CN114204050B - Fuel cell membrane electrode preparation process and continuous production line - Google Patents
Fuel cell membrane electrode preparation process and continuous production line Download PDFInfo
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- CN114204050B CN114204050B CN202111468249.1A CN202111468249A CN114204050B CN 114204050 B CN114204050 B CN 114204050B CN 202111468249 A CN202111468249 A CN 202111468249A CN 114204050 B CN114204050 B CN 114204050B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000000446 fuel Substances 0.000 title claims abstract description 19
- 238000010924 continuous production Methods 0.000 title claims abstract description 16
- 210000000170 cell membrane Anatomy 0.000 title claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 173
- 239000011248 coating agent Substances 0.000 claims abstract description 168
- 239000002131 composite material Substances 0.000 claims abstract description 136
- 239000003054 catalyst Substances 0.000 claims abstract description 96
- 238000005266 casting Methods 0.000 claims abstract description 72
- 230000007246 mechanism Effects 0.000 claims abstract description 71
- 238000001035 drying Methods 0.000 claims abstract description 63
- 239000012528 membrane Substances 0.000 claims abstract description 63
- 239000002002 slurry Substances 0.000 claims abstract description 40
- 238000001514 detection method Methods 0.000 claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 claims abstract description 37
- 230000001681 protective effect Effects 0.000 claims abstract description 36
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- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000013329 compounding Methods 0.000 claims abstract description 6
- 238000005096 rolling process Methods 0.000 claims description 41
- 239000002904 solvent Substances 0.000 claims description 38
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 28
- 239000012982 microporous membrane Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 26
- 238000007731 hot pressing Methods 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 20
- 210000004027 cell Anatomy 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000002950 deficient Effects 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000004804 winding Methods 0.000 claims description 6
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 239000011949 solid catalyst Substances 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000010410 layer Substances 0.000 claims 17
- 201000000760 cerebral cavernous malformation Diseases 0.000 claims 15
- 239000011247 coating layer Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 230000008961 swelling Effects 0.000 abstract description 4
- 238000005470 impregnation Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 description 11
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- 230000000052 comparative effect Effects 0.000 description 7
- 150000003460 sulfonic acids Chemical class 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
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- 238000007599 discharging Methods 0.000 description 3
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- 238000011068 loading method Methods 0.000 description 2
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- 230000002829 reductive effect Effects 0.000 description 2
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- 238000007581 slurry coating method Methods 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
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- 239000012071 phase Substances 0.000 description 1
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- 238000010248 power generation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
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- 238000011084 recovery Methods 0.000 description 1
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- 238000010023 transfer printing Methods 0.000 description 1
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Classifications
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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
- H01M4/8825—Methods for deposition of the catalytic active composition
- H01M4/8828—Coating with slurry or ink
-
- 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
-
- 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
- H01M4/8825—Methods for deposition of the catalytic active composition
-
- 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
- H01M4/8875—Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
-
- 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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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inert Electrodes (AREA)
- Fuel Cell (AREA)
Abstract
The invention discloses a preparation process of a fuel cell membrane electrode and a continuous production line, wherein the preparation process comprises the following steps: coating a layer of casting solution on the protective base film, heating to form gel state, then compounding with the microporous film, then coating the casting solution, heating again to form gel state, and then coating catalyst slurry to obtain CCM; the continuous production line comprises a conveying roller mechanism, and a base film unreeling roller mechanism, a casting film liquid coating die head A, a drying channel I, a microporous film composite roller conveying mechanism, a casting film liquid coating die head B, a drying channel II, a back pressure roller mechanism, a defect detection mechanism I, a catalyst coating die head, a drying channel III, a thickness detection mechanism, a defect detection mechanism and the like are sequentially arranged along the conveying direction of the conveying roller mechanism; the invention integrates the composite membrane preparation and CCM preparation production line, solves the problems of membrane swelling and the like caused in the continuous coating process of the catalytic layer, and can also solve the defects of pinholes, incomplete impregnation and the like in the continuous coating preparation process of the proton exchange composite membrane.
Description
Technical Field
The invention relates to a preparation process of a fuel cell membrane electrode and a continuous production line, belonging to the field of fuel cell membrane electrodes.
Background
The fuel cell is an efficient and environment-friendly energy conversion device and has wide application prospects in various fields such as automobile transportation, distributed power generation and the like. The performance and yield of the membrane electrode as a core component of the fuel cell directly determine the performance and yield of the fuel cell stack and the system, and the high price of the proton exchange membrane required for preparing the membrane electrode also restricts the rapid development of the fuel cell. At present, the fuel cell technology has been introduced into the market of commercial mass production, and a device and a process technology capable of meeting the requirements of mass production of proton exchange membranes and continuous coating of catalysts are urgently needed.
