CN116678217A - Graphitization process and equipment for lithium battery cathode material - Google Patents
Graphitization process and equipment for lithium battery cathode material Download PDFInfo
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- CN116678217A CN116678217A CN202310969524.0A CN202310969524A CN116678217A CN 116678217 A CN116678217 A CN 116678217A CN 202310969524 A CN202310969524 A CN 202310969524A CN 116678217 A CN116678217 A CN 116678217A
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- furnace
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- furnace body
- lithium battery
- negative electrode
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 72
- 238000005087 graphitization Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 27
- 230000008569 process Effects 0.000 title claims abstract description 26
- 239000010406 cathode material Substances 0.000 title claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 85
- 239000007773 negative electrode material Substances 0.000 claims abstract description 44
- 238000007789 sealing Methods 0.000 claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000007599 discharging Methods 0.000 claims abstract description 13
- 238000004321 preservation Methods 0.000 claims abstract description 11
- 238000012545 processing Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 44
- 238000009413 insulation Methods 0.000 claims description 36
- 239000010405 anode material Substances 0.000 claims description 29
- 239000011261 inert gas Substances 0.000 claims description 18
- 238000011084 recovery Methods 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 230000000903 blocking effect Effects 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 244000309464 bull Species 0.000 description 14
- 238000001816 cooling Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 10
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009529 body temperature measurement Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012615 aggregate Substances 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D1/00—Casings; Linings; Walls; Roofs
- F27D1/18—Door frames; Doors, lids, removable covers
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D17/00—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases
- F27D17/008—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases cleaning gases
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D19/00—Arrangements of controlling devices
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D19/00—Arrangements of controlling devices
- F27D2019/0028—Regulation
- F27D2019/0034—Regulation through control of a heating quantity such as fuel, oxidant or intensity of current
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The application provides a graphitization process and equipment for a lithium battery cathode material, and particularly relates to the technical field of material graphitization. The lithium battery negative electrode material graphitizing equipment comprises a graphitizing furnace, an electric control console and a gas control device, wherein the graphitizing furnace comprises a furnace cover for sealing the graphitizing furnace, a furnace body part for storing negative electrode materials in the graphitizing process and a furnace bottom part for discharging the lithium battery negative electrode materials after processing is completed, the furnace cover is arranged on the furnace body part in a sliding manner, the furnace cover is used for feeding materials into the furnace body part when opened and sealing the furnace body part when closed, the furnace body part comprises a furnace body part shell and a furnace body part heat preservation layer, and a heating device is arranged in the furnace body part heat preservation layer and is used for heating the furnace interior to graphitize the materials. The process and the equipment provided by the application greatly shorten the production period, improve the production efficiency, greatly improve the energy utilization rate and reduce the energy loss.
Description
Technical Field
The application relates to the technical field of material graphitization, in particular to a graphitization process and equipment for a lithium battery anode material.
Background
The energy storage battery is beneficial to the high-speed growth of the new energy industry, and the power electrode and the energy storage battery of the new energy automobile are in an coming continuous high-grade scenic development period. The 22-year artificial graphite anode material has the advantages of high entrusted processing price, new history, capacity gap and wide market prospect of global dynamism, attracts a great deal of capital investment in the lithium battery industry and the corresponding matched anode material industry, reports graphitization capacity exceeding 1000 weight percent, and has market demand blowout. Most of the current graphitization devices still use a conventional graphitization furnace, which has the following problems: the production period of each process flow link is too long, the natural cooling time is only fifteen days, and the feeding and discharging of the material consume a great deal of manpower and material resources, so that the production efficiency is low; in addition, the smoke and waste gas of the traditional graphitizing furnace are discharged in an unorganized way, so that the working environment of workers is very bad, and the requirements and policies of energy conservation and emission reduction advocated by the nation are not met; and the traditional graphitization furnace has the problems that the operation temperature is difficult to reach the temperature standard required by graphitization of the anode material of the lithium battery, the temperature rising effect of each position is inconsistent easily, the consistency and purity of graphitization are difficult to ensure, and meanwhile, the heat loss is large and the energy utilization rate is low in the process.
Disclosure of Invention
In order to solve the technical problems, the application provides a graphitization process and equipment for a lithium battery cathode material.
The technical scheme of the application is realized as follows:
the utility model provides a lithium cell negative pole material graphitization equipment, includes graphitization stove, electric control cabinet and gas control device, graphitization stove includes, is used for sealing the furnace lid of graphitization stove, is used for depositing the furnace body part of negative pole material and is used for discharging the stove bottom part of the lithium cell negative pole material that processing accomplished in the graphitization process, wherein:
the furnace cover is arranged on the furnace body part in a sliding manner, the furnace cover is used for feeding materials into the furnace body part when being opened and is used for sealing the furnace body part when being closed, the furnace body part comprises a furnace body part shell and a furnace body part heat preservation layer, the furnace body part shell is arranged in a hollow manner, the furnace body part heat preservation layer is arranged in a hollow manner and is arranged in a furnace body part shell cavity, a heating device which is arranged in the hollow manner is arranged in the furnace body part heat preservation layer cavity, the heating device is arranged in a hollow manner and is used for heating the furnace interior to graphitize materials, a gas conveying head penetrating through the furnace body part, the heat preservation layer and the heating device is fixedly arranged on the furnace body part and is used for exchanging gas in the furnace interior and the gas control device, a temperature measuring port is formed in the furnace body part and is positioned below the gas conveying head, and the furnace bottom part is fixedly arranged at the bottom of the furnace body part and is used for discharging when being opened and is used for sealing the furnace body part when being closed.
