Impregnation device for catalyst carriers and control method

Abstract

The application relates to the field of catalyst preparation and discloses a catalyst carrier impregnation device and a control method. The device comprises an impregnation bottle (1) for containing materials to be impregnated; a height adjusting rod (34) arranged beside the impregnation bottle and having a lifting plate (35) slidingly connected thereto; a fixed plug (33) for fixing a sensor integrated tube (2), a feeding pipe (3) and a emptying pipe (9) penetrating into the impregnation bottle and fixed to the lifting plate (35) on the side; a rotary sealing device (8) sleeved and rotationally connected to the outer circumferential side of the fixed plug and sealingly connected to the bottle mouth of the impregnation bottle to drive the impregnation bottle to rotate; and an electric heater (28) arranged at the bottom of the impregnation bottle, the top of the electric heater being provided with an inner concave spherical heating cavity matched with the impregnation bottle and used for regulating the temperature in the impregnation bottle in the impregnation process. The impregnation device can effectively solve the problems of metal aggregation and uneven distribution of active sites caused by temperature and pressure fluctuations and reduce the activity difference of catalyst batches.

Description

Technical Field

[0001] This invention relates to the field of catalyst preparation technology, specifically to an impregnation apparatus for a catalyst support, and also to a method for controlling the impregnation of a catalyst support. Background Technology

[0002] Chinese invention patent CN110961165B discloses an integrated device and method for catalyst impregnation and drying, and its application. This invention places the catalyst carrier in a carrier rotating disk (rotating horizontally), and sprays the impregnation liquid onto the carrier surface through an impregnation liquid atomizer. The carrier does not tumble up and down during the impregnation process, which is close to static impregnation. When a large number of carriers are impregnated, it is easy to be uneven. The impregnation process conditions (temperature, pressure) are not monitored in real time, resulting in poor repeatability of multiple batches of impregnation. It is not compatible with low-pressure and high-pressure impregnation functions.

[0003] Chinese invention patent CN102806109B discloses a continuous catalyst impregnation device and method. This invention conveys a carrier to the bottom of an impregnation liquid atomization system, and after impregnation, it is immediately conveyed to a dryer via a screw for drying. However, the material conveying speed, the impregnation liquid spraying speed, and the carrier impregnation time cannot be matched, and the carrier is easily damaged during the conveying process.

[0004] In the field of catalyst preparation, impregnation is a core process for loading active metals onto the porous structure of a support. It achieves metal ion adsorption and diffusion by immersing the support in a solution containing the active components. Traditional impregnation devices are susceptible to changes in ambient temperature and pore adsorption pressure, leading to uneven metal dispersion, localized agglomeration, and difficulty in precisely controlling the gradient distribution of multi-component metals, which can easily result in competitive adsorption effects. Existing impregnation processes often employ static impregnation or simple mechanical stirring, lacking real-time feedback adjustment mechanisms. This makes it impossible to dynamically optimize impregnation conditions and achieve uniform metal particle deposition. Especially under high-precision conditions, the diffusion rate of the solution within the support pores and the metal salt deposition kinetics are difficult to match, resulting in uneven distribution of catalyst active sites and affecting catalytic efficiency and selectivity.

[0005] The existing technology has the following drawbacks: 1. Low process control precision: Traditional impregnation equipment relies on constant temperature baths or manual pressure adjustment, which cannot achieve dynamic and precise control of temperature and pressure during the impregnation process. This leads to an imbalance between the diffusion rate and deposition rate of metal ions in the carrier channels, which can easily cause metal particle agglomeration and uneven distribution of active sites, resulting in significant performance differences between batches of catalysts.

[0006] 2. Defects of multi-component impregnation and competitive adsorption: Existing single-impregnation processes cannot accurately control the gradient distribution of multi-component metals. In high-concentration metal salt solutions, different ions compete for adsorption, resulting in preferential deposition of low surface energy metals and shielding of high surface energy metals. This leads to low utilization rate and poor selectivity of active components.

[0007] 3. Lack of real-time feedback and dynamic optimization: Conventional equipment cannot monitor process parameters during impregnation and cannot accurately match diffusion-deposition kinetics, resulting in a lack of effective control measures for the impregnation process and an inability to meet the requirements of high-requirement impregnation scenarios.

[0008] 4. Unstable repeated preparation: Traditional static impregnation or mechanical stirring impregnation processes require multiple impregnation-drying cycles and are subject to human operation errors, which directly leads to low product qualification rate and makes it difficult to meet the production requirements of high-performance catalysts.

