A catalyst heat treatment device

By designing a catalyst heat treatment device and utilizing a real-time gas concentration monitoring and control module, the problems of incomplete impurity removal and oxidation of Pt-M/C alloy catalysts during heat treatment were solved, achieving efficient and stable heat treatment and automated production of the catalyst.

CN119687688BActive Publication Date: 2025-10-28SHENZHEN ACAD OF AEROSPACE TECH
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Patent Information

Application Number
CN202411871307.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-18
Publication Date
2025-10-28
Estimated Expiration
2044-12-18

AI Technical Summary

Technical Problem

Existing heat treatment equipment is prone to incomplete removal of impurities, insufficient metal migration, agglomeration or oxidation when processing Pt-M/C alloy catalysts, leading to deterioration of catalyst performance and even smoldering. Furthermore, the catalyst is easily oxidized during the removal process, affecting its activity and lifespan.

Method used

A catalyst heat treatment device was designed, comprising a heating module, an inlet module, and an outlet module. The gas concentration is monitored in real time using reaction gas inlet and outlet probes, and the gas flow rate and temperature are adjusted by a control module to ensure that the catalyst is treated in an inert atmosphere, preventing oxidation and achieving automated production.

Benefits of technology

It effectively removes impurities from the catalyst, ensures sufficient metal migration, avoids oxidation reactions, improves catalyst activity and stability, and enables efficient thermal treatment and automated production of the catalyst.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention provides a catalyst heat treatment device, including a heating module for heat treating the catalyst, an inlet module and an outlet module both connected to the heating module. The heating module includes a reaction vessel for containing the catalyst and a heating device for heating the catalyst. The inlet module includes a reaction gas tank for providing a reaction gas to react with the catalyst, an inert gas tank for providing an inert gas, and an inlet device. The reaction gas and the inert gas are mixed in the inlet device to form a mixed gas that enters the reaction vessel. The inlet device is equipped with a reaction gas inlet probe for monitoring the inlet concentration of the reaction gas in the inlet device. After the mixed gas reacts with the catalyst in the reaction vessel, it enters the outlet module. The outlet module is equipped with a reaction gas outlet probe for monitoring the outlet concentration of the reaction gas in the outlet module.
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Description

Technical Field

[0001] This invention relates to a heat treatment device for industrial production, and more particularly to a catalyst heat treatment device. Background Technology

[0002] Currently, proton exchange membrane fuel cells mainly use Pt-based noble metal catalysts, the most typical being carbon-supported platinum (Pt / C) catalysts. However, Pt-based catalysts require a high Pt metal loading, leading to problems such as poor durability and low mass activity. To address these issues, Pt-M / C alloy catalysts (M = Ni, Co, Fe, Cu, Cr) have been developed in recent years. These catalysts offer significant improvements in electrical performance compared to traditional catalysts, particularly as cathode catalysts in fuel cells, demonstrating great application potential.

[0003] To further improve the performance of Pt-M / C alloy catalysts, heat treatment is required in the later stages of the preparation process. The purpose is to remove impurities that remain after the previous treatment and affect the catalyst performance, and also to allow different metals in the alloy nanoparticles to migrate, thereby increasing the surface Pt content and giving the alloy catalyst more active sites for oxygen reduction, thus improving the catalyst activity.

[0004] However, in general heat treatment equipment, the catalyst semi-finished product is usually placed in the equipment cavity, and a mixed gas of a specific composition is introduced through the gas inlet. This mixed gas also contains gaseous components that can react with the catalyst sample. The mixture is heated to a certain temperature and treated in this specific gas atmosphere for a certain period of time, thus proceeding with subsequent processing or becoming the finished product. This process is prone to several problems: 1. Insufficient heat treatment leads to incomplete removal of impurities that affect catalyst performance from previous treatments, and insufficient migration of different metals in nanoparticles, severely impacting catalyst performance; 2. Over-heat treatment not only causes agglomeration of alloy catalyst particles, reducing catalyst activity; 3. Poor atmosphere protection or sealing during heat treatment allows the catalyst to come into contact with oxygen during the process, resulting in oxidation, severely degrading catalyst performance, or even direct smoldering, leading to scrap; 4. During the removal of the catalyst after heat treatment, the catalyst comes into contact with air. Due to the high oxygen concentration in the air and the high catalyst activity, a violent oxidation reaction easily occurs, severely degrading catalyst performance, or even direct smoldering, leading to scrap. Summary of the Invention

