CN106299387B - The method for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk - Google Patents
The method for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk Download PDFInfo
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- CN106299387B CN106299387B CN201610893214.5A CN201610893214A CN106299387B CN 106299387 B CN106299387 B CN 106299387B CN 201610893214 A CN201610893214 A CN 201610893214A CN 106299387 B CN106299387 B CN 106299387B
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- stalk
- gas
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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
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8803—Supports for the deposition of the catalytic active composition
- H01M4/8807—Gas diffusion layers
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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 kind of methods for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk; using stalk as raw material; after by the precursor solution of iron dipping and drying; using pressure sintering, disposable fabricated in situ contains the gas-diffusion electrode of Fe-N-C non-platinum catalyst in protective gas atmosphere; the method of the present invention is implemented reliable; save the cost, and the utilization of the value maximization of stalk can be avoided unnecessary waste.
Description
Technical field
The present invention relates to fuel cell electrode fields, especially a kind of to prepare Proton Exchange Membrane Fuel Cells gas using stalk
The method of body diffusion electrode.
Background technique
Proton Exchange Membrane Fuel Cells has many advantages, such as high-efficient, low pollution, therefore is considered as ideal energy conversion
One of mode.In recent decades, highest attention of the Proton Exchange Membrane Fuel Cells by government, enterprise and scientific research institution, obtains
Great development, but Proton Exchange Membrane Fuel Cells is mainly using noble metal platinum and platinum base alloy as catalyst, platinum is high
Price significantly limits the commercialization of Proton Exchange Membrane Fuel Cells, non-platinum catalyst and the gas containing non-platinum catalyst
The research of diffusion electrode is being risen.
In recent years the study found that the catalyst containing iron (Fe), nitrogen (N), carbon (C) three kinds of elements show can be with platinum
Oxygen reduction reaction (ORR) activity that catalyst compares favourably, is made non-platinum catalyst and the gas diffusion containing non-platinum catalyst
It is expected to that platinum is replaced to be applied to fuel battery cathode with proton exchange film gas-diffusion electrode after electrode.
China is a large agricultural country, generates a large amount of stalk every year, with the development of economy and society, rural area is fewer and fewer
Ground uses stalk as life fuel, and the mode of on-site incineration compost is selected to handle stalk, this not only brings great ring
Border harm, but also the value of stalk resource is not fully utilized.Due to C, N, H, O element rich in stalk
（Account for about the 75% of stalk gross mass）, organic fibres such as cellulose, hemicellulose, lignin of these elements composition are stalks
Main component, therefore will be straw-carbonized after can be used conveniently to prepare the non-platinum gas-diffusion electrode of Proton Exchange Membrane Fuel Cells.
Summary of the invention
In order to solve the deficiencies in the prior art, the present invention provides that a kind of preparation cost is low, method is simple and strong operability
The method for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk.
In order to realize above-mentioned technical purpose, the technical scheme is that：It is a kind of to prepare proton exchange membrane using stalk
The method of fuel cell gas diffusion electrode, process are：Using stalk as raw material, impregnates and dry by the precursor solution of iron
Afterwards, using pressure sintering, disposable fabricated in situ contains the gas diffusion electricity of Fe-N-C non-platinum catalyst in protective gas atmosphere
Pole.
Further, following steps are specifically included：
（1）Stalk is cut into the stalk billet that length is 5~10cm, width is 0.1~1cm；
（2）Stalk net is made in above-mentioned stalk billet；
（3）Above-mentioned stalk net is immersed in the precursor solution of iron, the impregnation time is 10~90min；
（4）The stalk net being disposed taking-up is dried；
（5）Take 3~10 layers it is above-mentioned dry after stalk net be overlapped and be placed in hot press, while leading in hot press
Enter protective gas, makes stalk net under protective gas atmosphere with 1~5Mpa pressure, 200~500 DEG C of at a temperature of progress hot pressing 15
The gas-diffusion electrode containing Fe-N-C non-platinum catalyst can be obtained in~120min after compacting.
Further, the stalk include wheat stalk, rice straw, corn stover, sugarcane cauline leaf, cotton stalk,
One of rape stalk, sweet potato vine, potato vine or more than one.
