CN113213449A - Continuous reaction treatment method for graphite cathode material/phosphate and ternary anode material of lithium ion battery - Google Patents
Continuous reaction treatment method for graphite cathode material/phosphate and ternary anode material of lithium ion battery Download PDFInfo
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- CN113213449A CN113213449A CN202110437664.4A CN202110437664A CN113213449A CN 113213449 A CN113213449 A CN 113213449A CN 202110437664 A CN202110437664 A CN 202110437664A CN 113213449 A CN113213449 A CN 113213449A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
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- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- 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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- 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
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- 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 invention relates to a continuous reaction treatment method of graphite cathode materials/phosphates and ternary cathode materials of a lithium ion battery, which comprises the following steps: s1: starting the rotary reactor and the heating device to enable the coating section and the carbonization section of the rotary reactor to reach a preset temperature zone; s2: feeding the mixed raw materials into the feeding end of the rotary reactor through a feeding mechanism; s3: enabling the mixed raw materials entering the feeding end to enter a coating section of the rotary reactor through rotation and self-pushing of the rotary reactor, and performing medium-temperature coating treatment on the mixed raw materials; s4: the material after the medium-temperature coating treatment is continuously pushed by the rotary reactor to enter a carbonization section of the rotary reactor, and the material is subjected to high-temperature carbonization treatment; s5: and (3) cooling the material after high-temperature carbonization treatment, and finally discharging the graphite cathode material prepared by a discharge mechanism. The method has the advantages of reducing cost, saving energy, protecting environment, simplifying process flow and improving product quality.
Description
Technical Field
The invention mainly relates to the field of preparation of graphite cathode materials of lithium ion batteries, in particular to a continuous reaction treatment method of graphite cathode materials/phosphate and ternary cathode materials of lithium ion batteries.
Background
The preparation process of the graphite cathode material of the lithium ion battery at present adopts the following process in the coating carbonization section: firstly, the needle coke and the asphalt are respectively crushed to be below 20 microns below minus by a crushing device. The two are mixed according to a certain proportion, and then are sent into a coating reaction kettle, a resistance wire is arranged outside the reaction kettle, the raw materials are transferred into the reaction kettle through the wall of the reaction kettle, the temperature of the materials is controlled according to a certain temperature control curve, the softening and melting of the asphalt and the coating and carbonization of needle coke are completed, the heat transfer of the equipment is limited, the highest temperature can only reach 650 ℃ generally, part of the aromatic hydrocarbon which can be decomposed only by the high temperature of more than 650 ℃ can not be decomposed, the materials which are discharged from the coating reaction kettle are required to be sprayed and cooled to be less than 100 ℃ through another spraying and cooling kettle provided with a spraying and cooling device, then are sent into a roller kiln or a pushed slab kiln to be heated to 1000 ℃ to further decompose and carbonize the aromatic hydrocarbon in the asphalt, then are sent to a graphitization furnace to complete graphitization at about 3000 ℃, and are treated after spraying and cooled to obtain the carbon-based lithium battery graphite cathode material. The material that directly will spout the water cooling cauldron and come out is also sent into graphitizing furnace directly, accomplishes the further task of decomposing the carbomorphism of aromatic hydrocarbon in pitch at graphitizing furnace, but graphitizing furnace all takes acheson stove as the main at present, and acheson stove does not have any flue gas and catches and flue gas processing apparatus, and environmental pollution is serious.
The process is similar to the coating carbonization process of the graphite cathode material of the lithium ion battery. At present, lithium iron phosphate, lithium nickel cobalt manganese oxide/lithium nickel cobalt aluminate (NCM/NCA) ternary lithium ion battery anode materials are also subjected to high-temperature static sintering in a pushed slab kiln or a roller kiln. The fully mixed raw materials are loaded into a corundum-mullite ceramic sagger and then enter a pushed slab kiln or a roller kiln for sintering, the temperature of a pre-sintering section is controlled below 600 ℃, and the drainage, coke removal and coating work of the materials is completed; the temperature of the high-temperature sintering section is controlled within the range of 600-1000 ℃, and the solid-phase sintering reaction of the precursor of the anode material and the lithium salt is completed. In the sintering process, a large amount of heat is absorbed by the ceramic sagger, and a large amount of heat loss is caused by the fact that the materials and the sagger need to be cooled at the discharge hole. In addition, because static sintering is adopted, heat transfer is limited, longer heat treatment residence time is needed compared with dynamic sintering, and the overall energy consumption is higher.
The existing lithium ion battery graphite negative electrode material coating carbonization process has the following problems: 1. the main thermal equipment, the reaction kettle and the water spray cooling kettle are all discontinuous operation equipment, and the single equipment has low processing capacity and high labor cost; 2. the single equipment has small processing capacity and low production efficiency due to heat transfer and limitation; 3. the thermal regulation is unreasonable, the materials are heated to 650 ℃ in the coating reaction kettle, the materials are cooled to normal temperature by an indirect water cooling method through a water spray cooling kettle during discharging, then the materials are sent into a roller kiln or a pushed slab kiln, the temperature is raised to about 1000 ℃ again, and the materials are cooled to normal temperature by water spray, so that the energy waste is serious.