[0005] In view of the above, the present invention aims to at least solve one of the technical problems existing in the prior art. To this end, the present invention proposes a catalyst heat treatment apparatus that can quickly and conveniently heat treat catalysts.

[0006] This invention provides a catalyst heat treatment apparatus, comprising a heating module for heat treating the catalyst, an inlet module and an outlet module both connected to the heating module, the heating module including a reaction vessel for containing the catalyst and a heating device for heating the catalyst, the inlet module including a reaction gas tank for providing a reaction gas to react with the catalyst, an inert gas tank for providing an inert gas and an inlet device, the reaction gas and the inert gas being mixed in the inlet device to form a mixed gas that enters the reaction vessel, the inlet device being equipped with a reaction gas inlet probe for monitoring the inlet gas concentration in the inlet device, the mixed gas reacting with the catalyst in the reaction vessel and then entering the outlet module, the outlet module being equipped with a reaction gas outlet probe for monitoring the outlet gas concentration in the outlet module.

[0007] In some embodiments, the catalyst heat treatment equipment further includes a control module. The reaction gas inlet probe sends the monitored reaction gas inlet concentration signal to the control module, and the reaction gas outlet probe sends the monitored reaction gas outlet concentration signal to the control module. When the outlet concentration of the reaction gas is less than the inlet concentration of the reaction gas, the control module determines that the catalyst is still in the heat treatment process. When the outlet concentration of the reaction gas is equal to the inlet concentration of the reaction gas, the control module determines that the catalyst has completed the heat treatment.

[0008] In some embodiments, a first flow meter is provided at the outlet of the reaction gas tank. The first flow meter is electrically connected to the control module, and the control module can control the first flow meter to increase or decrease the flow rate of the reaction gas.

[0009] In some embodiments, the outlet of the inert gas tank is provided with a second flow meter, which is electrically connected to the control module. The control module can control the second flow meter to increase or decrease the flow rate of the inert gas.

[0010] In some embodiments, the catalyst heat treatment equipment further includes an oxygen gas tank containing oxygen, the oxygen gas tank being connected to the air inlet device, through which the oxygen can enter the reaction vessel.

[0011] In some embodiments, a third flow meter is provided at the outlet of the oxygen gas cylinder. The third flow meter is electrically connected to the control module, and the control module can control the third flow meter to increase or decrease the oxygen flow rate.

[0012] In some embodiments, the air intake device is provided with an oxygen intake probe for monitoring the oxygen intake concentration in the air intake device, and the air outlet module is provided with an oxygen outlet probe for monitoring the oxygen outlet concentration in the air outlet module.

[0013] In some embodiments, the oxygen inlet probe sends the monitored oxygen inlet concentration signal to the control module, and the oxygen outlet probe sends the monitored oxygen outlet concentration signal to the control module. When the catalyst is heat-treated, if oxygen permeation occurs due to poor equipment atmosphere protection measures or sealing failure, the oxygen inlet concentration or the oxygen outlet concentration will change. The control module will control the second flow meter to increase the inert gas flow rate for purging to reduce the oxygen concentration.

[0014] In some embodiments, before removing the catalyst after the catalyst heat treatment is completed, the control module controls the first flow meter and the second flow meter to reduce the flow rates of the reaction gas and the inert gas, respectively, and controls the third flow meter to increase the oxygen flow rate, so as to gradually increase the oxygen intake concentration until the oxygen intake concentration detected by the oxygen intake probe reaches the oxygen concentration in the air.

