MOFs derivative material heating reaction device and preparation equipment

Abstract

The utility model provides an MOFs derivative material heating reaction device and preparation equipment, and relates to the technical field of MOFs derivative material preparation. The heating reaction device comprises a lifting assembly and a reactor borne at the top of the lifting assembly, an electromagnetic induction coil surrounds the reactor, and an adjusting gap exists between the reactor and the electromagnetic induction coil; a crucible made of conductive materials is arranged in the reactor, the area where the electromagnetic induction coil is located is a first area in the axial direction of the electromagnetic induction coil, the area where the crucible is located is a second area, and the first area completely covers the second area. The preparation equipment comprises a control unit and the heating reaction device, wherein the electromagnetic induction coil of the heating reaction device is connected to the control unit. The heating reaction device and the preparation equipment for preparing the MOFs derivative material are convenient to operate, 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 utility model relates to the technical field of the preparation of MOFs derivative materials, in particular to a heating reaction device and a preparation device for MOFs derivative materials. Background Art

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

[0003] Among them, in the process of preparing MOFs derivative materials, it is necessary to pyrolyze MOFs precursors at pyrolysis temperature. Specifically, generally, a tube furnace / muffle furnace is used to prepare MOFs derivative materials by high-temperature pyrolysis method. However, the preparation process of the above tube furnace / muffle furnace not only has poor operation convenience, long time consumption, high energy consumption, low yield, but also the catalytic performance of the generated MOFs derivative materials is poor. Summary of the Utility Model

[0004] The purpose of the utility model is to provide a heating reaction device and a preparation device for MOFs derivative materials, so as to solve the technical problems of poor operation convenience, long time consumption, high energy consumption, low yield of the existing equipment for preparing MOFs derivative materials, and poor catalytic performance of the generated MOFs derivative materials.

[0005] To solve the above problems, the utility model provides a heating reaction device for MOFs derivative materials, which includes a lifting component and a reactor carried on the top of the lifting component. An electromagnetic induction coil is wound around the reactor, and there is an adjustment gap between the reactor and the electromagnetic induction coil. A crucible made of a conductive material is arranged inside the reactor. Along the axial direction of the electromagnetic induction coil, the area where the electromagnetic induction coil is located is the first area, and the area where the crucible is located is the second area, and the first area completely covers the second area.

[0006] Optionally, the crucible and the electromagnetic induction coil are coaxially arranged.

[0007] Optionally, the outer diameter of the reactor ranges from 10 mm to 500 mm, and the outer diameter of the reactor is 10 mm to 20 mm smaller than the inner diameter of the electromagnetic induction coil.

[0008] Optionally, the heating reaction device for MOFs derivative materials further includes a collector. The reactor is provided with an air inlet hole and an air outlet hole. Among them, the air inlet hole is used to connect an inert gas source, and the air outlet hole is connected with an air outlet pipe, and the air outlet end of the air outlet pipe extends into the collector.

[0009] Optionally, a temperature detector is provided inside the reactor, and the temperature detector is used to detect the temperature of the crucible.

[0010] 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 correspondingly 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.

[0011] Optionally, an air outlet is provided at the top of the cover; the base is provided with an air inlet hole, and the air inlet hole includes a vertical hole section arranged in the inner ring area and a horizontal hole section arranged on the side wall of the base. The inner end of the horizontal hole section communicates with the bottom end of the vertical hole section.

[0012] Optionally, the MOFs derivative material preparation device further includes a cooling component, and the cooling component is connected to the electromagnetic induction coil for cooling and temperature reduction of the electromagnetic induction coil.

[0013] The present utility model also provides a MOFs derivative material preparation device, which includes a control unit and the above-mentioned heating reaction device, and the electromagnetic induction coil of the heating reaction device is connected to the control unit.

[0014] Optionally, the control unit includes a housing and a control module accommodated in the housing. The housing is provided with a control panel, and both the control panel and the electromagnetic induction coil are connected to the control module; the housing is provided with heat dissipation holes or a first cooling fan;

[0015] And / or, the MOFs derivative material preparation device further includes a protection box. The control unit and the heating reaction device are both accommodated in the protection box, and the protection box is provided with a second cooling fan.

[0016] When the MOFs derivative material heating reaction device provided by the present utility model is applied to a MOFs derivative material preparation device for preparing MOFs derivative materials:

[0017] (1) During use, the lifting assembly 600 can be controlled to adjust the reactor 200 to rise or fall so that the reactor 200 is separated from above or below the electromagnetic induction coil 300, facilitating the loading of MOFs precursors, the taking out of MOFs derivative materials, and the installation and taking out of the crucible 100, thereby improving the use convenience of the heating reaction device; meanwhile, by adjusting the relative position of the reactor and the electromagnetic induction coil along the axial direction through the lifting assembly 600, it can be ensured that the crucible is located in the height area where the electromagnetic induction coil is located to ensure the effective heating of the crucible by the electromagnetic induction coil.

[0018] (2) During the heating process, the crucible is completely enclosed within the inner region of the electromagnetic induction coil. As a result, the alternating magnetic field lines generated by the electromagnetic induction coil act on the crucible with a relatively high density and magnetic flux, ensuring the heating effect of the electromagnetic induction coil on the crucible, improving the heating effect of the heating reaction device on the crucible and the MOF precursor therein, correspondingly reducing the heating time and increasing the yield.

[0019] (3) During the heating process, the electromagnetic induction coil can instantaneously raise the crucible 100 to the target temperature required for the sufficient pyrolysis of the MOF precursor and precisely maintain the target temperature for heat preservation heating of the MOF precursor. As a result, the MOF precursor that is not adversely affected by the heating-up process can rapidly nucleate and be fully pyrolyzed to completely form MOF derivatives at the target temperature. Moreover, the finally formed MOF derivative material has a higher degree of defects, smaller and more uniform particle sizes, correspondingly exhibiting more active sites and a higher specific surface area, thereby effectively improving the catalytic performance of the MOF derivative material.