Further, the electric control table is connected with a temperature measuring port, the temperature measuring port is used for feeding back the temperature in the furnace to the control table, the control table is connected with a heating device, the other end, far away from the furnace body, of the heating device is connected with a direct current power supply, and the direct current power supply is used for supplying power to the heating device to heat the heating device.
Further, one end of the temperature measuring port, which is close to the heating device, is fixedly provided with an infrared temperature measuring head for measuring the temperature in the furnace, the infrared temperature measuring head penetrates through the furnace body part, the heat insulation layer and the heating device, and one end of the temperature measuring port, which is far away from the heating device, is connected with an electric control console for feeding back the temperature in the furnace to the control console.
Further, be provided with the bull stick of vertical placing in heating device's the cavity, the top of bull stick rotates the top that sets up at furnace body part, the symmetry is provided with a plurality of crossbars on the bull stick for stirring lithium cell negative pole material when the bull stick rotates, the top fixed mounting of bull stick has first bevel gear, first bevel gear meshing is connected with second bevel gear, the one end fixed setting that first bevel gear was kept away from to the second bevel gear is on the motor, the motor is connected with the electric control cabinet for control the rotatory start-up and the stop of bull stick.
Further, the outside of the furnace body part is provided with a gas conveying pipe connected with a gas conveying head, the other end of the gas conveying pipe, which is far away from the graphitizing furnace, is provided with a first pipeline, a second pipeline, a third pipeline and a fourth pipeline, and the positions, which are respectively close to the conveying pipes, of the gas conveying pipe are correspondingly provided with a first valve, a second valve, a third valve and a fourth valve which can work independently, the first valve, the second valve, the third valve and the fourth valve are respectively used for controlling the opening and closing of the corresponding pipelines, one end of the first pipeline is connected with the gas conveying pipe, the other end of the first pipeline is connected with a volatile matter recovery device, the volatile matter recovery device is used for recovering volatile matter generated during heating, one end of the second pipeline is connected with the gas conveying pipe, the other end of the second pipeline is connected with a vacuum machine and is used for vacuumizing the sealing furnace body part during heating, one end of the third pipeline is connected with the gas conveying pipe, the other end of the inert gas output device is used for conveying inert protective gas into the sealing furnace body part after vacuumizing, one end of the fourth pipeline is connected with the gas conveying pipe, the other end of the inert gas output device is connected with a cold air output device, the other end of the inert gas output device is used for sealing the lithium battery, and the negative electrode is used for cooling the valve in the sealing the furnace part after the cooling down, and the valve is opened fast enough to cool the anode material is guaranteed, and the rest of the valve is used for cooling the anode material is fast and stable when the valve is closed.
Further, the outside fixed mounting of furnace body part has the connecting plate, be fixed with the hydraulic stem on the connecting plate, the other end and the bell fixed connection of connecting plate are kept away from to the hydraulic stem, and when the hydraulic stem stretched out, the bell rose, and when the hydraulic stem contracted, the bell descended, the hydraulic stem was used for opening and closing of bell, form charging channel between bell and the furnace body part when the bell was opened for add lithium cell negative pole material to the furnace body part.
Further, a first connecting ring is fixedly arranged at the bottom of the furnace cover, a second connecting ring fixedly arranged at the top of the furnace body part is arranged at the bottom of the first connecting ring, a plurality of sealing rings which are concentric with the connecting ring and have different diameters are fixedly arranged at the bottom of the first connecting ring, and a sealing groove corresponding to the sealing ring is formed at the top of the second connecting ring and used for sealing the furnace body part when the sealing ring is inserted into the sealing groove.
Further, the inside of first go-between is fixed and is provided with the heat insulating board, the heat insulating board is used for carrying out heat insulation to the bell when furnace body part intensifies, the bottom of furnace body part is provided with the conical surface board of fixed connection in the cavity setting of heating device bottom, the conical surface board is used for making things convenient for the material to discharge, the bottom opening of conical surface board sets up, and its bottom is provided with the insulation board that fixed mounting is located furnace bottom part top on the furnace body part shell, furnace bottom part slip is provided with the sealing bottom plate that runs through insulation board and top and conical surface board bottom parallel and level for sealed furnace body part.
Further, the heat insulation connecting piece fixed at the end part of the rotating rod is arranged at the circle center position of the heat insulation plate and used for blocking conduction of the upper temperature inside the furnace body part, and the connecting piece penetrates through the heat insulation plate and is rotatably arranged on the heat insulation plate.
