CN103752189B - A kind of preparation method with the microporous barrier of ion exchanging function - Google Patents
A kind of preparation method with the microporous barrier of ion exchanging function Download PDFInfo
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- CN103752189B CN103752189B CN201410022504.3A CN201410022504A CN103752189B CN 103752189 B CN103752189 B CN 103752189B CN 201410022504 A CN201410022504 A CN 201410022504A CN 103752189 B CN103752189 B CN 103752189B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to technical field of membrane, be specifically related to a kind of preparation method with the microporous barrier of ion exchanging function, melt extrude diaphragm, twice biaxial tension, thermal finalization, to obtain final product.Perfluor microporous barrier prepared by the present invention has ion exchanging function, adds the caking property of reinforcing material and resin, and microporous barrier thickness is even, uniform pore diameter, dimensionally stable.As the reinforcing material of PEM and Membrane Used In Chlor-alkali Cell, can increase the effective area of cation permeable film, corresponding reduction film resistance and tank voltage, be that suitability for industrialized production lowers energy consumption.
Description
Technical field
The invention belongs to technical field of membrane, be specifically related to a kind of preparation method with the microporous barrier of ion exchanging function.
Background technology
Exchange after composite membrane exhibits one's skill to the full in chlorine industry from perfluorinated ion, the whole world that is applied in of perfluorinated ion-exchange membrane obtains and studies widely.No matter perfluorinated ion-exchange membrane is in chlorine industry or application in a fuel cell, current known technology all needs to adopt enhancing framework material to strengthen, no matter be adopt poromerics to strengthen or fiber reinforcement, these reinforcing materials are polytetrafluoroethylene (PTFE), meltable poly and auxiliary a small amount of sacrificial fiber material nothing more than.The reinforcing material of these perfluor types belongs to the insulating materials without ion exchanging function, its specific insulation will exceed than the resistivity of general chlorine industry perfluor type ion-exchange more than 14 orders of magnitude, thus will occur " blind area " at the directed back side through film of cation, the corresponding effective area decreasing cation permeable film, add film resistance and tank voltage, this is a technical barrier of current this area; Another one technical barrier is no matter polytetrafluoroethylene (PTFE) or meltable poly, be all have very low surface energy, adhesion property is very poor, and the interlayer adhesion of itself and exchange membrane material is weak, in use procedure, easily off, stripping between rete, shortens the service life of membrane material.
Reinforcing material in current fuel cell mainly microporous teflon membran, due to the strong-hydrophobicity of microporous teflon membran and the strong absorptive of resin solution, causes the loading of resin not enough, affects the performance of film.Although a lot of research improves microporous teflon membran water imbibition by the surface modification of polytetrafluoroethylene (PTFE) and blending modification, all have no idea fundamentally to address this problem.
Summary of the invention
The object of this invention is to provide a kind of preparation method with the microporous barrier of ion exchanging function, scientific and reasonable, simple, the microporous barrier thickness of preparation evenly, uniform pore diameter, dimensionally stable.
The preparation method with the microporous barrier of ion exchanging function of the present invention, step is as follows:
(1) diaphragm is melt extruded: by there is the fluororesin of ion exchanging function by melt extruding, prepare diaphragm;
(2) twice biaxial tension: the diaphragm of preparation is carried out synchronous in length and breadth to twice biaxial tension;
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization, to obtain final product.
The fluororesin with ion exchanging function described in step (1) is the perfluorinated resin with sulfonyl fluoride group.
Perfluor sulfonyl base vinyl ethers, tetrafluoroethene and hexafluoropropene monomer or perfluor sulfonyl base vinyl ethers, tetrafluoroethene and alkyl vinyl ether are caused combined polymerization through free radical and prepare by the described perfluorinated resin with sulfonyl fluoride group under dispersant, solvent and initator exist.
The preparation of the described perfluorinated resin with sulfonyl fluoride group can select any one method of this area, and the preparation method of the perfluorinated resin that the present invention adopts is see 200610166294.0 and 200610166293.6.
The ion exchange capacity value with the fluororesin of ion exchanging function described in step (1) is 0.10-0.45mmol/g, is 5-50g/10min the melt flow index of 372 DEG C.