The development of the preparation process of the Membrane Electrode (MEA) has been proved in many ways, and according to the difference of the supporting substrate of the catalyst layer in the preparation process, the preparation method of the membrane electrode is often divided into two methods, namely, catalyst preparation onto substrate (CCS) and catalyst preparation onto membrane (CCM). At present, a method is generally adopted, wherein catalyst slurry is directly sprayed on a proton exchange membrane in a gas drainage mode to form a catalyst direct coating film assembly, and the method has the biggest defects of low spraying speed and long processing period. Another method more suitable for mass production is to directly coat the catalyst slurry on a gas diffusion layer or transfer membrane, and form CCM by hot pressing transfer to a proton exchange membrane. However, the process adds a transfer printing step, and is complex and tedious to operate. Obviously, the catalyst slurry is directly coated on the proton exchange membrane, so that the manufacturing process is greatly simplified, and the production efficiency is improved. In the prior art, the catalyst slurry is directly coated on the proton exchange membrane, and the following modes are generally adopted: the CCM is prepared after the composite membrane is rolled for standby, or the finished membrane is directly purchased to prepare the CCM, and the two modes have certain 'gap' phenomena such as static electricity and the like when the liquid phase catalyst slurry contacts with the solid phase membrane, so that the final CCM has the appearance of cracks, falling and pinholes.
Disclosure of Invention
The invention aims to provide a preparation process and a continuous production line of a fuel cell membrane electrode, which can be used for solving the defects of pinholes, incomplete impregnation and the like in the continuous coating preparation process of a proton exchange composite membrane and the problems of membrane swelling and the like caused in the continuous coating process of a catalytic layer; on the other hand, the invention solves the technical problem of independent preparation of the proton exchange composite membrane and the CCM in the prior art, integrates the preparation of the composite membrane and the preparation production line of the CCM, and realizes automatic, standardized and batch production.
The technical aim of the invention is realized by the following technical scheme:
in one aspect, the present invention provides a process for preparing a fuel cell CCM, the process comprising the steps of:
(1) Coating the casting film liquid on a protective base film, and heating to obtain a first coating in a semi-viscous state; the semi-viscous state solvent content is 20-50wt%;
(2) Rolling and compounding the microporous membrane on the first coating to form a composite layer;
(3) Coating the casting film liquid on the composite layer, and heating to form gel state attached to the composite layer, wherein the solvent content of the gel state is 1-20wt%;
(4) Carrying out secondary rolling treatment on the gel-state composite layer to obtain a gel-state composite film, wherein the solvent content of the gel-state composite film is the same as that of the step (3);
(5) Coating catalyst slurry on one side of the composite membrane in a gel state, and drying to form a CCM with a single-side catalyst layer;
(6) Simultaneously with steps (1) - (5), obtaining another CCM having a single-sided catalyst layer;
(7) Stripping two protective base films with a single-side catalyst layer CCM, attaching the composite films of the two protective base films, and drying the composite films through composite hot pressing to obtain the CCM.
On the other hand, the invention provides a continuous production line of a fuel cell CCM used by the process, the continuous production line of the CCM comprises a first surface coating production line and a second surface coating production line, the first surface coating production line and the second surface coating production line both comprise a conveying roller mechanism, the conveying roller mechanisms both comprise a base film unreeling roller and a base film reeling roller, the conveying roller mechanisms are positioned between the base film unreeling roller and the base film reeling roller, a casting film liquid coating die head A, a drying channel I, a microporous film composite roller conveying mechanism, a casting film liquid coating die head B, a drying channel II, a back pressure roller mechanism, a defect detection mechanism I, a catalyst coating die head, a drying channel III, a thickness detection mechanism II and a composite hot pressure roller are sequentially arranged along the conveying direction of the conveying roller mechanisms, and the continuous production line of the CCM also comprises a drying channel IV and a CCM reeling roller which are sequentially arranged at the discharging ends of the two composite hot pressure rollers.
