CN114146635A - Pre-granulation method of graphite negative electrode material - Google Patents

Pre-granulation method of graphite negative electrode material Download PDF

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Publication number
CN114146635A
CN114146635A CN202111414756.7A CN202111414756A CN114146635A CN 114146635 A CN114146635 A CN 114146635A CN 202111414756 A CN202111414756 A CN 202111414756A CN 114146635 A CN114146635 A CN 114146635A
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Prior art keywords
temperature
minutes
granulation method
raising
material according
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CN202111414756.7A
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Chinese (zh)
Inventor
徐坚
夏云川
仰韻霖
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Guangdong Kaijin New Energy Technology Co Ltd
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Guangdong Kaijin New Energy Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/10Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in stationary drums or troughs, provided with kneading or mixing appliances
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M2004/026Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027Negative electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention relates to the field of lithium ion battery cathode materials, in particular to a pre-granulation method of a graphite cathode material, which comprises the following steps: s1, processing the coal-based coke by a shaping machine to obtain primary particles; s2, mixing the primary particles and asphalt through a mixer to obtain a mixture; and S3, adding the mixture into a roller furnace, and obtaining different granulation results by utilizing different temperature rising curves. The invention carries out temperature-rising curve treatment on the artificial graphite raw materials by different roller furnaces respectively, and then carries out blending treatment according to a certain proportion, thereby laying a cushion for obtaining a product which can give consideration to excellent charging and circulating performances of the secondary particle material and high tap density and high capacity performance of the single particle material.