The application provides a graphitization process of a lithium battery anode material from another aspect, which adopts the graphitization equipment of the lithium battery anode material, and comprises the following steps:
opening a furnace cover, and adding a lithium battery anode material to be graphitized;
closing a furnace cover, heating a heating device through an electric control console, preheating a lithium battery negative electrode material to be graphitized, simultaneously rotating a rotating rod through the electric control console, stirring the negative electrode material, simultaneously opening a first valve, opening a volatile recovery device, and recovering volatile generated in the furnace;
heating the heating device to the temperature required by graphitizing the anode material through the electric control console, stopping rotating the rotating rod through the electric control console when the temperature reaches the required temperature, closing the first valve, opening the second valve, opening the vacuum machine, closing the second valve after evacuating the gas in the furnace, opening the third valve, opening the inert gas output device, and introducing protective inert gas into the furnace;
step four, observing the temperature in the furnace through an infrared temperature measuring head, controlling the temperature of a heating device through a control console so as to control the temperature in the furnace, intermittently rotating and stopping the rotating rod through the control console, and fully heating the cathode material;
step five, after the graphitization process is finished, closing the heating device, opening the fourth valve, opening the cold air output device, introducing cold air into the furnace, and simultaneously rotating the rotating rod through the electric control console so as to quickly cool the graphitized lithium battery cathode material;
and step six, opening the bottom part of the furnace, and discharging the cooled graphitized lithium battery anode material.
The application has the following beneficial effects:
1. the application achieves three effects in three stages through the rotatable design of the rotating rod: the method has the advantages that volatile matters generated by the lithium battery negative electrode material to be graphitized are fully discharged in the preheating stage, the graphitized purity is improved, the lithium battery negative electrode material to be graphitized is heated more fully in the heating stage, the phenomenon that graphitized effects are inconsistent due to different temperatures at different positions is avoided, the graphitized purity is ensured, the graphitized lithium battery negative electrode material is cooled to the required temperature more quickly in the cooling stage, and the time required in the cooling stage is saved.
The application overcomes the defects of the traditional graphitization furnace, effectively recovers the volatile matters generated in the preheating process, namely the waste gas, greatly reduces the pollution of workshops and optimizes the artificial working environment.
The application solves the problems of discontinuous graphitization process, long production period and low production efficiency in the prior art, greatly shortens the production period, improves the production efficiency, and simultaneously greatly improves the energy utilization rate and reduces the energy loss through the cooperation of all the components.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the related art, the drawings that are required to be used in the embodiments or the related technical descriptions will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained according to the drawings without inventive effort to those skilled in the art.
FIG. 1 is a side view of a lithium battery negative electrode material graphitization apparatus of the present application;
FIG. 2 is an enlarged view of the lithium battery negative electrode material graphitizing apparatus of the present application at B in FIG. 1;
FIG. 3 is an enlarged view of the lithium battery negative electrode material graphitizing apparatus of the present application at A in FIG. 1;
FIG. 4 is a top view of the lithium battery negative electrode material graphitizing apparatus of the present application;
FIG. 5 is an enlarged view of the lithium battery negative electrode material graphitization apparatus of the present application at C in FIG. 4;
FIG. 6 is an enlarged view of the lithium battery negative electrode material graphitizing apparatus of the present application at D in FIG. 5;
FIG. 7 is a view showing a state in which a furnace cover of the graphitizing apparatus for a negative electrode material of a lithium battery of the present application is opened;
FIG. 8 is a bottom view of the bottom of the lithium battery negative electrode material graphitization apparatus of the present application;
FIG. 9 is a cross-sectional view of a graphitizing furnace of the graphitizing apparatus for negative electrode material of lithium battery of the present application;
FIG. 10 is a split view of the interior of a graphitizing furnace of the graphitizing apparatus for lithium battery negative electrode material according to the present application;
FIG. 11 is a schematic view of a first connecting ring and a second connecting ring of the lithium battery negative electrode material graphitizing apparatus of the present application;
fig. 12 is a split view of the graphitizing apparatus for the negative electrode material of the lithium battery according to the present application.
Reference numerals in the drawings: 1. 1.1 parts of graphitization furnace, 1.2 parts of furnace body, 1.2.1 parts of shell, 1.2.2 heat insulation layers, 1.2.3 parts of heating device, 1.2.4 parts of direct current power supply, 1.3 parts of furnace bottom, 1.4 parts of connecting plate, 1.5 parts of hydraulic rod, 2 parts of electric control table, 3 parts of gas control device, 4 parts of gas delivery head, 5 parts of temperature measuring port, 5.1 parts of infrared temperature measuring head, 6 parts of rotating rod, 6.1 parts of cross rod, 6.2 parts of first bevel gear, 6.3 parts of second bevel gear, 6.4 parts of motor, 7.1 parts of first pipeline, 7.1.1 parts of first valve, 7.1.2, volatile recovery unit, 7.2, second pipeline, 7.2.1, second valve, 7.2.2, vacuum machine, 7.3, third pipeline, 7.3.1, third valve, 7.3.2, inert gas output unit, 7.4, fourth pipeline, 7.4.1, fourth valve, 7.4.2, cold air output unit, 8, charging channel, 9, first go-between, 9.1, sealing washer, 10, second go-between, 10.1, seal groove, 11, heat insulating board, 12, conical surface board, 13, insulation board, 14, sealing bottom plate, 15, heat insulating connector.
