CN114204050A - Preparation process and continuous production line of membrane electrode of fuel cell - Google Patents
Preparation process and continuous production line of membrane electrode of fuel cell Download PDFInfo
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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
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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
-
- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- 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 fuel cell membrane electrode preparation process and a continuous production line, wherein the preparation process comprises the following steps: coating a layer of casting solution on a protective base film, heating the protective base film to form a gel state, compounding the gel state with a microporous film, then coating the casting solution, heating the casting solution to form a gel state, and coating catalyst slurry to obtain CCM; the continuous production line comprises a transfer roller mechanism, and a base film unreeling roller mechanism, a casting film liquid coating die head A, a first drying channel, a microporous film composite roller transfer mechanism, a casting film liquid coating die head B, a second drying channel, a re-pressing roller mechanism, a first defect detection mechanism, a catalyst coating die head, a third drying channel, a thickness detection mechanism, a second defect detection mechanism and the like are sequentially arranged along the transfer direction of the transfer roller mechanism; the invention integrates the composite membrane preparation and the CCM preparation production line, solves the problems of membrane swelling and the like caused in the continuous coating process of the catalyst 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 and a continuous production line of a fuel cell membrane electrode, 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 multiple fields of automobile transportation, distributed power generation and the like. The performance and yield of the membrane electrode, which is used 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 by the membrane electrode preparation also restricts the rapid development of the fuel cell. At present, the fuel cell technology has already met the market lead-in period of commercial mass production, and an apparatus and a process technology capable of meeting the mass production of proton exchange membranes and the continuous coating of catalysts are urgently needed.
The development of Membrane Electrode (MEA) preparation technology has been verified, and membrane electrode preparation methods are often classified into catalyst on substrate (CCS) and catalyst on membrane (CCM) methods according to the difference of the catalyst layer supporting substrates during the preparation process. At present, the method which is generally adopted is to directly spray catalyst slurry on a proton exchange membrane in a gas drainage mode to form a catalyst direct coating membrane assembly, and the biggest defect of the method is that the spraying speed is slow, so that the processing period is long. Another method more suitable for mass production is to directly coat the catalyst slurry on the gas diffusion layer or the transfer film, and form the CCM by hot-pressing and transferring onto the proton exchange membrane. However, the process adds a transfer step, and the operation is complicated and cumbersome. 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 methods are generally adopted: the CCM is prepared after the composite membrane is prepared and rolled for later use, or the finished membrane is directly purchased to prepare the CCM, and the two modes have the phenomenon of certain gap caused by the contact between the liquid-phase catalyst slurry and the solid-phase membrane, such as static electricity, so that the final CCM has cracks, falls and pinholes.
Disclosure of Invention
The invention aims to provide a fuel cell membrane electrode preparation process and a continuous production line, which solve the defects of pinholes, incomplete impregnation and the like in the proton exchange composite membrane continuous coating preparation process and solve the problems of membrane swelling and the like caused in the catalytic layer continuous coating process; on the other hand, the invention solves the process problem of independently preparing the proton exchange composite membrane and the CCM in the prior art, integrates the composite membrane preparation and the CCM preparation production line, and realizes automatic, standardized and batch production.
The technical purpose of the invention is realized by the following technical scheme:
in one aspect, the present invention provides a process for preparing a CCM for a fuel cell, 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 flow state; the content of the semi-viscous state solvent is 20-50 wt%;
(2) rolling and compounding the microporous membrane on the first coating to form a composite layer;
(3) coating the casting solution on a composite layer, and heating to form a gel state attached to the composite layer, wherein the gel state solvent content is 1-20 wt%;
(4) carrying out secondary rolling treatment on the gel-state composite layer to obtain a gel-state composite film, wherein the content of the gel-state solvent is the same as that in 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) synchronously performing the steps (1) to (5) to obtain another CCM with a single-side catalyst layer;
(7) and (3) stripping two protective base films with a single-side catalyst layer CCM, attaching the composite films of the two protective base films, and carrying out composite hot pressing and drying to obtain the CCM.
