Process device for preparing graphene
By designing the process device of microwave units and adopting the microwave graphene production process with pneumatic conveying and infrared temperature measurement modules, the problems of high energy consumption and batch production in the existing technology are solved, and high-quality and low-cost continuous production and large-scale applications are achieved.
Patent Information
- Application Number
- CN202421711797.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-18
- Publication Date
- 2025-07-11
- Estimated Expiration
- 2034-07-18
AI Technical Summary
The existing microwave graphene production process has problems such as high power, high temperature, easy aging, batch production, large energy consumption, and inability to achieve continuous production, resulting in high production costs and low output, making it difficult to apply on a large scale on industrial scale.
A process device including a microwave unit is designed, including a feed section, a microwave section and a discharge section. A pneumatic conveying module and an infrared temperature measurement module are used to modify and expand graphite intercalation by microwave cavity to achieve continuous production, reducing energy consumption and equipment footprint.
It has achieved low energy consumption, pollution-free and continuous production, high quality, defect-free and large output, reducing equipment costs and manpower demand, and simplifying the operation process.
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Figure CN223087604U_ABST
Abstract
Description
Technical Field
[0001] The present application relates to a process device for preparing graphene and belongs to the technical field of graphene. Background Art
[0002] Due to the two-dimensional few-layer crystal structure of graphene, it exhibits excellent electron transport ability and thermal conductivity. Graphene has broad application prospects in the fields of humanoid robots, new energy batteries, functional coatings, conductive inks, rubber tires, lubricating oils, etc. Along with the discovery of graphene, the preparation methods of graphene have also become the main research directions in this industry.
[0003] The mainstream graphene preparation methods include the graphite oxide reduction method (Hummers method) and the chemical vapor deposition method (CVD method). In the Hummers method, graphite is first oxidized into graphite oxide with strong oxidants such as concentrated sulfuric acid, concentrated nitric acid, and potassium permanganate, then exfoliated into graphene oxide by ultrasonic treatment, and finally purified and reduced by dialysis to obtain graphene powder. The Hummers method has a long process cycle, serious pollution, and the obtained graphene has the disadvantages of many defects and poor quality, which limits its application in high-end scenarios. The CVD method can prepare high-quality graphene, but has the disadvantages of complex process and high cost, making it difficult to be applied industrially on a large scale.
[0004] Microwave exfoliation method graphene refers to using the huge energy released by the gasification effect generated by microwaves to exfoliate graphite sheets to prepare graphene. Moreover, this preparation method has the advantages of high efficiency and environmental friendliness, and shows great potential in the field of large-scale rapid preparation of graphene.
[0005] The existing microwave method graphene production process has problems such as high power (above 20 kW), high temperature (about 500 °C), easy aging (plastic reactors are not resistant to high temperatures), batch production (pulse feeding, static sintering, with a certain waiting time), large energy consumption, inability to achieve continuous production, relatively low output, and some production processes require atmosphere protection during operation. These problems greatly increase the production cost of graphene and severely restrict the output of graphene. Summary of the Utility Model
[0006] In order to solve the problems existing in the prior art, the present application proposes a new microwave method graphene production device.
[0007] In one aspect of the present application, a process device for preparing graphene is provided, and the process device includes a microwave unit;
[0008] The microwave unit includes a feeding section, a microwave section, and a discharging section that are horizontally connected in sequence;
[0009] The feeding section includes a horizontally arranged microwave suppression tube I. The fixed end of the microwave suppression tube I is communicated with the microwave section, and an air inlet pipe is arranged in the microwave suppression tube I;
[0010] The feeding section further includes a feeding pipe, the feeding pipe is communicated with the air inlet pipe, and the feeding port I of the feeding pipe is located above the microwave suppression tube I; the air inlet pipe is provided with an air inlet and an air outlet;
[0011] The microwave section is provided with a microwave cavity, and a microwave irradiation area is arranged in the microwave cavity; an expansion tube is arranged in the microwave cavity, and the air outlet is communicated with the expansion tube;
[0012] The discharging section includes a horizontally arranged microwave suppression tube II. The fixed end of the microwave suppression tube II is communicated with the microwave section, a discharging pipe is arranged in the microwave suppression tube II, the feeding port II of the discharging pipe is communicated with the expansion tube, and the free end of the discharging pipe is provided with a discharging port.