The high-temperature sintering process of the prior lithium ion battery lithium iron phosphate, ternary anode materials and the like has the following problems: 1. high-temperature static sintering, wherein materials are contained in a ceramic sagger, the heat transfer of the materials is limited, the retention time is long, the processing capacity of single equipment is low, the energy consumption is high, and the manpower and equipment investment cost is high; 2. the sagger for containing the materials absorbs a large amount of heat in the high-temperature sintering process, and the discharge port needs to be cooled together to cause high energy consumption.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the continuous reaction treatment method for the graphite positive/negative electrode materials of the lithium ion battery, which can reduce the cost, save energy, protect environment, simplify the process flow and improve the product quality.
In order to solve the technical problems, the invention adopts the following technical scheme:
a continuous reaction treatment method for graphite anode/cathode materials of a lithium ion battery is characterized in that a rotary reactor is adopted to carry out continuous coating treatment and carbonization treatment on reaction raw materials; the method specifically comprises the following steps:
s1: starting the rotary reactor and the heating device to enable the coating section and the carbonization section of the rotary reactor to reach a preset temperature zone;
s2: feeding mixed raw materials for preparing the graphite cathode material into the feed end of the rotary reactor through a feed mechanism;
s3: enabling the mixed raw materials entering the feeding end to enter a coating section of the rotary reactor through rotation and self-pushing of the rotary reactor, and performing medium-temperature coating treatment on the mixed raw materials;
s4: the material after the medium-temperature coating treatment is continuously pushed by the rotary reactor to enter a carbonization section of the rotary reactor, and the material is subjected to high-temperature carbonization treatment;
s5: and (3) cooling the material after high-temperature carbonization treatment, and finally discharging the graphite cathode material prepared by a discharge mechanism.
As a further improvement of the above technical solution:
the rotary reactor is a rotary kiln which is obliquely arranged along the horizontal direction; the feed end of the rotary kiln is high, and the discharge end of the rotary kiln is low.
The included angle between the axis of the rotary reactor and the horizontal line is a, and a is more than 0 degree and less than or equal to 10 degrees; the rotating speed of the rotating reactor is set to be n, wherein n is more than 0r/min and less than or equal to 15 r/min.
The heating device comprises a first heating furnace and a second heating furnace, wherein the first heating furnace is arranged outside the rotary reactor and used for heating the coating section, and the second heating furnace is used for heating the carbonization section.
In the middle-temperature coating treatment process of the step S3, the temperature zone is set to be t1 by the regulation and control of a first heating furnace, and the temperature is more than 0 ℃ and less than or equal to t1 and less than or equal to 650 ℃;
in the high-temperature carbonization treatment process of the step S4, the temperature zone is set to be t2 by the regulation and control of the second heating furnace, and the temperature is more than 450 ℃ and less than or equal to t2 and less than or equal to 1100 ℃.
The cooling treatment of the step S5 is also arranged in the cavity of the rotary reactor, so that the material can be continuously coated, carbonized and cooled, and the specific operation is that a cooling section is additionally arranged between the carbonization section and the discharge end of the rotary reactor, and a cooling component for directly cooling the outer wall of the cooling section is arranged outside the cooling section.
Cooling module includes water spray cooling basin, circulating water cooling tower, hot-water pump, inlet tube, outlet pipe, sprays mechanism and cold water pump, water spray cooling basin sets up in the rotary reactor lower part, it installs the top at rotary reactor to spray the mechanism, the circulating water cooling tower passes through the inlet tube and sprays the mechanism and be connected, water spray cooling basin pass through the outlet pipe with the circulating water cooling tower is connected, the hot-water pump is installed on the outlet pipe, the cold water pump is installed on the inlet tube, the warp cooling zone warm area behind the cooling module effect sets up to t3, and t3 is greater than or equal to 0 ℃ and is less than or equal to 200 ℃.
The rotating speed of the rotary reactor is controlled by the driving device, the temperature zones of the coating section and the carbonization section are controlled by the heating device and the temperature sensor, the temperature zone of the cooling section is controlled by the flow control part of the cooling assembly, and the rotating speed of the rotary reactor and the temperature zones of the coating section, the carbonization section and the cooling section are comprehensively adjusted and controlled by a control system, so that the automatic continuous production of the continuous coating carbonization process is realized.
The feeding end and the discharging end of the rotary reactor are sealed in a combined mode through a sealing device, the sealing device comprises a first solid sealing group, a gas sealing group and a second solid sealing group which are arranged along the circumferential direction of the rotary reactor, and the first solid sealing group, the gas sealing group and the second solid sealing group are sequentially arranged at the gas leakage point along the axial direction and form axial sealing; the first, gas, and second solid seal groups each form a radial seal against the rotary reactor.
The inner chamber of rotary reactor realizes the stirring of material through a material raising scraper mechanism and raises the material and scrape the material, the material raising scraper mechanism scrapes the plate including raising material scraper blade driving piece, transmission shaft and raising the material, the transmission shaft extends in the rotary reactor and is connected with the material raising scraper blade driving piece, the material raising is scraped the plate and is installed on the transmission shaft.
