Graphene raw material processing technology

Abstract

The invention discloses a graphene raw material processing technology, and relates to the technical field of graphene production, and the graphene raw material processing technology comprises the following steps: raw material mixing and stirring, oxidation reaction, washing and filtering, mechanical grinding and magnetic separation, ultrasonic dispersion, reduction reaction and post-treatment. According to the method, the quality and purity of graphite oxide can be effectively guaranteed by accurately controlling the early-stage procedures such as raw material mixing and stirring, oxidation reaction, washing and filtering, and a good foundation is laid for subsequent graphene preparation; a high-energy ball mill is adopted for mechanical grinding, the graphite oxide structure can be refined, the material performance can be improved, iron-based metal impurities can be accurately removed through the arrangement of a magnetic separation device, the quality of a graphene product is further improved, and application of the graphene product in the high-end field is facilitated; through close cooperation of ultrasonic dispersion, reduction reaction and post-treatment procedures, graphene oxide can be stably converted into high-quality graphene, the whole process cost is relatively low, and large-scale industrial production, popularization and application are facilitated.

Description

Technical Field

[0001] The invention relates to the technical field of graphene production, and in particular to a graphene raw material processing technology. Background Art

[0002] With the rapid development of modern science and technology, graphene has shown great application potential in many fields, such as electronic devices, energy storage, and composite material reinforcement, due to its excellent electrical, thermal, and mechanical properties. However, the large-scale preparation of high-quality graphene has always been a key factor restricting its widespread application. Traditional graphene preparation methods face many challenges. For example, although the physical exfoliation method can obtain high-quality graphene, the output is extremely low and it is difficult to meet the needs of industrial large-scale production; although the chemical vapor deposition method can achieve the preparation of large-area graphene, its equipment is expensive, the process is complex and the cost is high, and the production environment requirements are extremely harsh, which limits its popularization and application in large-scale industrial production. In this context, it is particularly urgent to develop a graphene raw material processing technology with relatively simple process steps, low cost, and capable of achieving a certain scale of production. The present invention aims to overcome the shortcomings of the existing preparation process, and through optimizing a series of process steps such as raw material mixing and stirring, oxidation reaction, washing and filtration, mechanical grinding and magnetic separation, ultrasonic dispersion, reduction reaction and post-treatment, a magnetic separation device with a reasonable structural design is used to effectively remove impurities and improve the purity and quality of graphene products, so as to provide a feasible and efficient solution for the industrial production of graphene, meet the growing market demand for graphene materials, and promote the rapid development of graphene-related industries. Summary of the invention

[0003] The purpose of the present invention is to provide a graphene raw material processing technology in order to solve the above problems, which solves the problems existing in the traditional graphene preparation process, such as low output, expensive and complex equipment, high cost, difficulty in large-scale industrial production, and difficulty in ensuring product purity and quality.

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

[0005] A. Mixing and stirring raw materials: Add graphite powder, concentrated sulfuric acid and sodium nitrate into the reaction container in proportion, and start the stirring equipment to fully mix the raw materials;

[0006] B. Oxidation reaction: The temperature of the reaction vessel in step A is controlled at 0-5°C, and then potassium permanganate solution is slowly added dropwise while controlling the dropping speed to maintain a stable temperature, and stirring is continued for several hours to oxidize the graphite to form graphite oxide;

[0007] C. Washing and filtering: dilute the graphite oxide in step B with a large amount of deionized water, and then wash and filter for multiple times to remove impurity ions;

[0008] D. Mechanical grinding and magnetic separation:

[0009] a. Mechanical grinding: placing the graphite oxide treated in step C in a high-energy ball mill for grinding;

[0010] b. Magnetic separation: The ground graphite oxide is transported to a magnetic separation device for magnetic separation;

[0011] E. Ultrasonic dispersion: dispersing the graphite oxide treated in step D in water and performing ultrasonic treatment to form a graphene oxide suspension;

[0012] F. Reduction reaction: adding a reducing agent to the graphene oxide suspension in step E, wherein the reducing agent reduces the oxygen-containing functional groups in the graphene oxide to carbon atoms, thereby obtaining graphene;

[0013] G. Post-treatment: washing and filtering the graphene in step F to remove unreacted reducing agent and impurities, and then vacuum drying or freeze drying to obtain graphene powder or film;