[0013] Optionally, with the microwave cavity as the horizontal line and the air inlet as the starting point, in the clockwise direction, the inclination angles of the air inlet pipe, the feeding pipe, and the discharging pipe satisfy:
[0014] The inclination angle of the air inlet pipe is 0° to 90° or 270° to 360°;
[0015] The inclination angle of the feeding pipe is 45° to 90°;
[0016] The inclination angle of the discharging pipe is 120° to 240°.
[0017] Optionally, the process device further includes a pneumatic conveying module, and the pneumatic conveying module is communicated with the air inlet.
[0018] Optionally, in the process device,
[0019] The cross-sectional area of the air inlet pipe is 0.5 to 3 cm 2 ;
[0020] The cross-sectional area of the feeding pipe is 0.5 to 3 cm 2 ;
[0021] The cross-sectional area of the expansion tube is 1 to 30 cm 2 ;
[0022] The cross-sectional area of the discharging pipe is 1 to 30 cm 2 .
[0023] Optionally, in the process device, the air inlet pipe, the feed pipe, the expansion pipe and the discharge pipe are connected to form a material flow bin. The material of the material flow bin is quartz, ceramic, etc., preferably quartz. Preferably, the cross-sectional areas of the feed pipe, the air inlet pipe, the expansion pipe and the discharge pipe are respectively: 2 cm 2 、2 cm 2 、16.6 cm 2 、16.6 cm 2 。
[0024] Optionally, in the centralized process device, an automatic feeding machine is further included, and the automatic feeding machine is connected to the feed port I;
[0025] The automatic feeding machine is a feeding device composed of at least one of a vibrating feeder, a weighing feeder, a volumetric screw feeder, a syringe, a compressed air assisted feeder, a vacuum assisted feeder, a gravity feeder, a drum feeder, a wheel feeder, a slide rail, a chute, a conveyor type feeder.
[0026] Specifically, the above feeding machine includes a feeder device selected from a loss-in-weight feeder, a vibrating feeder, a weighing feeder, a volumetric screw feeder, a syringe, a compressed air assisted feeder, a vacuum assisted feeder, a gravity feeder, a drum feeder, a wheel feeder, a slide rail, a chute, a conveyor type feeder or a combination thereof.
[0027] Optionally, the microwave section has a rectangular parallelepiped microwave cavity;
[0028] A microwave window is provided on the upper surface of the microwave cavity;
[0029] The microwave section is further provided with a waveguide, the waveguide is provided with a microwave inlet and a microwave outlet, and the microwave outlet is connected to the microwave window.
[0030] Optionally, the microwave section is further provided with a microwave generator, and the microwave inlet is connected to the microwave generator.
[0031] Optionally, the microwave section is further provided with an infrared temperature measurement module for monitoring the temperature in the microwave irradiation area.
[0032] Specifically, the process device is equipped with an infrared temperature measurement module, which can be used to monitor the reaction temperature of the intercalation modified graphite sample under microwave irradiation, so as to monitor the stability of the process.
[0033] Optionally, on the microwave section, an exhaust gas outlet is further provided on the cavity wall at one end near the discharge port.
[0034] Specifically, the above process device includes a device allowing the exhaust gas to leave or a scrubber device for capturing the exhaust gas. At the discharge port of the above process device, there is a blanking module, and the above blanking module is provided with a bottom suction container. The powder sample obtained in the above suction device is the graphene product.
[0035] Another aspect of the present application provides a process for preparing graphene, and the above process device is adopted in the process method;
[0036] The process method includes:
[0037] (1) Pretreatment: Immerse Graphite I in an intercalating agent solution containing an intercalating agent, seal and store, and dry to obtain intercalation-modified Graphite II;
[0038] (2) Push the Graphite II obtained in step (1) to the above feed port I, and the gas entering through the air inlet transports the Graphite II to the microwave irradiation area in the above microwave section, where a physical reaction occurs to obtain graphene.
