Membrane electrode catalyst layer stripping device and method, failure detection method and catalyst layer recovery method
The membrane electrode catalytic layer stripping device and method have achieved high integrity stripping and accurate failure diagnosis of membrane electrodes, solving the environmental protection and efficiency problems of membrane electrode detection and recycling in the prior art. It is applicable to membrane electrode samples of different sizes and models.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-21
- Publication Date
- 2026-05-12
AI Technical Summary
Existing technologies cannot accurately detect the location and cause of failure without damaging the membrane electrode structure, and the catalyst recovery process uses a large amount of organic solvents, which poses environmental and efficiency problems.
A membrane electrode catalytic layer stripping device is adopted, which uses solvent atomization, controllable pressure and heating drying unit to achieve mechanical anchoring-assisted differential swelling stripping of the catalytic layer through gradient pore size porous plate. Failure diagnosis and catalytic layer recovery are carried out by combining component cross-combination test method.
It achieves high integrity peeling of membrane electrode assemblies, accurately diagnoses failure sites, reduces the use of organic solvents, and improves the environmental friendliness and efficiency of catalyst recovery. It is applicable to membrane electrode samples of different sizes and models.
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Figure CN122013251A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of water electrolysis for hydrogen production, specifically to a membrane electrode catalytic layer stripping device, method, failure detection method, and catalytic layer recovery method. Background Technology
[0002] Hydrogen production through water electrolysis is one of the most promising pathways to achieving the "dual carbon target." Among these technologies, proton exchange membrane electrolysis (PEMWE) has seen significant development in recent years due to its advantages such as long lifespan and good resistance to fluctuations. However, membrane electrode performance degradation is the primary cause of PEMWE electrolyzer failures. The possible causes of membrane electrode degradation or failure are diverse and complex, including anion / anode catalyst layer failure (catalyst layer shedding, catalyst layer poisoning, polymer loss, etc.) and proton exchange membrane failure (perforation, decreased proton conductivity). Accurately pinpointing the location and mechanism of electrolyzer or membrane electrode failure is crucial for the design, production, and long-term operation of commercial PEM electrolyzers; however, reliable related technologies are currently lacking.
[0003] CN108107090A proposes a method for detecting membrane electrode fouling in a solid polymer electrolyte water electrolyzer. Specifically, the method involves: measuring the voltage of the electrolyzer in current mode and observing any voltage abrupt changes; then measuring the electrochemical impedance spectroscopy (EIS) performance of the electrolyzer and observing any significant abrupt changes in internal resistance; combining the voltage and EIS abrupt changes to determine whether performance degradation is caused by fouling. This method can accurately and effectively evaluate whether the membrane electrode has deteriorated. However, it cannot further confirm the location and cause of the deterioration.
[0004] CN114678553A and CN118983457A propose a method for recycling and reusing waste proton exchange membrane electrolysis (PEM) electrodes. The method involves immersing the waste EPM electrode in alcohol / water, then using ultrasonication, scraping, and rinsing to peel the catalyst layer from the proton exchange membrane. The proton exchange membrane is then washed with a solvent and regenerated. The liquid suspension is collected, filtered, and centrifuged to obtain the catalyst residue, which is then recycled. Both methods focus on catalyst recovery. While physicochemical testing can be performed on the catalyst washed off the EPM electrode, the potential causes of failure at the structural and process levels of the EPM electrode remain difficult to trace.
[0005] The problems with these existing technologies are that they can only perform overall testing of the membrane electrode or complete destruction for physicochemical analysis, and cannot provide feedback on structural problems of the electrolyzer or membrane electrode (such as insufficient local proton conductivity of the proton exchange membrane, uneven membrane thickness distribution, local perforation, etc.), which significantly restricts the research and development and operation of commercial PEM electrolyzer products.
[0006] Currently, PEM water electrolysis technology is in the stage of commercialization, but there is still a lack of reliable technical means for failure detection of product-grade PEM membrane electrodes, which seriously hinders the technological development of related products. Summary of the Invention
[0007] In view of this, the purpose of this invention is to provide a membrane electrode catalytic layer stripping device, method, failure detection method, and catalytic layer recovery method, aiming to overcome at least one related technical problem existing in the prior art. This method and device can completely strip the catalytic layer and accurately and comprehensively evaluate the failure location and failure mechanism of the membrane electrode. Furthermore, it can directly achieve dry-state recovery of the catalyst, avoiding the use of large amounts of organic solvents in the methods described in related patents, making it more environmentally friendly and efficient.
[0008] To achieve the above objectives, the present invention adopts the following technical solution: In a first aspect, this application provides a membrane electrode catalytic layer stripping device, comprising: The solvent supply unit includes an organic reagent storage tank and pipelines connected in sequence; The pressure control unit includes a hydraulic actuation module and a heating module, and the output pressure and output temperature of the pressure control unit are adjustable; The stripping chamber includes an end plate with microchannels, an elastic sealing assembly, and a porous plate. The end plate and the porous plate are arranged opposite to each other and form a pressurizable sealed chamber through the elastic sealing assembly. The inner surface of the end plate and the inner wall of the microchannels are coated with polytetrafluoroethylene. The waste liquid recovery unit is connected to the exhaust / liquid port of the stripping chamber via a pipeline; The porous plate is used to support and contact the catalytic layer of the membrane electrode to be stripped.
[0009] In some embodiments, the porous plate has a gradient pore size structure, wherein the pore size gradually decreases from the side facing the end plate to the side facing the catalyst layer.
[0010] In some embodiments, the pore size of the porous plate facing the end plate is 100±10μm, and the pore size facing the catalyst layer is 10±2μm; and the surface of the porous plate in contact with the catalyst layer is roughened by acid treatment.
[0011] In some embodiments, the pressure control unit has an output pressure range of 0-30 tons of force and an output temperature range of room temperature to 200°C.
[0012] In some embodiments, the microchannels on the end plate are uniformly distributed for uniformly introducing organic solvents into the sealed chamber.