In yet another aspect, the present invention provides a process for preparing a fuel cell CCM by the above-described production line, the first side coating line and the second side coating line being synchronized to perform the same steps of:
(1) The protective base film is tensioned and placed in a conveying roller mechanism to realize conveying, and the microporous film is tensioned and placed in a microporous film composite roller conveying mechanism for standby;
(2) Coating the casting solution on the protective base film at the casting solution coating die head A, and heating the protective base film through a first drying channel to form a semi-viscous first coating; the semi-viscous state is a state that the solvent content is 20-50%;
(3) At the position of the microporous membrane composite roller conveying mechanism, the microporous membrane is rolled and compounded on the first coating to form a composite layer;
(4) Coating the casting solution on the composite layer at the casting solution coating die head B, and forming a gel state attached to the composite layer after passing through a drying tunnel II; the solvent content of the gel state is 1-20wt%;
(5) The secondary rolling treatment of the composite layer with gel state is realized through a double-roll mechanism, and the composite film in gel state is obtained, wherein the solvent content in gel state is the same as that in the step (4);
(6) The composite film is subjected to defect detection through one part of the defect detection mechanism, and the defective composite film part is marked;
(7) The catalyst coating die head is used for coating catalyst slurry on the untagged composite film, a CCM with a single-side catalyst layer is formed after the catalyst coating die head is completely dried through a drying tunnel III, and rolling and recycling of the protective base film are realized at a base film rolling roller after passing through a thickness detection mechanism and a defect detection mechanism II;
(8) Two rolls of CCM with single-side catalyst layers respectively transmitted on a first coating production line and a second coating production line realize composite hot pressing through a composite hot pressing roller, and then form CCM after being completely dried through a drying tunnel four and are wound by a CCM winding roller.
The invention is further provided with: the heating temperature of the first coating is 30-80 ℃; the concentration of the casting solution is 20-50wt%, the solvent used in the casting solution is a mixed solvent of deionized water and alcohols, and the alcohols solvent comprises one or more of methanol, ethanol, isopropanol and n-propanol.
The invention is further provided with: the coating thickness of the casting film liquid on the protective base film is 100-200 mu m, and the coating speed is 1-10m/min; the coating thickness of the casting film liquid on the composite layer is 50-300 mu m, and the coating speed is 1-10m/min; the coating thickness of the catalyst slurry on the composite film is 150-350 mu m, and the coating speed is 1-10m/min.
The invention is further provided with: the pressure of rolling and compounding the microporous membrane on the first coating is 1-1OMPa; the heating temperature of the casting solution after being coated on the composite layer is 40-80 ℃; the rolling pressure in the secondary rolling treatment is 1-10MPa.
The invention is further provided with: the catalyst slurry comprises, by mass, 10-20% of solid catalyst particles, 5-10% of perfluorosulfonic acid resin liquid and 70-80% of alcohol organic solvent; the catalyst slurry is dispersed by means of a high-speed dispersing machine or ultrasonic dispersion.
The invention is further provided with: the drying temperature of the catalyst slurry is 60-100 ℃; the dry thickness of the catalyst layer coated is 6-15 μm.
The invention is further provided with: the rolling pressure at the two CCM composite hot-pressing rollers with single-side catalyst layers is 1-5MPa, and the drying temperature is 60-80 ℃.
In addition, the invention also provides a fuel cell membrane electrode, which comprises the CCM prepared by the process, and the membrane electrode can be obtained by hot press molding of the CCM, the carbon paper and the plastic frame.
In summary, the invention has the following beneficial effects:
1. compared with the prior art, the method has the advantages that the composite membrane is firstly prepared for winding for standby, then the CCM is prepared, or the finished membrane is directly purchased to prepare the CCM, and the two modes have certain 'gap' phenomena such as static electricity and the like when the liquid phase catalyst slurry contacts the solid phase membrane, so that the final CCM has the appearance of cracks, falling and pinholes; the process adopts the integrated continuous production of the proton exchange membrane composite membrane process and the CCM preparation process, on one hand, the catalyst slurry can be directly coated on the proton exchange composite membrane in a gel state, so that the catalyst slurry with two phases close to each other and the composite membrane in the gel state have a more intimate contact effect, and the problems can be effectively solved;
further, after the catalyst slurry coating is finished, drying is performed again in a drying tunnel, and at the moment, the gel state composite membrane and the solvent in the catalyst slurry layer are completely volatilized, and the catalyst layer is tightly contacted with the proton exchange composite membrane, so that the contact resistance of the fuel cell is reduced, and the proton conduction capacity is improved; and because the composite film is in gel state at this moment, in the course of entering drying tunnel, in the course of volatilizing solvent together with catalyst slurry layer, the solvent volatilizes and forms the gaseous action to the catalyst layer in the composite film of gel state under this state and then has certain "pore-forming" ability to the catalyst layer, thus has improved the gas and transmitted the ability in the catalyst layer, and then has improved the response speed of the battery and utilization factor of the gas, has reduced the potential loss of the battery, and help the water produced to discharge in time, avoid the question such as the flooding; on the other hand, the preparation process of the composite membrane and the preparation process of the CCM are continuous, the production efficiency is high, the yield is high, and the gel-state composite membrane is coated in a state of having a protective base membrane, so that swelling of the proton exchange membrane is avoided;