[0014] The specific structure of the magnetic separation device in step D includes a feeding funnel, a conveying and screening mechanism, a fixed shell, a separation chamber, a conveying and magnetic separation mechanism, an iron collection mechanism and a graphite oxide collection mechanism; a separation chamber is arranged inside the fixed shell; the conveying and screening mechanism is externally fixedly connected to the upper left side of the separation chamber, and the upper left inlet of the conveying and screening mechanism is connected to the feeding funnel outlet; the conveying and magnetic separation mechanism is arranged on the upper side of the separation chamber; the iron collection mechanism is located on the lower left side of the conveying and magnetic separation mechanism, and the iron collection mechanism is arranged on the lower left side of the separation chamber; the graphite oxide collection mechanism is located on the lower right side of the conveying and magnetic separation mechanism, and the graphite oxide collection mechanism is arranged on the lower right side of the separation chamber.

[0015] Preferably, the reaction temperature in step F is 80 - 120°C.

[0016] Preferably, the specific structure of the conveying and screening mechanism includes an outer shell, a conveying channel, a screw rod, a driven gear, a motor 1, a driving gear, a blanking port, a diversion groove, a diversion plate, a guide block, a longitudinal guide groove, a movable shell, an inner cavity, a vertical guide groove, a turntable, a motor 2, a connecting shaft, a screening hole and an output port; the outer shell is fixedly connected to the upper left side of the separation chamber on the outside, and the motor 1 is fixedly connected to the center of the left side of the outer shell; a driving gear is fixedly connected to the right output shaft of the motor 1; the blanking port is opened on the upper left side of the outer shell; there are two conveying channels, and the two conveying channels are respectively arranged longitudinally and arranged inside the left side of the outer shell, and the upper left side openings of the two conveying channels are connected to the lower side opening of the blanking port; there are two screw rods, and the two screw rods are respectively movably connected to the corresponding conveying channels, and the left side of the screw rods are fixedly connected to the driven gear on the outside Wheel, and the driven gears are connected with the driving gear; the inner cavity is arranged inside the right side of the outer shell, a longitudinal guide groove is opened on the top surface of the inner cavity, a diverter groove is arranged on the left side of the inner cavity, and the inside of the diverter groove is communicated with the right opening of the conveying channel, and an output port is opened on the lower side of the inner cavity; there are several diverter plates, and several diverter plates are respectively and evenly fixedly connected inside the diverter groove; the movable shell is movably connected inside the inner cavity, a guide block is fixedly connected to the top of the movable shell, and the outside of the guide block is longitudinally movably connected inside the longitudinal guide groove, a number of screening holes are opened on the bottom surface of the movable shell, and a vertical guide groove is opened in the center of the right side of the movable shell; the second motor is fixedly connected inside the right side of the outer shell, and a turntable is fixedly connected to the left output shaft of the second motor; a connecting shaft is fixedly connected to the left edge of the turntable, and the outside of the connecting shaft is movably connected inside the vertical guide groove.

[0017] Preferably, the motor 1 is a servo motor or a stepper motor, and the longitudinal guide groove is a T-shaped longitudinal guide groove, and matches the outer part of the guide block.

[0018] Preferably, the specific structure of the conveying magnetic separation mechanism includes motor three, active roller one, conveyor belt one, conveying plate, mounting seat, electromagnetic suction cup and driven roller one; motor three is fixedly connected to the outside of the rear side of the outer shell; active roller one is movably connected to the upper left side of the separation chamber, and the rear center of active roller one is fixedly connected to the output shaft of motor three; driven roller one is movably connected to the right side of the separation chamber, and driven roller one is connected to active roller one through conveyor belt one, and a plurality of conveying plates are fixedly connected to the outer surface of conveyor belt one; mounting seat is fixedly connected to the upper side of the separation chamber, the top surface of mounting seat is connected to the inner top surface of conveyor belt one, and an electromagnetic suction cup is fixedly connected to the lower side of mounting seat.

[0019] Preferably, the motor three is a servo motor or a stepper motor.

[0020] Preferably, the specific structure of the iron collection mechanism includes motor four, active roller two, conveyor belt two, support block one, driven roller two and collection box one; the motor four is fixedly connected to the outside of the lower left rear side of the fixed shell; the active roller two is movably connected to the lower left side of the separation chamber; the driven roller two is located on the right side of the active roller two, the driven roller two is movably connected to the lower side of the separation chamber, and the driven roller two is connected to the active roller two through conveyor belt two; the support block one is fixedly connected to the lower side of the separation chamber, and the top surface of the support block one is connected to the inner top surface of the conveyor belt two; the collection box one is located on the lower left side of the separation chamber.

