CN107978779A - A kind of fuel cell selfreparing anion-exchange membrane and preparation method thereof - Google Patents
A kind of fuel cell selfreparing anion-exchange membrane and preparation method thereof Download PDFInfo
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- CN107978779A CN107978779A CN201711152612.2A CN201711152612A CN107978779A CN 107978779 A CN107978779 A CN 107978779A CN 201711152612 A CN201711152612 A CN 201711152612A CN 107978779 A CN107978779 A CN 107978779A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1065—Polymeric electrolyte materials characterised by the form, e.g. perforated or wave-shaped
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/14—Monomers containing only one unsaturated aliphatic radical containing one ring substituted by heteroatoms or groups containing heteroatoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/42—Nitriles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/42—Nitriles
- C08F220/44—Acrylonitrile
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1067—Polymeric electrolyte materials characterised by their physical properties, e.g. porosity, ionic conductivity or thickness
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
- H01M8/1069—Polymeric electrolyte materials characterised by the manufacturing processes
- H01M8/1072—Polymeric electrolyte materials characterised by the manufacturing processes by chemical reactions, e.g. insitu polymerisation or insitu crosslinking
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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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Abstract
The invention discloses a kind of fuel cell selfreparing anion-exchange membrane and preparation method thereof, this method includes mixing trimethyl [1 (trifluoromethyl) vinyl] silane, polymerized monomer, 4 vinyl benzyl chlorides, tetra allyl ammonium chloride, emulsifying agent, it is placed in the microwave reaction kettle under nitrogen or atmosphere of inert gases, reacted 15 25 minutes at 60 90 DEG C, generation polymerisation, obtains polymer film；Again by polymer film progress ion exchange and etc..The fuel cell selfreparing anion-exchange membrane of the present invention, preparation method is simple and practicable, and mechanical performance, alkali resistance and chemical stability are more excellent, conductivity higher, and can automatically repair and reuse after degraded in use, so as to prolong the service life, the problem of wasting is reduced.
Description
Technical field
The invention belongs to technical field of polymer materials, is related to a kind of fuel cell component, and in particular to a kind of fuel electricity
Pond selfreparing anion-exchange membrane and preparation method thereof.
Background technology
Anion-exchange membrane fuel cells are a kind of clean energy resource devices, and chemical energy directly can be converted into electrical appliance by it to be made
Electric energy, has the advantages that energy transformation ratio is high, power density is high, it is fast, pollution-free to start, it is wide to cause researchers in the industry
General concern.
Anion-exchange membrane is one of critical component of anion-exchange membrane fuel cells, it plays resistance in a fuel cell
Every the effect of fuel and transmission anion, the quality of its performance directly affects the working performance and service life of fuel cell.It is cloudy
Ion-exchange membrane fuel cell with anion-exchange membrane need to have good mechanical performance, heat endurance, chemical stability and
Alkali resistance, it is also necessary to which there is high ionic conductivity.
Conventional anion exchange membrane is more relatively low in the presence of thermally and chemically stability, the polymer under higher temperature or alkaline condition
In quaternary ammonium group be easy to degrade, cause ion exchange capacity to decline so that monoblock film service life shortens, shape
Into the problem of waste.
Therefore, in the industry there is an urgent need for a kind of mechanical performance, alkaline resistance properties and chemical stability are excellent, the high anion of conductivity is handed over
Change film.
The content of the invention
In order to overcome the defects of the prior art, the present invention provide a kind of fuel cell with selfreparing anion-exchange membrane and
Its preparation method, the preparation method is simple and practicable, and not high to equipment requirement, raw material is easy to get, cheap, passes through this preparation side
Disclosed anion-exchange membrane mechanical performance, alkali resistance and chemistry are steady than in the prior art for the anion-exchange membrane that method is prepared
It is qualitative more excellent, conductivity higher, and can automatically repair, reuse, so as to extend using the longevity after degraded in use
Life, reduces the problem of wasting.