2. the invention discloses a continuous preparation production line and process of a proton exchange composite membrane, wherein in the preparation process, a layer of casting solution is coated on a protective base membrane before the composite membrane is attached, the microporous membrane is paved and compounded after the coating is heated, and finally the casting solution is coated again, so that the microporous membrane can be well infiltrated by an upper layer of casting solution and a lower layer of casting solution, on the one hand, the defects that the casting solution cannot be fully infiltrated and is filled into pores of the microporous membrane when the casting solution is directly coated on the microporous membrane due to higher hydrophobicity and surface tension of the microporous membrane are avoided, and the like are overcome; on the other hand, the casting solution on the protective base film is heated to be in a semi-viscous flow state, so that the defects of natural flow of the casting solution, extrusion outflow of the casting film during composite rolling and the like are avoided;
3. in the preparation process, after the gel state composite layer is formed, the composite film prepared by rolling in the gel state is subjected to secondary rolling, so that the uniformity of the composite film is better, and defects such as pinholes and bubbles caused by solvent volatilization and air flow in the drying process of a drying tunnel are eliminated;
4. the intelligent detection equipment is arranged at the front end of CCM preparation and aims at the gel state composite membrane, the positions with defects such as cracks, micropores, missing coating and the like are detected and marked, and are fed back to a CCM coating system, and the defective positions are directly skipped to be coated, so that the waste of materials is avoided;
5. according to the invention, different coatings are dried through the multi-section drying tunnel, different temperature settings are carried out through the wet thickness of the coatings and the content of solvents such as casting solution, catalyst slurry and the like, the required state of the process is accurately controlled, and various required temperatures have differences, so that the differential regulation and control are carried out on the different coatings;
6. the invention adopts an integrated continuous coating production process, the composite membrane is firstly prepared, and then CCM preparation is carried out, the preparation process is simple and continuous, the method is suitable for large-scale production, a plurality of detection and supervision devices are arranged from the initial coating to the rear rolling, the prepared composite membrane is thin in thickness and good in performance, and the prepared catalytic layer is good in uniformity and free from flaws.
Drawings
FIG. 1 is a schematic diagram of a CCM continuous production line provided by the invention;
FIG. 2 is a composite membrane prepared using the scheme of example 3 of the present invention;
FIG. 3 is a composite membrane prepared using the protocol of comparative example 2.
In the figure: 1. a conveying roller mechanism; 1-1, a base film unreeling roller; 1-2, a base film wind-up roll; 2. coating a die head A by a casting solution; 3. a first drying tunnel; 4. a microporous membrane composite roller conveying mechanism; 5. coating a die head B with a casting solution; 6. a second drying tunnel; 7. a back pressure roller mechanism; 8. a first defect detection mechanism; 9. a catalyst coating die; 10. a third drying tunnel; 11. a thickness detection mechanism; 12. a second defect detection mechanism; 13. a protective base film; 14. a microporous membrane; 15. a composite hot press roll; 16. a drying tunnel IV; 17. CCM wind-up roll.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings. Unless otherwise specified, the raw materials used in the following examples and comparative examples were all commercially available conventional raw materials. In the following examples and comparative examples, the concentration or percentage thereof was the mass percentage concentration.
In the present invention, the continuous production line of the fuel cell CCM comprises a first side coating production line and a second side coating production line, wherein the first side coating production line and the second side coating production line comprise a conveying roller mechanism, each conveying roller mechanism comprises a plurality of groups of roller shafts with an automatic adjusting function, a driving electric appliance and the like, the conveying direction of the conveying roller mechanism in the first side coating production line and the second side coating production line is the conveying direction of the base film unreeling roller at the conveying start end, the base film reeling roller at the position close to the conveying tail end, and simultaneously, the continuous production line also comprises a casting film liquid coating die head a, a drying channel I, a microporous film compound roller conveying mechanism, a casting film liquid coating die head B, a drying channel II, a compound hot pressing roller mechanism, a defect detecting mechanism I, a catalyst coating die head III, a thickness detecting mechanism II, a compound hot pressing roller and a hot pressing roller which are sequentially arranged at the two compound discharging ends and a CCM four hot pressing roller at the two compound discharging ends.