[0009] Therefore, constructing a precision control system for the impregnation process, rapidly and dynamically adjusting the impregnation temperature and pressure, and combining it with a step-by-step impregnation strategy to achieve uniform layer-by-layer loading of multi-component metals is a research direction for developing high-precision impregnation processes. Summary of the Invention

[0010] The purpose of this invention is to overcome the above-mentioned problems existing in the prior art and to provide an impregnation device and control method for a catalyst support. The impregnation device for the catalyst support completely solves the problems of metal agglomeration and uneven distribution of active sites caused by temperature and pressure fluctuations in the traditional process, and the difference in activity between batches of catalysts is greatly reduced. By setting a rotary sealing device, the temperature uniformity of the material to be impregnated is significantly improved.

[0011] To achieve the above objectives, the present invention provides an impregnation apparatus for a catalyst support, comprising: Impregnation bottles are used to hold materials to be impregnated. A rotary sealing device that is sealed to the mouth of the impregnation bottle; A fixed plug is installed on the rotary sealing device and is fixed with a sensor integrated tube, a feed tube and a vent tube that penetrate into the impregnation bottle. A pressure regulating component for adjusting the impregnation pressure is provided at the inlet of the feed tube. Gas in the impregnation bottle can be discharged through the vent tube. The rotary sealing device can be driven to rotate the impregnation bottle relative to the fixed plug. A height adjustment mechanism, comprising a height adjustment rod and a lifting plate slidably connected to the height adjustment rod, wherein a fixed plug is fixed to the lifting plate to enable the rotary sealing device and the impregnation bottle to move up and down along the height adjustment rod; and An electric heater is provided at the bottom of the impregnation bottle, and its top has a concave spherical heating cavity adapted to the impregnation bottle, which is used to regulate the temperature inside the impregnation bottle during the impregnation process.

[0012] Preferably, an intelligent control module is connected to the top of the sensor integrated tube, and the intelligent control module is electrically connected to a display control module to allow input of parameters required for the impregnation process through the display control module.

[0013] Preferably, the outlet of the feed pipe extends into the impregnation bottle and is equipped with an atomizing nozzle, the inlet of the feed pipe is connected to an impregnation liquid storage tank via a pipeline, and a one-way valve and a precision impregnation liquid feed pump are sequentially installed in the downstream pipeline of the impregnation liquid storage tank.

[0014] Preferably, the pressure regulating assembly includes a first compressed air inlet pipe branching off from the feed pipe at a position downstream of the precision impregnation liquid feed pump, and an air valve is provided on the first compressed air inlet pipe; a second compressed air inlet pipe is branched off from the pipeline between the precision impregnation liquid feed pump and the one-way valve, and a pipeline purge valve is provided on the second compressed air inlet pipe.

[0015] Preferably, the outlet of the vent pipe extends out of the impregnation bottle and is connected to a precision pressure control valve. The two outlets of the precision pressure control valve are respectively connected to a vent pipe and a vacuum pump exhaust port. A vacuum pump body is installed on the pipeline between the vacuum pump exhaust port and the precision pressure control valve.

[0016] Preferably, the device also includes a drive motor mounted on the lifting plate, the output shaft of the drive motor is equipped with a drive gear, and an external gear ring is fixedly fitted on the outer side wall of the rotary sealing device, the drive gear meshing with the external gear ring for transmission.

[0017] Preferably, the system also includes a support base and an electric push rod mounted on the support base, with the lower end of the height adjustment rod fixed to the support base and the telescopic end of the electric push rod connected to the lifting plate.

[0018] Preferably, the device further includes a ground glass rotating sleeve fixed inside the rotary sealing device. The mouth of the immersion bottle is inserted into the outer periphery of the ground glass rotating sleeve and fastened by a snap fastener, so that the rotary sealing device is sealed to the mouth of the immersion bottle and can drive the immersion bottle to rotate.

