Graphene production and manufacturing process

Abstract

The invention discloses a graphene production and manufacturing process, and relates to the technical field of graphene production.The graphene production and manufacturing process comprises a fixed shell, a lifting stirring mechanism and an oscillation mechanism, the structure is reasonable and simple, the production cost is low, installation is convenient, through the unique stirring and oscillation synergistic effect, the reaction temperature can be accurately controlled, and the production efficiency is improved. The materials can be fully mixed and reacted in the low-temperature and heating stages, so that the reaction efficiency and the product quality after the reaction are improved; the stirring shaft is driven by the motor and a complex transmission structure, the stability is high, the stirring effect can be guaranteed, and graphite particles are fully oxidized to prepare graphite oxide; the vibration design of the reaction tank body is ingenious, the motor, the rotating disc, the column body and the clamping hole are matched, and the sliding block, the sliding groove, the guide column, the ball body and other structures are combined, so that the periodicity and stability of vibration are guaranteed, friction is reduced, and sufficient mixing of materials is facilitated.

Description

Technical Field

[0001] The present invention relates to the technical field of graphene production, and in particular to a graphene production process. Background Art

[0002] Graphene is a very special material, which is composed of a single-atom-thick layer of carbon atoms. Specifically, carbon atoms are arranged in an sp2 hybrid manner, forming hexagonal planes that are only a single layer of atoms thick. These planes are arranged in an orderly manner into a honeycomb lattice, thus constructing this unique single-layer two-dimensional crystal structure. Graphene occupies a unique position in the field of materials. It is one of the thinnest materials currently known. However, its characteristics are far more than that. Graphene also shows amazing strength and is extremely strong and hard. From the perspective of electrical properties, as a single substance, graphene transfers electrons at a speed faster than all known conductors and semiconductors at room temperature. This excellent electrical property gives it great application potential in the field of electronics. What is more worth mentioning is that the single-layer carbon atom structure of graphene gives it an extremely high theoretical specific surface area, which can reach 3000m² / g. Such a huge specific surface area makes graphene-based materials a promising active material in the field of energy storage. In terms of hydrogen storage, graphene's large specific surface area provides sufficient adsorption sites for hydrogen; in the field of new lithium-ion batteries, it helps to improve the charging and discharging efficiency and capacity of batteries; for supercapacitors, it can greatly improve their energy storage performance; in the field of fuel cells, it is also expected to bring new breakthroughs in their performance optimization. Currently, the redox method is one of the common methods for large-scale production of graphene. Although this method has certain advantages in terms of output, there are problems of low efficiency and poor quality in the preparation process. These problems seriously restrict the performance of graphene and need to be improved urgently to fully tap the potential of graphene in various application fields. Summary of the invention

[0003] The purpose of the present invention is to provide a graphene production and manufacturing process in order to solve the above problems, thereby solving the problems of low efficiency and poor quality in the graphene preparation process.

[0004] In order to solve the above problems, the present invention provides a technical solution: a graphene production process, comprising the following steps:

[0005] A. Raw material preparation: graphite raw material preparation and chemical reagent preparation;

[0006] B. Preparation of graphite raw materials in step A: Select high-purity graphite blocks with a purity of not less than 99%, put them into a crusher, and crush them into graphite particles with uniform particle size, with the particle size range controlled at 0.1-1 mm;

[0007] C. Preparation of chemical reagents in step A: select potassium permanganate with a purity of ≥99.5%, concentrated sulfuric acid with a concentration of 98%, and hydrazine hydrate solution with a concentration of 80%;

[0008] D. Preparation of graphite oxide: Mixing reaction is carried out through a mixing reaction device, and then washing treatment is carried out;

[0009] E. Mixing reaction in step D: mixing potassium permanganate, concentrated sulfuric acid and graphite particles in a mixing reaction device according to a mass ratio of graphite particles: potassium permanganate: concentrated sulfuric acid = 1:3:20, first stirring the reaction at 0-5 ° C for 30 minutes, and then continuing to stir the reaction at 35 ° C for 2 hours to fully oxidize the graphite particles to obtain graphite oxide;

[0010] F. Washing treatment in step D: slowly pour the graphite oxide obtained in step E into a large amount of ice water, where the mass of the ice water is 10 times the mass of the reaction mixture, stir evenly and filter, and wash the obtained filter cake repeatedly with deionized water until the filtrate is neutral to remove residual acid and impurities;

