Preparation method and device of MOFs derivative material

Abstract

The application provides a MOFs derivative material preparation method and device, and relates to the technical field of MOFs derivative material preparation. The MOFs derivative material preparation method comprises the following steps: placing MOFs precursors in a crucible made of conductive material, and placing the crucible in a reactor; performing electromagnetic induction heating on the MOFs precursors by an electromagnetic induction coil surrounding the reactor to obtain a first product, wherein the heating temperature is 300 DEG C to 1300 DEG C, and the heating duration is 20 s to 10 min; and cooling the first product to a preset temperature to obtain a second product, i.e., a MOFs derivative material. The MOFs derivative material prepared by the preparation method has the advantages of short preparation time, low energy consumption, high yield, and good catalytic performance.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of MOFs derivative material preparation, and in particular to a MOFs derivative material preparation method and device. BACKGROUND

[0002] Metal-Organic Frameworks (MOFs) derivative materials are widely used in adsorption, catalysis, drug loading, sensing, energy, antibacterial and other fields due to the advantages of adjustable porosity, super large specific surface area, rich active sites and high water / thermal stability.

[0003] In the process of preparing the MOFs derivative material, the MOFs precursor needs to be pyrolyzed at a pyrolysis temperature. Specifically, the existing preparation methods mainly include a water / solvent thermal method and a tube furnace / muffle furnace high-temperature pyrolysis method. However, the above preparation methods need a long heating time to reach the pyrolysis temperature of the MOFs precursor, which causes the MOFs precursor to react during the heating process and greatly hinders the subsequent pyrolysis. A long time of heat preservation is needed to make the MOFs precursor fully pyrolyze, which not only consumes a long time, a large amount of energy and has a low yield, but also causes the generated MOFs derivative material to have a low degree of defects, a small number of active sites, a large particle size, a low uniformity and a small specific surface area, and thus the catalytic performance of the MOFs derivative material is poor. SUMMARY

[0004] The application aims to provide a MOFs derivative material preparation method and device to solve the technical problems of long time consumption, large energy consumption, low yield and poor catalytic performance of the generated MOFs derivative material in the existing preparation of the MOFs derivative material.

[0005] To solve the above problems, the application provides a MOFs derivative material preparation method, which comprises the following steps:

[0006] The MOFs precursor is placed in a crucible made of conductive material, and the crucible is placed in a reactor.

[0007] The MOFs precursor is subjected to electromagnetic induction heating by an electromagnetic induction coil surrounding the reactor to obtain a first product, wherein the heating temperature is 300 DEG C to 1300 DEG C, and the heating time is 20 s to 10 min.

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

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

[0010] Optionally, after obtaining the first product, the reactor is placed in a cooling liquid for cooling until the temperature of the first product is reduced to below 30℃, obtaining a second product MOFs derivative material; wherein the cooling time is 1min-2min.

[0011] Optionally, the cooling liquid is alcohol.

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

[0013] The application also provides a MOFs derivative material preparation device capable of performing the above preparation method, comprising a control unit and a reactor, wherein an electromagnetic induction coil is arranged around the reactor, the electromagnetic induction coil is connected to the control unit; an electrically conductive crucible is arranged in the reactor, the crucible is located in the heating area of the electromagnetic induction coil, and a temperature detector is arranged in the reactor, the temperature detector is used to detect the temperature of the crucible.

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

[0015] Optionally, the reactor comprises a base and a cover, the top surface of the base 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 corresponds to the abutment of the outer ring area; the temperature detector is arranged in the inner ring area, and the crucible is arranged in the central placement area.

[0016] Optionally, the top of the cover is provided with a gas outlet hole; the base is provided with a gas inlet hole, the gas inlet hole comprises a vertical hole section arranged in the inner ring area and a horizontal hole section arranged on the side wall of the base, and the inner end of the horizontal hole section is communicated with the bottom end of the vertical hole section.

[0017] Optionally, the MOFs derivative material preparation device further comprises a lifting assembly, and the reactor is carried on the top carrying table of the lifting assembly.

[0018] The preparation method provided by the application uses electromagnetic heating technology to heat and keep warm 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) Electromagnetic heating technology heats up quickly during the heating process, and shortens the thermal decomposition reaction time, i.e., the holding time, of the MOFs precursor, thereby greatly shortening the heating time, improving the preparation yield, and 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 embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the specific embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any 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 device for preparing MOFs derivative materials provided in an embodiment of the present invention;

[0025] 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;

[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 the ZIF-67 derived metal / carbon composite material Co / C material prepared according to the preparation method of the comparative example;

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

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

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

[0031] Figure 9 XRD pattern of ZIF-67 derived metal oxide material Co304 material prepared according to the preparation method of Example 2;

[0032] Figure 10 SEM image of ZIF-67 derived metal oxide material Co304 material prepared according to the preparation method of Example 2;