[0020] (4) During the heating process, the electromagnetic induction coil heats up quickly and shortens the pyrolysis reaction time (i.e., the heat preservation time) of the MOF precursor, thus greatly reducing the heating time and increasing the preparation yield. At the same time, it effectively reduces the preparation energy consumption and cost; moreover, the electromagnetic heating technology is simple to operate, at normal temperature and pressure, safe and reliable, thus improving the convenience and safety of the preparation of the MOF derivative material.

[0021] (5) The reactor 200 is small in volume. In the cooling step, the reactor 200 can be directly placed in the coolant for rapid cooling, thereby quickly cooling the first product to the second product. This not only increases the defect richness of the formed second product, the MOF derivative material, and the number of active sites, improving the catalytic performance of the MOF derivative material, but also shortens the preparation time and further increases the yield. 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 will briefly introduce the drawings required for use in the description of the specific embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on these drawings.

[0023] Figure 1 Schematic diagram of the equipment for preparing MOF derivative materials provided by the embodiment of the present invention;

[0024] Figure 2 Schematic diagram of the layout of the lifting assembly, reactor, and crucible in the heating reaction device for MOF derivative materials provided by the embodiment of the present invention;

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

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

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

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

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

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

[0031] Figure 9 XRD pattern of the Co3O4 material, a ZIF-67-derived metal oxide material, prepared according to the preparation method of Example 2;

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

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

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

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

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

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

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

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

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

[0041] Explanation of reference numerals:

[0042] 100 - crucible; 200 - reactor; 210 - base; 211 - air inlet hole; 211a - horizontal hole section; 211b - vertical hole section; 212 - air inlet nozzle; 220 - cover; 221 - air outlet hole; 222 - air outlet nozzle; 230 - inlet pipe; 240 - outlet pipe; 250 - collector; 300 - electromagnetic induction coil; 400 - control unit; 410 - housing; 411 - control panel; 412 - heat dissipation holes; 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 implementation manners

[0043] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

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

[0045] In the description of the present utility model, it should be noted that unless otherwise clearly specified and defined, the terms "installation", "connection", and "coupling" 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 directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two components. For those of ordinary skill in the art, the specific meanings of the above terms in the present utility model can be understood according to specific circumstances.

[0046] This embodiment provides a heating reaction device for MOFs derivative materials, as Figure 1 and Figure 2 shown, including a lifting assembly 600 and a reactor 200 carried on the top of the lifting assembly 600. An electromagnetic induction coil 300 is wound around the reactor 200, and there is an adjustment gap between the reactor 200 and the electromagnetic induction coil 300; a crucible 100 made of a conductive material is disposed inside the reactor 200. Along the axial direction of the electromagnetic induction coil 300, the area where the electromagnetic induction coil 300 is located is the first region, and the area where the crucible 100 is located is the second region, and the first region completely covers the second region.

[0047] This embodiment also provides a preparation device for MOFs derivative materials, as Figure 1 shown, including a control unit 400 and the above heating reaction device, and the electromagnetic induction coil 300 of the heating reaction device is connected to the control unit 400.

[0048] When the heating reaction device for MOFs derivative materials provided by this embodiment is applied to a preparation device for MOFs derivative materials to prepare MOFs derivative materials, it may include an arrangement step, an electromagnetic induction heating step, and a cooling step, which are specifically as follows:

[0049] Arrangement step: The lifting assembly 600 adjusts the reactor 200 to be separated from the electromagnetic induction coil 300, places the MOFs precursor in the crucible 100 made of a conductive material, places the crucible 100 in the reactor 200, and then controls the lifting assembly 600 to adjust the reactor 200 to be inserted into the electromagnetic induction coil 300, and the crucible 100 is located within the height range where the electromagnetic induction coil 300 is located. The prepared MOFs precursor is used as a reaction material and loaded into the crucible 100, 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 material and the reaction equipment.

[0050] Electromagnetic induction heating step: The MOF precursor is heated by electromagnetic induction through the electromagnetic induction coil 300 surrounding the reactor 200 to obtain the first product. Among them, the heating temperature is 300 °C to 1300 °C, preferably 500 °C to 1200 °C; the heating duration is 20 s to 10 min, preferably 2 min to 4 min. There is an electromagnetic induction coil 300 surrounding the reactor 200. A high-frequency alternating current is applied to the electromagnetic induction coil 300. The alternating magnetic lines of force generated in the inner area of the electromagnetic induction coil 300 pass through the crucible 100. The crucible 100 cuts the alternating magnetic lines of force to generate a high eddy current, so that the temperature rises and serves as a heating medium to heat the MOF precursor therein to the target temperature.

[0051] Among them, in this application, the electromagnetic induction coil 300 is used to heat the crucible 100, which can enable the crucible 100 to instantaneously reach the target temperature required for the sufficient pyrolysis of the MOF precursor within a few seconds, thus effectively reducing the long time required for the crucible 100 to heat up to the target temperature, resulting in a large hindrance to the subsequent pyrolysis of the MOF precursor during the heating-up process, and the situation that the MOF precursor needs to be heated for a long time for heat preservation to fully pyrolyze; after the crucible 100 reaches the target temperature, the target temperature is maintained to heat the MOF precursor therein for heat preservation. Then, the MOF precursor that has not been affected by the adverse effects during the heating-up process can be rapidly and fully pyrolyzed at the target temperature within a short time to completely generate MOF derivatives. At this time, the obtained MOF derivatives are used as the first product.

[0052] Cooling step: The first product is cooled to a preset temperature to obtain the second product, the MOF derivative material. After the electromagnetic induction heating step reaches the heating duration, the generated first product has a high temperature. It is cooled to near room temperature. During the cooling process, the first product further undergoes reactions such as pyrolysis, thereby obtaining the required MOF derivative material. This MOF derivative material is used as the second product and also the final product.

[0053] After the cooling step is completed, the lifting assembly 600 is controlled to adjust the lifting of the reactor 200, so that the reactor 200 moves outside the electromagnetic induction coil 300, and then the crucible 100 can be conveniently taken out to obtain the required MOF derivative material.

