CN113258063A - Method for preparing graphite cathode material of lithium ion battery by spray drying method - Google Patents
Method for preparing graphite cathode material of lithium ion battery by spray drying method Download PDFInfo
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- CN113258063A CN113258063A CN202110473593.3A CN202110473593A CN113258063A CN 113258063 A CN113258063 A CN 113258063A CN 202110473593 A CN202110473593 A CN 202110473593A CN 113258063 A CN113258063 A CN 113258063A
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- 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
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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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- 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
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- 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
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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 the technical field of preparation of lithium ion battery cathode materials, in particular to a method for preparing a lithium ion battery graphite cathode material by a spray drying method, which comprises the following steps: (1) preparing asphalt slurry: mixing asphalt with water and grinding into asphalt slurry; (2) preparing CMC glue solution: mixing CMC powder with water and stirring to prepare CMC glue solution; (3) pulping: mixing needle coke powder or petroleum coke powder or graphite powder, asphalt slurry, CMC glue solution and water to make slurry; (4) spray drying and granulating: spray drying the slurry by using spray drying equipment to obtain particles with the particle size of 15-20 um; (5) carbonizing and shaping: carbonizing the spray-dried particles by using a carbonization furnace; (6) and obtaining the negative electrode material after graphitization treatment. The method for preparing the graphite cathode material of the lithium ion battery by using the spray drying method provided by the invention adopts spray drying granulation, so that the preparation granularity is controllable, and shaping is not required; and the cost is saved.
Description
Technical Field
The invention relates to the technical field of preparation of lithium ion battery cathode materials, in particular to a method for preparing a lithium ion battery graphite cathode material by a spray drying method.
Background
The graphite material is considered to be an ideal negative electrode material of the lithium battery at present due to the advantages of high stability, good conductivity, wide source and the like. The traditional preparation process of the graphite negative electrode material comprises the following steps: (1) mixing needle-shaped coke powder or petroleum coke powder with asphalt; (2) using a high-temperature reaction kettle, preheating 180 ℃, adding the mixture, heating for 8-12 hours, and heating to 700 ℃; (3) discharging the materials into a cooling kettle, cooling for 6-8 h and cooling to 60 ℃; (4) shaping to a proper granularity; (5) and (6) graphitizing. The traditional process has uncontrollable granularity, needs shaping and is complex in process.
The publication number is CN110611100A, entitled method for reducing the specific surface area of a graphite cathode material of a lithium ion battery, and discloses that a graphite cathode raw material and low-temperature modified petroleum asphalt are added into a high-speed coating kettle to coat the surface of the graphite cathode raw material, and the process cannot control the particle size after coating.
Disclosure of Invention
The invention provides a method for preparing a graphite cathode material of a lithium ion battery by a spray drying method, aiming at solving the problems of uncontrollable granularity, shaping and complex process of the existing process.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for preparing a graphite cathode material of a lithium ion battery by a spray drying method comprises the following steps:
(1) preparing asphalt slurry: mixing asphalt powder with water, and then grinding the mixture by using a sand mill to prepare asphalt slurry, wherein the granularity of asphalt in the asphalt slurry is 600-700 nm; because the asphalt powder is insoluble in water and needs to be ground, asphalt slurry needs to be prepared in advance for later use when preparing slurry;
(2) preparing CMC glue solution: mixing CMC powder (also called carboxymethyl cellulose CMC) with water, and stirring to prepare CMC glue solution, wherein the stirring speed is 1200 r/min-1500 r/min, and the stirring time is 2 hours; because CMC powder is difficult to dissolve in water, the CMC powder needs to be dispersed in water in advance for standby when preparing glue solution;
(3) pulping: mixing any one of needle coke powder, petroleum coke powder or graphite powder, asphalt slurry, CMC glue solution and water, and stirring uniformly for later use; wherein the needle coke powder or the petroleum coke powder or the graphite powder are all commercial products, the particle sizes of the needle coke powder and the petroleum coke powder are 4-5 um, and the particle size of the graphite powder is 5-8 um;
(4) spray drying and granulating: spray drying the slurry uniformly stirred in the step (3) by using spray drying equipment to obtain particles with the particle size of 15-20 um;
(5) carbonizing and shaping: carbonizing the spray-dried particles by using a carbonization furnace to coke the asphalt, wherein the carbonization temperature is 550-650 ℃, and the carbonization time is 5 hours;
(6) graphitization: and putting the carbonized particles into a graphitization furnace for graphitization treatment to obtain the negative electrode material.