[0019] A second aspect of the present invention provides a method for controlling the impregnation of a catalyst support, comprising the following steps: Step S100: Fill the impregnation bottle with a certain amount of material to be impregnated, tilt the impregnation bottle and adjust the height of the impregnation bottle. Step S200: Install the bottom of the impregnation bottle onto the electric heater and adjust the rotation speed of the impregnation bottle; Step S300: Set the parameters of the total feed volume, feed time, pressure and heating temperature of the impregnation bottle; Step S400: Control the feeding of the impregnation liquid according to the set total feeding amount and feeding time, and spray the impregnation liquid evenly onto the surface of the material to be impregnated. Step S500: Control the air intake in the impregnation bottle through the air valve on the first compressed air inlet pipe, and intelligently regulate the air intake volume; Step S600: The gas from the impregnation bottle is discharged through the vent pipe and switched to atmospheric pressure venting or venting through the vacuum pump body via a precision pressure control valve. Step S700: After the impregnation liquid is sprayed, the impregnation liquid in the pipeline is blown into the impregnation bottle through the pipeline purge valve on the second compressed air inlet pipe, and the pressure of the impregnation bottle is controlled to be stable. Step S800: Remove the lower impregnation bottle, pour out the impregnated material, and then put the impregnation bottle back into its original position.

[0020] Preferably, step S710 is further included between step S700 and step S800: adjusting the heating temperature, air purging rate and exhaust rate of the impregnation bottle, drying the material to be impregnated in the first impregnation, and adding a second impregnation solution for a second impregnation.

[0021] The above technical solution enables real-time pressure regulation of the impregnation process in the impregnation bottle by using a pressure regulating component installed at the inlet of the feed pipe, and temperature regulation of the impregnation process in the impregnation bottle by using an electric heater. This completely solves the problems of metal agglomeration and uneven distribution of active sites caused by temperature and pressure fluctuations in traditional processes, and significantly reduces the batch-to-batch activity difference of catalysts. By setting up a rotary sealing device, the temperature uniformity of the material to be impregnated is significantly improved. Attached Figure Description

[0022] Figure 1 This is a structural diagram of an impregnation apparatus for a catalyst support according to one embodiment of the present invention; Explanation of reference numerals in the attached figures 1-Immersion bottle; 2-Sensor integrated tube; 3-Feed pipe; 4-Atomizing nozzle; 5-Material to be impregnated; 6-Ground glass rotating sleeve; 7-Snap fastener; 8-Rotary sealing device; 9-Vacuum pipe; 10-Support base; 11-Support lifting button; 12-Rotary speed control button; 13-Precision pressure control valve; 14-Vacuum pump body; 15-Vacuum pipe; 16-Vacuum pump exhaust port; 17-Air valve; 18-First compressed air inlet pipe ; 19-Precision impregnation liquid feed pump; 20-One-way valve; 21-Impregnation liquid storage tank; 22-Pipeline purge valve; 23-Second compressed air inlet pipe; 24-Intelligent control module; 25-Display control module; 26-Integrated control box; 27-Control signal line; 28-Electric heater; 29-Electric push rod; 30-External gear ring; 31-Drive gear; 32-Drive motor; 33-Fixing plug; 34-Height adjustment rod; 35-Lifting plate. Detailed Implementation

[0023] The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0024] See Figure 1As shown, an impregnation device for a catalyst carrier according to the present invention includes: an impregnation bottle 1, a height adjusting rod 34, a fixing plug 33, a rotary sealing device 8, a sensor integrated tube 2, a feed pipe 3, an vent pipe 9, and an electric heater 28. The impregnation bottle 1 is used to hold the material to be impregnated 5, and the volume of the material 5 inside is approximately one-third of the full bottle, the specific volume being determined according to the range of the impregnation liquid spray. The height adjusting rod 34 is disposed beside the impregnation bottle 1 and a lifting plate 35 is slidably connected to it. The height adjusting rod 34 can be a vertical rod structure, with its lower end fixedly disposed. The lifting plate 35 is slidably connected to the height adjusting rod 34 via a slide rail or a sleeve. The lifting and lowering of the lifting plate 35 is driven by a linear reciprocating drive device, which can be any one of a hydraulic cylinder, a pneumatic cylinder, or an electric push rod. The fixing plug 33 is used to fix the sensor integrated tube 2, the feed pipe 3, and the vent pipe 9 inserted into the impregnation bottle 1, and its side is fixed to the lifting plate 35. Specifically, the side of the fixed plug 33 is provided with a branch that is vertically fixed to the lifting plate 35. The forward-extending end of the branch is provided with a cylindrical plug that matches the mouth of the immersion bottle 1. The branch and the cylindrical plug form an L-shaped bending structure. The sensor integrated tube 2, the feed tube 3, and the drain tube 9 are all inserted into the cylindrical plug. The inlet of the feed tube 3 is provided with a pressure regulating component for adjusting the immersion pressure and is connected to the immersion liquid storage tank 21. The drain tube 9 can realize venting. The rotary sealing device 8 is sleeved and rotatably connected to the outer periphery of the cylindrical plug of the fixed plug 33 and is sealed to the mouth of the immersion bottle 1 to drive the immersion bottle 1 to rotate. The outer diameter of the rotary sealing device 8 is smaller than the length of the branch that constitutes the fixed plug 33 to avoid structural interference between the rotary sealing device 8 and the lifting plate 35 when the rotary sealing device 8 is installed. The rotary sealing device 8 is connected to the drive device through a transmission mechanism. The drive device can be a motor or an electric motor. An electric heater 28 is located at the bottom of the immersion bottle 1, and its top has a concave spherical heating cavity adapted to the immersion bottle 1. Heating tubes are evenly distributed on the bottom surface of the concave spherical heating cavity. The electric heater 28 is used to regulate the temperature inside the immersion bottle 1 during the immersion process.