[0039] Optionally, in step (1), the intercalating agent solution includes a polar solvent;
[0040] The polar solvent is selected from 1 to 4 of water, methanol, ethanol, propanol, ethylene glycol, and glycerol;
[0041] Among them, the volume ratio of each component is 0-1:0-1:0-1:0-1.
[0042] Optionally, the intercalating agent is at least one of bromine, chlorine, and iodine.
[0043] Optionally, the volume ratio of the intercalating agent to the polar solvent is 1-100:1-100.
[0044] Optionally, the volume ratio of the intercalating agent solution to Graphite I is 1:10-10:1.
[0045] Optionally, the volume ratio of the intercalating agent solution to Graphite I is 1:5.
[0046] Optionally, Graphite I is selected from at least one of artificial graphite and natural graphite.
[0047] Optionally, the natural graphite mainly includes flake graphite and earthy graphite.
[0048] Optionally, Graphite I is selected from natural flake graphite.
[0049] Optionally, the particle size of the natural flake graphite is 50 mesh.
[0050] Optionally, the time for sealed storage is 12h-120h.
[0051] Optionally, the soaking time is 6 h to 336 h.
[0052] Optionally, in step (1), the solid content of the intercalated modified graphite II is 50 to 80%.
[0053] Optionally, the solid content of the intercalated modified graphite II is 60 to 80%.
[0054] Optionally, the solid content of the intercalated modified graphite II is 70%.
[0055] Optionally, in step (2), the feeding rate of graphite II is 0.1 to 100 g / min.
[0056] Optionally, in step (2), the feeding rate of graphite II is 35 to 40 g / min.
[0057] Optionally, the transmission rate of the chain plate is 40 g / min.
[0058] Optionally, the pressure of the gas is 0.01 to 0.25 MPa;
[0059] The flow rate of the gas is 100 to 200 L / min;
[0060] Optionally, the gas is air.
[0061] Optionally, the pressure of the gas is 0.05 Mpa.
[0062] Optionally, the flow rate of the gas is 150 L / min.
[0063] Optionally, the microwave power in the microwave band is 1 to 300 kW.
[0064] Optionally, the microwave power in the microwave band is 6 to 10 kW.
[0065] Optionally, the temperature of the reaction is 200 to 500 °C.
[0066] Optionally, the residence time of the graphite II in the microwave irradiation area is 2 to 12 s.
[0067] Optionally, the expansion ratio of the graphene is ≥80 times.
[0068] Optionally, the expansion ratio of the graphene is ≥100 times.
[0069] Optionally, the number of layers of the graphene is ≤5 layers.
[0070] Optionally, the number of layers of the graphene is ≤3 layers.
[0071] Optionally, the intensity ratio I of the D peak to the G peak of the graphene D / I G ≤ 0.2.
[0072] Optionally, the I of the graphene D / I G ≤ 0.05.
[0073] As a specific implementation manner, the process method for preparing graphene in this application includes:
[0074] 1. Preparation of intercalated graphite:
[0075] Prepare a dispersant, and polar solvents can be selected: water, methanol, ethanol, propanol, ethylene glycol, glycerol, and other alcohol substances; any 1 to 4 of the above solvents are used as the dispersant, and the volume ratio is 0 to 1:0 to 1:0 to 1:0 to 1. Preferably, the volume ratio of water, methanol, ethanol, and propanol is 1:0:0:0.
[0076] Prepare an intercalant solution, and add bromine as the intercalant to the dispersant, with a volume ratio of 1 to 100:1 to 100; preferably, the volume ratio of bromine to the dispersant is 5:95;
[0077] Use the intercalant solution to soak and pretreat the graphite. After introducing the intercalant solution into the graphite, seal and store it for more than 12 h, preferably 72 h. At the same time, stir, with a stirring speed of 5 revolutions per minute or more, preferably 20 revolutions per minute. After stirring is completed, a graphite A solution is obtained. After filtering and air-drying the above dispersion, intercalated and modified graphite is obtained.
[0078] 2. Preparation of fluffy graphene:
[0079] Push the above intercalated and modified graphite B to the microwave feed port through an automatic feeding machine. Connect the pneumatic conveying module to the air inlet of the material flow bin, and spray graphite B into the microwave irradiation area through pneumatic conveying, so that graphite B stays in the microwave irradiation area for a period of time and then leaves to obtain a graphene product.