[0033] Figure 11 XRD pattern of MIL-88A(Fe) derived Fe203 / Fe304 composite material prepared according to the preparation method of Example 3;

[0034] Figure 12 SEM image of MIL-88A(Fe) derived Fe203 / Fe304 composite material prepared according to the preparation method of Example 3;

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

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

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

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

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

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

[0041] Explanation of reference signs:

[0042] 100 - crucible; 200 - reactor; 210 - base; 211 - gas inlet hole; 211a - horizontal hole section; 211b - vertical hole section; 212 - gas inlet nozzle; 220 - cover; 221 - gas outlet hole; 222 - gas outlet nozzle; 230 - gas inlet pipe; 240 - gas outlet pipe; 250 - collector; 300 - electromagnetic induction coil; 400 - control unit; 410 - housing; 411 - control panel; 412 - heat dissipation hole; 413 - first heat dissipation fan; 500 - temperature detector; 600 - lifting assembly; 610 - top bearing table; 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 heat dissipation fan. DETAILED DESCRIPTION

[0043] The technical solutions of the present application will be described clearly and completely below in conjunction with the drawings. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

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

[0045] In the description of the present application, it should be noted that unless otherwise explicitly specified and limited, the terms "mounting", "connecting", "connection" should be understood broadly, for example, it can be fixed connection, or detachable connection, or integrally connected; it can be mechanical connection, or electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, or the internal communication of two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0046] The embodiment provides a preparation method of MOFs derivative material, which comprises arrangement, electromagnetic induction heating and cooling steps, and specifically as follows.

[0047] The arrangement step is as follows: MOFs precursors are placed in a crucible 100 made of conductive material, and the crucible 100 is placed in a reactor 200. The prepared MOFs precursors are loaded into the crucible 100 as reaction materials, and the crucible 100 is made of conductive material capable of being heated by electromagnetic induction; then the crucible 100 containing the MOFs precursors is placed in the reactor 200, so that the arrangement of the reaction materials and the reactor materials is completed.

[0048] The electromagnetic induction heating step is as follows: the MOFs precursors are heated by electromagnetic induction through an electromagnetic induction coil 300 surrounding the reactor 200 to obtain first products, wherein the heating temperature is 300-1300 DEG C, preferably 500-1200 DEG C; and the heating time is 20 s-10 min, preferably 2 min-4 min. The reactor 200 is surrounded by the electromagnetic induction coil 300, high-frequency alternating current is applied to the electromagnetic induction coil 300, and the alternating magnetic lines of force generated in the ring region of the electromagnetic induction coil 300 pass through the crucible 100, so that the crucible 100 cuts the alternating magnetic lines of force to generate high eddy current, thereby the temperature is increased to heat the MOFs precursors in the crucible 100 to the target temperature.

[0049] In the preparation method, the crucible 100 is heated by the electromagnetic induction coil 300, so that the crucible 100 can reach the target temperature required for the MOFs precursors to be sufficiently pyrolyzed in a few seconds, thereby effectively reducing the long time required for the crucible 100 to reach the target temperature, and the MOFs precursors are not affected by the adverse effects of the heating process, so that the MOFs precursors can be rapidly and sufficiently pyrolyzed at the target temperature in a short time to completely generate the MOFs derivative, and the MOFs derivative obtained at this time is the first product.

[0050] The cooling step is as follows: the first product is cooled to a preset temperature to obtain a second product MOFs derivative material. After the electromagnetic induction heating step reaches the heating time, the first product generated has a high temperature, and is cooled to near room temperature. During the cooling process, the first product further pyrolyzes and reacts, so that the required MOFs derivative material is obtained, and the MOFs derivative material is also the final product as the second product.

[0051] In the preparation method, the MOFs precursors are heated and kept warm by electromagnetic heating technology to prepare the MOFs derivative material.

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

[0053] (2) The electromagnetic heating technology has a fast heating rate in the heating process, and makes the pyrolysis reaction time of the MOFs precursor, i.e. the heat preservation time, shorter, thereby greatly shortening the heating time, improving the preparation yield, and effectively reducing the preparation energy consumption and cost.

[0054] (3) The electromagnetic heating technology is simple to operate, safe and reliable at normal temperature and pressure, thereby improving the preparation convenience and safety of the MOFs derivative material.

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

[0056] Specifically, the MOFs precursor includes but is 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 composites or functional group modified materials, preferably MIL-88A (Fe), ZIF-67, ZIF-8, and MIL-125, and accordingly, the types of MOFs derivative materials prepared by using the preparation method of the present application are metal oxides, metal-carbon composite materials, metal sulfides, metal selenides, metal phosphides, and non-metal carbon materials, etc., preferably metal oxides, metal-carbon composite materials, and non-metal carbon materials, etc.

