CN105932316A - Production method of bipolar membrane electrode - Google Patents
Production method of bipolar membrane electrode Download PDFInfo
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- CN105932316A CN105932316A CN201610556640.XA CN201610556640A CN105932316A CN 105932316 A CN105932316 A CN 105932316A CN 201610556640 A CN201610556640 A CN 201610556640A CN 105932316 A CN105932316 A CN 105932316A
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- membrane electrode
- exchange resin
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- catalyst
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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
- H01M8/1004—Fuel cells with solid electrolytes characterised by membrane-electrode assemblies [MEA]
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention discloses a production method of a bipolar membrane electrode. A membrane electrode assembly for a fuel battery is produced from a bipolar polymer ion exchange solution and an organic polymer skeleton material. The production method comprises the following steps: forming a proton exchange layer or an oxyhydrogen ion exchange layer on the organic polymer skeleton material at a certain temperature through directly using a raw material slurry prepared by using a polymer and a solvent according to a certain ratio, mixing the cation exchange solution or anion exchange solution with a certain amount of a catalyst to obtain an anode catalyst slurry or a cathode catalyst slurry in order to make the bipolar membrane electrode assembly formed by the anode catalysis layer/the proton exchange layer/the oxyhydrogen ion exchange layer/a cathode catalysis layer; and combining a diffusion layer and the membrane electrode assembly to form the complete membrane electrode product. The method has the advantages of high integration level, agile operation, low cost and excellent product.
Description
Technical field
The present invention is the preparation method of a kind of low cost integration bipolar membrane electrode, relates to electrochemical industry
The contents such as middle polymer electrolyte membrane electrode, membrane electrode preparation technology.This kind of low cost integration bipolar membrane
Electrode preparation method is suitable for the membrane electrode of polymer electrolyte fuel cells (PEFC) to be prepared.
Background technology
Proton Exchange Membrane Fuel Cells is a kind of low operating temperatures excellent performance, cleaning, the conversion of efficient energy
Unit, has vast potential for future development in the field such as vehicle power, mobile power station.Membrane electrode (MEA) is matter
The core component of proton exchange film fuel cell, performance and the cost of membrane electrode determine to a great extent
The overall performance of PEMFC and cost.Preparation technology about each assembly of membrane electrode has many research reports, but
Traditional membrane electrode preparation technology has split the preparation of proton exchange membrane layer and Catalytic Layer, adds system overall
Complexity, use preparation facilities many, the integrated level making fuel cell preparation technology is low, the huge height of cost not under.
Cut down MEA integral thickness further and prepare the trend that high property superthin membrane electrode makes MEA preparation develop, tradition
MEA preparation technology be difficult to the flexible control to proton still layer, constrain MEA further
Development.
Summary of the invention
The invention aims to make up the deficiencies in the prior art, use bipolar ion exchange solution and height
Membrane-membrane electrode for fuel cell is prepared on molecular skeleton material and the same operating platform of catalyst slurry.By substrate bone
The tiling of frame film is fixed on and adds on hot substrate, at a certain temperature continuous spray cation exchange solution and catalyst
Slurries, then continuous spray anion exchange solution and catalyst slurry on another side, prepare one
Change bipolar membrane electrode.This kind of method makes dielectric substrate more closely improve MEA with the combination of Catalytic Layer
Performance, preparing the mechanical performance maintaining MEA while thinner MEA, using with platform integration system
Standby scheme decreases total system complexity and effectively reduces MEA production cost to relevant Preparation equipment, meanwhile,
The use of bipolar ion exchange solution can realize MEA from being humidified generating.
In order to reach the purpose of the present invention, technical scheme is as follows:
The preparation method of a kind of bipolar membrane electrode, it is characterised in that comprise the following steps:
1) cationic ion-exchange resin material and solvent are mixed, at 100-400 DEG C of high-temperature digestion, formed uniformly
Scattered cationic ion-exchange resin solution, wherein, cationic ion-exchange resin material: solvent=1:(5-500)；
2) by anode catalyst, cationic ion-exchange resin solution and dispersant, after ultrasonic vibration,
Form homodisperse anode catalyst slurries；
Wherein catalyst: cationic ion-exchange resin solution: dispersant=1:(1-100): (1-300)；
3) high-molecular bone frame material is put at 30-60 DEG C of dipping in methyl alcohol, after soak with aqueous isopropanol
24 hours；
4) the cationic ion-exchange resin solution prepared is prepared equably in step 3) the middle high score pre-processed
On sub-framework material, form proton exchange layer；
5) the anode-catalyzed agent composition prepared is prepared equably in step 4) in the proton for preparing hand over
Change a layer side, form the electrode assemblie being loaded with Catalytic Layer；
6) anion exchange resin material and solvent are mixed, at 100-400 DEG C of high-temperature digestion, formed uniformly
Scattered cationic ion-exchange resin solution, wherein, anion exchange resin material: solvent=1:(5-500)；
7) by cathod catalyst, anion exchange resin solution and dispersant, after ultrasonic vibration,
Form homodisperse cathod catalyst slurries；
Wherein catalyst: anion exchange resin solution: dispersant=1:(1-100): (1-300)；
8) the anion exchange resin solution prepared is prepared equably in step 5) in electrode assemblie another
Side, forms anion exchange layer；
9) cathode catalytic mixture prepared is prepared equably in step 8) in the anion for preparing
Switching layer side, forms negative electrode；
10) by above-mentioned 9) in negative electrode OH ionization, preparation integration bipolar membrane electrode；
11) diffusion layer is placed on step 10) in the both sides diffusion layer of three in one membreane electrode of preparation, pass through
Pressing forms five in one membrane electrode, and wherein, diffusion layer is porous carbon paper or metal polyporous material.