[0013] Secondly, this application provides a method for stripping the catalytic layer of a membrane electrode, employing any of the stripping devices described in the previous application, characterized by comprising the following steps: (a) Clamping pretreatment: Place the membrane electrode to be treated in the sealed chamber of the stripping chamber, so that its anode catalyst layer and cathode catalyst layer are in contact with the porous plates on both sides respectively; (b) Applying pressure: Applying axial pressure to the stripping chamber via the pressure control unit; (c) Solvent penetration wetting: The organic solvent (liquid or ultrasonically atomized gas) is introduced into the sealed chamber of the stripping chamber and maintained for a predetermined time; (d) Catalyst layer transfer: Utilizing the difference in swelling degree between the proton exchange membrane and the catalyst layer in the organic solvent, as well as the mechanical anchoring effect under pressure, the catalyst layer is peeled off from the proton exchange membrane and transferred to the porous plate; (e) Solvent Removal: The stripping chamber is heated by the heating module of the pressure control unit to evaporate and remove the organic solvent, thereby obtaining the anode catalyst layer, the cathode catalyst layer, and the independent proton exchange membrane loaded on the porous plate. In some embodiments, in step (b), the axial pressure is 1.2-6 MPa, so that the compression of the elastic sealing assembly reaches 20-35%; in step (c), the flow rate of the atomized organic solvent is 50-100 mL / min, and the holding time is 10-15 minutes; in step (e), the heating temperature is 40-70°C, and the holding time is 20-30 minutes.
[0014] Thirdly, this application provides a failure detection method for proton exchange membrane electrolysis water membrane electrodes, comprising: Using a membrane electrode catalytic layer stripping method, the anode catalytic layer, cathode catalytic layer, and proton exchange membrane were completely stripped from normal and failed membrane electrodes, respectively. The components of the normal membrane electrode and the failed membrane electrode are cross-combined and reassembled by hot pressing into multiple different test membrane electrode assemblies. The electrochemical performance of each of the test membrane electrode assemblies was tested separately; by comparing and analyzing the performance differences of each test membrane electrode assembly, the specific components and causes of failure that led to the performance degradation of the failed membrane electrode were determined.
[0015] In some embodiments, the cross combination specifically includes: The first reference membrane electrode assembly (MEA-0) was assembled using a normal anode catalyst layer, a normal proton exchange membrane, and a normal cathode catalyst layer. The second test membrane electrode assembly (MEA-1) was assembled using a failed anode catalyst layer, a normal proton exchange membrane, and a normal cathode catalyst layer. The third test membrane electrode assembly (MEA-2) was assembled using a normal anode catalyst layer, a failed proton exchange membrane, and a normal cathode catalyst layer. The fourth test membrane electrode assembly (MEA-3) was assembled using a normal anode catalyst layer, a normal proton exchange membrane, and a failed cathode catalyst layer.
[0016] Fourthly, this application provides a method for recovering the catalytic layer of a proton exchange membrane electrolysis water membrane electrode, comprising: By using a membrane electrode catalytic layer stripping method, the failed anode catalytic layer and the failed cathode catalytic layer loaded on a porous plate are completely stripped from the failed membrane electrode. The failed anode catalyst layer, the failed cathode catalyst layer, and a normal proton exchange membrane are recombined through a hot-pressing process to form a regenerable membrane electrode assembly that can function normally, thereby realizing the recycling and reuse of the catalyst layer.
[0017] The beneficial effects that the membrane electrode catalyst layer stripping device, method, failure detection method, and catalyst layer recovery method disclosed in this application may bring include, but are not limited to: Beneficial effects of the invention Compared with the prior art, the method and apparatus for disassembling and inspecting membrane electrodes provided by the present invention can achieve the following significant beneficial effects: 1. Achieved high integrity and controllable peeling of membrane electrode assemblies. This invention creates a novel "differential swelling peeling" method assisted by mechanical anchoring. This method utilizes a dedicated peeling device integrating solvent atomization supply, controllable pressure application, and heating drying units, and employs an optimized gradient pore size and rough-surface porous plate as the catalyst layer transfer carrier. The method can non-destructively or minimally destructively separate failed or untested membrane electrodes into structurally intact anode catalyst layer / PTL components, independent proton exchange membranes, and structurally intact cathode catalyst layer / PTL components, achieving a catalyst layer integrity peeling rate of ≥99%. This overcomes the technical bottleneck of existing methods such as immersion, which only result in fragmented detachment of the catalyst layer and fail to yield complete, independent components suitable for subsequent analysis.
[0018] 2. Provides a precise and systematic method for diagnosing membrane electrode failure sites. Based on the aforementioned high-integrity component separation, this invention proposes an innovative "component cross-combination testing method." By systematically cross-combining and comparing the performance of corresponding components (anode / cathode catalyst layers, proton exchange membrane) of normal and failed membrane electrodes, the overall performance degradation of the membrane electrode can be clearly attributed to one or more specific components. For example, through comparative testing, it is possible to clearly distinguish whether the performance degradation stems from proton exchange membrane perforation or a decrease in proton conductivity, or from the activity decay or poisoning of a particular catalyst layer. This method achieves a shift from vague judgments of overall performance failure to precise location of the root cause of component-level failure, providing a direct and reliable technical basis for product improvement and quality control.
[0019] 3. Achieved efficient and environmentally friendly direct recovery of precious metal catalysts. The stripping method provided by this invention can directly obtain a structurally intact degraded catalyst layer attached to a porous substrate. These catalyst layer components can be used directly as "semi-finished products" and assembled into a qualified regenerated membrane electrode by hot-pressing with a new proton exchange membrane. This process avoids the complex and highly polluting steps required in traditional wet recovery processes, such as strong acid dissolution, chemical separation, and resynthesis, greatly reducing the use of hazardous chemicals and the burden of wastewater treatment. It is a greener, more economical, and more efficient catalyst recovery strategy, and is particularly suitable for PEMWE membrane electrodes containing precious metals such as platinum and iridium.
[0020] 4. Improved the reliability, uniformity, and applicability of the disassembly and inspection process. The design of the device in this invention ensures reliable operation and repeatable results. The uniformly distributed microchannel design guarantees a uniform distribution of the atomized solvent on the membrane electrode contact surface, thereby achieving consistent overall peeling. The wide-range adjustable pressure and temperature control unit allows the device to adapt to the processing of membrane electrode samples of different sizes, models, or with special process requirements, enhancing the versatility and process adaptability of the method.
[0021] In summary, this invention integrates innovative device design, methodological processes, and application strategies, forming a closed-loop solution from complete disassembly to precise diagnosis and efficient recycling. It effectively overcomes the key defects in existing technologies and has significant practical value for promoting the commercial development and operation of PEM water electrolysis hydrogen production technology. Attached Figure Description
[0022] Figure 1 This is a schematic diagram of the separation device of the present invention.
[0023] Figure 2 This is a top view of the end plate.
[0024] Figure 3 This is a schematic diagram of a porous layer with gradient pore size.
[0025] Figure 4 The image shows a photograph of the component obtained using a self-made peeling device in Example 1.
[0026] Figure 5 This is a scanning electron microscope image of the catalyst layer in Example 1.
[0027] Figure 6 The graph shows the polarization curves of each membrane electrode in Example 2.