In another aspect, the invention provides a continuous CCM production line for fuel cells, the CCM continuous production line comprises a first surface coating production line and a second surface coating production line, both the first surface coating production line and the second surface coating production line comprise conveying roller mechanisms, the conveying roller mechanisms comprise a base film unwinding roller and a base film winding roller which are positioned between the base film unwinding roller and the base film winding roller, and a casting solution coating die head A, a drying channel I, a microporous membrane composite roller conveying mechanism, a casting solution coating die head B, a drying channel II, a re-pressing roller mechanism, a defect detection mechanism I, a catalyst coating die head, a drying channel III, a thickness detection mechanism, a defect detection mechanism II and a composite hot-pressing roller are sequentially arranged along the conveying direction of the conveying roller mechanism, the CCM continuous production line further comprises a drying tunnel IV and a CCM wind-up roll which are sequentially arranged at the discharge ends of the two composite hot-pressing rolls.
In another aspect, the present invention provides a process for manufacturing a fuel cell CCM through the above production line, wherein the first coating production line and the second coating production line synchronously perform the following steps:
(1) the protective base film is tensioned in a conveying roller mechanism to realize conveying, and the microporous film is tensioned in a microporous film composite roller conveying mechanism for standby;
(2) coating the casting solution on the protective base film at a casting solution coating die head A, and heating the protective base film through a first drying channel to form a first coating in a semi-viscous flow state; the semi-viscous state is a state with 20-50% of solvent content;
(3) at the microporous film composite roller conveying mechanism, realizing that the microporous film 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 second drying channel; the gel state solvent content is 1-20 wt%;
(5) secondary rolling treatment of the composite layer with the gel state is achieved through a double-rolling mechanism, and the composite film in the gel state is obtained, wherein the content of the solvent in the gel state is the same as that in the step (4);
(6) the composite membrane passes through a defect detection mechanism for defect detection, and the part of the composite membrane with the defects is marked;
(7) the catalyst coating die head is used for coating catalyst slurry on an unmarked composite membrane, CCM with a single-side catalyst layer is formed after the catalyst slurry is completely dried by a drying tunnel, and the protective base membrane is wound and recovered at a base membrane winding roller after passing through a thickness detection mechanism and a defect detection mechanism II;
(8) two rolls of CCM that have the unilateral catalyst layer that convey respectively on first coating production line and second coating production line realize compound hot pressing through compound hot pressing roller department simultaneously, later form CCM after drying tunnel four is dried completely, are rolled up by the CCM wind-up roll.
The invention is further configured to: the heating temperature of the first coating is 30-80 ℃; the concentration of the casting solution is 20-50 wt%, the solvent used by the casting solution is a mixed solvent of deionized water and alcohol, and the alcohol solvent comprises one or more of methanol, ethanol, isopropanol and n-propanol.
The invention is further configured to: the coating thickness of the casting solution on the protective basement membrane is 100-200 mu m, and the coating speed is 1-10 m/min; the coating thickness of the casting solution on the composite layer is 50-300 μm, and the coating speed is 1-10 m/min; the coating thickness of the catalyst slurry on the composite membrane is 150-350 mu m, and the coating speed is 1-10 m/min.
The invention is further configured to: the pressure of the microporous membrane on the first coating layer in a rolling and compounding mode is 1-1 OMPa; the heating temperature of the casting film liquid after being coated on the composite layer is 40-80 ℃; the rolling pressure during the secondary rolling treatment is 1-10 MPa.
The invention is further configured to: the catalyst slurry comprises 10-20% of solid catalyst particles, 5-10% of perfluorinated sulfonic acid resin liquid and 70-80% of alcohol organic solvent in percentage by mass; the catalyst slurry is dispersed by a high-speed disperser or by ultrasonic dispersion.
The invention is further configured to: the drying temperature of the catalyst slurry is 60-100 ℃; the dry thickness of the coated catalyst layer is 6-15 μm.
The invention is further configured to: the rolling pressure of the two CCM composite hot-pressing rollers with the single-side catalyst layer is 1-5MPa, and the drying temperature is 60-80 ℃.
In addition, the invention also provides a membrane electrode of the fuel cell, which comprises the CCM prepared by the process, and the membrane electrode can be obtained by hot-press molding the CCM, the carbon paper and the plastic frame.