Preferably, in dyeing: between the thickness 3-500 micron of described high-molecular bone frame material.
Preferably, the preparation method of described polymer electrolyte membrane electrode includes spraying or prints.
Preferably, described anode catalyst be Pt, Ru, Ir, Au, Ni, Co, Zn, Ag or they
Alloy and oxide；Cathod catalyst be Pt, Ru, Ir, Au, Ni, Co, Zn, Ag or they
Alloy and oxide.
Preferably, described metal polyporous material is stainless (steel) wire, titanium net or nickel screen.
The invention have the benefit that
(1) compared with traditional membrane electrode preparation technology flow process, low cost integration bipolar membrane electrode system
Standby technique improves the integrated level of membrane electrode entirety preparation technology.Achieve the dielectric substrate of membrane electrode, catalysis
The same platform of layer, the preparation process of integration.This technique is by reducing integrated artistic system complexity, simple
Change preparation technology equipment, the fixed cost of significantly lower production technology and variable cost.
(2) compared with traditional handicraft, integral process directly utilizes resin particle and can prepare complete
Membrane electrode, dielectric substrate becomes the intermediate products of membrane electrode preparation process, proton exchange layer or OH exchange
Layer is combined more tight with Catalytic Layer, improves production efficiency and membrane electrode performance.Integral process also makes
The producer can obtain different proton exchange by the usage amount of resin raw material flexibly according to the demand of oneself
The membrane electrode of layer thickness, reduces cost, improves production chains, operability.
(3) multinomial performance evaluation experiment shows, low cost integration bipolar membrane electrode fabrication institute
The membrane electrode produced has exceeded at aspects such as mechanical performance, chemical property, battery performances to be adopted under equal conditions
Membrane electrode with E.I.Du Pont Company's Nafion112 film preparation.By SEM, membrane electrode is carried out observing display, electric
Solve matter layer and fill good.Energy spectrum analysis also demonstrate that resin being uniformly distributed in porous matrix, well-formed.
Additionally, life test result explanation membrane electrode can realize successively working more than 24 hours performances without declining
Subtract.
(4) integration bipolar membrane electrode can realize the generating that is certainly humidified of fuel cell, it is not necessary to water source, greatly
The earth simplifies fuel cell generation and reduces cost.
Accompanying drawing explanation
Fig. 1 is membrane electrode of fuel batter with proton exchange film electrical property figure prepared by the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but protection scope of the present invention is not only limited to
In embodiment.
The preparation method of a kind of integration bipolar membrane electrode that the present invention provides, its concrete technology step is such as
Under:
1) preparation of cationic ion-exchange resin solution: cationic ion-exchange resin material and solvent are mixed,
100-400 DEG C of high-temperature digestion, forms homodisperse cationic ion-exchange resin solution, and wherein, cation is handed over
Change resin material: solvent=1:(5-500)；Cationic ion-exchange resin is: perfluorinated sulfonic acid macromolecule resin,
Acid doping polybenzimidazoles macromolecule resin etc..
2) preparation of anode catalyst slurries: by anode catalyst, cationic ion-exchange resin solution and dispersion
Agent mixes, and after ultrasonic vibration, forms homodisperse catalyst slurry.Wherein catalyst: cation
Exchanger resin solution: dispersant=1:(1-100): (1-300)；Described catalyst is Pt, Ru, Ir, Au,
Ni, Co, Zn, Ag or their alloy and oxide.
3) pretreatment of high-molecular bone frame material: high-molecular bone frame material is put in methyl alcohol 30-60 DEG C of leaching
Stain, after with aqueous isopropanol soak 24 hours.The thickness 3-500 micron of described high-molecular bone frame material
Between.