[0015] In some embodiments, the heating module is further provided with a temperature probe, which is housed inside the reactor to monitor the temperature inside the reactor in real time and send the temperature signal to the control module.

[0016] The catalyst heat treatment equipment of this invention performs heat treatment on the catalyst through a heating module, and uses the reaction gas inlet probe and the reaction gas outlet probe to monitor the concentration of reaction gas in the mixed gas in real time, and determines whether the catalyst has completed heat treatment based on the concentration of reaction gas inlet and outlet. In addition, the oxygen concentration in the mixed gas is monitored in real time by the oxygen inlet probe and the oxygen outlet probe to determine whether there are any problems such as poor sealing of the catalyst heat treatment equipment that allow oxygen to enter the equipment. Furthermore, the catalyst heat treatment equipment has a simple structure, can effectively heat treat the catalyst, and can be effectively connected to upstream and downstream processes, facilitating production automation. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of a catalyst heat treatment device according to an embodiment of the present invention;

[0018] Figure 2 This is a schematic diagram of the catalyst heat treatment equipment according to an embodiment of the present invention.

[0019] Figure label:

[0020] Catalyst heat treatment equipment 100;

[0021] Control module 10; Heating module 20;

[0022] 21. Reactor; 22. Heating device; 23. Temperature probe;

[0023] Intake module 30; Reactant gas tank 31; Pressure reducing valve 311; First flow meter 312;

[0024] Inert gas tank 32; pressure reducing valve 321; second flow meter 322;

[0025] Oxygen gas cylinder 33; pressure reducing valve 331; third flow meter 332;

[0026] Air intake device 34; reactive gas intake probe 341; oxygen intake probe 342; intake pressure gauge 343;

[0027] Gas outlet module 40; Reaction gas outlet probe 41; Oxygen outlet probe 42; Gas outlet pressure gauge 43;

[0028] Pipeline 50. Detailed Implementation

[0029] Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and intended to explain the present invention, and should not be construed as limiting the present invention.

[0030] The following disclosure provides numerous different embodiments or examples for implementing various structures of the invention. To simplify the disclosure, specific examples of components and arrangements are described below. These are merely examples and are not intended to limit the invention. Furthermore, reference numerals and / or letters may be repeated in different examples. Such repetition is for simplification and clarity and does not in itself indicate a relationship between the various embodiments and / or arrangements discussed. Additionally, examples of various specific processes and materials are provided, but those skilled in the art will recognize the reusability of other processes and / or the use of other materials.

[0031] This invention provides a catalyst heat treatment apparatus 100. The catalyst heat treatment apparatus 100 according to an embodiment of the present invention is described below with reference to the accompanying drawings.

[0032] Please see Figure 1The catalyst heat treatment equipment 100 is used to heat treat the catalyst 200, and includes a control module 10, a heating module 20, an air inlet module 30, and an air outlet module 40. The control module 10 is electrically connected to the heating module 20, the air inlet module 30, and the air outlet module 40 to control their operation. In this embodiment, the catalyst 200 is a Pt-M / C alloy catalyst, where M can be nickel, cobalt, iron, copper, or chromium metal, and the control module 10 can be a PLC controller.

[0033] Please see Figures 1 to 2 The heating module 20 is used to heat treat the catalyst 200. The heating module 20 includes a reaction vessel 21, a heating device 22, and a temperature probe 23. The reaction vessel 21 has a cavity for containing the catalyst 200. The heating device 22 is located at the bottom of the reaction vessel 21 to heat the catalyst 200. The temperature probe 23 is housed in the cavity to monitor the temperature inside the reaction vessel 21 in real time.

