Preparation method and device of MOFs derivative material

Abstract

The invention provides a preparation method and device of an MOFs derivative material, and relates to the technical field of preparation of MOFs derivative materials. The preparation method of the MOFs derivative material comprises the following steps: putting an MOFs precursor into a crucible made of a conductive material, and putting the crucible into a reactor; the MOFs precursor is subjected to electromagnetic induction heating through an electromagnetic induction coil surrounding the reactor, a first product is obtained, the heating temperature ranges from 300 DEG C to 1300 DEG C, and the heating time ranges from 20 s to 10 min; and cooling the first product to a preset temperature to obtain a second product MOFs derivative material. The preparation method for preparing the MOFs derivative material is short in time consumption, low in energy consumption and high in yield, and the generated MOFs derivative material is relatively good in catalytic performance.

Description

Technical Field

[0001] The present invention relates to the technical field of MOFs derivative material preparation, and in particular to a method and device for preparing a MOFs derivative material. Background Art

[0002] Metal-Organic Frameworks (MOFs) derivative materials are widely used in adsorption, catalysis, drug delivery, sensing, energy, antibacterial and other fields due to their advantages such as adjustable porosity, ultra-large specific surface area, abundant active sites and high water / thermal stability.

[0003] Among them, in the process of preparing MOFs derivative materials, it is necessary to make the MOFs precursor undergo pyrolysis reaction at the pyrolysis temperature. Specifically, the existing preparation methods mainly include water / solvent thermal method and tubular furnace / muffle furnace high-temperature pyrolysis method. However, in the process of preparing MOFs derivative materials, the above preparation methods require a long heating time to reach the pyrolysis temperature of the MOFs precursor, resulting in the MOFs precursor reacting during the heating process, which greatly hinders its subsequent pyrolysis. Subsequently, a long period of insulation heating is required to fully pyrolyze the MOFs precursor, which is not only time-consuming, energy-intensive, and low in yield, but also the generated MOFs derivative materials have a low degree of defects, few active sites, large particle size, low uniformity, and small specific surface area, resulting in poor catalytic performance of the MOFs derivative materials. Summary of the invention

[0004] The purpose of the present invention is to provide a method and device for preparing MOFs derivative materials to solve the technical problems that the existing preparation of MOFs derivative materials is time-consuming, energy-intensive, low-yield, and the catalytic performance of the generated MOFs derivative materials is poor.

[0005] In order to solve the above problems, the present invention provides a method for preparing a MOFs derivative material, comprising the following steps:

[0006] Placing a MOFs precursor in a crucible made of a conductive material, and placing the crucible in a reactor;

[0007] The first product is obtained by electromagnetically induction heating the MOFs precursor through an electromagnetic induction coil surrounding the reactor, wherein the heating temperature is 300° C. to 1300° C. and the heating time is 20 seconds to 10 minutes;

[0008] The first product is cooled to a preset temperature to obtain a second product, a MOFs derivative material.

[0009] Optionally, the heating time includes a heating time and a heat preservation time, wherein the heating time is 5s to 10s.

[0010] Optionally, after obtaining the first product, the reactor is placed in a coolant for cooling until the temperature of the first product drops below 30° C., thereby obtaining a second product, a MOFs derivative material; wherein the cooling time is 1 min to 2 min.

[0011] Optionally, the coolant is alcohol.

[0012] Optionally, before placing the crucible in the reactor and subjecting the MOFs precursor to electromagnetic induction heating, an inert gas is first introduced into the reactor to maintain an inert atmosphere therein until the second product MOFs derivative material is obtained.

[0013] The present invention also provides a MOFs derivative material preparation device that can carry out the above-mentioned preparation method. The MOFs derivative material preparation device includes a control unit and a reactor. The reactor is surrounded by an electromagnetic induction coil, and the electromagnetic induction coil is connected to the control unit; the reactor is equipped with a crucible made of conductive material, and the crucible is located in the heating area of ​​the electromagnetic induction coil. A temperature detector is provided in the reactor, and the temperature detector is used to detect the temperature of the crucible.

[0014] Optionally, the outer diameter of the reactor is in the range of 10 mm to 500 mm, and the height is in the range of 200 mm to 500 mm; the outer diameter of the reactor is 10 mm to 20 mm smaller than the inner diameter of the electromagnetic induction coil.

[0015] Optionally, the reactor includes a base and a cover, the top surface of the base includes a central placement area, an inner ring area surrounding the central placement area, and an outer ring area surrounding the inner ring area, the bottom end surface of the cover corresponds to and abuts against the outer ring area; the temperature detector is arranged in the inner ring area, and the crucible is placed in the central placement area.

[0016] Optionally, an air outlet is provided at the top of the cover; an air inlet is provided at the base, and the air inlet includes a vertical hole section provided in the inner ring area and a horizontal hole section provided on the side wall of the base, and the inner end of the horizontal hole section is connected to the bottom end of the vertical hole section.

[0017] Optionally, the MOFs derivative material preparation device further comprises a lifting component, and the reactor is supported on a top supporting platform of the lifting component.

[0018] The preparation method provided by the present invention uses electromagnetic heating technology to heat and keep the MOFs precursor to prepare the MOFs derivative material:

[0019] (1) During the heating process, the electromagnetic heating technology can make the crucible instantly reach the target temperature required for the full pyrolysis of the MOFs precursor, and accurately maintain the target temperature to heat the MOFs precursor, so that the MOFs precursor that is not adversely affected by the heating process can quickly nucleate and fully pyrolyze at the target temperature to completely generate MOFs derivatives. The final MOFs derivative material has a higher degree of defects, a smaller and more uniform particle size, and correspondingly exhibits more active sites and a higher specific surface area, thereby effectively improving the catalytic performance of the MOFs derivative material.

[0020] (2) The electromagnetic heating technology heats up quickly during the heating process and shortens the thermal decomposition reaction time, i.e., the insulation time, of the MOFs precursor, thereby greatly shortening the heating time and improving the preparation yield, while effectively reducing the preparation energy consumption and preparation cost.