[0025] In the above embodiments, the height of the impregnation bottle 1 is adjusted in real time by the lifting plate 35 set on the height adjustment rod 34, so as to realize the disassembly and replacement of the impregnation bottle 1 after impregnation and meet the needs of materials to be impregnated with different capacities. The pressure adjustment component set at the inlet of the feed pipe 3 realizes the real-time adjustment of the pressure in the impregnation process in the impregnation bottle 1, and the temperature of the impregnation process in the impregnation bottle 1 is adjusted by the electric heater 28, which completely solves the problems of metal agglomeration and uneven distribution of active sites caused by temperature and pressure fluctuations in traditional processes, and significantly reduces the batch activity difference of catalysts. By setting the rotary sealing device 8, the material to be impregnated 5 is turned over and heated by rotating the impregnation bottle 1, which significantly improves the temperature uniformity of the material to be impregnated 5.

[0026] See Figure 1 As shown, in a preferred embodiment of the present invention, an intelligent control module 24 is connected to the top of the sensor integrated tube 2. The intelligent control module 24 is electrically connected to a display control module 25, allowing the input of parameters required for the impregnation process via the display control module 25. Specifically, the intelligent control module 24 is a PLC controller or a microcontroller controller. Temperature sensors, pressure sensors, humidity sensors, and other sensors are installed at the end of the sensor integrated tube 2 located inside the impregnation bottle 1 to monitor parameters such as temperature, pressure, and humidity inside the impregnation bottle 1 in real time and transmit these parameters to the display control module 25 for display. This facilitates the user in adjusting relevant parameters according to the actual working conditions inside the impregnation bottle 1. The intelligent control module 24 is electrically connected to various electronic components via control signal lines 27. The display control module 25 can be a touch screen, using systems such as Android or Windows. By setting up the intelligent control module 24 and the display control module 25, the intelligence and automation level of the entire device is significantly improved, greatly reducing labor costs.

[0027] See Figure 1 As shown, in a preferred embodiment of the present invention, the outlet of the feed pipe 3 extends into the impregnation bottle 1 and is equipped with an atomizing nozzle 4. The atomizing nozzle 4 has several spray holes. To expand the spray area and coverage of the atomizing nozzle 4, it can be configured as a spherical structure with several spray holes. The inlet of the feed pipe 3 is connected to an impregnation liquid storage tank 21 via a pipeline. The impregnation liquid storage tank 21 is used to store the impregnation liquid. A one-way valve 20 and a precision impregnation liquid feed pump 19 are sequentially installed in the downstream pipeline of the impregnation liquid storage tank 21. During operation, the precision impregnation liquid feed pump 19 is electrically connected to the intelligent control module 24 via a control signal line 27. It controls the feed flow rate and velocity of the impregnation liquid according to the feed quantity and feed time set by the display control module 25. The one-way valve 20 is used to prevent backflow of liquid in the feed pipe 3. The atomizing nozzle 4 significantly improves the uniformity of the impregnation liquid spray. By setting up a precision impregnation liquid feed pump 19, high-precision input control of the impregnation liquid is achieved, avoiding waste of impregnation liquid during operation.

[0028] See Figure 1As shown, in a preferred embodiment of the present invention, the pressure regulating component includes a first compressed air inlet pipe 18 branching off from the feed pipe 3 downstream of the precision impregnation liquid feed pump 19. An air valve 17 is installed on the first compressed air inlet pipe 18. The air valve 17 is a solenoid valve and is electrically connected to the intelligent control module 24 via a control signal line 27. The air intake through the air valve 17 is detected by a pressure sensor in the sensor integrated pipe 2, which monitors the real-time pressure inside the impregnation bottle 1 and feeds it back to the intelligent control module 24 for intelligent regulation. This configuration enables intelligent control of the air intake, improving the automation level of the device.