[0011] D. Preparation of graphene oxide: The washed graphite oxide is placed in a microwave reactor, the microwave power is set to 500-800W, and the reaction time is 10-20 minutes. Under the action of microwaves, the interlayer force of the graphite oxide is further weakened, and the layers are gradually peeled off to obtain graphene oxide;

[0012] E. Graphene reduction: Graphene oxide is dispersed in water to form a uniform graphene oxide solution, hydrazine hydrate solution is slowly introduced, the mass ratio of hydrazine hydrate to graphene oxide is 1:5, and reflux reaction is carried out in a water bath at 80°C for 12 hours to reduce the oxygen-containing functional groups in the graphene oxide to obtain graphene;

[0013] F. Graphene treatment: The obtained graphene is placed in a vacuum drying oven and dried for 24 hours at 60-80°C and a vacuum degree of 0.01-0.1 MPa to remove moisture;

[0014] The specific structure of the mixing reaction equipment in step D includes a fixed shell, a lifting and stirring mechanism and an oscillating mechanism; the lifting and stirring mechanism is provided on the outside of the fixed shell, and the oscillating mechanism is provided inside the fixed shell.

[0015] Preferably, the specific structure of the lifting and stirring mechanism includes a guide hole seat, a guide hole 1, a lifting hole seat, a cylinder, a mounting seat, a temperature control valve, a discharge pipe, a driving gear 1, a motor 1, a driven gear 1, an internal gear, a guide seat, a guide pipe, a movable block, an inner groove 1, an inner groove 2, a motor 2, a connecting gear, a rotating seat, a driven gear 2, a driving gear, a fixed cover, a stirring shaft, a heat exchange hole, a stirring rod, a connecting block and a connecting shaft; there are two guide hole seats, and the two guide hole seats are respectively fixedly connected to the left and right sides of the fixed shell, and the two guide hole seats are each provided with a guide hole 1 inside the upper side, and the guide hole 1 is movably connected to the lifting hole seat; the left and right bottoms of the mounting seat are respectively connected to the corresponding lifting hole seat tops The two oil cylinders are fixedly connected; there are two oil cylinders, the bottoms of the two oil cylinders are respectively fixedly connected to the bottom surface of the corresponding guide hole, the outsides of the two oil cylinders are respectively movably connected to the inside of the corresponding mounting seat, and the ends of the piston rods on the upper sides of the two oil cylinders are respectively fixedly connected to the left and right sides of the bottom of the mounting seat; the rotating seat is movably connected to the central inside of the lower side of the mounting seat through a fixed cover, and the lower side of the rotating seat is fixedly connected to the driven gear 2; the second motor is fixedly connected to the right side of the top surface of the mounting seat, and the output shaft of the lower side of the second motor is fixedly connected to a driving gear, and the driving gear is connected to the second driven gear; the outside of the internal gear is movably connected to the central inside of the mounting seat, and the top of the internal gear is fixedly connected There is a driven gear 1; the motor 1 is fixedly connected to the left side of the top surface of the mounting seat, and a driving gear 1 is fixedly connected to the output shaft on the lower side of the motor, and the driving gear 1 is connected to the driven gear 1; the movable block is movably connected to the central interior of the upper side of the mounting seat, and the inner walls on the left and right sides of the movable block are provided with an inner groove 1 and an inner groove 2; the lower outer side of the guide seat is fixedly connected to the central interior of the upper side of the mounting seat, and the lower inner side of the guide seat is connected to the inner groove 1 through a connecting hole, and the upper left opening of the guide seat is connected to the outlet of the temperature control valve through a water pipe; the upper outer side of the guide pipe is fixedly connected to the central interior of the upper side of the guide seat, and the lower opening of the guide pipe is connected to the inner groove 2 through a connecting hole The upper opening of the guide pipe is connected to the discharge pipe; there are two stirring shafts, and the upper outer parts of the two stirring shafts are movably connected to the left and right inner parts of the rotating seat respectively; the upper outer parts of the two stirring shafts are fixedly connected with connecting gears, and the connecting gears are connected to the internal gears; the interiors of the two stirring shafts are provided with heat exchange holes, and the openings on one side of the heat exchange holes are respectively connected to the corresponding interiors of the inner tank one, and the openings on the other side of the heat exchange holes are respectively connected to the corresponding interiors of the inner tank two; the bottom centers of the two stirring shafts are fixedly connected with connecting shafts, and the exteriors of the two stirring shafts are fixedly connected with a plurality of stirring rods; the interiors on the left and right sides of the connecting block are movably connected to the corresponding exteriors of the connecting shafts respectively.