Wherein, the casting film liquid coating die head A and the casting film liquid coating die head B are communicated with a feeding system of the casting film liquid; the catalyst coating die head is communicated with a feeding system of the catalyst slurry; the microporous membrane composite roller conveying mechanism is also composed of a plurality of groups of roller shafts with an automatic adjusting function, a driving electric appliance and the like; the double-pressing roller mechanism consists of a pair of roller shafts and driving electric appliances, wherein the roller shafts have an automatic adjusting function and can realize relative rotation and tangency; the first defect detection mechanism and the second defect detection mechanism are special detectors for the proton exchange membrane; the thickness detection mechanism is a thickness detector special for the proton exchange membrane; the base film wind-up roller can realize stripping recovery of the protective base film; the composite hot press roller realizes the composite of the two-layer structure by heating and relative rolling.
Example 1:
(1) Deionized water and isopropanol are used as solvents, and the mass ratio of the water to the isopropanol is 1:1; preparing perfluorinated sulfonic acid resin into a casting solution with the concentration of 20 percent for later use;
(2) Weighing 20g of Pt/C catalyst particles and 10g of 5% perfluorinated sulfonic acid resin solution, adding the mixture into 120g of isopropanol solvent, stirring and dispersing at a high speed at 25 ℃ for 60min, and using vacuum defoaming bubbles to obtain uniformly dispersed catalyst slurry;
after that, the first side coating line and the second side coating line start to synchronously perform the following same steps:
(3) The protective base film 13 is placed in the conveying roller mechanism 1 in a tensioning manner to realize conveying, and the microporous film 14 is placed in the microporous film 14 composite roller conveying mechanism 4 in a tensioning manner to realize conveying;
(4) Filling the casting solution in the step (1) into a casting solution coating die head A2, coating the casting solution on a protective base film 13 by adopting parameters of 200 mu m of coating wet thickness and 10m/min of coating speed, and heating the protective base film through a first drying channel 3 at 80 ℃ to form a first coating in a semi-viscous state, wherein the semi-viscous state is a state that the solvent content is 20%;
(5) At the position of the microporous membrane 14 composite roller conveying mechanism 4, the microporous membrane 14 is rolled and compounded on the first coating to form a composite layer, and the rolling and compounding pressure is 5MPa;
(6) Filling the casting solution in the step (1) into a casting solution coating die head B5, coating the casting solution on the composite layer in the step (5) by adopting coating parameters with the coating wet thickness of 300 mu m and the coating speed of 10m/min, and drying the composite layer at the temperature of 80 ℃ for two 6 days to form a gel state attached to the composite layer, wherein the solvent content in the gel state is 10%;
(7) Carrying out secondary rolling treatment on the gel-state composite layer in the step (6) through a composite roller mechanism 7 to obtain a gel-state composite film, wherein the pressure during secondary rolling is 10MPa;
(8) The composite film is subjected to defect detection at the first position 8 of the defect detection mechanism, and the defective composite film is marked; filling the catalyst slurry prepared in the step (2) into a catalyst coating die head 9, coating the catalyst slurry on an unlabeled composite film by adopting coating parameters with the coating wet thickness of 350 mu m and the coating speed of 10m/min, drying the composite film through a drying tunnel at 100 ℃ to form a CCM with a catalyst layer on one side, detecting the coated catalyst layer with the dry thickness of 8 mu m through a thickness detection mechanism 11 and a defect detection mechanism II 12 again, and stripping, rolling and recovering the protective base film at the position of a base film rolling roller 1-2 by using the CCM with the catalyst layer on one side which is qualified in detection;
(9) And two rolls of CCM with a catalyst layer on one side are respectively conveyed to a first coating production line and a second coating production line, meanwhile, compound hot pressing is realized through the two compound hot pressing rollers 15 under the pressure of 5MPa, and then the CCM is formed after drying through a drying tunnel IV 16 at the temperature of 80 ℃ until no solvent exists, and is wound by a CCM winding roller 17.
