A system for the mass production and homogeneous preparation of high-loading catalysts and its application method

Abstract

This invention relates to a system and method for the large-scale, uniform preparation of high-loading catalysts. The apparatus is suitable for the engineering development and large-scale, uniform preparation of high-loading (above 20 wt.%) catalysts, enabling single-tube, kilogram-level batch preparation. It provides stable control of batch production conditions, stable process parameters, and ensures uniform dispersion of the high-loading active metal and consistent batch quality. This catalyst preparation apparatus is applied to the development, large-scale production, and engineering applications of high-loading catalysts for liquid propellant decomposition.

Description

Technical Field

[0001] This invention relates to the field of catalytic decomposition technology for aerospace propulsion chemical propellants, specifically a high-loading catalyst batch scale-up uniform preparation system and its application. This catalyst preparation system enables rapid and stable batch uniform preparation of high-loading metal catalysts, controls the uniformity of active metal loading, achieves kilogram-level batch scale-up preparation of high-loading catalysts, and ensures consistency in catalyst batch production. Background Technology

[0002] Catalysts used in traditional chemical industries have low active metal content and are mainly prepared by impregnation, deposition precipitation, sol-gel methods, etc. The carriers involved are mainly conventional activated carbon, titanium dioxide, zinc oxide, aluminum oxide, etc. Their main applications are in chemical fields such as electrochemical hydrogen evolution, ammonia synthesis, Fischer-Tropsch synthesis, and hydrogenation reactions.

[0003] Existing technologies lack methods for large-scale production of catalysts, particularly for those with high loading capacities. For instance, compared to traditional chemical catalysts, ruthenium-based catalysts used in aerospace propulsion require high ruthenium content, uniform activity, and consistent batch quality. Due to the physical properties of the ruthenium active metal precursor solution, achieving highly uniform dispersion and loading of active components in ruthenium metal nanoparticles is difficult. Traditional preparation equipment cannot control the uniform loading of high-content ruthenium metal. Therefore, there is an urgent need for a large-scale, uniformly scaled-up system and process for high-loading catalysts, capable of stable batch production of high-content ruthenium-based aerospace catalysts to meet the needs of aerospace engineering applications. Summary of the Invention

[0004] The present invention addresses the problem that existing devices and technologies cannot reliably achieve the uniform scale-up preparation of highly loaded catalysts. The purpose of this invention is to provide a batch uniform scale-up preparation system and application for aerospace catalysts with nanoscale uniform dispersion of highly loaded metal active components, so as to achieve uniform dispersion of highly loaded active metals and good consistency in batch preparation.

[0005] To achieve the above objectives, the present invention adopts the following technical process solution:

[0006] A high-loading catalyst batch scale-up uniform preparation system is provided, comprising an impregnation and drying device and a tube furnace; the impregnation and drying device includes an impregnation reaction unit, an tilt control unit, a rotation control unit and a visible microwave heating unit, used to complete the impregnation and drying process of catalyst preparation, and the tube furnace is used to complete the calcination-level reduction and activation process of catalyst preparation.

[0007] The tilt control unit and the rotation control unit can drive the impregnation reaction unit to tilt and rotate, respectively, so that the active components of the catalyst are uniformly and fully loaded onto the carrier; the visible microwave heating unit dries the catalyst material in the impregnation reaction unit through the combined action of microwaves and inert gas.

[0008] Furthermore, the impregnation reaction unit includes an impregnator 9 and a filter sieve plate 14. The impregnator 9 is used to provide the required environment for the precursor solution to impregnate the carrier. An air inlet 7 is provided at the top of the impregnator 9 and connected to an air inlet pipe. An air outlet is provided at the bottom of the impregnator 9 and connected to an air outlet pipe. The filter sieve plate 14 is provided at the bottom inside the impregnator 9 and is used to intercept the carrier during the impregnation and drying process to avoid clogging the air inlet 7 and the air outlet. The impregnator 9 is connected to the inclined frame 24 and can not only tilt with the inclined frame 24, but also rotate within the inclined frame 24.

[0009] Furthermore, the top and bottom of the impregnator 9 are positioned by a positioning ring 8, a positioning shaft 17, and fixed plates fixed to the upper and lower ends of the inclined frame 24, respectively, to ensure that the position of the impregnator 9 remains fixed to the inclined frame 24 during rotation.

[0010] Furthermore, the tilt control unit includes a tilt motor 11 and a tilt drive assembly 12. The tilt drive assembly 12 includes a worm gear 16 and a worm. The tilt motor 11 is fixed on the tilt bracket 28, and the tilt bracket 28 is fixed on the base frame 26. The output shaft of the tilt motor 11 is fixed to the worm. The worm gear 16 is fixed to the tilt frame 24 through a fixing block. The rotation of the tilt motor 11 drives the worm to rotate, which in turn drives the worm gear 16 to rotate. The rotation of the worm gear 16 drives the tilt frame 24 to rotate, which in turn drives the impregnator 9 to rotate.

