CN109301295A - A kind of inorfil enhancing fuel battery proton exchange film and preparation method thereof - Google Patents
A kind of inorfil enhancing fuel battery proton exchange film and preparation method thereof Download PDFInfo
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- CN109301295A CN109301295A CN201811042142.9A CN201811042142A CN109301295A CN 109301295 A CN109301295 A CN 109301295A CN 201811042142 A CN201811042142 A CN 201811042142A CN 109301295 A CN109301295 A CN 109301295A
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- inorfil
- proton exchange
- fuel battery
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- exchange film
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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
- H01M8/1086—After-treatment of the membrane other than by polymerisation
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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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- 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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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fuel Cell (AREA)
Abstract
The present invention relates to a kind of inorfil enhancing fuel battery proton exchange films and preparation method thereof, belong to fuel battery proton exchange film field.A kind of preparation method of inorfil enhancing fuel battery proton exchange film, specially a, is added magnetic-particle after melting inorganic material, the slurry after melting is prepared as to load the inorfil for the particle that is magnetic by spinneret；B, the load prepared in step a is magnetic in the inorfil and perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoropropene and auxiliary agent addition organic solution of particle, it is stirred by ultrasonic at 40 DEG C, form suspension, suspension is subjected to casting film on base material surface layer in the case where externally-applied magnetic field is controlled, then membrane material is placed in vacuum drying oven drying, obtains required inorfil enhancing fuel battery proton exchange film.A kind of preparation method simple process of inorfil enhancing fuel battery proton exchange film of the invention, intensity is high, cost is relatively low, film water retention property is good, conductivity is high.
Description
Technical field
The present invention relates to a kind of inorfil enhancing fuel battery proton exchange films and preparation method thereof, belong to fuel cell
Proton exchange membrane field.
Background technique
Fuel cell is since 1966 begin to use the nafion perfluorosulfonic acid proton exchange film of E.I.Du Pont Company, Ge Xiangji
Art gradually tends to be mature.The chemical stability of Nafion membrane is very good, and the fuel cell for long-life, high power density provides
Strong support, but still there are many disadvantages, one is expensive, the sulfonation of raw material is extremely complex with flaorination process, leads
It causes its product price high, lacks competitiveness in the competition of battery industry；The second is the use environment of membrane material is relatively severe
It carves, needs at 100 DEG C or less and suitable humidity range works, once temperature is excessively high and moisture content is excessive, will lead to
The proton conductivity of membrane material is substantially reduced and degrades；The third is permeability with higher for non-hydrogen fuel, limits
The scope of application of membrane material.
Moisture content is depended on for the conductivity control of membrane material at present, it is general for the control of moisture content in membrane material
It is the doping of inorganic hydrophilic particle, such as SiO2, TiO2, ZrO2 to be carried out to membrane material, but pass through one-dimensional granulated mostly all over method
State is doped, and has a certain impact to the mechanical performance tool of membrane material, membrane material is caused to crack during making and using.Therefore
Its mechanical and physical performance application value with higher in production is kept and improved while improving membrane material water retention property.
Application No. is 201210189858.8 Chinese patents to disclose a kind of composite proton exchange used for high-temperature fuel cell
Film and preparation method thereof.The exchange membrane is the compound proton exchange membrane based on UV laser ablation polyimide matrix, by with equal
Even, orderly straight-through pore structure polyimide-based body thin film, dipping prepare perfluorinated sulfonic resin film composition.Preparation method is to use
Straight-through pore structure of the UV laser etching techniques in the preparation of Kapton surface uniformly, orderly, mentions by soda acid hydrophilic treated
Its high hydrophilicity, then perfluor sulfoacid resin solution is filled into treated polyimide-based body thin film, subsequently heat-treated
To the compound proton exchange membrane of UV laser ablation polyimide matrix.Prepared compound proton exchange membrane has high temperature dwell aqueous
The features such as energy, high mechanical strength, gas permeability are low, swelling stress is low, especially suitable for Proton Exchange Membrane Fuel Cells.