[0054] Among them, when the MOF derivative material heating reaction device of this application is applied to a MOF derivative material preparation device for preparing MOF derivative materials:

[0055] (1) During use, the lifting assembly 600 can be controlled to adjust the reactor 200 to rise or fall so that the reactor 200 is separated from above or below the electromagnetic induction coil 300, facilitating the loading of MOF precursors, the extraction of MOF derivative materials, and the installation and extraction of the crucible 100, thereby improving the convenience of use of the heating reaction device; at the same time, by adjusting the relative position of the reactor and the electromagnetic induction coil along the axis through the lifting assembly 600, it can ensure that the crucible is located in the height area where the electromagnetic induction coil is located to ensure the effective heating of the crucible by the electromagnetic induction coil.

[0056] (2) During the heating process, when the crucible is completely wrapped in the inner area of the electromagnetic induction coil, the density and magnetic flux of the alternating magnetic field lines generated by the electromagnetic induction coil acting on the crucible are relatively large, thereby ensuring the heating effect of the electromagnetic induction coil on the crucible, improving the heating effect of the heating reaction device on the crucible and the MOF precursors therein, and correspondingly reducing the heating time and increasing the yield.

[0057] (3) During the heating process, the electromagnetic induction coil can instantaneously raise the crucible 100 to the target temperature required for the sufficient pyrolysis of the MOF precursors and precisely maintain the target temperature for heat preservation heating of the MOF precursors, so that the MOF precursors not affected by the adverse effects of the heating process can rapidly nucleate and be fully pyrolyzed to completely form MOF derivatives at the target temperature, and the finally formed MOF derivative materials have a higher degree of defects, smaller and more uniform particle sizes, correspondingly showing more active sites and a higher specific surface area, thereby effectively improving the catalytic performance of the MOF derivative materials.

[0058] (4) The electromagnetic induction coil heats up quickly during the heating process, and the pyrolysis reaction time of the MOF precursors, that is, the heat preservation time, is short, thus greatly shortening the heating time and increasing the preparation yield. At the same time, it effectively reduces the preparation energy consumption and preparation cost; at the same time, the electromagnetic heating technology is simple to operate, at normal temperature and pressure, safe and reliable, thereby improving the convenience and safety of the preparation of MOF derivative materials.

[0059] (5) The reactor 200 is small in volume, and in the cooling step, the reactor 200 can be directly placed in the coolant for rapid cooling, thereby realizing the rapid cooling of the first product to the second product. This not only improves the defect richness of the formation of the second product MOF derivative materials, increases the active sites, improves the catalytic performance of the MOF derivative materials, but also can shorten the preparation time and further increase the yield.

[0060] 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 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 so on.

[0061] 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, they are MIL - 88A(Fe), ZIF - 67, ZIF - 8 and MIL - 125. Correspondingly, the types of MOFs derivative materials that can be 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, they are metal oxides, metal - carbon composite materials and non - metal carbon materials, etc.

[0062] Specifically, in this embodiment, the crucible 100 and the electromagnetic induction coil 300 are coaxially arranged. Then, the maximum - density region of the alternating magnetic force lines formed in the region inside the electromagnetic induction coil 300 heats the crucible 100, thereby further increasing the magnetic flux acting on the crucible 100, ensuring the heating efficiency of the heating reaction device for the crucible 100 and the MOFs precursor therein, and correspondingly further reducing the heating time, increasing the yield and improving the catalytic performance of the prepared MOFs derivative materials.

[0063] Specifically, in this embodiment, the heating duration includes a temperature-rising duration and a heat-preserving duration. Among them, the temperature-rising duration is the time taken for the electromagnetic induction coil 300 to heat the crucible 100 from the start until it reaches the pyrolysis temperature at which the MOFs precursor can be fully pyrolyzed. Specifically, the temperature-rising duration is 5 s to 10 s, indicating that the electromagnetic induction technology can make the crucible 100 reach 300 °C to 1300 °C within 5 s to 10 s, instantaneously completing the temperature-rising process during the heating process; the heat-preserving duration is the time taken for the crucible 100 to maintain this temperature to heat the MOFs precursor after reaching the pyrolysis temperature until the MOFs precursor is fully pyrolyzed to completely generate the MOFs derivative. Specifically, the heat-preserving duration is 15 s to 10 min, indicating that the MOFs precursor not affected by the temperature-rising process can complete the full pyrolysis reaction within a relatively short time, quickly, efficiently, and with high quality to complete the preparation of the MOFs derivative material.

[0064] 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 the coolant for cooling until the temperature of the first product drops below 30 °C to obtain the second product, the MOFs derivative material; among them, the temperature-dropping duration is 1 min to 2 min. In this application, the reactor 200 used in the electromagnetic heating technology is small in volume 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 lifting assembly 600 can be used to adjust the lifting of the reactor 200 to separate it from the electromagnetic induction coil 300, and then the reactor 200 is removed from the lifting assembly 600 and placed in the coolant with a lower temperature for cooling treatment, so that the reactor 200, the crucible 100, and the first product can be quickly cooled to near room temperature within 1 min to 2 min. During this rapid temperature-dropping process, the first product, the MOFs derivative, can generate a richer defect structure to obtain the second product, the MOFs derivative material, correspondingly further improving the defect degree of the prepared MOFs derivative material, and further improving the richness of the active sites of the MOFs derivative material and the catalytic performance of the MOFs derivative material; at the same time, the temperature-dropping duration is only 1 min to 2 min, which can further improve its yield on the basis of improving the catalytic performance of the prepared MOFs derivative material.

[0065] Specifically, the coolant can be selected as alcohol, and the temperature of the alcohol can be -115 °C to -20 °C.

[0066] In this embodiment, according to the types of MOFs precursors and the required MOFs derivative materials, during the heating process, the atmosphere inside the reactor 200 can be an air atmosphere or an inert atmosphere. When it is necessary to set the atmosphere inside the reactor 200 to be an inert atmosphere, correspondingly, the arrangement step can also include setting the inert atmosphere inside the reactor 200. Specifically, before placing the crucible 100 inside the reactor 200 and performing electromagnetic induction heating on the MOFs precursor, that is, before the electromagnetic heating step, an inert gas is introduced into the reactor 200 to maintain an inert atmosphere inside it, and then the electromagnetic heating step is carried out until the second product, the MOFs derivative material, is obtained.

