CN112978725A - Modified artificial graphite cathode material of power lithium ion battery and preparation method thereof - Google Patents
Modified artificial graphite cathode material of power lithium ion battery and preparation method thereof Download PDFInfo
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 25
- 229910021383 artificial graphite Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000010406 cathode material Substances 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 98
- 239000002245 particle Substances 0.000 claims abstract description 32
- 229910021384 soft carbon Inorganic materials 0.000 claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 21
- 239000002006 petroleum coke Substances 0.000 claims abstract description 20
- 239000003607 modifier Substances 0.000 claims abstract description 19
- 239000011329 calcined coke Substances 0.000 claims abstract description 17
- 238000005087 graphitization Methods 0.000 claims abstract description 12
- 239000010426 asphalt Substances 0.000 claims abstract description 9
- 239000012798 spherical particle Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 12
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- 239000007773 negative electrode material Substances 0.000 claims description 7
- 238000004220 aggregation Methods 0.000 claims description 5
- 230000002776 aggregation Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 2
- 239000003610 charcoal Substances 0.000 claims 3
- 238000000034 method Methods 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 3
- 230000003111 delayed effect Effects 0.000 abstract description 3
- 239000000571 coke Substances 0.000 abstract description 2
- 239000011163 secondary particle Substances 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 238000007493 shaping process Methods 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000010902 jet-milling Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000009818 secondary granulation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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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
-
- 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
- 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
- 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 & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium ion battery cathode materials, and particularly relates to a modified artificial graphite cathode material of a power lithium ion battery and a preparation method thereof, wherein the modified artificial graphite cathode material comprises calcined coke and a soft carbon coating modifier, the soft carbon coating modifier comprises soft carbon and petroleum coke spherical particle materials, and the mass ratio of the soft carbon to the petroleum coke spherical particle materials is as follows: petroleum coke =1-5: 100. The method comprises the following steps of coating and modifying petroleum coke by using soft, inflammable and easily-oxidized delayed petroleum coke as a main material, using high-temperature asphalt and calcined coke as auxiliary materials and using micron-sized high-temperature asphalt as a modifier, extruding and fusing the petroleum coke to the surface and the interior of a spherical-like material, and making up the defects of the surface and the interior of particles; delaying coke crushing to obtain micron-sized spheroidal materials, coating and modifying the materials by micron-sized high-temperature asphalt, and extruding and fusing at high temperature to obtain secondary particles; the modified artificial graphite product is prepared by high-temperature graphitization and sintering treatment, the cycle performance of the material is improved, the small particles are aggregated and granulated, the efficiency and the cycle performance are improved, and the modified artificial graphite product is applied to power lithium ion batteries.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery cathode materials, and particularly relates to a modified artificial graphite cathode material for a power type lithium ion battery and a preparation method thereof.
Background
Due to the gradual depletion of non-renewable resources and the era background that environmental awareness is more and more attracting people to pay attention, battery technology makes a rapid progress, and secondary environment-friendly green batteries become the first choice for the development of battery technology. The lithium ion battery becomes a preferred secondary battery series developed in the battery industry due to the advantages of high specific energy, high specific capacity, long cycle stability, environmental protection and the like. The artificial graphite has the advantages of low production cost and good development prospect, and is valued by the lithium ion battery industry at home and abroad.
The current artificial negative electrode material for the lithium ion battery has some defects, and the surface of the material is easy to generate irreversible reaction with electrolyte to cause the reduction of charge-discharge efficiency, the reduction of battery reversible capacity caused by solvent co-embedding, the expansion of material volume, poor cycle performance and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a modified artificial graphite cathode material of a power lithium ion battery and a preparation method thereof.
In order to solve the above problems, the specific technical scheme of the invention is as follows: the modified artificial graphite cathode material for the power type lithium ion battery comprises calcined coke and a soft carbon coating modifier, wherein the mass ratio of the calcined coke to the soft carbon coating modifier is as follows: soft carbon coating modifier =3:7, the soft carbon coating modifier comprises soft carbon and petroleum coke spherical particle materials, and the mass ratio of the soft carbon to the petroleum coke spherical particle materials is as follows: petroleum coke =1-5: 100.
