Alloy catalyst post-processing system and post-processing method

Abstract

The invention discloses an alloy catalyst post-processing system and a post-processing method, and particularly relates to the technical field of fuel cells. The drying chamber is in airtight sealing connection with the airtight reaction chamber, the heat treatment chamber is in airtight sealing connection with the airtight reaction chamber, and the screening device is arranged in the airtight reaction chamber and used for screening and weighing an alloy catalyst; the passivation sealing bin is arranged in the airtight reaction chamber and is used for passivating the alloy catalyst; the atmosphere control device comprises a vacuum pump communicated with the drying chamber, and atmosphere inflation equipment and a tail gas treatment device which are respectively communicated with the airtight reaction chamber, the drying chamber, the heat treatment chamber and the passivation sealing bin; and the heating device is used for independently heating the airtight reaction chamber, the drying chamber and the heat treatment bin. Uniform passivation of the alloy catalyst can be realized, the stability and safety of the alloy catalyst are ensured, the operation is simple and convenient, the treatment efficiency is improved, and the process controllability is ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of fuel cells, and in particular to an alloy catalyst post-processing system and a post-processing method. Background Art

[0002] Proton exchange membrane fuel cells (PEMFCs) are capable of producing electricity directly from chemicals with high efficiency, noiseless operation, and no pollutant emissions compared to traditional internal combustion engines. In proton exchange membrane fuel cells, the oxygen reduction reaction (ORR) is a key process. However, the reaction kinetics of the oxygen reduction reaction (ORR) are relatively slow, so efficient catalysts are needed to accelerate the reaction and thus improve the performance of the cell. Commonly used catalysts are platinum-based catalysts, but platinum is expensive and scarce. At present, great progress has been made in reducing the amount of platinum by alloying with transition metals such as Fe, Co, Ni, Cu and Mn. These Pt-M alloy catalysts can increase the mass activity (MA) to a higher level compared to pure Pt catalysts.

[0003] However, alloy catalysts usually need to be treated in a high-temperature atmosphere after synthesis to optimize their structure and catalytic activity. Traditional post-treatment methods often require multi-step atmosphere adjustment, but during the transfer and treatment of each step, the catalyst is easily exposed to air, causing oxidation or sintering of the catalyst surface, thereby affecting the catalytic performance. Summary of the invention

[0004] The purpose of the present invention is to provide an alloy catalyst post-treatment system and a post-treatment method to solve the problems existing in the above-mentioned prior art, to achieve uniform passivation of the alloy catalyst, to ensure the stability and safety of the alloy catalyst, to simplify the operation, to improve the treatment efficiency, and to ensure the controllability of the process.

[0005] To achieve the above object, the present invention provides the following solutions: The present invention provides an alloy catalyst post-treatment system, comprising: an airtight reaction chamber; a drying chamber, which is airtightly connected to the airtight reaction chamber through a first chamber door, and the drying chamber is used to dry the alloy catalyst; a heat treatment chamber, which is airtightly connected to the airtight reaction chamber through a second chamber door, and the heat treatment chamber is used to heat treat the alloy catalyst after drying; a screening device, which is placed in the airtight reaction chamber, and the screening device is used to screen and weigh the alloy catalyst after heat treatment; a passivation sealed chamber, which is placed in the airtight reaction chamber, and the passivation sealed chamber is used to passivate the alloy catalyst after screening and weighing; an atmosphere control device, including a vacuum pump, Atmosphere inflation equipment, exhaust gas treatment device and atmosphere control module, the atmosphere control module is signal-connected with the vacuum pump and the atmosphere inflation equipment, the vacuum pump is connected with the drying chamber through a pipeline, the atmosphere inflation equipment is respectively connected with the airtight reaction chamber, the drying chamber, the heat treatment chamber and the passivation sealing chamber through pipelines, the exhaust gas treatment device is respectively connected with the airtight reaction chamber, the heat treatment chamber and the passivation sealing chamber through pipelines; a heating device, the airtight reaction chamber, the drying chamber and the heat treatment chamber of the heat treatment chamber are all connected with the heating device, and the heating device is used to independently heat the airtight reaction chamber, the drying chamber and the heat treatment chamber.