[0011] Furthermore, the rotation control unit includes a clamp 15, a rotation drive assembly 27, and a rotation motor 18. The rotation drive assembly 27 includes a worm gear 16 and a worm. The rotation motor 18 is fixed to the integrated base 22 at the bottom of the inclined frame 24. The output shaft of the rotation motor 18 is fixed to the worm. The worm gear 16 clamps the bottom of the impregnator 9 through the clamp 15. The rotation of the rotation motor 18 drives the worm to rotate, which in turn drives the worm gear 16 to rotate. The rotation of the worm gear 16 drives the clamp 15 to rotate, which in turn drives the impregnator 9 to rotate.

[0012] Furthermore, a PTFE two-way ball valve 19 is installed on the outlet pipe.

[0013] Furthermore, the visible microwave heating unit includes a gas cylinder 1, a filter 2, a two-way ball valve 3, a flow controller 4, a one-way valve 6, a flow controller 5, a microwave heater 10, and a thermocouple sheath 13 connected in sequence; the flow controller 5 is used to control the flow controller 4 to detect the gas flow rate; the microwave heater 10 is wrapped around the impregnator 9 and used to heat the impregnator 9; the thermocouple sheath 13 is used to detect the temperature inside the impregnator 9.

[0014] Furthermore, the gas in the gas cylinder 1 is an inert gas or air;

[0015] Furthermore, the thermocouple sleeve 13 is a sleeve installed on the thermocouple to prevent materials from damaging it.

[0016] Furthermore, reactor seals 20 are installed at the air inlet 7 and the air outlet;

[0017] Furthermore, a rotating bearing 21 and a load bearing assembly 23 are respectively provided at the top and bottom of the impregnator 9 to ensure the smoothness of the rotation process.

[0018] Furthermore, the microwave heater 10 controls the temperature by power, with a temperature range of (60~150)℃ and a gas flow rate of (1.0-5.0)L / min.

[0019] Furthermore, the impregnator 9 is provided with a viewing window 25 for real-time observation of the catalyst material.

[0020] A method for using a high-loading catalyst batch scale-up uniform preparation system, characterized by the following process:

[0021] Add the carrier and precursor solution into impregnator 9. Using the tilt control unit, first swing impregnator 9 from a vertical 90° angle to a horizontal position. Then, start the rotation control unit to make impregnator 9 rotate the catalyst material, so as to achieve thorough and uniform mixing of the precursor solution and the carrier, and ensure that the active component is uniformly dispersed on the carrier. Control the rotation rate and rotation time in the above operation. After a period of time, stop the rotation and swing impregnator 9 to a vertical position and let it stand. Then repeat the above operation 1 to 3 times. Adjust impregnator 9 from a vertical position to a horizontal position.

[0022] Start the rotation control unit to control the rotation speed, and then start the gas flow controller 4 and flow controller 5 to make the flowing gas pass evenly through the impregnator 9, and together with the microwave heater 10, complete the uniform drying of the catalyst material, so that the solvent in the precursor solution evaporates evenly and the active components are always in a uniformly dispersed state.

[0023] The dried catalyst is transferred to a calcination tube and subjected to conventional heat treatment using a muffle furnace or tube furnace to obtain the finished catalyst.

[0024] Compared with the prior art, the device of the present invention has the following beneficial effects:

[0025] 1. This invention utilizes an operation mode that combines automatic swing rotation control with microwave rapid drying and gas control, and adopts a dynamic uniform control operation process. It can continuously and uniformly scale up the preparation of high-load catalysts, achieving uniform loading and dispersion of high-content active metals, and avoiding problems such as uneven dispersion and easy agglomeration on the active metal carrier in traditional static preparation devices.

[0026] 2. The device of the present invention uses a dual control method of microwave heating and gas flow to heat materials, which can not only ensure uniform heating of materials, but also shorten heating time and greatly improve preparation efficiency.

[0027] 2. The apparatus of this invention can prepare high-load catalysts in batches, avoiding the problems of small production volume and poor reproducibility of traditional single-tube reactors. It can rapidly and stably prepare kilogram-level high-content ruthenium-based catalysts in batches, ensuring the batch-to-batch consistency of high-load catalyst quality.

[0028] 3. The device of the present invention is applicable to different metal precursors and different support materials, and can be used to prepare different types of high-loading catalysts, exhibiting excellent versatility.

[0029] 4. The device of the present invention has low manufacturing cost and simple operation. It does not require expensive and precise empty instruments and complicated operating steps. It has a high degree of automation, reduces human error in manual operation, has high repeatability, and is suitable for engineering mass production.