[0057] Specifically, in the present embodiment, the heating time includes a heating-up time and a holding time, wherein the heating-up time is the time used for the electromagnetic induction coil 300 to heat the crucible 100 from the start to the temperature at which the MOFs precursor is fully pyrolyzed, and specifically, the heating-up time is 5s-10s, indicating that the electromagnetic induction technology can make the crucible 100 reach 300-1300℃ within 5s-10s, and instantaneously complete the heating-up process in the heating process; the holding time is the time used for the crucible 100 to keep the pyrolysis temperature after reaching the pyrolysis temperature to heat the MOFs precursor until the MOFs precursor is fully pyrolyzed to completely generate the MOFs derivative, and specifically, the holding time is 15s-10min, indicating that the MOFs precursor, which is not affected by the heating-up process, can complete the full pyrolysis reaction within a short time, and quickly, efficiently, and with high quality complete the preparation of the MOFs derivative material.

[0058] In this embodiment, after the first product is obtained by the electromagnetic induction heating step, the reactor 200 is placed in the cooling liquid for cooling until the temperature of the first product is reduced to below 30°C to obtain the second product MOFs derivative material; wherein the cooling time is 1-2 min. The reactor 200 used in the electromagnetic heating technology in this application is small in size and separated from the electromagnetic induction coil 300. After the first product is generated by heating the MOFs precursor by the electromagnetic induction coil 300, the reactor 200 can be taken out of the electromagnetic induction coil 300 and placed in a cooling liquid with a lower temperature for cooling treatment, so that the reactor 200, the crucible 100 and the first product are rapidly cooled to near room temperature within 1-2 min. In this rapid cooling process, the first product MOFs derivative can produce more abundant defect structures to obtain the second product MOFs derivative material, which further improves the defect degree of the prepared MOFs derivative material, and further improves the activity site abundance of the MOFs derivative material and the catalytic performance of the MOFs derivative material. At the same time, the cooling time is only 1-2 min, which can further improve the yield of the MOFs derivative material on the basis of improving the catalytic performance of the prepared MOFs derivative material.

[0059] Specifically, the cooling liquid can be alcohol, and the alcohol temperature can be -115°C to -20°C.

[0060] In this embodiment, according to the type of MOFs precursor and the required MOFs derivative material, the reactor 200 can be in an air atmosphere or an inert atmosphere during the heating process. When it is required to set the reactor 200 to an inert atmosphere, the setting step can also include the setting of 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, i.e. before the electromagnetic heating step, the 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 capable of performing the above preparation method, as shown in Figure 1 The MOFs derivative material preparation device includes a control unit 400 and a reactor 200, and 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 provided 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 the reactor 200 is provided with a temperature detector 500 for detecting the temperature of the crucible 100.

[0062] During use, after completing the arrangement step, the electromagnetic induction coil 300 is wound around the outside of the reactor 200 with a certain gap between the two. 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. 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. 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 the detected temperature 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] A cooling step is then 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 prepare MOFs derivative materials. In addition to having the technical effects of (1)-(3) above, it also has the advantages of simple structure and small size, thereby further improving the operational convenience 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 the 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 the MOFs derivative material, the size of the reactor 200 in the embodiment is small, 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, small in space occupation and low in preparation cost; on the other hand, when the arrangement step is performed, the reactor 200 can be taken out from the electromagnetic induction coil 300 upward or downward, the crucible 100 is taken out from the reactor 200, then the MOFs precursor is loaded into the crucible 100, then the crucible 100 is loaded into the reactor 200, and finally the reactor 200 is inserted into the electromagnetic induction coil 300 again, which is high in operation convenience; on the other hand, the reactor 200 is small in size and convenient to disengage from the electromagnetic induction coil 300, when the cooling step is performed, the reactor 200 can be directly taken out and immersed into the cooling liquid for rapid cooling treatment, which is convenient in operation and greatly improves the cooling rate of the first product, so that the second product MOFs derivative material is obtained, which is rich in defect structure, rich in active site and high in catalytic performance.

[0066] Specifically, the diameter of the electromagnetic induction coil 300 ranges from 20 mm to 500 mm, and preferably ranges from 30 mm to 80 mm; the coverage range of the electromagnetic induction coil 300 along the axial direction ranges from 50 mm to 500 mm, and preferably ranges from 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 along the axial direction is 10 mm to 20 mm smaller than the coverage height of the electromagnetic induction coil 300 along the axial direction.

[0067] In the embodiment, as shown in FIG. 1, the reactor 200 is a cylinder, and the electromagnetic induction coil 300 is a cylinder with a smaller diameter than the reactor 200. Figure 2As shown, the reactor 200 can specifically adopt the following structure: 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, and the bottom end surface of the cover 220 corresponds to abut 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. The top surface of the base 210 comprises the central placement area, the annular inner ring area, and the annular outer ring area in sequence from the center radially outward, in use, the cover 220 can be taken down upward, the crucible 100 is placed in the central placement area and is approximately coaxial with the base 210, then the cover 220 is covered on the top surface of the base 210 corresponding to the outer ring area, so that the crucible 100 is covered in it, and the electromagnetic induction coil 300 surrounding the reactor 200 is approximately coaxial with the reactor 200 and the crucible 100, which correspondingly ensures the density of the alternating magnetic lines of force acting on the crucible 100, ensures the disassembly and assembly convenience of the reactor 200, the taking and placing convenience of 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 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 each component, and further reducing the volume and space occupation of the reactor 200.

