CN113666368B - Artificial graphite negative electrode material and preparation method thereof - Google Patents
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Abstract
The invention provides an artificial graphite anode material and a preparation method thereof. According to the invention, the carbonaceous fine powder is dispersed in the asphalt, meanwhile, the asphalt distillate is used as a solvent to reduce the viscosity of the asphalt, the surface energy and the contact area of the carbonaceous fine powder and the asphalt are increased in the ball milling process, and the surface of the carbonaceous fine powder is preferably pre-oxidized, so that the carbonaceous fine powder is adsorbed with the asphalt mutually and is enabled to be uniformly dispersed in the asphalt. In the thermal polycondensation reaction, the carbon fine powder is used as a crystal nucleus center, the generated mesophase pellets are small in particle size and large in quantity, the viscosity of the system can be regulated by asphalt distillate, so that the asphalt distillate is fully grown and fused to form a plurality of small-domain and ordered fibrous shapes, the generated semicoke is needle coke with a short-range ordered small-piece structure, isotropy and strength of the cathode material are ensured, and a secondary granulating process can be omitted in the production of the cathode material.
Description
Technical Field
The invention relates to the technical field of lithium ion battery materials, in particular to an artificial graphite negative electrode material and a preparation method thereof.
Background
The lithium ion battery has a series of advantages of high specific capacity, high working voltage, good safety, no memory effect and the like, is widely applied to the fields of consumer electronics, electric automobiles, energy storage materials and the like, and along with the updating of consumer electronics products, the vigorous development of new energy automobile industry, the rapid popularization of intelligent power grids and the vigorous demand of other technical fields on high-performance batteries, the lithium ion battery industry is bound to continuously develop at a high speed in a long time in the future, and a great opportunity is provided for the development of lithium battery cathode material industry, but higher requirements are also provided.
The cathode material is an important component of the lithium ion battery, and the performance of the cathode material affects key indexes such as the safety, specific capacity, multiplying power performance, cycle life, high-low temperature performance and the like of the lithium ion battery, and is one of key materials of the lithium ion battery. The artificial graphite has good compatibility with electrolyte, good cycle performance and good rate capability, and is the preferred negative electrode material of the lithium ion battery. In particular, needle coke has been accepted in the industry because of its excellent properties such as ease of graphitization, high electrical conductivity, and low ash content. However, due to the streamline fiber structure of the needle coke, the needle coke is extremely easy to expand due to different orientation degrees in all directions after being assembled into a lithium ion battery, so that the rate performance is reduced and the cycle performance is deteriorated.
In order to improve isotropy of needle coke, the prior art is to crush large-particle needle coke into small particles, then bond the small particles together by using binders such as asphalt, and re-granulate to form large coke particles, thereby reducing orientation of the needle coke and improving multiplying power performance and cycle performance of artificial graphite. However, the process has the advantages of complex preparation process, high preparation cost and low tap density of the prepared artificial graphite.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the artificial graphite anode material and the preparation method thereof, wherein the method can omit a secondary granulation process in the production process of the artificial graphite anode material, can be used for embedding lithium ions in a plurality of directions and dispersing the lithium ions in all directions after being used for a lithium ion battery, can realize the effects of low raw material cost and simple process, and can prepare needle coke with a short-range ordered platelet structure, and the formed anode material has excellent isotropy, multiplying power performance and cycle performance.
The invention aims at realizing the following technical scheme:
the preparation method of the artificial graphite anode material comprises the following steps:
(1) Mixing the carbonaceous fine powder, the organic matters and the asphalt, and performing ball milling to obtain modified asphalt;
(2) Performing thermal polycondensation reaction on the modified asphalt obtained in the step (1) to obtain semicoke;
(3) Crushing, shaping and grading the semicoke obtained in the step (2) to obtain coke powder;
(4) Carbonizing the coke powder obtained in the step (3) to obtain cooked coke;
(5) And (3) graphitizing the cooked coke obtained in the step (4) at a high temperature, cooling, and scattering and screening the graphitized material to obtain the artificial graphite anode material.