Example 2:
(1) Preparing a perfluorinated sulfonic acid resin into a casting film solution with the concentration of 50% by using deionized water and isopropanol as solvents, wherein the mass ratio of the water to the isopropanol is 1:1;
(2) Weighing 20g of Pt/C catalyst particles and 20g of 5% perfluorinated sulfonic acid resin solution, adding the mixture into 100g of isopropanol solvent, stirring and dispersing at a high speed at 25 ℃ for 60min, and using vacuum defoaming bubbles to obtain uniformly dispersed catalyst slurry;
after that, the first side coating line and the second side coating line start to synchronously perform the following same steps:
(3) The protective base film 13 is placed in the conveying roller mechanism 1 in a tensioning manner to realize conveying, and the microporous film 14 is placed in the microporous film 14 composite roller conveying mechanism 4 in a tensioning manner to realize conveying;
(4) Filling the casting solution in the step (1) into a casting solution coating die head A2, coating the casting solution on a protective base film 13 by adopting parameters of 100 mu m of coating wet thickness and 1m/min of coating speed, and heating the protective base film through a first drying channel 3 at 30 ℃ to form a semi-viscous first coating with a solvent content of 50%;
(5) At the position of the microporous membrane 14 composite roller conveying mechanism 4, the microporous membrane 14 is rolled and compounded on the first coating to form a composite layer;
(6) Filling the casting solution in the step (1) into a casting solution coating die head B5, coating the casting solution on the composite layer in the step (5) by adopting coating parameters with the coating wet thickness of 50 mu m and the coating speed of 1m/min, and drying the composite layer in a second drying channel at 40 ℃ to form a gel state with the solvent content of 5% attached to the composite layer;
(7) Carrying out secondary rolling treatment on the gel-state composite layer in the step (6) through a composite roller mechanism 7 to obtain a gel-state composite film, wherein the pressure during secondary rolling is 5MPa;
(8) The composite film is subjected to defect detection at the first position 8 of the defect detection mechanism, and the defective composite film is marked; filling the catalyst slurry prepared in the step (2) into a catalyst coating die head 9, coating the unlabeled composite film with coating parameters of 150 mu m in coating wet thickness and 1m/min in coating speed, drying the composite film through a drying tunnel at 60 ℃ to form a CCM with a catalyst layer on one side, detecting the coated catalyst layer with the dry thickness of 4 mu m through a thickness detection mechanism 11 and a defect detection mechanism 12 again, and stripping, rolling and recovering the protective base film at the position of a base film rolling roller 1-2 by the CCM with the catalyst layer on one side, which is qualified in detection;
(9) And two rolls of CCM with a catalyst layer on one side are respectively conveyed to a first coating production line and a second coating production line, meanwhile, compound hot pressing is realized through the two compound hot pressing rollers 15 under the pressure of 1MPa, and then the CCM is formed after drying through a drying tunnel IV 16 at the temperature of 60 ℃ until no solvent exists, and is wound by a CCM winding roller 17.
Example 3:
(1) Deionized water and isopropanol with the volume ratio of 1:1 are used as solvents, and perfluorinated sulfonic acid resin is prepared into casting solution with the concentration of 40 percent for standby;
(2) Weighing 20g of Pt/C catalyst particles and 15g of 5% perfluorosulfonic acid resin solution, adding the mixture into 100g of isopropanol solvent, stirring and dispersing the mixture at a high speed at 25 ℃ for 60 minutes, and using vacuum defoaming bubbles to obtain uniformly dispersed catalyst slurry;
after that, the first side coating line and the second side coating line start to synchronously perform the following same steps:
(3) The protective base film 13 is placed in the conveying roller mechanism 1 in a tensioning manner to realize conveying, and the microporous film 14 is placed in the microporous film 14 composite roller conveying mechanism 4 in a tensioning manner to realize conveying;
(4) Filling the casting solution in the step (1) into a casting solution coating die head A2, coating the casting solution on a protective base film 13 by adopting parameters of 150 mu m of coating wet thickness and 5m/min of coating speed, and heating the protective base film through a first drying channel 3 at 60 ℃ to obtain a semi-viscous first coating with 30% of solvent content;
(5) At the position of the microporous membrane 14 composite roller conveying mechanism 4, the microporous membrane 14 is rolled and compounded on the first coating to form a composite layer;
(6) Filling the casting solution in the step (1) into a casting solution coating die head B5, coating the casting solution on the composite layer in the step (5) by adopting coating parameters with the coating wet thickness of 150 mu m and the coating speed of 5m/min, and drying the composite layer through a second drying channel at 60 ℃ for 6 to form a gel state with the solvent content of 8 percent attached to the composite layer;
(7) Carrying out secondary rolling treatment on the gel-state composite layer in the step (6) through a composite roller mechanism 7 to obtain a gel-state composite film, wherein the pressure during secondary rolling is 8MPa;
(8) The composite film is subjected to defect detection at the first position 8 of the defect detection mechanism, and the defective composite film is marked; filling the catalyst slurry prepared in the step (2) into a catalyst coating die head 9, coating the unlabeled composite film with coating parameters of 200 mu m in coating wet thickness and 5m/min in coating speed, drying the composite film through a drying tunnel at 80 ℃ to form a CCM with a catalyst layer on one side, detecting the coated catalyst layer with the dry thickness of 6 mu m through a thickness detection mechanism 11 and a defect detection mechanism 12 again, and stripping, rolling and recovering the protective base film at the position of a base film rolling roller 1-2 by the CCM with the catalyst layer on one side, which is qualified in detection;
(9) And two rolls of CCM with a catalyst layer on one side are respectively conveyed to a first coating production line and a second coating production line, meanwhile, compound hot pressing is realized through the two compound hot pressing rollers 15 under the pressure of 3MPa, and then the CCM is formed after drying through a drying tunnel IV 16 at the temperature of 70 ℃ until no solvent exists, and is wound by a CCM winding roller 17.