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

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

[0070] Specifically, the distance between the temperature detector 500 and the crucible 100 is in the range of 10mm-20mm, preferably 5mm-10mm.

[0071] Optionally, in the embodiment, as shown in FIG. 1, 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, and the bottom end surface of the cover 220 corresponds to abut 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. Figure 2As shown, the top of the cover 220 is provided with an air outlet hole 221; the base 210 is provided with an air inlet hole 211, which includes a vertical hole section 211b arranged in the inner ring area and a horizontal hole section 211a arranged in the sidewall of the base 210, and the inner end of the horizontal hole section 211a is communicated with the bottom end of the vertical hole section 211b. After the arrangement step is completed, when it is necessary to adjust the inert atmosphere in the reactor 200, the outer port of the horizontal hole section 211a can be connected to an inert gas source, and the inert gas source is started to deliver inert gas to the horizontal hole section 211a, which in turn enters the vertical hole section 211b and enters the reactor 200 through the top port thereof. As the inert gas gradually fills all the internal space of the reactor 200 from the bottom area, the air in the reactor 200 is discharged upward through the air outlet hole 221, so that the reactor 200 is in an inert atmosphere, and the entire area of the reactor 200 can be ensured to be in an inert atmosphere, ensuring that the environment of the crucible 100 is inert, and ensuring that the MOFs precursor in it can effectively react in an inert atmosphere. During the electromagnetic induction heating process, the inert gas source continuously introduces inert gas into the reactor 200 through the air inlet hole 211 to maintain the inert atmosphere in the reactor 200, further ensuring the sufficient reaction of the MOFs precursor in the inert atmosphere.

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

[0073] Specifically, the inert gas source can be a gas cylinder 700, and the gas outlet of the gas cylinder 700 is provided with a flow rate adjusting valve 710, which can be used to adjust the gas flow rate of the gas cylinder 700 to the reactor 200.

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

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

[0076] Optionally, as shown in Figure 1 and Figure 2 , the MOFs derivative material preparation device further comprises a lifting assembly 600, and the reactor 200 is carried on the top carrying table 610 of the lifting assembly 600. In use, the lifting assembly 600 can be controlled to adjust the top carrying table 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 loading 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 the cover 220 is covered, the lifting assembly 600 adjusts the top carrying table 610 and the reactor 200 to fall or rise to be inserted into the electromagnetic induction coil 300, thereby improving the operation convenience of the arrangement step.

[0077] In this embodiment, as shown in Figure 1 , the MOFs derivative material preparation device further comprises a cooling assembly 800 connected to the electromagnetic induction coil 300 for cooling the electromagnetic induction coil 300. During the electromagnetic induction heating step, the electromagnetic induction coil 300 can be continuously cooled by the cooling assembly 800 to reduce the occurrence of overheating and burning of the electromagnetic induction coil 300, thereby ensuring the normal heating operation of the electromagnetic induction coil 300 and the normal use of the preparation device.

[0078] Specifically, the cooling assembly 800 can be in the form of water cooling, and the water cooling assembly comprises a water cooling pipe 810 attached to the electromagnetic induction coil 300. The water inlet end 811 of the water cooling pipe 810 is connected to a cold water source, and a pump 820 such as a diaphragm pump 820 or a peristaltic pump 820 is arranged on the pipe section close to the cold water source or the water inlet end 811 of the water cooling pipe 810 to control the start and stop of the water cooling assembly; or the water inlet end 811 of the water cooling pipe 810 is connected to a faucet to control the water flow; at the same time, the water outlet end 812 of the water cooling pipe 810 can be extended to a designated position for drainage.

[0079] Specifically, as shown in Figure 1 , the control unit 400 comprises a housing 410, a control module accommodated in the housing 410, and a control panel 411 embedded in the housing 410. The control module is communicatively connected to the electromagnetic induction coil 300, the temperature detector 500, and the control panel 411, and an operator can control the operation through the control panel 411. The housing 410 is provided with a heat dissipation hole 412 and a first heat dissipation fan 413, and the heat generated by the operation of the control module can be discharged outward through the heat dissipation hole 412 and the first heat dissipation fan 413, thereby reducing the occurrence of unstable operation or even shutdown of the control module due to high temperature, and ensuring the normal operation of the control module.