The mass ratio of the calcined coke to the soft carbon coating modifier is as follows: soft carbon coating modifier = 2: 8.
the mass ratio of the calcined coke to the soft carbon coating modifier is as follows: soft carbon coating modifier = 1: 9.
the preparation method of the modified artificial graphite cathode material of the power type lithium ion battery comprises the following steps: step one, preparing a material A: crushing petroleum coke to obtain a material A with the median particle size of 5-13 um;
step two: preparation of material B: crushing the calcined coke to obtain a material B with a median particle size of 4.5-12.5 um; step three: preparation of Material C: crushing the high-temperature asphalt to obtain a material C with the median particle size of less than or equal to 3 mu m;
step four: mixing the material A and the material C prepared in the first step and the third step according to the mass ratio of A: C =100: 1-5;
step five: modifying the mixture obtained in the step four by using a reaction kettle at the temperature of 550-650 ℃ to obtain a material D;
step six: and (3) charging the material B obtained in the step (II) by using a crucible, carrying out graphitization at 2800-3100 ℃, conventionally charging the material D, keeping the graphitization at about 3000 ℃, and stopping heating after 3000 ℃ is maintained for 6 hours.
Step seven: and respectively carrying out self-mixing, cross-mixing and screening treatment on the material B and the material D, and carrying out secondary aggregation granulation according to the mass ratio of B: D =3:7 or 2:8 or 1:9, wherein the granulation temperature is higher than 930 ℃, so as to obtain the modified artificial graphite cathode material for the power lithium ion battery.
The invention has the following beneficial effects: the method comprises the following steps of (1) taking soft, inflammable and easily-oxidized delayed petroleum coke as a main material, taking high-temperature asphalt and calcined coke as auxiliary materials, carrying out precise grading and shaping on the calcined coke through a grading and shaping all-in-one machine to obtain a micron-sized spherical-like material, taking the micron-sized high-temperature asphalt as a modifier, coating and modifying the petroleum coke, extruding and fusing the petroleum coke to the surface and the inside of the spherical-like material, and making up the defects on the surface and the inside of particles; crushing and shaping the delayed coke to obtain a micron-sized spheroidal material, coating and modifying the micron-sized spheroidal material by using micron-sized high-temperature asphalt, and extruding and fusing the micron-sized high-temperature asphalt at high temperature to obtain secondary particles; high-temperature graphitization sintering treatment is carried out at 2800-.
Detailed Description
Example 1: the preparation method of the modified artificial graphite cathode material of the power type lithium ion battery comprises the following steps of 1: taking 100kg of raw material A, and mechanically treating petroleum coke by using a drying and crushing integrated machine to obtain a quasi-spherical material A with a median particle size of 5 um; and taking 2kg of auxiliary material C, and performing jet milling to obtain a material with the median particle size of 2 um. And (2) cold mixing the A and the C under the condition of gas flow atmosphere, and carrying out modification treatment on the mixture under the condition of utilizing the reaction kettle N2 atmosphere at the temperature curve of (350-30 min-350-60 min-450-90 min-450-30 min-500-60 min-640-150 min-640 ℃) to obtain a material D.
Step 2: and taking 25.5kg of auxiliary material B, and crushing the calcined coke by using a crushing and shaping integrated machine to obtain a spheroidal material B with the median particle size of 12.5 um.
And step 3: the sphere-like material B obtained in the step 2 is charged into a furnace by adopting a crucible, and the graphitization temperature is 3100 ℃; and (3) charging the material D in a conventional manner, maintaining the graphitization temperature at 3000 ℃ for 6h at 3000 ℃, and then stopping heating.
And 4, step 4: and 3, after discharging, adjusting the granularity of the material B, D, controlling the median particle size of the material B to be between 10.5 and 11.5um, controlling the median particle size of the material D to be between 5 and 6um, and then mixing the material B and the material D according to the mass ratio of 2: and 8, carrying out secondary aggregation granulation at the granulation temperature of more than 930 ℃ to obtain the power type lithium ion negative electrode material.
The discharge capacity of the product obtained by the method is 345.2 mAh/g, and the discharge efficiency is 93.0%.