Application No. is 200710032311.6 Chinese patents to disclose a kind of direct methanol fuel cell proton exchange
The preparation method of film.Polyether-ether-ketone is added progress sulfonating reaction in the concentrated sulfuric acid first and obtains sulfonated polyether-ether-ketone by this method；So
Sulfonated polyether-ether-ketone is dissolved in organic solvent afterwards, N is added, N '-carbonyl dimidazoles are added coupling agent after stirring 1~3 hour and stir
It mixes reaction 1.5~4 hours, adds inorganic crosslinking agent and reacted at 50~80 DEG C, proton conductor is then added and continues temperature herein
The lower reaction of degree obtains sulfonated polyether-ether-ketone/inorganic crosslinking agent/proton conductor mixed solution；Finally by sulfonated polyether-ether-ketone/nothing
Machine crosslinking agent/proton conductor mixture solution film forming, dry, demoulding is to obtain the direct methanol fuel cell proton
Exchange membrane.The features good methanol diffusion resistance of the film, at low cost, proton conductivity is high, the swelling behavior of water resistant is good under higher temperature.The preparation
Method is relatively simple, and the prices of raw materials are cheap, and production cost is relatively low.
Application No. is 201710800567.0 Chinese patents to disclose the preparation side of a proton exchanging film fuel battery
Method, in particular to a kind of preparation method of silicon substrate integration Proton Exchange Membrane Fuel Cells.Using silica micro-/ nano ball etc.
As template, double air-flows are passed through etching gas SF simultaneously6With auxiliary gas O2Deng being carried out by inductively coupled plasma etching machine
Deep silicon etching obtains three-dimensional silica micro-/ nano column array.By structure optimization, such as introduce conductive layer and scribing processing, Ji Kezuo
For the flow field of Proton Exchange Membrane Fuel Cells.Based on above-mentioned silicon substrate flow field, further integrated gas diffusion layers and Catalytic Layer are realized
The building of integrated silicon substrate Proton Exchange Membrane Fuel Cells.The simple and existing silicon substrate of the fuel cell preparation method is partly led
Body technology is mutually compatible with, and power density is higher, has potential application in fields such as the power supply supplies of micro-/nano electromechanical systems.
Above-mentioned patent is the modification to proton exchange membrane, does not solve to solve proton exchange membrane water retention property and machine simultaneously
The problem of tool physical property.
Summary of the invention
For disadvantages described above, the present invention proposes that a kind of inorfil enhances fuel battery proton exchange film and its preparation side
Method.
A kind of preparation method of inorfil enhancing fuel battery proton exchange film, sequentially includes the following steps:
A, magnetic-particle is added after melting inorganic material, the slurry after melting is prepared as to load the particle that is magnetic by spinneret
Inorfil；
B, by the load prepared in step a be magnetic particle inorfil and perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoropropene
And auxiliary agent is added in organic solution, is stirred by ultrasonic at 40 DEG C, forms suspension, will hang in the case where externally-applied magnetic field is controlled
Turbid carries out casting film on base material surface layer, and externally-applied magnetic field is parallel with film is poured, and is then placed in vacuum drying oven membrane material
Drying obtains required inorfil enhancing fuel battery proton exchange film.
Wherein, the weight ratio of inorganic material, magnetic-particle, perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoropropene and auxiliary agent is
10-25:3-5:10-18:20-40:15-40:3-8。
Be added magnetic-particle after inorganic material being melted in step a of the present invention, its purpose is to the slurries after melting
It is prepared as loading the inorfil for the particle that is magnetic by spinneret.
Wherein, inorganic material selects the glass powder for being easy into fiber.
In step b of the present invention by the load of preparation be magnetic particle inorfil and perfluorinated sulfonic acid monomer, tetrafluoroethene,
Hexafluoropropene and auxiliary agent are added in organic solution, are stirred by ultrasonic at 40 DEG C, form suspension, wherein perfluorinated sulfonic acid list
Body, tetrafluoroethene, hexafluoropropene and auxiliary agent purpose be to prepare perfluorinated sulfonic resin.The dosage of organic solution therein is according to specific
Viscosity requirement addition when pouring film uses.