[0016] Preferably, the motor 1 and the motor 2 are both servo motors or variable frequency motors.

[0017] Preferably, a cold water pipe and a hot water pipe are provided on the left side of the temperature control valve, and the water temperature in the cold water pipe is 0°C, and the water temperature in the hot water pipe is 45°C.

[0018] Preferably, the first guide hole is a rectangular guide hole.

[0019] Preferably, the specific structure of the oscillation mechanism includes a slide groove, a slider, a slide hole, a guide column, a reaction tank body, a ball, a sleeve body, a card hole block, a card hole, a column, a turntable and a motor three; there are several slide grooves, and several of the slide grooves are respectively longitudinally and transversely opened on the left and right sides and the front and rear inner walls of the fixed shell, and several of the slide grooves are movably connected with sliders, and the center of the slider is provided with a slide hole; the reaction tank body is located inside the fixed shell, and the left and right sides and the front and rear positions of the outside of the reaction tank body are fixedly connected with guide columns, and the guide columns are movably connected to the corresponding slide holes, and the center of the bottom of the reaction tank body is fixedly connected with a card hole block, and the center of the bottom surface of the card hole block is provided with a card hole; there are several spheres, and several of the spheres are movably connected to the bottom of the reaction tank body around the three motors through the sleeve body; the motor three is fixedly connected to the central interior of the lower side of the fixed shell, and the output shaft of the motor three is fixedly connected with a turntable, and the top edge of the turntable is fixedly connected with a column, and the outside of the column is movably connected to the inside of the card hole.

[0020] Preferably, the slide groove is a T-shaped slide groove.

[0021] Preferably, the motor three is a servo motor or a variable frequency motor.

[0022] The beneficial effects of the present invention are as follows: (1) The present invention has a reasonable and simple structure, low production cost and convenient installation. The unique synergistic effect of stirring and shaking can accurately control the reaction temperature, and the materials can be fully mixed and reacted in both the low temperature and heating stages, thereby improving the reaction efficiency and the quality of the product after the reaction.

[0023] (2) In the present invention, the stirring shaft is driven by a motor and a complex transmission structure, which has high stability and can ensure the stirring effect, so that the graphite particles are fully oxidized to produce graphite oxide.

[0024] (3) The vibration design of the reaction tank in the present invention is ingenious. Through the coordination of the motor, turntable, column and clamping hole, and combined with the structures of slider, slide groove, guide column and ball, it not only ensures the periodicity and stability of vibration, but also reduces friction, which is conducive to the full mixing of materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a structural schematic diagram of the present invention.

[0026] Figure 2 for Figure 1 sectional view of .

[0027] Figure 3 It is a structural schematic diagram of the lifting and stirring mechanism.

[0028] Figure 4 for Figure 3 Enlarged view of position A in the middle.

[0029] Figure 5 It is a structural diagram of the oscillation mechanism.

[0030] 1-fixed shell; 2-lifting stirring mechanism; 21-guide hole seat; 22-guide hole 1; 23-lifting hole seat; 24-oil cylinder; 25-mounting seat; 26-temperature control valve; 27-discharge pipe; 28-driving gear 1; 29-motor 1; 210-driven gear 1; 211-internal gear; 212-flow guide seat; 213-flow guide pipe; 214-movable block; 215-inner groove 1; 216-inner groove 2; 217-motor 2; 218-connecting gear; 219 - rotating seat; 220- driven gear 2; 221- driving gear; 222- fixed cover; 223- stirring shaft; 224- heat exchange hole; 225- stirring rod; 226- connecting block; 227- connecting shaft; 3- oscillation mechanism; 31- slide groove; 32- slider; 33- slide hole; 34- guide column; 35- reaction tank body; 36- ball body; 37- sleeve body; 38- clamping hole block; 39- clamping hole; 310- column body; 311- turntable; 312- motor 3. DETAILED DESCRIPTION

[0031] like Figure 1 and Figure 2 As shown, this specific embodiment adopts the following technical solution: a graphene production and manufacturing process, comprising the following steps:

[0032] A. Raw material preparation: graphite raw material preparation and chemical reagent preparation;