Further, the concentration of the precursor solution of the iron is 0.01~5mol/L.
Further, the precursor solution of the iron is ferric nitrate, iron chloride, ferric oxalate, ferrocene methanol, ferrocene
Formic acid, ferrous sulfide, ammonium ferric oxalate, ferrous oxalate, ethyl dicyclopentadienyl iron, ferric acetyl acetonade, ferric ammonium sulfate, ferrous sulfate
Ammonium, diacetyl group ferrocene, benzoyl ferrocene, vinyl ferrocene, normal-butyl ferrocene, trifluoromethanesulfonic acid iron, butyryl
One of base ferrocene or more than one mixing compositions.
Further, the protective gas is one of nitrogen, argon gas, helium or more than one mixing compositions.
Further, the step（2）The method of stalk net is made as braiding or compression moulding in stalk billet.
Through the above technical solution, beneficial effects of the present invention are：By being to prepare raw material with stalk, it is impregnated in
It is taken out and dries again after the precursor solution of iron, the precursor solution of iron is made to be supported on stalk surface, in the gas of protective gas
The stalk for having the presoma of iron that will be in debt under atmosphere carries out hot pressing, so that the presoma of iron is decomposed, iron atom and stalk surface are tight
Closely connected conjunction, and meet during straw-carbonized with carbon, nitrogen, Fe-N-C non-platinum catalyst is formed, due to hot pressing
The generation and diffusion of the gases such as carbonization and adjoint carbon monoxide occur for stalk in journey, and final stalk forms perforated grill structure, fit
It circulates in the diffusion of gaseous oxidant.
Detailed description of the invention
The present invention is further elaborated with reference to the accompanying drawings and detailed description：
Fig. 1 is the preparation stream that the present invention prepares Proton Exchange Membrane Fuel Cells non-platinum catalyst gas-diffusion electrode with stalk
Journey schematic diagram.
Specific embodiment
As shown in Figure 1, the method for the present invention using stalk as raw material, after by the precursor solution of iron dipping and drying, uses
Pressure sintering disposable fabricated in situ in protective gas atmosphere contains the gas-diffusion electrode of Fe-N-C non-platinum catalyst.
Further, following steps are specifically included：
（1）Stalk is cut into the stalk billet that length is 5~10cm, width is 0.1~1cm；
（2）Stalk net is made in above-mentioned stalk billet；
（3）Above-mentioned stalk net is immersed in the precursor solution of iron, the impregnation time is 10~90min；
（4）The stalk net being disposed taking-up is dried；
（5）Take 3~10 layers it is above-mentioned dry after stalk net be overlapped and be placed in hot press, while leading in hot press
Enter protective gas, makes stalk net under protective gas atmosphere with 1~5Mpa pressure, 200~500 DEG C of at a temperature of progress hot pressing 15
The gas-diffusion electrode containing Fe-N-C non-platinum catalyst can be obtained in~120min after compacting.
Further, the stalk include wheat stalk, rice straw, corn stover, sugarcane cauline leaf, cotton stalk,
One of rape stalk, sweet potato vine, potato vine or more than one.
Further, the concentration of the precursor solution of the iron is 0.01~5mol/L.
Further, the precursor solution of the iron is ferric nitrate, iron chloride, ferric oxalate, ferrocene methanol, ferrocene
Formic acid, ferrous sulfide, ammonium ferric oxalate, ferrous oxalate, ethyl dicyclopentadienyl iron, ferric acetyl acetonade, ferric ammonium sulfate, ferrous sulfate
Ammonium, diacetyl group ferrocene, benzoyl ferrocene, vinyl ferrocene, normal-butyl ferrocene, trifluoromethanesulfonic acid iron, butyryl
One of base ferrocene or more than one mixing compositions.
Further, the protective gas is one of nitrogen, argon gas, helium or more than one mixing compositions.
Further, the step（2）The method of stalk net is made as braiding or compression moulding in stalk billet.
