CN106410246A - Preparation method of alkaline anion-exchange membrane for fuel cell - Google Patents
Preparation method of alkaline anion-exchange membrane for fuel cell Download PDFInfo
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- CN106410246A CN106410246A CN201611002390.1A CN201611002390A CN106410246A CN 106410246 A CN106410246 A CN 106410246A CN 201611002390 A CN201611002390 A CN 201611002390A CN 106410246 A CN106410246 A CN 106410246A
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- exchange membrane
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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
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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
Abstract
The invention discloses a preparation method of an alkaline anion-exchange membrane. The preparation method comprises the treatment process on alkaline resin, and the treatment process comprises the steps that AER alkaline resin is placed in an inorganic salt aqueous solution for soaking, then the AER alkaline resin and the inorganic salt aqueous solution are transferred to a heat-insulated vessel, liquid nitrogen is injected into the vessel for cooling, and AER alkaline resin particles are fully ground and crushed; liquid nitrogen freezing treatment is stopped, when the temperature is naturally recovered to room temperature, materials in the vessel are filtered with a filter screen, and fine alkaline resin powder is obtained. The fine alkaline resin powder serves as anion exchange resin of a chemical active group to prepare the alkaline anion-exchange membrane. By means of the resin treatment process, the AER alkaline resin particles can be uniformly distributed in the prepared anion-exchange membrane, the electrochemical performance of the alkaline anion-exchange membrane is further improved, and a fuel cell assembled through the alkaline anion-exchange membrane prepared through the method shows the excellent electricity generation performance.
Description
Technical field
The present invention relates to fuel cell field, particularly to polymer dielectric film fuel cell intermediate base anion exchange
Film and preparation method thereof.
Background technology
Fuel cell as a kind of special device that chemical energy is converted to electric energy, due to have energy conversion efficiency high,
The incomparable superiority of other energy generating apparatus multiple such as low stain, ergastic substances range of choice width, low noise, is considered
It is one of most promising, eco-friendly mechanism of new electrochemical power sources.Wherein, polymer dielectric film fuel cell effectively overcomes
The problems such as fuel losses, and there is quick startup and the quick response to load variations, receive more and more attention,
Become nearest study hotspot.
Polymer dielectric film fuel cell with 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 one of polymer electrolyte fuel cells critical component.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, generally according to the difference of conduction ion, can be divided into the acid using PEM
Property polymer dielectric film fuel cell and using alkaline anion-exchange membrane alkaline polymer electrolyte membrane fuel cell.Mesh
Before, the Nafion membrane that business-like PEM such as du pont company produces, due to having high conductivity, excellent change
, electrochemistry and mechanical stability, are the most polymer dielectric films in fuel cell of current business application.But
Nafion membrane complicated process of preparation, price are high, preparation process works the mischief to environment, unstable under high temperature the problems such as, limit
Proton Exchange Membrane Fuel Cells is further commercially use.And on the other hand, with respect to Proton Exchange Membrane Fuel Cells, alkali
Property anion-exchange membrane fuel cells have a series of particular advantages：Due to its alkaline environment, fuel cell has anti-faster
Answer kinetics, fuel permeability low, can be using organic combustion such as non-precious metal catalyst and the methanol being readily transported or ethanol
Material.Just because of these advantages, alkaline anion-exchange membrane fuel cell becomes the fuel cell technology attracting various countries' concern, alkali
Property anion exchange membrane becomes research focus therein naturally.
At present, the research having various alkaline anion-exchange membranes is reported, with quaternary ammonium salt group and quaternary phosphonium salt groups is wherein
The most study of the alkaline anionic membrane of active group, especially more being paid close attention to quaternary ammonium salt group.For example publication No. is
The Chinese patent of CN 104311857 A, carries out nucleophilic substitution by the monomer containing quaternary ammonium group to main polymer chain, obtains
Alkaline anion-exchange membrane to a kind of pair of quaternary ammonium side long chain type；For another example publication No. is the Chinese patent of CN 103804631 A,
Disclose alkaline anion-exchange membrane and the preparation method of a kind of quaternized polyketide of side chain.Alkaline anion-exchange membrane
The preparation of middle quaternary ammonium type polymer is typically passed through chloromethylation, the quaternary ammoniated step arriving multiple complexity such as alkalization again, or
The method such as radiation grafting quaternary ammonium group on polymeric matrix, haves such problems as that complicated process of preparation, material cost are high.Alkalescence cloudy from
Proton exchange film fuel cell compares Proton Exchange Membrane Fuel Cells, also there is a problem of that ionic conductance is low, and this can directly reduce
The power generation performance of fuel cell, and the studies above this problem unresolved.Therefore, research is a kind of has good ion conduction
The inexpensive alkaline anion-exchange membrane of energy and fuel power generation function performance and preparation process is simple is to polymer dielectric film fuel
The development of battery has good meaning.
