Continuous graphitization treatment equipment

Abstract

The utility model relates to the technical field of graphene, and provides continuous graphitization treatment equipment which comprises a material transition chamber, a graphitization chamber and a cooling chamber which are all provided with vacuumizing pipes, and the material transition chamber and the cooling chamber are respectively arranged at the upper end and the lower end of the graphitization chamber through high-temperature valves. Vacuum ball valves are arranged at the upper end of the material transition chamber and the lower end of the cooling chamber; and a circulating heat exchange system is arranged between the cooling chamber and the material transition chamber. A large amount of heat released in the cooling chamber is conveyed into the material transition chamber through the circulating heat exchange system for heat exchange, the heat exchange is used for preheating materials in the material transition chamber, and a medium in the circulating heat exchange system exchanges heat in the second heat exchange pipe and then flows back to the first heat exchange pipe through the return pipe to absorb heat again. The process is circulated to realize cyclic utilization of heat, the production cost of graphitization is reduced, meanwhile, the material is preheated in advance, so that the material is heated more uniformly, and the graphitization efficiency and the product quality are improved.

Description

Technical Field

[0001] The utility model relates to the technical field of graphene, in particular to a continuous graphitization treatment device. Background Art

[0002] In the continuous production process of graphene, the heat recycling between the feeding bin and the cooling bin is a key technical link, which directly affects the production efficiency and product quality. However, many current graphene production lines still face technical bottlenecks in this link, resulting in the failure to effectively recycle heat. The specific background art is as follows:

[0003] As a new type of nanomaterial, graphene exhibits great application potential in many fields such as electronics, energy, and materials science due to its excellent electrical and thermal conductivity, as well as high strength and high toughness. However, the preparation process of graphene is complex and energy-consuming. Especially when using methods such as chemical vapor deposition (CVD) in a high-temperature environment, a large amount of heat energy is consumed. Therefore, optimizing thermal management and realizing heat recycling are of great significance for reducing production costs and improving production efficiency.

[0004] In the continuous production line of graphene, the feeding bin is responsible for stably and continuously feeding raw materials into the reaction zone, while the cooling bin is responsible for rapidly reducing the temperature after the graphene is prepared to prevent the product from overheating and being damaged or undergoing unnecessary phase changes. However, in the existing production line designs, there is often a lack of an effective heat transfer and recycling mechanism between the feeding bin and the cooling bin.

[0005] On the one hand, when the cooling bin cools the graphene product, a large amount of heat energy is generated, and this heat is directly discharged into the environment without being effectively utilized. On the other hand, the feeding bin also consumes a large amount of heat when preheating the raw materials. If an external heat source is used for heating, it will cause waste of energy. Due to the failure to effectively transfer and recycle the heat between the feeding bin and the cooling bin, the thermal efficiency of the entire production process is low, and the production cost is high.

[0006] In addition, the lack of heat recycling may also affect the quality of graphene products. For example, during the cooling process, if the cooling speed is too fast or uneven, it may cause incomplete crystallization of graphene, affecting its electrical conductivity and stability. If heat recycling can be achieved, by adjusting the initial temperature or cooling rate of the cooling bin, the crystallization process of graphene can be optimized, and the product quality can be improved.

[0007] In summary, the failure to achieve heat recycling between the feeding bin and the cooling bin in the continuous production process of graphene is a current technical problem. Summary of the Utility Model

[0008] The object of the present utility model is to overcome the above deficiencies of the prior art, and provide an efficient heat exchange system, optimize the structural layout of the feeding bin and the cooling bin, so as to achieve effective heat transfer and recycling, reduce production costs, improve production efficiency, and further improve the quality and performance of graphene products in a continuous graphitization treatment device.

[0009] The technical solution of the present utility model is: a continuous graphitization treatment device, including a material transition chamber, a graphitization chamber and a cooling chamber all provided with a vacuum extraction pipe. The material transition chamber and the cooling chamber are respectively arranged at the upper end and the lower end of the graphitization chamber through high-temperature valves. Vacuum ball valves are arranged at the upper end of the material transition chamber and the lower end of the cooling chamber. A circulating heat exchange system is arranged between the cooling chamber and the material transition chamber.