[0030] To more clearly illustrate the technical solution of this application, the drawings used in the embodiments will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort. Attached Figure Description

[0031] Figure 1 This is a three-dimensional view of the catalyst mass production scale-up apparatus.

[0032] Figure 2 This is a schematic diagram of the process system components for a catalyst mass production scale-up preparation device.

[0033] Figure 3 This is a front cross-sectional view of the main body of the system device.

[0034] Figure 4 This is a front view of the main body of the system device.

[0035] Figure 5 This is a right view of the main body of the system device.

[0036] In the diagram: 1. Gas cylinder, 2. Filter, 3. Two-way ball valve, 4. Flow controller, 5. Flow control instrument, 6. Check valve, 7. Inlet, 8. Positioning ring (PTFE), 9. Impregnator, 10. Microwave heater, 11. Tilting motor, 12. Tilting drive assembly, 13. Thermocouple sleeve, 14. Filter screen plate, 15. Clamp, 16. Worm gear, 17. Positioning shaft, 18. Rotary motor, 19. PTFE two-way ball valve, 20. Reactor seal, 21. Rotary bearing, 22. Integrated base, 23. Load bearing assembly, 24. Tilting platform, 25. Viewing window, 26. Base platform, 27. Rotary drive assembly, 28. Tilting bracket. Detailed Implementation

[0037] The present invention will be described in more detail below with reference to the embodiments, but the scope of protection of the present invention is not limited to the scope shown in the embodiments.

[0038] Add the carrier and precursor solution to the impregnator 9. Using the tilt control unit, first swing the impregnator 9 from a vertical 90° angle to a horizontal position. Then, activate the rotation control unit to rotate the impregnator 9, causing the catalyst material to rotate. This ensures thorough and uniform mixing of the precursor solution and the carrier, guaranteeing uniform dispersion of the active component on the carrier. The rotation rate is controlled at (20~60) rpm, and the rotation time is controlled within the range of (10~90) min. Then stop the rotation, swing the impregnator 9 back to a vertical position, and let it stand for 5 minutes. Repeat this operation 1~3 times. Adjust the impregnator 9 from a vertical position to a horizontal position.

[0039] Start the rotation control unit and control the rotation speed at (20~60) rpm. Then start the gas flow controller 4 and flow controller 5 to make the flowing gas pass evenly through the impregnator 9. Together with the microwave heater 10, the catalyst material is dried evenly, so that the solvent in the precursor solution evaporates evenly and the active components are always in a uniformly dispersed state.

[0040] The dried catalyst is transferred to a calcination tube and subjected to conventional heat treatment using a muffle furnace or tube furnace to obtain the finished catalyst.

[0041] Furthermore, the number of cycles for each of the above operations is determined based on the catalyst loading requirements, and generally multiple cycles are required.

[0042] The impregnating vessel 9 of the present invention is an open elliptical cylindrical impregnating vessel with a volume of (0.5~2.0)L, which can achieve batch preparation of 200g~1000g at a time.

[0043] The process system of this invention adopts a combination of visible microwave heating (composed of microwave heater 10 and thermocouple sheath 13) and gas flow control (composed of nitrogen cylinder 1, filter 2, two-way ball valve 3, flow controller 4, flow controller 5, and one-way valve 6) to rapidly and uniformly dry the catalyst. The catalyst state can be observed through a viewing window, enabling the batch production of catalysts, controlling the uniform dispersion of active metals, resulting in high production efficiency and precise control of process conditions.

[0044] Similar parts between the embodiments provided in this application can be referred to mutually. The specific implementation methods provided above are only a few examples under the overall concept of this application and do not constitute a limitation on the scope of protection of this application. For those skilled in the art, any other implementation methods extended from the solution of this application without creative effort shall fall within the scope of protection of this application.