Detailed Description
The following description of the technical solutions in the embodiments of the present application will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
In the embodiment of the application, the words "first", "second", etc. are used to distinguish identical items or similar items having substantially the same function and action, and the sequence thereof is not limited. It will be appreciated by those of skill in the art that the words "first," "second," and the like do not limit the amount and order of execution, and that the words "first," "second," and the like do not necessarily differ.
Referring to fig. 1 to 12, a graphitizing device for a negative electrode material of a lithium battery provided by an embodiment of the present application includes a graphitizing furnace 1, an electric control console 2 and a gas control device 3, wherein the graphitizing furnace 1 includes a furnace cover 1.1 for sealing the graphitizing furnace 1, a furnace body portion 1.2 for storing the negative electrode material during graphitizing, and a furnace bottom portion 1.3 for discharging the processed negative electrode material of the lithium battery, wherein:
the furnace cover 1.1 is arranged on the furnace body part 1.2 in a sliding manner, the furnace cover 1.1 is used for charging materials into the furnace body part 1.2 when being opened, the furnace body part 1.2 is used for sealing the furnace body part 1.2 when being closed, the furnace body part 1.2 comprises a shell 1.2.1 and a heat insulation layer 1.2.2, the shell 1.2.1 is arranged in a hollow manner, the heat insulation layer 1.2.2 is arranged in a cavity of the shell 1.2.1, a heating device 1.2.3 is arranged in the cavity of the heat insulation layer 1.2.2 in a hollow manner, the heating device 1.2.3 is used for heating the furnace temperature to graphitize materials, a gas conveying head 4 penetrating through the furnace body part 1.2, the heat insulation layer 1.2.2 and the heating device 1.2.3 is fixedly arranged on the furnace body part 1.2, a temperature measuring port 5 is arranged on the furnace body part 1.2 and used for measuring the temperature in the furnace, the temperature measuring port 5 is arranged below the gas conveying head 4, and the furnace bottom part 1.3 is fixedly arranged at the bottom of the furnace body part 1.2 and used for discharging materials when the furnace body part 1.2 is opened and is used for sealing the furnace body part. The heat preservation layer 1.2.2 is arranged firstly to ensure the temperature maintenance during heating in the furnace and ensure the graphitization purity of the cathode material, and secondly to isolate the high-temperature environment from the shell 1.2.1 so as to ensure the safety of the operation process.
Wherein, electric control cabinet 2 and temperature measurement mouth 5 pass through fixed connection, temperature measurement mouth 5 is used for feeding back the temperature in the stove to the control cabinet, the control cabinet is connected with heating device 1.2.3, the other end that heating device 1.2.3 kept away from furnace body part 1.2 is connected with DC power supply 1.2.4, DC power supply 1.2.4 is used for giving heating device 1.2.3 power transmission and makes its intensification, can control heating device 1.2.3's temperature through the size of adjusting DC power supply 1.2.4 electric current, the higher the electric current is, heating device 1.2.3 temperature is higher, the electric current is smaller, heating device 1.2.3 temperature is lower. The temperature measuring port 5 is near one end of the heating device 1.2.3 and is fixedly provided with an infrared temperature measuring head 5.1 for measuring the temperature in the furnace, the infrared temperature measuring head 5.1 penetrates through the furnace body part 1.2, the heat insulation layer 1.2.2 and the heating device 1.2.3, one end of the temperature measuring port 5 far away from the heating device 1.2.3 is connected with the electric control table 2 and is used for feeding back the temperature in the furnace to the electric control table 2, namely, the temperature of the direct current power supply 1.2.4 to the heating device 1.2.3 is controlled at the electric control table 2 through the feedback of the temperature of the infrared temperature measuring head 5.1 received by the electric control table 2, and then the temperature in the furnace is controlled.
In addition, be provided with the bull stick 6 of vertical placing in the cavity of heating device 1.2.3, the top rotation setting of bull stick 6 is at the top of furnace body part 1.2, the symmetry is provided with a plurality of horizontal poles 6.1 on the bull stick 6, be used for stirring lithium cell negative pole material when bull stick 6 rotates, the top fixed mounting of bull stick 6 has first bevel gear 6.2, first bevel gear 6.2 meshing is connected with second bevel gear 6.3, the one end that first bevel gear 6.2 was kept away from to second bevel gear 6.3 is fixed to be set up on motor 6.4, motor 6.4 is connected with electric control cabinet 2, be used for controlling the rotatory start-up and the stop of bull stick 6, horizontal pole 6.1 on bull stick 6 and the bull stick 6 is made by materials such as graphite, clay and aggregate, its fusing point is higher than the required fusing point of graphitization in this technology. The periphery at the top end of the rotating rod 6 is fixedly provided with a heat insulation connecting piece 15, and the heat insulation connecting piece 15 is rotationally arranged at the center of the heat insulation plate 11, so that when the rotating rod 6 rotates, the heat insulation connecting piece 15 rotates but does not drive the heat insulation plate 11 to rotate.
