CN112645318A - Method for preparing artificial graphite cathode material by using resistance material - Google Patents
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Abstract
The invention discloses a method for preparing an artificial graphite negative electrode material by using a resistance material, the artificial graphite negative electrode material which is not subjected to graphitization and is obtained by the method, and a lithium battery prepared from the artificial graphite negative electrode material. The method of the invention improves the tap density of the resistance material in the preparation process of the artificial graphite by crushing and shaping, and meets the use requirement of the artificial graphite by removing electromagnetism, and the method does not need high cost and time-consuming graphitization. Thereby obtaining the battery with the performance close to that of the artificial graphite, and the battery manufactured by the artificial graphite has the performance close to that of the battery manufactured by the common artificial graphite.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery cathode materials, and particularly relates to a method for preparing an artificial graphite cathode material by using a resistance material.
Background
Along with the development of the industry in the modern society, a great deal of fossil fuel is burned, and along with the increase of energy crisis and environmental pollution, the energy crisis is and the environmental pollution are increased. Therefore, the fuel vehicle sale prohibition schedule is released in all developed countries around the world, China can comprehensively prohibit fuel vehicles in 2040 years, and all countries are vigorously developing new energy vehicles. Meanwhile, the development of lithium ion secondary batteries is becoming more important due to the spread of various portable electronic devices and electric tools. Among them, the negative electrode material is an important constituent of the lithium ion secondary battery. The artificial graphite cathode material has the following advantages in various cathode materials (1) wide graphite source and abundant reserves; (2) the tap density is higher after modification; (3) the electrochemical performance is stable; (4) the actual specific capacity density can be close to the theoretical specific capacity. At present, the development direction of the artificial graphite cathode material is the improvement of the quick charging performance and the development of low-cost products. Particularly in the aspect of low-cost finished product development, 3 thousands of prices and 350 capacities are currently used as bidding standards by various power battery enterprises. The cost reduction pressure is great for various existing products, and therefore, the development of products with both high performance and low cost is the key point.
CN201810939044.9 (acid-washing method for purifying artificial graphite pore-forming negative electrode material of resistance material) removes impurities in the middle of the resistance material by using an acid-washing method, so that the artificial graphite negative electrode material is prepared by using the resistance material, however, the acid-washing method is complex in steps and is not environment-friendly. In addition, the existing artificial graphite production process needs to perform graphitization (price of 1.2-1.6 ten thousand per ton) with high price for a long period (shortest 30 days) anyway, and is not beneficial to greatly reducing the cost.
Disclosure of Invention
The invention provides a method for preparing an artificial graphite cathode material by using a resistance material and the artificial graphite cathode material prepared by the method, aiming at solving the defects that the artificial graphite in the prior art is too high in cost, the resistance material treatment method is backward and the artificial graphite cathode material cannot be used for industrial production. In the prior art, resistance materials are utilized for acidification treatment and are used for preparing the negative electrode material, but the process is laggard, and the prepared negative electrode material cannot be converted and applied to large-scale industrial production. Under the background, the inventors unexpectedly found that the negative electrode material prepared by removing the magnetic substance (the content of the magnetic substance is less than 3ppm, preferably 0.2-1.5 ppm) in the resistor material by using the resistor material at the lower layer in the same furnace, removing fine powder from the resistor material, shaping, and preparing a lithium battery such as a lithium battery of a two-wheeled vehicle. Specifically, the invention provides an artificial graphite cathode material which meets the requirement of 350mAh/g and achieves low cost of 2 ten thousand yuan. The artificial graphite prepared by the method not only has the advantage of extremely low cost, but also has the characteristics of high capacity and high efficiency, and in addition, the artificial graphite prepared by the method also has high dynamic performance.
In order to solve the above technical problems, one of the technical solutions of the present invention is: the method for preparing the artificial graphite cathode material by using the resistance material comprises the following steps:
(1) removing fine powder from the resistance material crushed by the crusher through a shaping machine, and improving the sphericity to obtain the shaped resistance material, wherein Dmin is more than or equal to 2.0 mu m, and D50 is 16.0-19.0 mu m;
(2) passing the shaped resistance material through an electromagnetic demagnetizer to obtain the resistance material with the magnetic substances removed, wherein the content of the magnetic substances is less than 3ppm, preferably 0.2-1.5 ppm, and more preferably 0.2-0.5 ppm;
(3) adding the resistance material without the magnetic substances into a mixer for mixing to obtain a mixed resistance material;
(4) coating asphalt on the surface of the mixed resistance material, and carbonizing in a carbonization furnace to obtain a carbonized resistance material;
(5) mixing the carbonized resistance material by a mixer to obtain an artificial graphite negative electrode material with the granularity D50 of 16.0-20.0 microns;
preferably, the crushed electric resistance material in the step (1) further comprises the following steps before crushing:
(0) the method comprises the steps of roughly crushing a resistance material raw material by a rough crusher to obtain a roughly crushed resistance material, wherein the average particle size D50 of the roughly crushed resistance material is 100-200 mu m; preferably, the resistance material raw material is produced by a graphitizing crucible furnace, and more preferably, the resistance material raw material is a lower layer resistance material in the same furnace resistance material.