[0080] In this embodiment, as shown in Figure 1 The MOFs derivative material preparation device further comprises a protection box 900, the control unit 400, the reactor 200, the electromagnetic induction coil 300, the lifting assembly 600 and the collector 250 are all accommodated in the protection box 900, and the protection box 900 can isolate and protect the above-mentioned components; preferably, the protection box 900 can be made of insulating material to play an insulating protection role, reduce the occurrence of the electromagnetic induction coil 300 leakage, and thus improve the use safety of the preparation device; alternatively, the protection box 900 can also be made of iron sheet or other materials capable of shielding magnetic lines to reduce the adverse effects of the magnetic lines generated by the electromagnetic induction coil 300 on surrounding electronic elements during the heating process.

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

[0082] The application will be further described in detail in combination with the drawings and embodiments.

[0083] Comparative example:

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

[0085] Step 1: arrangement step:

[0086] ①The MOFs precursor-ZIF-67 after methanol washing and centrifugation was placed in a 60°C oven for drying for 6 hours to obtain ZIF-67 powder; wherein the MOFs precursor-ZIF-67 can be prepared according to the preparation method recorded in the literature “Chemical Engineering Journal, 2022, 450, 138082”;

[0087] ②The ZIF-67 powder was placed in a porcelain boat, and then the porcelain boat was placed in a tubular furnace, and the two ends of the tubular furnace were closed.

[0088] ③Nitrogen was introduced into the tubular furnace for 20 min to make the tubular furnace in a nitrogen atmosphere.

[0089] Step 2: tubular furnace heating step:

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

[0091] Step 3: Cooling step: set the cooling rate of the tube furnace at 5℃ / min, the first product is naturally cooled to 30℃, stop the nitrogen flow, thereby preparing the second product ZIF-67 derived metal / carbon composite Co-N / C material; wherein the actual cooling time is greater than 134 min.

[0092] The structure and morphology of the ZIF-67 derived metal / carbon composite Co / C material prepared by the preparation method of the comparative example are detected by XRD, SEM and BET: wherein, Figure 3 The XRD pattern of the ZIF-67 derived metal / carbon composite Co / C material prepared according to the preparation method of the comparative example is shown in Figure 2, wherein, Figure 3 It can be seen that the characteristic peak intensity of Co and C corresponding to the Co / C material is poor, indicating that the crystallinity of the Co / C material is poor, the defect degree is low, and the active point is less; Figure 4 The SEM pattern of the ZIF-67 derived metal / carbon composite Co / C material prepared according to the preparation method of the comparative example is shown in Figure 3, wherein, Figure 4 The Co / C material has irregular, uneven morphology and obvious large agglomeration-particle size, and the particle size of the Co / C material is large and uneven, and the specific surface area is small; Figure 5 The BET pattern of the ZIF-67 derived metal / carbon composite Co / C material prepared according to the preparation method of the comparative example is shown in Figure 4, wherein, Figure 5 The desorption isotherm on the upper side and the adsorption isotherm on the lower side in Figure 4 can be analyzed by software to obtain that the specific surface area of the Co / C material is only 8m 2 g -1 .

[0093] It can be seen that the comparative example uses ZIF-67 as the MOFs precursor, and the ZIF-67 derived metal / carbon composite Co / C material is prepared by the tube furnace high-temperature pyrolysis method, wherein the total time of the tube furnace heating step and the cooling step is greater than 394 min, the time is long, the power consumption and the nitrogen energy consumption are large, the yield is low, the cost is high; At the same time, the defect degree of the prepared Co / C material is low, the active point is less, the particle size is large and uneven, and the specific surface area is small, resulting in poor catalytic performance of the Co / C material.

[0094] Example 1

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

[0096] Step 1: Arrangement step:

[0097] ①The MOFs precursor-ZIF-67 after methanol washing and centrifugation is placed in a 60℃ oven for drying for 6 hours to obtain ZIF-67 powder; wherein, the MOFs precursor-ZIF-67 can be prepared according to the preparation method recorded in the literature “Chemical Engineering Journal, 2022, 450, 138082”;

[0098] ②The ZIF-67 powder is placed in the crucible 100, then the crucible 100 is placed in the reactor 200, and the height of the reactor 200 is adjusted to be located in the ring of the electromagnetic induction coil 300 by the lifting assembly 600, at the same time, the crucible 100 is located in the central heating area of the electromagnetic induction coil 300;

[0099] ③Nitrogen is introduced into the reactor 200 for 20 min, so that the tube furnace is in a nitrogen atmosphere.

[0100] Step 2: Electromagnetic induction heating step:

[0101] The heating power of the electromagnetic induction coil 300 is set to 12kW, and the heating time is 3min; the electromagnetic induction coil 300 and the cooling assembly 800 are both started and operated, and nitrogen is introduced into the reactor 200 during the heating process; the crucible 100 is heated to 700℃ within 10s, then the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback of the temperature detector 500 to maintain the heating temperature at 700℃, until the heating time reaches 3min, the electromagnetic induction coil 300 and the cooling assembly 800 are turned off, and the first product MOFs derivative is obtained.

