CN107240707A - A kind of amberplex for reducing methanol fuel infiltration and preparation method thereof - Google Patents
A kind of amberplex for reducing methanol fuel infiltration and preparation method thereof Download PDFInfo
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- CN107240707A CN107240707A CN201710229197.XA CN201710229197A CN107240707A CN 107240707 A CN107240707 A CN 107240707A CN 201710229197 A CN201710229197 A CN 201710229197A CN 107240707 A CN107240707 A CN 107240707A
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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
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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
- H01M8/1074—Sol-gel processes
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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
- H01M8/1081—Polymeric electrolyte materials characterised by the manufacturing processes starting from solutions, dispersions or slurries exclusively of polymers
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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 & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Sustainable Energy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Dispersion Chemistry (AREA)
- Fuel Cell (AREA)
Abstract
The invention discloses a kind of amberplex for reducing methanol fuel infiltration and preparation method thereof, the film includes polyvinyl alcohol, ion-exchange resin particles and metallic particles, and polyvinyl alcohol constitutes film matrix, with the microchannel formed in film forming procedure；Ion-exchange resin particles are embedded in polyvinyl alcohol film matrix and play ion exchange；Metallic particles is filled in the microchannel of film matrix, hinders fuel methanol molecule to be spread using microchannel.The amberplex preparation process includes forming polyvinyl alcohol and ion-exchange resin powder is dissolved in deionized water formation gel and film forming；Film immerses metal salt solution and cleaned up, then film is immersed into sodium borohydride solution.The characteristics of amberplex of the present invention has efficient low methanol permeability, and preparation method is simple and easy to do, without precision equipment.
Description
Technical field
The present invention relates to fuel cell field, more particularly to polymer dielectric film fuel cell intermediate ion exchange membrane and its
Preparation method.
Background technology
Fuel cell as a kind of special device that chemical energy is converted to electric energy, due to energy conversion efficiency it is high,
The incomparable superiority of various other energy generating apparatus such as low stain, the wide, low noise of ergastic substances range of choice, are considered as
It is one of most promising, environment-friendly mechanism of new electrochemical power sources.Wherein, polymer dielectric film fuel cell has and quickly opened
It is dynamic and the advantages of to the quick responses of load variations, receive more and more attention, become nearest study hotspot.
Polymer dielectric film fuel cell using polymer dielectric film as solid electrolyte, play segmentation negative and positive the two poles of the earth and
Proton conducting（H+）Or hydroxide ion（OH-）Effect, be a critical component in polymer electrolyte fuel cells.It is poly-
The performance quality of polymer electrolyte membrane serves conclusive effect to the power generation performance of polymer dielectric film fuel cell, because
And the research and development of high-performance polymer dielectric film are just particularly important.
Polymer dielectric film fuel cell can be divided into the acid using PEM generally according to the difference of conduction ion
Property polymer dielectric film fuel cell and using alkaline anion-exchange membrane alkaline polymer electrolyte membrane fuel cell.Mesh
Before, the perfluorinated sulfonic acid of commercialized PEM such as du pont company's production（Nafion）Film, due to high conductivity,
Excellent chemistry, electrochemistry and mechanical stability, is current business application polymer dielectric film most in fuel cell.
But Nafion membrane preparation technology is complicated, price is high, preparation process causes harm to environment, must use noble metal catalyst
The problems such as, limit Proton Exchange Membrane Fuel Cells further commercially use.And on the other hand, relative to PEM
Fuel cell, alkaline anion-exchange membrane fuel cell has a series of particular advantages：Due to its alkaline environment, fuel cell tool
The organic-fuels such as the methanol or ethanol that have faster kinetics, non-precious metal catalyst can be used and be readily transported.