In the present invention, the resistance material from which the magnetic substance is removed contains a small amount of the magnetic substance due to the limitation of the demagnetization technique. As long as the content of the magnetic substance is <3ppm, it can be considered that the magnetic substance is removed.
In some preferred specific embodiments, the raw material of the electric resistance material is petroleum coke, and/or the diameter of the raw material of the electric resistance material is 2-10 cm. Preferably, the coarse crusher is a double-roller jaw crushing integrated machine, and/or the crusher is a mechanical mill 500.
In some preferred embodiments, in the step (1), the average particle size D50 of the crushed electric resistance material is 14.0-19.0 μm, and the tap of the shaped electric resistance material is 0.85-1.0 g/cm 3; the shaper is preferably an intermittent shaper 800 or a ball-type shaper 60.
In some preferred embodiments, in step (2), the electromagnetic demagnetizer is an electromagnetic demagnetizer DVMF50, and/or the magnetic substance content of the magnetic substance removing electric resistance material is 0.2 ppm.
In some preferred embodiments, in the step (3), the mixing time is 20 to 80 minutes, preferably 40 minutes, and/or the mixing speed is 20 HZ.
In some preferred embodiments, in the step (4), the ratio of the mixed resistance material to the asphalt is 100 (3-10), preferably 100: 3; the rotating speed of the equipment for coating the asphalt is 10-30 HZ, preferably 20HZ, and/or the coating time is 1-3 hours, preferably 2 hours; preferably, the equipment is a horizontal coating kettle WHR-500L.
In some preferred embodiments, in step (4), the carbonization is performed by heating in a calcination apparatus under an inert atmosphere; preferably, the carbonization is as follows: processing for 6-20 hours at the constant temperature of 900-1300 ℃; preferably, the treatment is carried out at a constant temperature of 1150-1200 ℃ for 10 hours.
In some preferred embodiments, in steps (3) and (5), the mixer is a high-efficiency wire rod mixer GPH-P-1.5P/C; preferably, in the step (5), the tap density of the artificial graphite cathode material is more than or equal to 0.85g/cm3Preferably 0.87g/cm or more3(ii) a The specific surface area is 1.0-4.0 m2(ii)/g; the discharge capacity is more than or equal to 353.0 mAh/g; and/or the first efficiency is more than or equal to 90.5 percent.
In order to solve the above technical problems, the second technical solution of the present invention is: there is provided an artificial graphite negative electrode material obtained by the method as described in any of the above without undergoing graphitization.
In order to solve the above technical problems, the third technical solution of the present invention is: providing a lithium battery, wherein the negative electrode of the lithium battery contains the artificial graphite negative electrode material; preferably, the lithium battery is used for a two-wheel vehicle.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
Compared with the prior art, the invention has the positive improvement effects that:
the low-cost lithium ion battery composite graphite cathode material prepared by the method can meet the requirement of 350 mAh/g; the tap density is higher and is more than 0.87g/cm3Easy to process; the coating of asphalt is provided, and the dynamic performance of the material is improved; without the need for costly and time-consuming graphitization. The artificial graphite cathode material prepared by the method has the advantages of short process route, simple process, easy mass production, low cost of the resistance material and stable source, and can be applied to power lithium batteries for motorcycles.
Drawings
FIG. 1 is a powder field emission scanning electron microscope of the artificial graphite anode material of example 1;
FIG. 2 is an AC impedance spectrum of the artificial graphite prepared in example 1, example 2, comparative example 1 and comparative example 2;
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
The average particle size and the particle size distribution are measured by a laser particle size distribution instrument MS 2000.
The equipment, manufacturer and model used in the invention are shown in the following table:
example 1
The embodiment is a method for preparing a low-cost lithium ion battery cathode material. The method comprises the following specific steps:
(1) the resistance material (the diameter is 2-10 cm) generated by the graphitizing crucible furnace is coarsely crushed by a coarse crusher (a double-roller jaw crushing integrated machine), and the average particle size D50 is 100.0-200.0 μm.