Claims

1. A system for the mass production and uniform preparation of high-loading catalysts, characterized in that, The high-loading catalyst batch scale-up uniform preparation system includes an impregnation and drying device and a tube furnace; the impregnation and drying device includes an impregnation reaction unit, an tilt control unit, a rotation control unit and a visible microwave heating unit, used to complete the impregnation and drying process of catalyst preparation, and the tube furnace is used to complete the calcination-level reduction and activation process of catalyst preparation. The tilt control unit and the rotation control unit can respectively drive the impregnation reaction unit to tilt and rotate, so that the active components of the catalyst are uniformly and fully loaded onto the support. The visible microwave heating unit dries the catalyst material in the impregnation reaction unit through the combined action of microwaves and inert gas. The impregnation reaction unit includes an impregnator (9) and a filter sieve plate (14). The impregnator (9) is used to provide the required environment for the precursor solution to impregnate the carrier. An air inlet (7) is provided at the top of the impregnator (9) and connected to an air inlet pipe. An air outlet is provided at the bottom of the impregnator (9) and connected to an air outlet pipe. The filter sieve plate (14) is located at the bottom of the impregnator (9) and is used to intercept the carrier during the impregnation and drying process to avoid clogging the air inlet (7) and the air outlet. The impregnator (9) is connected to the inclined frame (24) and can not only tilt with the inclined frame (24) but also rotate within the inclined frame (24). The visible microwave heating unit includes a gas cylinder (1), a filter (2), a two-way ball valve (3), a flow controller (4), a one-way valve (6), a flow controller (5), a microwave heater (10), and a thermocouple sleeve (13) connected in sequence. The flow controller (5) is used to control the flow controller (4) to detect the gas flow rate. The microwave heater (10) is wrapped around the impregnator (9) and used to heat the impregnator (9). The thermocouple sleeve (13) is used to detect the temperature inside the impregnator (9). The gas in the gas cylinder (1) is an inert gas or air; a reactor seal (20) is provided at the inlet (7) and outlet; a viewing window (25) is provided on the impregnator (9) for real-time observation of the catalyst material; a rotating bearing (21) and a load bearing group (23) are respectively provided at the top and bottom of the impregnator (9) to ensure the smoothness of the rotation process.

2. The high-loading catalyst batch scale-up uniform preparation system according to claim 1, characterized in that, The top and bottom of the impregnator (9) are positioned by a positioning ring (8), a positioning shaft (17) and a fixing plate fixed to the upper and lower ends of the inclined frame (24), respectively, to ensure that the position of the impregnator (9) remains fixed to the inclined frame (24) during rotation.

3. The high-loading catalyst batch scale-up uniform preparation system according to claim 1, characterized in that, The tilt control unit includes a tilt motor (11) and a tilt drive assembly (12). The tilt drive assembly (12) includes a worm wheel (16) and a worm. The tilt motor (11) is fixed on the tilt bracket (28), and the tilt bracket (28) is fixed on the base frame (26). The output shaft of the tilt motor (11) is fixed to the worm. The worm wheel (16) is fixed to the tilt frame (24) through a fixing block. The rotation of the tilt motor (11) drives the worm to rotate, which in turn drives the worm wheel (16) to rotate. The rotation of the worm wheel (16) drives the tilt frame (24) to rotate, which in turn drives the impregnator (9) to rotate.

4. The high-loading catalyst batch scale-up uniform preparation system according to claim 1, characterized in that, The rotation control unit includes a clamp (15), a rotation drive assembly (27), and a rotation motor (18). The rotation drive assembly (27) includes a worm gear (16) and a worm. The rotation motor (18) is fixed to the integrated base (22) at the bottom of the inclined platform (24). The output shaft of the rotation motor (18) is fixed to the worm. The worm gear (16) clamps the bottom of the impregnator (9) through the clamp (15). The rotation of the rotation motor (18) drives the worm to rotate, which in turn drives the worm gear (16) to rotate. The rotation of the worm gear (16) drives the clamp (15) to rotate, which in turn drives the impregnator (9) to rotate.

5. The high-loading catalyst batch scale-up uniform preparation system according to claim 1, characterized in that, The PTFE two-way ball valve (19) is installed on the outlet pipe.

6. The high-loading catalyst batch scale-up uniform preparation system according to claim 1, characterized in that, The thermocouple sleeve (13) is a sleeve installed on the basis of the thermocouple to prevent the material from damaging it; the microwave heater (10) controls the temperature by power, and the temperature range is (60~150)℃, and the gas flow rate is (1.0-5.0)L / min.

7. A method of using the high-loading catalyst batch scale-up uniform preparation system according to any one of claims 1-6, characterized in that, The process is as follows: Add the carrier and precursor solution into the impregnator (9). Use the tilt control unit to first swing the impregnator (9) from a vertical 90° position to a horizontal position. Then start the rotation control unit to make the impregnator (9) drive the catalyst material to rotate, so that the precursor solution and the carrier are fully and evenly mixed, and the active components are evenly dispersed on the carrier. Control the rotation rate and rotation time in the above operation. After a period of time, stop the rotation and swing the impregnator (9) to a vertical position and let it stand. Then repeat the above operation 1 to 3 times. Adjust the impregnator (9) from a vertical position to a horizontal position. Start the rotation control unit to control the rotation speed, and then start the gas flow controller (4) and flow controller (5) to uniformly pass the flowing gas through the impregnator (9), and together with the microwave heater (10) to uniformly dry the catalyst material, so that the solvent in the precursor solution evaporates uniformly and the active components are always in a uniformly dispersed state. The dried catalyst is transferred to a calcination tube and subjected to conventional heat treatment using a muffle furnace or tube furnace to obtain the finished catalyst.

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