[0028] Figure 7 The image shows a photograph of the component obtained in Comparative Example 1.
[0029] Diagram description: 1-Organic reagent storage tank, 2-Pipeline, 3-Ultrasonic nebulizer, 4-Pressure control unit, 5-Stripping chamber, 51a-Microchannel, 51-End plate, 52-Elastic sealing assembly, 53-Porous plate, 6-Membrane electrode, 61-Proton exchange membrane, 62-Anode catalyst layer, 63-Cathode catalyst layer, 7-Waste liquid recovery unit. Detailed Implementation
[0030] Various exemplary embodiments, features, and aspects of this application will now be described in detail with reference to the accompanying drawings. The same reference numerals in the drawings denote elements that have the same or similar functions. Although various aspects of the embodiments are shown in the drawings, they are not necessarily drawn to scale unless specifically indicated otherwise.
[0031] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, an indirect connection through an intermediate medium, or the internal communication between two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.
[0032] like Figure 1-6 As shown, in a first aspect, the present invention provides a catalytic layer stripping device for a membrane electrode 6, comprising: a solvent supply unit, including an organic reagent storage tank 1, a pipeline 2, and an ultrasonic atomizer 3 connected in sequence, wherein the output end of the ultrasonic atomizer 3 is connected to an atomizing gas delivery pipeline 2; a pressure control unit 4, including a hydraulic actuation module and a heating module, wherein the output pressure and output temperature of the pressure control unit 4 are adjustable; a stripping chamber 5, including an end plate 51 with microchannels 51a, an elastic sealing assembly 52, and a porous plate 53, wherein the end plate 51 and the porous plate 53 are disposed opposite to each other and form a pressurizable sealed chamber through the elastic sealing assembly 52, wherein the inner surface of the end plate 51 and the inner wall of the microchannels 51a are coated with a polytetrafluoroethylene coating; and a waste liquid recovery unit 7, connected to the exhaust / liquid port of the stripping chamber 5 through the pipeline 2; wherein the porous plate 53 is used to support and contact the catalytic layer of the membrane electrode 6 to be stripped.
[0033] To address the technical problem that existing technologies cannot completely separate the catalyst layer and the proton exchange membrane without severely damaging the structure of the membrane electrode 6, this invention integrates functions such as solvent atomization permeation, controllable pressure application, and local heating drying.
[0034] The solvent supply unit is configured to include an ultrasonic atomizer 3 in order to atomize organic solvents (such as ethanol) into micron-sized droplets, thereby enabling them to penetrate into the interface between the catalyst layer and the proton exchange membrane in a more uniform and controllable manner, reducing solvent consumption and improving penetration efficiency.
[0035] The pressure control unit 4 is configured to include a hydraulic actuation and heating module to provide precise and controllable mechanical pressure during the stripping process to "anchor" the catalyst layer, and to provide controllable heat after stripping to quickly remove the solvent. The core of the stripping chamber 5 is configured with a microchannel 51a end plate 51 and a porous plate 53 with a polytetrafluoroethylene (PTFE) coating to create a sealed reaction environment. The PTFE coating effectively prevents organic solvents from corroding the metal components of the device and reduces accidental adhesion of the catalyst layer or film during the stripping process.
[0036] The porous plate 53 is used as the support and transfer substrate for the catalyst layer to provide support under pressure and to directly support it after the catalyst layer is peeled off. The waste liquid recovery unit 7 is provided for the environmentally friendly collection and treatment of residual solvents and any trace amounts of waste liquid that may be generated. The units are sequentially connected via pipelines 2 or mechanical structures and work together to achieve high-integrity peeling of the catalyst layer.
[0037] Solvent in organic reagent storage tank 1 is transported to ultrasonic nebulizer 3 via pipeline 2. After atomization, it is carried into stripping chamber 5 by atomizing gas (such as inert gas) through pipeline 2. In stripping chamber 5, membrane electrode 6 is clamped between two end plates 51, with its catalytic layers on both sides tightly attached to porous plates 53. The hydraulic actuator of pressure control unit 4 drives the end plates 51 to move, applying a set axial pressure to the sealed chamber (containing membrane electrode 6). The atomized solvent enters the chamber uniformly through microchannels 51a on the end plates 51, wetting the membrane electrode 6. Under the combined action of pressure and solvent swelling, the catalytic layer separates from the proton exchange membrane and transfers to the surface of the porous plate 53. Subsequently, the heating module is activated to heat the chamber to evaporate the solvent, and the dry catalytic layer (attached to the porous plate 53) and the independent proton exchange membrane are separated and removed. The gaseous / liquid waste generated during the process is introduced into waste liquid recovery unit 7 through exhaust / liquid port via pipeline 2.
[0038] It should be noted that the ultrasonic atomizer 3 can be replaced with other devices capable of producing a fine atomization, such as a pressure atomizing nozzle. Alternatively, this device can be omitted, and the solvent can be directly introduced to achieve the final goal. The PTFE coating can be replaced with other coating materials with excellent resistance to organic solvent corrosion and non-stick properties, such as a PFA (fusible polytetrafluoroethylene) coating. The hydraulic actuator module can provide pressure via electric, pneumatic, or other methods.
[0039] To optimize solvent distribution and peeling force transfer, and to ensure that the catalyst layer adheres firmly and uniformly to the porous plate 53 after peeling, in some embodiments, the porous plate 53 has a gradient pore size structure, with the pore size gradually decreasing from the side facing the end plate 51 to the side facing the catalyst layer.
[0040] The porous plate 53 is configured with a gradient pore size structure. The larger pore size facing the end plate 51 (solvent inflow side) is conducive to the rapid introduction and uniform distribution of the atomized solvent; the smaller pore size facing the catalyst layer side can provide a denser support surface, increase the contact area and anchoring force with the catalyst layer, prevent the catalyst layer from cracking or falling off during the peeling process, and facilitate the subsequent removal of the complete catalyst layer sheet from the porous plate 53.
[0041] Various materials, including but not limited to porous meshes or felts made of nickel, iron, copper, and titanium, can be used as porous plates 53. In order to better ensure the peeling effect and the integrity of the catalyst layer transfer, in some embodiments, the pore size of the porous plate 53 facing the end plate 51 is preferably about 100 μm, and the pore size facing the catalyst layer is preferably about 10 μm; and the surface of the porous plate 53 in contact with the catalyst layer is roughened by acid treatment. However, the pore size parameters of the porous plate are not limited to the above values. The structure of the porous plate used needs to meet two conditions at the same time: On the one hand, the porous plate 53 should have sufficient mechanical support strength so that the stress distribution transmitted to the reaction area of the membrane electrode 6 through the end plate 51a and the porous plate 53 is sufficiently uniform; on the other hand, the side of the porous plate 53 that contacts the catalyst layer should have a relatively dense porous structure so that sufficient mechanical meshing (anchoring) force and frictional force are formed between the surface of the porous plate 53 and the catalyst layer under pressure. When the solvent swelling causes the interfacial adhesion force to decrease, it can more reliably hold the catalyst layer, ensuring that it is completely peeled off from the proton exchange membrane and firmly attached, preventing the catalyst layer from slipping or falling off during the peeling process or subsequent operations.