In conclusion, the invention has the following beneficial effects:
1. compared with the prior art, the CCM is prepared after the composite membrane is prepared for standby, or the finished membrane is directly purchased to prepare the CCM, and both the two modes have certain 'gap' phenomena such as static electricity and the like caused by the contact between the liquid-phase catalyst slurry and the solid-phase membrane, so that the final CCM has the appearance of cracks, falling and pinholes; the process adopts the continuous production integrating the proton exchange membrane composite membrane process and the CCM preparation process, on one hand, the catalyst slurry can be directly coated when the proton exchange membrane is in a gel state, so that the catalyst slurry and the gel-state composite membrane which are two-phase and close to each other have a more 'intimate' contact effect, and the problems can be effectively solved;
furthermore, after the catalyst slurry is coated, the drying tunnel is dried again, at the moment, the solvent in the gel-state composite membrane and the catalyst slurry layer is completely volatilized, the catalyst layer is tightly contacted with the proton exchange composite membrane, the contact resistance of the fuel cell is reduced, and the proton conductivity is improved; and because the composite membrane is in the gel state at this moment, in the drying process of entering the drying tunnel, it is in the process of solvent volatilization together with slurry layer of catalyst, the solvent in the composite membrane of gel state volatilizes and forms the gas to act on catalyst layer and then have certain "pore-forming" ability to catalyst layer under this state, thus has improved the gas and transmitted the ability in the catalysis layer, and then has improved the response speed and utilization rate of the gas of the battery, has reduced the potential loss of the battery, and help the water produced to discharge in time, avoid the problem such as 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 under the condition that the gel-state composite membrane has a protective base membrane, so that the swelling of a proton exchange membrane is avoided;
2. the invention discloses a continuous preparation production line and a continuous preparation process of a proton exchange composite membrane, wherein in the preparation process, a layer of membrane casting solution is firstly coated on a protective base membrane before the composite membrane is attached, the microporous membrane is laid and compounded after the coating is heated, and finally the membrane casting solution is coated again, so that the upper layer of membrane casting solution and the lower layer of membrane casting solution can well infiltrate the microporous membrane, thereby avoiding the defects that the membrane casting solution cannot be completely infiltrated and filled into pores of the microporous membrane when the membrane casting solution is directly coated on the microporous membrane due to the larger hydrophobicity and surface tension of the microporous membrane, and the like; on the other hand, the casting film liquid on the protective base film is heated to be in a semi-viscous state, so that the defects of natural flowing of the casting film liquid, extrusion and outflow of the casting film during composite rolling and the like are avoided;
3. in the preparation process, the gel-state composite layer is formed and then rolled for the second time, the composite film prepared by rolling in the gel state has better uniformity, and defects such as pinholes, bubbles and the like caused by solvent volatilization and air flow in the drying process of a drying tunnel are eliminated;
4. the invention has intelligent detection equipment aiming at the gel state composite membrane at the CCM preparation front end, detects and marks the positions with defects such as cracks, micropores, missing coating and the like, and feeds back the positions to a CCM coating system, and the defective positions are directly skipped to coat, thereby avoiding the waste of materials;
5. according to the invention, different coatings are dried by adopting multiple sections of drying tunnels, different temperature settings are carried out according to the wet thickness of the coatings and the content of solvents such as a casting solution, a catalyst slurry and the like, the required state of the process is accurately controlled, and different required temperatures have differences, so that different coatings are differentially regulated and controlled;
6. the invention adopts an integrated continuous coating production process, firstly prepares the composite membrane, then prepares the CCM, has simple and continuous preparation process, is suitable for large-scale production, is coated from the primary end to the back end and is coiled, and is provided with a plurality of detection and supervision devices, and the prepared composite membrane has thin thickness and good performance, and the prepared catalyst layer has good uniformity and no flaw.
Drawings
FIG. 1 is a schematic view of a CCM continuous production line provided by the present invention;
FIG. 2 is a composite membrane prepared according to the embodiment of example 3 of the present invention;
FIG. 3 is a composite membrane prepared using the scheme of comparative example 2.
In the figure: 1. a transfer roller mechanism; 1-1, unwinding a base film; 1-2, a base film winding roller; 2. coating the casting solution on a die head A; 3. a first drying channel; 4. a microporous membrane composite roller conveying mechanism; 5. coating the casting solution on a die head B; 6. a second drying tunnel; 7. a re-compression 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. protecting the base film; 14. a microporous membrane; 15. compounding hot pressing rollers; 16. a fourth drying tunnel; 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 are all commercially available conventional raw materials. In addition, the concentrations or percentages in the following examples and comparative examples are mass percentage concentrations.