[0080] The above graphene product is grayish-white and fluffy. Compared with the raw material graphite, the expansion ratio of the graphene product is ≥ 80 times, preferably ≥ 100 times. Through characterization equipment such as a transmission electron microscope or Raman, the number of layers of the above graphene product is ≤ 5 layers, preferably the number of layers of the graphene product is ≤ 3 layers. Through Raman spectroscopy characterization, the intensity ratio (I D / I G ) of the D peak to the G peak of the graphene is all ≤ 0.2, preferably, I D / I G ≤ 0.05, more preferably, I D / I G = 0.
[0081] 3. Preparation of Powdered Graphene
[0082] Through mechanical shearing treatment, the above-mentioned grayish-white and fluffy graphene can be prepared into powdered graphene. The above mechanical shearing treatment includes using air flow crushing, ball milling, rotating blade mechanical shearing, ultrasonic treatment, cavitation or a combination thereof. Preferably, mechanical shearing treatment is carried out using an air flow crusher. After the mechanical shearing treatment, the number of layers of graphene remains basically unchanged, and no defects are formed, and its I D / I G ≤0.2.
[0083] The beneficial effects that can be produced by this application include:
[0084] 1) The process device provided by this application has a simple process, low energy consumption, is green and environmentally friendly, pollution-free, has high product quality, no defects, can realize continuous production, and has a large output;
[0085] 2) The process device provided by this application uses the method of gravity feeding combined with air compressor for gas transportation to continuously feed the microwave process, saving time costs; no special atmosphere environment is required in the microwave zone, and the air environment can meet the production conditions, saving the cost of protective gas;
[0086] 3) Compared with the existing microwave equipment, the process device provided by this application requires very little output power, lower temperature for the expansion of graphite into graphene, and only stays in the microwave zone for a few seconds for a unit mass of graphite to expand into graphene, saving several times the power cost; and has high quality, no defects, low number of layers, and extremely large output;
[0087] 4) The process device provided by this application has a simple equipment structure and a small volume, greatly reducing the floor area of the equipment and saving site costs; at the same time, an equipment that originally required several people to operate and monitor simultaneously has become one person can operate and monitor 2-3 devices simultaneously, greatly reducing the labor cost. Brief Description of the Drawings
[0088] Figure 1 It is the process flow chart of graphene in the embodiment of this application;
[0089] Figure 2 It is the process system flow chart of graphene in the embodiment of this application;
[0090] Figure 3 It is the assembly drawing of the microwave unit in the process device for preparing graphene in the embodiment of this application;
[0091] Figure 4 It is the longitudinal section view of the microwave unit in the process device for preparing graphene in the embodiment of this application;
[0092] Figure 5 Structural diagram at the observation window in the microwave unit of the embodiment of the present application;
[0093] Figure 6 Schematic diagram of the observation window glass plate in the microwave unit of the embodiment of the present application;
[0094] Figure 7 Schematic diagram of the microwave suppression tube I in the microwave unit of the embodiment of the present application;
[0095] Figure 8 Schematic diagram of the microwave suppression tube II in the microwave unit of the embodiment of the present application;
[0096] Figure 9 Schematic diagram of the waveguide in the microwave unit of the embodiment of the present application;
[0097] Figure 10 Schematic diagram of the microwave cavity in the microwave unit of the embodiment of the present application;
[0098] Figure 11 Schematic diagram of the material flow bin in the microwave unit of the embodiment of the present application;
[0099] Figure 12 Schematic diagram of the side plate of the suppression plate in the microwave unit of the embodiment of the present application;
[0100] Figure 13 Schematic diagram of the mica plate in the microwave unit of the embodiment of the present application.
[0101] Figure 14 Raman spectrogram I obtained in the second embodiment of the present application.
[0102] Figure 15 Raman spectrogram II obtained in the second embodiment of the present application.
[0103] Figure 16 Transmission electron microscope image I obtained in the second embodiment of the present application, where the scale bar is 5 nm.
[0104] Figure 17 Transmission electron microscope image II obtained in the second embodiment of the present application, where the scale bar is 5 nm.