[0042] Working process: The rough surface and the microscopic protrusions of the catalyst layer form a mechanical interlock, which enhances the bond between the two under pressure.
[0043] In addition to acid etching, surface roughening treatment can also be achieved by sandblasting, laser etching, or deposition of rough coatings.
[0044] To ensure that the device has sufficient process adaptability and flexibility to meet the processing needs of membrane electrodes 6 of different sizes, types or requiring special processes, in some embodiments, the pressure control unit 4 has an output pressure range of 0-30 tons of force and an output temperature range of room temperature to 200°C.
[0045] The pressure control unit 4 is set to this capability range. A wide pressure output range of 0-30 tons of force (approximately corresponding to a pressure of 0-30 MPa, depending on the indenter area) allows the device to handle not only standard small-sized laboratory membrane electrodes 6, but also larger product-grade membrane electrode 6 samples. A wide temperature range from room temperature to 200°C allows the device to be used not only for drying low-boiling-point solvents such as ethanol, but also to meet process requirements that may require higher temperatures for activation, sintering, or other post-processing.
[0046] To completely solve the problem that uneven solvent distribution may lead to incomplete or inconsistent local peeling of the membrane electrode 6, in some embodiments, the microchannels 51a on the end plate 51 are evenly distributed to uniformly introduce the atomized organic solvent into the sealed chamber.
[0047] The microchannels 51a on the end plate 51 are configured to be uniformly distributed (e.g., uniformly covering the entire working surface of the end plate 51 in a grid, concentric circle, or parallel groove pattern). This configuration ensures that the atomized solvent flow from the ultrasonic atomizer 3 can be uniformly distributed and delivered to the entire cross-section of the stripping chamber 5 through the microchannel network 51a, thereby ensuring that the catalyst layer-proton exchange membrane interface in each area in contact with the membrane electrode 6 receives nearly identical solvent wetting conditions. This is one of the key guarantees for achieving synchronous and complete stripping of the catalyst layer.
[0048] Working process: The atomized solvent gas enters the gas collection chamber behind the end plate 51, and is then forced through the uniformly distributed microchannels 51a to be sprayed into the sealed chamber in the form of multiple fine and uniform airflows.
[0049] In a second aspect, the present invention provides a method for stripping the catalyst layer of a membrane electrode 6 using the above-described apparatus, comprising the following steps: (a) clamping pretreatment; (b) applying pressure; (c) solvent penetration wetting; (d) catalyst layer transfer; and (e) solvent removal.
[0050] To provide a repeatable, controllable process for achieving high-integrity catalytic layer stripping, the method comprises the five core steps described above. Step (a) ensures accurate positioning of the membrane electrode 6 within the device and good contact between the catalytic layer and the porous plate 53. Step (b) applies controllable pressure, serving two key purposes: first, it ensures the sealing of the stripping chamber 5 through the compression of the elastic sealing component 52; second, it generates axial clamping force on the membrane electrode 6 assembly, which is transmitted to the catalytic layer through the porous plate 53, forming a preliminary "mechanical anchoring" before solvent penetration, thus providing a foundation for subsequent stripping. Step (c) introduces atomized solvent for controllable wetting, significantly reducing solvent usage compared to the immersion method and allowing the solvent to concentrate its effect in the interfacial region. Step (d) is based on the principle that the swelling behavior of the proton exchange membrane and the catalytic layer material (especially the ionomers within it) in response to organic solvents is significantly different. Building upon the established mechanical anchoring, the internal stress generated by the swelling difference promotes interfacial separation, thereby achieving complete transfer of the catalytic layer. Step (e) rapidly removes residual solvent by heating, resulting in dry, separate components that facilitate subsequent testing or processing.
[0051] Working principle: The core principle of this method is "differential swelling and exfoliation assisted by mechanical anchoring". The anchoring force provided by pressure prevents the catalyst layer from randomly wrinkling or breaking during the swelling process, guiding it towards the porous plate 53 for directional separation. The solvent selectively and preferentially swells the ionomer phase in the proton exchange membrane or catalyst layer, weakening the interfacial bonding force, and achieving clean separation under the guidance of the anchoring force.
[0052] To achieve optimal peel integrity and efficiency, a validated optimal operating window is provided by limiting the range of key process parameters. A more preferred technical solution is that, in step (b), the axial pressure is 1.2-6 MPa, causing the compression of the elastic sealing component 52 to reach 20-35%; in step (c), the flow rate of the atomized organic solvent is 50-100 mL / min, and the holding time is 10-15 minutes; in step (e), the heating temperature is 40-70°C, and the holding time is 20-30 minutes.
[0053] Setting the lower limit of axial pressure to 1.2 MPa ensures sufficient anchoring force and sealing; setting the upper limit to 6 MPa prevents excessive pressure from damaging the proton exchange membrane or catalyst layer, or from overloading the device. A sealing component compression of 20-35% ensures reliable sealing without permanent deformation. A solvent flow rate of 50-100 mL / min and a wetting time of 10-15 minutes ensure sufficient and uniform wetting of the interface without excessive swelling or solvent consumption. A heating temperature of 40-70℃ and a time of 20-30 minutes effectively evaporates common solvents such as ethanol with reasonable energy consumption, avoiding damage to the membrane or catalyst layer materials from excessive temperature.
[0054] Of course, the specific pressure, flow rate, temperature, and time parameters can be adjusted adaptively according to the specific type of solvent used, the model and size of the membrane electrode 6.
[0055] Thirdly, the present invention provides a failure detection method based on stripped components. This includes: using a catalytic layer stripping method for membrane electrode 6, completely stripping and obtaining the anode catalytic layer 62, cathode catalytic layer 63, and proton exchange membrane from both a normal membrane electrode 6 and a failed membrane electrode 6, respectively; The normal membrane electrode 6 and the various components of the failed membrane electrode 6 are cross-combined and reassembled by hot pressing into multiple different test membrane electrode 6 assemblies. The electrochemical performance of each of the test membrane electrode 6 components was tested separately; By comparing and analyzing the performance differences of each of the test membrane electrode 6 components, the specific components and causes of failure that led to the performance degradation of the failed membrane electrode 6 can be identified.