Embodiment 1
（1）Wheat stalk is cut into the wheat stalk billet that length is 10cm, width is 1cm；
（2）Wheat stalk net is made in above-mentioned wheat stalk billet braiding；
（3）Above-mentioned wheat stalk net is immersed in the ammonium ferric oxalate solution that concentration is 3mol/L, impregnation
70min；
（4）The wheat stalk net handled is taken out from ammonium ferric oxalate solution and is dried；
（5）Take 3 layers it is above-mentioned dry after wheat stalk net be overlapped and be placed in hot press, while leading in hot press
Enter nitrogen, make wheat stalk net under the protective atmosphere of nitrogen to carry out hot pressing 100min at a temperature of 3Mpa pressure, 300 DEG C,
The gas-diffusion electrode containing Fe-N-C non-platinum catalyst can be obtained after compacting.
Embodiment 2
（1）Rice straw is cut into the rice straw billet that length is 8cm, width is 0.5cm；
（2）Rice straw net is made in above-mentioned rice straw billet braiding；
（3）Above-mentioned rice straw net is immersed in the iron nitrate solution that concentration is 3mol/L, impregnation 80min；
（4）The rice straw net handled is taken out from ammonium ferric oxalate solution and is dried；
（5）Take 6 layers it is above-mentioned dry after rice straw net be overlapped and be placed in hot press, while leading in hot press
Enter helium, makes rice straw net under the protective atmosphere of helium with 4Mpa pressure, 400 DEG C of at a temperature of progress hot pressing 90min, pressure
The gas-diffusion electrode containing Fe-N-C non-platinum catalyst can be obtained after system.
Embodiment 3
（1）Cotton stalk is cut into the cotton stalk billet that length is 5cm, width is 0.1cm；
（2）Cotton stalk net is made in above-mentioned corn stover billet braiding；
（3）Above-mentioned cotton stalk net is immersed in the ammonium ferric oxalate solution that concentration is 1mol/L, impregnation
90min；
（4）The cotton stalk net handled is taken out from ammonium ferric oxalate solution and is dried；
（5）Take 4 layers it is above-mentioned dry after cotton stalk net be overlapped and be placed in hot press, while leading in hot press
Enter argon gas, makes cotton stalk net under the protective atmosphere of argon gas with 5Mpa pressure, 460 DEG C of at a temperature of progress hot pressing 50min, pressure
The gas-diffusion electrode containing Fe-N-C non-platinum catalyst can be obtained after system.
Embodiment 4
（1）Rape stalk is cut into the rape stalk billet that length is 6cm, width is 0.6cm；
（2）Rape stalk net is made in above-mentioned wheat stalk billet braiding；
（3）Above-mentioned rape stalk net is immersed in the benzoyl solution of ferrocene that concentration is 0.01mol/L, dipping
Handle 10min；
（4）The rape stalk net handled is taken out from benzoyl solution of ferrocene and is dried；
（5）Take 10 layers it is above-mentioned dry after rape stalk net be overlapped and be placed in hot press, while in hot press
It is passed through nitrogen and helium volume ratio is 1:1 mixed gas, make rape stalk net under the protective atmosphere of nitrogen and helium with
1Mpa pressure carries out hot pressing 120min at a temperature of 200 DEG C, is can be obtained after compacting containing Fe-N-C non-platinum catalyst
Gas-diffusion electrode.
Embodiment 5
（1）Sweet potato vine stalk is cut into the sweet potato vine stalk billet that length is 7cm, width is 0.7cm；
（2）Sweet potato vine stalk net is made in above-mentioned sweet potato vine stalk billet；
（3）Above-mentioned sweet potato vine stalk net is immersed in the acetylacetone,2,4-pentanedione ferrous solution that concentration is 5mol/L, impregnation
60min；
（4）The sweet potato vine stalk net handled is taken out from acetylacetone,2,4-pentanedione ferrous solution and is dried；
（5）Take 7 layers it is above-mentioned dry after sweet potato vine stalk net be overlapped and be placed in hot press, while in hot press
It is passed through argon gas and helium volume ratio is 1：1 mixed gas, make sweet potato vine stalk net under the protective atmosphere of argon gas and helium with
2Mpa pressure carries out hot pressing 15min at a temperature of 500 DEG C, is can be obtained after compacting containing Fe-N-C non-platinum catalyst
Gas-diffusion electrode.
