CN112652767A - Preparation method of soft carbon negative electrode material of lithium ion battery - Google Patents
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- 229910021384 soft carbon Inorganic materials 0.000 title claims abstract description 34
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000002699 waste material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims description 9
- 238000007493 shaping process Methods 0.000 claims description 5
- 239000010406 cathode material Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000011362 coarse particle Substances 0.000 claims description 3
- 230000004927 fusion Effects 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000003763 carbonization Methods 0.000 abstract description 4
- 238000004146 energy storage Methods 0.000 abstract description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000002006 petroleum coke Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011295 pitch Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011300 coal pitch Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011331 needle coke Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- 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
-
- 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
-
- 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
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a soft carbon negative electrode material of a lithium ion battery. The preparation method comprises the following steps: preparing the prebaked anode waste into powder particles; the medium particle size of the powder particles is 5-20 mu m. The invention has the advantages of wide raw material source, low cost, simple preparation process (not involving carbonization treatment), large-scale production and the like, can be used for the negative electrode material of the lithium ion battery in the fields of power and energy storage, prepares soft carbon by prebaked anode waste material for electrolytic aluminum, and has good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of carbon and electrochemistry, and relates to a preparation method of a soft carbon negative electrode material of a lithium ion battery.
Background
Lithium ion batteries have become the first choice in the fields of portable electronic devices, electric vehicles and energy storage due to their high energy density and long cycle life. The negative electrode is one of the core materials of the lithium ion battery, mainly comprises carbon materials, and comprises negative electrode materials such as graphite, soft carbon, hard carbon and the like.
The soft carbon material is transition carbon from amorphous carbon to graphite crystal, is generally prepared by taking coal or petroleum as a precursor, and mainly comprises pitch, needle coke, petroleum coke, carbon fiber, carbon microspheres and the like. The soft carbon is amorphous carbon, has low crystallinity, small crystal grain size, larger crystal face spacing, good compatibility with electrolyte, long cycle life, good multiplying power performance and good safety performance, has lower cost compared with graphite cathode materials, and is suitable for industries of electric vehicles, energy storage and the like.
The preparation process of the soft carbon negative electrode material at present mainly comprises the following steps: the material is petroleum coke, which is prepared through crushing, surface modification, carbonization, sieving and other steps. However, the preparation process is complicated and the cost is high.
Disclosure of Invention
The invention aims to solve the technical problems of high preparation cost and complex preparation process of the soft carbon negative electrode material, and provides a preparation method of the soft carbon negative electrode material of a lithium ion battery. The invention uses the prebaked anode waste as the raw material to produce the soft carbon cathode material, and the preparation method has the advantages of cost saving, environmental protection and simple preparation process.
The prebaked anode is prepared by using petroleum coke as a raw material and coal pitch as a binder through the procedures of petroleum coke calcination, medium crushing, screening, fine crushing, pitch melting, blending, kneading, molding, roasting and the like, is used for producing electrolytic aluminum, and has a demand of 1800 million tons per year. The prebaked anode product generates various waste products during the baking process, such as waste products due to oxidation, corner chipping, vertical cracking, bulging, rotten bowls, etc., which are collectively called prebaked anode scrap.
The waste materials are generally used as raw materials for recycling, so that the soft carbon cathode material is prepared, the added value of products can be improved, and the energy conservation and consumption reduction are facilitated.
The invention provides a preparation method of a soft carbon negative electrode material of a lithium ion battery, which comprises the following steps: preparing the prebaked anode waste into powder particles; the medium particle size of the powder particles is 5-20 mu m.
The prebaked anode scrap may be conventional in the art; preferably, the prebaked anode scrap is a waste product generated in the production process of the prebaked anode.
The preparation method of the powder particles can be conventional in the field, and the powder particles are preferably obtained by coarse crushing, fine crushing, crushing and shaping.
Further, the soft carbon negative electrode material is preferably obtained by sieving and demagnetizing the powder particles.
In a preferred embodiment of the present invention, the preparation method comprises the following steps:
(1) coarsely crushing the prebaked anode waste material by an type crusher to obtain coarsely crushed particles;
(2) the coarse particles are finely crushed by a mechanical crusher or a roller mill, and then are crushed by a jet mill or a ball mill;
(3) then, shaping the particles obtained in the step (2) by using mechanical fusion equipment to obtain powder particles;
(4) and screening the powder particles by using a vibrating screen, and demagnetizing by using a demagnetizing machine.
The invention provides an application of prebaked anode scrap in preparing a soft carbon negative electrode material.
Preferably, the prebaked anode scrap is a waste product generated in the production process of the prebaked anode.
The soft carbon negative electrode material has the single-particle morphology, the medium particle size is 5-20 microns, and the specific surface area is less than 4m2The capacity is more than 250mAh/g, and the first efficiency is more than 80%.
