Catalyst heat treatment equipment

Abstract

The invention provides catalyst heat treatment equipment which comprises a heating module used for carrying out heat treatment on a catalyst, a gas inlet module and a gas outlet module, the gas inlet module and the gas outlet module are both communicated with the heating module, and the heating module comprises a reaction kettle used for containing the catalyst and a heating device used for heating the catalyst. The gas inlet module comprises a reaction gas tank used for providing reaction with the catalyst, an inert gas tank used for providing inert gas and a gas inlet device, the reaction gas and the inert gas are mixed in the gas inlet device to form mixed gas, and the mixed gas enters the reaction kettle; the gas inlet device is provided with a reaction gas inlet probe used for monitoring the inlet gas concentration of reaction gas in the gas inlet device, and the mixed gas reacts with a catalyst in the reaction kettle and then enters the gas outlet module. The gas outlet module is provided with a reaction gas outlet probe used for monitoring the outlet gas concentration of reaction gas in the gas outlet module.

Description

Technical Field

[0001] The invention relates to a heat treatment device for industrial production, in particular to a catalyst heat treatment device. Background Art

[0002] At present, proton exchange membrane fuel cells mainly use Pt-based precious metal catalysts, the most typical of which is carbon-supported platinum (Pt / C) catalyst. However, Pt-based catalysts have high requirements for Pt metal loading, which leads to problems such as poor durability and low mass activity. In response to the above problems, Pt-M / C alloy catalysts (M = Ni, Co, Fe, Cu, Cr) have been developed in recent years. Compared with traditional catalysts, the electrical performance has been greatly improved, especially the Pt-M / C alloy catalyst as a fuel cell cathode catalyst, which has great application prospects.

[0003] In order to further improve the performance of the Pt-M / C alloy catalyst, the Pt-M / C alloy catalyst needs to be heat treated in the latter stage of the preparation process. The purpose is to remove the impurities that affect the catalyst performance remaining from the previous treatment, and to allow the different metals of the alloy nanoparticles to migrate so that the surface Pt content is higher, thereby making the alloy catalyst have more active sites for oxygen reduction and improving the catalyst activity.

[0004] However, in general heat treatment equipment, the semi-finished catalyst is usually placed in the cavity of the equipment, and a mixed gas of a specific composition is introduced through the air inlet. The mixed gas also contains gas components that can react with the catalyst sample, and is heated to a certain temperature and treated in a specific gas atmosphere for a certain period of time, so as to be subsequently treated or used as a finished product. This process is prone to some problems: 1. Insufficient heat treatment leads to incomplete removal of impurities that affect the performance of the catalyst from the previous treatment, and insufficient migration of different metals in the nanoparticles, which seriously affects the performance of the catalyst; 2. Excessive heat treatment not only causes the agglomeration of alloy catalyst particles, but also reduces the activity of the catalyst; 3. Poor atmosphere protection measures or poor sealing during heat treatment lead to the catalyst contacting oxygen during the heat treatment process, causing oxidation reactions, which seriously deteriorates the performance of the catalyst, and even directly smolders, resulting in scrapping; 4. In the process of removing the catalyst after the heat treatment, the catalyst contacts the air. Due to the high oxygen concentration in the air and the high activity of the catalyst, it is easy to undergo a violent oxidation reaction, which seriously deteriorates the performance of the catalyst, and even directly smolders, resulting in scrapping. Summary of the invention

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

[0006] An embodiment of the present invention provides a catalyst heat treatment device, which includes a heating module for heat treating the catalyst, an air intake module and an air outlet module both connected to the heating module, the heating module includes a reactor for accommodating the catalyst and a heating device for heating the catalyst, the air intake module includes a reaction gas tank for providing a reaction gas with the catalyst, an inert gas tank for providing an inert gas and an air intake device, the reaction gas and the inert gas are mixed in the air intake device to form a mixed gas that enters the reactor, the air intake device is provided with a reaction gas intake probe for monitoring the intake concentration of the reaction gas in the air intake device, the mixed gas reacts with the catalyst in the reactor and enters the air outlet module, the air outlet module is provided with a reaction gas outlet probe for monitoring the outlet concentration of the reaction gas in the air outlet module.

[0007] In some embodiments, 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 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 disposed at the gas outlet of the reaction gas tank, and 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 of the reaction gas.

[0009] In some embodiments, the gas outlet of the inert gas tank is provided with a second flow meter, 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 flow of the inert gas.

[0010] In some embodiments, the catalyst heat treatment equipment further includes an oxygen gas tank storing oxygen, the oxygen gas tank is connected to the air intake device, and the oxygen can enter the reactor through the air intake device.