[0034] It is understood that both the heating device 22 and the temperature probe 23 are electrically connected to the control module 10. That is, the control module 10 can control the heating device 22 to turn on or off, and the temperature probe 23 can send the monitored temperature signal to the control module 10. Specifically, when heat-treating the catalyst 200, a preset temperature threshold is established. The temperature probe 23 monitors the temperature inside the reactor 21 and transmits the temperature signal to the control module 10. If the control module 10 determines that the temperature is below the temperature threshold, it will control the heating device 22 to increase its heating power; if the control module 10 determines that the temperature is above the temperature threshold, it will control the heating device 22 to decrease its heating power.

[0035] The air intake module 30 includes a reaction gas tank 31, an inert gas tank 32, an oxygen tank 33, and an air intake device 34. The reaction gas tank 31, the inert gas tank 32, and the oxygen tank 33 are all connected to the air intake device 34 via pipes 50.

[0036] The reaction gas tank 31 stores a gas for reacting with the catalyst 200. In this embodiment, the reaction gas can be a reducing gas such as hydrogen. The outlet of the reaction gas tank 31 is equipped with a pressure reducing valve 311 and a first flow meter 312. The pressure reducing valve 311 can reduce the gas pressure of the reaction gas in the pipeline 50. The first flow meter 312 is electrically connected to the control module 10, and the control module 10 can control the first flow meter 312 to increase or decrease the flow rate of the reaction gas.

[0037] The inert gas tank 32 stores a gas used to protect the catalyst. In this embodiment, the inert gas can be a gas such as helium. The outlet of the inert gas tank 32 is equipped with a pressure reducing valve 321 and a second flow meter 322. The pressure reducing valve 321 can reduce the gas pressure of the inert gas in the pipeline 50. The second flow meter 322 is electrically connected to the control module 10, and the control module 10 can control the second flow meter 322 to increase or decrease the flow rate of the inert gas.

[0038] The oxygen cylinder 33 contains oxygen. The outlet of the oxygen cylinder 33 is equipped with a pressure reducing valve 331 and a third flow meter 332. The pressure reducing valve 331 can reduce the oxygen pressure in the pipeline 50. The third flow meter 332 is electrically connected to the control module 10, and the control module 10 can control the third flow meter 332 to increase or decrease the oxygen flow rate.

[0039] The air intake device 34 is used to mix the gases flowing out of the reaction gas tank 31, the inert gas tank 32, and the oxygen tank 33, and to send the mixed gas into the reactor 21 of the heating module 20 through the pipe 50. The air intake device 34 is equipped with a reaction gas intake probe 341 and an oxygen intake probe 342, both of which are electrically connected to the control module 10. The reaction gas intake probe 341 is used to monitor the concentration of the reaction gas in the air intake device 34 in real time and send a signal to the control module 10. The oxygen intake probe 342 is used to monitor the concentration of oxygen in the air intake device 34 in real time and send a signal to the control module 10. The air intake device 34 is also equipped with an intake pressure gauge 343, which is used to monitor the intake pressure of the mixed gas entering the reactor 21 from the air intake device 34 in real time.

[0040] The gas outlet module 40 is connected to the reactor 21 via the pipe 50, allowing the mixed gas to exit from the reactor 21 and enter the gas outlet module 40. The gas outlet module 40 is equipped with a reaction gas outlet probe 41 and an oxygen outlet probe 42, both electrically connected to the control module 10. The reaction gas outlet probe 41 monitors the concentration of the reaction gas in the gas outlet module 40 in real time and sends a signal to the control module 10. The oxygen outlet probe 42 monitors the concentration of oxygen in the gas outlet module 40 in real time and sends a signal to the control module 10. The gas outlet module 40 is also equipped with an outlet pressure gauge 43, which monitors the outlet pressure of the mixed gas entering the gas outlet module 40 from the reactor 21 in real time.