[0006] Preferably, the airtight reaction chamber includes a main chamber and a discharge transition chamber, one side of the main chamber is airtightly connected to the drying chamber through the first chamber door, the other side of the main chamber is airtightly connected to the discharge transition chamber through a third chamber door, the bottom surface of the main chamber is airtightly connected to the airtight reaction chamber through the second chamber door, the screening device and the passivation sealing chamber are both located in the main chamber, and the heating device is used to heat the main chamber.

[0007] Preferably, the drying chamber has a vacuum interface and a drying chamber air inlet, the vacuum pump is connected to the vacuum interface and is used to evacuate the drying chamber, the atmosphere charging device is connected to the drying chamber air inlet and is used to charge inert gas into the drying chamber, and a tray for holding the alloy catalyst is provided in the drying chamber.

[0008] Preferably, the heat treatment chamber is provided with the heat treatment chamber and a lifting device, the lifting device is connected to the heat treatment chamber, and is used to lift the heat treatment chamber from the heat treatment chamber to the airtight reaction chamber, or to drop the heat treatment chamber from the airtight reaction chamber to the heat treatment chamber, the heat treatment chamber has a heat treatment chamber door, a heat treatment air inlet and a heat treatment air outlet, the atmosphere charging equipment is connected to the heat treatment air inlet, and is used to charge the heat treatment chamber with reaction gas for post-treatment of the catalyst, the reaction gas is a N2 / H2 mixed gas or an Ar / H2 mixed gas, and the exhaust gas treatment device is connected to the heat treatment air outlet.

[0009] Preferably, the screening device includes a screening box and a weighing base, the screening box is arranged on the weighing base, the screening box includes a screening box body, a primary screen, a secondary screen, a primary vibrator and a secondary vibrator, the first-level screen and the secondary screen are arranged in sequence from top to bottom inside the screening box body, the first-level screen is connected to the first-level vibrator, the second-level screen is connected to the second-level vibrator, a feed port is arranged at the top of the screening box body, a discharge port is arranged at the bottom of the screening box body, and the weighing base is used to weigh the alloy catalyst falling from the discharge port.

[0010] Preferably, the passivation sealed chamber has a passivation chamber inlet, a passivation chamber outlet, a passivation air inlet and a passivation air outlet, the atmosphere charging device is connected to the passivation air inlet for charging oxygen into the passivation sealed chamber, the exhaust gas treatment device is connected to the passivation air outlet, the passivation chamber inlet is located at the top of the passivation sealed chamber, and an inlet baffle door for opening or closing the passivation chamber inlet is provided at the passivation chamber inlet, the passivation chamber outlet is located at the bottom of the passivation sealed chamber, and an outlet baffle door for opening or closing the passivation chamber outlet is provided at the passivation chamber outlet; a stirring device is provided in the passivation sealed chamber, the stirring device includes a driving element, a stirring shaft and a plurality of stirring blades, the driving element can be detachably mounted on the bottom plate of the passivation sealed chamber, the output shaft of the driving element is fixedly connected to the stirring shaft, the plurality of stirring blades are connected to the stirring shaft and arranged along the axial direction of the stirring shaft, the driving element drives the stirring shaft to rotate, and causes the stirring blades to stir the alloy catalyst in the passivation sealed chamber.

[0011] Preferably, the atmosphere inflation equipment includes a quantitative oxygen generator, which is located in the airtight reaction chamber. The quantitative oxygen generator includes a reaction chamber, a catalyst storage chamber and an oxygen storage chamber. The reaction chamber is filled with a quantitative amount of hydrogen peroxide. The catalyst storage chamber is communicated with the reaction chamber. The reaction chamber and the oxygen storage chamber are sealed and connected through an oxygen delivery pipe. The oxygen generation speed and amount are controlled by adjusting the amount of catalyst entering the reaction chamber and the temperature in the reaction chamber. The oxygen storage chamber is connected and communicated with the passivation sealed chamber.

[0012] Preferably, the atmosphere aeration equipment comprises a micro water electrolysis device, which is located in the airtight reaction chamber. The hydrogen prepared by the micro water electrolysis device is quantitatively controlled by a flow meter and is mixed with N2 or an inert gas delivered by the atmosphere aeration equipment and then introduced into the heat treatment chamber.