Melt temperature described in step (1) is 200-400 DEG C, the die head temperature that it melt extrudes at least 300 DEG C.
Biaxial tension temperature described in step (2) is 180-350 DEG C, and preferred draft temperature is 200-300 DEG C.
The rate of extension of the biaxial tension described in step (2) is 1-20m/min, and preferred rate of extension is 1-10m/min; The draw ratio of biaxial tension is 1-500, and preferred draw ratio is 2-200; The time interval that biaxial tension stretches at every turn is 1-60 second.
Heat setting temperature described in step (3) is 260-380 DEG C, and preferred heat setting temperature is 300-340 DEG C; The time of thermal finalization is 20-80 second.
The drawing process of described microporous barrier is biaxial tension, and namely synchronous vertical, horizontal stretches.
When the present invention melt extrudes, the part of equipment and resin contact adopts Langaloy, prevents from introducing foreign ion in resin.
The thickness of microporous barrier prepared by the present invention is 0.1-20 micron, and aperture is 0.1-10 micron, and longitudinal contraction rate is less than 5%, and lateral shrinkage is less than 4%.
Microporous barrier prepared by the present invention can be used for the reinforcing material of PEM and Membrane Used In Chlor-alkali Cell, reaches the effect strengthening and improve ion-exchange capacity simultaneously.
The present invention compared with prior art, has following beneficial effect:
Perfluor microporous barrier prepared by the present invention has ion exchanging function, adds the caking property of reinforcing material and resin, and microporous barrier thickness is even, uniform pore diameter, dimensionally stable.As the reinforcing material of PEM and Membrane Used In Chlor-alkali Cell, can increase the effective area of cation permeable film, corresponding reduction film resistance and tank voltage, be that suitability for industrialized production lowers energy consumption.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
(1) melt extrude diaphragm: be 265 DEG C by this fluororesin at extruder temperature, die head temperature is under the condition of 305 DEG C, by melt extruding the diaphragm of preparation biaxial tension.
(2) twice biaxial tension: by the cooling of the diaphragm of preparation, and carry out synchronous in length and breadth to twice biaxial tension at 180 DEG C.First time, rate of extension was 5m/min, and second time rate of extension is 1m/min, and twice stretching time is spaced apart 30s.
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization is 20s in the time of 280 DEG C of thermal finalizations.
The microporous barrier thickness prepared as stated above is 15 microns, and thickness is even, and aperture is 0.3 micron, and uniform pore diameter, longitudinal contraction rate is 5%, and lateral shrinkage is 4%, good stability of the dimension.
Embodiment 2
(1) melt extrude diaphragm: be 320 DEG C by this fluororesin at extruder temperature, die head temperature is under the condition of 380 DEG C, by melt extruding the diaphragm of preparation biaxial tension.
(2) twice biaxial tension: by the cooling of the diaphragm of preparation, and carry out synchronous in length and breadth to twice biaxial tension at 260 DEG C.First time, rate of extension was 10m/min, and second time rate of extension is 3m/min, and twice stretching time is spaced apart 60s.
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization is 50s in the time of 320 DEG C of thermal finalizations.
The microporous barrier thickness prepared as stated above is 5 microns, and thickness is even, and aperture is 5 microns, and uniform pore diameter, longitudinal contraction rate is 4.5%, and lateral shrinkage is 3%, good stability of the dimension.
Embodiment 3
(1) melt extrude diaphragm: be 350 DEG C by this fluororesin at extruder temperature, die head temperature is under the condition of 400 DEG C, by melt extruding the diaphragm of preparation biaxial tension.
(2) twice biaxial tension: by the cooling of the diaphragm of preparation, and carry out synchronous in length and breadth to twice biaxial tension at 350 DEG C.First time, rate of extension was 20m/min, and second time rate of extension is 5m/min, and twice stretching time is spaced apart 10s.
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization is 80s in the time of 340 DEG C of thermal finalizations.
The microporous barrier thickness prepared as stated above is 0.1 micron, and thickness is even, and aperture is 10 microns, and uniform pore diameter, longitudinal contraction rate is 3.5%, and lateral shrinkage is 3%, good stability of the dimension.