Description

Pre-granulation method of graphite negative electrode material
Technical Field
The invention relates to the field of lithium ion battery cathode materials, in particular to a pre-granulation method of a graphite cathode material.
Background
The lithium ion battery has the advantages of high specific energy, high working voltage, high charging and discharging speed, long cycle life, safety, no pollution and the like, has successfully replaced other secondary batteries, becomes a main energy source of small electronic products such as mobile phones, notebook computers, video cameras and the like, greatly promotes the industrialization process of electric automobiles, and has comprehensively started the development of the lithium ion battery in the fields of military affairs and aerospace in many countries, so that higher requirements are put forward for the lithium ion battery. With the continuous development of science and technology, the requirements of 3C electronic consumer products and new energy automobiles on graphite cathode materials are higher, and especially the requirements of energy automobiles on high power and rapid charge and discharge are great.
The single-particle graphite anode material cannot meet the development requirements of the existing new energy industry, cannot meet the excellent performances of quick charge, high capacity and the like, and therefore modification treatment aiming at graphite has become a research hotspot in recent years.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides a pre-granulation method of a graphite negative electrode material having excellent properties.
The invention adopts the following technical scheme:
a pre-granulation method of a graphite negative electrode material comprises the following steps:
s1, processing the coal-based coke by a shaping machine to obtain primary particles;
s2, mixing the primary particles and asphalt through a mixer to obtain a mixture;
and S3, adding the mixture into a roller furnace, and obtaining different granulation results by utilizing different temperature rising curves.
In a further improvement of the above technical solution, in step S1, the shaping machine is a rolling, grinding and shaping integrated machine.
In a further improvement of the above technical solution, in the step S1, the coal-based coke is coal-based needle coke.
In a further improvement of the above technical solution, in the step S1, the volatile matter of the coal-based char is 5%.
In a further improvement of the above technical solution, in the step S1, the average particle diameter D50 of the primary particles is 8.0 μm.
In a further improvement of the above technical solution, in the step S2, the mixer is a V-type batch mixer.
In a further improvement of the above technical solution, in step S2, the rotation speed of the mixing is 250r/min, and the time of the mixing is 15 min.
In a further improvement of the above technical solution, in step S3, the specific temperature raising step is: raising the temperature from room temperature to 450 ℃ after 60 minutes, then preserving the heat at 450 ℃ for 30 minutes, raising the temperature to 500 ℃ after 30 minutes, preserving the heat for 120 minutes, raising the temperature to 520 ℃ after 20 minutes, preserving the heat for 30 minutes, finally reducing the temperature to 45 ℃, and discharging.
In a further improvement of the above technical solution, in step S3, the specific temperature raising step is: raising the temperature from room temperature to 450 ℃ after 60 minutes, then raising the temperature to 500 ℃ after 30 minutes, preserving the heat for 120 minutes, raising the temperature to 520 ℃ after 20 minutes, preserving the heat for 30 minutes, finally reducing the temperature to 45 ℃, and discharging.
The technical scheme is further improved in that in the step S3, the temperature is increased to 450 ℃ from room temperature after 60 minutes, the temperature is kept at 450 ℃ for 30 minutes, then the temperature is increased to 500 ℃ after 30 minutes, the temperature is increased to 520 ℃ after 20 minutes, the temperature is kept for 30 minutes, and finally the temperature is reduced to 45 ℃ to discharge.
The invention has the beneficial effects that:
the invention carries out temperature-rising curve treatment on the artificial graphite raw materials by different roller furnaces respectively, and then carries out blending treatment according to a certain proportion, thereby laying a cushion for obtaining a product which can give consideration to excellent charging and circulating performances of the secondary particle material and high tap density and high capacity performance of the single particle material.
Drawings
Fig. 1 is a scanning electron micrograph of a product of example 1 of a pre-granulation method of a graphite negative electrode material of the present invention;
fig. 2 is another scanning electron micrograph of the product of example 1 of the pre-granulation method for a graphite negative electrode material of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples for better understanding of the present invention, but the embodiments of the present invention are not limited thereto.
As shown in fig. 1 and 2, a pre-granulation method of a graphite negative electrode material includes the following steps:
s1, processing the coal-based coke by a shaping machine to obtain primary particles;
s2, mixing the primary particles and asphalt through a mixer to obtain a mixture;
and S3, adding the mixture into a roller furnace, and obtaining different granulation results by utilizing different temperature rising curves.
In the step S1, the shaping machine is a rolling, grinding and shaping integrated machine.
In step S1, the coal-based coke is coal-based needle coke.
In step S1, the coal-based char has a volatile content of 5%.
In the step S1, the average particle diameter D50 of the primary particles was 8.0 μm.
In the step S2, the mixer is a V-type batch mixer.
In the step S2, the rotation speed of the mixing is 250r/min, and the mixing time is 15 min.
In step S3, the specific temperature raising step is: raising the temperature from room temperature to 450 ℃ after 60 minutes, then preserving the heat at 450 ℃ for 30 minutes, raising the temperature to 500 ℃ after 30 minutes, preserving the heat for 120 minutes, raising the temperature to 520 ℃ after 20 minutes, preserving the heat for 30 minutes, finally reducing the temperature to 45 ℃, and discharging.