The present inventor discloses a kind of preparation method of alkaline anion-exchange membrane and this film in early-stage Study
Application in a fuel cell（Publication No.：CN 105680055 A）.A kind of alkaline anion-exchange membrane of this disclosure of the invention
Preparation method is：Using polyvinyl alcohol as matrix, provide the mechanical strength of film；Lived as chemistry using commercial alkaline resin
The anion exchange resin of property group, both carry out cross-linking reaction by mixing；Meanwhile, formed in this alkaline anion-exchange membrane
During, with the addition of the inorganic salt of transition metal, film has carried out the doping of transition metal ionss.Make use of transition metal from
The catalysis characteristicses of son so that the fuel that is permeated from galvanic anode, can in ion exchange membrane timely catalytic reaction, thus
Improve the ion on-state rate of film, effectively reduce the resistivity of fuel cell；The anion exchange membrane that finally this invention is obtained
The fuel cell being assembled into shows excellent power generation performance really；The generating peak power output density of the exchange membrane of this invention
For 242 mW cm-2, its power generation performance is substantially better than the film not carrying out doped transition metal ionses and proton in the market
Exchange membrane N117.
In further research, inventor finds, in the preparation of this alkaline anion-exchange membrane, using AER alkalescence tree
Fat as the anion exchange resin of chemical active radical, because prepared anion exchange film thickness about 100 ~ 2000 is micro-
Rice, and about 600 microns of AER basic resin granule initial particle size, comparison is difficult to be evenly distributed in exchange membrane, accordingly, it would be desirable to carefully
Change resin particle.In addition in exchange membrane uses, the thinner person of resin particle, response speed is larger, and fine grained passes through to liquid
Resistance larger, so in order to improve the reaction rate of basic resin exchange membrane and increase the resistance that liquid passes through, suppressing boron hydrogen
The diffusion of the big ion of acid group, in the urgent need to the abundant size refining resin particle.Therefore, in preparation process, how by AER alkali
Property resin particle refinement and be evenly distributed on prepared anion exchange membrane be impact membrane electrochemical performance key factor it
One.
Content of the invention
For how AER basic resin granule to be uniformly distributed in the preparation process of above-mentioned existing alkaline ion exchange membrane
To improve the technical problem of the chemical property of this alkaline ion exchange membrane further in prepared anion exchange membrane, this
The purpose of invention is to provide a kind of preparation method of alkaline ion exchange membrane, in preparation process, employs a kind of technique letter
The method of process AER basic resin single, inexpensive and that there is good technique effect.
For realizing the object of the invention, the invention provides AER basic resin granule can efficiently fully be refined by one kind
And it is evenly distributed on the processing method of anion exchange membrane.The technical solution used in the present invention is：
The invention provides a kind of preparation method of alkaline anion-exchange membrane, comprise the steps：
1）First, pva powder is dissolved in deionized water, heats and stir, obtain the first gel；
2）AER basic resin is placed in inorganic salt solution and soaks, afterwards AER basic resin is turned together with inorganic salt solution
Move in heat-insulated container, inject liquid nitrogen in this container, extremely subzero 50 degrees Celsius of cooling AER basic resin, to AER basic resin
Granule is ground；Then stop liquid nitrogen freezing processing, after temperature clear-cutting forestland to room temperature, with filter screen to suspension in container
Filtered, take and can be added in the first gel through the AER basic resin fine powder of filter screen eyelet, both carry out cross-linking reaction,
Form the second gel；By the second gel film forming on substrate, dry；Caustic dip pretreatment is carried out to the film after drying.
Further, AER basic resin is placed in soak time 0.1 ~ 2 hour in inorganic salt solution.
Further, described inorganic salt is sodium chloride, CoSO4Or CoCl2One of, its concentration is 0.1M ~ 5M.
Further, time AER basic resin granule being ground is 15 minutes～1 hour.
Present invention also offers a kind of a kind of alkaline anion-exchange membrane being obtained according to above-mentioned preparation method.