[0013] Preferably, the temperature range in the airtight reaction chamber is 20-90°C, the temperature range in the drying chamber is 20-150°C, and the temperature range in the heat treatment chamber is 20-1000°C.

[0014] The present invention also provides a post-processing method using the alloy catalyst post-processing system, comprising the following steps: Step 1, placing the alloy catalyst to be treated into the drying chamber, and evacuating the drying chamber by the vacuum pump until the drying chamber is in a vacuum state; Step 2: adjust the heating device to heat the drying chamber so that the temperature in the drying chamber is 80°C, dry at 80°C for 12 hours, adjust the atmosphere charging device to charge the drying chamber with inert gas, then turn off the heating device to cool the drying chamber to room temperature; Step three, open the second chamber door, adjust the atmosphere charging device, fill the airtight reaction chamber with inert gas, and adjust the heating device to heat the airtight reaction chamber to maintain the temperature in the airtight reaction chamber at 25°C, open the first chamber door, put the dried sample into the heat treatment chamber, close the second chamber door, adjust the atmosphere charging device, first pass nitrogen into the heat treatment chamber for 20 min, and then pass nitrogen and hydrogen mixed gas, adjust the heating device, increase the temperature to 700°C at a heating rate of 5°C / min, and then keep it at 700°C for 2 h, and finally slowly cool the heat treatment chamber to room temperature; Step 4, opening the second chamber door, placing the cooled alloy catalyst into the screening device, collecting the dispersed alloy catalyst powder at the discharge port of the screening device, and weighing the alloy catalyst powder; Step 5, placing the alloy catalyst powder in the passivation sealed chamber, the atmosphere charging device charges a fixed amount of oxygen into the passivation sealed chamber according to the mass of the alloy catalyst, and stirring the alloy catalyst in the passivation sealed chamber for 3 hours to ensure a sufficient passivation effect; Step six, weigh and pack the passivated alloy catalyst in the airtight reaction chamber, and finally take out the sample.

[0015] Compared with the prior art, the present invention has achieved the following technical effects: The present invention provides an alloy catalyst post-processing system and a post-processing method, wherein various devices for post-processing the alloy catalyst are placed in a closed system consisting of an airtight reaction chamber, a drying chamber and a heat treatment chamber, and the airtight reaction chamber, the drying chamber and the heat treatment chamber are controlled by an atmosphere control device to control the atmosphere environment inside each of the chambers. During the transfer and treatment of the alloy catalyst, the alloy catalyst can be effectively prevented from contacting with air to cause spontaneous combustion, thereby ensuring the stability and safety of the alloy catalyst; and the post-processing devices are integrated together, which can greatly improve the convenience of operation, and enhance the treatment efficiency and process controllability. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0017] Figure 1 It is a structural schematic diagram of the alloy catalyst post-treatment system; Figure 2 is a cross-sectional view of an alloy catalyst post-treatment system; Figure 3 The LSV diagram of the PtCo alloy catalyst prepared by the post-treatment method of Example 2 and commercial 50 wt.% Pt / C; Figure 4 The polarization curve diagram of a single cell test of a PtCo alloy catalyst prepared by the post-treatment method of Example 2 and commercial 50 wt.% Pt / C; Figure 5 The LSV diagram of the PtCo alloy catalyst prepared by the post-treatment method of Example 2 before and after 30,000 cycles of endurance cycling.

[0018] In the figure: 1-airtight reaction chamber; 2-drying chamber; 3-heat treatment chamber; 4-screening device; 5-passivation sealing chamber; 6-main chamber; 7-discharge transition chamber; 8-vacuum interface; 9-drying chamber air inlet; 10-tray; 11-heat treatment chamber; 12-lifting device; 13-heat treatment air inlet; 14-heat treatment air outlet; 15-screening box; 16-weighing base; 17-screening box; 18-first-level screen; 19-second-level screen; 20-first-level exciter; 21-second-level exciter; 22-feeding port; 23-discharge port; 24-passivation air inlet; 25-passivation air outlet; 26-stirring device; 27-quantitative oxygen generator; 28-micro electrolytic water device. DETAILED DESCRIPTION

[0019] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] The purpose of the present invention is to provide an alloy catalyst post-treatment system and a post-treatment method to solve the problems existing in the above-mentioned prior art, to achieve uniform passivation of the alloy catalyst, to ensure the stability and safety of the alloy catalyst, to simplify the operation, to improve the treatment efficiency, and to ensure the controllability of the process.