[0021] Preferably, the motor four is a servo motor or a stepper motor.

[0022] Preferably, the specific structure of the graphite oxide collection mechanism includes a baffle, a motor five, an active roller three, a support block two, a conveyor belt three, a transition roller, a support block three, a driven roller three and a collection box two; the motor five is fixedly connected to the outside of the lower rear center of the fixed shell; the active roller three is movably connected to the center of the lower side of the separation chamber, and the rear center of the active roller three is fixedly connected to the output shaft of the motor five; the baffle is located on the left side of the active roller three, and the baffle is fixedly connected to the left side of the center of the lower side of the separation chamber; the collection box two is located on the lower side of the active roller three; the transition roller position On the upper right side of the active roller three, the transition roller is movably connected inside the separation chamber; the driven roller three is movably connected on the lower right side of the separation chamber, and the driven roller three is connected to the transition roller and the active roller three through the conveyor belt three; the support block two is located between the active roller three and the transition roller, the support block two is fixedly connected inside the separation chamber, and the top surface of the support block two is connected to the inner side surface of the conveyor belt three; the support block three is located between the transition roller and the driven roller three, the support block three is fixedly connected inside the separation chamber, and the top surface of the support block three is connected to the inner side surface of the conveyor belt three.

[0023] Preferably, the motor five is a servo motor or a stepper motor.

[0024] The beneficial effects of the present invention are as follows: (1) The present invention has the characteristics of clear and reasonable process steps, convenient and efficient operation, and can effectively ensure the quality and purity of graphite oxide by accurately controlling the preliminary processes such as raw material mixing and stirring, oxidation reaction, washing and filtration, thus laying a good foundation for the subsequent graphene preparation.

[0025] (2) The high-energy ball mill used in the present invention for mechanical grinding can refine the structure of graphite oxide and improve the material properties. The magnetic separation device can accurately remove iron-based metal impurities, further improving the quality of graphene products and facilitating their application in high-end fields.

[0026] (3) In the present invention, through the close coordination of ultrasonic dispersion, reduction reaction and post-treatment steps, graphene oxide can be stably converted into high-quality graphene, and the cost of the entire process is relatively low, which is conducive to large-scale industrial production and promotion and application. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a schematic diagram of the structure of the present invention.

[0028] Figure 2 for Figure 1 sectional view of .

[0029] Figure 3 It is a structural diagram of the conveying and screening mechanism.

[0030] Figure 4 It is a structural diagram of the conveying magnetic separation mechanism.

[0031] Figure 5 Schematic diagram of the structure of the iron collection mechanism.

[0032] Figure 6 Schematic diagram of the structure of graphite oxide collection mechanism.

[0033] 1-feeding hopper; 2-conveying and screening mechanism; 3-fixed shell; 4-separation chamber; 5-conveying and magnetic separation mechanism; 6-iron collection mechanism; 7-graphite oxide collection mechanism; 21-outer shell; 22-conveying channel; 23-screw rod; 24-driven gear; 25-motor 1; 26-driving gear; 27-feeding port; 28-diverter slot; 29-diverter plate; 210-guide block; 211-longitudinal guide slot; 212-movable shell; 213-inner cavity; 214-vertical guide slot; 215-turntable; 216-motor 2; 217-connecting shaft; 218-screening hole; 219-output port; 51-motor three; 52-active roller one; 53-conveyor belt one; 54-conveyor plate; 55-mounting seat; 56-electromagnetic suction cup; 57-driven roller; 61-motor four; 62-active roller two; 63-conveyor belt two; 64-support block one; 65-driven roller; 66-collection box one; 71-baffle; 72-motor five; 73-active roller three; 74-support block two; 75-conveyor belt three; 76-transition roller; 77-support block three; 78-driven roller three; 79-collection box two. DETAILED DESCRIPTION

[0034] like Figure 1 and Figure 2 As shown, this specific embodiment adopts the following technical solution: a graphene raw material processing process, comprising the following steps:

[0035] A. Mixing and stirring raw materials: Add graphite powder, concentrated sulfuric acid and sodium nitrate into the reaction container in proportion, and start the stirring equipment to fully mix the raw materials;

[0036] B. Oxidation reaction: The temperature of the reaction vessel in step A is controlled at 0-5°C, and then potassium permanganate solution is slowly added dropwise while controlling the dropping speed to maintain a stable temperature, and stirring is continued for several hours to oxidize the graphite to form graphite oxide;

[0037] C. Washing and filtering: dilute the graphite oxide in step B with a large amount of deionized water, and then wash and filter for multiple times to remove impurity ions;

[0038] D. Mechanical grinding and magnetic separation:

[0039] a. Mechanical grinding: placing the graphite oxide treated in step C in a high-energy ball mill for grinding;

[0040] b. Magnetic separation: The ground graphite oxide is transported to a magnetic separation device for magnetic separation;

[0041] E. Ultrasonic dispersion: dispersing the graphite oxide treated in step D in water and performing ultrasonic treatment to form a graphene oxide suspension;

[0042] F. Reduction reaction: adding a reducing agent to the graphene oxide suspension in step E, wherein the reducing agent reduces the oxygen-containing functional groups in the graphene oxide to carbon atoms, thereby obtaining graphene;

[0043] G. Post-treatment: washing and filtering the graphene in step F to remove unreacted reducing agent and impurities, and then vacuum drying or freeze drying to obtain graphene powder or film;

[0044] The specific structure of the magnetic separation device in step D includes a feeding funnel 1, a conveying and screening mechanism 2, a fixed shell 3, a separation chamber 4, a conveying and magnetic separation mechanism 5, an iron collection mechanism 6 and a graphite oxide collection mechanism 7; a separation chamber 4 is arranged inside the fixed shell 3; the conveying and screening mechanism 2 is externally fixedly connected to the upper left side of the separation chamber 4, and the upper left inlet of the conveying and screening mechanism 2 is connected to the outlet of the feeding funnel 1; the conveying and magnetic separation mechanism 5 is arranged on the upper side of the separation chamber 4; the iron collection mechanism 6 is located on the lower left side of the conveying and magnetic separation mechanism 5, and the iron collection mechanism 6 is arranged on the lower left side of the separation chamber 4; the graphite oxide collection mechanism 7 is located on the lower right side of the conveying and magnetic separation mechanism 5, and the graphite oxide collection mechanism 7 is arranged on the lower right side of the separation chamber 4.

[0045] Wherein, the reaction temperature in step F is 80 - 120°C.

[0046] like Figure 3As shown, the specific structure of the conveying and screening mechanism 2 includes an outer shell 21, a conveying channel 22, a screw rod 23, a driven gear 24, a motor 1 25, a driving gear 26, a blanking port 27, a diverter slot 28, a diverter plate 29, a guide block 210, a longitudinal guide slot 211, a movable shell 212, an inner cavity 213, a vertical guide slot 214, a turntable 215, a motor 216, a connecting shaft 217, a screening hole 218 and an output port 219; the outer shell 21 is fixedly connected to the upper left side of the separation chamber 4, and the left center of the outer shell 21 is fixedly connected to the motor 21. The motor 25 is provided with a driving gear 26 fixedly connected to the right output shaft of the motor 25; the blanking port 27 is provided on the upper left side of the outer shell 21; there are two conveying channels 22, which are arranged longitudinally and arranged inside the left side of the outer shell 21, and the upper left openings of the two conveying channels 22 are connected to the lower opening of the blanking port 27; there are two screw rods 23, which are movably connected to the corresponding conveying channels 22, and the left side of the screw rods 23 are fixedly connected to the driven gear 24, and The driven gears 24 are connected to the driving gears 26; the inner cavity 213 is arranged inside the right side of the outer shell 21, and a longitudinal guide groove 211 is provided on the top surface of the inner cavity 213. A diverter groove 28 is provided on the left side of the inner cavity 213, and the inside of the diverter groove 28 is connected to the right opening of the conveying channel 22, and an output port 219 is provided on the lower side of the inner cavity 213; there are several diverter plates 29, and several diverter plates 29 are evenly fixedly connected inside the diverter groove 28; the movable shell 212 is movably connected inside the inner cavity 213, and the movable shell 21 A guide block 210 is fixedly connected to the top of the outer shell 21, and the outer portion of the guide block 210 is longitudinally movably connected to the inner portion of the longitudinal guide groove 211. A plurality of screening holes 218 are provided on the bottom surface of the movable shell 212, and a vertical guide groove 214 is provided in the center of the right side of the movable shell 212. The second motor 216 is fixedly connected to the inner portion of the right side of the outer shell 21, and a rotating disk 215 is fixedly connected to the left output shaft of the second motor 216. A connecting shaft 217 is fixedly connected to the left edge of the rotating disk 215, and the outer portion of the connecting shaft 217 is movably connected to the inner portion of the vertical guide groove 214.