[0021] (3) Electromagnetic heating technology is simple to operate, operates at room temperature and pressure, and is safe and reliable, thereby improving the convenience and safety of the preparation of MOFs derivative materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0023] Figure 1 A schematic diagram of a device for preparing MOFs derivative materials provided in an embodiment of the present invention;

[0024] Figure 2 A schematic diagram of the arrangement of a lifting assembly, a reactor and a crucible in a MOFs derivative material preparation device provided in an embodiment of the present invention;

[0025] Figure 3 is an XRD pattern of a ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of the comparative example;

[0026] Figure 4 is a SEM image of a ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of the comparative example;

[0027] Figure 5 is a BET diagram of a ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of the comparative example;

[0028] Figure 6The XRD pattern of the ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of Example 1;

[0029] Figure 7 This is a SEM image of the ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of Example 1;

[0030] Figure 8 is a BET diagram of the ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of Example 1;

[0031] Fig. 9 is an XRD pattern of the ZIF-67 derived metal oxide material Co3O4 material prepared according to the preparation method of Example 2;

[0032] Fig.10 This is a SEM image of the ZIF-67 derived metal oxide material Co3O4 material prepared according to the preparation method of Example 2;

[0033] Fig.11 is an XRD pattern of the Fe2O3 / Fe3O4 composite material derived from MIL-88A(Fe) prepared according to the preparation method of Example 3;

[0034] Fig.12 is a SEM image of the Fe2O3 / Fe3O4 composite material derived from MIL-88A(Fe) prepared according to the preparation method of Example 3;

[0035] Fig.13 is an XRD pattern of the Fe / C material derived from MIL-88A(Fe) prepared according to the preparation method of Example 4;

[0036] Fig.14 is a SEM image of the Fe / C material derived from MIL-88A(Fe) prepared according to the preparation method of Example 4;

[0037] Fig.15 is an XRD pattern of the ZIF-8 derived ZnO material prepared according to the preparation method of Example 5;

[0038] Fig.16 is a SEM image of a ZIF-8 derived ZnO material prepared according to the preparation method of Example 5;

[0039] Fig.17 is an XRD pattern of the ZIF-8 derived N / C material prepared according to the preparation method of Example 6;

[0040] Fig.18This is a SEM image of the ZIF-8 derived N / C material prepared according to the preparation method of Example 6.

[0041] Description of reference numerals:

[0042] 100-crucible; 200-reactor; 210-base; 211-air inlet; 211a-horizontal hole section; 211b-vertical hole section; 212-air inlet nozzle; 220-cover; 221-air outlet; 222-air outlet nozzle; 230-air inlet pipe; 240-air outlet pipe; 250-collector; 300-electromagnetic induction coil; 400-control unit; 410-housing; 411-control panel; 412-heat dissipation hole; 413-first cooling fan; 500-temperature detector; 600-lifting assembly; 610-top bearing platform; 700-gas cylinder; 710-flow rate regulating valve; 800-cooling assembly; 810-water cooling pipe; 811-water inlet end; 812-water outlet end; 820-pump; 900-protection box; 910-second cooling fan. DETAILED DESCRIPTION

[0043] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0044] In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance.

[0045] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" 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 a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0046] This embodiment provides a method for preparing a MOFs derivative material, including an arrangement step, an electromagnetic induction heating step, and a cooling step, as follows:

[0047] Arrangement step: placing the MOFs precursor in a crucible 100 made of a conductive material, and placing the crucible 100 in a reactor 200. The prepared MOFs precursor is loaded into the crucible 100 as a reaction material, and the crucible 100 is made of a conductive material that can be electromagnetically heated; then the crucible 100 containing the MOFs precursor is placed in the reactor 200, thereby completing the arrangement of the reaction materials and reaction equipment.

[0048] Electromagnetic induction heating step: electromagnetic induction heating is performed on the MOFs precursor by the electromagnetic induction coil 300 surrounding the reactor 200 to obtain the first product, wherein the heating temperature is 300°C to 1300°C, preferably 500°C to 1200°C; the heating time is 20s to 10min, preferably 2min to 4min. The reactor 200 is surrounded by an electromagnetic induction coil 300, and high-frequency alternating current is applied to the electromagnetic induction coil 300. The alternating magnetic field lines generated by the inner ring area of ​​the electromagnetic induction coil 300 pass through the crucible 100, and the crucible 100 cuts the alternating magnetic field lines to generate high eddy currents, so that the temperature rises as a heating medium to heat the MOFs precursor inside to the target temperature.

[0049] Among them, the present application adopts an electromagnetic induction coil 300 to heat the crucible 100, which can make the crucible 100 instantly reach the target temperature required for the MOFs precursor to be fully pyrolyzed within a few seconds, thereby effectively reducing the time taken to heat the crucible 100 to the target temperature, resulting in the MOFs precursor reacting during the heating process, which greatly hinders its subsequent pyrolysis, and a longer period of insulation heating is required to fully pyrolyze the MOFs precursor; after the crucible 100 reaches the target temperature, the target temperature is maintained to keep the MOFs precursor therein heat-insulated and heated, so that the MOFs precursor that is not adversely affected by the heating process can be quickly and fully pyrolyzed in a shorter time at the target temperature to completely generate MOFs derivatives, and the MOFs derivatives obtained at this time serve as the first product.

[0050] Cooling step: Cool the first product to a preset temperature to obtain the second product, a MOFs derivative material. After the electromagnetic induction heating step reaches the heating time, the temperature of the first product is relatively high, and it is cooled to near room temperature. During the cooling process, the first product further undergoes pyrolysis and other reactions to obtain the desired MOFs derivative material, which is also the final product as the second product.

[0051] Among them, the preparation method of the present application uses electromagnetic heating technology to heat and keep the MOFs precursor warm to prepare the MOFs derivative material:

[0052] (1) During the heating process, the electromagnetic heating technology can make the crucible 100 instantly reach the target temperature required for the full pyrolysis of the MOFs precursor, and accurately maintain the target temperature to heat the MOFs precursor, so that the MOFs precursor that is not adversely affected by the heating process can quickly nucleate and fully pyrolyze at the target temperature to completely generate MOFs derivatives. The final MOFs derivative material has a higher degree of defects, a smaller and more uniform particle size, and correspondingly exhibits more active sites and a higher specific surface area, thereby effectively improving the catalytic performance of the MOFs derivative material.

[0053] (2) The electromagnetic heating technology heats up quickly during the heating process and shortens the thermal decomposition reaction time, i.e., the insulation time, of the MOFs precursor, thereby greatly shortening the heating time and improving the preparation yield, while effectively reducing the preparation energy consumption and preparation cost.

[0054] (3) Electromagnetic heating technology is simple to operate, operates at room temperature and pressure, and is safe and reliable, thereby improving the convenience and safety of the preparation of MOFs derivative materials.

[0055] Among them, the crucible 100 can be made of iron or graphite; the MOFs precursor can be prepared by existing preparation methods, such as the MOFs precursor ZIF-67 prepared according to the preparation method recorded in the document "Chemical Engineering Journal, 2022, 450, 138082", or the MOFs precursor MIL-88A (Fe) prepared according to the preparation method recorded in the document "Chemical Engineering Journal, 2021, 426, 131927", or the MOFs precursor ZIF-8 prepared according to the preparation method recorded in the document "Chinese Chemical Letters, 2023, 34 (2), 107425", etc.