Further, the mass ratio of the asphalt powder to the water in the step (1) is 1 (4-7).
Further, the mass percentage of the CMC powder in the step (2) in the water is 1-2%.
Further, the graphite powder or needle coke powder or petroleum coke powder: asphalt powder: the mass ratio of the CMC powder is 1 (0.05-0.08) to 0.005-0.015; the graphite powder or the needle-shaped coke powder or the petroleum coke powder has the following quality: the ratio of the total mass of the water used in the steps (1), (2) and (3) is 1: (2.3-3.6).
Further, the parameters of the spray drying are:
rotating speed of the atomizer: 1200 r/min-1500 r/min;
slurry feed rate: 6 kg/min-10 kg/min;
rotating speed of the blower: 750 r/min-1200 r/min;
rotating speed of the induced draft fan: 750 r/min-1200 r/min;
temperature: the air inlet temperature of the spray drying tower is 600 ℃, the tower body temperature is 350 ℃ and the air outlet temperature is 125 ℃.
Further, the asphalt is low-temperature asphalt powder, namely coal asphalt with the softening point lower than 70 ℃.
Through the technical scheme, the invention has the beneficial effects that:
1. according to the method for preparing the graphite cathode material of the lithium ion battery by using the spray drying method, spray drying granulation is adopted, so that the preparation granularity is controllable, shaping is not needed, and the cost is reduced; compared with the method for preparing the graphite cathode material of the lithium ion battery in a reaction kettle by adopting a spray drying method, the method for preparing the graphite cathode material of the lithium ion battery reduces the environmental pollution.
2. The asphalt of the invention is low-temperature asphalt, and compared with petroleum coke and high-temperature asphalt coating granulation technology in the current market, the asphalt has low price. The asphalt has the following functions: a) the adhesive plays a role in the granulation processing process; b) the surface of graphite powder, needle coke powder or petroleum coke powder is coated and modified. The CMC has the functions as follows: a) the dispersing function is realized in the pulping process; b) after spraying, the adhesive has the function of adhesion.
Detailed Description
The invention will be further illustrated with reference to specific embodiments:
example 1
A method for preparing a graphite cathode material of a lithium ion battery by a spray drying method comprises the following steps:
(1) preparing asphalt slurry: mixing 25kg of asphalt powder with 100kg (or 100L) of water, and grinding for 2 hours by using a sand mill to prepare asphalt slurry, wherein the granularity of asphalt in the asphalt slurry is 600-700 nm;
(2) preparing CMC glue solution: mixing 2.5kg of CMC powder with 247.5kg (or 247.5L) of water, and stirring for 2h to prepare CMC glue solution, wherein the stirring speed is 1200 r/min;
(3) pulping: 500kg of needle coke powder, 125kg of asphalt slurry, 250kg of CMC glue solution and 1452.5kg of water are mixed for slurry preparation and are uniformly stirred for standby;
(4) spray drying and granulating: spray drying the slurry uniformly stirred in the step (3) by using spray drying equipment to obtain particles with the particle size of 15-17 um; the specific operation steps are as follows:
a) the rotation speed of a tower body induced draft fan is 750r/min, and the rotation speed of a tower body blower is 750 r/min;
b) open spraying oil pump cooling water, atomizer oil pump, atomizer, the atomizer rotational speed: 1200 r/min;
c) the air inlet temperature of the spray drying tower is 600 ℃, the tower body temperature is 350 ℃ and the air outlet temperature is 125 ℃;
d) slurry feed rate: 6 kg/min;
(5) carbonizing and shaping: and carbonizing the spray-dried particles by using a carbonization furnace to coke the asphalt, wherein the carbonization temperature is 550 ℃, and the carbonization time is 5 hours.
(6) Graphitization: and putting the carbonized particles into a graphitization furnace for graphitization treatment to obtain the negative electrode material. The graphitization step may be by any conventional graphitization step known in the art.
