High-loading-capacity catalyst batch amplification uniform preparation system and use method

Abstract

The invention relates to a high-load catalyst batch amplification uniform preparation system and a use method thereof. The device disclosed by the invention is suitable for engineering development and batch amplification uniform preparation of a high-loading-capacity (more than 20wt.%) catalyst, can realize single-tube kilogram-level batch preparation of the catalyst, can stably control batch production conditions, is stable in preparation process parameter operation, and ensures uniform dispersion of high-loading-capacity active metal and consistency of batch quality of the catalyst. The catalyst preparation device disclosed by the invention is applied to research and batch production of a high-load catalyst for liquid propellant decomposition and meets engineering application requirements.

Description

Technical Field

[0001] The present invention relates to the technical field of catalytic decomposition of aerospace power chemical propellants, and specifically to a high-load catalyst batch-scale uniform preparation system and application. The catalyst preparation system can be used to quickly and stably realize the batch-scale uniform preparation of high-load metal catalysts, control the uniformity of active metal loading, realize kilogram-level batch-scale preparation of high-load catalysts, and ensure the batch production consistency of catalysts. Background Art

[0002] The catalysts used in the traditional chemical industry have a low content of active metal components. The main preparation methods are impregnation, deposition precipitation, sol-gel, etc. The carriers involved are mainly conventional activated carbon, titanium oxide, zinc oxide, aluminum oxide, etc. Their main uses are electrochemical hydrogen evolution, synthetic ammonia, Fischer-Tropsch synthesis, hydrogenation reaction and other chemical fields.

[0003] The preparation devices used in the prior art do not involve batch-scale preparation methods, especially for batch preparation and production of high-load catalysts. For example, compared with traditional chemical catalysts, the ruthenium-based catalysts used in the field of aerospace propulsion technology for decomposing liquid hydrazine propellants require high content, uniform activity, and high consistency in product batch quality. Due to the physical properties of the ruthenium active metal precursor solution, it is difficult for its ruthenium metal nanoparticles to achieve highly uniform dispersion of active components. The uniform load of high-content ruthenium metal cannot be controlled using traditional preparation devices. Therefore, it is urgent to find a high-load catalyst batch uniform amplification preparation system and process that can be used for the stable batch preparation of high-content ruthenium-based aerospace catalysts to meet the application of aerospace model engineering. Summary of the invention

[0004] Based on the problem that existing devices and technologies cannot stably achieve uniform scale-up preparation of high-loaded catalysts, the purpose of the present invention is to provide a system and application for batch uniform scale-up preparation of aerospace catalysts with high-loaded metal active components uniformly dispersed at nanometer level, so as to achieve the purpose of uniform dispersion of high-loaded active metals and good consistency of batch preparation.

[0005] To achieve the above purpose, the present invention adopts the following technical process scheme:

[0006] A high-load catalyst batch-scale uniform preparation system, the high-load catalyst batch-scale uniform preparation system comprising an impregnation and drying device and a tubular furnace; the impregnation and drying device comprises an impregnation reaction unit, a tilt control unit, a rotation control unit and a visible microwave heating unit, which are used to complete the impregnation and drying process of catalyst preparation, and the tubular furnace is used to complete the roasting-level reduction activation process of catalyst preparation;

[0007] The tilt control unit and the rotation control unit can respectively drive the impregnation reaction unit to perform tilting motion and rotation motion, so that the active components of the catalyst are evenly 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 screen plate 14. The impregnator 9 is used to provide a required environment for the precursor solution to impregnate the carrier. An air inlet 7 is provided at the top of the impregnator 9 and is connected to the air inlet pipe. An air outlet is provided at the bottom of the impregnator 9 and is connected to the air outlet pipe. The filter screen plate 14 is provided at the bottom of the impregnator 9 and is used to intercept the carrier during the impregnation and drying process to avoid blocking the air inlet 7 and the air outlet. The impregnator 9 is connected to the tilting stand 24 and can not only tilt with the tilting stand 24 but also rotate within the tilting stand 24.