Beneficial effects of the present invention：
1）Effectively refine resin particle.Conventional grinding is only capable of the fine powder of 80 mesh obtaining 0.3 g weight for 1 hour, using this
Bright method can obtain the fine powder of 120 mesh of 4 g weight in 1 hour.
2）The film roughness that the conventional resin fine powder grinding acquisition is made is about 120 μm, and adopts the method for the present invention
The film roughness that the resin fine powder obtaining is made is only 20 μm about.
3）Maximum measured by fuel cell is assembled into using the film that the resin fine powder that the method for the present invention obtains is made
Power density, compares that conventional to grind the peak power that the film that the resin fine powder obtaining made is assembled into measured by fuel cell close
Degree, all shows as the excellent technique effect being doubled and redoubled；Voltage degradation rate also effectively lowers simultaneously.
Brief description
Fig. 1 is the step 2 of embodiment 1）Grind the photo in kind of the AER basic resin fine powder completing.
Fig. 2 is the step 2 of comparative example 1）Grind the photo in kind of the AER basic resin fine powder completing.
Fig. 3 is the change in voltage under different discharge currents for the battery of the exchange membrane being obtained using embodiment 1 and comparative example 1
With power density curve.
Specific embodiment
Preparing alkaline anion-exchange membrane process of the present invention, the AER basic resin granule of use has good at room temperature
Good elasticity, each granule, as if little ball, is difficult to fully refine by conventional polishing.How effectively to refine AER alkalescence
Resin, present inventive concept is as follows：Hardening by under liquid nitrogen freezing treatment conditions, allowing AER basic resin granule become fragile, then carry out
Grind, so in process of lapping, resin is easily fully refined as the fine powder of some tens of pm, is then sieved.Ground by liquid nitrogen
Mill is obtained in that the toner of uniform and smooth, ensures that resin is evenly distributed in film matrix when adding gel preparation film forming；Separately
Outer granule is thinner, also ensure that response speed；Increase resistance, suppression boron hydracid root big ion diffusion is oozed thus alleviating fuel simultaneously
Problem thoroughly.But the freezing air slaking directly carrying out routine can lead to resin dehydration destruction resin structure to make resin lose ion exchange
Ability, this is also that naval stores usually requires that room temperature preserves, it is to avoid supercool and the reason affect product quality.The present invention is to keep away
Exempt to freeze the risk leading to resin to lose ion-exchange capacity, employ following method：Before freezing crushing, resin is soaked
Inorganic salt solution, the deposit ion of high concentration and moisture content in advance, it is to avoid the air slaking water loss problem that liquid nitrogen freezing leads to；Thus it is real
Show the purpose that abundant refinement resin particle keeps the good ion-exchange capacity of resin simultaneously.
Below by specific embodiment, the present invention is further detailed.Wherein adopt polyvinyl alcohol（PVA）Make
For matrix, provide the mechanical strength of film；The IRA-402 of the Amberlite series being produced using Alfa Aesar company of the U.S.
（OH）Basic resin（Hereinafter referred to as AER basic resin）As the anion exchange resin of chemical active radical, both pass through mixed
Conjunction carries out cross-linking reaction.
Embodiment 1：
The process preparing the alkaline anion-exchange membrane of this example is：
1）5g PVA powder is dissolved in 30 mL deionized water solutions, is heated to 80 ~ 95 degrees Celsius, stirring obtains for 2.5 ~ 3 hours
PVA gel；
2）Take 2.5g AER basic resin to be placed in 20 mL sodium-chloride water solutions to soak 0.5 hour, sodium-chloride water solution concentration 1
M；Afterwards AER basic resin is transferred in heat-insulated container together with sodium-chloride water solution, the injection liquid nitrogen cooling AER in this container
Basic resin, to subzero 50 degrees Celsius, is ground broken 15 minutes to AER basic resin granule；Then stop liquid nitrogen freezing
Process, after temperature clear-cutting forestland to room temperature, with 120 mesh filter screens, capsule contents are filtered, take and can pass through filter screen eyelet
AER basic resin fine powder standby；
3）By step 2）AER basic resin fine powder be added to PVA gel, both carry out cross-linking reaction, form PVA-AER and coagulate
Glue；This gel blade applicator is scraped on glass plate, sets film forming thickness as 1000 microns, naturally dry；By the film after drying
It is immersed in 24 hours in 1M KOH solution, then take out deionized water and repeatedly rinse.