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

[0103] The structure and morphology of the ZIF-67 derivative derived metal / carbon composite Co / C material prepared in Example 1 are detected by XRD, SEM and BET: wherein, Figure 6 is the XRD pattern of the ZIF-67 derivative derived metal / carbon composite Co / C material prepared according to the preparation method of Example 1, and Figure 6 It can be seen that the characteristic peak of Co is obvious, the characteristic peak intensity of Co corresponding to the Co / C material is high and the noise peak interference is less, indicating that the Co-N / C material has good crystallinity, purity without impurities, high defect degree, more active points, and good hydrothermal stability; at the same time, it can be seen that Figure 6 the peak intensity of C in the comparative example Figure 3The peak intensity of the middle C is greatly enhanced, indicating that Figure 6 The Co / C material has more defects and more active sites.

[0104] Figure 7 The SEM image of the ZIF-67-derived metal / carbon composite Co / C material prepared according to the preparation method of Example 1, Figure 7 In the middle, the Co / C material has regular and uniform extremely small nanoparticle morphology, and no obvious agglomeration is generated, which shows that the particle size of the Co / C material is small and uniform, and accordingly has a large specific surface area and good catalytic performance. Figure 8 The BET image of the ZIF-67-derived metal / carbon composite Co / C material prepared according to the preparation method of Example 1, Figure 8 According to the desorption isotherm, the specific surface area of the Co / C material can be analyzed by software to reach 330 m2 g-1. Compared with the ZIF-67-derived Co / C material prepared by the traditional tube furnace pyrolysis method, the BET result proves that the ZIF-67-derived Co / C material synthesized by the method of the application has a larger BET specific surface area of 330 m 2 g -1 , which provides more active sites and improves the subsequent catalytic performance.

[0105] As can be seen, Example 1 uses ZIF-67 as the MOFs precursor, and the ZIF-67-derived metal / carbon composite Co / C material is prepared by electromagnetic heating technology under a nitrogen atmosphere, wherein the total time of the electromagnetic induction heating step and the cooling step is about 5 min, the time is short, the power consumption is low, the yield is high, and the cost is low; at the same time, the Co / C material prepared has high defect degree, more active sites, small particle size, high uniformity and large specific surface area, so that the Co / C material has good catalytic performance.

[0106] Example 2

[0107] ZIF-67 is used as the MOFs precursor, and the ZIF-67-derived metal oxide material Co3O4 material is prepared by electromagnetic heating technology using the MOFs derivative material preparation device of the application:

[0108] Step 1: Arrangement step:

[0109] ① The MOFs precursor-ZIF-67 after methanol washing and centrifugation is placed in a 60℃ oven for drying for 6 hours to obtain ZIF-67 powder; wherein the MOFs precursor-ZIF-67 can be prepared according to the preparation method recorded in the literature "Chemical Engineering Journal, 2022, 450, 138082";

[0110] 2. Put the ZIF-67 powder into the crucible 100, then place the crucible 100 into the reactor 200, and adjust the height of the reactor 200 to be within the ring of the electromagnetic induction coil 300 by the lifting assembly 600, while the crucible 100 is located in the central heating area of the electromagnetic induction coil 300.

[0111] Step 2: Electromagnetic induction heating step:

[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, the crucible 100 is heated to 1200℃ within 10s, then the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback of the temperature detector 500 to maintain the heating temperature at 1200℃, until the heating time reaches 3 min, the electromagnetic induction coil 300 and the cooling assembly 800 are closed and stopped, and the first product MOFs derivative is obtained.

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

[0114] The structure and morphology of the ZIF-67 derived metal oxide material Co3O4 material prepared in Example 2 are detected by XRD and SEM: wherein, Figure 9 The XRD pattern of the ZIF-67 derived metal oxide material Co3O4 material prepared according to the preparation method of Example 2 is shown in FIG. 2, wherein Figure 9 It can be seen that the characteristic peak intensity of Co of the Co3O4 material is high and the noise peak interference is less, indicating that the Co-N / C material has good crystallinity, no impurities, and high defect degree, more active points; Figure 10 The SEM pattern of the ZIF-67 derived metal oxide material Co3O4 material prepared according to the preparation method of Example 2 is shown in FIG. 3, Figure 10 In FIG. 3, the Co3O4 material exhibits a regular and uniform nanoparticle morphology, and the particle size of the Co3O4 material is small and uniform, which corresponds to a large specific surface area and good catalytic performance.

[0115] It can be seen that, in Example 2, ZIF-67 is used as a MOFs precursor, and a ZIF-67 derived metal oxide material Co3O4 material is prepared by using electromagnetic heating technology. The total time of the electromagnetic induction heating step and the cooling step is about 5 minutes, which is short in time and low in power consumption. The yield is high, and the cost is low. At the same time, the prepared Co3O4 material has high defect degree, more active sites, small particle size, high uniformity and large specific surface area, so that the catalytic performance of the Co3O4 material is better.