[0029] In the above embodiment, the pressure regulating component further includes a second compressed air inlet pipe 23 branched off from the precision impregnation liquid feed pump 19 and the one-way valve 20. A pipeline purge valve 22 is installed on the second compressed air inlet pipe 23. The pipeline purge valve 22 is a solenoid valve and is electrically connected to the intelligent control module 24 via a control signal line 27. During operation, when the impregnation liquid is sprayed, compressed air enters the pipeline purge valve 22 through the second compressed air inlet pipe 23, purging the impregnation liquid in the pipeline into the impregnation bottle 1. Simultaneously, the intelligent control module 24 maintains stable pressure within the impregnation bottle 1 based on real-time feedback from the pressure sensor in the sensor integration pipe 2.

[0030] See Figure 1 As shown, in a preferred embodiment of the present invention, the outlet of the vent pipe 9 extends out of the impregnation bottle 1 and is connected to a precision pressure control valve 13. Specifically, the precision pressure control valve 13 is a three-way solenoid valve with one inlet and two outlets. The inlet end is connected to the outlet of the vent pipe 9, and the two outlets of the precision pressure control valve 13 are respectively connected to a vent pipe 15 and a vacuum pump exhaust port 16. A vacuum pump body 14 is installed on the pipeline between the vacuum pump exhaust port 16 and the precision pressure control valve 13. The vacuum pump body 14 and the precision pressure control valve 13 are electrically connected to the intelligent control module 24 via a control signal line 27.

[0031] In the above embodiment, during operation, when atmospheric pressure impregnation is required, the pipeline connected to the vent pipe 15 of the precision pressure control valve 13 is open and the vacuum pump body 14 is turned off, achieving atmospheric pressure impregnation; when vacuum impregnation is required, the pipeline connected to the vacuum pump body 14 of the precision pressure control valve 13 is open and the vacuum pump body 14 is turned on, achieving vacuum impregnation. Through the above structural design, on-demand switching between atmospheric pressure impregnation and vacuum impregnation is achieved, greatly improving the versatility of the device and meeting impregnation requirements under different pressures. Relying solely on the switching control of the precision pressure control valve 13 significantly reduces the cost of having two separate sets of equipment required to achieve the two impregnation processes.

[0032] See Figure 1As shown, in a preferred embodiment of the present invention, a drive motor 32 is further included, mounted on the lifting plate 35. The motor housing of the drive motor 32 is fixed to the vertical side of the lifting plate 35 by bolts and a connecting base. The output shaft of the drive motor 32 is keyed to a drive gear 31. An external gear ring 30 is fitted and fixed to the outer wall of the rotary sealing device 8, and the drive gear 31 meshes with the external gear ring 30 for transmission. To improve the stability and accuracy of the meshing transmission, the tooth profiles of the drive gear 31 and the external gear ring 30 are helical or spiral.

[0033] See Figure 1 As shown, in a preferred embodiment of the present invention, it further includes a support base 10 and an electric push rod 29 mounted on the support base 10. The lower end of the height adjustment rod 34 is fixed on the support base 10. The support base 10 is a circular plate structure. The fixed end of the electric push rod 29 is mounted on the support base 10 through bolts and a flange. The telescopic end of the electric push rod 29 is connected to the lifting plate 35.

[0034] In the above embodiment, to adjust the lifting height of the impregnation bottle 1 according to actual needs, a support lifting button 11 is provided on the support base 10. The support lifting button 11, the electric push rod 29, and the intelligent control module 24 form a closed-loop circuit. The extension and retraction of the telescopic end of the electric push rod 29 are operated by the support lifting button 11, thereby realizing the raising or lowering of the lifting plate 35. Then, through the drive of the fixed plug 33, the rotation sealing device 8 and the impregnation bottle 1 installed on it are raised and lowered. When the system needs to be cleaned after impregnation, the impregnation bottle 1 is raised to detach it from the electric heater 28 and removed. After the impregnated material is poured out, the impregnation bottle 1 is installed on the rotation sealing device 8 and lowered into the top heating chamber of the electric heater 28. Through the above settings, manual operation is effectively saved, eliminating the need for manual lifting of the impregnation bottle 1 for replacement, reducing the difficulty of operation, improving the degree of automation, and greatly reducing labor costs.