A continuous reaction treatment method for phosphate and ternary cathode materials of a lithium ion battery is characterized in that a rotary reactor is adopted to carry out continuous pre-sintering treatment and sintering treatment on reaction raw materials; the method specifically comprises the following steps:
s1: starting the rotary reactor and the heating device to enable the pre-sintering section and the sintering section of the rotary reactor to reach a preset temperature zone;
s2: feeding mixed raw materials for preparing the anode material into the feed end of the rotary reactor through a feed mechanism;
s3: the mixed raw materials entering the feeding end enter the rotary reactor for presintering through the rotation and self-pushing of the rotary reactor, and the mixed raw materials are subjected to medium-temperature presintering treatment;
s4: the materials after the medium-temperature pre-sintering treatment are continuously pushed by the rotary reactor to enter a sintering section of the rotary reactor, and the materials are subjected to high-temperature sintering treatment;
s5: and (3) cooling the material subjected to high-temperature sintering treatment, and finally discharging the prepared anode material through a discharging mechanism.
Compared with the prior art, the invention has the advantages that:
the invention relates to a continuous reaction treatment method of graphite cathode materials of a lithium ion battery, which comprises the steps of firstly starting a rotary reactor to enable the rotary reactor to rotate; then starting the first heating furnace, the second heating furnace and the cooling assembly to enable the body of the corresponding section to reach a corresponding preset temperature zone; then starting the feeding mechanism to enable the needle coke and the asphalt mixed according to a certain proportion to enter the rotary reactor through the feeding mechanism; and finally, starting the discharging mechanism to output the completely-coated and carbonized material from the discharging mechanism. Compared with the traditional structure, the equipment realizes the continuity of the coating, carbonization and cooling processes of the graphite cathode material of the lithium ion battery through the integrated rotary reactor, ensures the consistency of the product and obviously improves the product quality; the equipment for coating the reaction kettle, cooling the cooling kettle, carbonizing the roller kiln or the pusher kiln and indirectly cooling water at present is replaced, the process flow and the labor intensity and the number of workers of the operators are greatly simplified, the energy consumption per ton of the product is greatly reduced, the equipment investment, the labor cost and the energy consumption cost are obviously reduced, and the large-scale equipment can be realized; meanwhile, the computer automatic control is easy to realize, so that the production cost is greatly reduced.
According to the continuous reaction treatment method for the lithium ion phosphate and ternary cathode materials, the continuity of the procedures of pre-sintering, sintering and cooling of the graphite cathode materials of the lithium ion battery is realized through the integrated rotary reactor by adopting the method, the consistency of products is ensured, and the product quality is obviously improved; the method has the advantages that the existing box-type furnace and roller kiln or pushed slab kiln sintering equipment is replaced, the process flow and the labor intensity and the number of workers for operating the workers are greatly simplified, the energy consumption per ton of products is greatly reduced, the equipment investment, the labor cost and the energy consumption cost are obviously reduced, and the large-scale equipment can be realized; meanwhile, the computer automatic control is easy to realize, so that the production cost is greatly reduced. .
Drawings
FIG. 1 is a flow chart of a continuous reaction treatment method of graphite cathode materials/lithium ion battery phosphates and ternary cathode materials of a lithium ion battery.
FIG. 2 is a schematic structural diagram of an artificial graphite type negative electrode material continuous coating carbonization device of a lithium ion battery in the invention.
Fig. 3 is an enlarged schematic view of a portion a of fig. 2.
Fig. 4 is a schematic view of the structure of the cooling module of the present invention.
Fig. 5 is a schematic structural view of the material lifting scraper mechanism of the present invention.
Fig. 6 is a schematic view of the structure of the sealing device of the present invention.
The reference numerals in the figures denote:
1. a feeding mechanism; 2. rotating the reactor; 21. a reactor body; 22. a rotary drive member; 221. driving the supporting seat; 222. a drive motor; 223. a speed reducer; 224. a drive wheel; 225. a driving wheel; 3. a discharging mechanism; 4. a first heating furnace; 41. a first furnace body; 42. a first heating member; 5. a second heating furnace; 51. a second furnace body; 52. a second heating member; 6. a cooling assembly; 61. a water spray cooling water tank; 62. circulating water cooling tower; 63. a hot water pump; 64. a water inlet pipe; 65. a water outlet pipe; 66. a spraying mechanism; 67. a cold water pump; 7. a support device; 71. a roller seat; 72. a support wheel; 8. a material lifting scraper mechanism; 81. a material raising scraper drive; 82. a drive shaft; 821. a minor axis; 822. a movable joint bearing; 83. a material lifting scraper plate; 831. a first material raising scraper unit; 8311. a material guide cylinder; 83111. a material leaking hole; 8312. the material guiding is spiral; 832. a second material raising scraper unit; 833. a cage-shaped support frame; 8331. a support ring frame; 8332. a material raising scraper plate; 9. a sealing device; 91. a first solid seal pack; 911. a first stationary ring; 912. a first resilient seal member; 913. a first rotating ring; 92. a gas seal group; 921. a second stationary ring; 922. an inflation cavity; 923. an inflation tube; 93. a second solid seal group; 931. a third stationary ring; 932. a second resilient seal member; 933. a biasing member; 934. a fourth stationary ring; 935. a third resilient seal member; 936. a second rotating ring.