[0056] To address the challenge of accurately locating specific failed components within the membrane electrode 6 using existing technologies, this invention creatively proposes a "component cross-combination testing method." This method first utilizes the aforementioned high-integrity stripping technique to obtain the "dissected" components (anode / cathode catalyst layers 63 and proton exchange membrane) of both normal and failed membrane electrodes 6. By systematically cross-recombining these components like "puzzle pieces" and testing their performance, the overall performance degradation can be attributed to one or more specific components. For example, if the assembly containing only the failed proton exchange membrane exhibits significantly reduced performance, while the assembly containing only the failed catalyst layer performs normally, then the cause of failure can be clearly determined to be proton exchange membrane degradation. This method represents a leap from "overall failure judgment" to "component-level failure diagnosis."
[0057] Working process: After cleaning and drying the stripped components, the different anodic / cathode catalyst layers 63 (attached to their porous plates 53 or transferred to a new substrate) are recombined with the proton exchange membrane using a standard membrane electrode 6 hot-pressing process to fabricate multiple single cells for testing. Electrochemical performance tests (such as polarization curves and impedance spectra) are performed under the same test conditions (temperature, pressure, flow rate), and the performance data are compared and analyzed.
[0058] Preferably, the cross combination specifically includes: The first reference membrane electrode assembly (MEA-0) is assembled using a normal anode catalyst layer 62, a normal proton exchange membrane, and a normal cathode catalyst layer 63. The second test membrane electrode assembly (MEA-1) was assembled using the failed anode catalyst layer 62, the normal proton exchange membrane and the normal cathode catalyst layer 63. The third test membrane electrode assembly (MEA-2) is assembled using a normal anode catalyst layer 62, a failed proton exchange membrane, and a normal cathode catalyst layer 63. The fourth test membrane electrode assembly (MEA-3) is assembled using a normal anode catalyst layer 62, a normal proton exchange membrane, and a failed cathode catalyst layer 63.
[0059] To provide a standardized and highly systematic failure attribution analysis scheme, the cross-combinations are specified into these four most representative combinations. MEA-0 serves as the baseline where all components are functioning correctly. MEA-1, MEA-2, and MEA-3 individually replace the failed anode catalyst layer 62, the failed proton exchange membrane, and the failed cathode catalyst layer 63, respectively. By comparing the performance differences between MEA-1 / 2 / 3 and MEA-0, it is possible to clearly and directly determine whether the failure of the original membrane electrode 6 was caused by the anode catalyst layer 62, the proton exchange membrane, or the cathode catalyst layer 63. This setup covers all possibilities of single-component failure, has the fewest combinations, and offers the highest analytical efficiency.
[0060] Fourthly, the present invention provides a method for recovering a catalyst layer, comprising: using a catalyst layer stripping method for a membrane electrode 6 to completely strip and obtain a failed anode catalyst layer 62 and a failed cathode catalyst layer 63 loaded on a porous plate 53; The failed anode catalyst layer 62 and the failed cathode catalyst layer 63 are recombined with a normal proton exchange membrane through a hot pressing process to form a regenerated membrane electrode 6 assembly that can work normally, thereby realizing the recycling and reuse of the catalyst layer.
[0061] To achieve efficient and environmentally friendly recovery of noble metal catalysts (such as iridium and platinum) in the failed membrane electrode 6, this invention utilizes the aforementioned stripping method to directly obtain structurally intact failed catalyst layers attached to the porous plate 53. These catalyst layers can be directly used as "components". The method is configured to include hot-pressing the failed anode / cathode catalyst layers 63 with a new, normal proton exchange membrane to verify whether the recovered catalyst layers still possess electrochemical activity and can be directly assembled into a working membrane electrode 6. This achieves direct recycling "from failed components to functional components," avoiding complex wet recycling processes such as chemical dissolution and refining, significantly reducing the use of chemicals such as strong acids and strong oxidants, making it more environmentally friendly, economical, and efficient.
[0062] Working process: The porous plate 53 with the degraded catalyst layer obtained by stripping (which can be used as a gas diffusion layer PTL) is aligned with the new proton exchange membrane and composited using a standard hot pressing process to obtain the regenerated membrane electrode assembly 6 (MEA).
[0063] The present application will now be described in detail with reference to several embodiments: Example A: This embodiment details the specific structure and operation of the membrane electrode 6 catalyst layer stripping device according to claim 1.
[0064] Device composition: Solvent supply unit: includes a 5L ethanol storage tank, which is connected to an ultrasonic nebulizer 3 with a frequency of 1.7MHz via a polytetrafluoroethylene (PTFE) pipe 2. The outlet of the ultrasonic nebulizer 3 is connected to a high-purity nitrogen cylinder via a stainless steel pipe 2, forming an atomized gas delivery pipe 2 for carrying atomized ethanol.
[0065] Pressure control unit 4: It adopts a servo electro-hydraulic system as the hydraulic actuation module, with a maximum output pressure of 30 tons of force (approximately 30 MPa). The heating module is a ring heater embedded in the end plate 51 of the stripping chamber 5. With the help of a PID temperature controller, it can achieve precise temperature control from room temperature to 200°C.
[0066] The stripping chamber 5 consists of two circular end plates 51, each 150mm in diameter. The upper end plate 51 has a network of radial and concentric ring-shaped microchannels 51a (e.g., ...). Figure 2 (As shown). The working surface of the end plate 51 and the inner walls of all microchannels 51a are coated with a polytetrafluoroethylene coating of approximately 20 μm thickness by a spray sintering process. The stripping chamber 5 uses fluororubber O-rings as elastic sealing components 52. The lower end plate 51 is fixed in position, and the upper end plate 51 is connected to the piston rod of the pressure control unit 4. Two perforated plates 53 are placed inside the upper and lower end plates 51 respectively, forming a sealable cylindrical chamber together with the end plates 51.
[0067] Waste liquid recovery unit 7: is a glass solvent recovery bottle with condensation function, which is connected to the exhaust / liquid port on the top of the stripping chamber 5 through pipeline 2.
[0068] Operating Procedure: A 120mm diameter failed membrane electrode 6 is placed on the lower porous plate 53, aligned, and the stripping chamber 5 is closed. The pressure control unit 4 is activated to apply axial pressure, compressing and sealing the sealing ring. Nitrogen gas and the ultrasonic nebulizer 3 are turned on, and atomized ethanol (flow rate 80mL / min) is uniformly introduced into the chamber through the microchannel network 51a of the upper end plate 51, and maintained for 12 minutes. Subsequently, the heating module is activated to raise the chamber temperature to 50°C and maintain it for 25 minutes to evaporate the ethanol. Finally, the pressure is released and the chamber is opened, allowing the upper and lower porous plates 53 with intact catalyst layers and the individual proton exchange membranes to be removed separately. This embodiment demonstrates that the integrated device can achieve high-integrity stripping of the catalyst layer.