[0035] In the above embodiment, in order to control the speed of the drive motor 32, a rotary speed adjustment button 12 is provided on the bracket base 10. The rotary speed adjustment button 12, the drive motor 32 and the intelligent control module 24 form a closed loop circuit. By rotating the rotary speed adjustment button 12 clockwise or counterclockwise, the speed of the drive motor 32 can be controlled, so that the material in the impregnation bottle 1 can be turned at different speeds during use, thereby significantly improving the reaction efficiency between the material to be impregnated 5 and the sprayed impregnation liquid.

[0036] See Figure 1As shown, in a preferred embodiment of the present invention, a ground glass rotating sleeve 6 is further included within the rotating sealing device 8. The ground glass rotating sleeve 6 has a circular structure. The mouth of the immersion bottle 1 is inserted into the outer periphery of the ground glass rotating sleeve 6 and secured by a buckle 7. A sealing ring is provided at the connection between the outer ring of the mouth of the immersion bottle 1 and the inner ring of the ground glass rotating sleeve 6, thereby ensuring the airtightness of the immersion bottle 1 during connection. In the above embodiment, the buckle 7 can be in the form of a clamp, with its lower edge of the circular structure fitted and fixed to the mouth of the immersion bottle 1, and its upper edge of the circular structure fitted and fixed to the ground glass rotating sleeve 6. By setting the fixing form of the buckle 7, the quick disassembly and replacement of the immersion bottle 1 is realized, and the fixing requirements of immersion bottles 1 with different diameters can be met. Through the above settings, the quick replacement of the immersion bottle 1 is realized, improving the replacement efficiency.

[0037] In the above embodiment, to facilitate quick and easy movement of the electric heater 28, multiple sets of self-locking casters are provided at the bottom of the electric heater 28. When it is necessary to move the electric heater 28, the movement is achieved by unlocking the self-locking casters. The electric heater 28 is electrically connected to the intelligent control module 24 via the control signal line 27, thereby realizing intelligent control of the electric heater 28 and meeting the adjustment requirements of different temperatures.

[0038] To protect the various electrical components, an integrated control box 26 is also provided. The intelligent control module 24, precision impregnation liquid feed pump 19, pipeline purge valve 22, check valve 20, precision pressure control valve 13, vacuum pump body 14, etc., are all housed within the integrated control box 26. The display control module 25 is embedded on the outer surface of the integrated control box 26. Through these measures, protection is achieved for each electrical component, effectively extending their service life.

[0039] The present invention also provides a method for controlling the impregnation of a catalyst support, comprising the following steps: Step S100: Fill the impregnation bottle 1 with a fixed amount of material 5 to be impregnated. The amount of material 5 to be impregnated should be within the coverage area of ​​the atomizing nozzle 4. Set the impregnation bottle 1 at an angle and insert it into the ground glass rotating sleeve 6 and lock it with a buckle. Fix the sensor integrated tube 2, feed tube 3 and drain tube 9 in the fixing plug 33 and carefully insert them into the impregnation bottle 1. Drive the lifting plate 35 up and down by the electric push rod 29 to adjust the height of the impregnation bottle 1. At this time, the impregnation bottle 1 is fixed at an angle. When the impregnation bottle 1 is rotated, the material 5 to be impregnated can be fully turned over. Step S200: Place the electric heater 28, install the bottom of the impregnation bottle 1 on the electric heater 28, turn on the rotation speed control button 12 and adjust the rotation speed of the impregnation bottle 1 to a suitable speed, turn on the power of the integrated control box 26, and power on each module. Step S300: After the system self-test is normal, set the parameters of total feed amount, feed time, pressure and heating temperature of the impregnation bottle 1 on the display control module 25. After the system parameters are set, each module of the system can run automatically. Step S400: Pour the impregnation liquid into the impregnation liquid storage tank 21. The precision impregnation liquid feed pump 19 controls the feeding of the impregnation liquid according to the set total feeding amount and feeding time. After passing through the feed pipe 3 and the atomizing nozzle 4, the impregnation liquid is evenly sprayed onto the surface of the material to be impregnated 5. Step S500: The air intake in the impregnation bottle 1 is controlled by the air valve 17 on the first compressed air inlet pipe 18, and the air intake volume is intelligently regulated by the intelligent control module 24 through the pressure sensor set on the sensor integrated pipe 2. In step S600, the gas from the impregnation bottle 1 is discharged through the vent pipe 9 and switched to atmospheric pressure venting via the precision pressure control valve 13 for atmospheric pressure impregnation, or switched to venting via the vacuum pump body 14 for vacuum impregnation. Step S700: After the impregnation liquid is sprayed, the impregnation liquid in the pipeline is blown into the impregnation bottle 1 through the pipeline purge valve 22 on the second compressed air inlet pipe 23. At the same time, the intelligent control module 24 controls the pressure of the impregnation bottle 1 to stabilize. After the impregnation liquid spraying and purging are completed, the system is controlled by the intelligent control module 24 to run according to the set pressure, temperature, impregnation time and other programs. Step S710: If a second impregnation is required, i.e., distributed impregnation, the heating temperature, air purging volume and exhaust volume of the electric heater 28 can be adjusted by the intelligent control module 24. The material to be impregnated 5 in the first impregnation is dried according to the process requirements, and the second impregnation liquid is added to the impregnation liquid storage tank 21 to complete the second impregnation. Step S800: When the display control module 25 confirms that the impregnation is completed, remove the impregnation bottle 1, pour out the impregnated material, put the impregnation bottle 1 back into its original position, click the display control module 25 to automatically start the cleaning program, add deionized water to the impregnation liquid storage tank 21, and the system controls the feed pipe 3, precision impregnation liquid feed pump 19, first compressed air inlet pipe 18, second compressed air inlet pipe 23, vent pipe 15 and vacuum pump exhaust port 16 to carry out system cleaning and purging.