To achieve the above object of the invention, the technical solution adopted by the present invention is a kind of fuel cell selfreparing anion
The preparation method of exchange membrane, includes the following steps：
1) preparation of polymer film：By trimethyl [1- (trifluoromethyl) vinyl] silane, polymerized monomer, 4- vinyl benzyls
Chlorine, tetra allyl ammonium chloride, emulsifying agent mixing, are placed in the microwave reaction kettle under nitrogen or atmosphere of inert gases, in 60-90
Reacted 15-25 minutes at DEG C, polymerisation occurs, obtains polymer film；
2) ion exchange：It is by the mass fraction that the polymer film being prepared by step 1) is immersed at 60-70 DEG C
It is rear to take out when soaking that 12-24 is small in deionized water again when 65-75 is small in the potassium hydroxide solution of 5-10%, take out, in 60-
When drying 12-18 is small in 70 DEG C of vacuum drying chamber；
Wherein, trimethyl described in step 1) [1- (trifluoromethyl) vinyl] silane, polymerized monomer, 4- vinyl benzyls
Chlorine, tetra allyl ammonium chloride, the mass ratio of emulsifying agent are (2-3)：(2-3)：(1-2)：(1-2)：(0.1-0.3)；
The polymerization type monomer is selected from acrylonitrile, styrene, α-methylstyrene, methacrylonitrile, sulfonated phenylethylene, eight
One or more in fluorobenzene ethene, methyl methacrylate, ethyl acrylate or methyl sulfonated phenylethylene；
The emulsifying agent is selected from neopelex, polyoxypropylene polyethylene glycols ether, nonylphenol polyoxyethylene ether
In one or more；
One or more of the inert gas in neon, helium, argon gas；
A kind of fuel cell selfreparing anion-exchange membrane, is handed over using a kind of fuel cell selfreparing anion
The preparation method for changing film is prepared；
A kind of anion-exchange membrane fuel cells, polymerization is used as using fuel cell selfreparing anion-exchange membrane
Thing dielectric film.
It is using beneficial effect caused by above-mentioned technical proposal：
1) a kind of fuel cell provided by the invention is simple and practicable with the preparation method of selfreparing anion-exchange membrane, pair sets
Standby of less demanding, raw material is easy to get, cheap.
2) a kind of fuel cell selfreparing anion-exchange membrane provided by the invention, in molecular structure at the same time containing fluorine and
Element silicon, possesses the excellent properties of fluorine silicon materials so that film has preferable mechanical mechanics property, chemical stability, thermostabilization
Property and alkali resistance.
3) a kind of fuel cell selfreparing anion-exchange membrane provided by the invention, contains cl radical in molecular structure,
This season amine groups degrade in alkaline conditions scission of link when, cl radical can it is spontaneous with degraded after product amino react, play restorative
The effect of energy, so as to extend the service life of film, reduces and wastes.
4) a kind of fuel cell selfreparing anion-exchange membrane provided by the invention, raw material tetra allyl ammonium chloride are dividing
Play the role of crosslinking agent in minor structure at the same time, ion-exchange group is provided, form three-dimensional net structure so that polymer film machine
Tool excellent performance, chemically and thermally mechanical stability is good, and forms ion transfer channels, is conducive to ion transport, improves ion and leads
Electric rate.
Embodiment
In order to make those skilled in the art more fully understand technical scheme, and make the present invention features described above,
Purpose and advantage become apparent from understandable, and with reference to embodiment, the present invention is described further.Embodiment is only used for
It is bright the present invention rather than limit the scope of the invention.
Raw material used in the following embodiments of the present invention comes from Haiquan sunrise foreign trade Co., Ltd.
Embodiment 1
A kind of fuel cell preparation method of selfreparing anion-exchange membrane, includes the following steps：
1) preparation of polymer film：By trimethyl [1- (trifluoromethyl) vinyl] silane 2g, acrylonitrile 2g, 4- vinyl
Benzyl chloride 1g, tetra allyl ammonium chloride 1g, neopelex 0.1g mixing, are placed in microwave reaction kettle under nitrogen atmosphere
In, reacted 15 minutes at 60 DEG C, polymerisation occurs, obtains polymer film；
2) ion exchange：The mass fraction polymer film being prepared by step 1) being immersed at 60 DEG C is 5%
Potassium hydroxide solution in 65 it is small when, it is rear take out soak again in deionized water 12 it is small when, take out, in 60 DEG C of vacuum drying chamber
When middle drying 12 is small；
A kind of fuel cell selfreparing anion-exchange membrane, is handed over using a kind of fuel cell selfreparing anion
The preparation method for changing film is prepared；
A kind of anion-exchange membrane fuel cells, polymerization is used as using fuel cell selfreparing anion-exchange membrane
Thing dielectric film.