[0116] Example 3

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

[0118] Step 1: arrangement step:

[0119] ① Place the MOFs precursor MIL-88A(Fe) washed with anhydrous ethanol and centrifuged in a 60°C oven 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 the 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 to be located in the ring of the electromagnetic induction coil 300 by the lifting assembly 600, and at the same time the crucible 100 is located in the central heating area of the electromagnetic induction coil 300.

[0121] Step 2: electromagnetic induction heating step:

[0122] The heating power of the electromagnetic induction coil 300 is set to 12kW, and the heating time is 3min; the electromagnetic induction coil 300 and the cooling assembly 800 are both started and run, the crucible 100 is heated to 1200℃ within 10s, then the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback of the temperature detector 500 to maintain the heating temperature at 1200℃, until the heating time reaches 3min, the electromagnetic induction coil 300 and the cooling assembly 800 are closed and stopped, and the first product MOFs derivative is obtained.

[0123] Step 3: cooling step: remove the reactor 200 and place it in alcohol at-78℃ for 2min, and the temperature of the reactor 200 is reduced to below 30℃, thereby preparing the second product MIL-88A(Fe) derived Fe2O3 / Fe3O4 composite material.

[0124] The structure and morphology of the MIL-88A(Fe) derived Fe2O3 / Fe3O4 composite material prepared in Example 3 were detected by XRD and SEM, wherein, Figure 11 is the XRD pattern of the MIL-88A(Fe) derived Fe2O3 / Fe3O4 composite material prepared according to the preparation method of Example 3, and Figure 11 It can be seen that the Fe2O3 / Fe3O4 composite material has good crystallinity, is pure and free of impurities, and has a high degree of defects and a large number of active sites; Figure 12 is the SEM pattern of the MIL-88A(Fe) derived Fe2O3 / Fe3O4 composite material prepared according to the preparation method of Example 3, Figure 12 In the figure, the Fe2O3 / Fe3O4 composite material exhibits a regular and uniform nanoparticle morphology, and it can be seen that the Fe2O3 / Fe3O4 composite material has a small and uniform particle size, and accordingly has a large specific surface area and good catalytic performance.

[0125] It can be seen that, in Example 3, MIL-88A(Fe) is used as the MOFs precursor, and the MIL-88A(Fe) derived Fe2O3 / Fe3O4 composite material is prepared by electromagnetic heating technology, wherein the total time of the electromagnetic induction heating step and the cooling step is about 5 min, the time consumption is short, the power consumption is low, the yield is high, and the cost is low; at the same time, the Fe2O3 / Fe3O4 composite material has a high degree of defects, a large number of active sites, a small particle size, a high uniformity and a large specific surface area, so that the Fe2O3 / Fe3O4 composite material has good catalytic performance.

[0126] Example 4

[0127] Example 3 is carried out under air atmosphere, and the difference between Example 4 and Example 3 is that Example 4 is carried out under nitrogen atmosphere. Specifically, compared with Example 3, Example 4 adds step ③ of introducing nitrogen into the reactor 200 for 20 min before step 2: the 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 introduction is stopped after the completion of the cooling step in step 3, so that the MIL-88A(Fe) derived Fe / C material is prepared under a nitrogen atmosphere by using MIL-88A(Fe) as the MOFs precursor.

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

[0129] Example 5

[0130] ZIF-8 derived ZnO material was prepared by using ZIF-8 as the MOFs precursor and using the MOFs derivative material preparation device of the application by electromagnetic heating technology:

[0131] Step 1: arrangement step:

[0132] ① Place the MOFs precursor-ZIF-8 washed with anhydrous ethanol and centrifuged in a 60℃ oven for 6 hours to obtain ZIF-8 powder; wherein the MOFs precursor-ZIF-8 can be prepared according to the preparation method recorded in the literature (Chinese Chemical Letters, 2023, 34(2), 107425);

[0133] ② Place the ZIF-8 powder in the crucible 100, then place the crucible 100 in the reactor 200, and adjust the height of the reactor 200 to be located in the ring of the electromagnetic induction coil 300 by the lifting assembly 600, and at the same time the crucible 100 is located in the central heating area of the electromagnetic induction coil 300.

[0134] Step 2: electromagnetic induction heating step:

[0135] Set the heating power of the electromagnetic induction coil 300 to 12kW, and the heating time to 3min; the electromagnetic induction coil 300 and the cooling assembly 800 are both started and operated, the crucible 100 is heated to 1200℃ within 10s, then the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback of the temperature detector 500 to maintain the heating temperature at 1200℃, until the heating time reaches 3min, the electromagnetic induction coil 300 and the cooling assembly 800 are closed and stopped, and the first product MOFs derivative is obtained.