(2) And (2) crushing the coarsely crushed graphitized resistor material obtained in the step (1) by a crusher (mechanical mill 500), wherein the average particle size D50 is 14.0-19.0 μm.
(3) Removing fine powder from the crushed resistance material obtained in the step (2) through a shaping machine (an intermittent shaping machine 800) to improve the sphericity so as to improve the tap density, wherein Dmin is more than or equal to 2.0 mu m, the average particle size D50 is 16.0-19.0 mu m, and the tap density is 0.85-1.0 g/cm3。
(4) And (4) removing magnetic substances from the shaped resistance material obtained in the step (3) through an electromagnetic demagnetizer DVMF50-6, wherein the total amount of the magnetic substances is 0.2-0.5 ppm.
(5) And (5) adding the demagnetized resistance material obtained in the step (4) into a high-efficiency wire rod test mixer GPH-P-1.5P/C for mixing to improve the uniformity of the material, wherein the mixing rotating speed is 20HZ, and the mixing time is 40 minutes.
(6) And (3) adding the resistance material obtained in the step (5) into high-temperature asphalt, and coating the asphalt in a horizontal coating kettle, wherein the asphalt is coated on the surface of the resistance material, and the ratio of the resistance material to the asphalt is 100: 3. The rotating speed of the horizontal coating kettle is 20 HZ; the treatment time of the horizontal coating kettle was 2 hours. The treatment temperature of the horizontal coating kettle is normal temperature.
(7) And (4) carbonizing the resistance material coated with the asphalt in the step (6) in a carbonization furnace in nitrogen atmosphere, wherein the conventional treatment in the field is to keep the temperature of 900-1300 ℃ for 6-20 hours, and the experiment is to keep the temperature of 1200 ℃ for 10 hours.
(8) And (3) mixing the carbonized carbon resistor material obtained in the step (7) to obtain an artificial graphite material with the particle size D50 of 16.0-20.0 micrometers (the average particle size is 18.5 micrometers). The tap density of the obtained graphite negative electrode material is 0.95g/cm3Specific surface area of 2.5m2The magnetic material content is 0.2ppm, the discharge capacity is 354.5mAh/g, the first efficiency is 91.5 percent, and the cycle capacity retention rate is 94.3 percent at 1C/1C 500 cycle.
Example 2
The present embodiment is different from embodiment 1 in that: the crushing equipment used in the step (2): and (3) replacing the mechanical mill 500 and the 800 shaping machine used in the step (3) by 60-ball shaping equipment, wherein the Dmin of the resistance material is more than or equal to 2.0 mu m, the ratio of the resistance material to the asphalt is 100:3, and the rest is unchanged. The average grain diameter D50 of the graphite of the electric resistance material coating product is 16.0-19.0 mu m, and the tap density is 0.87g/cm3A specific surface area of 4.0m2The magnetic material content is 1.5ppm, the discharge capacity is 353.1mAh/g, the first efficiency is 90.5 percent, and the cycle capacity retention rate is 92.1 percent at 1C/1C 500 cycles.
Comparative example 1
This comparative example differs from example 1 in that: and (4) removing the 800 shaping machine used in the step (3), and keeping the rest unchanged. The average grain diameter D50 of the graphite of the electric resistance material coating product is 15.0-19.0 mu m, and the tap density is 0.70g/cm3Specific surface area of 7.5m2The magnetic material content is 0.5-1.5ppm, the discharge capacity is 352.5mAh/g, the first efficiency is 89.5 percent, and the circulation capacity retention rate of 1C/1C for 500 weeks is 85.3 percent.
Comparative example 2
This comparative example differs from example 1 in that: and (4) removing the demagnetizing process used in the step (4), and keeping other processes unchanged. The artificial graphite material with the granularity D50 of 16.0-20.0 μm is obtained. The tap density of the obtained graphite negative electrode material is 0.95g/cm3Specific surface area of 2.5m2The magnetic material content is 10.0ppm, the discharge capacity is 351.5mAh/g, the first efficiency is 91.5 percent, and the cycle capacity retention rate is 60.3 percent at 1C/1C 500 cycles.
Effects of the embodiment
The artificial graphites obtained in examples 1 and 2 and comparative example 1 were respectively subjected to particle size, tap density, specific surface area and the like, and the results are shown in table 1. The name and model of the instrument used for the test are as follows: particle size, laser particle size distribution instrument MS 3000; ash content, tap density, tap instrument TF-100B; specific surface area, specific surface area determinator NOVATouch 2000; compacted Density, FT-100F powder Autodensitometer compacted.