[0041] When the catalyst heat treatment equipment 100 provided by the present invention is working, the catalyst 200 to be treated is placed in the cavity of the reaction vessel 21. The control module 10 controls the first flow meter 312 and the second flow meter 322 to open, so that the reaction gas in the reaction gas tank 31 and the inert gas in the inert gas tank 32 enter the air inlet device 34 after passing through the pressure reducing valve 321 and the pressure reducing valve 331, respectively. The reaction gas and the inert gas are mixed in the air inlet device 34 to form a mixed gas and enter the reaction vessel 21 through the pipe 50. The air inlet pressure gauge 343 monitors the air inlet pressure of the mixed gas entering the reaction vessel 21 from the air inlet device 34 in real time.

[0042] After the mixed gas displaces the original air in the reactor 21, the control module 10 controls the heating device 22 to turn on to heat the catalyst 200. The temperature probe 23 monitors the temperature inside the reactor 21 in real time and transmits the temperature signal to the control module 10. The control module 10 compares the temperature signal with a preset temperature threshold to control the heating device 22 to increase or decrease the heating power, thereby maintaining the temperature inside the reactor 21 within a stable range.

[0043] In this embodiment, when the catalyst heat treatment equipment 100 is working, the reaction gas inlet probe 341 monitors the inlet concentration of the reaction gas in the inlet device 34 in real time and sends the signal to the control module 10. The reaction gas outlet probe 41 monitors the outlet concentration of the reaction gas in the outlet module 40 in real time and sends the signal to the control module 10. The control module 10 compares the inlet concentration of the reaction gas with the outlet concentration of the reaction gas to determine whether the catalyst 200 has completed heat treatment. Specifically, when the outlet concentration of the reaction gas is less than the inlet concentration of the reaction gas, it indicates that the reaction gas is still reacting with the catalyst, and the control module 10 determines that the catalyst is still in the heat treatment process. At this time, the control module 10 can control the first flow meter 312 to increase the flow rate of the reaction gas to avoid insufficient heat treatment of the catalyst 200. When the outlet concentration of the reaction gas is equal to the inlet concentration of the reaction gas, it indicates that the reaction gas is no longer reacting with the catalyst, and the control module 10 determines that the catalyst 200 has completed heat treatment. At this time, the control module 10 controls the heating device 22 to stop heating, and the first flow meter 312 shuts off the reaction gas tank 31 to avoid overheating of the catalyst 200.

[0044] Furthermore, during the operation of the catalyst heat treatment equipment 100, the oxygen inlet probe 342 monitors the oxygen inlet concentration in the inlet device 34 in real time and sends the signal to the control module 10. Similarly, the oxygen outlet probe 42 monitors the oxygen outlet concentration in the outlet module 40 in real time and sends the signal to the control module 10. If oxygen permeates into the catalyst heat treatment equipment 100 due to factors such as poor equipment atmosphere protection measures or sealing failure, the oxygen inlet and outlet concentrations will change. The control module 10 will then control the second flow meter 322 to increase the inert gas flow rate for purging based on the oxygen concentration data, thereby reducing the oxygen concentration and preventing the catalyst 200 from coming into contact with oxygen during the heat treatment process.

[0045] After the catalyst heat treatment is completed, to prevent the catalyst 200 from undergoing a violent oxidation reaction with oxygen in the air during removal, which could lead to performance degradation, the catalyst heat treatment equipment 100 of the present invention, after heat treatment, controls the heating device 22 to shut down. After the temperature probe 23 detects that the temperature inside the reaction vessel 21 has dropped to room temperature, the control module 10 controls the third flow meter 332 to open, allowing oxygen from the oxygen gas tank 33 to enter the reaction vessel 21 through the air inlet device 34. During this process, the control module 10 controls the first flow meter 312 and the second flow meter 322 to reduce the flow rates of the reaction gas and inert gas, and controls the third flow meter 332 to increase the oxygen flow rate. The oxygen inlet probe 342 monitors the oxygen inlet concentration, which slowly increases until the oxygen inlet concentration equals the oxygen concentration in the air. At the same time, the oxygen outlet probe 42 sends a signal to the control module 10. When the control module 10 determines that the oxygen outlet concentration is equal to the oxygen inlet concentration, it can open the catalyst heat treatment equipment 100 to remove the catalyst 200, thereby preventing the catalyst 200 from undergoing a violent oxidation reaction due to sudden contact with oxygen after heat treatment.