DMFC（Direct methanol fuel cells write a Chinese character in simplified form DMFC）It is directly to utilize methanol-water
Solution is fuel, oxygen or air as oxidant a kind of new fuel cell.DMFC is a kind of polymer
Battery, its operation principle is：In anode region, after negative electrode active material methanol aqueous solution is evenly distributed through anode flow field board, lead to
Anode diffusion layer is crossed to spread and enter in anode catalyst layer（That is anode electrochemical active reaction region）, in pallium-on-carbon ruthenium electro-catalysis
Electrochemical oxidation reactions, generation proton, electronics and carbon dioxide occur in the presence of agent.The proton of generation passes through perfluoro sulfonic acid membrane
Polymer dielectric moves to negative electrode, and electronics is delivered to negative electrode by external circuit, carbon dioxide under acidic electrolyte bath help from
Anode export is discharged；After cathodic region, positive active material oxygen or air are uniformly matched somebody with somebody through cathode flow field plate, pass through cathode diffusion layer
Spread and enter in cathode catalysis layer（That is negative electricity chemism conversion zone）, in the presence of pallium-on-carbon ruthenium electro-catalyst with from
The proton that anode migration comes occurs electrochemical reducting reaction generation water and discharged with reaction end gas from cathode outlet.Its electrode reaction
It is as follows：
Anode reaction：CH3OH+H2O→CO2+6H++ 6e；
Cathode reaction：3/2 O2+6H++ 6e → 3H2O；
Overall reaction：CH3OH+3/2 O2→CO2+2H2O 。
Because methanol is at room temperature liquid, with very high energy density, and it is cheap, can be directly from oil, day
Obtained in the raw materials such as right gas, coal, without carrying out fuel reforming as indirect methanol fuel cell, simplify reformation and set
It is standby.
But DMFC also faces that catalyst activity is low, methanol fuel permeates two big key issues.Work as first
After alcohol is through film to negative electrode, mixed potential reduction battery total voltage infringement cell power generation efficiency can be produced, while reaching negative electrode
Methanol seriously poisons cathod catalyst, reduces catalyst activity.
Patent（Publication number 105884948A）A kind of fuel cell anionic membrane of blocking methanol crossover is disclosed, using different
Butylene, 1- chlorine iso-amylene and cross-linking monomer 2- trifluoromethyl -6- methyl -5- heptene acetic acid esters, by cation pre-polymerization, amination,
Quaternized, dehydration ethylene linkage, last radical polymerization densification crosslinking is polyisobutene anionic membrane.Due to being the tertiary alkyl master of saturation
Chain, will not highly basic degraded.With excellent alkali resistance and methanol blocking ability, room temperature membrane conductivity can reach >=80mS/cm.
Patent（Publication number 105826584A）Using the method that sulfonated graphene is mixed in Nafion, Nafion membrane is reduced
Methanol permeability.Patent（Patent No. ZL03137306.2）Disclose and belong to being used for for fuel cell material technology of preparing scope
The aromatic heterocyclic polymer containing sulfonic acid lateral group of DMFC is doped with inorganic material prepares PEM
A kind of methanol tolerance permeates the preparation method of PEM.Aromatic heterocyclic polymer of the film matrix containing sulfonic acid lateral group is added to solvent
In, formed after homogeneous mixture, add inorganic matter, form suspension.The suspension is crushed by nanometer crushing technology,
Finely dispersed slurry is obtained, is film-made with casting.Its membrane structure formed is uniform, quite fine and close.It can not only resist well
Methanol crossover, also with good chemical stability and proton-conducting, methanol permeability is less than 5%.
The ion exchange membrane preparation method of current existing low methanol permeability is universal more complicated, therefore exploitation is a kind of efficiently
The amberplex of low methanol permeability and the preparation method of simplicity have weight for DMFC large-scale application
Want meaning.
The content of the invention
The shortcoming existed for above-mentioned proposed amberplex, the present invention is intended to provide a kind of efficiently low methanol crossover
The amberplex of rate and the preparation method of simplicity.
The amberplex of methanol fuel infiltration is reduced the invention provides a kind of, the amberplex has efficient low first
The characteristics of alcohol permeability, it includes polyvinyl alcohol（PVA）, ion exchange resin（AER）Particle and metal nanoparticle, wherein poly-
Vinyl alcohol is constituted in film matrix, and film matrix containing self-assembling formation in film forming procedure in the microchannel in film；Ion exchange resin
Particle is embedded in polyvinyl alcohol film matrix and plays ion exchange；Metallic particles is filled in the microchannel of film matrix, hinders combustion
Expect that methanol molecules are spread using microchannel；And the amberplex does not constitute electricity from one surface to another surface
Connection, i.e., it is not short-circuit.