Detailed Description
The invention will be described in further detail below with reference to the drawings and specific examples.
As shown in fig. 1 to 6, in an embodiment of the method for continuously reacting and processing a graphite-based negative electrode material/a phosphate and a ternary positive electrode material of a lithium ion battery according to the present invention, a rotary reactor is used to continuously coat and carbonize a reaction raw material; the method specifically comprises the following steps:
s1: starting the rotary reactor 2 and the heating device to enable the coating section and the carbonization section of the rotary reactor 2 to reach a preset temperature zone;
s2: feeding mixed raw materials for preparing graphite cathode materials into a feed end of a rotary reactor 2 through a feed mechanism 1;
s3: the mixed raw materials entering the feeding end enter the coating section of the rotary reactor 2 through the rotation and self-pushing of the rotary reactor 2, and the mixed raw materials are subjected to medium-temperature coating treatment;
s4: the material after the medium-temperature coating treatment is continuously pushed by the rotary reactor 2 to enter a carbonization section of the rotary reactor 2, and the material is subjected to high-temperature carbonization treatment;
s5: and (3) cooling the material after high-temperature carbonization treatment, and finally discharging the graphite cathode material prepared by the preparation method through a discharging mechanism 3.
By adopting the method, the continuity of the coating, carbonization and cooling processes of the graphite cathode material of the lithium ion battery is realized through the integrated rotary reactor 2, the consistency of the product is ensured, and the product quality is obviously improved; the equipment for coating the reaction kettle, cooling the cooling kettle, carbonizing the roller kiln or the pusher kiln and indirectly cooling water at present is replaced, the process flow and the labor intensity and the number of workers of the operators are greatly simplified, the energy consumption per ton of the product is greatly reduced, the equipment investment, the labor cost and the energy consumption cost are obviously reduced, and the large-scale equipment can be realized; meanwhile, the computer automatic control is easy to realize, so that the production cost is greatly reduced.
In this embodiment, the rotary reactor 2 is a rotary kiln arranged obliquely in the horizontal direction; the feed end of the rotary kiln is high, and the discharge end of the rotary kiln is low. Set up like this for the material is in the rotatory effort of self gravity and rotatory reactor 2 and is lastingly carried to the discharge end, has improved efficiency.
In the embodiment, the included angle between the axis of the rotary reactor 2 and the horizontal line is a, and a is more than 0 degree and less than or equal to 10 degrees; the rotating speed of the rotating reactor 2 is set as n, and n is more than 0r/min and less than or equal to 15 r/min. The angle a is set to 7 ° in this embodiment. By the arrangement, the uniform coating, full carbonization and cooling effects of the materials can be guaranteed, and the discharging efficiency can be guaranteed. In the embodiment, n is specifically set to be 10r/min, so that the continuous conveying of materials is ensured while the full reaction of each section is ensured.
In this embodiment, the heating means includes a first heating furnace 4 for heating the covered zone and a second heating furnace 5 for heating the carbonized zone, which are disposed outside the rotary reactor 2. The coating section is heated by a first heating furnace 4, and the carbonization section is heated by a second heating furnace 5, so that the corresponding section can reach a corresponding preset temperature zone.
In the embodiment, in the middle-temperature coating treatment process of the step S3, the temperature zone is set to t1 by the regulation and control of the first heating furnace 4, and t1 is more than 0 ℃ and less than or equal to 650 ℃; in the high-temperature carbonization treatment process of the step S4, the temperature zone is set to be t2 by the regulation and control of the second heating furnace 5, and the temperature is more than 450 ℃ and less than or equal to t2 and less than or equal to 1100 ℃. The task of the first heating furnace 4 is mainly to complete the coating and partial carbonization of the carbon raw material by the asphalt, and t1 is specifically set to be 600 ℃. The second heating furnace 5 is mainly used for carbonizing the coated asphalt, and t2 is specifically set to be 1000 ℃.
In this embodiment, the cooling treatment in step S5 is also provided in the cavity of the rotary reactor 2, so that the material can be continuously coated, carbonized, and cooled, and specifically, a cooling section is additionally provided between the carbonization section and the discharge end of the rotary reactor 2, and a cooling assembly 6 for directly cooling the outer wall of the cooling section is provided outside the cooling section. This cooling module 6 continuously cools off the outer wall of rotatory reactor 2 and lowers the temperature, guarantees the material temperature of rotatory reactor 2 export.
In this embodiment, the cooling module 6 includes a water spray cooling water tank 61, a circulating water cooling tower 62, a hot water pump 63, a water inlet pipe 64, a water outlet pipe 65, a spraying mechanism 66 and a cold water pump 67, the water spray cooling water tank 61 is disposed at the lower part of the rotary reactor 2, the spraying mechanism 66 is disposed above the rotary reactor 2, the circulating water cooling tower 62 is connected with the spraying mechanism 66 through the water inlet pipe 64, the water spray cooling water tank 61 is connected with the circulating water cooling tower 62 through the water outlet pipe 65, the hot water pump 63 is mounted on the water outlet pipe 65, and the cold water pump 67 is mounted on the water. In the structure, cooling water in a circulating water cooling tower 62 enters a spraying mechanism 66 through a water inlet pipe 64 under the action of a cold water pump 67 to spray and cool a rotary reactor 2, and then the water after heat exchange flows back to the circulating water cooling tower 62 through a hot water pump 63 and a water outlet pipe 65, so that a circulating cooling system is integrally formed. The material temperature at the outlet of the rotary reactor 2 is ensured to be 0-200 ℃.