[0056] Specifically, MOFs precursors include but are not limited to Fe-MOFs (MIL-88A (Fe), MIL-88B (Fe), MIL-100 (Fe), MIL-101 (Fe), BUC-96, etc.), Co-MOFs (ZIF-67, ZIF-62, ZIF-L, MOF-74 (Co), etc.) and other metal-based MOFs (ZIF-8, UiO-66, MIL-101 (Cr) and MIL-125, etc.) and their complexes or functional group modified materials, preferably MIL-88A (Fe), ZIF-67, ZIF-8 and MIL-125. Correspondingly, the types of MOFs derivative materials that can be prepared by the preparation method of the present application are metal oxides, metal-carbon composites, metal sulfides, metal selenides, metal phosphides, non-metallic carbon materials, etc., preferably metal oxides, metal-carbon composites and non-metallic carbon materials, etc.

[0057] Specifically, in this embodiment, the heating time includes a heating time and a holding time, wherein the heating time is the time taken for the electromagnetic induction coil 300 to heat the crucible 100 from the beginning to the heating of the crucible 100 to the pyrolysis temperature at which the MOFs precursor can be fully pyrolyzed. Specifically, the heating time is 5s to 10s, indicating that the electromagnetic induction technology can make the crucible 100 reach 300°C to 1300°C within 5s to 10s, and instantly complete the heating process in the heating process; the holding time is the time taken for the crucible 100 to maintain the temperature after reaching the pyrolysis temperature to heat the MOFs precursor until the MOFs precursor is fully pyrolyzed to completely generate the MOFs derivative. Specifically, the holding time is 15s to 10min, indicating that the MOFs precursor that is not affected by the heating process can complete the full pyrolysis reaction in a shorter time, and the preparation of the MOFs derivative material can be completed quickly, efficiently and with high quality.

[0058] In this embodiment, after the first product is obtained in the electromagnetic induction heating step, in the cooling step, the reactor 200 is placed in a coolant for cooling until the temperature of the first product drops below 30°C to obtain a second product, a MOFs derivative material; wherein the cooling time is 1 min to 2 min. The reactor 200 used in the electromagnetic heating technology in the present application is small in size and separated from the electromagnetic induction coil 300. After the MOFs precursor is heated by the electromagnetic induction coil 300 to generate the first product, the reactor 200 can be taken out from the electromagnetic induction coil 300 and placed in a coolant with a relatively low temperature for cooling treatment, so that the reactor 200, the crucible 100 and the first product are rapidly cooled to near room temperature within 1 to 2 minutes. During the rapid cooling process, the first product MOFs derivative can produce a richer defect structure to obtain the second product MOFs derivative material, which further improves the defect degree of the obtained MOFs derivative material, thereby further improving the richness of the active sites of the MOFs derivative material and improving the catalytic performance of the MOFs derivative material. At the same time, the cooling time is only 1 to 2 minutes, which can further improve the yield of the obtained MOFs derivative material on the basis of improving the catalytic performance of the obtained MOFs derivative material.

[0059] Specifically, the coolant may be alcohol, and the alcohol temperature may be -115°C to -20°C.

[0060] In this embodiment, according to the types of MOFs precursor and the required MOFs derivative material, during the heating process, the reactor 200 can be an air atmosphere or an inert atmosphere. When it is necessary to set the reactor 200 to an inert atmosphere, the arrangement step can also include setting the inert atmosphere in the reactor 200. Specifically, before the crucible 100 is placed in the reactor 200 and the MOFs precursor is subjected to electromagnetic induction heating, that is, before the electromagnetic heating step, an inert gas is introduced into the reactor 200 to maintain an inert atmosphere therein, and then the electromagnetic heating step is performed until the second product MOFs derivative material is obtained.

[0061] This embodiment also provides a MOFs derivative material preparation device, which can perform the above preparation method, such as Figure 1 As shown, the MOFs derivative material preparation device includes a control unit 400 and a reactor 200. The reactor 200 is surrounded by an electromagnetic induction coil 300, and the electromagnetic induction coil 300 is connected to the control unit; the reactor 200 is equipped with a crucible 100 made of conductive material, and the crucible 100 is located in the heating area of ​​the electromagnetic induction coil 300, and a temperature detector 500 is provided in the reactor 200, and the temperature detector 500 is used to detect the temperature of the crucible 100.

[0062] During use, after the arrangement step is completed, the electromagnetic induction coil 300 is wound around the outside of the reactor 200 with a certain gap between the two, and at the same time, the crucible 100 and the electromagnetic induction coil 300 are approximately coaxial; the control unit 400 controls the electromagnetic induction coil 300 to be powered on and applies high-frequency alternating current to it, and the inner ring area of ​​the electromagnetic induction coil 300 generates alternating magnetic lines of force with greater intensity and the alternating magnetic lines of force with greater density in the axial area can pass through the crucible 100 axially, and high eddy currents are generated in the crucible 100 and the temperature rises rapidly accordingly. During the heating process, the temperature detector 500 can detect the temperature of the crucible 100 in real time and report the detected temperature to the temperature sensor 500. The signal is fed back to the control unit 400; when the control unit 400 determines that the crucible 100 has reached the target temperature of 300°C to 1300°C at which the MOFs precursor can be pyrolyzed based on the received temperature signal, the current frequency applied to the electromagnetic induction coil 300 is adjusted in real time based on the temperature signal fed back in real time by the temperature detector 500, so that the crucible 100 maintains the target temperature to heat the MOFs precursor until the heating time reaches a preset time of 20s to 10min, and then the electromagnetic induction coil 300 is disconnected from the power supply, the heating of the crucible 100 is stopped, the electromagnetic induction heating step is completed, and the first product is prepared.

[0063] Then, a cooling step is performed to cool the first product to a preset temperature, thereby preparing a second product, a MOFs derivative material.

[0064] The MOFs derivative material preparation device provided in this embodiment can carry out the above-mentioned preparation method to obtain MOFs derivative materials. In addition to having the technical effects of the above-mentioned (1)-(3), it also has the advantages of simple structure and small size, thereby further improving the convenience of operation of the preparation method; at the same time, the reactor 200 is small in size, and the subsequent cooling step can directly place the reactor 200 in the coolant for rapid cooling, thereby realizing rapid cooling of the first product to the second product, which not only improves the defect richness of the second product MOFs derivative material, increases the active sites, and improves the catalytic performance of the MOFs derivative material, but also can shorten the preparation time and further improve the yield.