In step S3, the specific temperature raising step is: raising the temperature from room temperature to 450 ℃ after 60 minutes, then raising the temperature to 500 ℃ after 30 minutes, preserving the heat for 120 minutes, raising the temperature to 520 ℃ after 20 minutes, preserving the heat for 30 minutes, finally reducing the temperature to 45 ℃, and discharging.
In the step S3, the temperature is raised to 450 ℃ from room temperature after 60 minutes, the temperature is preserved for 30 minutes at 450 ℃, then the temperature is raised to 500 ℃ after 30 minutes, the temperature is raised to 520 ℃ after 20 minutes, the temperature is preserved for 30 minutes, finally the temperature is lowered to 45 ℃, and the material is discharged.
Example 1
Raw materials of the coal-based needle coke after passing through the rough breaking, shaping and grading integrated machine are put into a roller furnace, a temperature rise program is set, the temperature is raised from room temperature to 450 ℃ after 60 minutes, then the temperature is preserved for 30 minutes at 450 ℃, the temperature is raised to 500 ℃ after 30 minutes, then the temperature is preserved for 120 minutes, the temperature is raised to 520 ℃ after 20 minutes, the temperature is preserved for 30 minutes, finally the temperature is lowered to 45 ℃, and discharging is carried out.
Example 2
Raw materials of the coal-based needle coke after passing through the rough breaking, shaping and grading integrated machine are put into a roller furnace, a temperature rising program is set, the temperature rises from room temperature to 450 ℃ after 60 minutes, then the temperature rises to 500 ℃ after 30 minutes, the temperature is preserved for 120 minutes, then the temperature rises to 520 ℃ after 20 minutes, the temperature is preserved for 30 minutes, finally the temperature is reduced to 45 ℃, and discharging is carried out.
Example 3
And (3) putting raw materials of the coal-based needle coke after passing through the rough breaking, shaping and grading integrated machine into a roller furnace, setting a temperature raising program, raising the temperature from room temperature to 450 ℃ after 60 minutes, preserving the heat at 450 ℃ for 30 minutes, raising the temperature to 500 ℃ after 30 minutes, raising the temperature to 520 ℃ after 20 minutes, preserving the heat for 30 minutes, finally lowering the temperature to 45 ℃, and discharging.
The products of examples 1-3 were tested individually and the results are shown in Table 1.
TABLE 1
Experiment number D50 particle size/. mu.m Specific surface area/m2/kg Tap density/g/cm3
Example 1 17.87 0.98 1.01
Example 2 15.20 1.16 1.34
Example 3 13.46 1.43 1.52
The invention carries out temperature-rising curve treatment on the artificial graphite raw materials by different roller furnaces respectively, and then carries out blending treatment according to a certain proportion, thereby laying a cushion for obtaining a product which can give consideration to excellent charging and circulating performances of the secondary particle material and high tap density and high capacity performance of the single particle material.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The pre-granulation method of the graphite negative electrode material is characterized by comprising the following steps of:
s1, processing the coal-based coke by a shaping machine to obtain primary particles;
s2, mixing the primary particles and asphalt through a mixer to obtain a mixture;
and S3, adding the mixture into a roller furnace, and obtaining different granulation results by utilizing different temperature rising curves.
2. The pre-granulation method for the graphite anode material according to claim 1, wherein in the step S1, the shaping machine is a roll mill shaping machine.
3. The pre-granulation method for a graphite negative electrode material according to claim 1, wherein in step S1, the coal-based coke is a coal-based needle coke.
4. The pre-granulation method for a graphite negative electrode material according to claim 1, wherein in step S1, the coal-based char has a volatile content of 5%.
5. The pre-granulation method for a graphite anode material according to claim 1, wherein, in the step S1, the average particle diameter D50 of the primary particles is 8.0 μm.
6. The pre-granulation method for a graphite anode material according to claim 1, wherein in the step S2, the mixer is a V-type batch mixer.
7. The pre-granulation method for the graphite negative electrode material according to claim 1, wherein in the step S2, the rotation speed of the mixing is 250r/min, and the time of the mixing is 15 min.
8. The pre-granulation method for the graphite negative electrode material according to claim 1, wherein in the step S3, the specific temperature raising step is: raising the temperature from room temperature to 450 ℃ after 60 minutes, then preserving the heat at 450 ℃ for 30 minutes, raising the temperature to 500 ℃ after 30 minutes, preserving the heat for 120 minutes, raising the temperature to 520 ℃ after 20 minutes, preserving the heat for 30 minutes, finally reducing the temperature to 45 ℃, and discharging.
9. The pre-granulation method for the graphite negative electrode material according to claim 1, wherein in the step S3, the specific temperature raising step is: raising the temperature from room temperature to 450 ℃ after 60 minutes, then raising the temperature to 500 ℃ after 30 minutes, preserving the heat for 120 minutes, raising the temperature to 520 ℃ after 20 minutes, preserving the heat for 30 minutes, finally reducing the temperature to 45 ℃, and discharging.
10. The pre-granulation method for the graphite anode material according to claim 1, wherein in the step S3, the temperature is raised from room temperature to 450 ℃ over 60 minutes, the temperature is maintained at 450 ℃ for 30 minutes, then the temperature is raised to 500 ℃ over 30 minutes, the temperature is raised to 520 ℃ over 20 minutes, the temperature is maintained for 30 minutes, and finally the temperature is lowered to 45 ℃ to be discharged.
CN202111414756.7A 2021-11-25 2021-11-25 Pre-granulation method of graphite negative electrode material Pending CN114146635A (en)

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