[0033] B. Preparation of graphite raw materials in step A: Select high-purity graphite blocks with a purity of not less than 99%, put them into a crusher, and crush them into graphite particles with uniform particle size, with the particle size range controlled at 0.1-1 mm;

[0034] C. Preparation of chemical reagents in step A: select potassium permanganate with a purity of ≥99.5%, concentrated sulfuric acid with a concentration of 98%, and hydrazine hydrate solution with a concentration of 80%;

[0035] D. Preparation of graphite oxide: Mixing reaction is carried out through a mixing reaction device, and then washing treatment is carried out;

[0036] E. Mixing reaction in step D: mixing potassium permanganate, concentrated sulfuric acid and graphite particles in a mixing reaction device according to a mass ratio of graphite particles: potassium permanganate: concentrated sulfuric acid = 1:3:20, first stirring the reaction at 0-5 ° C for 30 minutes, and then continuing to stir the reaction at 35 ° C for 2 hours to fully oxidize the graphite particles to obtain graphite oxide;

[0037] F. Washing treatment in step D: slowly pour the graphite oxide obtained in step E into a large amount of ice water, where the mass of the ice water is 10 times the mass of the reaction mixture, stir evenly and filter, and wash the obtained filter cake repeatedly with deionized water until the filtrate is neutral to remove residual acid and impurities;

[0038] D. Preparation of graphene oxide: The washed graphite oxide is placed in a microwave reactor, the microwave power is set to 500-800W, and the reaction time is 10-20 minutes. Under the action of microwaves, the interlayer force of the graphite oxide is further weakened, and the layers are gradually peeled off to obtain graphene oxide;

[0039] E. Graphene reduction: Graphene oxide is dispersed in water to form a uniform graphene oxide solution, hydrazine hydrate solution is slowly introduced, the mass ratio of hydrazine hydrate to graphene oxide is 1:5, and reflux reaction is carried out in a water bath at 80°C for 12 hours to reduce the oxygen-containing functional groups in the graphene oxide to obtain graphene;

[0040] F. Graphene treatment: The obtained graphene is placed in a vacuum drying oven and dried for 24 hours at 60-80°C and a vacuum degree of 0.01-0.1 MPa to remove moisture;

[0041] The specific structure of the mixing reaction equipment in step D includes a fixed shell 1, a lifting and stirring mechanism 2 and an oscillating mechanism 3; the lifting and stirring mechanism 2 is provided on the outside of the fixed shell 1, and the oscillating mechanism 3 is provided inside the fixed shell 1.

[0042] like Figure 3 and Figure 4As shown, the specific structure of the lifting and stirring mechanism 2 includes a guide hole seat 21, a guide hole 22, a lifting hole seat 23, a cylinder 24, a mounting seat 25, a temperature control valve 26, a discharge pipe 27, a driving gear 28, a motor 29, a driven gear 210, an inner gear 211, a guide seat 212, a guide pipe 213, a movable block 214, an inner tank 215, an inner tank 216, a motor 217, a connecting gear 218, a rotating seat 219, a driven gear 220, a driving gear 221, a fixed cover 222, a stirring shaft 223, a heat exchange hole 224, a stirring rod 225, a connecting block 226 and a connecting shaft 227; the guide hole seat 21 is two, and the two guide holes The seats 21 are respectively fixedly connected to the outside of the left and right sides of the fixed shell 1, and the upper sides of the two guide hole seats 21 are each provided with a guide hole 22, and the guide hole 22 is movably connected to the lifting hole seat 23; the bottom of the mounting seat 25 is respectively fixedly connected to the top of the corresponding lifting hole seat 23; there are two oil cylinders 24, the bottoms of the two oil cylinders 24 are respectively fixedly connected to the bottom surfaces of the corresponding guide holes 22, the outsides of the two oil cylinders 24 are respectively movably connected to the inside of the corresponding mounting seat 25, and the piston rod ends of the two oil cylinders 24 are respectively fixedly connected to the left and right sides of the bottom of the mounting seat 25; the rotating seat 219 is movably connected to the bottom of the mounting seat 25 through the fixed cover 222 The central part of the side, the lower side of the rotating seat 219 is fixedly connected to the driven gear 220; the motor 217 is fixedly connected to the right side of the top surface of the mounting seat 25, and the lower output shaft of the motor 217 is fixedly connected to the driving gear 221, and the driving gear 221 is connected to the driven gear 220; the inner gear 211 is externally movably connected to the central part of the mounting seat 25, and the top of the inner gear 211 is fixedly connected to the driven gear 1 210; the motor 1 29 is fixedly connected to the left side of the top surface of the mounting seat 25, and the lower output shaft of the motor 1 29 is fixedly connected to the driving gear 1 28, and the driving gear 1 28 is connected to the driven gear 1 210; the movable The movable block 214 is movably connected to the central interior of the upper side of the mounting seat 25, and the inner walls on the left and right sides of the movable block 214 are provided with an inner groove 1 215 and an inner groove 216; the lower outer side of the guide seat 212 is fixedly connected to the central interior of the upper side of the mounting seat 25, and the lower inner side of the guide seat 212 is connected to the inner groove 1 215 through a connecting hole, and the upper left opening of the guide seat 212 is connected to the outlet of the temperature control valve 26 through a water pipe; the upper outer side of the guide pipe 213 is fixedly connected to the central interior of the upper side of the guide seat 212, and the lower opening of the guide pipe 213 is connected to the inner groove 2 216 through a connecting hole, and the upper opening of the guide pipe 213 is connected to the discharge pipe 27;There are two stirring shafts 223, and the upper outer parts of the two stirring shafts 223 are movably connected to the left and right sides of the rotating seat 219, and the upper outer parts of the two stirring shafts 223 are fixedly connected with connecting gears 218, and the connecting gears 218 are connected to the inner gear 211. The two stirring shafts 223 are provided with heat exchange holes 224, and the openings on one side of the heat exchange holes 224 are respectively connected to the corresponding inner groove 1 215, and the openings on the other side of the heat exchange holes 224 are respectively connected to the corresponding inner groove 2 216. The bottom centers of the two stirring shafts 223 are fixedly connected with connecting shafts 227, and the outer parts of the two stirring shafts 223 are fixedly connected with a plurality of stirring rods 225; the inner parts on the left and right sides of the connecting block 226 are movably connected to the outer parts of the corresponding connecting shafts 227. ;