[0136] Step 3: cooling step: remove the reactor 200 and place it in alcohol at-78℃ for 2min, and the temperature of the reactor 200 is reduced to below 30℃, 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 Figure 2. Figure 15 and Figure 16 ,in, Figure 15 is the XRD pattern of the ZIF-8 derived ZnO material prepared according to the preparation method of Example 5, Figure 16 is a SEM image of the ZIF-8 derived ZnO material prepared according to the preparation method of Example 5, Figure 15 and Figure 16 The characterization results show 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 under an air atmosphere. The difference between Example 6 and Example 5 is that Example 6 performs a pyrolysis reaction under a nitrogen atmosphere. Specifically, compared with Example 5, Example 6 adds step ③ before step 2: electromagnetic induction heating step, introducing nitrogen into the reactor 200 for 20 minutes to make the reactor 200 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 under 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. Figure 17 and Figure 18 ,in, Figure 17 is the XRD pattern of the ZIF-8 derived N / C material prepared according to the preparation method of Example 6, Figure 18 is a SEM image of the ZIF-8 derived N / C material prepared according to the preparation method of Example 6, Figure 17 and Figure 18 The characterization results show 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] The manufacturer information of the 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 Analytically pure Beijing Chemical Plant Anhydrous ethanol Analytically pure Beijing Chemical Plant

[0144] Table 2 Component and Vendor Information

[0145] Equipment name Model Factory XRD DX-2700-B Dandong Haoyuan Co., Ltd. SEM SU8020 Hitachi, Ltd. Centrifuge KH-20A Hunan Kaida Scientific Instruments Co., Ltd. Diaphragm pump KLP40 Carter Flow Technology (Shanghai) Co., Ltd. Oven DHG-9013A Shanghai Yiheng Scientific Instruments Co., Ltd.

[0146] Finally, it should be noted that the above embodiments are merely used to illustrate the technical solutions of the present application, and are not intended to limit the present application; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacements for some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A device for preparing MOFs derivative materials, characterized in that: The MOFs derivative material preparation device comprises a control unit (400) and a reactor (200), wherein the reactor (200) comprises a base (210) and a cover (220) detachably connected to the base (210), wherein 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 base (210) is provided with an air inlet (211), wherein the air inlet (211) comprises a vertical hole section (211b) provided in the inner ring area and a horizontal hole section (211a) provided on a side wall of the base (210), wherein the inner end of the horizontal hole section (211a) is connected to the bottom end of the vertical hole section (211b); the bottom end surface of the cover (220) is correspondingly abutted against the outer ring area, and the top of the cover (220) is provided with an air outlet (221); The reactor (200) is surrounded by an electromagnetic induction coil (300), and the outer diameter of the reactor (200) is 10 mm to 20 mm smaller than the inner diameter of the electromagnetic induction coil (300). The electromagnetic induction coil (300) is coaxially arranged with the reactor (200) and the crucible (100), and the electromagnetic induction coil (300) is connected to the control unit (400). The reactor (200) is equipped with a crucible (100) made of a conductive material, and the crucible (100) is placed in the central placement area. A temperature detector (500) is provided in the inner ring area, and the temperature detector (500) is used to detect the temperature of the crucible (100).

2. The MOFs derivative material preparation device according to claim 1, 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.

3. The MOFs derivative material preparation device according to claim 1, characterized in that: The MOFs derivative material preparation device further comprises a lifting component (600), and the reactor (200) is supported on a top supporting platform (610) of the lifting component (600).

4. A method for preparing a MOFs derivative material, characterized in that: The MOFs derivative material preparation device according to any one of claims 1 to 3 is used, and the preparation method comprises the following steps: Placing a MOFs precursor in a crucible (100) made of a conductive material, and placing the crucible (100) in a reactor (200); The first product is obtained by electromagnetic induction heating the MOFs precursor by an electromagnetic induction coil (300) surrounding the reactor (200), wherein the heating temperature is 300° C. to 1300° C. and the heating time is 20 seconds to 10 minutes; The electromagnetic induction coil (300) is wound outside the reactor (200), and the outer diameter of the reactor (200) is 10 mm to 20 mm smaller than the inner diameter of the electromagnetic induction coil (300); after obtaining the first product, the reactor (200) is taken out from the electromagnetic induction coil (300), and the reactor (200) is placed in a coolant for cooling until the temperature of the first product drops below 30°C, so as to obtain a second product, a MOFs derivative material, wherein the coolant is alcohol with a temperature of -115°C to -20°C, and the cooling time is 1 min to 2 min.

5. The preparation method according to claim 4, characterized in that The heating time includes a heating time and a heat preservation time, wherein the heating time is 5s to 10s.

6. The preparation method according to claim 4, characterized in that The crucible (100) is placed in the reactor (200) and before the MOFs precursor is subjected 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.

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