Technical advantage of the invention: after inorfil carried magnetic particle, keep externally-applied magnetic field parallel with film is poured, in magnetic
Under field condition load be magnetic particle inorfil inside resin orientation having the same accumulated, protected improving membrane material
While aqueous energy, inorfil can serve as the skeleton of membrane material, be improved the mechanical performance of membrane material.
Further, magnetic-particle is nanometer iron-based magnetic-particle in step a.
Further, auxiliary agent is thickener or stabilizer in step b, and thickener is ethylene glycol, glycerine and polyethylene glycol
One of, stabilizer TritonX-100.
Further, organic solvent is one of dehydrated alcohol, isopropanol, n-butanol in step b.
Further, the temperature of vacuum drying oven is 70-100 DEG C in step b.
Further, the vacuum drying time is 36-50h in step b.
The invention solves second technical problem be to provide a kind of inorfil enhancing fuel battery proton exchange film,
It is prepared by above-mentioned preparation method.
Compared with prior art, the invention has the following beneficial effects:
1, after inorfil carried magnetic particle, outside plus under magnetic field condition there is inorfil inside perfluorinated sulfonic resin
Identical orientation is accumulated, and while improving membrane material water retention property, inorfil can serve as the skeleton of membrane material, make membrane material
Mechanical performance be improved.
A kind of inorfil enhancing fuel battery proton exchange film stability 2, being prepared using the method for the present invention is high,
Mechanical and physical performance is good.
3, the preparation method simple process of a kind of inorfil of the invention enhancing fuel battery proton exchange film, cost
It is lower, film water retention property is good, conductivity is high.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
A kind of inorfil of embodiment 1 enhances fuel battery proton exchange film
Raw material is taken by weight: 10 parts of glass micro mist, 3 parts of nanometer Fe 3 O 4 magnetic particle, 10 parts of perfluorinated sulfonic acid monomer, four
20 parts of vinyl fluoride, 15 parts of hexafluoropropene, 3 parts of auxiliary agent, appropriate organic solvent.
Specific preparation method sequentially includes the following steps:
A, after melting glass micro mist, magnetic-particle is added under nitrogen protection, the slurry after melting is prepared as by spinneret
Load the inorfil for the particle that is magnetic；
B, by the load prepared in step a be magnetic particle inorfil and perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoropropene
And auxiliary agent is added in organic solution, is stirred by ultrasonic at 40 DEG C, forms suspension, will hang in the case where externally-applied magnetic field is controlled
Turbid carries out casting film on base material surface layer, and magnetic direction is parallel with film is poured, and is then placed in vacuum drying oven membrane material,
In 70 DEG C of drying 36h, required inorfil enhancing fuel battery proton exchange film is obtained.Wherein, auxiliary agent is ethylene glycol；It is organic
Solvent is dehydrated alcohol.
A kind of inorfil of embodiment 2 enhances fuel battery proton exchange film
Raw material is taken by weight: 25 parts of glass micro mist, 5 parts of ferriferrous oxide nano magnetic-particle, 18 parts of perfluorinated sulfonic acid monomer, four
40 parts of vinyl fluoride, 40 parts of hexafluoropropene, 8 parts of auxiliary agent, appropriate organic solvent.
Specific preparation method sequentially includes the following steps:
A, magnetic-particle is added after melting glass micro mist, the slurry after melting is negative by spinneret preparation under nitrogen protection
It is loaded with the inorfil of magnetic-particle；
B, by the load prepared in step a be magnetic particle inorfil and perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoro third
Alkene and auxiliary agent are added in organic solution, are stirred by ultrasonic at 40 DEG C, and suspension is formed, will in the case where externally-applied magnetic field is controlled
Suspension carries out casting film on base material surface layer, and externally-applied magnetic field direction is parallel with film is poured, and membrane material is then placed in vacuum
In baking oven, in 100 DEG C of drying 50h, required inorfil enhancing fuel battery proton exchange film is obtained.Wherein, auxiliary agent is
TritonX-100；Organic solvent is n-butanol.