[0105] List of components and reference numerals:
[0106] 1. Feed inlet I 2. Air inlet 3. Microwave suppression tube I
[0107] 4. Microwave cavity 5. Waveguide 6. Infrared temperature measurement module
[0108] 7. Mica plate 8. Observation window 9. Microwave irradiation area
[0109] 10. Exhaust gas outlet 11. Material flow bin 12. Microwave suppression tube II
[0110] 13. Discharge port 14. Feed pipe 15. Inlet pipe
[0111] 16. Expansion pipe 17. Discharge pipe 18. Observation window glass plate
[0112] 19. Observation window perforated plate Specific implementation mode
[0113] The present application will be described in detail below in conjunction with embodiments, but the present application is not limited to these embodiments.
[0114] Unless otherwise specified, the raw materials in the embodiments of the present application are all purchased through commercial channels.
[0115] The analysis methods in the embodiments of the present application are as follows:
[0116] Use Raman spectroscopy to analyze graphene, obtain the spectrum in the range of 200 - 3250 cm -1 and fit it to obtain the I D / I G value and the I 2D / I G value, and judge the defects and number of layers of graphene;
[0117] Use transmission electron microscopy to analyze graphene and judge the number of layers of graphene.
[0118] In the present application, the preparation method of graphene includes:
[0119] (1) Graphite intercalation modification technology, that is, the formula of the intercalating agent and the pretreatment process of graphite;
[0120] (2) Microwave reaction system technology, including an automatic feeding module, a pneumatic conveying continuous expansion technology, a reaction cavity temperature measurement module, a discharging module, and an exhaust gas absorption module;
[0121] (3) Crushing technology of fluffy graphene.
[0122] According to an implementation mode of the present application, the process flow diagram is as Figure 1 shown, and includes the following steps:
[0123] Pretreatment: Soak graphite A with an intercalating agent to form a graphite A solution;
[0124] Filtration and drying: Perform solid-liquid separation on the graphite A solution, and then dry the surface of the graphite to remove the residual liquid to obtain graphite B;
[0125] Microwave feeding: The material is transported to the microwave equipment by pneumatic conveying. After treatment, Graphite B reaches the microwave area under the push of compressed air. After a short period of time, physical expansion is completed to form Graphene A. Subsequently, the compressed air blows Graphene A out of the microwave equipment and into the receiving bin.
[0126] Crushing: Graphene A is sent into a jet mill for crushing through pneumatic conveying to obtain Graphene B. According to different particle size requirements of users, Graphene B is wet-ground (in a sand mill) with a dispersant to obtain Graphene C. According to different particle size requirements of users, Graphene B is mechanically ground to form Graphene D.
[0127] Example 1
[0128] A process device for preparing graphene, the process device includes a microwave unit, as Figure 3 shown; as Figure 4 shown, the microwave unit includes a feeding section, a microwave section, and a discharging section that are horizontally connected in sequence;
[0129] The feeding section includes a horizontally arranged microwave suppression tube I (as Figure 7 shown) 3. The fixed end of the microwave suppression tube I 3 is connected to the microwave section. An air inlet pipe 15 is provided inside the microwave suppression tube I 3;
[0130] The feeding section further includes a feeding pipe 14. The feeding pipe 14 is vertically connected to the air inlet pipe 15. The feeding port I1 of the feeding pipe is located above the microwave suppression tube I 3; The air inlet pipe 15 is provided with an air inlet 2 and an air outlet;
[0131] The microwave section is provided with a microwave cavity 4. The microwave cavity 4 is as Figure 10 shown in Figures a and b of Figure 9 and is assembled by suppression plates to form a cuboid-shaped microwave cavity. A microwave irradiation area 9 is provided inside the microwave cavity 4; An expansion pipe 16 is provided inside the microwave cavity 4. The air outlet is connected to the expansion pipe 16; A microwave window is provided on the upper surface of the microwave cavity 4; The microwave section further includes a waveguide 5 (as Figure 13 shown). The waveguide 5 is provided with a microwave inlet and a microwave outlet. The microwave outlet is connected to the microwave window. A mica plate 7 (as
[0132] shown) is also provided between the waveguide and the microwave cavity; Figure 8 The discharging section includes a horizontally arranged microwave suppression tube II 12 (as
[0133] The intake pipe 15, the feed pipe 14, the expansion pipe 16 and the discharge pipe 17 are connected to form a material flow bin 11 (as Figure 11 shown), the material of the material flow bin 11 is quartz, and the cross-sectional areas of the feed pipe 14, the intake pipe 15, the expansion pipe 16, and the discharge pipe 17 are respectively: 2 cm 2 , 2 cm 2 , 16.6 cm 2 , 16.6 cm 2 .