[0047] The motor 25 is a servo motor or a stepper motor, so that the motor 25 can be easily controlled by existing automation technology. The longitudinal guide groove 211 is a T-shaped longitudinal guide groove, and matches the outer part of the guide block 210 .

[0048] like Figure 4As shown, the specific structure of the conveying magnetic separation mechanism 5 includes a motor 3 51, an active roller 1 52, a conveyor belt 1 53, a conveying plate 54, a mounting seat 55, an electromagnetic suction cup 56 and a driven roller 1 57; the motor 3 51 is fixedly connected to the outside of the rear side of the outer shell 21; the active roller 1 52 is movably connected to the upper left side of the separation chamber 4, and the rear center of the active roller 1 52 is fixedly connected to the output shaft of the motor 3 51; the driven roller 1 57 is movably connected to the right side of the separation chamber 4, and the driven roller 1 57 is connected to the active roller 1 52 through the conveyor belt 1 53, and a plurality of conveying plates 54 are fixedly connected to the outer surface of the conveyor belt 1 53; the mounting seat 55 is fixedly connected to the upper side of the separation chamber 4, the top surface of the mounting seat 55 is connected to the inner top surface of the conveyor belt 1 53, and the lower side of the mounting seat 55 is fixedly connected to the electromagnetic suction cup 56.

[0049] Wherein, the motor three 51 is a servo motor or a stepper motor, so that the motor three 51 can be easily controlled by existing automation technology.

[0050] like Figure 5 As shown, the specific structure of the iron collecting mechanism 6 includes a motor 4 61, an active roller 2 62, a conveyor belt 2 63, a support block 1 64, a driven roller 2 65 and a collecting box 1 66; the motor 4 61 is fixedly connected to the outside of the lower left rear side of the fixed shell 3; the active roller 2 62 is movably connected to the lower left side of the separation chamber 4; the driven roller 2 65 is located on the right side of the active roller 2 62, the driven roller 2 65 is movably connected to the lower side of the separation chamber 4, and the driven roller 2 65 is connected to the active roller 2 62 through the conveyor belt 2 63; the support block 1 64 is fixedly connected to the lower side of the separation chamber 4, and the top surface of the support block 1 64 is connected to the inner top surface of the conveyor belt 2 63; the collecting box 1 66 is located on the lower left side of the separation chamber 4.

[0051] Among them, the motor four 61 is a servo motor or a stepper motor, so it is convenient to control the motor four 61 through existing automation technology.

[0052] like Figure 6As shown, the specific structure of the graphite oxide collecting mechanism 7 includes a baffle 71, a motor 5 72, an active roller 3 73, a support block 2 74, a conveyor belt 3 75, a transition roller 76, a support block 3 77, a driven roller 3 78 and a collection box 2 79; the motor 5 72 is fixedly connected to the outside of the lower rear center of the fixed shell 3; the active roller 3 73 is movably connected to the center of the lower side of the separation chamber 4, and the rear center of the active roller 3 73 is fixedly connected to the output shaft of the motor 5 72; the baffle 71 is located on the left side of the active roller 3 73, and the baffle 71 is fixedly connected to the left side of the lower center of the separation chamber 4; the collection box 2 79 is located on the lower side of the active roller 3 73; the transition roller 76 is located On the upper right side of the active roller three 73, the transition roller 76 is movably connected to the inside of the separation chamber 4; the driven roller three 78 is movably connected to the lower right side of the separation chamber 4, and the driven roller three 78 is connected to the transition roller 76 and the active roller three 73 through the conveyor belt three 75; the support block two 74 is located between the active roller three 73 and the transition roller 76, and the support block two 74 is fixedly connected to the inside of the separation chamber 4, and the top surface of the support block two 74 is connected to the inner side surface of the conveyor belt three 75; the support block three 77 is located between the transition roller 76 and the driven roller three 78, and the support block three 77 is fixedly connected to the inside of the separation chamber 4, and the top surface of the support block three 77 is connected to the inner side surface of the conveyor belt three 75.