[0040] The advantages of the above-described implementation method over the prior art are mainly as follows: 1. Precise dynamic control of temperature and pressure in impregnation process: Multiple test modules can be added through sensor integrated tube 2; Compared with the crude control of traditional constant temperature bath and manual pressure adjustment, this invention improves the matching degree of diffusion-deposition kinetics of metal ions in the carrier channels, and the particle size distribution is uniform. It completely solves the problems of metal agglomeration and uneven distribution of active sites caused by temperature and pressure fluctuations in traditional processes, and the difference in catalyst batch activity is greatly reduced.

[0041] 2. Stepwise impregnation and gradient control strategy: It can realize the stepwise impregnation process of multi-components. By intelligently adjusting parameters such as solution concentration gradient, impregnation time and temperature and pressure, it can achieve the layer-by-layer uniform loading of multi-component metals and the construction of core-shell gradient structure. It supports the customized gradient distribution design of multi-component metals, avoids competitive adsorption, and improves the utilization rate of active components.

[0042] 3. High batch production repeatability and scalability: Through the collaborative optimization of real-time monitoring systems and machine learning algorithms, a precise and controllable multi-stage continuous preparation system is constructed. This technology enables digital and standardized control of impregnation process parameters, ensuring batch-to-batch consistency of catalyst performance parameters (such as activity and selectivity), and meeting the requirements for low-cost and high-stability preparation of high-performance catalysts.

[0043] In the description of this invention, the terms "first," "second," "front," "rear," "upper," and "lower" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0044] The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various specific technical features in any suitable manner. To avoid unnecessary repetition, the present invention will not describe the various possible combinations separately. However, these simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.

Claims

1. An impregnation apparatus for a catalyst support, characterized in that, include: Impregnation bottle (1), used to hold the material to be impregnated (5); A rotary sealing device (8) is provided, which is connected to the mouth of the immersion bottle (1) in a sealed manner. A fixed plug (33) is installed on the rotary sealing device (8) and is fixed with a sensor integrated tube (2), a feed pipe (3) and a drain pipe (9) that penetrate into the impregnation bottle (1). A pressure regulating component for adjusting the impregnation pressure is provided at the inlet of the feed pipe (3). The gas in the impregnation bottle (1) can be discharged through the drain pipe (9). The rotary sealing device (8) can be driven to rotate the impregnation bottle (1) relative to the fixed plug (33). The height adjustment mechanism includes a height adjustment rod (34) and a lifting plate (35) slidably connected to the height adjustment rod (34), and the fixing plug (33) is fixed to the lifting plate (35) so as to drive the rotary sealing device (8) and the immersion bottle (1) to rise and fall along the height adjustment rod (34); as well as An electric heater (28) is provided at the bottom of the impregnation bottle (1), and its top is provided with a concave spherical heating cavity adapted to the impregnation bottle (1) for regulating the temperature inside the impregnation bottle (1) during the impregnation process.