Secondly, a gas conveying pipe 7 connected with the gas conveying head 4 is arranged outside the furnace body part 1.2, a first pipeline 7.1, a second pipeline 7.2, a third pipeline 7.3 and a fourth pipeline 7.4 are arranged at the other end of the gas conveying pipe 7 far away from the graphitization furnace 1, and a first valve 7.1.1, a second valve 7.2.1, a third valve 7.3.1 and a fourth valve 7.4.1 which can independently work are correspondingly arranged at positions close to the conveying pipes respectively, are respectively used for controlling the opening and closing of the corresponding pipelines, one end of the first pipeline 7.1 is connected with the gas conveying pipe 7, the other end is connected with a volatile recovery device 7.1.2, when the volatile components are largely escaped, the volatile components are insufficiently combusted, a great amount of black smoke is produced, environmental pollution or environmental protection accidents are easily caused, one end of the second pipeline 7.2 is connected with the gas conveying pipe 7, the other end is connected with the vacuum machine and used for vacuumizing the sealed furnace body part 1.2 during heating, graphitization purity is guaranteed, one end of the third pipeline 7.3 is connected with the gas conveying pipe 7, the other end is connected with the inert gas output device 7.3.2, the inert gas output device 7.3.2 is used for conveying inert protective gas into the sealed furnace body part 1.2 after vacuumizing, one end of the fourth pipeline 7.4 is connected with the gas conveying pipe 7, the other end is connected with the cold air output device 7.4.2, the cold air output device 7.4.2 is used for conveying cold air into the sealed furnace body part 1.2 after graphitization is completed so that lithium battery cathode materials are cooled rapidly, and when one valve is opened, other valves are all closed and used for guaranteeing stability of gas in the furnace.
Specifically, the first valve 7.1.1 is used for opening or closing the volatile recovery device 7.1.2 connected with the first pipeline 7.1 and is used for timely collecting volatile matters generated in the preheating process, the second valve 7.2.1 is used for opening or closing a vacuum machine connected with the second pipeline 7.2 and is used for evacuating air in the closed furnace body part 1.2 during heating, the third valve 7.3.1 is used for opening or closing the inert gas output device 7.3.2 connected with the third pipeline 7.3 and is used for conveying inert protective gas into the sealed furnace body part 1.2 after evacuating, the fourth valve 7.4.1 is used for opening or closing the cold air output device 7.4.2 connected with the fourth pipeline 7.4 and is used for conveying cold air into the sealed furnace body part 1.2 after graphitization is completed so as to enable negative electrode materials of the lithium battery to be cooled rapidly. The device controls the gas environment required in the whole graphitization process so as to ensure the graphitization effect.
In addition, connecting plate 1.4 is fixedly arranged on the outer side of furnace body part 1.2, hydraulic rod 1.5 is fixed on connecting plate 1.4, the other end of hydraulic rod 1.5 away from connecting plate 1.4 is fixedly connected with furnace cover 1.1, when hydraulic rod 1.5 stretches out, furnace cover 1.1 rises, when hydraulic rod 1.5 contracts, furnace cover 1.1 descends, hydraulic rod 1.5 is used for opening and closing furnace cover 1.1, a charging channel 8 is formed between furnace cover 1.1 and furnace body part 1.2 when furnace cover 1.1 is opened, lithium battery cathode material is added into furnace body part 1.2, the optimal stretching length of hydraulic rod 1.5 is the height of charging channel 8 which is most convenient to feed, and the optimal shrinking length is the distance of sealing ring 9.1 for clamping sealing groove 10.1 exactly.
Secondly, the bottom of bell 1.1 is fixed and is provided with first go-between 9, and the bottom of first go-between 9 is provided with the second go-between 10 at furnace body part 1.2 top of fixed mounting, and the bottom of first go-between 9 is fixed mounting has a plurality of sealing washer 9.1 that are different with go-between concentric diameter, and sealing groove 10.1 corresponding with sealing washer 9.1 has been seted up at the top of second go-between 10 for sealing washer 9.1 seals furnace body part 1.2 when inserting sealing groove 10.1, in order to guarantee that whole heating process furnace body all is in sealing state.
And a heat insulation plate 11 is fixedly arranged in the first connecting ring 9, the heat insulation plate 11 is used for insulating the furnace cover 1.1 when the furnace body part 1.2 is heated, a hollow conical surface plate 12 fixedly connected to the bottom of the heating device 1.2.3 is arranged at the bottom of the furnace body part 1.2, the conical surface plate 12 is used for facilitating material discharge, an insulating plate 13 fixedly arranged on the shell 1.2.1 of the furnace body part 1.2 and positioned at the top of the furnace bottom part 1.3 is arranged at the bottom of the conical surface plate 12, a sealing bottom plate 14 penetrating through the insulating plate 13 and with the top being flush with the bottom of the conical surface plate 12 is slidably arranged at the furnace bottom part 1.3, the sealing bottom plate 14 is fixed with the furnace bottom part 1.3 through a screw, and when discharging, the screw is unscrewed, the sealing bottom plate 14 is opened, and a container capable of aligning with a notch at the bottom of the conical surface plate 12 is used for receiving materials.