[0053] Wherein, the motor five 72 is a servo motor or a stepper motor, so that the motor five 72 can be easily controlled by existing automation technology.

[0054] The use status of the present invention is as follows: the present invention has a reasonable and simple structure, low production cost, and convenient installation. In the graphene raw material processing process, firstly, graphite powder, concentrated sulfuric acid and sodium nitrate are put into a specific reaction container in proportion. After the stirring device is turned on, the raw materials are quickly mixed. Then, the temperature of the reaction container is accurately controlled at 0-5°C, and potassium permanganate solution is slowly dripped in. The dripping speed is strictly controlled to maintain low temperature stability. Continuous stirring for several hours promotes the successful oxidation of graphite to graphite oxide. Subsequently, a large amount of deionized water is used to dilute the graphite oxide. Multiple washing and filtering operations are performed to completely remove the impurity ions therein. The treated graphite oxide is placed in a high-energy ball mill. Under the strong grinding action, its structure The ground graphite oxide is gradually refined and then transported to the magnetic separation device for magnetic separation. When the magnetic separation device is used, the graphite oxide is first added to the feeding funnel 1 for grinding, and then the ground graphite oxide enters the conveying channel 22 through the drop port 27, and then the motor 1 25 is started to drive the driven gear 24 and the screw rod 23 to rotate through the driving gear 26, and the rotation of the screw rod 23 can transport the ground graphite oxide to the diversion groove 28, and then the diversion plate 29 is diverted and evenly enters the movable shell 212, and then the started motor 216 drives the turntable 215 to rotate, and the rotation of the turntable 215 is connected through the connecting shaft 217. The vertical guide groove 214 drives the movable shell 212 to move repeatedly in the longitudinal direction as a whole, so that the incoming graphite oxide can be screened and scattered, which makes it easier for the graphite oxide to be evenly spread on the conveyor belt 1 53, thereby ensuring the efficiency and quality of subsequent magnetic separation. The conveying magnetic separation mechanism 5 set here can evenly convey the graphite oxide to the conveyor belt 3 75, and then the conveyor belt 3 75 conveys the graphite oxide to the lower side of the electromagnetic suction cup 56 for iron-based metal adsorption, and the remaining graphite oxide continues to be conveyed by the conveyor belt 3 75 and finally falls into the collection box 2 79 for collection. In addition, as the conveying magnetic separation mechanism 5 works, the adsorbed iron-based metal can be conveyed to the iron On the collecting mechanism 6, when the iron-based metal is separated from the electromagnetic suction cup 56, it will directly fall onto the conveyor belt 2 63, so that the iron-based metal can be transported to the collecting box 1 66 for collection through the conveyor belt 2 63, which improves the convenience during use. After the magnetic separation is completed, the graphite oxide is dispersed in water and subjected to ultrasonic treatment to form a graphene oxide suspension. Then, a reducing agent is added to the suspension. Under the reaction conditions of 80-120°C, the oxygen-containing functional groups are reduced to carbon atoms, and graphene is successfully obtained. Finally, the graphene is washed and filtered to remove unreacted reducing agent and impurities, and then vacuum dried or freeze-dried to finally obtain a graphene powder or film product.

[0055] 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.

[0056] 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.

[0057] 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.