[0069] Example B This embodiment focuses on describing the specific structure of the porous plate 53, its preparation method, and its role in the peeling process.
[0070] Preparation of porous plate 53: A porous titanium plate with gradient pore size was prepared by powder metallurgy sintering. Titanium powders of different particle sizes were selected: titanium powder with a particle size range of 90-110 μm was used for the bottom layer (facing the end plate 51); titanium powder with a progressively decreasing particle size was used for the intermediate transition layer; and fine titanium powder with a particle size range of 8-12 μm was used for the top layer (facing the catalyst layer). Titanium powders of different particle sizes were laid in a mold according to the designed gradient and sintered in a vacuum sintering furnace at 1200℃ to obtain a gradient porous plate 53 with a thickness of 2 mm and a pore size that gradually changes from about 100 μm at the bottom layer to about 10 μm at the top layer.
[0071] Surface treatment: The top layer (catalytic layer contact surface) of the sintered porous plate 53 was immersed in a 20wt% hydrochloric acid solution and etched at 60°C for 30 minutes. After removal, it was rinsed with deionized water and dried. After this acid treatment, a micron-scale rough structure was formed on the surface of the top layer of the porous plate 53, and its surface roughness Ra value increased from about 0.8 μm before treatment to about 3.5 μm.
[0072] Application and Effects: The prepared porous plate 53 was applied to the apparatus of Example A. During the peeling process, atomized ethanol rapidly entered from the large-pore bottom layer and diffused uniformly. Under pressure, the small-pore top layer with a rough surface generated a strong mechanical engagement with the catalyst layer. Compared with the use of a porous plate 53 with uniform pore size (50 μm) and no acid treatment, the porous plate 53 of this example increased the complete peeling rate of the catalyst layer from about 85% to ≥99%, and the adhesion of the peeled catalyst layer on the porous plate 53 was significantly improved, with no detachment during subsequent handling operations.
[0073] Example C This embodiment describes in detail the operation steps and parameters of the stripping method.
[0074] Step (a) Clamping Pre-treatment: Carefully place a failed membrane electrode 6 (MEA, 80 mm in diameter) taken from a PEM electrolyzer that has been running for more than 5000 hours onto the lower porous plate 53 of the stripping chamber 5. Adjust its position so that its anode catalyst layer 62 faces upward and its cathode catalyst layer 63 faces downward, aligning it with the upper and lower porous plates 53 respectively.
[0075] Step (b) Applying pressure: Activate pressure control unit 4 and slowly apply axial pressure up to 2.5 MPa at a rate of 0.1 MPa / s. At this point, the fluororubber sealing ring is compressed by approximately 25%, and the membrane electrode assembly 6 is firmly pressed. The calculated pressure on the catalyst layer surface is approximately 1.8 MPa.
[0076] Step (c) Solvent penetration wetting: Maintain a pressure of 2.5 MPa, turn on nitrogen (flow rate 2 L / min) and ultrasonic nebulizer 3. Atomized anhydrous ethanol is continuously introduced into the sealed chamber of the stripping chamber 5 through the microchannel 51a of the upper end plate 51 at a flow rate of 60 mL / min, and the wetting time is 12 minutes.
[0077] Step (d) Catalyst Layer Transfer: Under the combined action of pressure and atomized ethanol, the proton exchange membrane (PEM) swells. Since the swelling ratio of the PEM is much higher than that of the ionomers in the catalyst layer, the interfacial bonding is weakened. Simultaneously, the catalyst layer is pre-pressed and anchored onto the rough surface of the porous plate 53. After approximately 8 minutes, signs of separation between the PEM and the catalyst layer can be observed at the edges. After wetting, the catalyst layer has been completely peeled off from the PEM and firmly adhered to both sides of the porous plate 53.
[0078] Step (e) Solvent Removal: The solvent supply is shut off. The temperature of the stripping chamber 5 is raised to 60°C at a rate of 5°C / min using the heating module of the pressure control unit 4, and maintained at this temperature for 22 minutes. During this process, residual ethanol is completely evaporated.
[0079] Results: After depressurization and opening the chamber, three parts were successfully obtained: ① a complete anodic catalyst layer 62 loaded on the upper porous plate 53 (forming the "anodic catalyst layer 62 / PTL" assembly together with the porous plate 53); ② an independent, morphologically intact degraded proton exchange membrane; ③ a complete cathode catalyst layer 63 loaded on the lower porous plate 53 ("cathode catalyst layer 63 / PTL" assembly). The entire process used minimal solvent and resulted in the complete removal of the components.
[0080] Example D This embodiment details the implementation process and data analysis of the failure detection method.
[0081] Component Acquisition: Using the method of Example C, “normal anode catalyst layer 62 / PTL(NA)”, “normal proton exchange membrane (N-PEM)”, and “normal cathode catalyst layer 63 / PTL(NC)” were obtained by peeling off a brand new membrane electrode 6 (of the same type) with known good performance.
[0082] Using the same method, the failed membrane electrode 6 (performance degradation ≥30%) was peeled off to obtain "failed anode catalyst layer 62 / PTL(FA)", "failed proton exchange membrane (F-PEM)", and "failed cathode catalyst layer 63 / PTL(FC)". All PTL substrates were kept consistent.
[0083] Cross-assembly and assembly: Using a standard hot-pressing process (conditions: 130℃, 1MPa, 3 minutes), the above components are assembled into four types of membrane electrode assemblies (MEAs) of 6 modules: MEA-0 (Benchmark): N-A+N-PEM+NC MEA-1 (Anode Measurement): F-A+N-PEM+NC MEA-2 (measures PEM): N-A+F-PEM+NC MEA-3 (Cathode Measurement): N-A+N-PEM+FC Performance Testing: All MEAs were installed in the same standard electrolytic cell test fixture. Under identical test conditions (temperature: 60℃, pressure: atmospheric pressure, deionized water flow rate: 100 mL / min each for anode and cathode), the polarization curves (voltage-current density curves) of each MEA were measured using an electrochemical workstation. The results are shown in [reference needed]. Figure 6 .
[0084] Failure Analysis: MEA-0 exhibits a normal polarization curve.