2. The impregnation apparatus for the catalyst support according to claim 1, characterized in that, The top of the sensor integrated tube (2) is connected to an intelligent control module (24), which is electrically connected to a display control module (25) to allow the input of parameters required for the impregnation process through the display control module (25).

3. The impregnation apparatus for the catalyst support according to claim 1, characterized in that, The outlet of the feed pipe (3) extends into the impregnation bottle (1) and is equipped with an atomizing nozzle (4). The inlet of the feed pipe (3) is connected to the impregnation liquid storage tank (21) through a pipeline. The downstream pipeline of the impregnation liquid storage tank (21) is equipped with a one-way valve (20) and a precision impregnation liquid feed pump (19) in sequence.

4. The impregnation apparatus for the catalyst support according to claim 3, characterized in that, The pressure regulating assembly includes a first compressed air inlet pipe (18) branching off from the feed pipe (3) at a position downstream of the precision impregnation liquid feed pump (19), and an air valve (17) provided on the first compressed air inlet pipe (18); a second compressed air inlet pipe (23) branching off from the pipeline between the precision impregnation liquid feed pump (19) and the check valve (20), and a pipeline purge valve (22) provided on the second compressed air inlet pipe (23).

5. The impregnation apparatus for the catalyst support according to claim 1, characterized in that, The outlet of the vent pipe (9) extends out of the immersion bottle (1) and is connected to a precision pressure control valve (13). The two outlets of the precision pressure control valve (13) are respectively connected to a vent pipe (15) and a vacuum pump exhaust port (16). A vacuum pump body (14) is installed on the pipeline between the vacuum pump exhaust port (16) and the precision pressure control valve (13).

6. The impregnation apparatus for the catalyst support according to claim 1, characterized in that, It also includes a drive motor (32) installed on the lifting plate (35), the output shaft of the drive motor (32) is equipped with a drive gear (31), and an outer gear ring (30) is fixedly fitted on the outer side wall of the rotary sealing device (8), and the drive gear (31) meshes with the outer gear ring (30) for transmission.

7. The impregnation apparatus for the catalyst support according to claim 1, characterized in that, It also includes a support base (10) and an electric push rod (29) mounted on the support base (10). The lower end of the height adjustment rod (34) is fixed on the support base (10), and the telescopic end of the electric push rod (29) is connected to the lifting plate (35).

8. The impregnation apparatus for the catalyst support according to claim 1, characterized in that, It also includes a ground glass rotating sleeve (6) fixed inside the rotating sealing device (8), the mouth of the immersion bottle (1) is inserted into the outer periphery of the ground glass rotating sleeve (6) and fastened by a buckle (7) so that the rotating sealing device (8) is sealed to the mouth of the immersion bottle (1) and can drive the immersion bottle (1) to rotate.

9. A method for controlling the impregnation of a catalyst support, characterized in that, Includes the following steps: Step S100: Fill the impregnation bottle (1) with a certain amount of material (5) to be impregnated, tilt the impregnation bottle (1) and adjust the height of the impregnation bottle (1); Step S200: Install the bottom of the impregnation bottle (1) on the electric heater (28) and adjust the rotation speed of the impregnation bottle (1); Step S300: Set the parameters of the total feed volume, feed time, pressure and heating temperature of the impregnation bottle (1); Step S400: Control the feeding of the impregnation liquid according to the set total feeding amount and feeding time, and spray the impregnation liquid evenly onto the surface of the material to be impregnated (5); Step S500: Control the air intake in the impregnation bottle (1) through the air valve (17) on the first compressed air inlet pipe (18) to intelligently regulate the air intake volume; Step S600: The gas from the impregnation bottle (1) is discharged through the vent pipe (9) and switched to atmospheric pressure venting or venting through the vacuum pump body (14) via the precision pressure control valve (13). Step S700: After the impregnation liquid is sprayed, the impregnation liquid in the pipeline is blown into the impregnation bottle (1) through the pipeline purge valve (22) on the second compressed air inlet pipe (23), and the pressure of the impregnation bottle (1) is controlled to be stable. Step S800: Remove the lower impregnation bottle (1), pour out the impregnated material, and then put the impregnation bottle (1) back into its original position.

10. The method for controlling the impregnation of the catalyst support according to claim 9, characterized in that, Between steps S700 and S800, there is also step S710, which involves adjusting the heating temperature, air purging rate and exhaust rate of the impregnation bottle (1), drying the material to be impregnated (5) for the first impregnation, and adding a second impregnation solution for the second impregnation.

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