A CCM continuous production line of fuel cells used in the following embodiments, as shown in FIG. 1, includes a first surface coating production line and a second surface coating production line, both of which include a transfer roller mechanism composed of a plurality of sets of rollers with automatic adjustment function and a driving electrical appliance, and the like Catalyst coating die head, drying tunnel three, thickness detection mechanism, defect detection mechanism two and compound hot pressing roller, CCM continuous production line still includes drying tunnel four and the CCM wind-up roll that sets gradually at two compound hot pressing roller discharge ends department at last.
Wherein the casting solution coating die head A and the casting solution coating die head B are both communicated with a feeding system of the casting solution; 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 automatic adjusting functions, a driving electric appliance and the like; the double-pressing roller mechanism consists of a pair of roller shafts and a driving electric appliance, 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 both special proton exchange membrane detectors; the thickness detection mechanism is a thickness detector special for the proton exchange membrane; the base film winding roller can realize the stripping and recycling of the protective base film; the composite hot-press roller realizes the composition of the two-layer structure by heating and opposite 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 a casting solution with the concentration of 20% by using perfluorinated sulfonic acid resin for later use;
(2) weighing 20g of Pt/C catalyst particles and 10g of 5% perfluorosulfonic acid resin solution, adding into 120g of isopropanol solvent, stirring and dispersing at a high speed for 60min at 25 ℃, and defoaming bubbles by using vacuum to obtain uniformly dispersed catalyst slurry;
then, the first surface coating production line and the second surface coating production line start to synchronously carry out the following same steps:
(3) the protective base film 13 is placed in the conveying roller mechanism 1 in a tensioning mode to realize conveying, and the microporous film 14 is placed in the microporous film 14 composite roller conveying mechanism 4 in a tensioning mode 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 the protective base film 13 by adopting the parameters of coating wet thickness of 200 mu m and coating speed of 10m/min, and heating the coating through a drying channel I3 at 80 ℃ to form a first coating in a semi-viscous state, wherein the semi-viscous state is a state that the content of a solvent is 20%;
(5) at the position of the microporous membrane 14 composite roller conveying mechanism 4, realizing that the microporous membrane 14 is rolled and compounded on the first coating to form a composite layer, wherein the pressure of the rolling and compounding is 5 MPa;
(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 of a coating wet thickness of 300 mu m and a coating speed of 10m/min, and forming a gel state attached to the composite layer after passing through a drying channel II 6 at the temperature of 80 ℃, wherein the content of a solvent in the gel state is 10%;
(7) secondary rolling treatment is carried out on the gel-state composite layer in the step (6) through a secondary rolling mechanism 7 to obtain a gel-state composite film, and the pressure during secondary rolling is 10 MPa;
(8) the composite membrane passes through a first 8-position defect detection mechanism to be subjected to defect detection, and the position of the defective composite membrane is marked; loading the catalyst slurry prepared in the step (2) into a catalyst coating die head 9, coating the catalyst slurry on an unmarked composite membrane by adopting coating parameters of the coating wet thickness of 350 mu m and the coating speed of 10m/min, drying the composite membrane by a drying tunnel at 100 ℃ to form CCM with a catalyst layer on one side, wherein the dry thickness of the coated catalyst layer is 8 mu m, and detecting the coated catalyst layer by a thickness detection mechanism 11 and a defect detection mechanism II 12 again, so that the qualified CCM with the catalyst layer on one side can realize the peeling, winding and recycling of the protective base membrane at a base membrane winding roller 1-2;
(9) the CCM with the catalyst layer on one side is conveyed to the first coating production line and the second coating production line respectively, composite hot pressing is achieved through the two composite hot pressing rollers 15 under the pressure of 5MPa, then the CCM is dried at the temperature of 80 ℃ through the drying tunnel four 16 until no solvent exists, the CCM is formed, and the CCM is wound by the CCM winding roller 17.