According to the invention, in the step (1), the asphalt is selected from one or more compositions of petroleum asphalt, coal asphalt and petroleum residue, the softening point of the asphalt is 35-90 ℃, quinoline insoluble matters are less than 0.3wt%, and the particle size of the asphalt is 20-60 mu m.
According to the invention, in the step (1), the carbon fine powder is selected from one or more compositions of natural graphite, petroleum coke, needle coke and pitch coke, and D is 50 The grain diameter is 1-5 mu m.
According to the invention, in said step (1), said carbonaceous fines are pre-oxidized for 1-3 hours, preferably in an air atmosphere at 250-320 ℃ before mixing, the purpose of this operation being to form a rich surface functional group on the surface of the carbonaceous fines for mutual adsorption with pitch.
According to the invention, in the step (1), the organic matter is selected from one or more of the compositions of naphthalene oil, wash oil and anthracene oil.
According to the invention, in the step (1), the mass ratio of the carbonaceous fine powder to the organic matters to the asphalt is (1-10): (8-20): 100.
according to the invention, in the step (1), the temperature of the mixing is room temperature.
According to the present invention, in the step (1), the rotational speed of the ball milling and the time of the ball milling are not particularly defined as long as the uniform dispersion of the material can be ensured, i.e., the purpose of the ball milling is to uniformly disperse the carbonaceous fines in the pitch.
According to the invention, in the step (2), modified asphalt is added into an autoclave, nitrogen is introduced, then the temperature is raised to 420-460 ℃ at a heating rate of 1-5 ℃/min, the temperature is kept for 4-6 hours, the temperature is continuously raised to 480-540 ℃, the temperature is kept for 5-10 hours, the thermal polycondensation is carried out, and light oil gas generated in the system is utilized to pull coke in the thermal polycondensation process, so that semicoke is prepared; preferably, the reaction kettle is cooled to room temperature along with the temperature after the heat preservation is finished.
According to the invention, in the step (2), the thermal polycondensation is performed under a pressure of 0.2 to 0.5 MPa.
According to the invention, in the step (2), the semicoke is needle coke with a short-range ordered platelet structure.
According to the present invention, in the step (3), the operation process and equipment used in the operation of the pulverizing, shaping, classifying and the like are not particularly limited, and are known in the art. The equipment used for the pulverization may be exemplified by one selected from the group consisting of impact pulverizer, roll mill, ultra-micro ball mill, pendulum mill; the shaping equipment is selected from airflow vortex pulverizers; the equipment used for classification is selected from air classifiers.
According to the invention, in the step (3), the coke powder D 50 The grain diameter is 12-25 mu m.
According to the invention, in the step (4), the carbonization treatment temperature is 800-1300 ℃. The carbonization treatment is carried out for 1 to 6 hours, for example, 2 to 5 hours, and exemplary is carried out for 4 hours and 6 hours. Wherein the carbonization treatment is performed under the protection of an inert atmosphere, for example, the inert atmosphere is a nitrogen atmosphere or an argon atmosphere. Further, after the carbonization treatment is completed, the obtained product is naturally cooled.
According to the invention, in step (5), the graphitization temperature is 2800 to 3000 ℃, e.g. 2850 to 2950 ℃, exemplary 2800 ℃, 2900 ℃ or 3000 ℃. Further, the graphitization time is 2 to 10 hours, for example, 3 to 8 hours, and exemplary is 3 hours, 6 hours. Wherein, the graphitization can be performed by using a graphitization processing furnace.
According to the invention, the average particle diameter D of the artificial graphite anode material 50 Is 12-25 mu m.
According to the invention, the tap density of the artificial graphite anode material is more than or equal to 1.2g/cm 3 。
According to the invention, the first charge capacity of the artificial graphite anode material is more than or equal to 355mAh/g.
According to the invention, the capacity retention rate of the artificial graphite anode material at the normal temperature in a 1C charge-discharge cycle of 2000 weeks is more than 80%.
According to the invention, the expansion rate of the electrode plate of the artificial graphite anode material is less than or equal to 20% when the electrode is full.