In this embodiment, the rotation speed of the rotary reactor 2 is controlled by the driving device, the temperature zones of the coating section and the carbonization section are controlled by the heating device and the temperature sensor, the temperature zone of the cooling section is controlled by the flow control part of the cooling assembly 6, and the rotation speed of the rotary reactor 2 and the temperature zones of the coating section, the carbonization section and the cooling section are comprehensively adjusted and controlled by a control system, so that the automatic continuous production of the continuous coating and carbonization process is realized. The operation is simple and convenient.
In this embodiment, the first heating furnace 4, the second heating furnace 5 and the cooling module 6 are all arranged coaxially with the rotary reactor 2. By the arrangement, the consistent distance between the first heating furnace 4, the second heating furnace 5 and the cooling assembly 6 and the circumferential direction of the rotary reactor 2 is ensured, namely the hot and cold uniformity of the corresponding temperature area and the corresponding cold area of the rotary reactor 2 is ensured.
In this embodiment, the first heating furnace 4, the second heating furnace 5 and the cooling module 6 are arranged at intervals along the rotary reactor 2. The arrangement is convenient for the temperature arrangement and regulation of each temperature area and each cold area, and the mutual influence is reduced.
In this embodiment, the support devices 7 for supporting the respective corresponding positions of the rotary reactor 2 are installed outside the rotary reactor 2 at intervals. Because the rotary reactor 2 is a continuous integrated structure, the length of the rotary reactor is longer, and the supporting devices 7 are arranged at intervals, so that the rotary reactor 2 is conveniently supported, and the stability of the equipment is improved.
In this embodiment, the supporting device 7 includes a roller seat 71 and a supporting wheel 72, the supporting wheel 72 is fixed on the rotating reactor 2, the roller seat 71 is fixed on the ground and contacts with the supporting wheel 72, and the normal rotating function of the rotating reactor 2 can be ensured while the rotating reactor 2 is supported.
In this embodiment, the rotary reactor 2 includes a body 21 and a rotary driving member 22, the body 21 is inserted into the first heating furnace 4, the second heating furnace 5 and the cooling module 6 and is connected with the feeding mechanism 1 and the discharging mechanism 3, and the rotary driving member 22 is disposed outside the body 21 and drives the body 21 to rotate. In this structure, the rotary driving member 22 is used to drive the body 21 to rotate, and the structure is simple and reliable.
In this embodiment, the rotary driving member 22 includes a driving support seat 221, a driving motor 222, a speed reducer 223, a driving wheel 224 and a driving wheel 225, the driving support seat 221 is fixed on the ground, the driving wheel 224 is installed on the driving support seat 221, the driving wheel 225 is fixed on the rotary reactor 2 and connected to the driving wheel 224, and the driving motor 222 drives the driving wheel 224 to rotate through the speed reducer 223, so as to drive the rotary reactor 2 to rotate through the driving wheel 225.
In the present embodiment, the first heating furnace 4 includes a first furnace body 41 and a first heating member 42 mounted on the first furnace body 41 and extending to the inside thereof, the first furnace body 41 being disposed outside the rotary reactor 2; the second heating furnace 5 includes a second furnace body 51 and a second heating member 52 installed on the second furnace body 51 and extending to the inside thereof, the second furnace body 51 being disposed outside the rotary reactor 2. In the structure, the first heating furnace 4 is designed to be at a temperature of 0-650 ℃, an electric heating element (a first heating element 42), combustion fuel oil, combustion producer gas and combustion natural gas can be used for heating, in order to ensure the uniformity of a temperature field, a burner for combusting the fuel can adopt a radiation type burner, and the task of the first section is mainly to complete the coating and partial carbonization of the carbon raw material by the asphalt; the second heating furnace 5 is designed to be at a temperature of 450-1100 ℃, and the heating mode can use an electric heating element (the second heating element 52), fuel oil combustion, producer gas combustion and natural gas combustion. In order to reduce energy consumption, a regenerative burner can be adopted as a burner for burning fuel. The second stage of the process mainly completes the carbonization of the coated asphalt.
In this embodiment, the feed end and the discharge end of the rotary reactor 2 are sealed in a combined manner by a sealing device 9, the sealing device 9 includes a first solid seal group 91, a gas seal group 92 and a second solid seal group 93 which are arranged along the circumferential direction of the rotary reactor 2, and the first solid seal group 91, the gas seal group 92 and the second solid seal group 93 are sequentially arranged along the axial direction at a gas leakage point and form axial seals with each other; the first solids seal pack 91, the gas seal pack 92 and the second solids seal pack 93 all form radial seals to the rotary reactor 2. In the structure, a rotating gap exists at the butt joint of the rotating reactor 2 and a fixing piece at the end part of the rotating reactor, and the rotating reactor 2 is sealed by the first solid sealing group 91 to prevent harmful gas from leaking; protective gas is further introduced through the gas seal group 92, so that on one hand, the gas pressure of the gas seal group 92 is greater than the gas pressure in the rotary reactor 2 to form further positive pressure seal, and on the other hand, if the protective gas enters the rotary reactor 2, the protective gas can be provided for the rotary reactor 2, and the reaction efficiency is further improved; and the second solid sealing group 93 further forms a seal for the rotary reactor 2, which is equivalent to forming a third stage seal, and further prevents harmful gas from leaking. The whole structure is simple and reliable, and the sealing performance is good. Through the axial and radial double sealing, the sealing performance is greatly improved.