[0085] The polarization curves of MEA-1 and MEA-3 largely overlap with those of MEA-0 in most current density ranges, especially in the low current density region (<0.3 A / cm²) characterizing catalytic activity and the medium-to-high current density region characterizing mass transfer. This indicates that the intrinsic electrochemical activity of the anodic and cathode catalytic layers 63 of the failed membrane electrode 6 has not decreased significantly.
[0086] The polarization curve of MEA-2 shows a significant voltage surge (step) after the current density exceeds 0.8 A / cm², indicating that its internal resistance increases sharply or mass transfer is hindered.
[0087] Conclusion: Through cross-combination testing, it was clearly determined that the performance degradation of the failed membrane electrode 6 was mainly due to the failure of its proton exchange membrane (F-PEM) (possibly due to a decrease in local proton conductivity or slight perforation leading to gas permeation). The cathode and anolyte catalyst layers 62 were not the primary failure components. This method accurately pinpointed the root cause of the failure.
[0088] Example E This embodiment specifically demonstrates the method for direct recycling and reuse of the catalyst layer as described in claim 8.
[0089] The recovered components were the "failed anode catalyst layer 62 / PTL(FA)" and the "failed cathode catalyst layer 63 / PTL(FC)" which were identified as "non-major failure components" in Example D. Although these catalyst layers originated from the failed MEA, their intrinsic activity was still present according to the tests conducted in Example D.
[0090] Recovery steps: Align and stack the above two components, FA and FC (i.e., the porous plate 53 with the catalyst layer) with a brand new proton exchange membrane (New-PEM) of the same type (in the order: FA, New-PEM, FC).
[0091] Recombination and regeneration: Using the same standard hot pressing process as in Example D (130°C, 1MPa, 3 minutes), the three components are hot-pressed together to form a new membrane electrode assembly 6, denoted as MEA-R (regenerated assembly).
[0092] Performance verification: The MEA-R was subjected to polarization curve testing under the exact same test conditions as in Example D.
[0093] Results: The polarization curve of MEA-R basically coincides with that of MEA-0, which is composed of completely new components, and its performance has recovered to the normal level (the voltage difference is less than 20mV at a current density of 1A / cm²).
[0094] Conclusion: This embodiment successfully achieved the direct, dry-state physical recovery and reuse of the noble metal catalyst layer in the failed membrane electrode 6. This method avoids complex chemical dissolution, separation, and resynthesis steps, eliminates the need for large amounts of strong acids, oxidants, and other reagents, and is environmentally friendly and efficient. Furthermore, the recovered catalyst layer can be directly used to assemble a new MEA with satisfactory performance, demonstrating its economic value and practicality.
[0095] Example F This embodiment aims to verify the wide range adaptability of the device and the effectiveness of the uniform microchannel 51a design.
[0096] Wide parameter range verification: High-pressure testing: To simulate the handling of large membrane electrode 6 samples or those requiring stronger anchoring force, a hydraulic module with a maximum output of 50 tons of force was used. When handling a large membrane electrode 6 sample (200mm x 200mm), the axial pressure was set to 25 tons of force (approximately corresponding to a chamber pressure of 8.3MPa), and the sealing ring was compressed by about 32%. Under this high pressure, combined with solvent permeation, the complete stripping of the catalyst layer was still successfully achieved, demonstrating the reliability of the device near the pressure limit.
[0097] High-temperature test: To verify the wide temperature range capability of the heating module, the temperature of the peeling chamber 5 was set to 180℃ and maintained for 30 minutes during the post-peeling treatment of a special polymer film (requiring high-temperature drying). The temperature control system of the device operated stably, and the temperature uniformity inside the chamber was within ±3℃, successfully removing the high-boiling-point solvent residue, proving its high-temperature processing capability.
[0098] Uniform microchannel 51a design verification: Design: The microchannel 51a of the end plate 51 adopts the following design: Figure 2 The grid design of "radial main channel + dense concentric ring secondary channel" shown ensures that any point on the working surface of the end plate 51 is no more than 2mm away from the nearest air outlet microhole.
[0099] Performance Verification: Computational Fluid Dynamics (CFD) software was used to simulate the flow of atomized ethanol gas within the chamber. Simulation results show that with the uniform distribution of microchannels 51a, a uniform velocity and concentration field can be rapidly formed after the gas enters the chamber. A comparative experiment was conducted with an end plate 51 design featuring only a simple central inlet: Under the same process conditions, using the uniform microchannels 51a end plate 51 of this invention, the difference in residual ionomer thickness in different regions of the catalyst layer after peeling is <10%; while using the simple central inlet end plate 51, the peeling integrity of the catalyst layer in the edge regions is significantly worse than in the central region, with a residual ionomer thickness difference >50%. This directly proves that the uniformly distributed microchannels 51a are crucial for achieving uniform peeling of the membrane electrode 6.
[0100] Comparative Example 1 This comparative example uses a simple immersion method commonly used in the prior art to treat the same failed membrane electrode 6, in order to highlight the effectiveness of the device and method of the present invention.
[0101] Operating steps: Take a failed membrane electrode 6 from the same source and of the same model as in Example C.
[0102] The entire membrane electrode 6 was directly and completely immersed in a glass container containing a 50% ethanol aqueous solution and left to soak at room temperature for 30 minutes.
[0103] After soaking, carefully remove the membrane electrode 6 assembly with tweezers and lay it flat on a lint-free paper.
[0104] The membrane electrode assembly 6, along with the lint-free paper, was placed in a 60°C oven and dried for 30 minutes to remove the solvent.
[0105] Results and phenomena: Observe after drying (e.g.) Figure 7 As shown in the figure, the structure of the membrane electrode 6 assembly was severely damaged, and no complete separation of any component could be achieved.
[0106] Non-uniform and uncontrollable localized detachment occurs between the proton exchange membrane and the catalyst layer. The catalyst layer adheres irregularly to the proton exchange membrane in the form of fragments, flocculent material, or flakes, or falls off onto the lint-free paper, making it impossible to obtain a complete and independent "anodic catalyst layer 62 / PTL", "cathode catalyst layer 63 / PTL", or a clean "proton exchange membrane".
[0107] When attempting to separate the catalyst layer by hand or with tools, a large amount of adhesive bands remain between the residual catalyst layer and the membrane, and forced separation will lead to further breakage.
[0108] Analysis and Comparison Conclusions: Peeling integrity: Compared with the ≥99% complete peeling rate achieved in embodiments A and C of the present invention, the immersion method is basically unable to achieve complete peeling, thus damaging the structural integrity of the component.
[0109] Failure analysis feasibility: Compared with Embodiment D of the present invention, which can accurately locate the failed component through cross-combination, the broken component generated by the immersion method cannot be used for subsequent systematic reconstruction and performance comparison testing, and therefore cannot achieve accurate diagnosis of the root cause of failure.