A kind of inorfil of embodiment 3 enhances fuel battery proton exchange film
Raw material is taken by weight: 20 parts of glass micro mist, 3 parts of ferriferrous oxide nano magnetic-particle, 15 parts of perfluorinated sulfonic acid monomer, four
20 parts of vinyl fluoride, 15 parts of hexafluoropropene, 5 parts of auxiliary agent, appropriate organic solvent.
Specific preparation method sequentially includes the following steps:
A, nano magnetic particle is added after melting glass micro mist, under nitrogen protection prepares the slurry after melting by spinneret
It is negative and is loaded with the inorfil of magnetic-particle；
B, by the load prepared in step a be magnetic particle inorfil and perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoropropene
And auxiliary agent is added in organic solution, is stirred by ultrasonic at 40 DEG C, forms suspension, will hang in the case where externally-applied magnetic field is controlled
Turbid carries out casting film on base material surface layer, and externally-applied magnetic field direction is parallel with film is poured, and membrane material is then placed in vacuum and is dried
In case, in 70 DEG C of drying 40h, required inorfil enhancing fuel battery proton exchange film is obtained.Wherein, auxiliary agent is thickener
Glycerine；Organic solvent is dehydrated alcohol.
A kind of inorfil of embodiment 4 enhances fuel battery proton exchange film
Raw material is taken by weight: 25 parts of glass micro mist, 4 parts of ferriferrous oxide nano magnetic-particle, 18 parts of perfluorinated sulfonic acid monomer, four
30 parts of vinyl fluoride, 40 parts of hexafluoropropene, 7 parts of auxiliary agent, 35 parts of organic solvent.
Specific preparation method sequentially includes the following steps:
A, nano magnetic particle is added after melting glass micro mist, under nitrogen protection prepares the slurry after melting by spinneret
It is negative and is loaded with the inorfil of magnetic-particle；
B, by the load prepared in step a be magnetic particle inorfil and perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoropropene
And auxiliary agent is added in organic solution, is stirred by ultrasonic at 40 DEG C, forms suspension, will hang in the case where externally-applied magnetic field is controlled
Turbid carries out casting film on base material surface layer, and externally-applied magnetic field direction is parallel with film is poured, and membrane material is then placed in vacuum and is dried
In case, in 90 DEG C of drying 50h, required inorfil enhancing fuel battery proton exchange film is obtained.Wherein, auxiliary agent is
TritonX-100；Organic solvent is n-butanol.
A kind of inorfil of comparative example 1 enhances fuel battery proton exchange film
Raw material is taken by weight: 25 parts of glass micro mist, 4 parts of ferriferrous oxide nano magnetic-particle, 18 parts of perfluorinated sulfonic acid monomer, four
30 parts of vinyl fluoride, 40 parts of hexafluoropropene, 7 parts of auxiliary agent, 35 parts of organic solvent.
Specific preparation method sequentially includes the following steps:
A, nano magnetic particle is added after melting glass micro mist, under nitrogen protection prepares the slurry after melting by spinneret
It is negative and is loaded with the inorfil of magnetic-particle；
B, by the load prepared in step a be magnetic particle inorfil and perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoropropene
And auxiliary agent is added in organic solution, is stirred by ultrasonic at 40 DEG C, forms suspension, will hang in the case where externally-applied magnetic field is controlled
Turbid carries out casting film on base material surface layer, is then placed in vacuum drying oven membrane material, in 90 DEG C of drying 50h, obtains institute
The inorfil needed enhances fuel battery proton exchange film.Wherein, auxiliary agent TritonX-100；Organic solvent is n-butanol.
Comparative example 1 does not use the externally-applied magnetic field parallel with film is poured, and inorfil is not orientated accumulation, and disperses unevenness,
Influence proton exchange film strength, water-retaining property and conductivity.