Comparative example 1：
It is step 2 with implementing 1 difference）AER basic resin processing procedure, other just the same.Concrete steps 2）For：AER alkali
Property resin using conventional Ginding process, be placed directly within grinding alms bowl without any process and grind 15 minutes at normal temperatures.
Embodiment 2
Prepare the process of alkaline anion-exchange membrane of this example and the difference of embodiment 1 is：Step 2）Using inorganic salt
For CoSO4, concentration is 0.1 M, and AER basic resin is placed in CoSO4Soak time 1 hour in aqueous solution, milling time is little for 1
When, other specification is identical
Comparative example 2：
It is step 2 with implementing 2 differences）AER basic resin processing procedure, other just the same.Concrete steps 2）For：AER alkali
Property resin using conventional Ginding process, be placed directly within grinding alms bowl without any process and grind 1 hour at normal temperatures.
Embodiment 3：
Prepare the process of alkaline anion-exchange membrane of this example and the difference of embodiment 1 is：Step 2）Sodium-chloride water solution
Concentration is 5 M, and it is 0.1 hour that AER basic resin is placed in soak time in sodium-chloride water solution, and milling time is little for 0.5
When, filter screen is 80 mesh, and other specification is identical.
Comparative example 3：
It is step 2 with implementing 3 differences）AER basic resin processing procedure, other just the same.Concrete steps 2）For：AER alkali
Property resin using conventional Ginding process, be placed directly within grinding alms bowl without any process and grind 0.5 hour at normal temperatures.
Embodiment 4：
Prepare the process of alkaline anion-exchange membrane of the present embodiment and the difference of embodiment 1 is：Step 2）Inorganic salt used
For CoCl2, its concentration is 0.2 M, and AER basic resin is placed in CoCl2In solution, soak time is 2 hours, and milling time is 1
Hour, filter screen is 200 mesh, and other specification is identical.
Comparative example 4：
It is step 2 with embodiment 4 difference）AER basic resin processing procedure, other just the same.Concrete steps 2）For：AER
Basic resin, using conventional Ginding process, is placed directly within grinding alms bowl without any process and grinds 1 hour at normal temperatures.
For preferably embodying pre-soaking inorganic salt solution disclosed by the invention and liquid nitrogen freezing polishing is compared to conventional polishing
Effect, take two part of 5 g resin respectively, a copy of it adopt pre-soaking inorganic salt solution liquid nitrogen freezing grind 1 hour, another
Part is ground 1 hour using room temperature, all grinding product is sieved afterwards.The former is sieved with 120 eye mesh screens and is obtained in that 4 g fine powders,
The latter is sieved with 80 eye mesh screens and is only capable of obtaining 0.3 g fine powder.
The Membrane properties and structure test being obtained：
1）Surface average roughness using atomic force microscope test film.
2）Using the film prepared by fuel cell test as direct sodium borohydride fuel cell dielectric film electrochemistry
Performance.Cell active area used is 6 cm2, using Ni-Pd catalyst, loading is 10 mg/cm to anode2, negative electrode uses Pt/
C catalyst, loading is 5 mg/cm2, fuel is 5wt.%NaBH4With 10wt.%NaOH mixed aqueous solution, oxidant is pure oxygen
Gas, pressure is 0.2MPa, and test temperature is 30 degrees Celsius.Battery maximum is obtained by the voltage under the different discharge current of test defeated
Go out power density.By constant current discharge, test cell voltage over time thus evaluating cell performance decay rate.
The film mean roughness of above-described embodiment and comparative example, battery peak power output density and 50 mA/cm2Electric discharge
Voltage degradation rate is as shown in table 1 within 20 hours.
The film mean roughness of table 1 embodiment and comparative example, battery peak power output density and 50 mA/cm2Electric discharge 20
Hour voltage degradation rate.
The film mean roughness that embodiment is obtained as shown in Table 1, significantly less than comparative example, illustrates liquid nitrogen disclosed in this invention
Freeze grinding can effectively refine resin particle.The film that embodiment is obtained as shown in Table 1 is applied to obtained in fuel cell
Peak power output density be above comparative example, illustrate that the first pre-invasion disclosed in this invention adsorbs the process energy of inorganic salt
Enough it is prevented effectively from the Conventional cryogenic freezing infringement to resin property for the air slaking, the film prepared by the second refinement resin particle is conducive to changing
Kind cell power generation performance.Also know that the film that embodiment is obtained is applied to the voltage degradation rate of fuel cell and is generally less than by table 1
Comparative example, illustrates that refinement resin particle can increase really sterically hindered, the suppression big ion of boron hydracid root spreads thus alleviating fuel
Infiltration problem.