In this embodiment, the first solids seal group 91 comprises a first stationary ring 911, a first elastic seal 912 and a first rotating ring 913, the first elastic seal 912 is press-fitted between the first stationary ring 911 and the rotary reactor 2, the first rotating ring 913 is connected with the end of the first stationary ring 911 and axially presses the first elastic seal 912, and the gas seal group 92 is connected with the first rotating ring 913; the gas sealing group 92 comprises a second stationary ring 921, a gas filling cavity 922 with the gas pressure larger than the gas pressure in the rotary reactor 2 is formed between the second stationary ring 921 and the rotary reactor 2, a gas filling pipe 923 used for filling protective gas into the gas filling cavity 922 is arranged on the second stationary ring 921, and a second solid sealing group 93 is connected with the second stationary ring 921; the second solid sealing group 93 comprises a third static ring 931, a second elastic sealing element 932 and a pushing element 933, wherein the third static ring 931 is connected with the gas sealing group 92, the second elastic sealing element 932 is pressed between the third static ring 931 and the rotary reactor 2, and the pushing element 933 is arranged on the third static ring 931 and applies radial pressure to the second elastic sealing element 932; the second solid seal group 93 further comprises a fourth stationary ring 934, a third elastic seal 935 and a second moving ring 936, wherein the fourth stationary ring 934 is connected with the third stationary ring 931, the third elastic seal 935 is press-fitted between the fourth stationary ring 934 and the rotary reactor 2, and the second moving ring 936 is end-connected with the fourth stationary ring 934 and axially compresses the third elastic seal 935. In the structure, the first elastic sealing element 912 is formed by asbestos packing to form a soft high-temperature-resistant sealing material, and the first movable ring 913 axially compresses the first elastic sealing element 912, so that the first elastic sealing element 912 radially expands, and the first elastic sealing element 912 radially seals the rotary reactor 2. Nitrogen is filled through the gas filling pipe 923 to make the gas pressure of the gas filling cavity 922 larger than the gas pressure in the rotary reactor 2, thereby forming further positive pressure sealing. The second elastic sealing member 932 is formed of an asbestos packing to form a soft high temperature resistant sealing material, and the biasing member 933 radially biases the second elastic sealing member 932 to radially seal the rotary reactor 2. The third elastic sealing member 935 is formed of an asbestos packing to form a soft high temperature resistant sealing material, and the second moving ring 936 axially compresses the third elastic sealing member 935 to cause radial expansion of the third elastic sealing member 935, thereby achieving radial sealing of the third elastic sealing member 935 against the rotary reactor 2.
In this embodiment, the inner chamber of rotary reactor 2 realizes the stirring of material through a material raising scraper mechanism 8 and raises the material and scrape the material, and material raising scraper mechanism 8 scrapes plate 83 including raising material scraper blade driving piece 81, transmission shaft 82 and raising the material, and transmission shaft 82 extends in rotary reactor 2 and is connected with material raising scraper blade driving piece 81, and the material raising scrapes plate 83 and installs on transmission shaft 82. The material lifting scraper driving piece 81 drives the transmission shaft 82 to rotate, the transmission shaft 82 drives the material lifting scraper 83 to rotate, when the material lifting scraper 83 and the rotary reactor 2 rotate synchronously, the material can be effectively stirred, and the coating quality of the needle coke by the asphalt is ensured; when the lifting scraper plate 83 rotates the reactor 2 asynchronously, the material stuck on the rotating reactor 2 can be cleaned, the ring formation caused by the material sticking on the wall in the rotating reactor 2 is effectively prevented, and the long-period operation of the process is ensured.
In this embodiment, the lifting scraper plate 83 includes a first lifting scraper unit 831 and a second lifting scraper unit 832 at the rear of the first lifting scraper unit 831, which are disposed at the feeding end, and the first lifting scraper unit 831 and the second lifting scraper unit 832 are disposed on the transmission shaft 82 at intervals along the material conveying direction; the first material raising scraper blade unit 831 and the second material raising scraper blade unit 832 are both composed of cage-shaped support frames 833, and the cage-shaped support frames 833 are installed on the transmission shaft 82. In this structure, through the first material raising scraper blade unit 831 and the second material raising scraper blade unit 832 of interval arrangement, can realize that the effective material that turns over of each position falls the material that glues on rotary reactor 2 with the clearance, further guaranteed the cladding quality and effectively prevented in the rotary reactor 2 because of the material glues the knot circle that the wall arouses.