The invention has the beneficial effects that:
the invention provides an artificial graphite anode material and a preparation method thereof. According to the invention, the carbonaceous fine powder is dispersed in asphalt, meanwhile, asphalt distillate (at least one of naphthalene oil, wash oil and anthracene oil) is used as a solvent to reduce the viscosity of the asphalt, the surface energy and contact area of the carbonaceous fine powder and the asphalt are increased in the ball milling process, and the surface of the carbonaceous fine powder is preferably pre-oxidized, so that the carbonaceous fine powder is mutually adsorbed with the asphalt and is enabled to be uniformly dispersed in the asphalt. In the thermal polycondensation reaction, the carbon fine powder is used as a crystal nucleus center, the generated mesophase pellets are small in particle size and large in quantity, the viscosity of the system can be regulated by asphalt distillate, so that the asphalt distillate is fully grown and fused to form a plurality of small-domain and ordered fibrous shapes, the generated semicoke is needle coke with a short-range ordered small-piece structure, isotropy and strength of the cathode material are ensured, and a secondary granulating process can be omitted in the production of the cathode material.
Compared with the existing negative electrode material, the artificial graphite negative electrode material prepared by the method has good isotropy, good cycle performance, high capacity and charge-discharge multiplying power, small expansion of the electrode in the process of absorption charge-discharge and stable product property.
Detailed Description
The preparation method of the present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; the reagents, materials, etc. used in the examples described below are commercially available unless otherwise specified.
Example 1
Natural crystalline flake graphite (D) 50 3 μm) was oxidized in an air atmosphere at 300℃for 1.5 hours and cooled to room temperature to give a modified natural crystalline flake graphite. 1g of modified natural crystalline flake graphite, 10g of wash oil and 100g of coal pitch (softening point 60 ℃ C., quinoline insoluble matter 0.1wt%, D) 50 100 μm), and then starting the ball milling tank to start ball milling for 6 hours under the condition of 1200r/min rotation speed to obtain the modified asphalt.
Adding the modified asphalt into an autoclave, introducing nitrogen, heating to 430 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 4.5 hours, continuously heating to 520 ℃, keeping the temperature for 8 hours, performing high-temperature thermal polycondensation reaction, and cooling to room temperature along with the temperature of the autoclave after the heat preservation is finished, thus obtaining the semicoke.
Crushing semicoke in an impact crusher, shaping in a vortex crusher, and classifying by an air classifier to obtain average particle size D 50 17 μm coke breeze. At N 2 And (3) treating for 4 hours at the temperature of 1200 ℃ under the protection to obtain the cooked coke. And then graphitizing at 2800 ℃ for 12 hours, cooling to room temperature, scattering and screening to obtain the artificial graphite anode material.
Example 2
Needle coke (D) 50 1.5 μm) was oxidized in an air atmosphere at 270℃for 2 hours and then cooled to room temperature to obtain a modified needle coke. 2g of modified needle coke, 15g of wash oil and 100g of petroleum asphalt (softening point 45 ℃ C., quinoline insoluble matter 0.1wt%, D) 50 140 μm), and then starting the ball milling tank to start ball milling for 8 hours under the condition of 780r/min rotation speed to obtain the modified asphalt.
Adding the modified asphalt into an autoclave, introducing nitrogen, heating to 450 ℃ at a heating rate of 3 ℃/min under the pressure of 0.3MPa, keeping the temperature for 3 hours, continuously heating to 510 ℃, keeping the temperature for 10 hours, performing high-temperature thermal polycondensation reaction, and cooling to room temperature along with the temperature of the autoclave after the heat preservation is finished, so as to obtain the semicoke.
Crushing semicoke in an impact crusher, shaping in a vortex crusher, and classifying by an air classifier to obtain average particle size D 50 Is coke powder of 14 μm. At N 2 And (3) treating for 6 hours at 1100 ℃ under protection to obtain cooked coke. Graphitizing at 3000 deg.c for 6 hr, cooling to room temperature, scattering and sieving to obtain the final productAnd (5) manufacturing a graphite cathode material.