[0021] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0022] Example 1 This embodiment provides an alloy catalyst post-treatment system, such as Figure 1-2As shown, it includes: an airtight reaction chamber 1; a drying chamber 2, which is airtightly connected to the airtight reaction chamber 1 through a first chamber door, and the drying chamber 2 is used to dry the alloy catalyst; a heat treatment chamber 3, which is airtightly connected to the airtight reaction chamber 1 through a second chamber door, and the heat treatment chamber 3 is used to heat treat the alloy catalyst after drying; a screening device 4, which is placed in the airtight reaction chamber 1, and the screening device 4 is used to screen and weigh the alloy catalyst after heat treatment; a passivation sealed chamber 5, which is placed in the airtight reaction chamber 1, and the passivation sealed chamber 5 is used to passivate the alloy catalyst after screening and weighing; an atmosphere control device, including a vacuum pump, an atmosphere charging device, an exhaust gas treatment device and an atmosphere control module The atmosphere control module is connected with the vacuum pump and the atmosphere charging device by signal. The vacuum pump is connected with the drying chamber 2 through a pipeline. The atmosphere charging device is connected with the airtight reaction chamber 1, the drying chamber 2, the heat treatment chamber 3 and the passivation sealing chamber 5 through pipelines. The atmosphere gas in the atmosphere charging device includes hydrogen, oxygen, nitrogen and inert gas. The exhaust gas treatment device is connected with the airtight reaction chamber 1, the heat treatment chamber 3 and the passivation sealing chamber 5 through pipelines; the heating device, the airtight reaction chamber 1, the drying chamber 2 and the heat treatment chamber 3 The heat treatment chamber 11 is connected with the heating device, the heating device selects an electric heating wire, and the heating device is electrically connected with the power supply device, which is used to independently heat the airtight reaction chamber 1, the drying chamber 2 and the heat treatment chamber 11. The various devices for post-treatment of the alloy catalyst are placed in a closed system consisting of an airtight reaction chamber 1, a drying chamber 2 and a heat treatment chamber 3, and the atmosphere environment inside the airtight reaction chamber 1, the drying chamber 2 and the heat treatment chamber 3 is controlled by an atmosphere control device. During the transfer and treatment of the alloy catalyst, the spontaneous combustion caused by the contact between the alloy catalyst and the air can be effectively avoided, thereby ensuring the stability and safety of the alloy catalyst; and the post-treatment devices are integrated together, which can greatly improve the convenience of operation, and enhance the treatment efficiency and process controllability.

[0023] It is further preferred in the implementation manner of the present embodiment that the airtight reaction chamber 1 includes a main chamber 6 and a discharge transition chamber 7, one side of the main chamber 6 is airtightly connected to the drying chamber 2 through a first chamber door, the other side of the main chamber 6 is airtightly connected to the discharge transition chamber 7 through a third chamber door, the bottom surface of the main chamber 6 is airtightly connected to the airtight reaction chamber 1 through a second chamber door, the screening device 4 and the passivation sealing chamber 5 are both located in the main chamber 6, and the heating device is surrounded on the outside of the main chamber 6 for heating the main chamber 6.

[0024] It is further preferred in the implementation manner of this embodiment that the drying chamber 2 has a vacuum interface 8 and a drying chamber air inlet 9, a vacuum pump is connected to the vacuum interface 8 for evacuating the drying chamber 2, an atmosphere charging device is connected to the drying chamber air inlet 9 for charging an inert gas into the drying chamber 2, and a tray 10 for holding an alloy catalyst is provided in the drying chamber 2.