[0134] A microwave generator (such as the microwave source shown in Figure 2 ) is also provided in the microwave section, and the microwave inlet is connected to the microwave generator;
[0135] An infrared temperature measurement module 6 is also provided in the microwave section for monitoring the reaction temperature of the intercalated modified graphite sample under microwave irradiation to facilitate the stability of the monitoring process technology.
[0136] An exhaust gas outlet 10 is also provided on the cavity wall at one end near the discharge port in the microwave section.
[0137] An observation window 8 is provided on the side plate of the suppression plate (as shown in Figure 12 ), as shown in Figure 5 , and it is composed of an observation window glass plate 18 (as shown in Figure 6 ) and an observation window perforated plate 19.
[0138] The process device, as shown in the process system flow chart in Figure 2 , further includes a feed bin, which is connected to the feed port I. In this embodiment, the feed bin is made of quartz;
[0139] The process device further includes a pneumatic conveying module, which is connected to the air inlet. The pneumatic conveying module includes an air compressor, a gas storage tank, a filter, and a pressure valve.
[0140] The process device includes an exhaust gas recovery module, specifically a device that allows exhaust gas to leave or a scrubber device that captures exhaust gas, which is connected to the exhaust gas outlet 10.
[0141] A receiving bin is also provided at the discharge port of the process device.
[0142] The process device further includes a pulverization module, which is connected to the receiving bin and the pneumatic conveying module, and uses a jet mill to mechanically shear graphene.
[0143] Example 2
[0144] Using the process device obtained in Example 1, prepare graphene according to the Figure 1 , Figure 2 process, and the specific steps are as follows:
[0145] 1. Preparation of intercalated graphite:
[0146] (1) Prepare a dispersant, and select 98 ml of water as the dispersant;
[0147] (2) Prepare an intercalating agent solution, add 2 ml of bromine element intercalating agent to the dispersant, and the volume concentration is 2%;
[0148] (3) Use the obtained intercalating agent solution to pre-treat the graphite by soaking. The graphite is natural flake graphite with a particle size of 50 mesh; the volume ratio of the intercalating agent solution to the graphite is 1:5. Soak the graphite in the intercalating agent solution. After soaking for 6 h, seal and store for 12 h. At the same time, stir, and the stirring speed is 20 revolutions per minute. After stirring is completed, obtain graphite A solution. After filtering and air-drying the above graphite A solution, obtain intercalated and modified graphite B. Among them, the solid content of the intercalated and modified graphite B is 65%.
[0149] 2. Preparation of fluffy graphene:
[0150] Push the above intercalated and modified graphite B to the microwave feeding port through an automatic feeding machine (loss-in-weight feeder). Connect the pneumatic conveying module to the air inlet of the material flow bin, and spray graphite B into the microwave irradiation area through pneumatic conveying, so that graphite B stays in the microwave irradiation area for 10 s and then leaves. Among them, the gas source is air, and the pressure is 0.05 MPa. The gas flow rate in the pipe is 150 L / min; the power of the above microwave equipment is 15 kW. The feeding speed of graphite B is 50 g / min. The reaction temperature of the above microwave equipment is 300 °C.
[0151] Use a graduated cylinder to measure the volume of graphene, and through conversion, it is obtained that the expansion ratio of the graphene product obtained in step (2) compared with the raw material graphite is 98 times.
[0152] Use a transmission electron microscope to measure that the number of layers of the graphene product is 3 - 5 layers, as Figure 16 、 17 shown.
[0153] Characterized by Raman spectroscopy, as Figure 15 shown, from the Raman fitting results, it is also verified that the number of layers of the graphene product is 3 - 5 layers.