[0011] In some embodiments, a third flow meter is disposed at the gas outlet of the oxygen gas tank, and 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 flow of oxygen.

[0012] In some embodiments, an oxygen intake probe is provided in the air intake device, and the oxygen intake probe is used to monitor the oxygen intake concentration in the air intake device. The air outlet module is provided with an oxygen outlet probe, and the oxygen outlet probe is used to monitor 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 subjected to heat treatment, if oxygen penetration occurs due to poor equipment atmosphere protection measures or sealing failure, the oxygen inlet concentration or the oxygen outlet concentration will change, and the control module will control the second flowmeter 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 flowmeter and the second flowmeter to respectively reduce the flow rates of the reaction gas and the inert gas, and controls the third flowmeter to increase the oxygen flow rate, so as to gradually increase the oxygen intake concentration until the oxygen intake concentration monitored 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 in the reactor to monitor the temperature in the reactor in real time and send a temperature signal to the control module.

[0016] The catalyst heat treatment equipment of the present 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 the reaction gas in the mixed gas in real time, and judges whether the catalyst has completed the heat treatment according to the reaction gas inlet concentration and the reaction gas outlet concentration. In addition, the oxygen concentration in the mixed gas is also monitored by the oxygen inlet probe and the oxygen outlet probe to judge whether the catalyst heat treatment equipment has poor sealing and other phenomena that cause oxygen to enter the catalyst heat treatment equipment. In addition, the catalyst heat treatment equipment has a simple structure, can effectively heat treat the catalyst, and can be effectively connected with the front-end and back-end processes to facilitate the realization of production automation. BRIEF DESCRIPTION OF THE DRAWINGS

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

[0018] Figure 2 Schematic diagram of the structure of a catalyst heat treatment device according to an embodiment of the present invention.

[0019] Reference numerals:

[0020] Catalyst heat treatment equipment 100;

[0021] Control module 10; Heating module 20;

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

[0023] Intake module 30; reaction 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 tank 33; pressure reducing valve 331; third flow meter 332;

[0026] Air intake device 34; reaction 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 DESCRIPTION

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

[0030] The disclosure below provides many different embodiments or examples to implement different structures of the present invention. In order to simplify the disclosure of the present invention, the parts and settings of specific examples are described below. Of course, they are only examples, and the purpose is not to limit the present invention. In addition, the present invention can repeat reference numbers and / or letters in different examples. This repetition is for the purpose of simplicity and clarity, and does not itself indicate the relationship between the various embodiments and / or settings discussed. In addition, the present invention provides examples of various specific processes and materials, but those of ordinary skill in the art can appreciate the reusability of other processes and / or the use of other materials.

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

[0032] See also 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 intake module 30 and an air outlet module 40. The control module 10 is electrically connected to the heating module 20, the air intake module 30 and the air outlet module 40 to control the operation of the heating module 20, the air intake module 30 and the air outlet module 40. In this embodiment, the catalyst 200 is a Pt-M / C alloy catalyst, wherein M can be nickel, cobalt, iron, copper and chromium metal, and the control module 10 can be a PLC controller.

[0033] See also Figure 1 to Figure 2 The heating module 20 is used to heat treat the catalyst 200, and the heating module 20 includes a reactor 21, a heating device 22 and a temperature probe 23. The reactor 21 is provided with a cavity for accommodating the catalyst 200, the heating device 22 is provided at the bottom of the reactor 21 to heat the catalyst 200, and the temperature probe 23 is accommodated in the cavity to monitor the temperature in the reactor 21 in real time.

[0034] It can be understood that the heating device 22 and the temperature probe 23 are both electrically connected to the control module 10. That is, the control module 10 can control the heating device 22 to be turned on or off, and the temperature probe 23 can send the monitored temperature signal to the control module 10. Specifically, when the catalyst 200 is heat-treated, a temperature threshold is preset, and the temperature probe 23 monitors the temperature in the reactor 21 and transmits the temperature signal to the control module 10. When the control module 10 determines that the temperature is lower than the temperature threshold, it will control the heating device 22 to increase the heating power. When the control module 10 determines that the temperature is higher than the temperature threshold, it will control the heating device 22 to reduce the 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 through a pipeline 50 .

[0036] The reaction gas tank 31 stores a gas for reacting with the catalyst 200. In this embodiment, the reaction gas may be a reducing gas such as hydrogen. A pressure reducing valve 311 and a first flow meter 312 are provided at the gas outlet of the reaction gas tank 31. The pressure reducing valve 311 may 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. The control module 10 may 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 for protecting the catalyst. In this embodiment, the inert gas may be helium or other gases. A pressure reducing valve 321 and a second flow meter 322 are provided at the gas outlet of the inert gas tank 32. 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. The control module 10 can control the second flow meter 322 to increase or decrease the flow of the inert gas.