[0043] Among them, the motor 1 29 and the motor 2 217 are both servo motors or variable frequency motors; a cold water pipe and a hot water pipe are provided on the left side of the temperature control valve 26, and the water temperature in the cold water pipe is 0°C, and the water temperature in the hot water pipe is 45°C; the guide hole 1 22 is a rectangular guide hole.

[0044] like Figure 5 As shown, the specific structure of the oscillation mechanism 3 includes a slide groove 31, a slider 32, a slide hole 33, a guide column 34, a reaction tank body 35, a ball 36, a sleeve body 37, a clamping hole block 38, a clamping hole 39, a column 310, a turntable 311 and a motor 312; there are several slide grooves 31, and several of the slide grooves 31 are respectively opened longitudinally and transversely on the left and right sides and the front and rear inner walls of the fixed shell 1, and the sliders 32 are movably connected inside the several slide grooves 31, and the slide holes 33 are opened in the center of the sliders 32; the reaction tank body 35 is located inside the fixed shell 1, and the left and right sides and the front and rear positions of the reaction tank body 35 are opened outside They are all fixedly connected with guide pillars 34, and the guide pillars 34 are movably connected to the corresponding sliding holes 33 respectively. A clamping hole block 38 is fixedly connected to the center of the bottom of the reaction tank body 35, and a clamping hole 39 is opened in the center of the bottom surface of the clamping hole block 38; there are several spheres 36, and the several spheres 36 are movably connected to the bottom surface of the reaction tank body 35 around through a clamping sleeve body 37; the motor three 312 is fixedly connected to the center of the lower side of the fixed shell 1, and a turntable 311 is fixedly connected to the output shaft on the upper side of the motor three 312, and a column 310 is fixedly connected to the edge of the top surface of the turntable 311, and the outside of the column 310 is movably connected to the inside of the clamping hole 39.

[0045] Wherein, the slide slot 31 is a T-shaped slide slot; the motor three 312 is a servo motor or a variable frequency motor.