[0065] Specifically, in this embodiment, the outer diameter of the reactor 200 ranges from 10 mm to 500 mm, and the height ranges from 200 mm to 500 mm; the outer diameter of the reactor 200 is 10 mm to 20 mm smaller than the inner diameter of the electromagnetic induction coil 300 . On the basis of realizing the preparation of MOFs derivative materials, the reactor 200 in this embodiment is small in size, and the electromagnetic induction coil 300 is small in size and has a gap with the reactor 200; on the one hand, the entire preparation device is small in size, occupies a small space, and has a low preparation cost; on the other hand, when performing the arrangement step, the reactor 200 can be taken out from the electromagnetic induction coil 300 upward or downward, the crucible 100 can be taken out from the reactor 200, and then the MOFs precursor can be loaded into the crucible 100, and then the crucible 100 can be loaded into the reactor 200, and finally the reactor 200 can be inserted into the electromagnetic induction coil 300 again, and the operation is convenient; on the other hand, the reactor 200 is small in size and easy to disassemble from the electromagnetic induction coil 300. When performing the cooling step, the reactor 200 can be directly removed and immersed in the coolant for rapid cooling treatment, which is convenient to operate and greatly improves the cooling rate of the first product, so as to obtain a second product MOFs derivative material with richer defect structure, richer active sites and higher catalytic performance.

[0066] Specifically, the diameter of the electromagnetic induction coil 300 is in the range of 20 mm to 500 mm, preferably 30 mm to 80 mm; the coverage of the electromagnetic induction coil 300 in the axial direction is 50 mm to 500 mm, preferably 80 mm to 150 mm. The outer diameter of the crucible 100 is 5 mm to 10 mm smaller than the inner diameter of the reactor 200, and the height of the crucible 100 in the axial direction is 10 mm to 20 mm smaller than the coverage height of the electromagnetic induction coil 300 in the axial direction.

[0067] In this embodiment, Figure 2As shown, the reactor 200 can specifically adopt the following structure: the reactor 200 includes a base 210 and a cover 220. The top surface of the base 210 includes a central placement area, an inner ring area surrounding the central placement area, and an outer ring area surrounding the inner ring area. The bottom end surface of the cover 220 corresponds to the outer ring area; the temperature detector 500 is arranged in the inner ring area, and the crucible 100 is placed in the central placement area. The top surface of the base 210 includes a central placement area, an annular inner ring area, and an annular outer ring area in sequence from the center to the outside in a radial direction. When in use, the cover 220 can be removed upwards, and the crucible 100 can be placed in the central placement area approximately coaxial with the base 210, and then the cover 220 is corresponding to the outer ring area of ​​the top surface of the base 210, so that the crucible 100 is covered therein, and the electromagnetic induction coil 300 surrounding the outside of the reactor 200 is approximately coaxial with the reactor 200 and the crucible 100, so as to ensure that the action on The density of the alternating magnetic lines of force of the crucible 100 ensures the convenience of disassembly and assembly of the reactor 200, the convenience of taking and placing the crucible 100, and the heating efficiency of the electromagnetic induction coil 300 on the crucible 100; wherein, the temperature detector 500 is arranged in the inner ring area and will not be damaged by the collision of the cover 220, and is close to the crucible 100 to accurately detect the temperature of the crucible 100, thereby dividing the radial area of ​​the base 210, improving the compactness of the arrangement of the components, and further reducing the volume and space occupied by the reactor 200.

[0068] The base 210 and the cover 220 are detachably connected, and a sealing gasket is provided between the base 210 and the cover 220 to improve the firmness and stability of the cover 220 on the base 210 and ensure the sealing inside the reactor 200.

[0069] Preferably, after the arrangement step is completed, the crucible 100 is located within the coverage range of the electromagnetic induction coil 300 along the axial direction of the electromagnetic induction coil 300, so as to further increase the density of the alternating magnetic lines of force on the crucible 100, and improve the heating efficiency and heating effect of the electromagnetic induction coil 300 on the crucible 100 and the MOFs precursor therein.

[0070] Specifically, the distance between the temperature detector 500 and the crucible 100 ranges from 10 mm to 20 mm, preferably from 5 mm to 10 mm.

[0071] Optionally, in this embodiment, if Figure 2As shown, an air outlet 221 is provided at the top of the cover 220; an air inlet 211 is provided at the base 210, and the air inlet 211 includes a vertical hole section 211b provided in the inner ring area and a horizontal hole section 211a provided on the side wall of the base 210, and the inner end of the horizontal hole section 211a is connected to the bottom end of the vertical hole section 211b. After completing the arrangement steps, when it is necessary to adjust the reactor 200 to an inert atmosphere, the outer port of the horizontal hole segment 211a can be connected to an inert gas source, and the inert gas source is turned on to deliver inert gas to the horizontal hole segment 211a, and the inert gas then enters the vertical hole segment 211b and enters the reactor 200 through its top port. As the inert gas gradually fills all the internal spaces of the reactor 200 from the bottom area upward, the air in the reactor 200 is discharged upward through the air outlet 221, so that the reactor 200 is in an inert atmosphere, and it can be ensured that the entire area of ​​the reactor 200 is in an inert atmosphere, ensuring that the environment of the crucible 100 is an inert environment, and ensuring the effective reaction of the MOFs precursor therein in the inert atmosphere; wherein, during the electromagnetic induction heating process, the inert gas source continuously introduces inert gas into the reactor 200 through the air inlet 211 to maintain the inert atmosphere in the reactor 200, further ensuring the full reaction of the MOFs precursor in the inert atmosphere.

[0072] Preferably, the top of the air outlet hole 221 is connected to an air outlet nozzle 222, and the outer end of the horizontal hole section 211a is connected to an air inlet nozzle 212. The air inlet nozzle 212 can be connected to the air inlet pipe 230, and is connected to the inert gas source through the air inlet pipe 230, thereby improving the convenience of connecting the air inlet hole 211 with the inert gas source; similarly, the air outlet nozzle 222 can be connected to the air outlet pipe 240, and the output gas is discharged to a designated location through the air outlet pipe 240.

[0073] Specifically, the inert gas source may be a gas cylinder 700 , and a flow rate regulating valve 710 is provided at the gas outlet of the gas cylinder 700 , and the flow rate regulating valve 710 may be used to adjust the gas flow rate from the gas cylinder 700 to the reactor 200 .

[0074] Specifically, Figure 1 As shown, the MOFs derivative material preparation device also includes a collector 250, and the outlet end of the outlet pipe 240 extends into the collector 250. When harmful substances are generated during the pyrolysis reaction, the collector 250 is filled with an absorption liquid, and the outlet end of the outlet pipe 240 is immersed in the absorption liquid. When the gas discharged from the outlet pipe 240 passes through the absorption liquid, the harmful substances in it can be absorbed by the absorption liquid, and the purified gas is discharged upward, thereby reducing the pollution caused by the gas discharged from the outlet pipe 240 to the environment.