[0038] Oxygen is stored in the oxygen gas tank 33. A pressure reducing valve 331 and a third flow meter 332 are provided at the gas outlet of the oxygen gas tank 33. The pressure reducing valve 331 can reduce the gas pressure of oxygen in the pipeline 50. The third flow meter 332 is electrically connected to the control module 10. The control module 10 can control the third flow meter 332 to increase or decrease the flow of oxygen.

[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 send the mixed gas into the reactor 21 of the heating module 20 through the pipeline 50. The reaction gas intake probe 341 and the oxygen intake probe 342 are provided in the air intake device 34, and the reaction gas intake probe 341 and the oxygen intake probe 342 are both electrically connected to the control module 10. The reaction gas intake probe 341 is used to monitor the intake concentration of the reaction gas in the air intake device 34 in real time and send a signal to the control module 10, and the oxygen intake probe 342 is used to monitor the intake concentration of the 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 provided with an intake pressure gauge 343, and the intake pressure gauge 343 is used to monitor the intake pressure of the mixed gas from the air intake device 34 into the reactor 21 in real time.

[0040] The gas outlet module 40 is connected to the reactor 21 through the pipeline 50, and the mixed gas can be discharged from the reactor 21 into the gas outlet module 40. The gas outlet module 40 is provided with a reaction gas outlet probe 41 and an oxygen outlet probe 42, and the reaction gas outlet probe 41 and the oxygen outlet probe 42 are both electrically connected to the control module 10. The reaction gas outlet probe 41 is used to monitor the outlet concentration of the reaction gas in the gas outlet module 40 in real time and send a signal to the control module 10, and the oxygen outlet probe 42 is used to monitor the outlet concentration of the oxygen in the gas outlet module 40 in real time and send a signal to the control module 10. The gas outlet module 40 is also provided with a gas outlet pressure gauge 43, and the gas outlet pressure gauge 43 is used to monitor the outlet pressure of the mixed gas from the reactor 21 into the gas outlet module 40 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 reactor 21, and the control module 10 controls the first flow meter 312 and the second flow meter 322 to be opened, so that the reaction gas in the reaction gas tank 31 and the inert gas in the inert gas tank 32 respectively pass through the pressure reducing valve 321 and the pressure reducing valve 331 and enter the air intake device 34. The reaction gas and the inert gas are mixed in the air intake device 34 to form a mixed gas and enter the reactor 21 through the pipeline 50, and the air intake pressure gauge 343 monitors the air intake pressure of the mixed gas entering the reactor 21 from the air intake device 34 in real time.

[0042] When the mixed gas squeezes out the original air in the reactor 21, the control module 10 controls the heating device 22 to turn on to heat the catalyst 200, and the temperature probe 23 monitors the temperature in the reactor 21 in real time and transmits the temperature signal to the control module 10. The control module 10 judges the temperature signal and the preset temperature threshold to control the heating device 22 to increase or decrease the heating power, thereby maintaining the temperature in 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 a signal to the control module 10, and the reaction gas outlet probe 41 monitors the outlet concentration of the reaction gas in the outlet module 40 in real time and sends a signal to the control module 10, and the control module 10 compares the inlet concentration of the reaction gas with the outlet concentration of the reaction gas to determine whether the heat treatment of the catalyst 200 is completed. Specifically, when the outlet concentration of the reaction gas is less than the inlet concentration of the reaction gas, it means 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 flowmeter 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 means that the reaction gas no longer reacts with the catalyst, and the control module 10 determines that the catalyst 200 has completed the heat treatment. At this time, the control module 10 controls the heating device 22 to stop heating, and the first flow meter 312 turns off the reaction gas tank 31 to prevent the catalyst 200 from being overheated.

[0044] In addition, when the catalyst heat treatment equipment 100 is working, the oxygen intake probe 342 monitors the oxygen intake concentration in the intake device 34 in real time and sends a signal to the control module 10, and the oxygen outlet probe 42 monitors the oxygen outlet concentration in the outlet module 40 in real time and sends a signal to the control module 10. Once oxygen infiltration occurs due to factors such as poor equipment atmosphere protection measures or sealing failure, causing oxygen to enter the catalyst heat treatment equipment 100, the oxygen intake concentration and oxygen outlet concentration will change, and the control module 10 will control the second flowmeter 322 to increase the inert gas flow rate for purging according to the oxygen concentration data to reduce the oxygen concentration, thereby avoiding the problem of the catalyst 200 contacting oxygen during the heat treatment process.