[0058] 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 raw material processing process, characterized in that: The following steps are involved: A. Mixing and stirring raw materials: Add graphite powder, concentrated sulfuric acid and sodium nitrate into the reaction container in proportion, and start the stirring equipment to fully mix the raw materials; B. Oxidation reaction: The temperature of the reaction vessel in step A is controlled at 0-5°C, and then potassium permanganate solution is slowly added dropwise while controlling the dropping speed to maintain a stable temperature, and stirring is continued for several hours to oxidize the graphite to form graphite oxide; C. Washing and filtering: dilute the graphite oxide in step B with a large amount of deionized water, and then wash and filter for multiple times to remove impurity ions; D. Mechanical grinding and magnetic separation: a. Mechanical grinding: placing the graphite oxide treated in step C in a high-energy ball mill for grinding; b. Magnetic separation: The ground graphite oxide is transported to a magnetic separation device for magnetic separation; E. Ultrasonic dispersion: dispersing the graphite oxide treated in step D in water and performing ultrasonic treatment to form a graphene oxide suspension; F. Reduction reaction: adding a reducing agent to the graphene oxide suspension in step E, wherein the reducing agent reduces the oxygen-containing functional groups in the graphene oxide to carbon atoms, thereby obtaining graphene; G. Post-treatment: washing and filtering the graphene in step F to remove unreacted reducing agent and impurities, and then vacuum drying or freeze drying to obtain graphene powder or film; The specific structure of the magnetic separation device in step D comprises a feeding funnel (1), a conveying and screening mechanism (2), a fixed shell (3), a separation chamber (4), a conveying and magnetic separation mechanism (5), an iron collection mechanism (6) and a graphite oxide collection mechanism (7); A separation chamber (4) is provided inside the fixed shell (3); The conveying and screening mechanism (2) is externally fixedly connected to the upper left side of the separation chamber (4), and the upper left inlet of the conveying and screening mechanism (2) is connected to the outlet of the feeding funnel (1); The conveying magnetic separation mechanism (5) is arranged on the upper side of the separation chamber (4); The iron collecting mechanism (6) is located at the lower left side of the conveying magnetic separation mechanism (5), and the iron collecting mechanism (6) is arranged at the lower left side of the separation chamber (4); The graphite oxide collecting mechanism (7) is located at the lower right side of the conveying magnetic separation mechanism (5), and the graphite oxide collecting mechanism (7) is arranged at the lower right side of the separation chamber (4).

2. The graphene raw material processing process according to claim 1, characterized in that: The reaction temperature in step F is 80 - 120°C.

3. The graphene raw material processing process according to claim 1, characterized in that: The specific structure of the conveying and screening mechanism (2) includes an outer shell (21), a conveying channel (22), a screw rod (23), a driven gear (24), a motor 1 (25), a driving gear (26), a material drop opening (27), a diverter groove (28), a diverter plate (29), a guide block (210), a longitudinal guide groove (211), a movable shell (212), an inner cavity (213), a vertical guide groove (214), a rotating disk (215), a motor 2 (216), a connecting shaft (217), a screening hole (218) and an output port (219); The outer shell (21) is fixedly connected to the upper left side of the separation chamber (4) on the outside, and the left center of the outer shell (21) is fixedly connected to the motor 1 (25); A driving gear (26) is fixedly connected to the right output shaft of the motor 1 (25); The blanking opening (27) is opened on the upper left side of the outer shell (21); There are two conveying channels (22), the two conveying channels (22) are respectively arranged longitudinally and are arranged inside the left side of the outer shell (21), and the upper left openings of the two conveying channels (22) are connected to the lower opening of the blanking port (27); There are two spiral rods (23), and the two spiral rods (23) are movably connected to the inside of the corresponding conveying channel (22), and the left side of the spiral rod (23) is fixedly connected to a driven gear (24), and the driven gear (24) is connected to the driving gear (26); The inner cavity (213) is arranged inside the right side of the outer shell (21), a longitudinal guide groove (211) is provided on the top surface of the inner cavity (213), a diversion groove (28) is provided on the left side of the inner cavity (213), and the inside of the diversion groove (28) is connected to the right opening of the conveying channel (22), and an output port (219) is provided on the lower side of the inner cavity (213); There are a plurality of the diverter plates (29), and the plurality of the diverter plates (29) are evenly fixedly connected to the inside of the diverter slot (28); The movable shell (212) is movably connected to the inner cavity (213); a guide block (210) is fixedly connected to the top of the movable shell (212); and the outer portion of the guide block (210) is longitudinally movably connected to the inner portion of the longitudinal guide groove (211); a plurality of screening holes (218) are provided on the bottom surface of the movable shell (212); and a vertical guide groove (214) is provided in the center of the right side of the movable shell (212); The second motor (216) is fixedly connected to the inside of the right side of the outer shell (21), and a rotating disk (215) is fixedly connected to the output shaft on the left side of the second motor (216); A connecting shaft (217) is fixedly connected to the left edge of the rotating disk (215), and the outside of the connecting shaft (217) is movably connected to the inside of the vertical guide groove (214).