[0009] Furthermore, the top and bottom ends of the macerator 9 are positioned respectively by the positioning ring 8, the positioning shaft 17 and the fixing plates fixed at the upper and lower ends of the tilting stand 24, so as to ensure that the position of the macerator 9 is always fixed with the tilting stand 24 during the rotation process.

[0010] Furthermore, the tilt control unit includes a tilt motor 11 and a tilt drive assembly 12, the tilt drive assembly 12 includes a turbine 16 and a worm, the tilt motor 11 is fixed on a tilt bracket 28, the tilt bracket 28 is fixed on a base frame 26, the output shaft of the tilt motor 11 is fixed to the worm, the turbine 16 is fixed to the tilt frame 24 through a fixing block, the rotation of the tilt motor 11 drives the worm to rotate, and then drives the turbine 16 to rotate, the rotation of the turbine 16 drives the tilt frame 24 to rotate, and then 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 turbine 16 and a worm. The rotation motor 18 is fixed to the integrated base 22 at the bottom end of the tilting stand 24. The output shaft of the rotation motor 18 is fixed to the worm. The turbine 16 clamps the bottom end of the impregnator 9 through the clamp 15. The rotation of the rotation motor 18 drives the worm to rotate, thereby driving the turbine 16 to rotate. The rotation of the turbine 16 drives the clamp 15 to rotate, thereby driving the impregnator 9 to rotate.

[0012] Furthermore, a polytetrafluoroethylene two-way ball valve 19 is arranged on the air 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 sleeve 13 connected in sequence; the flow controller 5 is used to control the flow controller 4 to perform gas flow detection; the microwave heater 10 is wrapped and arranged outside the impregnator 9, and is used to heat the impregnator 9, and the thermocouple sleeve 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 provided on the basis of the thermocouple to prevent it from being damaged by the material.

[0016] Further, a reactor seal 20 is provided at the air inlet 7 and the air outlet;

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

[0018] Furthermore, the microwave heater 10 controls the temperature by power, the temperature range is (60-150)°C, and the gas flow rate is (1.0-5.0) L / min.

[0019] Furthermore, a window 25 is provided on the impregnator 9 for observing the catalyst material condition in real time.

[0020] A method for using a high-load catalyst batch-scale uniform preparation system, characterized in that the process is as follows:

[0021] Add the carrier and the precursor solution into the impregnator 9, first swing the impregnator 9 from a vertical position of 90° to a horizontal position by using the tilt control unit, then start the rotation control unit to make the impregnator 9 drive the catalyst material to rotate, so as to achieve full and uniform mixing of the precursor solution and the carrier, and ensure that the active components are evenly dispersed on the carrier; control the rotation rate and rotation time in the above operation, stop the rotation after a period of time, swing the impregnator 9 to a vertical state and let it stand, then repeat the above operation, and repeat the operation 1 to 3 times; swing the impregnator 9 from a vertical state to a horizontal state;

[0022] Start the rotation control unit to control the rotation rate, then start the gas flow controller 4 and the flow controller 5 to evenly pass the flowing gas through the impregnator 9, and work together with the microwave heater 10 to evenly dry 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 a tubular furnace to obtain a finished catalyst.

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

[0025] 1. The present invention utilizes an operation mode combining automatic swing rotation control with microwave rapid drying and gas control, and adopts a dynamic uniform control operation process, which can continuously and uniformly scale up the preparation of high-load catalysts in batches, achieving uniform amount and uniform dispersion of high-content active metals, avoiding the problems of uneven dispersion and easy agglomeration on the active metal carrier of traditional static preparation equipment.

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

[0027] 2. The device of the present invention can prepare high-load catalysts in batches, avoiding the problems of small preparation volume and poor repeatability of traditional single-tube reactors. It can quickly and stably prepare kilogram-level high-content ruthenium-based catalysts in batches, ensuring the quality of high-load catalysts in batches.

[0028] 3. The device of the present invention can be applied to different metal precursors and different carrier materials, and can be used to prepare different types of high-load catalysts, and has excellent universality.

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

[0030] In order to more clearly illustrate the technical solution of the present application, the drawings required for use in the embodiments are briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 This is a three-dimensional diagram of the catalyst batch-scale preparation device.