In this embodiment, a part of the first material lifting scraper unit 831, which is close to the feed inlet, is provided with a material guide cylinder 8311, an internal cavity of the material guide cylinder 8311 is provided with a material guide screw 8312, and a wall of the material guide cylinder 8311 is uniformly provided with material leaking holes 83111, in the structure, continuous material guide conveying is formed under the action of the material guide cylinder 8311 and the material guide screw 8312, and the material leaking holes 83111 are arranged, so that on one hand, materials can pass quickly, and a normal conveying function is ensured; on the other hand, the material from the material leakage hole 83111 temporarily supports the material guide cylinder 8311, which is equivalent to indirectly supporting the transmission shaft 82, thereby improving the stability; the cage-shaped supporting frame 833 comprises supporting ring frames 8331 arranged at the front end and the rear end and a material lifting scraper 8332 connected with the two supporting ring frames 8331. In the structure, the support ring frames 8331 rotate along with the transmission shaft 82, and when the material lifting scraper 8332 between the two support ring frames 8331 and the rotary reactor 1 synchronously rotate, the material can be effectively turned, so that the coating quality of the needle coke by the asphalt is ensured; when the lifting scraper plate 33 rotates the reactor 1 asynchronously, the material stuck on the rotating reactor 1 can be cleaned, so that the ring formation caused by the material sticking to the wall in the rotating reactor 1 is effectively prevented, and the long-period operation of the process is ensured.
In this embodiment, the transmission shaft 82 is formed by connecting a plurality of short shafts 821 through movable knuckle bearings 822, a first material raising scraper unit 831 is installed on one short shaft 821 near the feeding end, and a second material raising scraper unit 832 is installed on each subsequent short shaft 821. In the structure, the transmission shaft 82 is formed by connecting a plurality of short shafts 821 through movable knuckle bearings 822, so that the whole bending resistance of the transmission shaft 82 is enhanced; and a first material raising scraper blade unit 831 is installed on a section of short shaft 821 near the feeding end, and a second material raising scraper blade unit 832 is installed on each subsequent section of short shaft 821, so that the materials at the feeding end can be fully turned through the first material raising scraper blade unit 831, and the rapid material conveying is ensured through the second material raising scraper blade unit 832 subsequently.
The invention relates to an embodiment of a continuous reaction treatment method of phosphate and ternary cathode materials of a lithium ion battery, which adopts a rotary reactor to carry out continuous pre-sintering treatment and sintering treatment on reaction raw materials; the method specifically comprises the following steps:
s1: starting the rotary reactor 2 and the heating device to enable the pre-sintering section and the sintering section of the rotary reactor 2 to reach a preset temperature zone;
s2: feeding mixed raw materials for preparing graphite anode materials into a feed end of the rotary reactor 2 through a feed mechanism 1;
s3: the mixed raw materials entering the feeding end enter a pre-sintering section of the rotary reactor 2 through the rotation and self-pushing of the rotary reactor 2, and the mixed raw materials are subjected to medium-temperature pre-sintering treatment;
s4: the materials after the medium-temperature pre-sintering treatment are continuously pushed by the rotary reactor 2 to enter a sintering section of the rotary reactor 2, and the materials are subjected to high-temperature sintering treatment;
s5: and (3) cooling the material subjected to high-temperature sintering treatment, and finally discharging the graphite anode material prepared by the method through a discharging mechanism 3.
By adopting the method, the continuity of the coating, sintering and cooling processes of the graphite anode material of the lithium ion battery is realized through the integrated rotary reactor 2, the consistency of the product is ensured, and the product quality is obviously improved; the method has the advantages that the existing box-type furnace and roller kiln or pushed slab kiln sintering equipment is replaced, the process flow and the labor intensity and the number of workers for operating the workers are greatly simplified, the energy consumption per ton of products is greatly reduced, the equipment investment, the labor cost and the energy consumption cost are obviously reduced, and the large-scale equipment can be realized; meanwhile, the computer automatic control is easy to realize, so that the production cost is greatly reduced.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make numerous possible variations and modifications to the present invention, or modify equivalent embodiments to equivalent variations, without departing from the scope of the invention, using the teachings disclosed above. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (11)
1. A lithium ion battery graphite negative electrode material continuous reaction processing method is characterized in that the continuous reaction processing method adopts a rotary reactor (2) to carry out continuous coating processing and carbonization processing on reaction raw materials; the method specifically comprises the following steps:
s1: starting the rotary reactor (2) and the heating device to enable the coating section and the carbonization section of the rotary reactor (2) to reach a preset temperature zone;
s2: feeding mixed raw materials for preparing graphite cathode materials into the feed end of the rotary reactor (2) through a feed mechanism (1);
s3: the mixed raw materials entering the feeding end enter the coating section of the rotary reactor (2) through the rotation and self-pushing of the rotary reactor (2), and the mixed raw materials are subjected to medium-temperature coating treatment;
s4: the material after the medium-temperature coating treatment is continuously pushed by the rotary reactor (2) to enter a carbonization section of the rotary reactor (2), and the material is subjected to high-temperature carbonization treatment;
s5: and (3) cooling the material after high-temperature carbonization treatment, and finally sending out the graphite cathode material prepared by the method through a discharging mechanism (3).