Further, metallic particles is only distributed in the internal layer of the film matrix, i.e., on the top layer of the amberplex not
Metallic particles is distributed, so that the amberplex is direct from one surface to that can not be constituted another surface
Electrical connection.
Further, metallic particles does not constitute continuous insertion distribution in film thickness direction, it is to avoid film short circuit problem.
It is preferred that, the metallic particles is selected from Cu, Ag or Pd.
The present invention also provides a kind of method for preparing the amberplex, comprises the following steps：
1）PVA powder is dissolved in deionized water, heats and stirs, PVA gels are obtained；AER is added into PVA gels, heating stirring
Obtain PVA-AER gels；By gel coating method film on the glass substrate, dry naturally；
2）The film dried is immersed into metal salt solution certain time, taken out afterwards and with deionized water flushing membrane surface repeatedly, so
Immerse deionized water certain time again afterwards；
3）Film is taken out from deionized water, and immerses sodium borohydride solution certain time, taking-up, which is rinsed well, afterwards obtains
The efficient low-permeability amberplex of the present invention.
Further, wherein step 2）It is mantoquita, silver salt or tetrachloro-palladium acid sodium that middle metal salt, which is selected from,.
Further, wherein step 2）It is middle immersion metal salt solution time be 1~10 hour, immersion deionized water when
Between be 1~5 minute.
The present invention core thinking be：No matter at present there is methanol fuel infiltration problem in which kind of amberplex, its root
This reason is that high-molecular polymerization membrane matrix inevitably has microchannel, if it is possible to blocks these microchannels, then can show
Write and reduce fuel infiltration.The present invention propose it is a kind of block the thinking of microchannel from blocking effect, be specifically by high molecular polymerization
Film is immersed in metal salt solution in advance, makes metal ion diffusion, adsorbs in the microchannel of film, the film is immersed in into boron hydrogen afterwards
Change in sodium fuel, metal ion is reduced to metal simple-substance when sodium borohydride enters microchannel and is filled in microchannel, produce
Blockage effect is born from, hinders methanol fuel to be permeated using microchannel, so as to reduce fuel infiltration problem.
Thinking is wherein stated in realization simultaneously, also requires that filling metallic particles for overlay is same inside the microchannel of amberplex
When, do not result in the short circuit of amberplex and fail.Specifically, the present invention is by controlling by sodium borohydride reduction into simple substance
Metallic particles does not constitute continuous insertion in film thickness direction, so that it is guaranteed that amberplex is from one surface to another surface
Between will not be formed directly electrical connection and cause film because of short-circuit failure.Specifically, in technical scheme, passing through control
The metallic particles for being filled in microchannel is only distributed in the internal layer of amberplex, removes the metal on the top layer of amberplex
Grain, so that metallic particles does not constitute continuous insertion in film thickness direction.More specifically, will in various embodiments of the present invention
Amberplex is repeatedly rinsed in pre-soaking after metal salt solution with deionized water, the gold unnecessary by washing membrane removal top layer
Belong to ion, only leave metal ion of the diffusion absorption in microchannel, immerse deionized water again afterwards 1~5 minute, make microchannel
The interior Metal ion release close to film top layer is into water；The film is just finally put into sodium borohydride solution immersion, so produced
Although metal simple-substance is filled in microchannel, but can't insertion film thickness direction, it is to avoid the problem of short-circuit.
Beneficial effects of the present invention：
1）Amberplex produced by the present invention is because elemental metals block microchannel and significantly reduce methanol fuel infiltration
Rate, so that the methanol fuel for avoiding infiltration produces mixed potential reduction cell voltage in negative electrode or even poisons cathod catalyst
Adverse effect, it is achieved thereby that the efficiently amberplex of low methanol permeability, ensures that battery has given play to excellent performance；
2）The preparation method of the present invention is simple and easy to do, without precision equipment, and easily amplification realization is prepared on a large scale.
Brief description of the drawings
Fig. 1 is that each embodiment is only completed step（1）Carbon face near the amberplex cross section microchannel of acquisition
The power spectrum test result of distribution.White bright spot represents carbon signaling point in figure.
Fig. 2 is using the silver element EDS maps near the last obtained amberplex cross section microchannel of embodiment 2
White bright spot represents silver element signaling point in power spectrum test result, figure.
Embodiment
Below by specific embodiment, the present invention is described further.