Embodiment 4
(1) melt extrude diaphragm: be 350 DEG C by this fluororesin at extruder temperature, die head temperature is under the condition of 390 DEG C, by melt extruding the diaphragm of preparation biaxial tension.
(2) twice biaxial tension: by the cooling of the diaphragm of preparation, and carry out synchronous in length and breadth to twice biaxial tension at 210 DEG C.First time, longitudinal stretching speed was 10m/min, and cross directional stretch speed is 8m/min, and second time longitudinal stretching speed is 2m/min, and horizontal line rate of extension is 1m/min, and twice stretching time is spaced apart 10s.
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization is 80s in the time of 300 DEG C of thermal finalizations.
The microporous barrier thickness prepared as stated above is 0.1 micron, and thickness is even, and aperture is 0.1 micron, and uniform pore diameter, longitudinal contraction rate is 4%, and lateral shrinkage is 3.5%, good stability of the dimension.
The perfluorinated resin that embodiment 1-4 adopts is perfluor sulfonyl base vinyl ethers, tetrafluoroethene and hexafluoropropylene copolymer.
Embodiment 5
(1) melt extrude diaphragm: be 260 DEG C by this fluororesin at extruder temperature, die head temperature is under the condition of 300 DEG C, by melt extruding the diaphragm of preparation biaxial tension.
(2) twice biaxial tension: by the cooling of the diaphragm of preparation, and carry out synchronous in length and breadth to twice biaxial tension at 180 DEG C.First time, rate of extension was 5m/min, and second time rate of extension is 1m/min, and twice stretching time is spaced apart 30s.
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization is 20s in the time of 280 DEG C of thermal finalizations.
The microporous barrier thickness prepared as stated above is 15 microns, and thickness is even, and aperture is 0.2 micron, and uniform pore diameter, longitudinal contraction rate is 5%, and lateral shrinkage is 4%, good stability of the dimension.
Embodiment 6
(1) melt extrude diaphragm: be 315 DEG C by this fluororesin at extruder temperature, die head temperature is under the condition of 375 DEG C, by melt extruding the diaphragm of preparation biaxial tension.
(2) twice biaxial tension: by the cooling of the diaphragm of preparation, and carry out synchronous in length and breadth to twice biaxial tension at 260 DEG C.First time, rate of extension was 10m/min, and second time rate of extension is 3m/min, and twice stretching time is spaced apart 60s.
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization is 50s in the time of 320 DEG C of thermal finalizations.
The microporous barrier thickness prepared as stated above is 5 microns, and thickness is even, and aperture is 4.5 microns, and uniform pore diameter, longitudinal contraction rate is 4.5%, and lateral shrinkage is 3%, good stability of the dimension.
Embodiment 7
(1) melt extrude diaphragm: be 345 DEG C by this fluororesin at extruder temperature, die head temperature is under the condition of 395 DEG C, by melt extruding the diaphragm of preparation biaxial tension.
(2) twice biaxial tension: by the cooling of the diaphragm of preparation, and carry out synchronous in length and breadth to twice biaxial tension at 350 DEG C.First time, rate of extension was 20m/min, and second time rate of extension is 5m/min, and twice stretching time is spaced apart 10s.
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization is 80s in the time of 340 DEG C of thermal finalizations.
The microporous barrier thickness prepared as stated above is 0.1 micron, and thickness is even, and aperture is 9.5 microns, and uniform pore diameter, longitudinal contraction rate is 3.5%, and lateral shrinkage is 3%, good stability of the dimension.
Embodiment 8
(1) melt extrude diaphragm: be 345 DEG C by this fluororesin at extruder temperature, die head temperature is under the condition of 385 DEG C, by melt extruding the diaphragm of preparation biaxial tension.
(2) twice biaxial tension: by the cooling of the diaphragm of preparation, and carry out synchronous in length and breadth to twice biaxial tension at 210 DEG C.First time, longitudinal stretching speed was 10m/min, and cross directional stretch speed is 8m/min, and second time longitudinal stretching speed is 2m/min, and horizontal line rate of extension is 1m/min, and twice stretching time is spaced apart 10s.