Furthermore, the heat insulation plate 11 at the position of the furnace cover 1.1 is provided with a heat insulation connecting piece 15 fixed at the end part of the rotating rod 6 at the center position, the heat insulation connecting piece 15 is used for blocking the conduction of the temperature in the furnace body part 1.2 upwards, and the heat insulation connecting piece 15 penetrates through the heat insulation plate 11 and is rotatably arranged on the heat insulation plate 11, so that the heat insulation plate 11 is not influenced when the rotating rod 6 rotates. While the motor 6.4 is also placed on the top surface of the heat shield 11.
Specifically, the application provides a lithium battery anode material graphitization process, which applies the lithium battery anode material graphitization equipment, and the process comprises the following steps:
step one, opening a furnace cover 1.1, and adding a lithium battery anode material to be graphitized;
step two, closing a furnace cover 1.1, heating a heating device 1.2.3 through an electric control table 2, preheating a lithium battery anode material to be graphitized, simultaneously rotating a rotating rod 6 through the electric control table 2, stirring the anode material, simultaneously opening a first valve 7.1.1, opening a volatile recovery device 7.1.2, and recovering volatile generated in the furnace;
step three, heating the heating device 1.2.3 to the temperature required by graphitizing the anode material through the electric control table 2, stopping rotating the rotating rod 6 through the electric control table 2 when the temperature reaches the required temperature, closing the first valve 7.1.1, opening the second valve 7.2.1, opening the vacuum machine, closing the second valve 7.2.1 after evacuating the gas in the furnace, opening the third valve 7.3.1, opening the inert gas output device 7.3.2, and introducing protective inert gas into the furnace;
step four, observing the temperature in the furnace through an infrared temperature measuring head 5.1, controlling the temperature of a heating device 1.2.3 through a control console so as to control the temperature in the furnace, intermittently rotating and stopping a rotating rod 6 through the control console 2, and fully heating a cathode material;
step five, after the graphitization process is finished, closing the heating device 1.2.3, opening the fourth valve 7.4.1, opening the cold air output device 7.4.2, introducing cold air into the furnace, and simultaneously enabling the rotating rod 6 to rotate through the electric control console 2 so as to enable the graphitized lithium battery cathode material to be rapidly cooled;
and step six, opening the bottom part 1.3, and discharging the cooled graphitized lithium battery anode material.
It should be noted that the application has three effects respectively in three stages of graphitization through the rotatable design of the rotating rod 6, and the rotation of the rotating rod is controlled in the first stage and the preheating stage, so that the volatile matters generated by the negative electrode material of the lithium battery to be graphitized can escape sufficiently, and environmental pollution or environmental protection accidents caused by the volatile matters are avoided; secondly, the rotation of the heating device is controlled in the heating stage, so that the negative electrode material of the lithium battery to be graphitized is heated more fully, the phenomenon of inconsistent graphitization effect caused by uneven temperature distribution of the heating device 1.2.3 or different placement positions of the negative electrode material is avoided, the negative electrode material is ensured to be heated fully, and the graphitization purity is ensured; thirdly, the rotation of the lithium battery cathode material is controlled in the cooling stage, so that the graphitized lithium battery cathode material is in full contact with the introduced cooling air for cooling, the temperature is cooled to the required discharging temperature more quickly, and the time required in the cooling stage is saved. The rotating speed of the rotating rod 6 is not too high, and the rotating rod is reasonably arranged to rotate once every ten seconds.
In the process of using the device, according to the temperature in the furnace fed back by the infrared temperature measuring head 5.1, the electric current passing through the heating device 1.2.3 is controlled by the electric control console 2, and the higher the temperature is, the lower the electric current is, and the lower the temperature is, the higher the electric current passing through the heating device 1.2.3 is. The temperature of the heating device 1.2.3 is controlled, so that the heating temperature in the furnace is controlled, wherein the temperature in the furnace is controlled to be about 200-1000 ℃ to be optimal in the preheating stage, and a large amount of volatile matters in the lithium battery anode material to be graphitized are discharged in the temperature range, and the volatile matters in the lithium battery anode material can be fully escaped by matching with the rotation of the rotating rod 6. In addition, in the heating process, the temperature in the furnace is controlled within the range of 2300-3000 ℃ according to specific production requirements, the graphitization effect of the anode material is optimal within the range, and the phenomenon of uneven heating possibly occurs due to the different positions of the heating device 1.2.3 and the anode material, so that the graphitization effect of the whole furnace anode is affected, and the anode material can be fully heated by matching with the rotation of the rotating rod 6, so that the graphitization quality is ensured. And in the discharging process, the negative electrode material is cooled to about 150 ℃ to be discharged from the furnace optimally, and is taken out too early, so that the negative electrode material is oxidized due to the too high temperature, and the specific surface area is increased. Too late extraction can oxidize the cathode powder material, the production period is prolonged, and the cost is increased. In the cooling process, the rotating rod 6 rotates to enable the graphitized negative electrode material to be in more full contact with the introduced cold air, so that the cooling effect can be rapidly achieved. That is, the rotating rod 6 should rotate in the preheating, heating and cooling stages, and different effects are achieved, and the quality and efficiency of graphitization are greatly improved by the three effects.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the application.