Embodiment 1：
（1）1 g PVA powder is dissolved in 50 mL deionized waters, 80oC is heated and stirred 0.5 hour, obtains PVA gels；Will
0.5 gAER adds PVA gels, 80oC heating stirrings obtain PVA-AER gels in 0.5 hour；By gel coating method in glass
Film in substrate, dries naturally；
（2）The film dried is immersed to the CuCl of 1 M concentration2Solution 1 hour, takes out and with deionized water flushing membrane surface afterwards,
Then deionized water is immersed again 5 minutes；
（3）Film is taken out from deionized water, and immerses the sodium borohydride solution 0.5 hour of 0.1M concentration, takes out rinse afterwards
The clean amberplex for obtaining the present invention.
Embodiment 2:
Difference with embodiment 1 is step（2）Middle CuCl2For AgNO3Substitute, other specification is identical.
Embodiment 3：
Difference with embodiment 1 is step（2）Middle CuCl2For Cl4Na2Pd is substituted, and other specification is identical.
Embodiment 4：
Difference with embodiment 1 is：Step（2）Immersion deionized water is shorten to 1 minute for 5 minutes, and other specification is identical.
Comparative example 1：
With the difference of embodiment 1：Step（2）Immersion deionized water is extended for 24 hours for 5 minutes, and other specification is identical.
Comparative example 2：
With the difference of embodiment 1：Step（2）Immersion deionized water is shorten to 0 minute for 5 minutes, and other specification is identical.
Comparative example 3：
With the difference of embodiment 1：Not comprising step（3）, other specification is identical.
With reference to national standard GB/T 26813-2011《Dual-beam ultraviolet-uisible spectrophotometer》, using double diffusion osmotic cell, profit
Permeability of the film to methanol fuel is measured with chemical analysis.The experimental result that specific each test is obtained is as shown in table 1.In addition,
Step in embodiment will be only completed（1）Amberplex transmission electron microscope sample is prepared with ultra-thin section, and in transmission electron microscope
Coordinate the distribution of the neighbouring carbon of energy disperse spectroscopy test film cross section microchannel, as shown in Figure 1 to be only completed each embodiment step
（1）White bright spot in the power spectrum test result of carbon EDS maps near the amberplex cross section microchannel of acquisition, picture
Represent carbon signaling point.The last obtained amberplex of embodiment 2 also with ultra-thin section and is coordinated into energy with transmission electron microscope
The distribution of the silver element of spectrometer test film cross section, as shown in Figure 2.Microchannel is implicitly present in from the visible film of accompanying drawing 1, from accompanying drawing
2 visible silver elements are filled in microchannel.
The permeability of film obtained by each embodiment of table 1 and comparative example to methanol fuel.
The amberplex that can be seen that the present invention from the permeability of table 1 has relatively low methanol permeability, and this is exactly
Have benefited from proposed by the invention from blocking effect thinking.
Contrast from embodiment Isosorbide-5-Nitrae and comparative example 1,2 is visible, very crucial in the soak time of deionized water.If during immersion
Between it is long, original absorption will be diffused into water again in the metal ion of microchannel, so that can not be the（3）It is reduced in step
And it is produced from blockage effect；If soak time is 0, metal ion, which is reduced and fills up microchannel, will cause insertion film thickness side
To and produce short-circuit hidden danger.
From the contrast of embodiment 1 and comparative example 3, if lacking sodium borohydride reduction the step, metal ion without
Method is changed into metal solid, and can not block micro pores road.
Claims (7)
1. a kind of reduce the amberplex of methanol fuel infiltration, it is characterised in that：The amberplex is included by polyethylene
Alcohol constitute film matrix, ion-exchange resin particles and metallic particles, and in the film matrix contain film forming procedure in be formed at
Microchannel in film；Wherein described ion-exchange resin particles are distributed in the film matrix, and the metallic particles is filled in institute
State in microchannel, and the amberplex is from one surface to not constituting electrical connection another surface.
2. amberplex according to claim 1, it is characterised in that：The metallic particles is only distributed in the film matrix
Internal layer.
3. amberplex according to claim 1, it is characterised in that：On a surface of the amberplex to separately
Between one surface, metallic particles does not constitute continuous insertion distribution.
