing cross-linking doping ionic membrane and preparation method thereof

A fiber-reinforced, ion-doped technology, applied in semi-permeable membrane separation, chemical instruments and methods, membrane technology, etc., can solve problems such as membrane inhomogeneity and conductivity drop

Active Publication Date: 2009-01-21
SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the membrane obtained by utilizing this patent will be an inhomogeneous membrane, because ammonia gas enters the membrane through the method of permeation, and ammonia gas will react with sulfuryl fluoride during the permeation process, and the sulfuryl fluoride of the reaction will prevent ammonia gas from further Diffusion to the inside of the membrane, resulting in a high crosslink density on the surface of the membrane, while almost no crosslinking occurs inside the membrane
Large surface cross-links lead to a sharp drop in the conductivity of the membrane

Method used

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  • Microporous-film-and-fiber-reinforced multilayer fluorine-containing cross-linking doping ionic membrane and preparation method thereof
  • Microporous-film-and-fiber-reinforced multilayer fluorine-containing cross-linking doping ionic membrane and preparation method thereof
  • Microporous-film-and-fiber-reinforced multilayer fluorine-containing cross-linking doping ionic membrane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] the repeating unit as

[0091]

[0092] Polymer with EW=1000 and Zr (HPO with particle size 0.005 μm) 4 ) 2 (Zr(HPO 4 ) 2 The mass ratio of the resin to the resin is 3:100) to prepare a 5wt% propanol aqueous solution, and then it is placed in a 5% perfluoromalonyl peroxide DMF solution, and a 30 μm thick expanded polytetrafluoroethylene film (porous rate 70%) was soaked in the above solution for about 1 hour, and then the soaked film was dried on a hot plate, during which the film was rolled with a rubber roller. Polytetrafluoroethylene fibers (1 μm in diameter, 50 μm in length, and polymer mass ratio of 7:100) were added to the above solution, then cast into a horizontally placed polytetrafluoroethylene casting mold, and dried at 80° C. for 12 hours in vacuum. Membrane peeling in 0.5 M HO 2 SO 4 The solution was boiled for 1 hour and washed with deionized water. After the heat treatment, the membrane was sequentially treated with NaOH solution and sulfuric ac...

Embodiment 2

[0094] the repeating unit as

[0095]

[0096] EW=800 polymer and 0.03 μm SiO particle size 2 (SiO 2 The mass ratio to perfluorosulfonic acid resin is 5:100), and alkali-free glass fiber (diameter 0.05 μm length 5um, the mass ratio of alkali-free glass fiber and perfluorosulfonic acid resin is 1:40) is mixed and extruded to obtain a thickness of The 30 μm membrane and the 12 μm silica-modified porous hexafluoropropylene membrane were hot pressed together under vacuum at 260 °C, and then soaked in NH in a vacuum oven at 150 °C for 1 hour. 4 Cl in DMF solution for 5 hours. The soaked membrane was then placed in triethylamine at 200°C for 2 hours to obtain a cross-linked membrane. The membrane was sequentially treated with KOH solution and hydrochloric acid solution to obtain an ion exchange membrane with a cross-linked structure (II) (single-layer membrane 2#).

[0097] the repeating unit as

[0098]

[0099] The polymer with EW=1200 and tetraphenyltin were extruded i...

Embodiment 3

[0101] the repeating unit as

[0102]

[0103] The polymer with EW=1100 and H 3 PW 12 O 40 A 3% polymer solution was prepared at a ratio of 100:1, and the porous Al 2 O 3 The film was immersed in the above solution, and after 30 minutes, the film was taken out and dried, and then the film was cross-linked by 50KGy radiation to obtain a 20 μm cross-linked structure of type (I) ion membrane. (Single layer film 4#)

[0104] the repeating unit as

[0105]

[0106] The polymer with EW=940 and H 3 PW 12 O 40 By polymer with H 3 PW 12 O 40 The mass ratio of 100:20 was made into a 30% DMSO solution, and silicic acid-modified polytetrafluoroethylene fibers (0.2 μm in diameter, 80 μm in length, and the weight ratio to the polymer was 7:100) were cast in 170° C., 60 min to obtain a 10 μm film (single-layer film 5#).

[0107] The single-layer membrane 2#, 4, 5# perfluorosulfonic acid ionic membrane was stacked for hot pressing, and then hot-pressed with the multi-layer ...

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Abstract

The invention pertains to the filed of functional macromolecular composite materials, relating to a microporous film and fiber reinforced multi-layer fluoric cross-linked doped ion film and a preparation method thereof. Fluoric ion-exchange resin (EW=600-1300) is used to form 2-40 film layers, wherein, at least 1 layer is in a cross-linked mesh structure, at least 1 layer is a microporous film taking microporous film as reinforce, at least 1 layer is added with inorganic adulterant which has water-retaining function or proton-exchange function, and at least 1 layer is added with fibers which serve as reinforce. The multi-layer fluoric cross-linked doped ion film adopts microporous film, reinforced fibers, cross-linking and other means to improve the mechanical strength of the ion film to a very large extent; the existence of inorganic adulterant which has water-retaining function ensures much higher electric conductivity of the achieved film under high temperature or low humidity compared with traditional ion-exchange film.

Description

technical field [0001] The invention belongs to the field of functional polymer composite materials, and relates to a multi-layer fluorine-containing cross-linked ion membrane and a preparation method thereof. Background technique [0002] Proton exchange membrane fuel cell is a power generation device that directly converts chemical energy into electrical energy through electrochemical means, and is considered to be the preferred clean and efficient power generation technology in the 21st century. Proton exchange membrane (PEM) is the key material of proton exchange membrane fuel cell (PEMFC). [0003] Although the perfluorosulfonic acid proton exchange membranes currently in use have been used for many years, there are still shortcomings that cannot meet the requirements of commercialization, such as low high temperature proton conductivity, poor dimensional stability, and low mechanical strength. Especially in terms of dimensional stability, the swelling rate of the film...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M8/02H01M2/16C08J5/22C08L27/12C08K7/02B01D71/32H01M8/0243H01M50/403H01M50/44H01M50/446H01M50/457H01M50/491H01M50/494H01M50/497
CPCY02E60/50
Inventor 张永明王军唐军柯王汉利
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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