The half cell test method comprises the following steps: weighing a graphite sample, conductive carbon black SP, CMC and SBR according to a mass ratio of 95.6:1.0:1.1:2.3, uniformly stirring in water to prepare negative electrode slurry, coating the negative electrode slurry on two sides of a copper foil by using a coater, putting a pole piece coated on the two sides into a vacuum drying oven at the temperature of 110 ℃ for vacuum drying for 4 hours, and then pressing the pole piece to prepare the negative electrode. Wherein the compacted density is the surface density/(the thickness of the rolled pole piece-the thickness of the current collector). The CR-2430 type button cell is assembled in an argon-filled Michelona glove box, the electrolyte is 1M LiPF6+ EC: EMC: DMC ═ 1: 1(V: V: V), the negative electrode of the counter electrode is metal, the voltage interval of a charge-discharge test on a blue cell test cabinet is 0.005-1.0V, and the charge-discharge multiplying factor is 0.1C.
The test voltage range is 0.005-1.0V when the multiplying power, the direct current impedance and the alternating current impedance are tested on an ArbinBT2000 battery tester.
Table 1 materials powders and electrochemical performance test results:
both example 1 and example 2 have a larger tap and a greatly reduced BET relative to comparative example 1. This is because the electric resistance material in examples 1 and 2 has a shaping process after being crushed, and the shaping process can remove fine powder and burrs on the particle surface, modify the particle surface, and simultaneously make the material denser, which leads to larger tap and greatly reduced BET in examples 1 and 2.
Meanwhile, due to the improvement of tap and the reduction of BET, the capacities of the embodiment 1 and the embodiment 2 are higher, and the first coulombic efficiency is also higher, because the larger BET of the comparative example 1 consumes more electrolyte and lithium ions, so that the efficiency is lower, the 500-week cycle capacity retention rate of 1C/1C is further lower than that of the comparative example 1 and the comparative example 2.
On the other hand, compared with examples 1 and 2, since comparative example 2 was not demagnetized, the content of the magnetic substance was as high as-10 ppm, and the use requirement of the artificial graphite could not be satisfied. Meanwhile, in the 500-week cycle capacity retention rate result of further 1C/1C, the capacity retention rate of the comparative example 2 is greatly attenuated to 60.3%, and the possible reason is that the content of the magnetic substance is too high, so that excessive side reactions are caused, and capacity diving is caused in the cycle process.
As can be seen from the SEM image of example 1 in FIG. 1, the artificial graphite anode material prepared in example 1 has smooth and flat surface and no burr on the surface of the particles, which results in the highest tap density in example 1.
Table 2 discharge rate data for example 1, example 2 and comparative example 1
| Serial number | 0.1C/0.1C | 0.2C/0.1C | 0.5C/0.1C | 1C/0.1C | 2C/0.1C | 3C/0.1C |
| Example 1 | 98.1％ | 95.3％ | 80.8％ | 60.1％ | 23.9％ | 10.2％ |
| Example 2 | 98.0％ | 94.6％ | 76.1％ | 54.1％ | 18.6％ | 6.4％ |
| Comparative example 1 | 96.7％ | 92.9％ | 73.7％ | 45.9％ | 10.1％ | 4.0％ |
| Comparative example 2 | 97.1％ | 96.3％ | 78.8％ | 53.1％ | 18.9％ | 9.2％ |
Fig. 2 is an ac impedance profile of example 1, example 2, comparative example 1 and comparative example 2. It is obvious that compared with comparative examples 1 and 2, the alternating current resistance of the materials in examples 1 and 2 is smaller, which shows that the charge transfer resistance of the resistance material is reduced after the shaping process and the demagnetizing process, and the materials have good dynamic performance. While the impedance of example 1 is minimal, indicating the best material dynamics of example 1.