Comparative example 1:
(1) Weighing 20g of Pt/C catalyst particles and 15g of 5% perfluorosulfonic acid resin solution, adding the mixture into 100g of isopropanol solvent, stirring and dispersing the mixture at a high speed at 25 ℃ for 60 minutes, and using vacuum defoaming bubbles to obtain uniformly dispersed catalyst slurry;
(2) And (3) tensioning the proton exchange membrane, placing the proton exchange membrane in a conveying roller mechanism to realize conveying, loading the catalyst slurry prepared in the step (1) into a catalyst coating die head, coating the proton exchange membrane by adopting coating parameters with the coating wet thickness of 200 mu m and the coating speed of 5m/min, drying the proton exchange membrane by a drying tunnel at 80 ℃, detecting the thickness and detecting defects, rolling the proton exchange membrane by a rolling roller, and coating the reverse side of the proton exchange membrane by the same to finally obtain the CCM.
Comparative example 2:
(1) Preparing a film casting solution with the concentration of 40% from perfluorinated sulfonic acid resin by using deionized water and isopropanol as solvents for standby, wherein the mass ratio of the water to the isopropanol is 1:1;
(2) Weighing 20g of Pt/C catalyst particles and 15g of 5% perfluorosulfonic acid resin solution, adding the mixture into 100g of isopropanol solvent, stirring and dispersing the mixture at a high speed at 25 ℃ for 60 minutes, and using vacuum defoaming bubbles to obtain uniformly dispersed catalyst slurry;
(3) Attaching a microporous membrane to a protective base membrane and conveying the microporous membrane, filling the casting solution in the step (1) into a casting solution coating die head, coating the microporous membrane by adopting parameters of 150 mu m coating wet thickness and 5m/min coating speed, and heating and drying the microporous membrane through a drying channel at 60 ℃ to form a composite membrane (non-gel state);
(4) The composite film is subjected to defect detection, and the defective composite film part is marked; loading the catalyst slurry prepared in the step (2) into a catalyst coating die head, coating the unlabeled composite film by adopting coating parameters with the coating wet thickness of 200 mu m and the coating speed of 5m/min, drying through a drying tunnel at 80 ℃, detecting the thickness and detecting defects, rolling at a rolling roller, and stripping to coat the reverse catalyst slurry to prepare the CCM.
Through comparison, the CCM is prepared by coating a casting solution on a protective base film, then attaching a microporous film, then coating the casting solution, and after a roll compacting process, coating catalyst slurry when the catalyst slurry is in a gel state. The preparation method is characterized in that the preparation process of the composite membrane is continuously operated to the preparation process of the catalyst layer, so that the prepared CCM is excellent in uniformity and electrochemical performance, and the prepared composite membrane is uniform in thickness and has good flatness and transparency, as shown in figure 2; in comparative example 1, catalyst slurry coating was directly performed on the proton exchange membrane to prepare CCM with poor electrochemical performance, which is caused by swelling of the proton exchange membrane; in comparative example 2, microporous membrane adhesion was first performed in the membrane preparation process, and then the casting solution coating was performed, so that a composite membrane was prepared, which had defects such as pinholes, bubbles, and the like, and the thickness of the composite membrane was uneven, as shown in fig. 3, and the electrochemical performance of the resulting CCM was significantly poor.
The catalyst slurry prepared by the invention is prepared into a catalytic electrode to be assembled into a battery, and then the battery performance under the oxyhydrogen condition is evaluated. Test conditions: battery operating temperature: the air inlets are all at normal pressure at 60 ℃ and the H2/O2 of 100RH% and 60RH% and the flow of 40/100mL/min, and the test results are shown in Table 1.
The test results are shown in table 1:
the present embodiment is only for explanation of the present invention and is not to be construed as limiting the present invention, and modifications to the present embodiment, which may not creatively contribute to the present invention as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present invention.