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

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

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

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

[0036] In the figure: 1 gas cylinder, 2 filter, 3 two-way ball valve, 4 flow controller, 5 flow control instrument, 6 check valve, 7 air 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 turbine, 17 positioning shaft, 18 rotating motor, 19 PTFE two-way ball valve, 20 reactor seal, 21 rotating bearing, 22 integrated base, 23 load bearing group, 24 tilting stand, 25 window, 26 base stand, 27 rotating drive assembly, 28 tilting bracket. DETAILED DESCRIPTION

[0037] The present invention is described in more detail below in conjunction with embodiments, but the protection scope of the present invention is not limited to the scope represented by the embodiments.

[0038] Add the carrier and the precursor solution into the impregnator 9, and use the tilt control unit to first swing the impregnator 9 from a vertical 90° to a horizontal position, and then start the rotation control unit to rotate the impregnator 9 to drive the catalyst material to achieve sufficient and uniform mixing of the precursor solution and the carrier, and ensure that the active components are evenly dispersed on the carrier. The rotation rate in the above operation is controlled at (20-60) rpm, and the rotation time control range is (10-90) min; then stop the rotation, swing the impregnator 9 to a vertical state and let it stand for 5 minutes, and then repeat the above operation, and repeat the operation 1 to 3 times. Swing the impregnator 9 from a vertical state to a horizontal state,

[0039] Start the rotation control unit, control the rotation rate at (20-60) rpm, then start the gas flow controller 4 and the flow controller 5 to evenly pass the flowing gas through the impregnator 9, and work together with the microwave heater 10 to evenly dry the catalyst material, so that the solvent in the precursor solution evaporates evenly, keeping the active components in a uniformly dispersed state at all times.

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

[0041] Furthermore, the number of cycles of the above steps is determined according to the catalyst loading requirement, and generally multiple cycles are required.

[0042] The impregnator 9 of the present invention adopts an open elliptical cylindrical impregnator 9 with a volume specification of (0.5-2.0) L, which can achieve batch preparation of 200 grams to 1000 grams at a time.

[0043] The process system of the present invention adopts a combination of visible microwave heating (composed of a microwave heater 10 and a thermocouple sleeve 13) and gas flow control (composed of a nitrogen bottle 1, a filter 2, a two-way ball valve 3, a flow controller 4, a flow controller 5, and a one-way valve 6) to quickly and evenly dry the catalyst, observe the state of the catalyst through a window, realize batch-scale preparation of the catalyst, control the amount of active metal to be evenly dispersed, have high preparation production efficiency, and accurately control the process conditions.

[0044] Similar parts between the embodiments provided in this application can be referenced to each other. The specific implementation methods provided above are only a few examples under the general concept of this application and do not constitute a limitation on the protection scope of this application. For those skilled in the art, any other implementation methods expanded based on the scheme of this application without creative work belong to the protection scope of this application.

Claims

1. A high-load catalyst batch-scale uniform preparation system, characterized in that: The high-load catalyst batch-scale uniform preparation system includes an impregnation and drying device and a tubular furnace; the impregnation and drying device includes an impregnation reaction unit, a tilt control unit, a rotation control unit and a visible microwave heating unit, which are used to complete the impregnation and drying process of catalyst preparation, and the tubular furnace is used to complete the roasting-level reduction activation process of catalyst preparation; The tilt control unit and the rotation control unit can respectively drive the impregnation reaction unit to perform tilting motion and rotational motion, so that the active components of the catalyst are evenly 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.

2. A high-load catalyst batch-scale uniform preparation system according to claim 1, characterized in that: The impregnation reaction unit comprises an impregnator (9) and a filter screen plate (14). The impregnator (9) is used to provide a required environment for the precursor solution to impregnate the carrier. An air inlet (7) is arranged at the top of the impregnator (9) and is connected to the air inlet pipe. An air outlet is arranged at the bottom of the impregnator (9) and is connected to the air outlet pipe. The filter screen plate (14) is arranged 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 tilting stand (24) and can not only tilt with the tilting stand (24) but also rotate within the tilting stand (24).