[0010] Further, a graphitization device is arranged in the graphitization chamber. The graphitization device includes a high-purity graphite crucible, a heat-insulating layer and an induction coil. The induction coil is arranged on the periphery of the crucible, and a heat-insulating layer is arranged between the induction coil and the crucible. The graphitization chamber adopts a sandwich structure, and cooling water circulates in the sandwich.

[0011] Further, insulating protective layers are arranged on both the inner and outer sides of the induction coil.

[0012] Further, the crucible is in a circular tube shape with a diameter of 10 - 100 cm. Preferably, the diameter of the crucible is 20 - 90 cm and the length is 100 - 400 cm. More preferably, the diameter of the crucible is 40 cm and the length is 200 cm to ensure the graphitization effect of the material.

[0013] Further, both the cooling chamber and the material transition chamber are of double-layer jacket structures.

[0014] Further, the circulating heat exchange system includes an inlet heat pipe, a first heat exchange pipe, a second heat exchange pipe and a heat exchange pump. The first heat exchange pipe and the second heat exchange pipe are respectively arranged in the jackets of the cooling chamber and the material transition chamber. The upper end and the lower end of the inlet heat pipe are respectively connected to the second heat exchange pipe and the first heat exchange pipe. The heat exchange pump is arranged on the inlet heat pipe. A return pipe is also arranged between the second heat exchange pipe and the first heat exchange pipe.

[0015] Preferably, a medium circulates in the circulating heat exchange system, and the medium is a circulating liquid such as water, molten salt, oil, etc. that can achieve heat exchange.

[0016] Further, the circulating liquid in the first heat exchange pipe enters from the bottom and exits from the top, and the circulating liquid in the second heat exchange pipe enters from the top and exits from the bottom. Preferably, both the first heat exchange pipe and the second heat exchange pipe adopt the bottom-in and top-out mode to facilitate the efficiency of heat exchange.

[0017] Further, air inlets are arranged at the lower ends of the material transition chamber, the graphitization chamber and the cooling chamber, and air outlets are arranged at the upper ends, which are used to circulate protective gas to protect the material.

[0018] Furthermore, a temperature measuring device is provided on the graphitization chamber. The temperature measuring device includes an infrared measuring device for measuring inside the graphite crucible and a thermocouple temperature measuring device for measuring the induction coil part; the measured temperature is sampled by a PLC and stored in a removable disk regularly. The temperature control uses a thyristor inverter system to control the output to control the heating power. The temperature control instrument sets the temperature to be controlled, and the temperature control instrument performs PID closed-loop control according to the set temperature.

[0019] Furthermore, it also includes a PLC controller. The system is controlled and displayed in real time through the touch screen graphic display operation terminal on the controller, and the temperature, vacuum degree, and equipment operation status are controlled and operated.

[0020] The utility model has the following beneficial effects:

[0021] Through the circulating heat exchange system, a large amount of heat released in the cooling chamber is transported to the material transition chamber for heat exchange. The exchanged heat is used to preheat the materials in the material transition chamber. The medium in the circulating heat exchange system exchanges heat in the second heat exchange tube and then returns to the first heat exchange tube through the return pipe to absorb heat again. In the above process, the heat is recycled, reducing the production cost of graphitization. At the same time, the materials are preheated in advance, making the materials heated more evenly, improving the efficiency of graphitization and the product quality.

[0022] The following further describes the detailed structure of the utility model in conjunction with the drawings and specific embodiments. Description of the Drawings

[0023] Figure 1 - is the structural schematic diagram of the utility model;

[0024] 1 - air inlet, 2 - cooling chamber, 3 - thermocouple temperature measuring device, 4 - crucible, 5 - heat insulation layer, 6 - induction coil, 7 - graphitization chamber, 8 - feed inlet, 9 - filter collector, 10 - water ring vacuum pump, 11 - solenoid valve, 12 - vacuum pump, 13 - material transition chamber, 14 - discharge valve, 15 - air outlet, 16 - vacuum ball valve. Specific Embodiments

[0025] As shown in the attached drawings: A continuous graphitization processing device includes a material transition chamber 13, a graphitization chamber 7, and a cooling chamber 2, all of which are provided with evacuation tubes. The evacuation tubes are connected to a vacuum pump 12, and solenoid valves 11 are provided on the evacuation tubes. The material transition chamber 13 and the cooling chamber 2 are respectively arranged at the upper and lower ends of the graphitization chamber 7 through high-temperature valves. Vacuum ball valves 16 are provided at the upper end of the material transition chamber 13 and the lower end of the cooling chamber 2. Preferably, air inlets 1 are provided at the lower ends of the material transition chamber 13, the graphitization chamber 7, and the cooling chamber 2, and air outlets 15 are provided at the upper ends, for circulating protective gas to protect the material. The protective gas is argon or nitrogen; both the cooling chamber 2 and the material transition chamber 13 are double-layer jacket structures. In this embodiment, the material is carbon powder, and a feed inlet 8 is provided at the top of the material transition chamber 13; a circulating heat exchange system is provided between the cooling chamber 2 and the material transition chamber 13.