Claims (10)
1. A preparation process of a fuel cell CCM is characterized in that: the process comprises the following steps:
(1) Coating the casting film liquid on a protective base film, and heating to obtain a first coating in a semi-viscous state; the semi-viscous state solvent content is 20-50wt%;
(2) Rolling and compounding the microporous membrane on the first coating to form a composite layer;
(3) Coating the casting film liquid on the composite layer, and heating to form gel state attached to the composite layer, wherein the solvent content of the gel state is 1-20wt%;
(4) Carrying out secondary rolling treatment on the gel-state composite layer to obtain a gel-state composite film, wherein the solvent content of the gel-state composite film is the same as that of the step (3);
(5) Coating catalyst slurry on one side of the composite membrane in a gel state, and drying to form a CCM with a single-side catalyst layer;
(6) Simultaneously with steps (1) - (5), obtaining another CCM having a single-sided catalyst layer;
(7) Stripping two protective base films with a single-side catalyst layer CCM, attaching the composite films of the two protective base films, and drying the composite films through composite hot pressing to obtain the CCM.
2. A continuous production line for the process of claim 1, the CCM continuous production line comprising a first side coating line and a second side coating line, the first side coating line and the second side coating line each comprising a transfer roller mechanism, characterized in that: the CCM continuous production line further comprises a drying tunnel four and a CCM rolling roller which are sequentially arranged at the discharge end of the composite hot pressing roller.
3. A process for mass production of CCMs using the production line of claim 2, characterized by: the first surface coating production line and the second surface coating production line synchronously carry out the steps (1) - (7);
(1) The protective base film is tensioned and placed in a conveying roller mechanism to realize conveying, and the microporous film is tensioned and placed in a microporous film composite roller conveying mechanism for standby;
(2) Coating the casting film liquid on the protective base film by using a casting film liquid coating die head A, and heating the protective base film through a first drying tunnel to obtain a first coating in a semi-viscous state; the semi-viscous state solvent content is 20-50wt%;
(3) Rolling and compositing the microporous membrane on the first coating layer at the position of the microporous membrane composite roller conveying mechanism to form a composite layer;
(4) The casting solution is coated on the composite layer through a casting solution coating die head B, and is in a gel state attached to the composite layer after being heated through a drying channel II, wherein the solvent content of the gel state is 1-20wt%;
(5) Carrying out secondary rolling treatment on the gel-state composite layer through a double-roll mechanism to obtain a gel-state composite film, wherein the solvent content of the gel state is the same as that of the step (4);
(6) The composite film is subjected to defect detection through one part of the defect detection mechanism, and the defective composite film part is marked;
(7) The catalyst coating die head coats catalyst slurry on one side of the untagged composite film, a CCM with a single-side catalyst layer is formed after drying in a drying tunnel III, and rolling and recycling of the protective base film are realized at a base film rolling roller after passing through a thickness detection mechanism and a defect detection mechanism II;
(8) Two rolls of CCM with single-side catalyst layers respectively conveyed on a first coating production line and a second coating production line are laminated by a composite hot pressing roller to realize composite hot pressing, and then are dried by a drying tunnel four to form CCM which is wound by a CCM winding roller.
4. A process according to claim 1 or 3, characterized in that: the heating temperature of the first coating is 30-80 ℃; the concentration of the film casting solution is 20-50wt%, the solvent used in the film casting solution is a mixed solvent of deionized water and alcohols, and the alcohols comprise one or more of methanol, ethanol, isopropanol and n-propanol.
5. A process according to claim 1 or 3, characterized in that: the coating thickness of the casting film liquid on the protective base film is 100-200 mu m, and the coating speed is 1-10m/min; the coating thickness of the casting film liquid on the composite layer is 50-300 mu m, and the coating speed is 1-10m/min; the coating thickness of the catalyst slurry on the composite film is 150-350 mu m, and the coating speed is 1-10m/min.
6. A process according to claim 1 or 3, characterized in that: the pressure of rolling and compounding the microporous membrane on the first coating is 1-10MPa; the heating temperature of the casting solution after being coated on the composite layer is 40-80 ℃; the rolling pressure in the secondary rolling treatment is 1-10MPa.
7. A process according to claim 1 or 3, characterized in that: the catalyst slurry comprises, by mass, 10-20% of solid catalyst particles, 5-10% of perfluorosulfonic acid resin liquid and 70-80% of alcohol organic solvent; the catalyst slurry is dispersed by means of a high-speed dispersing machine or ultrasonic dispersion.
8. A process according to claim 1 or 3, characterized in that: the drying temperature of the catalyst slurry is 60-100 ℃; the dry thickness of the catalyst layer coated is 6-15 μm.
9. A process according to claim 1 or 3, characterized in that: the pressure of the two CCM composite hot pressing with the single-side catalyst layers is 1-5MPa, and the drying temperature is 60-80 ℃.
10. A fuel cell membrane electrode comprising a CCM prepared by the process of claim 1 or 3.
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