[0067] Optionally, in this embodiment, as Figure 2 shown, a temperature detector 500 is provided inside the reactor. The temperature detector 500 is used to detect the temperature of the crucible 100, and the temperature detector 500 is communicatively connected to the control unit 400. During use, after the arrangement step is completed, the control unit 400 controls the electromagnetic induction coil 300 to be powered on and applies high-frequency alternating current to it. A strong alternating magnetic field line is generated in the inner area of the loop of the electromagnetic induction coil 300, and the alternating magnetic field line with a large density in the axial center area can pass through the crucible 100 along the axis. A high eddy current is generated inside 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 feedback the detected temperature signal 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 according to the temperature signal feedback by the temperature detector 500 in real time, so that the crucible 100 maintains this target temperature to perform heat preservation heating on the MOFs precursor. Until the heating duration reaches the preset duration of 20 s to 10 min, the control disconnects the conduction between the electromagnetic induction coil 300 and the power supply, stops heating the crucible 100, and completes the electromagnetic induction heating step to obtain the first product. Subsequently, a cooling step is carried out to cool the first product to the preset temperature, thereby obtaining the second product, the MOFs derivative material.

[0068] Then the setting of the temperature detector 500 can effectively improve the precise control of the heating temperature of the crucible 100 by the electromagnetic induction coil 300, and correspondingly ensure the quality of the obtained MOFs derivative material.

[0069] 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 the MOFs derivative material, the reactor 200 in this embodiment is small in size, the electromagnetic induction coil 300 is small in volume and there is an adjustment gap between the electromagnetic induction coil 300 and the reactor 200; on the one hand, the whole preparation device is small in size, occupies little space and has low preparation cost; on the other hand, when performing the arrangement step, the reactor 200 can be taken out from within the electromagnetic induction coil 300 upward or downward, the crucible 100 can be 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, with a relatively high operation convenience; on the other hand, the reactor 200 is small in volume and is easy to be detached 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, with convenient operation and greatly improved cooling rate of the first product, and a second product MOFs derivative material with richer defect structures, more active sites and higher catalytic performance is obtained.

[0070] Specifically, the diameter of the electromagnetic induction coil 300 ranges from 20 mm to 500 mm, preferably 30 mm to 80 mm; the axial coverage range of the electromagnetic induction coil 300 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 axial height of the crucible 100 is 10 mm to 20 mm smaller than the axial coverage height of the electromagnetic induction coil 300.

[0071] In this embodiment, as 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 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. The top surface of the base 210 successively includes a central placement area, an annular inner ring area, and an annular outer ring area from the center along the radial direction. During use, the cover 220 can be removed upward, the crucible 100 is placed in the central placement area and is approximately coaxial with the base 210, and 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 therein, and the electromagnetic induction coil 300 surrounding the reactor 200 is approximately coaxial with the reactor 200 and the crucible 100, correspondingly ensuring the density of the alternating magnetic force lines acting on the crucible 100, ensuring the disassembly and assembly convenience of the reactor 200, the placement and removal convenience of the crucible 100, and the heating efficiency of the electromagnetic induction coil 300 on the crucible 100. Among them, the temperature detector 500 is arranged in the inner ring area, will not be damaged by collision with the cover 220, and can accurately detect the temperature of the crucible 100 close to the crucible 100, thereby dividing the radial area of the base 210, improving the layout compactness of each component, and further reducing the volume and space occupation of the reactor 200.

[0072] Among them, 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 covering the base 210, and at the same time ensure the sealing performance inside the reactor 200.

[0073] Specifically, the distance range between the temperature detector 500 and the crucible 100 is 10 mm to 20 mm, preferably 5 mm to 10 mm.

[0074] Optionally, in this embodiment, as Figure 2As shown, an air outlet hole 221 is provided at the top of the cover 220; the base 210 is provided with an air inlet hole 211, and the air inlet hole 211 includes a vertical hole section 211b provided in the inner ring area and a horizontal hole section 211a provided in the side wall of the base 210. The inner end of the horizontal hole section 211a communicates with the bottom end of the vertical hole section 211b. After completing the layout step, when it is necessary to adjust the inside of the reactor 200 to an inert atmosphere, the outer port of the horizontal hole section 211a can be connected to an inert gas source, and the inert gas source is opened to deliver inert gas to the horizontal hole section 211a. The inert gas then enters the vertical hole section 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 upwards, the air inside the reactor 200 is discharged upwards through the air outlet hole 221, making the inside of the reactor 200 an inert atmosphere, and ensuring that all areas of the reactor 200 are in an inert atmosphere, ensuring that the environment where the crucible 100 is located is an inert environment, and ensuring the effective reaction of the MOF precursor therein in an inert atmosphere; wherein, during the electromagnetic induction heating process, the inert gas source continuously passes inert gas into the reactor 200 through the air inlet hole 211 to maintain the inert atmosphere inside the reactor 200, further ensuring the full reaction of the MOF precursor in an inert atmosphere.

[0075] Preferably, the top end of the air outlet hole 221 is connected with an air outlet nozzle 222, and the outer end of the horizontal hole section 211a is connected with an air inlet nozzle 212. The air inlet nozzle 212 can be connected to an air inlet pipe 230 and communicated with 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 an air outlet pipe 240 and discharge the output gas to a designated position through the air outlet pipe 240.

[0076] Specifically, the inert gas source can be a gas cylinder 700, and a flow rate regulating valve 710 is provided at the air outlet of the gas cylinder 700, and the gas delivery flow rate of the gas cylinder 700 to the reactor 200 can be adjusted through the flow rate regulating valve 710.

[0077] Specifically, as Figure 1 shown, the MOF 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, an absorption solution is contained in the collector 250, the air outlet end of the air outlet pipe 240 is immersed in the absorption solution, and when the gas discharged from the air outlet pipe 240 passes through the absorption solution, the harmful substances therein can be absorbed by the absorption solution, and the purified gas is discharged upwards, thereby reducing the pollution to the environment and the like caused by the gas discharged from the air outlet pipe 240.