[0026] In the embodiment, the circulating heat exchange system includes an inlet heat pipe, a first heat exchange pipe, a second heat exchange pipe, and a heat exchange pump. The first heat exchange pipe and the second heat exchange pipe are respectively arranged in the interlayers of the cooling chamber 2 and the material transition chamber 13. The upper and lower ends of the inlet heat pipe are respectively connected to the second heat exchange pipe and the first heat exchange pipe. The heat exchange pump is arranged on the inlet heat pipe, and a return pipe is also provided between the second heat exchange pipe and the first heat exchange pipe. Preferably, a circulating medium is provided in the circulating heat exchange system, and the medium is a circulating liquid such as water, molten salt, or oil that can achieve heat exchange. In this embodiment, molten salt is used as the circulating liquid to improve the efficiency and effect of heat exchange. More preferably, the circulating liquid in the first heat exchange pipe enters from the top and exits from the bottom, and the circulating liquid in the second heat exchange pipe enters from the bottom and exits from the top. Preferably, both the first heat exchange pipe and the second heat exchange pipe adopt the method of entering from the bottom and exiting from the top to facilitate the efficiency of heat exchange. The graphitized powder after being cooled by the cooling chamber 2 is output from the continuous discharge valve 14.

[0027] In the embodiment, a graphitization device is provided in the graphitization chamber 7. The graphitization device includes a high-purity graphite crucible 4, a heat insulation layer 5, and an induction coil 6. The induction coil 6 is arranged on the periphery of the crucible 4, and a heat insulation layer 5 is provided between the induction coil 6 and the crucible 4. The graphitization chamber 7 adopts a sandwich structure, and cooling water circulates in the interlayer. Insulation protective layers are provided on both the inner and outer sides of the induction coil 6; the crucible 4 is in a circular tube shape, with a diameter of 10 - 100 cm. Preferably, the diameter of the crucible 4 is 20 - 90 cm, and the length is 100 - 400 cm. More preferably, the diameter of the crucible 4 is 40 cm, and the length is 200 cm to ensure the graphitization effect of the material. Optimally, in this embodiment, the diameter of the crucible 4 is 80 cm, and the length is 300 cm; due to the continuous feeding and discharging production method, the material is always in motion. When the crucible 4 adopts the dimensions within this range, it is not easy to agglomerate during heat treatment. In addition, a pressure gauge is installed on the graphitization chamber 7 to display the pressure inside the furnace, which is intuitive and reliable; at the same time, a safety valve is configured, and when the pressure inside the furnace is overpressure, it automatically relieves pressure to ensure the safety of the equipment.

[0028] Preferably, to ensure the vacuum effect of the graphitization chamber and reduce impurity gases, a water-ring vacuum pump 10 is provided on the atomization chamber. The water-ring vacuum pump 10 is connected to the upper, middle, and lower position points of the graphitization chamber through pipelines, facilitating the improvement of the air extraction effect. A filter collector 9 is provided on the pipeline to reduce the influence of dust impurities in the air on the service life of the water-ring vacuum pump 10. The system first pumps the vacuum degree to an extreme level below 1 Pa, and then uses a high-performance water-ring vacuum pump 10 for continuous air extraction operations, which not only effectively reduces the oxygen atmosphere but also quickly discharges impurity-containing gases. With the dual guarantees, the stability of the system and the purity of the product are significantly improved.

[0029] The present utility model further includes a PLC controller, and the system is controlled in real time and the temperature, vacuum degree, and equipment operation status are displayed and controlled through the touch screen graphic display operation terminal on the controller. A temperature measuring device is provided on the graphitization chamber 7. The temperature measuring device includes an infrared measuring device for measuring inside the graphite crucible 4 and a thermocouple temperature measuring device 3 for measuring part of the induction coil 6. The measured temperature is sampled by the PLC and stored in a removable disk regularly. The temperature control uses a thyristor inverter system to control the output to control the heating power, and the temperature control instrument sets the temperature control temperature, and the temperature control instrument performs PID closed-loop control according to the set temperature.