Embodiment 6
（1）Wheat stalk and rice straw are cut into the wheat stalk billet that length is 10cm, width is 1cm；
（2）Stalk net is made in above-mentioned wheat stalk billet braiding；
（3）Above-mentioned stalk net is immersed in the ferrocene methanol solution that concentration is 2mol/L, impregnation 30min；
（4）The stalk net handled is taken out from ferrocene methanol solution and is dried；
（5）Take 8 layers it is above-mentioned dry after wheat stalk net be overlapped and be placed in hot press, while leading in hot press
Enter nitrogen, make wheat stalk net under the protective atmosphere of nitrogen to carry out hot pressing 60min at a temperature of 1.5Mpa pressure, 480 DEG C,
The gas-diffusion electrode containing Fe-N-C non-platinum catalyst can be obtained after compacting.
The foregoing is merely presently preferred embodiments of the present invention, for the ordinary skill in the art, is not departing from
The case where the principle and spirit of the invention, descends to the mortal world equivalent change, modification, replacement and the change made according to scope of the present invention patent
Type is all covered by the present invention.
Claims (6)
1. a kind of method for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk, it is characterised in that：With stalk
For raw material, after by the precursor solution of iron dipping and drying, the disposable conjunction in situ in protective gas atmosphere using pressure sintering
At the gas-diffusion electrode containing Fe-N-C non-platinum catalyst；
Specifically include following steps：
（1）Stalk is cut into the stalk billet that length is 5~10cm, width is 0.1~1cm；
（2）Stalk net is made in above-mentioned stalk billet；
（3）Above-mentioned stalk net is immersed in the precursor solution of iron, the impregnation time is 10~90min；
（4）The stalk net being disposed taking-up is dried；
（5）Take 3~10 layers it is above-mentioned dry after stalk net be overlapped and be placed in hot press, while guarantor is passed through in hot press
Protect gas, make stalk net under protective gas atmosphere with 1~5Mpa pressure, 200~500 DEG C at a temperature of carry out hot pressing 15~
The gas-diffusion electrode containing Fe-N-C non-platinum catalyst can be obtained in 120min after compacting.
2. the method according to claim 1 for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk,
It is characterized in that：The stalk include wheat stalk, rice straw, corn stover, sugarcane cauline leaf, cotton stalk, rape stalk,
One or more of sweet potato vine, potato vine.
3. the method according to claim 1 for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk,
It is characterized in that：The concentration of the precursor solution of the iron is 0.01~5mol/L.
4. the method according to claim 1 for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk,
It is characterized in that：The precursor solution of the iron is ferric nitrate, iron chloride, ferric oxalate, ferrocene methanol, ferrocenecarboxylic acid, sulphur
Change ferrous iron, ammonium ferric oxalate, ferrous oxalate, ethyl dicyclopentadienyl iron, ferric acetyl acetonade, ferric ammonium sulfate, iron ammonium sulfate, biacetyl
Base ferrocene, benzoyl ferrocene, vinyl ferrocene, normal-butyl ferrocene, trifluoromethanesulfonic acid iron, in Butyrylferrocene
More than one mixing composition.
5. the method according to claim 1 for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk,
It is characterized in that：The protective gas is one or more of nitrogen, argon gas, helium mixing composition.
6. the method according to claim 1 for preparing Proton Exchange Membrane Fuel Cells gas-diffusion electrode using stalk,
It is characterized in that：The step（2）The method of stalk net is made as braiding or compression moulding in stalk billet.
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| CN107039668B (en) * | 2017-03-31 | 2020-05-26 | 武汉理工大学 | Method for testing durability acceleration of gas diffusion layer of proton exchange membrane fuel cell |
| CN109585863B (en) * | 2018-12-14 | 2021-08-13 | 广东工业大学 | Preparation method of gas diffusion layer of proton exchange membrane fuel cell |
| CN111682228B (en) * | 2020-07-06 | 2022-04-12 | 山东交通学院 | Preparation method of diffusion layer with catalysis promoting function |
| CN111682227B (en) * | 2020-07-06 | 2022-04-12 | 山东交通学院 | Preparation method of diffusion layer for fuel cell |
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