4. amberplex according to claim 1, it is characterised in that the metallic particles is selected from Cu or Ag or Pd.
5. a kind of preparation method of the amberplex of reduction methanol fuel infiltration according to any one of Claims 1-4,
It is characterized in that comprising the following steps：
1）PVA powder is dissolved in deionized water, heats and stirs, PVA gels are obtained；AER is added into PVA gels, heating stirring
Obtain PVA-AER gels；By gel coating method film on the glass substrate, dry naturally；
2）The film dried is immersed into metal salt solution, takes out and with the multiple flushing membrane surface of deionized water, then immerses again afterwards
Deionized water；
3）Film is taken out from deionized water, and immerses sodium borohydride solution, taking-up, which is rinsed well, afterwards obtains the ion
Exchange membrane.
6. the preparation method of amberplex according to claim 5, it is characterised in that：Wherein step 2）Middle metal salt is
Mantoquita, silver salt or tetrachloro-palladium acid sodium.
7. the preparation method of amberplex according to claim 5, it is characterised in that：Wherein step 2）Middle immersion metal
The time of salting liquid is 1~10 hour, and the time of immersion deionized water is 1~5 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710229197.XA CN107240707B (en) | 2017-04-10 | 2017-04-10 | Ion exchange membrane for reducing methanol fuel permeation and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710229197.XA CN107240707B (en) | 2017-04-10 | 2017-04-10 | Ion exchange membrane for reducing methanol fuel permeation and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107240707A true CN107240707A (en) | 2017-10-10 |
| CN107240707B CN107240707B (en) | 2020-11-17 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114083413A (en) * | 2021-12-01 | 2022-02-25 | 南京苏洋玻璃有限公司 | LOW-E glass intelligent film removing machine |
| CN114420987A (en) * | 2022-01-24 | 2022-04-29 | 一汽解放汽车有限公司 | Composite proton exchange membrane and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354532A (en) * | 2001-09-17 | 2002-06-19 | 中国科学院长春应用化学研究所 | Preparation method of compound electrolyte film formed by making low methyl alcohol penetrate proton conductor |
| CN101999188A (en) * | 2008-04-11 | 2011-03-30 | 日东电工株式会社 | Proton conductive polymer electrolyte membrane, process for producing the proton conductive polymer electrolyte membrane, and membrane-electrode assembly and polymer electrolyte fuel cell using the proton conductive polymer electrolyte membrane |
| US20120156582A1 (en) * | 2009-05-22 | 2012-06-21 | University Of Strathclyde | Fuel cell |
| CN105680055A (en) * | 2015-11-26 | 2016-06-15 | 杭州电子科技大学 | Preparation method of alkaline anion exchange membrane and application thereof in fuel cell |
-
2017
- 2017-04-10 CN CN201710229197.XA patent/CN107240707B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354532A (en) * | 2001-09-17 | 2002-06-19 | 中国科学院长春应用化学研究所 | Preparation method of compound electrolyte film formed by making low methyl alcohol penetrate proton conductor |
| CN101999188A (en) * | 2008-04-11 | 2011-03-30 | 日东电工株式会社 | Proton conductive polymer electrolyte membrane, process for producing the proton conductive polymer electrolyte membrane, and membrane-electrode assembly and polymer electrolyte fuel cell using the proton conductive polymer electrolyte membrane |
| US20120156582A1 (en) * | 2009-05-22 | 2012-06-21 | University Of Strathclyde | Fuel cell |
| CN105680055A (en) * | 2015-11-26 | 2016-06-15 | 杭州电子科技大学 | Preparation method of alkaline anion exchange membrane and application thereof in fuel cell |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114083413A (en) * | 2021-12-01 | 2022-02-25 | 南京苏洋玻璃有限公司 | LOW-E glass intelligent film removing machine |
| CN114083413B (en) * | 2021-12-01 | 2022-07-12 | 南京苏洋玻璃有限公司 | LOW-E glass intelligent film removing machine |
| CN114420987A (en) * | 2022-01-24 | 2022-04-29 | 一汽解放汽车有限公司 | Composite proton exchange membrane and preparation method and application thereof |
| CN114420987B (en) * | 2022-01-24 | 2024-03-19 | 一汽解放汽车有限公司 | Composite proton exchange membrane and preparation method and application thereof |
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