[0046] The use state of the present invention is as follows: the present invention has a reasonable and simple structure, low production cost, and convenient installation. When in use, the graphite particles, potassium permanganate, and concentrated sulfuric acid prepared according to the mass ratio are first added into the reaction tank body 35 through the opening above the fixed shell 1 to prepare for a mixing reaction, and then the motor 1 29 and the motor 2 217 are started (both are servo motors or variable frequency motors, and the speed can be accurately controlled as needed). The motor 1 29 drives the driven gear 1 210 to rotate through the driving gear 1 28, thereby rotating the internal gear 211, and the internal gear 211 drives the connecting gear 218 to rotate the stirring shaft 223. At the same time, the motor 2 217 drives the driven gear 2 220 and the rotating seat 219 to rotate through the driving gear 221, and further The stirring shaft 223 is ensured to rotate stably. The stirring rod 225 on the stirring shaft 223 stirs the materials in the reaction tank body 35. In the low temperature (0-5°C) reaction stage, the temperature control valve 26 supplies water to the guide seat 212 through the cold water pipe (the water temperature is 0°C). The water enters the inner tank 1 215 through the connecting hole inside the lower side of the guide seat 212, and then enters the inner tank 2 216 through the heat exchange hole 224 inside the stirring shaft 223. Finally, it is discharged through the guide pipe 213 and the discharge pipe 27 to maintain the low temperature required for the reaction. In addition, the motor 312 (servo motor or variable frequency motor) is started, and the motor 312 drives the turntable 311 to rotate. The column 310 on the turntable 311 cooperates with the card hole 39 on the card hole block 38 at the bottom of the reaction tank body 35, so that The reaction tank body 35 generates periodic vibrations. At the same time, the reaction tank body 35 moves in the sliding hole 33 of the slider 32 through the guide column 34, and the slider 32 slides in the T-shaped slide groove 31 to ensure the stable vibration of the reaction tank body 35. The balls 36 connected by the ferrule body 37 around the bottom surface of the reaction tank body 35 also help to reduce vibration friction and make the vibration smoother. This vibration and the stirring of the stirring shaft 223 work together to make the materials fully mixed and reacted at low temperature (0-5°C) for 30 minutes, thereby improving the efficiency of the reaction and the quality after the reaction. When the low-temperature reaction stage is over, the temperature control valve 26 supplies water through the hot water pipe (the water temperature is 45°C) to raise the temperature in the reaction tank body 35 to 35°C, and continue to stir and react for 2 hours to make the graphite particles full. Graphite oxide is obtained by partial oxidation. During this process, the rotation of the stirring shaft 223 and the vibration of the reaction tank body 35 are continuously carried out to ensure that the materials are evenly mixed and the oxidation reaction is fully carried out, which further improves the efficiency of the reaction and the quality after the reaction. After the reaction is completed, the motor 1 29, the motor 217 and the motor 312 are turned off, the stirring shaft 223 stops stirring, and the reaction tank body 35 stops vibrating. Then, the obtained graphite oxide is slowly transferred out of the reaction tank body 35, and subsequent washing treatment steps are carried out, such as slowly pouring the graphite oxide into a large amount of ice water (the mass of the ice water is 10 times the mass of the reaction mixture), stirring it evenly and filtering it. The obtained filter cake is repeatedly washed with deionized water until the filtrate is neutral to remove residual acid and impurities.The subsequent steps include graphene oxide preparation, graphene reduction and graphene treatment, and finally the production of graphene is completed.

[0047] The control method in the present invention is to start manually or control through existing automation technology. The wiring diagram of the power element and the provision of power supply are common knowledge in the field, and the present invention is mainly used to protect mechanical devices, so the present invention will no longer explain the control method and wiring layout in detail.

[0048] In the description of the invention, it should be understood that the terms "coaxial", "bottom", "one end", "top", "middle", "the other end", "upper", "one side", "top", "inside", "front", "center", "both ends" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the invention and simplifying the description, and do 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 cannot be understood as a limitation on the invention.

[0049] In the invention, unless otherwise clearly stipulated and limited, the terms such as "installation", "setting", "connection", "fixation", "screw-on" and the like should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral one; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be the internal connection of two elements or the interaction relationship between two elements. Unless otherwise clearly defined, ordinary technicians in this field can understand the specific meanings of the above terms in the invention according to the specific circumstances.

[0050] The above shows and describes the basic principles, main features and advantages of the invention. Those skilled in the art should understand that the invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the invention. Without departing from the spirit and scope of the invention, the invention may have various changes and improvements, which shall fall within the scope of the invention to be protected. The scope of protection of the invention shall be defined by the attached claims and their equivalents.