[0078] In this embodiment, the cover 220 can be made of transparent quartz glass material. The operator can clearly observe the reaction process inside the reactor 200 from the outside, thereby ensuring the operator's control of the preparation process.

[0079] In this embodiment, as Figure 1 shown, the MOFs derivative material preparation device further includes a cooling component 800, which is connected to the electromagnetic induction coil 300 and used to cool down the electromagnetic induction coil 300. During the electromagnetic induction heating process, the electromagnetic induction coil 300 can be continuously cooled by the cooling component 800 to reduce the occurrence of the situation that the electromagnetic induction coil 300 is burned out due to overheating, so as to ensure the normal heating operation of the electromagnetic induction coil 300 and the normal use of the preparation device.

[0080] Specifically, the cooling component 800 can be of the water-cooling type. The water-cooling component includes a water-cooling pipe 810 attached to the electromagnetic induction coil 300. The water inlet end 811 of the water-cooling pipe 810 is communicated with 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 of the water-cooling pipe 810 close to the cold water source or the water inlet end 811 of the water-cooling pipe 810. The start and stop of the water-cooling component are controlled by the pump 820; alternatively, the water inlet end 811 of the water-cooling pipe 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 pipe 810 can extend to a designated position for drainage.

[0081] Specifically, as Figure 1 shown, the control unit 400 includes a housing 410, a control module housed inside 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. An operator can perform control operations through the control panel 411; the housing 410 is provided with heat dissipation holes 412 and a first cooling fan 413. The heat generated during the operation of the control module can be discharged outwards through the heat dissipation holes 412 and the first cooling fan 413 to reduce the occurrence of the situation that the control module operates unstably or even crashes due to overheating, so as to ensure the normal operation of the control module.

[0082] In this embodiment, as Figure 1 shown, the MOFs derivative material preparation device further includes a protection box 900. The control unit 400, the reactor 200, the electromagnetic induction coil 300, the lifting component 600, and the collector 250 are all housed in the protection box 900. Then the protection box 900 can play an isolation and protection role for the above-mentioned components; preferably, the protection box 900 can be made of an insulating material to play an insulating protection role and reduce the occurrence of the situation that the electromagnetic induction coil 300 leaks electricity, thereby improving the use safety of the preparation device; alternatively, the protection box 900 can also be made of a material such as an iron sheet that can shield magnetic lines of force to reduce the adverse effects of the magnetic lines of force generated by the electromagnetic induction coil 300 during the heating process on the surrounding electronic components.

[0083] Preferably, the protection box 900 is provided with a second cooling fan 910 to dissipate the heat inside the protection box 900 and ensure the normal operation of the preparation equipment.

[0084] The application of the MOFs derivative material heating reaction device of the present utility model will be further described in detail below with reference to the accompanying drawings and embodiments.

[0085] Comparative example:

[0086] Using ZIF-67 as the MOFs precursor, a ZIF-67-derived metal / carbon composite Co / C material was prepared by high-temperature pyrolysis in a tube furnace:

[0087] Step 1: Arrangement step:

[0088] ① Place the MOFs precursor - ZIF-67 after methanol washing and centrifugation in an oven at 60 °C and dry for 6 hours to obtain ZIF-67 powder; among them, the MOFs precursor - ZIF-67 can be prepared according to the preparation method described in the literature "Chemical Engineering Journal, 2022, 450, 138082";

[0089] ② Place the ZIF-67 powder in a porcelain boat, and then place the porcelain boat in a tube furnace and seal both ends of the tube furnace;

[0090] ③ Introduce nitrogen into the tube furnace for 20 min to make the atmosphere in the tube furnace a nitrogen atmosphere.

[0091] Step 2: Tube furnace heating step:

[0092] Set the heating rate of the tube furnace to 5 °C / min, the pyrolysis temperature to 700 °C, and the pyrolysis time to 2 h; start the operation of the tube furnace, and keep introducing nitrogen into the tube furnace during the heating process until the tube furnace runs for a heating duration of 140 min and a heat preservation duration of 120 min to obtain the first product MOFs derivative.

[0093] Step 3: Cooling step: Set the cooling rate of the tube furnace to 5 °C / min, and let the first product cool naturally to 30 °C, then stop introducing nitrogen, thereby preparing the second product ZIF-67-derived metal / carbon composite Co-N / C material; among them, the actual cooling duration is greater than 134 min.

[0094] XRD, SEM, and BET were used to conduct relevant tests on the structure and morphology of the ZIF-67-derived metal / carbon composite Co / C material prepared in the comparative example: among them, Figure 3 is the XRD pattern of the ZIF-67-derived metal / carbon composite Co / C material prepared according to the preparation method of the comparative example. From Figure 3It 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 degree, and few active sites; Figure 4 Figure 2 is the SEM image of the Co / C material, a ZIF-67-derived metal / carbon composite material prepared by the preparation method of the comparative example; Figure 4 In it, the Co / C material has an irregular and uneven morphology and obvious large-scale agglomeration - large particle size. It can be seen that the Co / C material has a large and uneven particle size and a small specific surface area; Figure 5 Figure 3 is the BET image of the Co / C material, a ZIF-67-derived metal / carbon composite material prepared by the preparation method of the comparative example. According to Figure 5 the desorption isotherm located above and the adsorption isotherm located below in it, the software can analyze that the specific surface area of the Co / C material is only 8m 2 g -1 .

[0095] 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 was prepared by the high-temperature pyrolysis method in a tube furnace. The total time consumed in the heating step and the cooling step of the tube furnace is greater than 394 min, which is a long time-consuming. Both the electric energy consumption and the nitrogen energy consumption are large, the yield is low, and the cost is high; at the same time, the Co / C material prepared has a low defect degree, few active sites, a large, uneven particle size, and a small specific surface area, resulting in poor catalytic performance of the Co / C material.