Embodiment 2
A kind of fuel cell preparation method of selfreparing anion-exchange membrane, includes the following steps：
1) preparation of polymer film：By trimethyl [1- (trifluoromethyl) vinyl] silane 2.3g, octafluorostyrene
2.5g, 4- vinyl benzyl chloride 1.2g, tetra allyl ammonium chloride 1.6g, polyoxypropylene polyethylene glycols ether 0.2g mixing, are placed at
In microwave reaction kettle under argon atmosphere, reacted 20 minutes at 70 DEG C, polymerisation occurs, obtains polymer film；
2) ion exchange：The mass fraction polymer film being prepared by step 1) being immersed at 64 DEG C is 7%
Potassium hydroxide solution in 69 it is small when, it is rear take out soak again in deionized water 15 it is small when, take out, in 65 DEG C of vacuum drying chamber
When middle drying 14 is small；
A kind of fuel cell selfreparing anion-exchange membrane, is handed over using a kind of fuel cell selfreparing anion
The preparation method for changing film is prepared；
A kind of anion-exchange membrane fuel cells, polymerization is used as using fuel cell selfreparing anion-exchange membrane
Thing dielectric film.
Embodiment 3
A kind of fuel cell preparation method of selfreparing anion-exchange membrane, includes the following steps：
1) preparation of polymer film：By trimethyl [1- (trifluoromethyl) vinyl] silane 2.8g, α-methylstyrene 2g,
4- vinyl benzyl chlorides 1.8g, tetra allyl ammonium chloride 2g, nonylphenol polyoxyethylene ether 0.25g mixing, are placed under neon atmosphere
Microwave reaction kettle in, reacted 22 minutes at 80 DEG C, occur polymerisation, obtain polymer film；
2) ion exchange：The mass fraction polymer film being prepared by step 1) being immersed at 68 DEG C is 9%
Potassium hydroxide solution in 72 it is small when, it is rear take out soak again in deionized water 22 it is small when, take out, in 68 DEG C of vacuum drying chamber
When middle drying 16 is small；
A kind of fuel cell selfreparing anion-exchange membrane, is handed over using a kind of fuel cell selfreparing anion
The preparation method for changing film is prepared；
A kind of anion-exchange membrane fuel cells, polymerization is used as using fuel cell selfreparing anion-exchange membrane
Thing dielectric film.
Embodiment 4
A kind of fuel cell preparation method of selfreparing anion-exchange membrane, includes the following steps：
1) preparation of polymer film：By trimethyl [1- (trifluoromethyl) vinyl] silane 3g, methacrylonitrile 3g, 4-
Vinyl benzyl chloride 1g, tetra allyl ammonium chloride 2g, neopelex 0.3g mixing, are placed in microwave under nitrogen atmosphere
In reaction kettle, reacted 25 minutes at 90 DEG C, polymerisation occurs, obtains polymer film；
2) ion exchange：The mass fraction polymer film being prepared by step 1) being immersed at 70 DEG C is 10%
Potassium hydroxide solution in 75 it is small when, it is rear take out soak again in deionized water 24 it is small when, take out, in 70 DEG C of vacuum drying chamber
When middle drying 18 is small；
A kind of fuel cell selfreparing anion-exchange membrane, is handed over using a kind of fuel cell selfreparing anion
The preparation method for changing film is prepared；
A kind of anion-exchange membrane fuel cells, polymerization is used as using fuel cell selfreparing anion-exchange membrane
Thing dielectric film.
Comparative example
Commercially available conventional homogeneous anion-exchange membrane, purchased from Beijing court of a feudal ruler profit membrane technology exploitation limited company.
Correlated performance test is carried out to sample obtained by above-described embodiment 1-4 and comparative example, test result as shown in table 1,
Test method is as follows,
(1) tensile strength is tested：According to GB/T 1040-2006《Plastic tensile method for testing performance》Tested；
(2) electrical conductivity：The impedance of the anion-exchange membrane of preparation, is in electrochemical operation using two electrode AC impedance methods
Stand what is measured on (Zahner IM6 EX), test frequency is 1Hz~1MHz.Electrical conductivity test is to fill the appearance of deionized water
Measured in device, this is to ensure that the relative humidity of film is 100%, and control temperature at 30 DEG C.Tested in this temperature spot
Before, sample keeps constant temperature 30min at this temperature, and electrical conductivity is calculated according to following equation：
Wherein, σ is electrical conductivity (S cm-1), l is the distance between two electrodes (cm), and R is the AC impedance of institute's sample, S
For the cross-sectional area of film.
(3) oxidation stability：The oxidation stability of the anion-exchange membrane of preparation is by the way that film is immersed in 70 DEG C
Fenton reagent (contains 4ppm Fe2+3% hydrogen peroxide solution) in 20 it is small when, weigh and calculate film weight retention come
Weigh.Calculation formula is：Retention rate=(immersion caudacoria weight-immersion cephacoria weight)/immersion cephacoria weight × 100%.