Claims

1. A graphene production process, characterized in that: The following steps are involved: A. Raw material preparation: graphite raw material preparation and chemical reagent preparation; B. Preparation of graphite raw materials in step A: Select high-purity graphite blocks with a purity of not less than 99%, put them into a crusher, and crush them into graphite particles with uniform particle size, with the particle size range controlled at 0.1-1 mm; C. Preparation of chemical reagents in step A: select potassium permanganate with a purity of ≥99.5%, concentrated sulfuric acid with a concentration of 98%, and hydrazine hydrate solution with a concentration of 80%; D. Preparation of graphite oxide: Mixing reaction is carried out through a mixing reaction device, and then washing treatment is carried out; E. Mixing reaction in step D: mixing potassium permanganate, concentrated sulfuric acid and graphite particles in a mixing reaction device according to a mass ratio of graphite particles: potassium permanganate: concentrated sulfuric acid = 1:3:20, first stirring the reaction at 0-5 ° C for 30 minutes, and then continuing to stir the reaction at 35 ° C for 2 hours to fully oxidize the graphite particles to obtain graphite oxide; F. Washing treatment in step D: slowly pour the graphite oxide obtained in step E into a large amount of ice water, where the mass of the ice water is 10 times the mass of the reaction mixture, stir evenly and filter, and wash the obtained filter cake repeatedly with deionized water until the filtrate is neutral to remove residual acid and impurities; D. Preparation of graphene oxide: The washed graphite oxide is placed in a microwave reactor, the microwave power is set to 500-800W, and the reaction time is 10-20 minutes. Under the action of microwaves, the interlayer force of the graphite oxide is further weakened, and the layers are gradually peeled off to obtain graphene oxide; E. Graphene reduction: Graphene oxide is dispersed in water to form a uniform graphene oxide solution, hydrazine hydrate solution is slowly introduced, the mass ratio of hydrazine hydrate to graphene oxide is 1:5, and reflux reaction is carried out in a water bath at 80°C for 12 hours to reduce the oxygen-containing functional groups in the graphene oxide to obtain graphene; F. Graphene treatment: The obtained graphene is placed in a vacuum drying oven and dried for 24 hours at 60-80°C and a vacuum degree of 0.01-0.1 MPa to remove moisture; The specific structure of the mixing reaction equipment in step D includes a fixed shell (1), a lifting and stirring mechanism (2) and an oscillating mechanism (3); A lifting and stirring mechanism (2) is provided on the outside of the fixed shell (1), and an oscillating mechanism (3) is provided on the inside of the fixed shell (1).