[0075] In this embodiment, the cover 220 can be made of transparent quartz glass. The operator can clearly observe the reaction process in the reactor 200 from the outside, thereby ensuring that the operator has a good grasp of the preparation process.

[0076] Optionally, in this embodiment, if Figure 1 and Figure 2 As shown, the MOFs derivative material preparation device also includes a lifting assembly 600, and the reactor 200 is carried on the top bearing platform 610 of the lifting assembly 600. When in use, the lifting assembly 600 can be controlled to adjust its top bearing platform 610 and the reactor 200 thereon to rise or fall so that the reactor 200 is located above or below the electromagnetic induction coil 300, thereby facilitating the disassembly and assembly of the cover 220, the filling of the MOFs precursor, and the installation of the crucible 100; after the crucible 100 is placed on the top surface of the base 210 and covered with the cover 220, the lifting assembly 600 adjusts its top bearing platform 610 and the reactor 200 to descend or rise to insert the electromagnetic induction coil 300, thereby improving the convenience of the arrangement step.

[0077] In this embodiment, Figure 1 As shown, the MOFs derivative material preparation device also includes a cooling component 800, which is connected to the electromagnetic induction coil 300 and is used to cool the electromagnetic induction coil 300. During the electromagnetic induction heating step, the electromagnetic induction coil 300 can be continuously cooled by the cooling component 800 to reduce the occurrence of the electromagnetic induction coil 300 being burned due to excessive temperature, thereby ensuring the normal heating operation of the electromagnetic induction coil 300 and ensuring the normal use of the preparation device.

[0078] Specifically, the cooling component 800 can be water-cooled, and the water-cooling component includes a water-cooling tube 810 attached to the electromagnetic induction coil 300, the water inlet end 811 of the water-cooling tube 810 is connected to the cold water source, and the pipe section of the water-cooling tube 810 close to the cold water source or the water inlet end 811 of the water-cooling tube 810 is provided with a pump 820, such as a diaphragm pump 820 or a peristaltic pump 820, and the start and stop of the water-cooling component is controlled by the pump 820; or the water inlet end 811 of the water-cooling tube 810 is connected to a faucet, and the water flow is controlled by the faucet; at the same time, the water outlet end 812 of the water-cooling tube 810 can be extended to a designated position for drainage.

[0079] Specifically, Figure 1 As shown, the control unit 400 includes a shell 410, a control module accommodated inside the shell 410 and a control panel 411 embedded in the shell 410. The control module is communicatively connected to the electromagnetic induction coil 300, the temperature detector 500 and the control panel 411, and the operator can perform control operations through the control panel 411; the shell 410 is provided with heat dissipation holes 412 and a first heat dissipation fan 413. The heat generated by the operation of the control module can be discharged to the outside through the heat dissipation holes 412 and the first heat dissipation fan 413 to reduce the occurrence of over-temperature, unstable operation or even downtime of the control module, thereby ensuring the normal operation of the control module.

[0080] In this embodiment, Figure 1 As shown, the MOFs derivative material preparation device also includes a protection box 900, and the control unit 400, the reactor 200, the electromagnetic induction coil 300, the lifting assembly 600 and the collector 250 are all placed in the protection box 900, so that the protection box 900 can isolate and protect the above-mentioned components; preferably, the protection box 900 can be made of insulating materials to play an insulating protection role, reduce the occurrence of leakage of the electromagnetic induction coil 300, and thus improve the safety of the preparation device; or, the protection box 900 can also be made of materials such as iron sheets that can shield magnetic lines of force, so as to reduce the adverse effects of the magnetic lines of force generated by the electromagnetic induction coil 300 on surrounding electronic components during the heating process.

[0081] Preferably, the protection box 900 is provided with a second cooling fan 910 to dissipate the heat in the protection box 900 to ensure the normal operation of the preparation device.

[0082] The present invention is further described in detail below with reference to the accompanying drawings and embodiments.

[0083] Comparative Example:

[0084] Using ZIF-67 as MOFs precursor, the ZIF-67-derived metal / carbon composite material Co / C material was prepared by high-temperature pyrolysis in a tubular furnace:

[0085] Step 1: Layout steps:

[0086] ① Place the MOFs precursor ZIF-67 after methanol washing and centrifugation in a 60°C oven and dry for 6 hours to obtain ZIF-67 powder; wherein, the MOFs precursor ZIF-67 can be prepared according to the preparation method described in the document "Chemical Engineering Journal, 2022, 450, 138082";

[0087] ② Place ZIF-67 powder in a porcelain boat, then place the porcelain boat in a tube furnace and seal both ends of the tube furnace;

[0088] ③Introduce nitrogen into the tubular furnace for 20 minutes to create a nitrogen atmosphere in the tubular furnace.

[0089] Step 2: Tube furnace heating steps:

[0090] The heating rate of the tubular furnace was set to 5°C / min, the pyrolysis temperature was set to 700°C, and the pyrolysis time was set to 2h. The tubular furnace was started and nitrogen was introduced into the tubular furnace during the heating process until the tubular furnace ran for 140min of heating and 120min of insulation, to obtain the first product, a MOFs derivative.

[0091] Step 3: Cooling step: Set the cooling rate of the tubular furnace to 5°C / min, naturally cool the first product to 30°C, stop introducing nitrogen, and thus prepare the second product ZIF-67 derived metal / carbon composite material Co-N / C material; wherein the actual cooling time is greater than 134 min.

[0092] XRD, SEM and BET were used to test the structure and morphology of the ZIF-67-derived metal / carbon composite Co / C material prepared in the comparative example: Figure 3 is the XRD pattern of the ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of the comparative example, Figure 3 It can be seen that the characteristic peak intensities of Co and C corresponding to the Co / C material are poor, indicating that the Co / C material has poor crystallinity, low defect level, and fewer active sites; Figure 4 is a SEM image of a ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of the comparative example, Figure 4 In the figure, the Co / C material has an irregular and non-uniform morphology and obvious large agglomeration occurs - the particle size is large, which shows that the particle size of the Co / C material is large and non-uniform, and the specific surface area is small; Figure 5 The BET diagram of the ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of the comparative example is shown in FIG. Figure 5 The desorption isotherm at the top and the adsorption isotherm at the bottom can be analyzed using software to show that the specific surface area of ​​the Co / C material is only 8m 2 g -1 .