Above-described embodiment 1-4 and 1 gained inorfil of comparative example are enhanced into fuel battery proton exchange film, carry out performance survey
Examination, the results are shown in Table 1:
Table 1
| Number | Proton exchange film thickness (micron) | 100 DEG C of conductivity (S/cm) | Maximum operation (service) temperature (DEG C) | Service life (year) |
| Embodiment 1 | 100 | 0.18 | 230 | 3 |
| Embodiment 2 | 100 | 0.19 | 210 | 2.5 |
| Embodiment 3 | 100 | 0.15 | 2780 | 3.5 |
| Embodiment 4 | 100 | 0.14 | 250 | 2.6 |
| Comparative example 1 | 100 | 0.07 | 190 | 1 |
Claims (8)
1. a kind of preparation method of inorfil enhancing fuel battery proton exchange film, which is characterized in that sequentially include the following steps:
A, the slurry after magnetic-particle is melted is added after melting inorganic material, then the slurry after melting is passed through into spinneret system
Standby be negative is loaded with the inorfil of magnetic-particle；
B, by the load prepared in step a be magnetic particle inorfil and perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoropropene
And auxiliary agent is added in organic solution, is stirred by ultrasonic at 40 DEG C, forms suspension, will hang in the case where externally-applied magnetic field is controlled
Turbid carries out casting film on base material surface layer, and externally-applied magnetic field is parallel with film is poured, and is then placed in vacuum drying oven membrane material
Drying obtains required inorfil enhancing fuel battery proton exchange film；
Wherein, the weight ratio of inorganic material, magnetic-particle, perfluorinated sulfonic acid monomer, tetrafluoroethene, hexafluoropropene and auxiliary agent is 10-
25:3-5:10-18:20-40:15-40:3-8。
2. a kind of preparation method of inorfil enhancing fuel battery proton exchange film according to claim 1, feature
It is, inorganic material is glass micro mist in step a.
3. a kind of preparation method of inorfil enhancing fuel battery proton exchange film according to claim 1, feature
It is, magnetic-particle is nanometer iron-based magnetic-particle in step a.
4. a kind of preparation method of inorfil enhancing fuel battery proton exchange film according to claim 1, feature
It is, auxiliary agent is thickener or stabilizer in step b, and thickener is one of ethylene glycol, glycerine and polyethylene glycol, is stablized
Agent is TritonX-100.
5. a kind of preparation method of inorfil enhancing fuel battery proton exchange film according to claim 1, feature
It is, organic solvent is one of dehydrated alcohol, isopropanol, n-butanol in step b.
6. a kind of preparation method of inorfil enhancing fuel battery proton exchange film according to claim 1, feature
It is, the temperature of vacuum drying oven is 70-100 DEG C in step b.
7. a kind of preparation method of inorfil enhancing fuel battery proton exchange film according to claim 1, feature
It is, the vacuum drying time is 36-50h in step b.
8. a kind of inorfil enhances fuel battery proton exchange film, which is characterized in that described in any item by claim 1-7
A kind of preparation method of inorfil enhancing fuel battery proton exchange film is prepared.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112117468A (en) * | 2020-08-21 | 2020-12-22 | 同济大学 | Preparation method of framework fuel cell catalyst layer |
| CN115020721A (en) * | 2022-07-12 | 2022-09-06 | 一汽解放汽车有限公司 | Membrane electrode catalytic slurry, membrane electrode, preparation method of membrane electrode and fuel cell |
-
2018
- 2018-09-07 CN CN201811042142.9A patent/CN109301295A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112117468A (en) * | 2020-08-21 | 2020-12-22 | 同济大学 | Preparation method of framework fuel cell catalyst layer |
| CN115020721A (en) * | 2022-07-12 | 2022-09-06 | 一汽解放汽车有限公司 | Membrane electrode catalytic slurry, membrane electrode, preparation method of membrane electrode and fuel cell |
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Application publication date: 20190201 |