[0096] Example 1

[0097] Using ZIF-67 as the MOFs precursor, the ZIF-67-derived metal / carbon composite material Co / C was prepared by the electromagnetic heating technology using the MOFs derivative material preparation equipment of the present application:

[0098] Step 1: Arrangement step:

[0099] ① The MOFs precursor - ZIF-67 after methanol washing and centrifugation was placed in an oven at 60 °C and dried for 6 hours to obtain ZIF-67 powder; among them, the MOFs precursor - ZIF-67 can be prepared by the preparation method recorded in the literature "Chemical Engineering Journal, 2022, 450, 138082";

[0100] ② The ZIF-67 powder was placed in the crucible 100, and then the crucible 100 was placed in the reactor 200. The height of the reactor 200 was adjusted by the lifting assembly 600 so that it was located inside the loop of the electromagnetic induction coil 300. At the same time, the crucible 100 was located in the central heating area of the electromagnetic induction coil 300;

[0101] ③ Introduce nitrogen into the reactor 200 for 20 min to create a nitrogen atmosphere in the tubular furnace.

[0102] Step 2: Electromagnetic induction heating step:

[0103] Set the heating power of the electromagnetic induction coil 300 to 12 kW and the heating duration to 3 min; both the electromagnetic induction coil 300 and the cooling component 800 are started and operated, and nitrogen is continuously introduced 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 thermometer 500 to maintain the heating temperature at 700 °C until the heating duration reaches 3 min. Then, stop the electromagnetic induction coil 300 and the cooling component 800 to obtain the first product, the MOFs derivative.

[0104] Step 3: Cooling step: Remove the reactor 200 and place it in alcohol at -78 °C for 2 min. When the temperature of the reactor 200 drops below 30 °C, stop introducing nitrogen into the reactor 200, thereby preparing the second product, the ZIF-67-derived metal / carbon composite Co / C material.

[0105] Use XRD, SEM, and BET to conduct relevant tests on the structure and morphology of the ZIF-67-derived metal / carbon composite Co / C material prepared in Example 1: Among them, Figure 6 is the XRD pattern of the ZIF-67-derived metal / carbon composite Co / C material prepared according to the preparation method of Example 1. It can be Figure 6 clearly seen that the characteristic peaks of Co can be observed. It can be seen that the intensity of the characteristic peaks of Co corresponding to the Co / C material is relatively high and the interference of noise peaks is relatively small, indicating that the Co-N / C material has good crystallinity, is pure and free of impurities, has a high degree of defects and a relatively large number of active sites, and also has good hydrothermal stability; at the same time, it can be seen that Figure 6 the peak intensity of C in Figure 3 is greatly enhanced compared to that in the comparative example, indicating that Figure 6 the Co / C material has more defects generated and correspondingly has more active sites.

[0106] Figure 7 is 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 Figure 8 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 relatively small and uniform, and correspondingly has a relatively large specific surface area and good catalytic performance. is the BET diagram of the ZIF-67-derived metal / carbon composite Co / C material prepared according to the preparation method of Example 1. According toFigure 8 The desorption / adsorption isotherm can be analyzed by software, and the specific surface area of the Co / C material can reach 330 m2 g-1. Compared with the Co / C material derived from ZIF-67 prepared by the traditional tube furnace pyrolysis method, the BET results prove that the Co / C material derived from ZIF-67 synthesized by the method of the present utility model has a larger BET specific surface area, which is 330 m 2 g -1 , providing better active sites and improving the subsequent catalytic performance.

[0107] It can be seen that in Example 1, ZIF-67 is used as the MOFs precursor, and under a nitrogen atmosphere, the ZIF-67-derived metal / carbon composite material Co / C material is prepared by electromagnetic heating technology. The total time consumed by the electromagnetic induction heating step and the cooling step is about 5 minutes, with short time consumption, less power consumption, high yield and low cost. At the same time, the prepared Co / C material has a high degree of defects, many active sites, small particle size, high uniformity and large specific surface area, making the Co / C material have better catalytic performance.

[0108] Example 2

[0109] Using ZIF-67 as the MOFs precursor, the ZIF-67-derived metal oxide material Co3O4 material is prepared by electromagnetic heating technology using the MOFs derivative material preparation equipment of the present application:

[0110] Step 1: Arrangement step:

[0111] ① The MOFs precursor-ZIF-67 after methanol washing and centrifugation is placed in an oven at 60 °C and dried for 6 hours to obtain ZIF-67 powder. Among them, the MOFs precursor-ZIF-67 can be prepared according to the preparation method described in the literature "Chemical Engineering Journal, 2022, 450, 138082";

[0112] ② The ZIF-67 powder is placed in the crucible 100, and then the crucible 100 is placed in the reactor 200, and the height of the reactor 200 is adjusted by the lifting assembly 600 so that it is located inside the ring of the electromagnetic induction coil 300, and at the same time, the crucible 100 is located in the central heating area of the electromagnetic induction coil 300.

[0113] Step 2: Electromagnetic induction heating step:

[0114] Set the heating power of the electromagnetic induction coil 300 to 12 kW and the heating duration to 3 min; both the electromagnetic induction coil 300 and the cooling component 800 are started and operated. The crucible 100 is heated to 1200 °C within 10 s, and then the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback of the thermometer 500 to maintain the heating temperature at 1200 °C until the heating duration reaches 3 min. Then, the electromagnetic induction coil 300 and the cooling component 800 are shut down to obtain the first product, the MOFs derivative.

[0115] Step 3: Cooling step: Remove the reactor 200 and place it in alcohol at -78 °C for 2 min. The temperature of the reactor 200 drops below 30 °C, thereby preparing the second product, the ZIF-67-derived metal oxide material Co3O4 material.