[0093] It can be seen that in the comparative example, ZIF-67 was used as the MOFs precursor, and the ZIF-67-derived metal / carbon composite material Co / C material was prepared by the high-temperature pyrolysis method in a tubular furnace. The total time consumption of the tubular furnace heating step and the cooling step was greater than 394 minutes, which was time-consuming, and the electricity consumption and nitrogen energy consumption were both large, the yield was low, and the cost was high. At the same time, the obtained Co / C material had a low degree of defects, fewer active sites, larger and uneven particle size, and a small specific surface area, resulting in poor catalytic performance of the Co / C material.

[0094] Example 1

[0095] Using ZIF-67 as a MOFs precursor, the MOFs derivative material preparation device of the present application is used to prepare the ZIF-67 derived metal / carbon composite material Co / C material by electromagnetic heating technology:

[0096] Step 1: Layout steps:

[0097] ① Place the MOFs precursor ZIF-67 after methanol washing and centrifugation in a 60°C oven and dry for 6 hours to obtain ZIF-67 powder; wherein, the MOFs precursor ZIF-67 can be prepared according to the preparation method described in the document "Chemical Engineering Journal, 2022, 450, 138082";

[0098] ② Place ZIF-67 powder in the crucible 100, then place the crucible 100 in the reactor 200, and adjust the height of the reactor 200 by the lifting assembly 600 so that it is located in the ring of the electromagnetic induction coil 300, and the crucible 100 is located in the central heating area of ​​the electromagnetic induction coil 300;

[0099] ③ Nitrogen was introduced into the reactor 200 for 20 minutes to create a nitrogen atmosphere in the tubular furnace.

[0100] Step 2: Electromagnetic induction heating steps:

[0101] The heating power of the electromagnetic induction coil 300 is set to 12 kW, and the heating time is 3 min. The electromagnetic induction coil 300 and the cooling assembly 800 are both started and run, and nitrogen is kept passing into the reactor 200 during the heating process. The crucible 100 is heated to 700°C within 10 s, and then the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback from the temperature detector 500 to maintain the heating temperature at 700°C until the heating time reaches 3 min. The electromagnetic induction coil 300 and the cooling assembly 800 are shut down to obtain the first product, a MOFs derivative.

[0102] Step 3: Cooling step: remove the reactor 200 and place it in alcohol at -78°C for 2 minutes, the temperature of the reactor 200 drops below 30°C, and the nitrogen gas flow into the reactor 200 is stopped, thereby preparing the second product ZIF-67 derived metal / carbon composite material Co / C material.

[0103] XRD, SEM and BET were used to detect the structure and morphology of the ZIF-67-derived metal / carbon composite material Co / C prepared in Example 1: Figure 6 is the XRD pattern of the ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of Example 1, Figure 6 The characteristic peak of Co can be clearly seen. It can be seen that the characteristic peak intensity of Co corresponding to the Co / C material is higher and the noise peak interference is less, indicating that the Co-N / C material has good crystallinity, is pure and free of impurities, has a high degree of defects, has more active sites, and has good hydrothermal stability. At the same time, it can be seen Figure 6 The peak intensity of C in the comparison Figure 3The peak intensity of C in the middle is greatly enhanced, indicating that Figure 6 The Co / C material has more defects and correspondingly more active sites.

[0104] Figure 7 is a SEM image of the ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of Example 1, Figure 7 In the experiment, the Co / C material has a regular and uniform morphology of extremely small nanoparticles, and there is no obvious agglomeration. It can be seen that the particle size of the Co / C material is small and relatively uniform, and correspondingly has a larger specific surface area and better catalytic performance. Figure 8 The BET diagram of the ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of Example 1 is shown in FIG. Figure 8 The desorption / adsorption isotherms of the Co / C material can be analyzed by software to obtain a specific surface area of ​​330 m2 g-1. Compared with the ZIF-67-derived Co / C material prepared by the traditional tube furnace pyrolysis method, the BET results show that the ZIF-67-derived Co / C material synthesized by the method of the present invention has a larger BET specific surface area of ​​330 m2 g-1. 2 g -1 , providing better active sites and improving subsequent catalytic performance.

[0105] It can be seen that in Example 1, ZIF-67 is used as a MOFs precursor, and electromagnetic heating technology is used to prepare a ZIF-67-derived metal / carbon composite material Co / C material under a nitrogen atmosphere, wherein the total time consumption of the electromagnetic induction heating step and the cooling step is approximately equal to 5 minutes, which is short in time, low in electricity consumption, high in yield and low in cost; at the same time, the prepared Co / C material has a high degree of defects, more active sites, smaller particle size, higher uniformity and larger specific surface area, so that the Co / C material has better catalytic performance.

[0106] Example 2

[0107] Using ZIF-67 as a MOFs precursor, the MOFs derivative material preparation device of the present application is used to prepare the ZIF-67 derived metal oxide material Co3O4 material by electromagnetic heating technology:

[0108] Step 1: Layout steps:

[0109] ① Place the MOFs precursor ZIF-67 after methanol washing and centrifugation in a 60°C oven and dry for 6 hours to obtain ZIF-67 powder; wherein, the MOFs precursor ZIF-67 can be prepared according to the preparation method described in the document "Chemical Engineering Journal, 2022, 450, 138082";

[0110] ② Place ZIF-67 powder in the crucible 100, then place the crucible 100 in the reactor 200, and adjust the height of the reactor 200 through the lifting assembly 600 so that it is located in the ring of the electromagnetic induction coil 300, and the crucible 100 is located in the central heating area of ​​the electromagnetic induction coil 300.

[0111] Step 2: Electromagnetic induction heating steps:

[0112] The heating power of the electromagnetic induction coil 300 is set to 12 kW, and the heating time is 3 min. The electromagnetic induction coil 300 and the cooling assembly 800 are both started and operated, and the crucible 100 is heated to 1200°C within 10 s. Then, the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback from the temperature detector 500 to maintain the heating temperature at 1200°C until the heating time reaches 3 min. The electromagnetic induction coil 300 and the cooling assembly 800 are shut down to obtain the first product, the MOFs derivative.

[0113] Step 3: Cooling step: remove the reactor 200 and place it in alcohol at -78°C for 2 minutes, and the temperature of the reactor 200 drops below 30°C, thereby preparing the second product ZIF-67 derived metal oxide material Co3O4 material.

[0114] XRD and SEM were used to detect the structure and morphology of the ZIF-67-derived metal oxide material Co3O4 prepared in Example 2: Fig. 9 is the XRD pattern of the ZIF-67 derived metal oxide material Co3O4 material prepared according to the preparation method of Example 2, Fig. 9 It can be seen that the characteristic peak intensity of Co corresponding to the Co3O4 material is higher and the noise peak interference is less, indicating that the Co-N / C material has good crystallinity, is pure and free of impurities, has a high degree of defects, and has more active sites; Fig.10 is a SEM image of the ZIF-67 derived metal oxide material Co3O4 material prepared according to the preparation method of Example 2, Fig.10 In the experiment, the Co3O4 material showed a regular and uniform nanoparticle morphology. It can be seen that the particle size of the Co3O4 material was small and relatively uniform, and correspondingly had a larger specific surface area and better catalytic performance.