[0025] It is further preferred in the implementation of this embodiment that a heat treatment chamber 3 is provided with a heat treatment chamber 11 and a lifting device 12, the lifting device 12 is connected to the heat treatment chamber 11, and is used to lift the heat treatment chamber 11 from the heat treatment chamber 3 to the airtight reaction chamber 1, or to drop the heat treatment chamber 11 from the airtight reaction chamber 1 to the heat treatment chamber 3, the heat treatment chamber 11 has a heat treatment chamber 11 door, a heat treatment air inlet 13 and a heat treatment air outlet 14, the atmosphere charging device is connected to the heat treatment air inlet 13, and is used to charge nitrogen and hydrogen into the heat treatment chamber 11, and the tail gas treatment device is connected to the heat treatment air outlet 14. The heat treatment temperature of the heat treatment chamber 11 is relatively high, and the heat treatment chamber 3 can isolate a certain amount of heat to avoid damage to the equipment in the airtight reaction chamber 1.

[0026] It is further preferred in the implementation manner of this embodiment that the screening device 4 includes a screening box 15 and a weighing base 16, the screening box 15 is arranged on the weighing base 16, the screening box 15 includes a screening box body 17, a primary screen 18, a secondary screen 19, a primary vibrator 20 and a secondary vibrator 21, the interior of the screening box body 17 is sequentially provided with a primary screen 18 and a secondary screen 19 from top to bottom, the primary screen 18 is connected to the primary vibrator 20, the secondary screen 19 is connected to the secondary vibrator 21, a feed port 22 is arranged at the top of the screening box body 17, a discharge port 23 is arranged at the bottom of the screening box body 17, and the weighing base 16 is used to weigh the alloy catalyst falling from the discharge port 23.

[0027] It is further preferred in the implementation manner of the present embodiment that the passivation sealed chamber 5 has a passivation chamber inlet, a passivation chamber outlet, a passivation air inlet 24 and a passivation air outlet 25, the atmosphere charging device is connected to the passivation air inlet 24, and is used to fill oxygen into the passivation sealed chamber 5, the tail gas treatment device is connected to the passivation air outlet 25, the passivation chamber inlet is located at the top of the passivation sealed chamber 5, and an inlet baffle door for opening or closing the passivation chamber inlet is provided at the passivation chamber inlet, the passivation chamber outlet is located at the bottom of the passivation sealed chamber 5, and an outlet baffle door for opening or closing the passivation chamber outlet is provided at the passivation chamber outlet; a stirring device 26 is provided in the passivation sealed chamber 5, the stirring device 26 includes a driving element, a stirring shaft and a plurality of groups of stirring blades, the driving element can be detachably mounted on the bottom plate of the passivation sealed chamber 5, the output shaft of the driving element is fixedly connected to the stirring shaft, the plurality of groups of stirring blades are connected to the stirring shaft and are arranged along the axial direction of the stirring shaft, the driving element drives the stirring shaft to rotate, and causes the stirring blades to stir the alloy catalyst in the passivation sealed chamber 5. The stirring device 26 can keep the alloy catalyst in full contact with oxygen, ensuring that the catalyst powder is stably passivated in the oxygen atmosphere.

[0028] In the implementation of this embodiment, it is further preferred that the atmosphere filling device includes a quantitative oxygen generator 27, the quantitative oxygen generator 27 is located in the airtight reaction chamber 1, and the quantitative oxygen generator 27 includes a reaction chamber, a catalyst storage chamber and an oxygen storage chamber. The reaction chamber is filled with a quantitative amount of hydrogen peroxide, the catalyst storage chamber is connected to the reaction chamber, and the reaction chamber and the oxygen storage chamber are sealed and connected through an oxygen delivery pipe. The oxygen generation speed and amount are controlled by adjusting the amount of catalyst entering the reaction chamber and the temperature in the reaction chamber; the oxygen storage chamber is connected and connected to the passivation sealed chamber 5. Further, the release rate of oxygen can also be controlled by selecting the type of catalyst, so as to achieve quantitative release and constant rate release of oxygen at the stoichiometric level. The catalyst is manganese dioxide, copper sulfate, hydrogen iodide, lead dioxide, ferric chloride, iron oxide, etc. The generated stable and quantitative oxygen is passed into the passivation sealed chamber 5 by the quantitative oxygen generator 27, which can effectively achieve uniform passivation of the alloy catalyst, prevent it from being over-oxidized or spontaneously combusted, and ensure the stability and safety of the alloy catalyst during post-treatment.