[0116] XRD and SEM are used to perform relevant detections on the structure and morphology of the ZIF-67-derived metal oxide material Co3O4 material prepared in Example 2: Among them, Figure 9 is the XRD pattern of the ZIF-67-derived metal oxide material Co3O4 material prepared according to the preparation method of Example 2. From Figure 9 it can be seen that the characteristic peak intensity of Co corresponding to the Co3O4 material is relatively high and the noise peak interference is less, indicating that the Co-N / C 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 10 is the SEM image of the ZIF-67-derived metal oxide material Co3O4 material prepared according to the preparation method of Example 2. Figure 10 In it, the Co3O4 material shows a regular and uniform nanometer particle morphology. It can be seen that the particle size of the Co3O4 material is small and relatively uniform, and correspondingly has a large specific surface area and good catalytic performance.

[0117] It can be seen that in Example 2, ZIF-67 is used as the MOFs precursor, and the ZIF-67-derived metal oxide material Co3O4 material is prepared by electromagnetic heating technology. Among them, the total time consumption of the electromagnetic induction heating step and the cooling step is approximately equal to 5 min, the time consumption is short, the electric energy consumption is small, the yield is high, and the cost is low; at the same time, the Co3O4 material prepared has a high degree of defects, a large number of active sites, a small particle size, a high degree of uniformity, and a large specific surface area, making the catalytic performance of the Co3O4 material better.

[0118] Example 3

[0119] Using MIL-88A(Fe) as the MOFs precursor, the MIL-88A(Fe)-derived Fe2O3 / Fe3O4 composite material is prepared by electromagnetic heating technology using the MOFs derivative material preparation equipment of the present application:

[0120] Step 1: Arrangement step:

[0121] ① Place the MOFs precursor - MIL - 88A(Fe) after being washed with absolute ethanol and centrifuged in an oven at 60 °C for 6 hours to obtain MIL - 88A(Fe) powder; among them, the MOFs precursor - MIL - 88A(Fe) can be prepared according to the preparation method described in the literature (Chemical Engineering Journal, 2021, 426, 131927).

[0122] ② Place the MIL - 88A(Fe) powder in crucible 100, then place crucible 100 in reactor 200, and adjust the height of reactor 200 through lifting component 600 so that it is located within the loop of electromagnetic induction coil 300, and at the same time crucible 100 is located in the central heating area of electromagnetic induction coil 300.

[0123] Step 2: Electromagnetic induction heating step:

[0124] Set the heating power of electromagnetic induction coil 300 to 12 kW and the heating duration to 3 min; both electromagnetic induction coil 300 and cooling component 800 are started and run. Crucible 100 is heated to 1200 °C within 10 s, and then the heating power of electromagnetic induction coil 300 is adjusted according to the temperature feedback by temperature detector 500 to keep the heating temperature at 1200 °C until the heating duration reaches 3 min. Then stop electromagnetic induction coil 300 and cooling component 800 to obtain the first product, the MOFs derivative.

[0125] Step 3: Cooling step: Remove reactor 200 and place it in alcohol at - 78 °C for 2 min. The temperature of reactor 200 drops below 30 °C, thereby preparing the second product, the Fe2O3 / Fe3O4 composite material derived from MIL - 88A(Fe).

[0126] XRD and SEM are used to conduct relevant tests on the structure and morphology, etc. of the Fe2O3 / Fe3O4 composite material derived from MIL - 88A(Fe) prepared in Example 3: among them, Figure 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. It can be seen from Figure 11 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; Figure 12 is the SEM image of the Fe2O3 / Fe3O4 composite material derived from MIL - 88A(Fe) prepared according to the preparation method of Example 3, Figure 12In it, the Fe2O3 / Fe3O4 composite material exhibits a regular and uniform nanoparticle morphology. It can be seen that the Fe2O3 / Fe3O4 composite material has a small and relatively uniform particle size, and correspondingly has a large specific surface area and good catalytic performance.

[0127] It can be seen that in Example 3, MIL-88A(Fe) was used as the MOFs precursor, and the MIL-88A(Fe)-derived Fe2O3 / Fe3O4 composite material was prepared by electromagnetic heating technology. The total time consumed in the electromagnetic induction heating step and the cooling step is approximately equal to 5 minutes, with short time consumption, low power consumption, high yield and low cost. At the same time, the prepared Fe2O3 / Fe3O4 composite material has a high degree of defects, many active sites, a small particle size, high uniformity and a large specific surface area, making the catalytic performance of the Fe2O3 / Fe3O4 composite material better.

[0128] Example 4

[0129] The pyrolysis reaction in Example 3 was carried out in an air atmosphere. The difference between Example 4 and Example 3 is that the pyrolysis reaction in Example 4 was carried out in a nitrogen atmosphere. Specifically, compared with Example 3, in Example 4, step ③ was added before step 2: the electromagnetic induction heating step, in which nitrogen was introduced into the reactor 200 for 20 minutes to make the atmosphere in the reactor 200 a nitrogen atmosphere. At the same time, nitrogen was continuously introduced into the reactor 200 in step 2 until the nitrogen supply was stopped after the completion of step 3: the cooling step, so as to prepare the MIL-88A(Fe)-derived Fe / C material in a nitrogen atmosphere using MIL-88A(Fe) as the MOFs precursor.

[0130] XRD and SEM were used to detect the structure and morphology of the MIL-88A(Fe)-derived Fe / C material prepared in Example 4. The detection results are shown in Figure 13 and Figure 14 , where Figure 13 is the XRD pattern of the MIL-88A(Fe)-derived Fe / C material prepared according to the preparation method of Example 4, Figure 14 is the SEM image 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 prove that the MIL-88A(Fe)-derived Fe / C material 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.

[0131] Example 5

[0132] Using ZIF-8 as the MOFs precursor, the ZIF-8-derived ZnO material is prepared by the electromagnetic heating technology with the MOFs derivative material preparation equipment of the present application:

[0133] Step 1: Arrangement step:

[0134] ① Place the MOFs precursor - ZIF-8 after being washed with absolute ethanol and centrifuged in an oven at 60 °C for 6 hours to obtain ZIF-8 powder; among them, the MOFs precursor - ZIF-8 can be prepared according to the preparation method recorded in the literature (Chinese Chemical Letters, 2023, 34(2), 107425);

[0135] 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 through the lifting component 600 so that it is located inside the loop of the electromagnetic induction coil 300, and at the same time the crucible 100 is located in the central heating area of the electromagnetic induction coil 300.