[0110] Catalyst recovery value: Compared with Embodiment E of the present invention, which can directly recover and regenerate the complete catalyst layer component, the broken catalyst layer obtained by the immersion method is extremely difficult to recover, has high purification costs, and is difficult to reuse directly.
[0111] Environmental friendliness and controllability: Immersion methods use large amounts of liquid solvents, which are troublesome in subsequent processing; moreover, the process is completely uncontrollable, relying on the natural penetration of the solvent, resulting in poor repeatability. In contrast, this invention uses atomization technology, which uses very little solvent, and the process is precisely controlled by parameters such as pressure, temperature, and flow rate.
[0112] In summary, by directly comparing the various embodiments (AE) of the present invention with Comparative Example 1, it is fully demonstrated that: The stripping device (Example A, Example F) and stripping method (Example C) provided by the present invention can solve the technical problem that traditional methods cannot completely separate the components of the membrane electrode 6.
[0113] The failure detection method based on completely stripped components (Example D) can achieve precise location of component-level failures that is impossible with traditional methods.
[0114] The catalyst layer recovery method based on the complete stripped components (Example E) provides an efficient, environmentally friendly, and directly reusable recycling pathway, which is superior to traditional destructive recycling processes.
[0115] The device design of the present invention (such as a wide parameter range, uniform microchannel 51a, etc., Example F) provides a reliable and flexible hardware guarantee for the above-mentioned effects.
[0116] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
[0117] The various embodiments of this application have been described above. These descriptions are exemplary and not exhaustive, nor are they limited to the disclosed embodiments. Many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments.
Claims
1. A membrane electrode catalytic layer stripping device, characterized in that, include: The solvent supply unit includes an organic reagent storage tank and pipelines connected in sequence; The pressure control unit includes a hydraulic actuation module and a heating module, and the output pressure and output temperature of the pressure control unit are adjustable; The stripping chamber includes an end plate with microchannels, an elastic sealing assembly, and a porous plate. The end plate and the porous plate are arranged opposite to each other and form a pressurizable sealed chamber through the elastic sealing assembly. The inner surface of the end plate and the inner wall of the microchannels are coated with polytetrafluoroethylene. The waste liquid recovery unit is connected to the exhaust / liquid port of the stripping chamber via a pipeline; The porous plate is used to support and contact the catalytic layer of the membrane electrode to be stripped.
2. The membrane electrode catalytic layer stripping device according to claim 1, characterized in that, The porous plate has a gradient pore size structure, with the pore size gradually decreasing from the side facing the end plate to the side facing the catalyst layer.
3. The membrane electrode catalytic layer stripping device according to claim 2, characterized in that, The porous plate has a pore size of 100±10μm on the side facing the end plate and a pore size of 10±2μm on the side facing the catalyst layer; and the surface of the porous plate in contact with the catalyst layer is roughened by acid treatment.
4. The membrane electrode catalytic layer stripping device according to claim 1, characterized in that, The pressure control unit has an output pressure range of 0-30 tons of force and an output temperature range of room temperature to 200°C.
5. The membrane electrode catalytic layer stripping device according to claim 1, characterized in that, The microchannels on the end plate are evenly distributed to uniformly introduce the atomized organic solvent into the sealed chamber.
6. A method for stripping the catalytic layer of a membrane electrode, using the stripping device as described in any one of claims 1 to 5, characterized in that, Includes the following steps: (a) Clamping pretreatment: Place the membrane electrode to be treated in the sealed chamber of the stripping chamber, so that its anode catalyst layer and cathode catalyst layer are in contact with the porous plates on both sides respectively; (b) Applying pressure: Applying axial pressure to the stripping chamber via the pressure control unit; (c) Solvent penetration wetting: The organic solvent is introduced into the sealed chamber of the stripping chamber and maintained for a predetermined time. (d) Catalyst layer transfer: Utilizing the difference in swelling degree between the proton exchange membrane and the catalyst layer in the organic solvent, as well as the mechanical anchoring effect under pressure, the catalyst layer is peeled off from the proton exchange membrane and transferred to the porous plate; (e) Solvent removal: The stripping chamber is heated by the heating module of the pressure control unit to evaporate and remove the organic solvent, thereby obtaining the anode catalyst layer, the cathode catalyst layer and the independent proton exchange membrane loaded on the porous plate.
7. The method for stripping the catalytic layer of a membrane electrode according to claim 6, characterized in that, In step (b), the axial pressure is 1.2-6 MPa, so that the compression of the elastic sealing component reaches 20-35%; in step (c), the flow rate of the atomized organic solvent is 50-100 mL / min, and the holding time is 10-15 minutes; in step (e), the heating temperature is 40-70℃, and the holding time is 20-30 minutes.
8. A method for detecting the failure of a proton exchange membrane electrolysis water membrane electrode, characterized in that, include: Using the method described in claim 6 or 7, the anode catalyst layer, cathode catalyst layer, and proton exchange membrane are completely stripped from the normal membrane electrode and the failed membrane electrode, respectively. The components of the normal membrane electrode and the failed membrane electrode are cross-combined and reassembled by hot pressing into multiple different test membrane electrode assemblies. The electrochemical performance of each of the test membrane electrode assemblies was tested separately; by comparing and analyzing the performance differences of each test membrane electrode assembly, the specific components and causes of failure that led to the performance degradation of the failed membrane electrode were determined.
9. The failure detection method according to claim 8, characterized in that, The cross-combination specifically includes: The first reference membrane electrode assembly (MEA-0) was assembled using a normal anode catalyst layer, a normal proton exchange membrane, and a normal cathode catalyst layer. The second test membrane electrode assembly (MEA-1) was assembled using a failed anode catalyst layer, a normal proton exchange membrane, and a normal cathode catalyst layer. The third test membrane electrode assembly (MEA-2) was assembled using a normal anode catalyst layer, a failed proton exchange membrane, and a normal cathode catalyst layer. The fourth test membrane electrode assembly (MEA-3) was assembled using a normal anode catalyst layer, a normal proton exchange membrane, and a failed cathode catalyst layer.
10. A method for recovering the catalytic layer of a proton exchange membrane electrolysis water electrode, characterized in that, include: Using the method as described in claim 6 or 7, the failed anode catalyst layer and the failed cathode catalyst layer loaded on the porous plate are completely peeled off from the failed membrane electrode. The failed anode catalyst layer, the failed cathode catalyst layer, and a normal proton exchange membrane are recombined through a hot-pressing process to form a regenerable membrane electrode assembly that can function normally, thereby realizing the recycling and reuse of the catalyst layer.