[0029] It is further preferred in the implementation of the present embodiment that the atmosphere filling device includes a micro water electrolysis device 28, the micro water electrolysis device 28 is located in the airtight reaction chamber 1, and the hydrogen prepared by the micro water electrolysis device 28 is used to pass into the heat treatment chamber 11. The micro water electrolysis device 28 can generate high-purity hydrogen, and by real-time regulation of the current, voltage and reaction time of the water electrolysis device, it is possible to achieve precise control of the hydrogen flow and concentration, avoid the use of high-pressure gas cylinders, and thus improve the miniaturization and safety of the device.

[0030] It is further preferred in the implementation of this embodiment that the temperature range in the airtight reaction chamber is 20-90°C, the temperature range in the drying chamber 2 is 20-150°C, and the temperature range in the heat treatment chamber 11 is 20-1000°C.

[0031] Example 2 This embodiment provides a post-treatment method using the alloy catalyst post-treatment system of embodiment 1, comprising the following steps: Step 1: Place the alloy catalyst to be treated into the drying chamber 2, and evacuate the drying chamber 2 by a vacuum pump until the drying chamber 2 is in a vacuum state; Step 2: Adjust the heating device to heat the drying chamber 2 so that the temperature in the drying chamber 2 is 80°C, dry at 80°C for 12 hours, adjust the atmosphere charging device to charge the drying chamber 2 with inert gas, then turn off the heating device to cool the drying chamber 2 to room temperature; Step three, adjust the atmosphere charging equipment, fill the airtight reaction chamber 1 with inert gas, and adjust the heating device to heat the airtight reaction chamber 1 to maintain the temperature in the airtight reaction chamber 1 at 25°C, open the second chamber door, lift the heat treatment chamber 11 from the heat treatment chamber 3 to the airtight reaction chamber 1 by the lifting device 12, open the first chamber door, take out the dried sample from the drying chamber 2 and put it into the heat treatment chamber 11, close the first chamber door, and drop the heat treatment chamber 11 from the airtight reaction chamber 1 to the heat treatment chamber 3 by the lifting device 12, close the second chamber door, adjust the atmosphere charging equipment, first introduce nitrogen into the heat treatment chamber 11 for 20 min, and then introduce nitrogen and hydrogen mixed gas, adjust the heating device, raise the temperature to 700°C at a heating rate of 5°C / min, and then keep it at 700°C for 2 h, and finally slowly cool the heat treatment chamber 11 to room temperature; Step 4, open the second chamber door, put the cooled alloy catalyst into the screening device 4, turn on the vibrator to vibrate the primary screen 18 and the secondary screen 19, and disperse the alloy catalyst into powder by vibration, collect the dispersed alloy catalyst powder at the discharge port 23 of the screening device 4, and weigh the alloy catalyst powder by the weighing base 16; Step 5: placing the alloy catalyst powder in the passivation sealed chamber 5, and the atmosphere charging device generates a quantitative amount of oxygen by adjusting the amount of catalyst that reacts with the quantitative hydrogen peroxide in the quantitative oxygen generating device 27 and the temperature in the reaction chamber according to the mass of the alloy catalyst. For example, the mass of hydrogen peroxide and manganese dioxide is determined according to the mass ratio of the alloy catalyst, hydrogen peroxide, and manganese dioxide being 2:60:1, and the reaction temperature is adjusted to 60°C. The generated quantitative oxygen is slowly charged into the passivation sealed chamber 5, and the alloy catalyst in the passivation sealed chamber 5 is stirred for more than 3 hours by the stirring device 26 to ensure that the catalyst powder is stably passivated in the oxygen atmosphere; Step six, weigh and pack the passivated alloy catalyst in the airtight reaction chamber 1, open the third chamber door, put the weighed and packed samples into the discharge transition chamber, and finally open the outer door of the transition chamber to take out the samples.

[0032] like Figure 3 As shown, the initial mass activity of the PtCo alloy catalyst prepared according to the post-treatment method of Example 2 is as high as 568 mA / mg, which is much better than the commercial catalyst.

[0033] like Figure 4 As shown, the PtCo alloy catalyst prepared according to the post-treatment method of Example 2 is much better than the commercial catalyst in terms of single cell performance.