[0154] Characterized by Raman spectroscopy, the intensity ratio (I D / I G ) of the D peak and G peak of graphene is 0.011.
[0155] 3. Preparation of powdered graphene
[0156] Through mechanical shearing treatment, the above-mentioned graphene is prepared into powdered graphene. The mechanical shearing treatment is carried out using a jet mill. After the mechanical shearing treatment, the range of the number of layers of graphene remains basically unchanged, and no defects are formed (as Figure 14 shown), and its I D / I G is 0.012.
[0157] As mentioned above, these are only several embodiments of the present application and do not impose any form of limitation on the present application. Although the present application is disclosed above with preferred embodiments, it is not intended to limit the present application. Any person skilled in the art, without departing from the scope of the technical solution of the present application, making some changes or modifications using the technical content disclosed above is equivalent to equivalent implementation cases and all fall within the scope of the technical solution.
Claims
1. A process device for preparing graphene, characterized in that the process device includes a microwave unit; the microwave unit includes a feeding section, a microwave section, and a discharging section that are horizontally connected in sequence; the feeding section includes a microwave suppression tube I arranged horizontally, the fixed end of the microwave suppression tube I is connected to the microwave section, and an air inlet pipe is arranged inside the microwave suppression tube I; the feeding section further includes a feeding pipe, the feeding pipe is connected to the air inlet pipe, and the feeding port I of the feeding pipe is located above the microwave suppression tube I; the air inlet pipe is provided with an air inlet and an air outlet; the microwave section is provided with a microwave cavity, and a microwave irradiation area is arranged inside the microwave cavity; an expansion tube is arranged inside the microwave cavity, and the air outlet is connected to the expansion tube; the discharging section includes a microwave suppression tube II arranged horizontally, the fixed end of the microwave suppression tube II is connected to the microwave section, a discharging pipe is arranged inside the microwave suppression tube II, the feeding port II of the discharging pipe is connected to the expansion tube, and the free end of the discharging pipe is provided with a discharging port.
2. The process device according to claim 1, characterized in that taking the microwave cavity as the horizontal line and the air inlet as the starting point, along the clockwise direction, the inclination angles of the air inlet pipe, the feeding pipe, and the discharging pipe satisfy: the inclination angle of the air inlet pipe is 0° to 90° or 270° to 360°; the inclination angle of the feeding pipe is 45° to 90°; the inclination angle of the discharging pipe is 120° to 240°.
3. The process device according to claim 1, characterized in that the process device further includes a pneumatic conveying module, and the pneumatic conveying module is connected to the air inlet.
4. The process device according to claim 1, characterized in that in the process device The cross-sectional area of the intake pipe is 0.5 to 3 cm 2 ; The cross-sectional area of the feed pipe is 0.5 to 3 cm 2 ; The cross-sectional area of the pipeline of the expansion pipe is 1 to 30 cm 2 ; The cross-sectional area of the discharge pipe is 1 to 30 cm 2 .
5. The process device according to claim 1, characterized in that in the process device, it further includes an automatic feeding machine, and the automatic feeding machine is connected to the feeding port I; the automatic feeding machine is a feeding device composed of at least one of a vibrating feeder, a weighing feeder, a volumetric screw auger feeder, a syringe, a compressed air assisted feeder, a vacuum assisted feeder, a gravity feeder, a drum feeder, a wheel feeder, a slide rail, a chute, and a conveyor type feeder.
6. The process device according to claim 1, characterized in that the microwave section has a cuboid-shaped microwave cavity; a microwave window is arranged on the upper surface of the microwave cavity; the microwave section is further provided with a waveguide, the waveguide is provided with a microwave inlet and a microwave outlet, and the microwave outlet is connected to the microwave window.
7. The process device according to claim 6, characterized in that the microwave section is further provided with a microwave generator, and the microwave inlet is connected to the microwave generator.
8. The process device according to claim 1, characterized in that the microwave section is further provided with an infrared temperature measurement module for monitoring the temperature in the microwave irradiation area.
9. The process device according to claim 1, characterized in that on the microwave section, on the cavity wall near the discharging port end, an exhaust gas outlet is further arranged.