4. The graphene raw material processing process according to claim 3, characterized in that: The motor 1 (25) is a servo motor or a stepping motor, and the longitudinal guide groove (211) is a T-shaped longitudinal guide groove, and matches the outside of the guide block (210).

5. The graphene raw material processing process according to claim 1, characterized in that: The specific structure of the conveying magnetic separation mechanism (5) includes a motor three (51), an active roller one (52), a conveyor belt one (53), a conveyor plate (54), a mounting seat (55), an electromagnetic suction cup (56) and a driven roller one (57); The motor three (51) is fixedly connected to the rear exterior of the outer shell (21); The active roller wheel 1 (52) is movably connected to the upper left side of the separation chamber (4), and the rear center of the active roller wheel 1 (52) is fixedly connected to the output shaft of the motor 3 (51); The driven roller wheel 1 (57) is movably connected to the right side of the separation chamber (4); the driven roller wheel 1 (57) is connected to the driving roller wheel 1 (52) through a conveyor belt 1 (53); and a plurality of conveyor plates (54) are fixedly connected to the outer surface of the conveyor belt 1 (53); The mounting seat (55) is fixedly connected to the upper side of the separation chamber (4); the top surface of the mounting seat (55) is connected to the inner top surface of the conveyor belt (53); and an electromagnetic suction cup (56) is fixedly connected to the interior of the lower side of the mounting seat (55).

6. The graphene raw material processing process according to claim 5, characterized in that: The motor three (51) is a servo motor or a stepper motor.

7. The graphene raw material processing process according to claim 1, characterized in that: The specific structure of the iron collecting mechanism (6) includes a motor 4 (61), a driving roller 2 (62), a conveyor belt 2 (63), a supporting block 1 (64), a driven roller 2 (65) and a collecting box 1 (66); The motor 4 (61) is fixedly connected to the outside of the lower left rear side of the fixed housing (3); The second active roller (62) is movably connected to the lower left side of the separation chamber (4); The driven roller wheel 2 (65) is located on the right side of the active roller wheel 2 (62), the driven roller wheel 2 (65) is movably connected to the lower side of the separation chamber (4), and the driven roller wheel 2 (65) is connected to the active roller wheel 2 (62) through the conveyor belt 2 (63); The support block 1 (64) is fixedly connected to the lower side of the separation chamber (4), and the top surface of the support block 1 (64) is connected to the inner top surface of the conveyor belt 2 (63); The collecting box 1 (66) is located at the lower left side of the separation chamber (4).

8. The graphene raw material processing process according to claim 7, characterized in that: The motor four (61) is a servo motor or a stepper motor.

9. The graphene raw material processing process according to claim 1, characterized in that: The specific structure of the graphite oxide collecting mechanism (7) includes a baffle (71), a motor five (72), a driving roller three (73), a supporting block two (74), a conveyor belt three (75), a transition roller (76), a supporting block three (77), a driven roller three (78) and a collecting box two (79); The motor 5 (72) is fixedly connected to the outside of the lower rear center of the fixed housing (3); The active roller wheel three (73) is movably connected to the center of the lower side of the separation chamber (4), and the rear center of the active roller wheel three (73) is fixedly connected to the output shaft of the motor five (72); The baffle (71) is located on the left side of the active roller wheel 3 (73), and the baffle (71) is fixedly connected to the left side of the center of the lower side of the separation chamber (4); The second collecting box (79) is located at the lower side of the active roller (73); The transition roller (76) is located on the upper right side of the active roller three (73), and the transition roller (76) is movably connected inside the separation chamber (4); The driven roller wheel three (78) is movably connected to the lower right side of the separation chamber (4), and the driven roller wheel three (78) is connected to the transition roller wheel (76) and the driving roller wheel three (73) through the conveyor belt three (75); The support block 2 (74) is located between the active roller 3 (73) and the transition roller (76), the support block 2 (74) is fixedly connected to the inside of the separation chamber (4), and the top surface of the support block 2 (74) is connected to the inner side surface of the conveyor belt 3 (75); The support block three (77) is located between the transition roller (76) and the driven roller three (78), the support block three (77) is fixedly connected to the inside of the separation chamber (4), and the top surface of the support block three (77) is connected to the inner side surface of the conveyor belt three (75).

10. The graphene raw material processing process according to claim 9, characterized in that: The motor five (72) is a servo motor or a stepper motor.

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