Example 2:
(1) deionized water and isopropanol are used as solvents, and perfluorinated sulfonic acid resin is prepared into casting solution with the concentration of 50%, wherein the mass ratio of water to isopropanol is 1: 1;
(2) weighing 20g of Pt/C catalyst particles and 20g of 5% perfluorosulfonic acid resin solution, adding the Pt/C catalyst particles and the 5% perfluorosulfonic acid resin solution into 100g of isopropanol solvent, stirring and dispersing at a high speed for 60min at 25 ℃, and defoaming bubbles by using vacuum to obtain uniformly dispersed catalyst slurry;
then, the first surface coating production line and the second surface coating production line start to synchronously carry out the following same steps:
(3) the protective base film 13 is placed in the conveying roller mechanism 1 in a tensioning mode to realize conveying, and the microporous film 14 is placed in the microporous film 14 composite roller conveying mechanism 4 in a tensioning mode 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 the protective basement membrane 13 by adopting the parameters of the coating wet thickness of 100 mu m and the coating speed of 1m/min, and heating the coating solution by a drying channel I3 at the temperature of 30 ℃ to form a first coating in a semi-viscous state with the solvent content of 50 percent;
(5) at the position of the microporous membrane 14 composite roller conveying mechanism 4, realizing that 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 of coating wet thickness of 50 mu m and coating speed of 1m/min, and forming a gel state with the solvent content of 5 percent attached to the composite layer after passing through a drying channel II 6 at the temperature of 40 ℃;
(7) secondary rolling treatment is carried out on the gel-state composite layer in the step (6) through a secondary rolling mechanism 7 to obtain a gel-state composite film, and the pressure during secondary rolling is 5 MPa;
(8) the composite membrane passes through a first 8-position defect detection mechanism to be subjected to defect detection, and the position of the defective composite membrane is marked; loading the catalyst slurry prepared in the step (2) into a catalyst coating die head 9, coating the catalyst slurry on an unmarked composite membrane by adopting coating parameters of coating wet thickness of 150 mu m and coating speed of 1m/min, drying the composite membrane by a drying tunnel at 60 ℃ to form CCM with a catalyst layer on one side, detecting the coated catalyst layer with dry thickness of 4 mu m by a thickness detection mechanism 11 and a defect detection mechanism II 12, and realizing stripping, winding and recycling of the protective base membrane at a base membrane winding roller 1-2 by the qualified CCM with the catalyst layer on one side;
(9) the CCM with the catalyst layer on one side is conveyed to the first coating production line and the second coating production line respectively, composite hot pressing is achieved through the two composite hot pressing rollers 15 under the pressure of 1MPa, then the CCM is dried at the temperature of 60 ℃ through the drying tunnel four 16 until no solvent exists, the CCM is formed, and the CCM is wound by the CCM winding roller 17.
Example 3:
(1) deionized water and isopropanol in a volume ratio of 1: 1 are used as solvents, and perfluorinated sulfonic acid resin is prepared into casting solution with the concentration of 40% for later use;
(2) weighing 20g of Pt/C catalyst particles and 15g of 5% perfluorosulfonic acid resin solution, adding the Pt/C catalyst particles and the 5% perfluorosulfonic acid resin solution into 100g of isopropanol solvent, stirring and dispersing at a high speed for 60min at 25 ℃, and defoaming bubbles by using vacuum to obtain uniformly dispersed catalyst slurry;
then, the first surface coating production line and the second surface coating production line start to synchronously carry out the following same steps:
(3) the protective base film 13 is placed in the conveying roller mechanism 1 in a tensioning mode to realize conveying, and the microporous film 14 is placed in the microporous film 14 composite roller conveying mechanism 4 in a tensioning mode 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 the protective base film 13 by adopting the parameters of coating wet thickness of 150 mu m and coating speed of 5m/min, and heating the protective base film through a drying channel I3 at 60 ℃ to form a first coating in a semi-viscous state with the solvent content of 30 percent;
(5) at the position of the microporous membrane 14 composite roller conveying mechanism 4, realizing that 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 of coating wet thickness of 150 mu m and coating speed of 5m/min, and forming a gel state with the content of the solvent attached to the composite layer being 8% after passing through a drying channel II 6 at 60 ℃;
(7) secondary rolling treatment is carried out on the gel-state composite layer in the step (6) through a secondary rolling mechanism 7 to obtain a gel-state composite film, and the pressure during secondary rolling is 8 MPa;
(8) the composite membrane passes through a first 8-position defect detection mechanism to be subjected to defect detection, and the position of the defective composite membrane is marked; loading the catalyst slurry prepared in the step (2) into a catalyst coating die head 9, coating the catalyst slurry on an unmarked composite membrane by adopting coating parameters of the coating wet thickness of 200 mu m and the coating speed of 5m/min, drying the composite membrane by a drying tunnel at the temperature of 80 ℃ to form CCM with a catalyst layer on one side, detecting the coated catalyst layer with the dry thickness of 6 mu m by a thickness detection mechanism 11 and a defect detection mechanism II 12, and realizing the stripping, winding and recycling of the protective base membrane at a base membrane winding roller 1-2 by the qualified CCM with the catalyst layer on one side;
(9) the CCM with the catalyst layer on one side is conveyed to the first coating production line and the second coating production line respectively, composite hot pressing is achieved through the two composite hot pressing rollers 15 under the pressure of 3MPa, then drying is conducted through the drying tunnel IV 16 at the temperature of 70 ℃ until no solvent exists, the CCM is formed, and the CCM is wound through the 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 Pt/C catalyst particles and the 5% perfluorosulfonic acid resin solution into 100g of isopropanol solvent, stirring and dispersing at a high speed for 60min at 25 ℃, and defoaming bubbles by using vacuum to obtain uniformly dispersed catalyst slurry;
(2) and (3) tensioning the proton exchange membrane, placing the catalyst slurry prepared in the step (1) into a catalyst coating die head to realize conveying, coating the catalyst slurry on 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 the temperature of 80 ℃, detecting the thickness and the defects, rolling the proton exchange membrane on a winding roll, and coating the reverse side of the proton exchange membrane on the same way to finally obtain the CCM.