Example 3
Petroleum coke (D) 50 2 μm) was oxidized in an air atmosphere at 300 c for 1.0 hour and cooled to room temperature to obtain modified petroleum coke. 3g of modified petroleum coke, 16g of wash oil and 100g of coal tar pitch (softening point 75 ℃ C., quinoline insoluble matter 0.1wt%, D) 50 180 μm), and then starting the ball milling tank to start ball milling, wherein the ball milling time is 7 hours under the condition of 1120r/min of rotating speed, thus obtaining the modified asphalt.
Adding the modified asphalt into an autoclave, introducing nitrogen, heating to 460 ℃ at a heating rate of 4 ℃/min under the pressure of 0.3MPa, keeping the temperature for 4 hours, continuously heating to 500 ℃, keeping the temperature for 6 hours, performing high-temperature thermal polycondensation reaction, and cooling to room temperature along with the temperature of the autoclave after the heat preservation is finished, so as to obtain the semicoke.
Crushing semicoke in an impact crusher, shaping in a vortex crusher, and classifying by an air classifier to obtain average particle size D 50 Is 18 μm coke powder. At N 2 And (3) treating for 4 hours at the temperature of 1200 ℃ under the protection to obtain the cooked coke. And then graphitizing at 3000 ℃ for 8 hours, cooling to room temperature, scattering and screening to obtain the artificial graphite anode material.
Comparative example 1
Coal pitch (softening point 60 ℃ C., quinoline insoluble content 0.1wt%, D) 50 100 μm), introducing nitrogen, heating to 430 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 4.5h, continuously heating to 520 ℃ and keeping the temperature for 8h, performing high-temperature thermal polycondensation reaction, and cooling to room temperature along with the temperature of the reaction kettle after the heat preservation is finished, thus obtaining the semicoke.
Crushing semicoke in an impact crusher, shaping in a vortex crusher, and classifying by an air classifier to obtain average particle size D 50 17 μm coke breeze. At N 2 And (3) treating for 4 hours at the temperature of 1200 ℃ under the protection to obtain the cooked coke. Then graphitizing at 3000 ℃ for 6 hours, cooling to room temperature, scattering and screening to obtain the artificial graphite anode material.
The physicochemical indexes of the above examples 1 to 3 and comparative example 1 were tested as follows:
(1) Average particle size test
The sample was tested for particle size distribution using a laser particle sizer and the average particle size obtained from the test is shown in table 1.
(2) Isotropy test
The microstructure of the negative electrode material was observed using a polarizing microscope, and the isotropy ratio obtained by the test is shown in table 1.
(3) Electrochemical performance test
(3-1) half-test method:
the graphite negative electrode materials prepared in examples 1 to 3 and comparative example 1 were uniformly mixed with conductive carbon black (SP) carboxymethylcellulose (CMC) Styrene Butadiene Rubber (SBR) =95:1:1.5:2.5 (mass ratio), coated on copper foil, and the coated electrode sheet was dried in a vacuum oven at 120 ℃ for 12 hours. Simulated battery assembly was performed in an argon-protected Braun glove box with electrolyte 1M-LiPF 6 +EC: DEC: DMC (volume ratio: 1:1:1), metal lithium sheet as counter electrode, and simulation battery test was conducted in a 5V, 10mA New Wei battery test cabinet, charging and discharging voltage was 0.01-1.5V, charging and discharging rate was 0.1C, and the first reversible charging capacity obtained by the test was shown in Table 1.
(3-2) full battery test method:
the graphite materials prepared in examples 1-3 and comparative example 1 were used as negative electrodes, lithium cobaltate was used as positive electrode, and 1M-LiPF 6 The +EC:DEC:DMC (volume ratio 1:1:1) solution was used as an electrolyte to assemble a full cell, which was charged and discharged at normal temperature at a rate of 0.5C and 1C, with a voltage range of 3.0-4.2V, and the cycle properties obtained by the test were shown in Table 1.
(3-3) method for testing expansion rate of pole piece when full electrode:
the battery cell was charged to 100% soc at 0.2C, the battery cell was disassembled under low temperature and low humidity conditions, the thickness of the negative electrode sheet was tested, and the expansion ratio of the electrode sheet obtained by the test was compared with the thickness of the electrode sheet after rolling and is shown in table 1.