2. The continuous reaction treatment method according to claim 1, wherein the rotary reactor (2) is a rotary kiln disposed obliquely in a horizontal direction; the feed end of the rotary kiln is high, and the discharge end of the rotary kiln is low.
3. The continuous reaction treatment process according to claim 2, characterized in that the axis of the rotating reactor (2) has an angle a with the horizontal line, and 0 ° < a ≦ 10 °; the rotating speed of the rotating reactor (2) is set to be n, wherein n is more than 0r/min and less than or equal to 15 r/min.
4. The continuous reaction treatment process according to claim 1, characterized in that the heating means comprise a first heating furnace (4) for heating the coating section and a second heating furnace (5) for heating the charring section, arranged outside the rotary reactor (2).
5. The continuous reaction processing method according to claim 4, characterized in that: in the middle-temperature coating treatment process of the step S3, the temperature zone is set to be t1 by the regulation and control of the first heating furnace (4), and the temperature is more than 0 ℃ and less than or equal to t1 and less than or equal to 650 ℃;
in the high-temperature carbonization treatment process of the step S4, the temperature zone is set to be t2 by the regulation and control of the second heating furnace (5), and the temperature is more than 450 ℃ and less than t2 and less than or equal to 1100 ℃.
6. The continuous reaction processing method according to any one of claims 1 to 5, wherein the cooling process of step S5 is also arranged in the cavity of the rotary reactor (2) to allow the material to be continuously coated, carbonized and cooled, and specifically, a cooling section is additionally arranged between the carbonization section and the discharge end of the rotary reactor (2), and a cooling component (6) for directly cooling the outer wall of the cooling section is arranged outside the cooling section.
7. The continuous reaction processing method according to claim 6, characterized in that: cooling module (6) are including water spray cooling trough (61), circulating water cooling tower (62), hot water pump (63), inlet tube (64), outlet pipe (65), spray mechanism (66) and cold water pump (67), water spray cooling trough (61) sets up in rotatory reactor (2) lower part, it installs the top at rotatory reactor (2) to spray mechanism (66), circulating water cooling tower (62) are connected with spray mechanism (66) through inlet tube (64), water spray cooling trough (61) pass through outlet pipe (65) with circulating water cooling tower (62) are connected, hot water pump (63) are installed on outlet pipe (65), cold water pump (67) are installed on inlet tube (64), the process cooling zone behind cooling module (6) effect sets up to t3, and 0 ℃ is less than or equal to t3 and is less than or equal to 200 ℃.
8. The continuous reaction processing method according to claim 6, characterized in that: the rotating speed of the rotary reactor (2) is controlled by a driving device, the temperature zones of the coating section and the carbonization section are controlled by a heating device and a temperature sensor, the temperature zone of the cooling section is controlled by a flow control part of the cooling assembly (6), and the rotating speed of the rotary reactor (2) and the temperature zones of the coating section, the carbonization section and the cooling section are comprehensively adjusted and controlled by a control system, so that the automatic continuous production of the continuous coating carbonization process is realized.
9. The continuous reaction treatment method according to any one of claims 1 to 5, characterized in that the feed end and the discharge end of the rotary reactor (2) are sealed in a combined manner by a sealing device (9), the sealing device (9) comprises a first solid sealing group (91), a gas sealing group (92) and a second solid sealing group (93) which are arranged along the circumference of the rotary reactor (2), and the first solid sealing group (91), the gas sealing group (92) and the second solid sealing group (93) are arranged in sequence along the axial direction at the gas leakage point and form an axial seal with each other; the first solid seal group (91), the gas seal group (92) and the second solid seal group (93) each form a radial seal against the rotary reactor (2).
10. The continuous reaction treatment method according to any one of claims 1 to 5, characterized in that the inner cavity of the rotary reactor (2) is used for stirring and scraping materials through a material-lifting scraper mechanism (8), the material-lifting scraper mechanism (8) comprises a material-lifting scraper driving member (81), a transmission shaft (82) and a material-lifting scraper member (83), the transmission shaft (82) extends into the rotary reactor (2) and is connected with the material-lifting scraper driving member (81), and the material-lifting scraper member (83) is mounted on the transmission shaft (82).
11. A continuous reaction treatment method of lithium ion phosphate and ternary cathode materials is characterized in that a rotary reactor (2) is adopted to carry out continuous pre-sintering treatment and sintering treatment on reaction raw materials; the method specifically comprises the following steps:
s1: starting the rotary reactor (2) and the heating device to enable the pre-sintering section and the sintering section of the rotary reactor (2) to reach a preset temperature zone;
s2: feeding mixed raw materials for preparing graphite anode materials into the feed end of the rotary reactor (2) through a feed mechanism (1);
s3: the mixed raw materials entering the feeding end enter a pre-sintering section of the rotary reactor (2) through the rotation and self-pushing of the rotary reactor (2), and the mixed raw materials are subjected to medium-temperature pre-sintering treatment;
s4: the materials after the medium-temperature pre-sintering treatment are continuously pushed by the rotary reactor (2) to enter a sintering section of the rotary reactor (2), and the materials are subjected to high-temperature sintering treatment;
s5: and (3) cooling the material subjected to high-temperature sintering treatment, and finally discharging the graphite anode material prepared by the method through a discharging mechanism (3).
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