[0136] Step 2: Electromagnetic induction heating step:

[0137] Set the heating power of the electromagnetic induction coil 300 to 12 kW and the heating duration to 3 min; both the electromagnetic induction coil 300 and the cooling component 800 are started and run. The crucible 100 is heated to 1200 °C within 10 s, and then the heating power of the electromagnetic induction coil 300 is adjusted according to the temperature feedback by the thermometer 500 to keep the heating temperature at 1200 °C until the heating duration reaches 3 min. Then, stop the electromagnetic induction coil 300 and the cooling component 800 to obtain the first product MOFs derivative.

[0138] Step 3: Cooling step: Remove the reactor 200 and place it in alcohol at -78 °C for 2 min. The temperature of the reactor 200 drops below 30 °C, thereby preparing the second product ZIF-8-derived ZnO material.

[0139] The structure and morphology of the ZIF-8-derived ZnO material prepared in Example 5 are detected by XRD and SEM. The detection results are shown in Figure 15 and Figure 16 , where 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 the SEM pattern of the ZIF-8-derived ZnO material prepared according to the preparation method of Example 5, Figure 15 and Figure 16The 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.

[0140] Example 6

[0141] In Example 5, the pyrolysis reaction was carried out in an air atmosphere. The difference between Example 6 and Example 5 is that in Example 6, the pyrolysis reaction was carried out in a nitrogen atmosphere. Specifically, compared with Example 5, in Example 6, step ③ was added before step 2: the electromagnetic induction heating step to introduce nitrogen into the reactor 200 for 20 min to make the atmosphere in the reactor 200 a nitrogen atmosphere; at the same time, nitrogen was continuously introduced into the reactor 200 in step 2 until the nitrogen supply was stopped after the completion of step 3: the cooling step. Thus, using ZIF-8 as the MOF precursor, a ZIF-8-derived N / C material was prepared under a nitrogen atmosphere.

[0142] XRD and SEM were used to detect the structure and morphology of the ZIF-8-derived N / C material prepared in Example 6. The detection results are shown in Figure 17 and Figure 18 respectively, where 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 the 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 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.

[0143] Among them, the manufacturer information of the raw materials and components used in this application is shown in Table 1 and Table 2.

[0144] Table 1 Manufacturer Information of Raw Materials Used

[0145] Raw material name Purity Manufacturer Methanol Analytical reagent Beijing Chemical Plant Absolute ethanol Analytical reagent Beijing Chemical Plant

[0146] Table 2 Manufacturer Information of Components Used

[0147] Equipment name Model Manufacturer XRD DX-2700-B Dandong Haoyuan Co., Ltd. SEM SU8020 Hitachi, Ltd. (Japan) Centrifuge KH-20A Hunan Kaida Scientific Instrument Co., Ltd. Diaphragm pump KLP40 Kachuaner Fluid Technology (Shanghai) Co., Ltd. Oven DHG-9013A Shanghai Yiheng Scientific Instrument Co., Ltd.

[0148] 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 foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some or all of the technical features; and 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 heating reaction device for MOFs derivative materials, characterized in that It includes a lifting component (600) and a reactor (200) carried on the top of the lifting component (600). An electromagnetic induction coil (300) is wound around the reactor (200), and there is an adjustment gap between the reactor (200) and the electromagnetic induction coil (300). A crucible (100) made of a conductive material is arranged inside the reactor (200). Along the axial direction of the electromagnetic induction coil (300), the area where the electromagnetic induction coil (300) is located is the first area, and the area where the crucible (100) is located is the second area, and the first area completely covers the second area.

2. The MOFs derivative material heating reaction device according to claim 1, characterized in that The crucible (100) and the electromagnetic induction coil (300) are coaxially arranged.

3. The MOFs derivative material heating reaction device according to claim 1, characterized in that, The outer diameter of the reactor (200) ranges from 10 mm to 500 mm, 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).

4. The MOFs derivative material heating reaction device according to claim 1, wherein The MOFs derivative material heating reaction device further includes a collector (250). The reactor (200) is provided with an air inlet hole (211) and an air outlet hole (221). Among them, the air inlet hole (211) is used to connect to an inert gas source, the air outlet hole (221) is connected to an air outlet pipe (240), and the air outlet end of the air outlet pipe (240) extends into the collector (250).

5. The MOFs derivative material heating reaction device according to claim 1, characterized in that, A thermometer (500) is arranged inside the reactor, and the thermometer (500) is used to detect the temperature of the crucible (100).

6. The MOFs derivative material heating reaction device according to claim 5, characterized in that, 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) correspondingly abuts against the outer ring area. The thermometer (500) is arranged in the inner ring area, and the crucible (100) is placed in the central placement area.

7. The MOFs derivative material heating reaction device according to claim 6, wherein, 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). The air inlet hole (211) includes a vertical hole section (211b) arranged in the inner ring area and a horizontal hole section (211a) arranged on the side wall of the base (210). The inner end of the horizontal hole section (211a) communicates with the bottom end of the vertical hole section (211b).

8. The MOFs derivative material heating reaction device according to claim 1, characterized in that, The MOFs derivative material preparation equipment further includes a cooling component (800). The cooling component (800) is connected to the electromagnetic induction coil (300) and is used to cool down the electromagnetic induction coil (300).

9. A preparation device for MOFs derivative materials, characterized in that, It includes a control unit (400) and the heating reaction device according to any one of claims 1-8. The electromagnetic induction coil (300) of the heating reaction device is connected to the control unit (400).

10. The MOFs derivative material preparation device according to claim 9, characterized in that The control unit (400) includes a housing (410) and a control module accommodated in the housing (410). The housing is provided with a control panel (411), and both the control panel (411) and the electromagnetic induction coil (300) are connected to the control module; the housing (410) is provided with heat dissipation holes (412) or a first cooling fan (413); And / or, the MOFs derivative material preparation device further includes a protection box (900). The control unit (400) and the heating reaction device are both accommodated in the protection box (900), and the protection box is provided with a second cooling fan (910).

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