3. A high-load catalyst batch-scale uniform preparation system according to claim 2, characterized in that: The top and bottom ends of the macerator (9) are positioned respectively by means of a positioning ring (8), a positioning shaft (17) and fixing plates fixed at the upper and lower ends of the tilting frame (24), thereby ensuring that the position of the macerator (9) is always fixed with the tilting frame (24) during the rotation process.

4. A high-load catalyst batch-scale uniform preparation system according to claim 2, characterized in that: The tilt control unit comprises a tilt motor (11) and a tilt drive assembly (12), the tilt drive assembly (12) comprises a turbine (16) and a worm, the tilt motor (11) is fixed on a tilt bracket (28), the tilt bracket (28) is fixed on a base frame (26), the output shaft of the tilt motor (11) is fixed to the worm, the turbine (16) is fixed to the tilt frame (24) through a fixing block, the rotation of the tilt motor (11) drives the worm to rotate, thereby driving the turbine (16) to rotate, the rotation of the turbine (16) drives the tilt frame (24) to rotate, thereby driving the immersion device (9) to rotate.

5. A high-load catalyst batch-scale uniform preparation system according to claim 2, characterized in that: The rotation control unit comprises a clamp (15), a rotation drive assembly (27), and a rotation motor (18); the rotation drive assembly (27) comprises a turbine (16) and a worm; the rotation motor (18) is fixed to an integrated base (22) at the bottom end of the tilting platform (24); the output shaft of the rotation motor (18) is fixed to the worm; the turbine (16) clamps the bottom end of the impregnator (9) through the clamp (15); the rotation of the rotation motor (18) drives the worm to rotate, thereby driving the turbine (16) to rotate; the rotation of the turbine (16) drives the clamp (15) to rotate, thereby driving the impregnator (9) to rotate.

6. A high-load catalyst batch-scale uniform preparation system according to claim 2, characterized in that: A polytetrafluoroethylene two-way ball valve (19) is arranged on the air outlet pipe.

7. A high-load catalyst batch-scale uniform preparation system according to claim 2, characterized in that: The visible microwave heating unit comprises 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) which are connected in sequence; the flow controller (5) is used to control the flow controller (4) to detect the gas flow; the microwave heater (10) is wrapped and arranged outside the impregnator (9) to heat the impregnator (9); and the thermocouple sleeve (13) is used to detect the temperature inside the impregnator (9).

8. A high-load catalyst batch-scale uniform preparation system according to claim 2, characterized in that: The gas in the gas cylinder (1) is an inert gas or air; reactor seals (20) are provided at the air inlet (7) and the air 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.

9. A high-load catalyst batch-scale uniform preparation system according to claim 7, characterized in that: The thermocouple sleeve (13) is a sleeve arranged on the basis of the thermocouple to prevent the material from damaging it; the microwave heater (10) controls the temperature by power, the control temperature range is (60-150)°C, and the gas flow rate is (1.0-5.0)L / min.

10. A method for using a high-load catalyst batch-scale uniform preparation system according to any one of claims 2 to 9, characterized in that: The process is as follows: The carrier and the precursor solution are added to the impregnator (9), and the impregnator (9) is first swung from a vertical position of 90° to a horizontal position using a tilt control unit, and then the rotation control unit is started to rotate the impregnator (9) to drive the catalyst material to achieve full and uniform mixing of the precursor solution and the carrier, and ensure that the active components are evenly dispersed on the carrier; the rotation rate and rotation time in the above operation are controlled, and the rotation is stopped after a period of time, and the impregnator (9) is swung to a vertical state and left to stand, and then the above operation is repeated, and the operation is repeated 1 to 3 times; the impregnator (9) is swung from a vertical state to a horizontal state; Start the rotation control unit to control the rotation rate, then start the gas flow controller (4) and the flow control instrument (5) to evenly pass the flowing gas through the impregnator (9), and work together with the microwave heater (10) to evenly dry the catalyst material, so that the solvent in the precursor solution evaporates evenly, 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 a tubular furnace to obtain a finished catalyst.

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