[0115] It can be seen that Example 2 uses ZIF-67 as a MOFs precursor and adopts electromagnetic heating technology to prepare the ZIF-67-derived metal oxide material Co3O4 material, wherein the total time consumption of the electromagnetic induction heating step and the cooling step is approximately equal to 5 minutes, which is short in time, low in electricity consumption, high in yield and low in cost; at the same time, the prepared Co3O4 material has a high degree of defects, more active sites, smaller particle size, higher uniformity and larger specific surface area, which makes the Co3O4 material have better catalytic performance.

[0116] Example 3

[0117] Using MIL-88A(Fe) as a MOFs precursor, the MIL-88A(Fe)-derived Fe2O3 / Fe3O4 composite material was prepared by electromagnetic heating technology using the MOFs derivative material preparation device of the present application:

[0118] Step 1: Layout steps:

[0119] ① The MOFs precursor-MIL-88A(Fe) washed with anhydrous ethanol and centrifuged was placed in a 60°C oven and dried for 6 hours to obtain MIL-88A(Fe) powder; wherein the MOFs precursor-MIL-88A(Fe) can be prepared according to the preparation method described in the literature (Chemical Engineering Journal, 2021, 426, 131927);

[0120] ② Place MIL-88A (Fe) powder in the crucible 100, then place the crucible 100 in the reactor 200, and adjust the height of the reactor 200 through the lifting assembly 600 so that it is located in the ring of the electromagnetic induction coil 300, and the crucible 100 is located in the central heating area of ​​the electromagnetic induction coil 300.

[0121] Step 2: Electromagnetic induction heating steps:

[0122] The heating power of the electromagnetic induction coil 300 is set to 12 kW, and the heating time is 3 min. The electromagnetic induction coil 300 and the cooling assembly 800 are both started and operated, and the crucible 100 is heated to 1200°C within 10 s. Then, the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback from the temperature detector 500 to maintain the heating temperature at 1200°C until the heating time reaches 3 min. The electromagnetic induction coil 300 and the cooling assembly 800 are shut down to obtain the first product, the MOFs derivative.

[0123] Step 3: Cooling step: remove the reactor 200 and place it in alcohol at -78°C for 2 minutes, and the temperature of the reactor 200 drops below 30°C, thereby preparing the second product MIL-88A (Fe) derived Fe2O3 / Fe3O4 composite material.

[0124] The structure and morphology of the Fe2O3 / Fe3O4 composite material derived from MIL-88A(Fe) prepared in Example 3 were tested by XRD and SEM. Fig.11 is the XRD pattern of the Fe2O3 / Fe3O4 composite material derived from MIL-88A(Fe) prepared according to the preparation method of Example 3, Fig.11 It can be seen that the Fe2O3 / Fe3O4 composite material has good crystallinity, is pure and free of impurities, and correspondingly has a higher degree of defects and more active sites; Fig.12 is a SEM image of the Fe2O3 / Fe3O4 composite material derived from MIL-88A(Fe) prepared according to the preparation method of Example 3, Fig.12 In the experiment, the Fe2O3 / Fe3O4 composite material showed a regular and uniform nanoparticle morphology. It can be seen that the particle size of the Fe2O3 / Fe3O4 composite material was small and relatively uniform, and correspondingly had a larger specific surface area and better catalytic performance.

[0125] It can be seen that in Example 3, MIL-88A(Fe) is used as a MOFs precursor, and electromagnetic heating technology is adopted to prepare a MIL-88A(Fe)-derived Fe2O3 / Fe3O4 composite material, wherein the total time consumption of the electromagnetic induction heating step and the cooling step is approximately equal to 5 minutes, which is short in time, low in electricity consumption, high in yield and low in cost; at the same time, the prepared Fe2O3 / Fe3O4 composite material has a high degree of defects, more active sites, smaller particle size, higher uniformity and larger specific surface area, which makes the Fe2O3 / Fe3O4 composite material have better catalytic performance.

[0126] Example 4

[0127] Example 3 performs a pyrolysis reaction in an air atmosphere. The difference between Example 4 and Example 3 is that Example 4 performs a pyrolysis reaction in a nitrogen atmosphere. Specifically, compared with Example 3, Example 4 adds step ③ of introducing nitrogen into the reactor 200 for 20 minutes before step 2: electromagnetic induction heating step, so that the reactor 200 is in a nitrogen atmosphere; at the same time, nitrogen is continuously introduced into the reactor 200 in step 2 until the nitrogen is stopped after the cooling step in step 3 is completed, thereby using MIL-88A(Fe) as a MOFs precursor to prepare MIL-88A(Fe)-derived Fe / C material in a nitrogen atmosphere.

[0128] The structure and morphology of the Fe / C material derived from MIL-88A(Fe) prepared in Example 4 were tested by XRD and SEM. The test results are shown in Fig.13 and Fig.14 ,in, Fig.13is the XRD pattern of the Fe / C material derived from MIL-88A(Fe) prepared according to the preparation method of Example 4, Fig.14 is a SEM image of the Fe / C material derived from MIL-88A(Fe) prepared according to the preparation method of Example 4, Fig.13 and Fig.14 The characterization results prove that the Fe / C material derived from MIL-88A(Fe) synthesized in Example 4 has a regular and uniform nanoparticle morphology, is pure and free of impurities, has good hydrothermal stability, a certain defect structure and excellent catalytic performance.

[0129] Example 5

[0130] Using ZIF-8 as a MOFs precursor, the MOFs derivative material preparation device of the present application is used to prepare the ZIF-8 derived ZnO material by electromagnetic heating technology:

[0131] Step 1: Layout steps:

[0132] ① Place the MOFs precursor ZIF-8 after washing with anhydrous ethanol and centrifugation in a 60° C. oven and dry for 6 hours to obtain ZIF-8 powder; wherein the MOFs precursor ZIF-8 can be prepared according to the preparation method described in the literature (Chinese Chemical Letters, 2023, 34(2), 107425);

[0133] ② Place ZIF-8 powder in the crucible 100, then place the crucible 100 in the reactor 200, and adjust the height of the reactor 200 through the lifting assembly 600 so that it is located in the ring of the electromagnetic induction coil 300, and the crucible 100 is located in the central heating area of ​​the electromagnetic induction coil 300.