Example 2:
the preparation method of the modified artificial graphite cathode material of the power type lithium ion battery comprises the following steps of 1: preparation of Material D
Taking 100kg of raw material A, and mechanically treating petroleum coke by using a drying and crushing integrated machine to obtain a spherical material A with the median particle size of 6 um; and 3kg of auxiliary material C is taken and subjected to jet milling to obtain a material C with the median particle size of 3um, the A and the C are subjected to cold mixing under the condition of air flow atmosphere, and the mixture is subjected to modification treatment under the condition of utilizing a reaction kettle N2 atmosphere at the temperature curve of (320-30 min-320-60 min-400-90 min-400-30 min-450-60 min-620-150 min-620 ℃) to obtain a material D.
Step 2: preparation of Material B
And taking 12kg of auxiliary materials B, and crushing the calcined coke by using a crushing and shaping integrated machine to obtain a spheroidal material B with the median particle size of 11.5 um.
And step 3: graphitizing the material B and the material D
The sphere-like material B prepared in the step 2 is charged into a furnace by adopting a crucible, and the graphitization temperature is carried out under the condition of 2900 ℃; and (3) charging the material D in a conventional manner, maintaining the graphitization temperature at 3000 ℃ for 6h at 3000 ℃, and then stopping heating.
And 4, step 4: particle size adjustment
And 3, after the material B is discharged from the furnace, adjusting the particle size of the material B and the particle size of the material D, wherein the median particle size of the material B is between 9.5 and 10.5um, and the median particle size of the material D is controlled between 7 and 8 um.
And 5: secondary granulation
And (3) mixing the material B with the material D according to the mass ratio of 1:9, carrying out secondary aggregation granulation at the granulation temperature of more than 930 ℃ to prepare the power type lithium ion negative electrode material.
The discharge capacity of the product obtained by the method is 342.1 mAh/g, and the discharge efficiency is 93.1%.
Example 3:
the preparation method of the modified artificial graphite cathode material of the power type lithium ion battery comprises the following steps of 1: preparation of Material D
Taking 100kg of raw material A, and mechanically treating petroleum coke by using a drying and crushing integrated machine to obtain a spherical-like material A with the median particle size of 13 um; taking 2kg of auxiliary material C, carrying out jet milling to obtain a material with a median particle size of 1um, and carrying out cold mixing on the material A and the material C under the condition of air flow atmosphere; the mixture is modified under the condition of temperature curve (320-30 min-320-60 min-400-90 min-400-30 min-450-60 min-600-150 min-600 ℃) by utilizing the atmosphere of a reaction kettle N2 to obtain a material D.
Step 2: preparation of Material B
And taking 12kg of auxiliary materials B, and crushing the calcined coke by using a crushing and shaping integrated machine to obtain a spheroidal material B with the median particle size of 6.5 um.
And step 3: graphitizing the material B and the material D
The material B is charged into a furnace by adopting a crucible, and the graphitization temperature is carried out under the condition of 2900 ℃; and (3) charging the material D in a conventional manner, maintaining the graphitization temperature at 3000 ℃ for 6h at 3000 ℃, and then stopping heating.
And 4, step 4: particle size adjustment
And (3) after the material B and the material D are discharged from the furnace, the particle size of the median particle of the material B is between 4.5 and 5.5um, and the particle size of the median particle of the material D is between 12 and 13 um.
And 5: secondary granulation
And then mixing the material B and the material D according to the ratio of 1: and 9, carrying out secondary aggregation granulation at the granulation temperature of more than 930 ℃ to prepare the power type lithium ion negative electrode material.
The discharge capacity of the product obtained by the method is 335.8 mAh/g, and the discharge efficiency is 92.0%.
The optimal method obtained by multiple times of test regulation is as follows: the median particle diameter of A is 5-6um, the median particle diameter of B is 11.5-12.5um, C is 2um, the temperature of the reaction kettle is controlled between 620 and 630, and the ratio of A to C is 100: 5; b: when the proportion of D is 3:7, the discharge capacity of the obtained product is 349.6 mAh/g, and the discharge efficiency is 93.4%.