Claims (10)
1. A lithium battery negative electrode material graphitization apparatus, comprising:
graphitization stove (1), electric control cabinet (2) and gas control device (3), graphitization stove (1) is including being used for sealing bell (1.1) of graphitization stove (1), be used for depositing furnace body part (1.2) of negative pole material and be used for discharging the stove bottom part (1.3) of the lithium cell negative pole material that processing accomplished in graphitization process, wherein:
the furnace cover (1.1) slides and sets up the outer wall surface at furnace body part (1.2), be used for feeding in furnace body part (1.2) when furnace cover (1.1) is opened, be used for sealed furnace body part (1.2) when closing, furnace body part (1.2) include shell (1.2.1) and heat preservation (1.2.2), shell (1.2.1) cavity setting, heat preservation (1.2.2) cavity setting and its setting are in the cavity of shell (1.2.1), be provided with heating device (1.2.3) of cavity setting in heat preservation (1.2.2), heating device (1.2.3) are the cavity setting, and it is used for heating furnace internal temperature to make the material graphitization, fixed mounting has gas delivery head (4) that run through furnace body part (1.2), heat preservation (1.2.2) and heating device (1.3) for gas exchange device (1.2.3) and gas in the cavity setting are in the cavity setting, and furnace body part (1.2.3) are used for gas exchange part (1.5) and are located in the bottom part (1.5) bottom part, bottom part (1.5) is seted up.
2. The lithium battery anode material graphitization equipment according to claim 1, wherein the electric control table (2) is connected with a temperature measuring port (5), the temperature measuring port (5) is used for feeding back the temperature in the furnace to the control table, the control table is connected with a heating device (1.2.3), the other end of the heating device (1.2.3) far away from the furnace body part (1.2) is connected with a direct current power supply (1.2.4), and the direct current power supply (1.2.4) is used for supplying power to the heating device (1.2.3) to heat the heating device.
3. The graphitization device for the negative electrode material of the lithium battery according to claim 2, wherein an infrared temperature measuring head (5.1) is fixedly arranged at one end of the temperature measuring port (5) close to the heating device (1.2.3) and used for measuring the temperature in the furnace, the infrared temperature measuring head (5.1) penetrates through the furnace body part (1.2), the heat insulating layer (1.2.2) and the heating device (1.2.3), and one end of the temperature measuring port (5) far away from the heating device (1.2.3) is connected with the electric control console (2) and used for feeding back the temperature in the furnace to the control console.
4. The lithium battery negative electrode material graphitizing equipment according to claim 3, wherein a vertically placed rotating rod (6) is arranged in a cavity of the heating device (1.2.3), the top of the rotating rod (6) is rotationally arranged at the top of the furnace body part (1.2), a plurality of cross rods (6.1) are symmetrically arranged on the rotating rod (6) and are used for stirring lithium battery negative electrode material when the rotating rod (6) rotates, a first bevel gear (6.2) is fixedly arranged at the top of the rotating rod (6), a second bevel gear (6.3) is connected with the first bevel gear (6.2) in a meshed mode, one end, away from the first bevel gear (6.2), of the second bevel gear (6.3) is fixedly arranged on a motor (6.4), and the motor (6.4) is connected with the electric control console (2) and is used for controlling the starting and stopping of the rotation of the rotating rod (6).
5. The graphitizing equipment for negative electrode materials of lithium batteries according to claim 4, wherein a gas delivery pipe (7) connected with a gas delivery head (4) is arranged outside the furnace body part (1.2), the other end of the gas delivery pipe (7) far away from the graphitizing furnace (1) is provided with a first pipeline (7.1), a second pipeline (7.2), a third pipeline (7.3) and a fourth pipeline (7.4), and a first valve (7.1.1), a second valve (7.2.1), a third valve (7.3.1) and a fourth valve (7.4.1) which can work independently are respectively arranged at positions close to the delivery pipe, one end of the first pipeline (7.1) is connected with the gas delivery pipe (7), the other end is connected with a volatile recovery device (7.1.2), the volatile recovery device (7.1.2) is used for recovering volatile matters generated during heating, the second pipeline (7.2) is connected with the inert gas delivery pipe (7.2) in a vacuum state, the inert gas delivery pipe (7.2) is connected with the other end (7.2) in a vacuum state, the inert gas delivery pipe (2) is connected with the other end (7.3.2) in a sealing way, and the inert gas delivery pipe (2) is connected with one end (2.3.2) of the inert gas delivery pipe is sealed, one end of the fourth pipeline (7.4) is connected with the gas conveying pipe (7), the other end of the fourth pipeline is connected with the cold air output device (7.4.2), the cold air output device (7.4.2) is used for conveying cold air into the sealed furnace body part (1.2) after graphitization is completed so as to enable the lithium battery cathode material to be cooled rapidly, and when one valve is opened, the other valves are closed so as to ensure the stability of the gas in the furnace.