4) cation prepared exchange solution is prepared equably in step 3) the middle high-molecular bone pre-processed
On frame material, form proton exchange layer；Polymer dielectric is heated to the model of its vitrification point ± 40 degree
In enclosing.
5) the anode-catalyzed agent composition prepared is prepared equably in step 4) in the proton for preparing hand over
Change a layer side, form side and be loaded with the anode of Catalytic Layer；Cation exchange electrolyte is heated to its vitrifying
In the range of temperature ± 40 degree.
6) preparation of anion exchange resin solution: anion exchange resin material and solvent are mixed,
100-400 DEG C of high-temperature digestion, forms homodisperse anion exchange resin solution, and wherein, anion is handed over
Change resin material: solvent=1:(5-500)；Anion exchange resin mainly includes that quaternary anion is handed over
Change resin.
7) preparation of cathod catalyst slurries: by cathod catalyst, anion exchange resin solution and dispersion
Agent mixes, and after ultrasonic vibration, forms homodisperse catalyst slurry.Wherein catalyst: anion
Exchanger resin solution: dispersant=1:(1-100): (1-300)；Described catalyst is Pt, Ru, Ir, Au,
Ni, Co, Zn, Ag or their alloy and oxide.
8) the anion exchange resin solution prepared is prepared equably in step 5) in electrode assemblie another
Side, forms anion exchange layer, and is heat-treated in the range of its vitrification point ± 40 degree.
9) cathode catalytic mixture prepared is prepared equably in step 8) in the anion for preparing
Switching layer side, forms negative electrode；
10) by above-mentioned 9) in negative electrode OH ionization, preparation integration bipolar membrane electrode.
11) diffusion layer is placed on step 10) in the both sides diffusion layer of three in one membreane electrode of preparation, pass through
Pressing forms five in one membrane electrode.Wherein, diffusion layer is porous carbon paper or metal polyporous material, described
Metal polyporous material be stainless (steel) wire, titanium net or nickel screen；
Embodiment 1:
Perfluorinated sulfonic resin material and solvent are mixed according to mass ratio 1:100, at 400 DEG C of high-temperature digestions,
Form homodisperse polymer dielectric slurries.Solvent is according to isopropanol: water quality is prepared than 3:1.Take
A part of polymer dielectric slurries according to, according to Pt/C (40%) catalyst: polymer dielectric slurries:
Isopropanol mass ratio is 1:10:500, and sonic oscillation forms uniform catalyst slurry in 30 minutes.Take 15
The thick ePTFE membrane of micron, as substrate framework material, impregnates half an hour in the methyl alcohol in boiling, then different
Soaking 24 hours in propanol solution, rear taking-up is laid on to add and is heated to 120 degree on hot substrate.On ePTFE
Sprayed-on polymer electrolyte slurry, forms the proton exchange layer of viscosity flow state.And then to proton exchange layer one
Side spray is coated with catalyst slurry and forms the anode catalyst layer combined closely, turn over after cooling be placed on heated substrate standby
With.
Quaternized polysulfones (QAPS) resin material and solvent are mixed according to mass ratio 1:500, high at 100 DEG C
Temperature is dissolved, and forms homodisperse anion exchange resin solution.Solvent is according to isopropanol: water quality compares 3:1
Preparation.Take a part of above-mentioned anion exchange resin solution according to Ag catalyst: anion exchange resin is molten
Liquid: isopropanol mass ratio is 1:10:300, sonic oscillation forms uniform cathod catalyst slurries for 30 minutes.
The anion exchange resin solution prepared is prepared equably in the another side of above-mentioned anode catalyst, shape
Become cathode catalysis layer.And be heat-treated.
Install carbon paper in both sides additional and form membrane electrode five in one structure, membrane electrode is placed in two panels and is carved with definite shape
Runner carbon plate between, use two pieces of duralumin fixtures to be assembled into monocell, do not humidify at reacting gas and
Gas pressure is to carry out cell polarization curves test under conditions of normal pressure.Battery performance is shown in Fig. 1.
Last it is noted that above example only in order to the present invention is described and and unrestricted described in the invention
Technical scheme, therefore, although this specification with reference to each above-mentioned embodiment to present invention has been in detail
Thin explanation, but, it will be understood by those within the art that, still the present invention can be repaiied
Changing or equivalent, and all are without departing from the technical scheme of the spirit and scope of the present invention and improvement thereof, it is equal
Should contain in scope of the presently claimed invention.