Comparative example 2:
(1) deionized water and isopropanol are used as solvents, and perfluorinated sulfonic acid resin is prepared into casting solution with the concentration of 40% for later use, wherein the mass ratio of water to isopropanol is 1: 1;
(2) weighing 20g of Pt/C catalyst particles and 15g of 5% perfluorosulfonic acid resin solution, adding the Pt/C catalyst particles and the 5% perfluorosulfonic acid resin solution into 100g of isopropanol solvent, stirring and dispersing at a high speed for 60min at 25 ℃, and defoaming bubbles by using vacuum to obtain uniformly dispersed catalyst slurry;
(3) attaching a microporous membrane to a protective base membrane and transmitting, filling the casting solution obtained in the step (1) into a casting solution coating die head, coating the casting solution on the microporous membrane by adopting the parameters of coating wet thickness of 150 mu m and coating speed of 5m/min, and heating and drying the microporous membrane through a drying tunnel at 60 ℃ to form a composite membrane (non-gel state);
(4) detecting defects of the composite film, and marking the parts of the composite film with the defects; and (3) loading the catalyst slurry prepared in the step (2) into a catalyst coating die head, coating the catalyst slurry on an unmarked composite membrane by adopting coating parameters of the coating wet thickness of 200 mu m and the coating speed of 5m/min, drying in a drying tunnel at the temperature of 80 ℃, detecting the thickness and the defects, rolling at a wind-up roll, and then stripping to coat the catalyst slurry on the reverse side to prepare the CCM.
The comparison shows that the CCM is prepared by coating the casting solution on the protective base film, attaching the microporous film, coating the casting solution, rolling and compacting, coating the catalyst slurry in a gel state, and finally preparing the CCM. The CCM prepared by the method has excellent uniformity and electrochemical performance from the composite membrane preparation process to the catalyst layer preparation process, and the prepared composite membrane has uniform thickness, good flatness and transparency, as shown in figure 2; in the comparative example 1, the catalyst slurry is directly coated on the proton exchange membrane, and the electrochemical performance of the prepared CCM is poor, which is caused by the swelling of the proton exchange membrane; in comparative example 2, the microporous membrane was attached first in the membrane preparation process, and then the membrane casting solution was applied to the prepared composite membrane, which had defects such as pinholes and bubbles, and non-uniform thickness of the composite membrane, as shown in fig. 3, and the electrochemical performance of the finally obtained CCM was significantly poor.
The catalyst slurry prepared by the method is prepared into a catalytic electrode to be assembled into a battery, and then the battery performance under the hydrogen-oxygen condition is evaluated. And (3) testing conditions are as follows: battery operating temperature: 60 ℃, H2/O2100 RH% and 60 RH%, the flow rate is 40/100mL/min, the air inlet is normal pressure, and the test results are shown in Table 1.
The test results are shown in table 1:
the present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (10)
1. A process for preparing a CCM for a fuel cell, comprising: 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 flow state; the content of the semi-viscous state solvent is 20-50 wt%;
(2) rolling and compounding the microporous membrane on the first coating to form a composite layer;
(3) coating the casting solution on a composite layer, and heating to form a gel state attached to the composite layer, wherein the gel state solvent content is 1-20 wt%;
(4) carrying out secondary rolling treatment on the gel-state composite layer to obtain a gel-state composite film, wherein the content of the gel-state solvent is the same as that in 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) synchronously performing the steps (1) to (5) to obtain another CCM with a single-side catalyst layer;
(7) and (3) stripping two protective base films with a single-side catalyst layer CCM, attaching the composite films of the two protective base films, and carrying out composite hot pressing and drying to obtain the CCM.