6. The lithium battery negative electrode material graphitizing equipment according to claim 5, wherein a connecting plate (1.4) is fixedly arranged on the outer side of the furnace body part (1.2), a hydraulic rod (1.5) is fixed on the connecting plate, the other end of the hydraulic rod (1.5) away from the connecting plate (1.4) is fixedly connected with the furnace cover (1.1), when the hydraulic rod (1.5) stretches out, the furnace cover (1.1) rises, when the hydraulic rod (1.5) contracts, the furnace cover (1.1) descends, the hydraulic rod (1.5) is used for opening and closing the furnace cover (1.1), and a charging channel (8) is formed between the furnace cover (1.1) and the furnace body part (1.2) when the furnace cover (1.1) is opened, and is used for charging lithium battery negative electrode material into the furnace body part (1.2).
7. The lithium battery anode material graphitizing equipment according to claim 6, wherein a first connecting ring (9) is fixedly arranged at the bottom of the furnace cover (1.1), a second connecting ring (10) fixedly arranged at the top of the furnace body part (1.2) is arranged at the bottom of the first connecting ring, a plurality of sealing rings (9.1) with different diameters concentric with the connecting rings are fixedly arranged at the bottom of the first connecting ring (9), sealing grooves (10.1) corresponding to the sealing rings (9.1) are formed at the top of the second connecting ring (10), and the sealing rings (9.1) are used for sealing the furnace body part (1.2) when the sealing rings (9.1) are inserted into the sealing grooves (10.1).
8. The lithium battery negative electrode material graphitizing equipment according to claim 7, wherein the heat insulation plate (11) is fixedly arranged in the first connecting ring, the heat insulation plate (11) is used for insulating the furnace cover (1.1) when the furnace body part (1.2) is heated, the bottom of the furnace body part (1.2) is provided with a conical surface plate (12) fixedly connected with the bottom of the heating device (1.2.3) and arranged in a hollow mode, the conical surface plate (12) is used for facilitating material discharge, the bottom opening of the conical surface plate (12) is arranged, an insulating plate (13) fixedly arranged on the shell (1.2.1) of the furnace body part (1.2) and positioned at the top of the furnace bottom part (1.3) is arranged at the bottom of the furnace body part, and the insulating plate (1.3) is provided with a sealing bottom plate (14) penetrating through and flush with the bottom of the conical surface plate (12) in a sliding mode and used for sealing the furnace body part (1.2).
9. The graphitizing equipment for the negative electrode material of the lithium battery according to claim 8, wherein a heat insulation connecting piece (15) fixed at the end part of the rotating rod (6) is arranged at the center of the heat insulation plate, the heat insulation connecting piece (15) is used for blocking the conduction of the internal temperature of the furnace body part (1.2) upwards, and the connecting piece penetrates through the heat insulation plate and is rotatably arranged on the heat insulation plate.
10. A process for graphitizing a negative electrode material of a lithium battery, using the lithium battery negative electrode material graphitizing device as set forth in any one of claims 1 to 9, comprising:
step one, opening a furnace cover (1.1), and adding a lithium battery anode material to be graphitized;
closing a furnace cover (1.1), heating a heating device (1.2.3) through an electric control table (2), preheating a lithium battery anode material to be graphitized, simultaneously rotating a rotating rod (6) through the electric control table (2), stirring the anode material, simultaneously opening a first valve (7.1.1), opening a volatile recovery device (7.1.2), and recovering volatile generated in the furnace;
heating a heating device (1.2.3) to a temperature required by graphitizing a negative electrode material through an electric control table (2), stopping rotating a rotating rod (6) through the electric control table (2) when the temperature reaches the required temperature, closing a first valve (7.1.1), opening a second valve (7.2.1), opening a vacuum machine, evacuating furnace gas, closing the second valve (7.2.1), opening a third valve (7.3.1), opening an inert gas output device (7.3.2), and introducing protective inert gas into the furnace;
step four, observing the temperature in the furnace through an infrared temperature measuring head (5.1), controlling the temperature of a heating device (1.2.3) through a control console so as to control the temperature in the furnace, intermittently rotating and stopping a rotating rod (6) through an electric control console (2), and fully heating a negative electrode material;
step five, after the graphitization process is finished, the heating device (1.2.3) is closed, the fourth valve (7.4.1) is opened, the cold air output device (7.4.2) is opened, cold air is introduced into the furnace, and meanwhile, the rotating rod (6) is rotated through the electric control table (2) so as to quickly cool the graphitized lithium battery cathode material;
and step six, opening the bottom part (1.3) of the furnace, and discharging the cooled graphitized lithium battery anode material.
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