The positive progress effects of the invention are as follows:
the invention has the advantages of wide raw material source, low cost, simple preparation process (not involving carbonization treatment), large-scale production and the like, and can be used for the negative electrode material of the lithium ion battery in the fields of power and energy storage. The soft carbon is prepared from the prebaked anode waste for electrolyzing aluminum, and has good industrial application prospect.
Drawings
FIG. 1 is a scanning electron micrograph of soft carbon in example 1.
Fig. 2 is a XRD picture of soft carbon in example 1.
Fig. 3 is a picture of the charge and discharge performance of soft carbon in example 1.
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.
Example 1
As a contrast, the existing preparation process of the soft carbon negative electrode material is now provided. The petroleum coke is used as a raw material, and the specific preparation process comprises the following steps:
(1) mechanically grinding the raw materials, namely grinding the particles with the size of about 0.5-2 cm into micron-sized particles through mechanical or airflow grinding;
(2) powder surface modification: and (2) finishing modification treatment in a coating kettle, treating the material obtained in the step (1) in the coating kettle for 4-8 hours at 400-600 ℃, and modifying under the action of stirring. And after modification, carrying out water cooling in a cooling kettle to obtain the material with the modified surface.
(3) And (3) carbonizing the material subjected to surface modification at the highest carbonization temperature of 1100-1500 ℃ to obtain powder particles.
(4) And sieving the powder particles to remove magnetism, and preparing the soft carbon negative electrode powder with different particle size scales.
The soft carbon negative electrode material with the medium particle size of 13.4 mu m and the specific surface area of 3.3m is obtained by the process2The specific surface area per gram (mg/g), capacity 255mAh/g, and first efficiency 83.1%.
The preparation method of the soft carbon negative electrode material comprises the following steps:
(1) coarsely crushing the prebaked anode waste by an type crusher; obtaining particles with centimeter-level particle size;
(2) finely crushing the coarse particles by a mechanical crusher or a roller mill to obtain particles with micron-sized particle diameters;
(3) then crushing the mixture by a jet mill or a ball mill, and shaping the mixture by using mechanical fusion equipment. Performing surface treatment on the crushed particles to obtain powder particles with the medium particle size of 5-20 microns;
(4) and screening the powder particles by using a vibrating screen to remove large particles, and removing magnetic foreign matters in the particles by using a demagnetizing machine to obtain the soft carbon negative electrode materials with different particle size scales.
The soft carbon negative electrode material with the medium particle size of 7.3 mu m and the specific surface area of 3.4m is obtained by the process2(ii)/g, capacity of 253mAh/g, first efficiency of 81.2%.
The soft carbon negative electrode material with the medium particle size of 12.7 mu m and the specific surface area of 3.1m is obtained by the process2The specific surface area per gram (mAh/g) is 256, and the first efficiency is 82.4%.
The soft carbon negative electrode material with the medium particle size of 16.8 mu m and the specific surface area of 2.7m is obtained by the process2The specific surface area per gram (mg/g) was 261mAh/g, and the first efficiency was 83.5%.
The performances of the three soft carbon negative electrode materials are similar, the soft carbon negative electrode material with the median particle size of 7.3 mu m is analyzed, the scanning electron microscope picture is shown in figure 1, the phase is shown in figure 2, and the charging and discharging performances are shown in figure 3.
Claims (7)
1. A preparation method of a soft carbon negative electrode material of a lithium ion battery is characterized by comprising the following steps: preparing the prebaked anode waste into powder particles; the medium particle size of the powder particles is 5-20 mu m.
2. The method of claim 1, wherein the prebaked anode scrap is a waste product produced during the production of prebaked anodes.
3. The method according to claim 1, wherein the powder particles are obtained by coarse crushing, fine crushing, pulverization and shaping.
4. The preparation method according to any one of claims 1 to 3, wherein the soft carbon negative electrode material is obtained by sieving and demagnetizing the powder particles.
5. The method of claim 4, comprising the steps of:
(1) coarsely crushing the prebaked anode waste material by a type crusher to obtain coarsely crushed particles;
(2) the coarse particles are finely crushed by a mechanical crusher or a roller mill, and then are crushed by a jet mill or a ball mill;
(3) then, shaping the particles obtained in the step (2) by using mechanical fusion equipment to obtain powder particles;
(4) and screening the powder particles by using a vibrating screen, and demagnetizing by using a demagnetizing machine.
6. The application of the prebaked anode waste in preparing soft carbon cathode materials.
7. Use according to claim 6, wherein the prebaked anode scrap is a waste product produced in the production of prebaked anodes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116072818A (en) * | 2023-02-17 | 2023-05-05 | 大连理工大学 | Soft carbon material anode of double-ion battery and preparation method thereof |
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Application publication date: 20210413 |