Example 2
A method for preparing a graphite cathode material of a lithium ion battery by a spray drying method comprises the following steps:
(1) preparing asphalt slurry: mixing 30kg of asphalt powder with 150kg (or 150L) of water, and then grinding for 2 hours by using a sand mill to prepare asphalt slurry, wherein the granularity of asphalt in the asphalt slurry is 600-700 nm;
(2) preparing CMC glue solution: mixing 5kg of CMC powder with 328kg (or 328L) of water, and stirring for 2 hours to prepare CMC glue solution, wherein the stirring speed is 1300 r/min;
(3) pulping: 500kg of needle-shaped coke powder, 180kg of asphalt slurry, 333kg of CMC glue solution and 1072kg of water are mixed for slurry preparation and are uniformly stirred for standby;
(4) spray drying and granulating: spray drying the slurry uniformly stirred in the step (3) by using spray drying equipment to obtain particles with the particle size of 17-19 um; the specific operation steps are as follows:
a) opening the tower body to induce wind at 850r/min and blower at 850 r/min;
b) open spraying oil pump cooling water, atomizer oil pump, atomizer, the atomizer rotational speed: 1300 r/min;
c) the air inlet temperature of the spray drying tower is 600 ℃, the tower body temperature is 350 ℃ and the air outlet temperature is 125 ℃;
d) slurry feed rate: 7.5 kg/min;
(5) carbonizing and shaping: and carbonizing the spray-dried particles by using a carbonization furnace to coke the asphalt, wherein the carbonization temperature is 650 ℃, and the carbonization time is 5 hours.
(6) Graphitization: and putting the carbonized particles into a graphitization furnace for graphitization treatment to obtain the negative electrode material.
Example 3
A method for preparing a graphite cathode material of a lithium ion battery by a spray drying method comprises the following steps:
(1) preparing asphalt slurry: mixing 35kg of asphalt powder with 210kg (or 210L) of water, and then grinding for 2 hours by using a sand mill to prepare asphalt slurry, wherein the granularity of asphalt in the asphalt slurry is 600-700 nm;
(2) preparing CMC glue solution: mixing 6kg of CMC powder with 327kg (or 327L) of water, and stirring for 2 hours to prepare CMC glue solution, wherein the stirring speed is 1400 r/min;
(3) pulping: 500kg of petroleum coke powder, 245kg of asphalt slurry, 333kg of CMC glue solution and 813kg of water are mixed for slurry preparation and are uniformly stirred for standby;
(4) spray drying and granulating: spray drying the slurry uniformly stirred in the step (3) by using spray drying equipment to obtain particles with the particle size of 15-17 um; the specific operation steps are as follows:
a) starting a tower body induced draft fan at the rotating speed of 1000r/min and a tower body blower at the rotating speed of 1000 r/min;
b) open spraying oil pump cooling water, atomizer oil pump, atomizer, the atomizer rotational speed: 1400 r/min;
c) the air inlet temperature of the spray drying tower is 600 ℃, the tower body temperature is 350 ℃ and the air outlet temperature is 125 ℃;
d) slurry feed rate: 9 kg/min;
(5) carbonizing and shaping: and carbonizing the spray-dried particles by using a carbonization furnace to coke the asphalt, wherein the carbonization temperature is 550 ℃, and the carbonization time is 5 hours.
(6) Graphitization: and putting the carbonized particles into a graphitization furnace for graphitization treatment to obtain the negative electrode material. The graphitization step may be by any conventional graphitization step known in the art.
Example 4
A method for preparing a graphite cathode material of a lithium ion battery by a spray drying method comprises the following steps:
(1) preparing asphalt slurry: mixing 40kg of asphalt powder with 280kg (or 280L) of water, and then grinding for 2 hours by using a sand mill to prepare asphalt slurry, wherein the granularity of asphalt in the asphalt slurry is 600-700 nm;
(2) preparing CMC glue solution: mixing 7.5kg of CMC powder with 375kg (or 375L) of water, and stirring for 2 hours to prepare CMC glue solution, wherein the stirring speed is 1500 r/min;
(3) pulping: 500kg of graphite powder, 320kg of asphalt slurry, 382.5kg of CMC glue solution and 495kg of water are mixed to prepare slurry, and the slurry is uniformly stirred for later use;
(4) spray drying and granulating: spray drying the slurry uniformly stirred in the step (3) by using spray drying equipment to obtain particles with the particle size of 18-20 um; the specific operation steps are as follows:
a) starting the rotation speed of a tower body induced draft fan at 1200r/min and the rotation speed of a tower body blower at 1200 r/min;
b) open spraying oil pump cooling water, atomizer oil pump, atomizer, the atomizer rotational speed: 1500 r/min;
c) the air inlet temperature of the spray drying tower is 600 ℃, the tower body temperature is 350 ℃ and the air outlet temperature is 125 ℃;
d) slurry feed rate: 10 kg/min;
(5) carbonizing and shaping: and carbonizing the spray-dried particles by using a carbonization furnace to coke the asphalt, wherein the carbonization temperature is 600 ℃, and the carbonization time is 5 hours.