[0134] Step 2: Electromagnetic induction heating steps:

[0135] The heating power of the electromagnetic induction coil 300 is set to 12 kW, and the heating time is 3 min. The electromagnetic induction coil 300 and the cooling assembly 800 are both started and operated, and the crucible 100 is heated to 1200°C within 10 s. Then, the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback from the temperature detector 500 to maintain the heating temperature at 1200°C until the heating time reaches 3 min. The electromagnetic induction coil 300 and the cooling assembly 800 are shut down to obtain the first product, the MOFs derivative.

[0136] Step 3: Cooling step: remove the reactor 200 and place it in alcohol at -78°C for 2 minutes, and the temperature of the reactor 200 drops below 30°C, thereby preparing the second product ZIF-8-derived ZnO material.

[0137] The structure and morphology of the ZIF-8-derived ZnO material prepared in Example 5 were tested by XRD and SEM. The test results are shown in Fig.15 and Fig.16 ,in, Fig.15 is the XRD pattern of the ZIF-8 derived ZnO material prepared according to the preparation method of Example 5, Fig.16 is a SEM image of the ZIF-8 derived ZnO material prepared according to the preparation method of Example 5, Fig.15 and Fig.16 The characterization results prove that the ZIF-8-derived ZnO material prepared in Example 5 has a regular and uniform nanoparticle morphology, is pure and free of impurities, has good hydrothermal stability, a certain defect structure and excellent catalytic performance.

[0138] Example 6

[0139] Example 5 performs a pyrolysis reaction in an air atmosphere. The difference between Example 6 and Example 5 is that Example 6 performs a pyrolysis reaction in a nitrogen atmosphere. Specifically, compared with Example 5, Example 6 adds step ③ of introducing nitrogen into the reactor 200 for 20 minutes before step 2: electromagnetic induction heating step, so that the reactor 200 is in a nitrogen atmosphere; at the same time, nitrogen is continuously introduced into the reactor 200 in step 2 until the nitrogen is stopped after the cooling step in step 3 is completed, thereby using ZIF-8 as a MOFs precursor to prepare a ZIF-8-derived N / C material in a nitrogen atmosphere.

[0140] The structure and morphology of the ZIF-8-derived N / C material prepared in Example 6 were tested by XRD and SEM. The test results are shown in Fig.17 and Fig.18 ,in, Fig.17 is the XRD pattern of the ZIF-8 derived N / C material prepared according to the preparation method of Example 6, Fig.18 is a SEM image of the ZIF-8 derived N / C material prepared according to the preparation method of Example 6, Fig.17 and Fig.18 The characterization results prove that the ZIF-8-derived N / C material synthesized in Example 6 has a regular and uniform nanoparticle morphology, is pure and free of impurities, has good hydrothermal stability, a certain defect structure and excellent catalytic performance.

[0141] Among them, the manufacturer information of raw materials and components used in this application is shown in Table 1 and Table 2.

[0142] Table 1 Raw materials used and manufacturer information

[0143] Raw material name purity factory Methanol Analytical grade Beijing Chemical Plant Anhydrous ethanol Analytical grade Beijing Chemical Plant

[0144] Table 2 Parts used and manufacturer information

[0145] Device Name model factory XRD DX-2700-B Dandong Haoyuan Co., Ltd. SEM SU8020 Hitachi Corporation Centrifuge KH-20A Hunan Keda Scientific Instrument Co., Ltd. Diaphragm pumps KLP40 Kachuaner Fluid Technology (Shanghai) Co., Ltd. Oven DHG-9013A Shanghai Yiheng Scientific Instrument Co., Ltd.

[0146] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing a MOFs derivative material, characterized in that: The following steps are involved: Placing a MOFs precursor in a crucible (100) made of a conductive material, and placing the crucible (100) in a reactor (200); Electromagnetic induction heating is performed on the MOFs precursor by an electromagnetic induction coil (300) surrounding the reactor (200) to obtain a first product, wherein the heating temperature is 300° C. to 1300° C. and the heating time is 20 seconds to 10 minutes; The first product is cooled to a preset temperature to obtain a second product, a MOFs derivative material.

2. The preparation method according to claim 1, characterized in that: The heating time includes a heating time and a heat preservation time, wherein the heating time is 5s to 10s.

3. The preparation method according to claim 1, characterized in that: After obtaining the first product, the reactor (200) is placed in a coolant for cooling until the temperature of the first product drops below 30° C., thereby obtaining a second product, a MOFs derivative material; wherein the cooling time is 1 min to 2 min.

4. The preparation method according to claim 3, characterized in that: The coolant is alcohol.

5. The preparation method according to claim 1, characterized in that: Before placing the crucible (100) in the reactor (200) and subjecting the MOFs precursor to electromagnetic induction heating, an inert gas is first introduced into the reactor (200) to maintain an inert atmosphere therein until the second product MOFs derivative material is obtained.

6. A device for preparing MOFs derivative materials, characterized in that: The preparation method according to any one of claims 1 to 5 can be carried out, and the MOFs derivative material preparation device comprises a control unit (400) and a reactor (200), wherein the reactor (200) is surrounded by an electromagnetic induction coil (300), and the electromagnetic induction coil (300) is connected to the control unit (400); the reactor (200) is provided with a crucible (100) made of a conductive material, and the crucible (100) is located in the heating area of ​​the electromagnetic induction coil (300), and a temperature detector (500) is provided in the reactor (200), and the temperature detector (500) is used to detect the temperature of the crucible (100).

7. The MOFs derivative material preparation device according to claim 6, characterized in that: The outer diameter of the reactor (200) ranges from 10 mm to 500 mm, and the height ranges from 200 mm to 500 mm; the outer diameter of the reactor (200) is 10 mm to 20 mm smaller than the inner diameter of the electromagnetic induction coil (300).

8. The MOFs derivative material preparation device according to claim 6, characterized in that: The reactor (200) comprises a base (210) and a cover (220), the top surface of the base (210) comprises a central placement area, an inner ring area surrounding the central placement area, and an outer ring area surrounding the inner ring area, the bottom end surface of the cover (220) correspondingly abuts against the outer ring area; the temperature detector (500) is arranged in the inner ring area, and the crucible (100) is placed in the central placement area.

9. The MOFs derivative material preparation device according to claim 8, characterized in that: The top of the cover (220) is provided with an air outlet (221); the base (210) is provided with an air inlet (211), the air inlet (211) comprising a vertical hole section (211b) provided in the inner ring area and a horizontal hole section (211a) provided on the side wall of the base (210), the inner end of the horizontal hole section (211a) being connected to the bottom end of the vertical hole section (211b).

10. The MOFs derivative material preparation device according to claim 6, characterized in that: The MOFs derivative material preparation device further comprises a lifting component (600), and the reactor (200) is supported on a top support platform (610) of the lifting component (600).

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