(4) alkali resistance：The alkali resistance test of film is to be immersed in film in the 1mol/L KOH aqueous solutions at 80 DEG C 60 days, meter
The change rate of electrical conductivity before and after immersion is calculated to weigh.Calculation formula is：Change rate=(conductance after electrical conductivity-immersion before immersion
Rate)/immersion before electrical conductivity × 100%.
As it can be seen from table 1 fuel cell disclosed by the invention selfreparing anion-exchange membrane has preferable machinery
Performance, inoxidizability and alkali resistance, and electrical conductivity is also higher than conventional anion exchange membrane, meets anion-exchange membrane fuel electricity
Pond requirement.
1 embodiment of table and comparative example performance
The foregoing is only a preferred embodiment of the present invention, not makees limitation in any form to the present invention；It is all
The those of ordinary skill of the industry can be shown in by specification and described above and swimmingly implement the present invention；It is but all familiar
Professional and technical personnel without departing from the scope of the present invention, makes using disclosed above technology contents
A little variation, modification and evolution equivalent variations, be the present invention equivalent embodiment；Meanwhile all realities according to the present invention
Variation, modification and evolution of any equivalent variations that matter technology makees above example etc., still fall within the technology of the present invention
Within the protection domain of scheme.
Claims (8)
1. a kind of fuel cell preparation method of selfreparing anion-exchange membrane, it is characterised in that include the following steps：
1) preparation of polymer film：By trimethyl [1- (trifluoromethyl) vinyl] silane, polymerized monomer, 4- vinyl benzyl chlorides,
Tetra allyl ammonium chloride, emulsifying agent mixing, are placed in the microwave reaction kettle under nitrogen or atmosphere of inert gases, at 60-90 DEG C
Lower reaction 15-25 minutes, occurs polymerisation, obtains polymer film；
2) ion exchange：The mass fraction that the polymer film being prepared by step 1) is immersed at 60-70 DEG C is 5-
It is rear to take out when soaking that 12-24 is small in deionized water again when 65-75 is small in 10% potassium hydroxide solution, take out, in 60-70
DEG C vacuum drying chamber in dry 12-18 it is small when.
2. a kind of preparation method of fuel cell selfreparing anion-exchange membrane according to claim 1, its feature exist
In trimethyl described in step 1) [1- (trifluoromethyl) vinyl] silane, polymerized monomer, 4- vinyl benzyl chlorides, tetraallyl
Ammonium chloride, the mass ratio of emulsifying agent are (2-3)：(2-3)：(1-2)：(1-2)：(0.1-0.3).
3. a kind of preparation method of fuel cell selfreparing anion-exchange membrane according to claim 1, its feature exist
In the polymerization type monomer is selected from acrylonitrile, styrene, α-methylstyrene, methacrylonitrile, sulfonated phenylethylene, octafluoro benzene
One or more in ethene, methyl methacrylate, ethyl acrylate or methyl sulfonated phenylethylene.
4. a kind of preparation method of fuel cell selfreparing anion-exchange membrane according to claim 1, its feature exist
In, the emulsifying agent in neopelex, polyoxypropylene polyethylene glycols ether, nonylphenol polyoxyethylene ether one
Kind is several.
5. a kind of preparation method of fuel cell selfreparing anion-exchange membrane according to claim 1, its feature exist
In one or more of the inert gas in neon, helium, argon gas.
6. a kind of fuel cell selfreparing anion-exchange membrane, it is characterised in that using any one of claim 1-5 described one
Kind fuel cell is prepared with the preparation method of selfreparing anion-exchange membrane.
7. a kind of fuel cell application process of selfreparing anion-exchange membrane, it is characterised in that using described in claim 6
Polymer dielectric film of the fuel cell by the use of selfreparing anion-exchange membrane as battery.
8. a kind of anion-exchange membrane fuel cells, it is characterised in that cloudy with selfreparing using fuel cell described in claim 6
Amberplex is as polymer dielectric film.
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| CN109265616A (en) * | 2018-08-01 | 2019-01-25 | 湖南辰砾新材料有限公司 | A kind of insulating foam and preparation method thereof |
| CN114976477A (en) * | 2022-06-02 | 2022-08-30 | 界首市天鸿新材料股份有限公司 | Tape casting process of high-performance lithium battery diaphragm |
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| CN114976477A (en) * | 2022-06-02 | 2022-08-30 | 界首市天鸿新材料股份有限公司 | Tape casting process of high-performance lithium battery diaphragm |
| CN114976477B (en) * | 2022-06-02 | 2023-09-15 | 界首市天鸿新材料股份有限公司 | Tape casting forming process of high-performance lithium battery diaphragm |
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| CN107978779B (en) | 2020-03-27 |
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