(6) Graphitization: and putting the carbonized particles into a graphitization furnace for graphitization treatment to obtain the negative electrode material. The graphitization step may be by any conventional graphitization step known in the art.
The performances of the lithium ion battery graphite anode materials prepared by the spray drying method of the embodiments 1 to 4 of the invention are shown in table 1:
TABLE 1
The product produced by the invention basically meets the negative electrode materials of power batteries of electric tools and electric bicycles in the market, and compared with the existing negative electrode products in the market, the product supports multiplying power charging and discharging, and has low cost and low price.
The above-mentioned embodiments are merely preferred embodiments of the present invention, which are merely illustrative and not restrictive, and it should be understood that other embodiments may be easily implemented by those skilled in the art by means of replacement or modification according to the technical contents disclosed in the specification, and therefore, all changes and modifications that come within the spirit and technical conditions of the present invention should be included in the claims of the present invention.
Claims (7)
1. A method for preparing a graphite cathode material of a lithium ion battery by a spray drying method is characterized by comprising the following steps:
(1) preparing asphalt slurry: mixing asphalt powder with water, and then grinding the mixture by using a sand mill to prepare asphalt slurry, wherein the granularity of asphalt in the asphalt slurry is 600-700 nm;
(2) preparing CMC glue solution: mixing CMC powder with water, and stirring to prepare a CMC glue solution, wherein the stirring speed is 1200-1500 r/min, and the stirring time is 2 hours;
(3) pulping: mixing any one of needle coke powder, petroleum coke powder or graphite powder with asphalt slurry, CMC glue solution and water, and stirring uniformly for later use;
(4) spray drying and granulating: carrying out spray drying on the slurry uniformly stirred in the step (3) to obtain particles with the particle size of 15-20 um;
(5) carbonizing and shaping: carbonizing the spray-dried particles by using a carbonization furnace to coke the asphalt, wherein the carbonization temperature is 550-650 ℃, and the carbonization time is 5 hours;
(6) graphitization: and putting the carbonized particles into a graphitization furnace for graphitization treatment to obtain the negative electrode material.
2. The method for preparing the graphite negative electrode material of the lithium ion battery by the spray drying method according to claim 1, wherein the particle size of the needle coke powder is 4-5 um, the particle size of the petroleum coke powder is 4-5 um, and the particle size of the graphite powder is 5-8 um.
3. The method for preparing the graphite cathode material of the lithium ion battery by the spray drying method according to claim 1, wherein the mass ratio of the asphalt powder to the water in the step (1) is 1 (4-7).
4. The method for preparing the graphite negative electrode material of the lithium ion battery by the spray drying method according to claim 1, wherein the mass percentage of the CMC powder in the step (2) to the mass of the water is 1-2%.
5. The method for preparing the graphite negative electrode material of the lithium ion battery by the spray drying method according to claim 1, wherein the graphite powder or the needle-shaped coke powder or the petroleum coke powder: asphalt powder: the mass ratio of the CMC powder is 1 (0.05-0.08) to 0.005-0.015; the graphite powder or the needle-shaped coke powder or the petroleum coke powder has the following quality: the ratio of the total mass of the water used in the steps (1), (2) and (3) is 1: (2.3-3.6).
6. The method for preparing the graphite cathode material of the lithium ion battery by the spray drying method according to claim 1, wherein the parameters of the spray drying method are as follows:
rotating speed of the atomizer: 1200 r/min-1500 r/min;
slurry feed rate: 6 kg/min-10 kg/min;
rotating speed of the blower: 750 r/min-1200 r/min;
rotating speed of the induced draft fan: 750 r/min-1200 r/min;
temperature: the air inlet temperature of the spray drying tower is 600 ℃, the tower body temperature is 350 ℃ and the air outlet temperature is 125 ℃.
7. The method for preparing the graphite cathode material of the lithium ion battery by the spray drying method according to claim 1, wherein the asphalt powder is low-temperature asphalt powder.
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