Table 1 results of physical and chemical properties and electrochemical properties of artificial graphite anode materials of examples and comparative examples
The meaning of the "-" expression is that the capacity retention is less than 80%, indicating a failure of the battery.
As can be seen from table 1, the artificial graphite anode material prepared according to the present invention is better in rate performance and cycle performance than comparative example 1. In addition, the secondary granulation process is omitted in the preparation process of the artificial graphite anode material, the preparation process is simple, the cost is low, the practicability is high, and the method is suitable for lithium ion batteries for mobile electronic equipment such as mobile phones and digital cameras and power lithium ion batteries for electric vehicles, so that the cost is greatly reduced.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The preparation method of the artificial graphite anode material comprises the following steps:
(1) Mixing the carbonaceous fine powder, the organic matters and the asphalt, and performing ball milling to obtain modified asphalt;
(2) Performing thermal polycondensation reaction on the modified asphalt obtained in the step (1) to obtain semicoke;
(3) Crushing, shaping and grading the semicoke obtained in the step (2) to obtain coke powder;
(4) Carbonizing the coke powder obtained in the step (3) to obtain cooked coke;
(5) Performing high-temperature graphitization on the cooked coke obtained in the step (4), cooling, and scattering and screening graphitized materials to obtain the artificial graphite anode material;
in the step (1), the organic matter is selected from one or more compositions of naphthalene oil, wash oil and anthracene oil;
in the step (1), the carbonaceous fine powder is oxidized in advance for 1 to 3 hours in an air atmosphere at the temperature of 250 to 320 ℃ before being mixed;
in the step (2), the thermal polycondensation reaction is to add modified asphalt into an autoclave, introduce nitrogen, then heat up to 420-460 ℃ at a heating rate of 1-5 ℃/min, keep the temperature for 4-6 h, then continue heating up to 480-540 ℃ and keep the temperature for 5-10 h;
in the step (2), the thermal polycondensation reaction is carried out under the condition that the pressure is 0.2-0.5 MPa.
2. The method according to claim 1, wherein in the step (1), the asphalt is one or more selected from petroleum asphalt, coal asphalt, petroleum residue, the asphalt has a softening point of 35-90 ℃, quinoline insoluble content of less than 0.3wt%, and the asphalt has a particle size of 20-60 μm.
3. The method of claim 1, wherein in step (1), the carbonaceous fines are selected from one or more of natural graphite, petroleum coke, needle coke, pitch coke, and D 50 The grain diameter is 1-5 mu m.
4. The method of claim 1, wherein in the step (1), the mass ratio of the carbonaceous fines, the organic matter and the pitch is (1-10): (8-20): 100.
5. the method of claim 1, wherein in step (3), said coke powder D 50 The grain diameter is 12-25 mu m;
in the step (4), the carbonization treatment temperature is 800-1300 ℃; the carbonization treatment time is 1-6 hours;
in the step (5), the graphitization temperature is 2800-3000 ℃, and the graphitization time is 2-10 hours.
6. The method according to any one of claims 1 to 5, wherein the artificial graphite anode material has an average particle diameter D 50 Is 12-25 mu m; the tap density of the artificial graphite anode material is more than or equal to 1.2g/cm 3 。
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| CN114525153A (en) * | 2022-02-14 | 2022-05-24 | 深圳市翔丰华科技股份有限公司 | Preparation method of isotropic coke for lithium ion battery cathode material |
| CN115477301A (en) * | 2022-09-19 | 2022-12-16 | 力神（青岛）新能源有限公司 | Preparation method of energy storage long-cycle graphite negative electrode material |
| CN115806289A (en) * | 2022-11-29 | 2023-03-17 | 江西紫宸科技有限公司 | Graphite negative electrode material with long cycle life and preparation method and application thereof |
| CN116120079B (en) * | 2023-01-12 | 2023-11-10 | 四川宇星碳素有限公司 | Manufacturing method of porous graphite separator for growing silicon carbide crystal by physical vapor transport method |
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