[0034] like Figure 5 As shown, the LSV results show that the half-wave potential on the LSV only dropped by 10 mv before and after the stability test, indicating that the PtCo alloy catalyst has excellent stability and excellent activity.

[0035] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. An alloy catalyst post-treatment system, characterized in that: include: Airtight reaction chamber; A drying chamber, which is airtightly connected to the airtight reaction chamber through a first chamber door, and the drying chamber is used to dry the alloy catalyst; a heat treatment chamber, which is airtightly connected to the airtight reaction chamber through a second chamber door, and the heat treatment chamber is used to heat treat the alloy catalyst after the drying treatment; A screening device is placed in the airtight reaction chamber, and is used to screen and weigh the alloy catalyst after the heat treatment; A passivation sealed chamber, the passivation sealed chamber is placed in the airtight reaction chamber, and the passivation sealed chamber is used to passivate the alloy catalyst after screening and weighing; An atmosphere control device, comprising a vacuum pump, an atmosphere charging device, an exhaust gas treatment device and an atmosphere control module, wherein the atmosphere control module is signal-connected to the vacuum pump and the atmosphere charging device, the vacuum pump is communicated with the drying chamber through a pipeline, the atmosphere charging device is respectively communicated with the airtight reaction chamber, the drying chamber, the heat treatment chamber and the passivation sealed chamber through pipelines, and the exhaust gas treatment device is respectively communicated with the airtight reaction chamber, the heat treatment chamber and the passivation sealed chamber through pipelines; A heating device, wherein the airtight reaction chamber, the drying chamber and the heat treatment chamber of the heat treatment chamber are all connected to the heating device, and the heating device is used to independently heat the airtight reaction chamber, the drying chamber and the heat treatment chamber.

2. The alloy catalyst post-treatment system according to claim 1, characterized in that: The airtight reaction chamber includes a main chamber and a discharge transition chamber. One side of the main chamber is airtightly connected to the drying chamber through the first chamber door, and the other side of the main chamber is airtightly connected to the discharge transition chamber through the third chamber door. The bottom surface of the main chamber is airtightly connected to the airtight reaction chamber through the second chamber door. The screening device and the passivation sealing chamber are both located in the main chamber, and the heating device is used to heat the main chamber.

3. The alloy catalyst post-treatment system according to claim 1, characterized in that: The drying chamber has a vacuum interface and a drying chamber air inlet. The vacuum pump is connected to the vacuum interface and is used to evacuate the drying chamber. The atmosphere charging device is connected to the drying chamber air inlet and is used to charge inert gas into the drying chamber. A tray for holding an alloy catalyst is provided in the drying chamber.

4. The alloy catalyst post-treatment system according to claim 1, characterized in that: The heat treatment chamber is provided with the heat treatment chamber and a lifting device, the lifting device is connected to the heat treatment chamber, and is used to lift the heat treatment chamber from the heat treatment chamber to the airtight reaction chamber, or to drop the heat treatment chamber from the airtight reaction chamber to the heat treatment chamber, the heat treatment chamber has a heat treatment chamber door, a heat treatment air inlet and a heat treatment air outlet, the atmosphere charging device is connected to the heat treatment air inlet, and is used to charge the heat treatment chamber with a reaction gas for post-treatment of the catalyst, the reaction gas is a N2 / H2 mixed gas or an Ar / H2 mixed gas, and the exhaust gas treatment device is connected to the heat treatment outlet.

5. The alloy catalyst post-treatment system according to claim 1, characterized in that: The screening device includes a screening box and a weighing base, the screening box is arranged on the weighing base, the screening box includes a screening box body, a primary screen, a secondary screen, a primary vibrator and a secondary vibrator, the primary screen and the secondary screen are arranged in sequence from top to bottom inside the screening box body, the primary screen is connected to the primary vibrator, the secondary screen is connected to the secondary vibrator, a feed port is arranged at the top of the screening box body, a discharge port is arranged at the bottom of the screening box body, and the weighing base is used to weigh the alloy catalyst falling from the discharge port.