2. A continuous production line for the process of claim 1, wherein the CCM continuous production line comprises a first surface coating production line and a second surface coating production line, both of which comprise a conveying roller mechanism, and the continuous production line is characterized in that: conveying roller mechanism all includes that the base film unreels roller and base film wind-up roll, is located between base film unreeling roller and the base film wind-up roll, and follows conveying roller mechanism's direction of transfer all sets gradually membrane casting liquid coating die head A, drying tunnel one, microporous membrane composite roll conveying mechanism, membrane casting liquid coating die head B, drying tunnel two, double nip roller mechanism, defect detection mechanism one, catalyst coating die head, drying tunnel three, thickness detection mechanism, defect detection mechanism two and compound hot pressing roller, CCM continuous production line still sets gradually two drying tunnel four and CCM wind-up roll of compound hot pressing roller discharge end department.
3. A process for mass production of CCM using the production line of claim 2, wherein: synchronously performing the steps (1) - (7) on the first surface coating production line and the second surface coating production line;
(1) the protective base film is tensioned in a conveying roller mechanism to realize conveying, and the microporous film is tensioned in a microporous film composite roller conveying mechanism for standby;
(2) coating the casting film liquid on the protective base film by the casting film liquid coating die head A, and heating through the first drying channel to obtain a first coating in a semi-viscous flow state; the content of the semi-viscous state solvent is 20-50 wt%;
(3) rolling and compounding the microporous film on the first coating at the microporous film compound roller conveying mechanism to form a compound layer;
(4) the casting solution coating die head B coats the casting solution on the composite layer, and the casting solution is heated by the drying channel II to be in a gel state attached to the composite layer, wherein the content of the gel-state solvent is 1-20 wt%;
(5) carrying out secondary rolling treatment on the gel-state composite layer through a re-rolling mechanism to obtain a gel-state composite film, wherein the content of the gel-state solvent is the same as that in the step (4);
(6) the composite membrane passes through a defect detection mechanism for defect detection, and the part of the composite membrane with the defects is marked;
(7) the catalyst coating die head coats catalyst slurry on one side of an unmarked composite membrane, a CCM with a single-side catalyst layer is formed after drying in a drying tunnel III, and the rolling recovery of the protective base membrane is realized at a base membrane rolling roller after passing through a thickness detection mechanism and a defect detection mechanism II;
(8) two rolls of CCM that have the unilateral catalyst layer that convey respectively on first coating production line and second coating production line, simultaneously through compound hot pressing roller department, the laminating of the complex film of the two realizes compound hot pressing, later forms CCM after drying through drying tunnel four, by the rolling of CCM wind-up roll.
4. The process according to claim 1 or 3, characterized in that: the heating temperature of the first coating is 30-80 ℃; the concentration of the casting solution is 20-50 wt%, the solvent used by the 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. The process according to claim 1 or 3, characterized in that: the coating thickness of the casting solution on the protective basement membrane is 100-200 mu m, and the coating speed is 1-10 m/min; the coating thickness of the casting solution on the composite layer is 50-300 μm, and the coating speed is 1-10 m/min; the coating thickness of the catalyst slurry on the composite membrane is 150-350 mu m, and the coating speed is 1-10 m/min.
6. The process according to claim 1 or 3, characterized in that: the pressure of the microporous membrane on the first coating layer in a rolling and compounding way is 1-10 MPa; the heating temperature of the casting film liquid after being coated on the composite layer is 40-80 ℃; and the rolling pressure during the secondary rolling treatment is 1-10 MPa.
7. The process according to claim 1 or 3, characterized in that: the catalyst slurry comprises 10-20% of solid catalyst particles, 5-10% of perfluorinated sulfonic acid resin liquid and 70-80% of alcohol organic solvent in percentage by mass; the catalyst slurry is dispersed by a high-speed disperser or by ultrasonic dispersion.
8. The 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 coated catalyst layer is 6-15 μm.
9. The process according to claim 1 or 3, characterized in that: the pressure of the CCM composite hot pressing of the two CCMs with the single-side catalyst layer 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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