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization is 80s in the time of 300 DEG C of thermal finalizations.
The microporous barrier thickness prepared as stated above is 0.1 micron, and thickness is even, and aperture is 0.1 micron, and uniform pore diameter, longitudinal contraction rate is 4%, and lateral shrinkage is 3%, good stability of the dimension.
The perfluorinated resin that embodiment 5-8 adopts is perfluor sulfonyl base vinyl ethers, tetrafluoroethene and alkyl vinyl ether co-polymer.
Embodiment 9
The perfluor microporous barrier with ion exchanging function more than prepared can be widely used in the reinforcing material of PEM and Membrane Used In Chlor-alkali Cell and other films.
Claims (7)
1. there is a preparation method for the microporous barrier of ion exchanging function, it is characterized in that step is as follows:
(1) diaphragm is melt extruded: by there is the fluororesin of ion exchanging function by melt extruding, prepare diaphragm;
(2) twice biaxial tension: the diaphragm of preparation is carried out synchronous in length and breadth to twice biaxial tension;
(3) thermal finalization: biaxial stretching film prepared by step (2) is carried out thermal finalization, to obtain final product;
The fluororesin with ion exchanging function described in step (1) is the perfluorinated resin with sulfonyl fluoride group.
2. the preparation method with the microporous barrier of ion exchanging function according to claim 1, is characterized in that perfluor sulfonyl base vinyl ethers, tetrafluoroethene and hexafluoropropene monomer or perfluor sulfonyl base vinyl ethers, tetrafluoroethene and alkyl vinyl ether are caused combined polymerization through free radical and prepare by the described perfluorinated resin with sulfonyl fluoride group under dispersant, solvent and initator exist.
3. the preparation method with the microporous barrier of ion exchanging function according to claim 1, it is characterized in that the ion exchange capacity value with the fluororesin of ion exchanging function described in step (1) is 0.10-0.45mmol/g, is 5-50g/10min the melt flow index of 372 DEG C.
4. the preparation method with the microporous barrier of ion exchanging function according to claim 1, is characterized in that the melt temperature described in step (1) is 200-400 DEG C.
5. the preparation method with the microporous barrier of ion exchanging function according to claim 1, is characterized in that the biaxial tension temperature described in step (2) is 180-350 DEG C.
6. the preparation method with the microporous barrier of ion exchanging function according to claim 1, it is characterized in that the rate of extension of the biaxial tension described in step (2) is 1-20m/min, the draw ratio of biaxial tension is 1-500, and the time interval that biaxial tension stretches at every turn is 1-60 second.
7. the preparation method with the microporous barrier of ion exchanging function according to claim 1, is characterized in that the heat setting temperature described in step (3) is 260-380 DEG C, and the time of thermal finalization is 20-80 second.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003596A (en) * | 2006-12-25 | 2007-07-25 | 山东东岳神舟新材料有限公司 | Perfluoro - resin with ion exchange, and application |
| CN101768236A (en) * | 2009-12-25 | 2010-07-07 | 山东东岳神舟新材料有限公司 | Perfluorinated ion exchange resin as well as preparation method and application thereof |
| CN103183884A (en) * | 2011-12-28 | 2013-07-03 | 山东东岳高分子材料有限公司 | Fluoride-containing microporous membrane and preparation method thereof |
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| WO2011156934A1 (en) * | 2010-06-18 | 2011-12-22 | 山东东岳神舟新材料有限公司 | Proton exchange membrane, its preparing method and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003596A (en) * | 2006-12-25 | 2007-07-25 | 山东东岳神舟新材料有限公司 | Perfluoro - resin with ion exchange, and application |
| CN101768236A (en) * | 2009-12-25 | 2010-07-07 | 山东东岳神舟新材料有限公司 | Perfluorinated ion exchange resin as well as preparation method and application thereof |
| CN103183884A (en) * | 2011-12-28 | 2013-07-03 | 山东东岳高分子材料有限公司 | Fluoride-containing microporous membrane and preparation method thereof |
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