6. The alloy catalyst post-treatment system according to claim 1, characterized in that: The passivation sealed chamber has a passivation chamber inlet, a passivation chamber outlet, a passivation air inlet and a passivation air outlet. The atmosphere charging device is connected to the passivation air inlet for charging oxygen into the passivation sealed chamber. The tail gas treatment device is connected to the passivation air outlet. The passivation chamber inlet is located at the top of the passivation sealed chamber, and an inlet baffle door for opening or closing the passivation chamber inlet is provided at the passivation chamber inlet. The passivation chamber outlet is located at the bottom of the passivation sealed chamber, and an outlet baffle door for opening or closing the passivation chamber outlet is provided at the passivation chamber outlet. A stirring device is provided in the passivation sealed chamber, and the stirring device includes a driving element, a stirring shaft and a plurality of stirring blades. The driving element can be detachably mounted on the bottom plate of the passivation sealed chamber, the output shaft of the driving element is fixedly connected to the stirring shaft, the plurality of stirring blades are connected to the stirring shaft and arranged along the axial direction of the stirring shaft, the driving element drives the stirring shaft to rotate, and the stirring blades stir the alloy catalyst in the passivation sealed chamber.

7. The alloy catalyst post-treatment system according to claim 6, characterized in that: The atmosphere inflation equipment includes a quantitative oxygen generator, which is located in the airtight reaction chamber. The quantitative oxygen generator includes a reaction chamber, a catalyst storage chamber and an oxygen storage chamber. The reaction chamber is filled with a quantitative amount of hydrogen peroxide. The catalyst storage chamber is communicated with the reaction chamber. The reaction chamber and the oxygen storage chamber are sealed and connected through an oxygen delivery pipe. The oxygen generation speed and amount are controlled by adjusting the amount of catalyst entering the reaction chamber and the temperature in the reaction chamber. The oxygen storage chamber is connected and communicated with the passivation sealing chamber.

8. The alloy catalyst post-treatment system according to claim 4, characterized in that: The atmosphere aeration equipment comprises a micro water electrolysis device, which is located in the airtight reaction chamber. The hydrogen prepared by the micro water electrolysis device is quantitatively controlled by a flow meter and mixed with N2 or inert gas delivered by the atmosphere aeration equipment before being introduced into the heat treatment chamber.

9. The alloy catalyst post-treatment system according to claim 1, characterized in that: The temperature range in the airtight reaction chamber is 20-90°C, the temperature range in the drying chamber is 20-150°C, and the temperature range in the heat treatment chamber is 20-1000°C.

10. A post-treatment method using the alloy catalyst post-treatment system according to any one of claims 1 to 9, characterized in that: The steps include: Step 1, placing the alloy catalyst to be treated into the drying chamber, and evacuating the drying chamber by the vacuum pump until the drying chamber is in a vacuum state; Step 2: adjust the heating device to heat the drying chamber so that the temperature in the drying chamber is 80°C, dry at 80°C for 12 hours, adjust the atmosphere charging device to charge the drying chamber with inert gas, then turn off the heating device to cool the drying chamber to room temperature; Step three, open the second chamber door, adjust the atmosphere charging device, fill the airtight reaction chamber with inert gas, and adjust the heating device to heat the airtight reaction chamber to maintain the temperature in the airtight reaction chamber at 25°C, open the first chamber door, put the dried sample into the heat treatment chamber, close the second chamber door, adjust the atmosphere charging device, first pass nitrogen into the heat treatment chamber for 20 min, and then pass nitrogen and hydrogen mixed gas, adjust the heating device, increase the temperature to 700°C at a heating rate of 5°C / min, and then keep it at 700°C for 2 h, and finally slowly cool the heat treatment chamber to room temperature; Step 4, opening the second chamber door, placing the cooled alloy catalyst into the screening device, collecting the dispersed alloy catalyst powder at the discharge port of the screening device, and weighing the alloy catalyst powder; Step 5, placing the alloy catalyst powder in the passivation sealed chamber, the atmosphere charging device charges a fixed amount of oxygen into the passivation sealed chamber according to the mass of the alloy catalyst, and stirring the alloy catalyst in the passivation sealed chamber for 3 hours to ensure a sufficient passivation effect; Step six, weigh and pack the passivated alloy catalyst in the airtight reaction chamber, and finally take out the sample.

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