Claims (4)
1. The modified artificial graphite cathode material for the power type lithium ion battery is characterized in that: the soft charcoal coating modifier comprises calcined coke and a soft charcoal coating modifier, wherein the mass ratio of the calcined coke to the soft charcoal coating modifier is as follows: soft carbon-coated modified product is 3:7, the soft carbon coating modifier comprises soft carbon and petroleum coke spherical particle materials, and the mass ratio of the soft carbon to the petroleum coke spherical particle materials is as follows: petroleum coke is 1-5: 100.
2. The modified artificial graphite negative electrode material for power lithium ion batteries according to claim 1, characterized in that: the mass ratio of the calcined coke to the soft carbon coating modifier is as follows: soft carbon coating modifier 2: 8.
3. the modified artificial graphite negative electrode material for power lithium ion batteries according to claim 1, characterized in that: the mass ratio of the calcined coke to the soft carbon coating modifier is as follows: soft carbon-coated modified product 1: 9.
4. the preparation method of the modified artificial graphite negative electrode material of the power lithium ion battery as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps: step one, preparing a material A: crushing petroleum coke to obtain a material A with the median particle size of 5-13 um;
step two: preparation of material B: crushing the calcined coke to obtain a material B with a median particle size of 4.5-12.5 um;
step three: preparation of Material C: crushing the high-temperature asphalt to obtain a material C with the median particle size of less than or equal to 3 mu m;
step four: mixing the material A and the material C prepared in the first step and the third step according to the mass ratio of 100: 1-5;
step five: modifying the mixture obtained in the step four by using a reaction kettle at the temperature of 550-650 ℃ to obtain a material D;
step six: the material B obtained in the step two is loaded in a crucible, the graphitization temperature is carried out under the conditions of 2800-3100 ℃, the material D is loaded in a conventional furnace, the graphitization temperature is about 3000 ℃, and the temperature rise is stopped after 3000 ℃ is maintained for 6 hours;
step seven: and respectively carrying out self-mixing, cross-mixing and screening treatment on the material B and the material D, and carrying out secondary aggregation granulation according to the mass ratio of B to D being 3:7 or 2:8 or 1:9, wherein the granulation temperature is higher than 930 ℃, so as to obtain the modified artificial graphite cathode material for the power lithium ion battery.
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| CN202110175084.2A CN112978725A (en) | 2021-02-07 | 2021-02-07 | Modified artificial graphite cathode material of power lithium ion battery and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114477162A (en) * | 2021-12-31 | 2022-05-13 | 惠州锂威新能源科技有限公司 | Preparation method of graphite negative electrode material, product and application thereof |
| CN114950661A (en) * | 2022-04-19 | 2022-08-30 | 湖南铂威新能源科技有限公司 | Preparation method of energy-saving and environment-friendly artificial graphite cathode material |
| 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 |
| CN117401961A (en) * | 2023-12-15 | 2024-01-16 | 中民驰远实业有限公司 | Preparation method of scour-resistant magnesia-alumina spinel baking-free brick |
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| CN110723730A (en) * | 2019-10-21 | 2020-01-24 | 广东羚光新材料股份有限公司 | High-specific-volume high-cycle-performance artificial graphite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114950661A (en) * | 2022-04-19 | 2022-08-30 | 湖南铂威新能源科技有限公司 | Preparation method of energy-saving and environment-friendly artificial graphite cathode material |
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| CN117401961A (en) * | 2023-12-15 | 2024-01-16 | 中民驰远实业有限公司 | Preparation method of scour-resistant magnesia-alumina spinel baking-free brick |
| CN117401961B (en) * | 2023-12-15 | 2024-02-23 | 中民驰远实业有限公司 | Preparation method of scour-resistant magnesia-alumina spinel baking-free brick |
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Address after: 116000 Haitang street, Huayuankou Economic Zone, Dalian City, Liaoning Province Applicant after: Dalian Hongguang Lithium Industry Co.,Ltd. Address before: 116000 Haitang street, Huayuankou Economic Zone, Dalian City, Liaoning Province Applicant before: DALIAN HONGGUANG LITHIUM INDUSTRY CO.,LTD. |
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Application publication date: 20210618 |