[0030] The present utility model transports a large amount of heat released in the cooling chamber 2 to the material transition chamber 13 through a circulating heat exchange system for heat exchange. The exchanged heat is used to preheat the materials in the material transition chamber 13. The medium in the circulating heat exchange system exchanges heat in the second heat exchange tube and then returns to the first heat exchange tube through a return pipe to absorb heat again. In the above process, the recycling of heat is realized, reducing the production cost of graphitization. At the same time, the materials are preheated in advance, making the materials heat more evenly, improving the efficiency of graphitization and the quality of the product.

[0031] The above is the preferred embodiment of the present utility model and the technical principles applied. For those skilled in the art, any obvious changes such as equivalent transformation and simple replacement based on the technical solution of the present utility model without departing from the spirit and scope of the present utility model shall fall within the protection scope of the present utility model.

Claims

1. A continuous graphitization treatment device, comprising a material transition chamber, a graphitization chamber, and a cooling chamber, all of which are provided with evacuation tubes. The material transition chamber and the cooling chamber are respectively arranged at the upper end and the lower end of the graphitization chamber through high-temperature valves. Vacuum ball valves are provided at the upper end of the material transition chamber and the lower end of the cooling chamber. It is characterized in that: A circulating heat exchange system is provided between the cooling chamber and the material transition chamber.

2. The continuous graphitization treatment equipment according to claim 1, characterized in that: A graphitization device is provided in the graphitization chamber. The graphitization device includes a high-purity graphite crucible, a heat-insulating layer, and an induction coil. The induction coil is arranged on the periphery of the crucible, and a heat-insulating layer is provided between the induction coil and the crucible. The graphitization chamber adopts a sandwich structure, and cooling water circulates in the sandwich.

3. The continuous graphitization treatment equipment according to claim 2, wherein: Insulating protective layers are provided on both the inner and outer sides of the induction coil.

4. The continuous graphitization treatment equipment according to claim 2, characterized in that: The crucible is in a circular tube shape with a diameter of 10 - 100 cm.

5. The continuous graphitization treatment equipment according to claim 1, characterized in that: Both the cooling chamber and the material transition chamber are of a double-layer jacket structure.

6. The continuous graphitization treatment equipment according to claim 1, characterized in that: The circulating heat exchange system includes an inlet heat pipe, a first heat exchange pipe, a second heat exchange pipe, and a heat exchange pump. The first heat exchange pipe and the second heat exchange pipe are respectively arranged in the jackets of the cooling chamber and the material transition chamber. The upper and lower ends of the inlet heat pipe are respectively connected to the second heat exchange pipe and the first heat exchange pipe. The heat exchange pump is arranged on the inlet heat pipe, and a return pipe is also provided between the second heat exchange pipe and the first heat exchange pipe.

7. The continuous graphitization treatment equipment according to claim 6, characterized in that: The circulating liquid in the first heat exchange pipe enters from the bottom and exits from the top, and the circulating liquid in the second heat exchange pipe enters from the top and exits from the bottom.

8. The continuous graphitization treatment equipment according to claim 1, characterized in that: Air inlets are provided at the lower ends of the material transition chamber, the graphitization chamber, and the cooling chamber, and air outlets are provided at the upper ends for the circulation of protective gas.

9. The continuous graphitization treatment equipment according to claim 1, characterized in that: A temperature measuring device is provided on the graphitization chamber. The temperature measuring device includes an infrared measuring device for measuring inside the graphite crucible and a thermocouple temperature measuring device for measuring the induction coil part. The measured temperature is sampled by a PLC and stored in a removable disk regularly. The temperature control uses a thyristor inverter system to control the output to control the heating power. The temperature control value is set by a temperature controller, and the temperature controller performs PID closed-loop control according to the set temperature.

10. The continuous graphitization treatment equipment according to any one of claims 1-9, characterized in that: It also includes a PLC controller. The system is controlled and displayed in real time through the touch screen graphic display operation terminal on the controller for temperature, vacuum degree, and equipment operation status control operations.

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