[0045] After the heat treatment of the catalyst is completed, in order to prevent the catalyst 200 from having a violent oxidation reaction with oxygen in the air when it contacts the air during the removal process, resulting in the deterioration of the performance of the catalyst 200, the control module 10 controls the heating device 22 to be turned off after the heat treatment of the catalyst heat treatment equipment 100 of the present invention is completed, and after the temperature probe 23 monitors that the temperature in the reactor 21 drops to room temperature, the control module 10 controls the third flow meter 332 to be turned on, so that the oxygen in the oxygen gas tank 33 enters the reactor 21 through the air intake device 34. In this process, the control module 10 controls the first flowmeter 312 and the second flowmeter 322 to reduce the flow of reaction gas and inert gas, and controls the third flowmeter 332 to increase the oxygen flow. The oxygen intake concentration monitored by the oxygen intake probe 342 slowly increases until the oxygen intake concentration is equal to 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 intake concentration, the catalyst heat treatment equipment 100 can be opened to take out the catalyst 200, thereby avoiding the catalyst 200 from undergoing a violent oxidation reaction due to sudden contact with oxygen after heat treatment.

[0046] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected or indirectly connected through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0047] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example" or "some examples" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, unless they are contradictory.

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

Claims

1. A catalyst heat treatment device for heat treating a catalyst, characterized in that: The catalyst heat treatment equipment includes a heating module for heat treating the catalyst, an air intake module and an air outlet module both connected to the heating module, the heating module includes a reactor for accommodating the catalyst and a heating device for heating the catalyst, the air intake module includes a reaction gas tank for providing a reaction gas with the catalyst, an inert gas tank for providing an inert gas and an air intake device, the reaction gas and the inert gas are mixed in the air intake device to form a mixed gas that enters the reactor, the air intake device is provided with a reaction gas intake probe for monitoring the intake concentration of the reaction gas in the air intake device, the mixed gas reacts with the catalyst in the reactor and enters the air outlet module, the air outlet module is provided with a reaction gas outlet probe for monitoring the outlet concentration of the reaction gas in the air outlet module.

2. The catalyst heat treatment equipment according to claim 1, characterized in that: The catalyst heat treatment equipment also includes a control module. The reaction gas inlet probe sends a monitored reaction gas inlet concentration signal to the control module, and the reaction gas outlet probe sends a 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.

3. The catalyst heat treatment equipment according to claim 2, characterized in that: The gas outlet of the reaction gas tank is provided with a first flow meter, and 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 of the reaction gas.

4. The catalyst heat treatment equipment according to claim 3, characterized in that: The gas outlet of the inert gas tank is provided with a second flow meter, and 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 flow of the inert gas.

5. The catalyst heat treatment equipment according to claim 4, characterized in that: The catalyst heat treatment equipment also includes an oxygen gas tank storing oxygen, the oxygen gas tank is connected to the air intake device, and the oxygen can enter the reactor through the air intake device.

6. The catalyst heat treatment equipment according to claim 5, characterized in that: The gas outlet of the oxygen gas tank is provided with a third flow meter, and the third flow meter is electrically connected to the control module. The control module can control the third flow meter to increase or decrease the flow of oxygen.

7. The catalyst heat treatment equipment according to claim 6, characterized in that: The air intake device is provided with an oxygen intake probe, and the oxygen intake probe is used to monitor the oxygen intake concentration in the air intake device. The air outlet module is provided with an oxygen outlet probe, and the oxygen outlet probe is used to monitor the oxygen outlet concentration in the air outlet module.

8. The catalyst heat treatment equipment according to claim 7, characterized in that: The oxygen intake probe sends the monitored oxygen intake 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 subjected to heat treatment, if oxygen penetration occurs due to poor equipment atmosphere protection measures or sealing failure, the oxygen intake concentration or the oxygen outlet concentration will change, and the control module will control the second flowmeter to increase the inert gas flow rate for purging to reduce the oxygen concentration.

9. The catalyst heat treatment equipment according to claim 8, characterized in that: After the catalyst heat treatment is completed and before the catalyst is taken out, the control module controls the first flowmeter and the second flowmeter to reduce the flow rates of the reaction gas and the inert gas respectively, and controls the third flowmeter to increase the oxygen flow rate, so as to gradually increase the oxygen intake concentration until the oxygen intake concentration monitored by the oxygen intake probe reaches the oxygen concentration in the air.

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

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