[0046] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0047] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0048] Although embodiments of the invention have been shown and described, those skilled in the art will understand that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.

Claims

1. A catalyst heat treatment apparatus for heat treating a catalyst, characterized in that, The catalyst heat treatment equipment includes a heating module for heat treating the catalyst, an inlet module and an outlet module both connected to the heating module. The heating module includes a reaction vessel for containing the catalyst and a heating device for heating the catalyst. The inlet module includes a reaction gas tank for providing a reaction gas to react with the catalyst, an inert gas tank for providing an inert gas, and an inlet device. The reaction gas and the inert gas are mixed in the inlet device to form a mixed gas that enters the reaction vessel. The inlet device is equipped with a reaction gas inlet probe for monitoring the inlet concentration of the reaction gas in the inlet device. After the mixed gas reacts with the catalyst in the reaction vessel, it enters the outlet module. The outlet module is equipped with a reaction gas outlet probe for monitoring the outlet concentration of the reaction gas in the outlet module. The catalyst heat treatment equipment also includes a control module. The reaction gas inlet probe sends the monitored reaction gas inlet concentration signal to the control module, and the reaction gas outlet probe sends the monitored reaction gas outlet concentration signal to the control module. When the outlet concentration of the reaction gas is less than the inlet concentration, the control module determines that the catalyst is still undergoing heat treatment. When the outlet concentration of the reaction gas is equal to the inlet concentration, the control module determines that the catalyst has completed heat treatment. A second flow meter is installed at the outlet of the inert gas tank. The second flow meter is electrically connected to the control module, and the control module can control the second flow meter to increase or decrease the inert gas flow rate. The catalyst heat treatment equipment also includes an oxygen gas tank containing oxygen. The tank is connected to the air inlet device, allowing oxygen to enter the reactor. An oxygen inlet probe is installed within the air inlet device to monitor the oxygen inlet concentration. An oxygen outlet probe is installed within the outlet module to monitor the oxygen outlet concentration. The oxygen inlet probe sends the monitored oxygen inlet concentration signal to the control module, and the oxygen outlet probe sends the monitored oxygen outlet concentration signal to the control module. During catalyst heat treatment, if oxygen permeation occurs due to poor equipment atmosphere protection measures or sealing failure, the oxygen inlet concentration or the oxygen outlet concentration will change. The control module will then control the second flow meter to increase the inert gas flow rate for purging to reduce the oxygen concentration.

2. The catalyst heat treatment equipment according to claim 1, characterized in that, The outlet of the reaction gas tank is equipped with a first flow meter, which is electrically connected to the control module. The control module can control the first flow meter to increase or decrease the flow rate of the reaction gas.

3. The catalyst heat treatment equipment according to claim 2, characterized in that, The oxygen gas cylinder is equipped with a third flow meter at its outlet. The third flow meter is electrically connected to the control module, which can control the third flow meter to increase or decrease the oxygen flow rate.

4. The catalyst heat treatment equipment according to claim 3, characterized in that, Before removing the catalyst after the catalyst heat treatment is completed, the control module controls the first flow meter and the second flow meter to reduce the flow rates of the reaction gas and the inert gas, respectively, and controls the third flow meter to increase the oxygen flow rate, so as to gradually increase the oxygen intake concentration until the oxygen intake concentration detected by the oxygen intake probe reaches the oxygen concentration in the air.

5. The catalyst heat treatment equipment according to claim 1, characterized in that, The heating module is also equipped with a temperature probe, which is housed inside the reactor to monitor the temperature inside the reactor in real time and send the temperature signal to the control module.

Citation Information

Patent Citations

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