Step 2 as accompanying drawing 1 embodiment 1）Grind the photo in kind of the AER basic resin fine powder completing, accompanying drawing 2 is to compare
Example 1 step 2）Grind the photo in kind of the AER basic resin fine powder completing, the former is relatively fine and smooth uniformly.
As accompanying drawing 3）For being respectively adopted the battery of the exchange membrane that embodiment 1 and comparative example 1 are obtained under different discharge currents
Change in voltage and power density curve.Embodiment 1 and comparative example 1 battery peak power output density are divided as can be seen from Figure
Wei not 119 mW/cm2With 68 mW/cm2, the former is with respect to the latter close to double growth.
Claims (5)
1. a kind of preparation method of the alkaline anion-exchange membrane for fuel cell, comprises the steps：
1）First, pva powder is dissolved in deionized water, heats and stir, obtain the first gel；
2）Process AER basic resin and obtain AER basic resin fine powder；
3）By step 2）The AER basic resin fine powder obtaining is added in the first gel, and both carry out cross-linking reaction, forms second
Gel；By the second gel film forming on substrate, dry；Caustic dip pretreatment is carried out to the film after drying；
It is characterized in that：Step 2）Process AER basic resin step be：AER basic resin is placed in inorganic salt solution
Soak, afterwards AER basic resin is transferred in heat-insulated container together with inorganic salt solution, inject liquid nitrogen in this container, cold
But basic resin, to subzero 50 degrees Celsius, is then ground to AER basic resin granule；Stop liquid nitrogen freezing afterwards to process,
After temperature clear-cutting forestland to room temperature, with filter screen, suspension in container is filtered, obtain AER basic resin fine powder.
2. the preparation method of a kind of alkaline anion-exchange membrane for fuel cell according to claim 1, its feature
It is：Described inorganic salt is sodium chloride, CoSO4Or CoCl2One of, the concentration of described inorganic salt solution is 0.1M ~ 5M.
3. the preparation method of a kind of alkaline anion-exchange membrane for fuel cell according to claim 1, its feature
It is：AER basic resin was placed in the time soak in inorganic salt solution for 0.1 ~ 2 hour.
4. the preparation method of a kind of alkaline anion-exchange membrane for fuel cell according to claim 1, its feature
It is：The time that AER basic resin granule is ground is 15 minutes～1 hour.
5. a kind of alkaline anion-exchange membrane that the preparation method according to Claims 1 to 4 any one is obtained.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106972184A (en) * | 2017-04-10 | 2017-07-21 | 浙江大学 | It is a kind of to reduce the in-situ treatment method that amberplex permeates to sodium borohydride fuel |
| CN107240708A (en) * | 2017-04-10 | 2017-10-10 | 浙江大学 | It is a kind of for amphoteric ion exchange membrane of fuel cell and preparation method thereof |
| CN107482240A (en) * | 2017-07-24 | 2017-12-15 | 杭州电子科技大学 | A kind of alkaline anion-exchange membrane of core shell structure binary transition metal ion doping |
| CN107516743B (en) * | 2017-07-24 | 2019-10-11 | 杭州电子科技大学 | A kind of preparation method of the alkaline anion-exchange membrane of core-shell structure binary transition metal ion doping |
| CN111244512A (en) * | 2018-11-28 | 2020-06-05 | 中国科学院大连化学物理研究所 | Ultrathin cross-linked composite enhanced polymer anion exchange membrane and preparation method and application thereof |
| CN114551951A (en) * | 2022-01-10 | 2022-05-27 | 杭州电子科技大学 | Texturing anion exchange membrane for fuel cell and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106972184A (en) * | 2017-04-10 | 2017-07-21 | 浙江大学 | It is a kind of to reduce the in-situ treatment method that amberplex permeates to sodium borohydride fuel |
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| CN107516743B (en) * | 2017-07-24 | 2019-10-11 | 杭州电子科技大学 | A kind of preparation method of the alkaline anion-exchange membrane of core-shell structure binary transition metal ion doping |
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| CN111244512A (en) * | 2018-11-28 | 2020-06-05 | 中国科学院大连化学物理研究所 | Ultrathin cross-linked composite enhanced polymer anion exchange membrane and preparation method and application thereof |
| CN114551951A (en) * | 2022-01-10 | 2022-05-27 | 杭州电子科技大学 | Texturing anion exchange membrane for fuel cell and preparation method thereof |
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