2. The graphene production process according to claim 1, characterized in that: The specific structure of the lifting and stirring mechanism (2) comprises a guide hole seat (21), a guide hole 1 (22), a lifting hole seat (23), an oil cylinder (24), a mounting seat (25), a temperature control valve (26), a discharge pipe (27), a driving gear 1 (28), a motor 1 (29), a driven gear 1 (210), an internal gear (211), a flow guide seat (212), a flow guide pipe (213), a movable block (214), an inner tank 1 (215), an inner tank 2 (216), a motor 2 (217), a connecting gear (218), a rotating seat (219), a driven gear 2 (220), a driving gear (221), a fixed cover (222), a stirring shaft (223), a heat exchange hole (224), a stirring rod (225), a connecting block (226) and a connecting shaft (227); There are two guide hole seats (21), and the two guide hole seats (21) are respectively fixedly connected to the outside of the left and right sides of the fixed shell (1), and the upper sides of the two guide hole seats (21) are each provided with a guide hole 1 (22), and the guide hole 1 (22) is movably connected to a lifting hole seat (23); The bottom of the mounting seat (25) is fixedly connected to the top of the corresponding lifting hole seat (23) on the left and right sides respectively; There are two oil cylinders (24), the bottoms of the two oil cylinders (24) are respectively fixedly connected to the bottom surface of the corresponding guide hole 1 (22), the outsides of the two oil cylinders (24) are respectively movably connected to the inside of the corresponding mounting seat (25), and the ends of the upper piston rods of the two oil cylinders (24) are respectively fixedly connected to the inside of the left and right sides of the bottom of the mounting seat (25); The rotating seat (219) is movably connected to the central interior of the lower side of the mounting seat (25) via a fixed cover (222), and a driven gear 2 (220) is fixedly connected to the outer portion of the lower side of the rotating seat (219); The second motor (217) is fixedly connected to the right side of the top surface of the mounting seat (25), and a driving gear (221) is fixedly connected to the output shaft at the lower side of the second motor (217), and the driving gear (221) is connected to the second driven gear (220); The outer portion of the internal gear (211) is movably connected to the central interior of the mounting seat (25), and the top of the internal gear (211) is fixedly connected to a driven gear 1 (210); The motor 1 (29) is fixedly connected to the left side of the top surface of the mounting seat (25), and a driving gear 1 (28) is fixedly connected to the output shaft at the lower side of the motor 1 (29), and the driving gear 1 (28) is connected to the driven gear 1 (210); The movable block (214) is movably connected to the central interior of the upper side of the mounting seat (25), and inner groove 1 (215) and inner groove 2 (216) are provided on the inner walls on the left and right sides of the movable block (214); The lower exterior of the flow guide seat (212) is fixedly connected to the central interior of the upper side of the mounting seat (25); the lower interior of the flow guide seat (212) is connected to the interior of the inner groove (215) via a connecting hole; and the upper left opening of the flow guide seat (212) is connected to the outlet of the temperature control valve (26) via a water pipe; The upper outer portion of the flow guide pipe (213) is fixedly connected to the upper central interior of the flow guide seat (212); the lower opening of the flow guide pipe (213) is connected to the interior of the second inner groove (216) through a connecting hole; and the upper opening of the flow guide pipe (213) is connected to the discharge pipe (27); There are two stirring shafts (223), the upper outer parts of the two stirring shafts (223) are movably connected to the left and right inner parts of the rotating seat (219), the upper outer parts of the two stirring shafts (223) are fixedly connected to connecting gears (218), and the connecting gears (218) are connected to the internal gear (211), the interiors of the two stirring shafts (223) are provided with heat exchange holes (224), and the openings on one side of the heat exchange holes (224) are respectively connected to the interiors of the corresponding inner tanks 1 (215), while the openings on the other side of the heat exchange holes (224) are respectively connected to the interiors of the corresponding inner tanks 2 (216), the bottom centers of the two stirring shafts (223) are fixedly connected to connecting shafts (227), and the exteriors of the two stirring shafts (223) are fixedly connected to a plurality of stirring rods (225); The interiors of the left and right sides of the connection block (226) are movably connected to the exteriors of the corresponding connection shafts (227) respectively.

3. The graphene production process according to claim 2, characterized in that: The motor 1 (29) and the motor 2 (217) are both servo motors or variable frequency motors.

4. The graphene production process according to claim 2, characterized in that: A cold water pipe and a hot water pipe are provided on the left side of the temperature control valve (26), and the water temperature in the cold water pipe is 0°C, and the water temperature in the hot water pipe is 45°C.

5. The graphene production process according to claim 2, characterized in that: The guide hole 1 (22) is a rectangular guide hole.

6. The graphene production process according to claim 1, characterized in that: The specific structure of the oscillating mechanism (3) includes a slide groove (31), a slider (32), a slide hole (33), a guide column (34), a reaction tank body (35), a ball (36), a sleeve body (37), a clamping hole block (38), a clamping hole (39), a column (310), a rotating disk (311) and a motor three (312); There are a plurality of slide grooves (31), and the plurality of slide grooves (31) are respectively longitudinally and transversely opened on the left and right sides and the front and rear inner walls of the fixed housing (1); a slider (32) is movably connected to the interior of the plurality of slide grooves (31), and a slide hole (33) is opened in the center of the slider (32); The reaction tank body (35) is located inside the fixed housing (1), and guide pillars (34) are fixedly connected to the left and right sides and the front and rear positions of the reaction tank body (35), and the guide pillars (34) are movably connected to the corresponding sliding holes (33). A clamping hole block (38) is fixedly connected to the center of the bottom of the reaction tank body (35), and a clamping hole (39) is opened in the center of the bottom surface of the clamping hole block (38); There are a plurality of spheres (36), and the plurality of spheres (36) are movably connected to the periphery of the bottom surface of the reaction tank body (35) via a sleeve body (37); The motor three (312) is fixedly connected to the central interior of the lower side of the fixed housing (1); a turntable (311) is fixedly connected to the output shaft on the upper side of the motor three (312); a column (310) is fixedly connected to the edge of the top surface of the turntable (311); and the outside of the column (310) is movably connected to the inside of the clamping hole (39).

7. The graphene production process according to claim 6, characterized in that: The slide groove (31) is a T-shaped slide groove.

8. The graphene production process according to claim 6, characterized in that: The motor three (312) is a servo motor or a variable frequency motor.

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