Rate capability data of the artificial graphite prepared in example 1, example 2, comparative example 1 and comparative example 2 are provided in table 2. It can be clearly seen that examples 1, 2 and 2 have better cross-rate performance than comparative example 1, which indicates that the interface contact between material particles is better after the shaping process of the resistance material, that the artificial graphite negative electrode material after the shaping of the resistance material and the asphalt coating carbonization has good dynamic performance, and that the rate performance of the resistance material without demagnetization has no obvious change in the rate test of several weeks, but the test results of table 1 indicate that the demagnetization process has little influence on the short-term rate, but the capacity of the resistance material in a long cycle has a large water skip and a great safety problem. At the same time, the rate capability of example 1 is the best, indicating that example 1 is the best process. Thus, the processes of example 1 and example 2 can be used as the negative electrode material of the two-wheeled vehicle power lithium ion secondary battery.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments disclosed and described, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Claims (10)
1. A method for preparing an artificial graphite negative electrode material by using a resistance material is characterized by comprising the following steps:
(1) removing fine powder from the resistance material crushed by the crusher through a shaping machine, and improving the sphericity to obtain the shaped resistance material, wherein Dmin is more than or equal to 2.0 mu m, and D50 is 16.0-19.0 mu m;
(2) passing the shaped resistance material through an electromagnetic demagnetizer to obtain the resistance material with the magnetic substances removed, wherein the content of the magnetic substances is less than 3ppm, preferably 0.2-1.5 ppm, and more preferably 0.2-0.5 ppm;
(3) adding the resistance material without the magnetic substances into a mixer for mixing to obtain a mixed resistance material;
(4) coating asphalt on the surface of the mixed resistance material, and carbonizing in a carbonization furnace to obtain a carbonized resistance material;
(5) mixing the carbonized resistance material by a mixer to obtain an artificial graphite negative electrode material with the granularity D50 of 16.0-20.0 microns;
preferably, the crushed electric resistance material in the step (1) further comprises the following steps before crushing:
(0) the method comprises the steps of roughly crushing a resistance material raw material by a rough crusher to obtain a roughly crushed resistance material, wherein the average particle size D50 of the roughly crushed resistance material is 100-200 mu m; preferably, the resistance material raw material is produced by a graphitizing crucible furnace, and more preferably, the resistance material raw material is a lower layer resistance material in the same furnace resistance material.
2. The method according to claim 1, wherein the raw material of the electric resistance material is petroleum coke and/or the diameter of the raw material of the electric resistance material is 2-10 cm; preferably, the coarse crusher is a double-roller jaw crushing integrated machine, and/or the crusher is a mechanical mill 500.
3. The method of claim 1, wherein: in the step (1), the average grain diameter D50 of the crushed resistance material is 14.0-19.0 mu m, and the tap of the shaped resistance material is 0.85-1.0 g/cm3(ii) a The shaper is preferably an intermittent shaper 800 or a ball-type shaper 60.
4. The method of claim 1, wherein: in the step (2), the electromagnetic demagnetizer is an electromagnetic demagnetizer DVMF50, and/or the content of the magnetic substance in the resistance material from which the magnetic substance is removed is 0.2 ppm.
5. The method of claim 1, wherein: in the step (3), the material mixing time is 20-80 minutes, preferably 40 minutes, and/or the material mixing speed is 20 HZ.
6. The method of claim 1, wherein: in the step (4), the ratio of the mixed resistance material to the asphalt is 100 (3-10), and preferably 100: 3; the rotating speed of the equipment for coating the asphalt is 10-30 HZ, preferably 20HZ, and/or the coating time is 1-3 hours, preferably 2 hours; preferably, the equipment is a horizontal coating kettle WHR-500L.
7. The method according to claim 1, wherein in step (4), said carbonizing is carried out by heating in a calcination apparatus under an inert atmosphere; preferably, the carbonization is as follows: processing for 6-20 hours at the constant temperature of 900-1300 ℃; preferably, the treatment is carried out at a constant temperature of 1150-1200 ℃ for 10 hours.
8. The method according to any one of claims 1 to 7, wherein in steps (3) and (5), the mixer is a high-efficiency wire rod trial mixer GPH-P-1.5P/C; preferably, in step (5)The tap density of the artificial graphite cathode material is more than or equal to 0.85g/cm3Preferably 0.87g/cm or more3(ii) a The specific surface area is 1.0-4.0 m2(ii)/g; the discharge capacity is more than or equal to 353.0 mAh/g; and/or the first efficiency is more than or equal to 90.5 percent.
9. The non-graphitized artificial graphite negative electrode material obtained by the method according to any one of claims 1 to 8.
10. A lithium battery characterized in that a negative electrode thereof contains the artificial graphite negative electrode material according to claim 9; preferably, the lithium battery is used for a two-wheel vehicle.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114394590A (en) * | 2022-01-21 | 2022-04-26 | 山西沁新能源集团股份有限公司 | Graphitized negative electrode material prepared from graphitized waste and preparation method thereof |
| CN114620707A (en) * | 2022-03-24 | 2022-06-14 | 江西正拓新能源科技股份有限公司 | Preparation method of long-cycle lithium ion battery cathode 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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