Claims (5)
1. the preparation method of a bipolar membrane electrode, it is characterised in that comprise the following steps:
1) cationic ion-exchange resin material and solvent are mixed, at 100-400 DEG C of high-temperature digestion, formed uniformly
Scattered cationic ion-exchange resin solution, wherein, cationic ion-exchange resin material: solvent=1:(5-500)；
2) by anode catalyst, cationic ion-exchange resin solution and dispersant, after ultrasonic vibration,
Form homodisperse anode catalyst slurries；
Wherein catalyst: cationic ion-exchange resin solution: dispersant=1:(1-100): (1-300)；
3) high-molecular bone frame material is put at 30-60 DEG C of dipping in methyl alcohol, after with aqueous isopropanol soak 24
Hour；
4) the cationic ion-exchange resin solution prepared is prepared equably in step 3) the middle high score pre-processed
On sub-framework material, form proton exchange layer；
5) the anode-catalyzed agent composition prepared is prepared equably in step 4) in the proton for preparing hand over
Change a layer side, form the electrode assemblie being loaded with Catalytic Layer；
6) anion exchange resin material and solvent are mixed, at 100-400 DEG C of high-temperature digestion, formed uniformly
Scattered cationic ion-exchange resin solution, wherein, anion exchange resin material: solvent=1:(5-500)；
7) by cathod catalyst, anion exchange resin solution and dispersant, after ultrasonic vibration,
Form homodisperse cathod catalyst slurries；
Wherein catalyst: anion exchange resin solution: dispersant=1:(1-100): (1-300)；
8) the anion exchange resin solution prepared is prepared equably in step 5) in electrode assemblie another
Side, forms anion exchange layer；
9) cathode catalytic mixture prepared is prepared equably in step 8) in the anion for preparing
Switching layer side, forms negative electrode；
10) by above-mentioned 9) in negative electrode OH ionization, preparation integration bipolar membrane electrode；
11) diffusion layer is placed on step 10) in the both sides diffusion layer of three in one membreane electrode of preparation, pass through
Pressing forms five in one membrane electrode, and wherein, diffusion layer is porous carbon paper or metal polyporous material.
The preparation method of bipolar membrane electrode the most according to claim 1, it is characterised in that in dyeing
In technique: between the thickness 3-500 micron of described high-molecular bone frame material.
The preparation method of bipolar membrane electrode the most according to claim 1, it is characterised in that described
The preparation method of polymer electrolyte membrane electrode includes spraying or prints.
The preparation method of bipolar membrane electrode the most according to claim 1, it is characterised in that described
Anode catalyst is Pt, Ru, Ir, Au, Ni, Co, Zn, Ag or their alloy and oxide；Negative electrode
Catalyst is Pt, Ru, Ir, Au, Ni, Co, Zn, Ag or their alloy and oxide.
The preparation method of bipolar membrane electrode the most according to claim 1, it is characterised in that described
Metal polyporous material is stainless (steel) wire, titanium net or nickel screen.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107171010A (en) * | 2017-05-11 | 2017-09-15 | 厦门大学 | A kind of compound Bipolar Membrane and preparation method thereof |
| CN113769208A (en) * | 2021-09-28 | 2021-12-10 | 广东喜玛拉雅氢能科技有限公司 | Hydrogen-rich water spraying device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942672A (en) * | 2010-09-16 | 2011-01-12 | 清华大学 | Preparation method of polymer electrolyte membrane electrode |
| CN102820474A (en) * | 2012-09-06 | 2012-12-12 | 江苏冰城电材股份有限公司 | Preparation method of polymer electrolytic membrane electrode |
| CN104505528A (en) * | 2012-09-06 | 2015-04-08 | 江苏冰城电材股份有限公司 | Five-in-one polymer electrolyte membrane electrode |
-
2016
- 2016-07-15 CN CN201610556640.XA patent/CN105932316B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942672A (en) * | 2010-09-16 | 2011-01-12 | 清华大学 | Preparation method of polymer electrolyte membrane electrode |
| CN102820474A (en) * | 2012-09-06 | 2012-12-12 | 江苏冰城电材股份有限公司 | Preparation method of polymer electrolytic membrane electrode |
| CN104505528A (en) * | 2012-09-06 | 2015-04-08 | 江苏冰城电材股份有限公司 | Five-in-one polymer electrolyte membrane electrode |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107171010A (en) * | 2017-05-11 | 2017-09-15 | 厦门大学 | A kind of compound Bipolar Membrane and preparation method thereof |
| CN113769208A (en) * | 2021-09-28 | 2021-12-10 | 广东喜玛拉雅氢能科技有限公司 | Hydrogen-rich water spraying device |
| CN113769208B (en) * | 2021-09-28 | 2023-08-15 | 广东喜玛拉雅氢能科技有限公司 | Hydrogen-rich water spraying device |
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