CN115974066A - Method for preparing artificial graphite by using high-sulfur coke - Google Patents
Method for preparing artificial graphite by using high-sulfur coke Download PDFInfo
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- CN115974066A CN115974066A CN202211704638.4A CN202211704638A CN115974066A CN 115974066 A CN115974066 A CN 115974066A CN 202211704638 A CN202211704638 A CN 202211704638A CN 115974066 A CN115974066 A CN 115974066A
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- Prior art keywords
- artificial graphite
- intermediate material
- sulfur coke
- preparing artificial
- sulfur
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- 229910021383 artificial graphite Inorganic materials 0.000 title claims abstract description 46
- 239000011593 sulfur Substances 0.000 title claims abstract description 38
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 38
- 239000000571 coke Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 50
- 238000009656 pre-carbonization Methods 0.000 claims abstract description 13
- 238000007493 shaping process Methods 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000012216 screening Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 17
- 238000005469 granulation Methods 0.000 claims description 11
- 230000003179 granulation Effects 0.000 claims description 11
- 238000005087 graphitization Methods 0.000 claims description 9
- 239000010426 asphalt Substances 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000011331 needle coke Substances 0.000 description 7
- 239000012299 nitrogen atmosphere Substances 0.000 description 7
- 238000010000 carbonizing Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 239000012300 argon atmosphere Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000006256 anode slurry Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- 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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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for preparing artificial graphite by using high-sulfur coke, which comprises the following steps: s1, carrying out pre-carbonization treatment on the coarsely crushed high-sulfur coke, and then crushing to obtain an intermediate material 1 with 10-13wt% of volatile matter; s2, shaping the intermediate material 1, then uniformly mixing the intermediate material with a binder, and granulating to obtain an intermediate material 2; and S3, shaping the intermediate material 2, then graphitizing, and demagnetizing and screening to obtain the artificial graphite. The invention adopts high-sulfur coke as a raw material, reduces the cost, and selects a proper preparation process to ensure that the prepared artificial graphite has good tap density and electrical property.
Description
Technical Field
The invention relates to the technical field of artificial graphite, in particular to a method for preparing artificial graphite by using high-sulfur coke.
Background
The anode material is one of the key factors determining the performance of the lithium ion battery, and the artificial graphite is a commonly used raw material of the anode material of the lithium ion battery. The artificial graphite is mainly obtained by graphitizing a coke material at a high temperature, and part of products are also subjected to surface modification. The coke material mainly comprises petroleum coke, needle coke and the like.
The needle coke has low contents of elements such as sulfur, nitrogen and the like, has higher graphitization degree, excellent conductivity and larger lithium storage capacity, and is often used as a raw material for preparing artificial graphite. However, the price of the needle coke is high, about 10000 yuan/ton, and the needle coke is directly purchased for use, so that the cost is high.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for preparing artificial graphite by using high-sulfur coke, the high-sulfur coke is used as a raw material, the cost is reduced, and the prepared artificial graphite has good tap density and electrical property by selecting a proper preparation process.
The invention provides a method for preparing artificial graphite by using high-sulfur coke, which comprises the following steps:
s1, carrying out pre-carbonization treatment on the coarsely crushed high-sulfur coke, and then crushing to obtain an intermediate material 1 with 10-13wt% of volatile components;
s2, shaping the intermediate material 1, then uniformly mixing the intermediate material with a binder, and granulating to obtain an intermediate material 2;
and S3, shaping the intermediate material 2, then graphitizing, and demagnetizing and screening to obtain the artificial graphite.
The invention selects high-sulfur coke as raw material, the price of the high-sulfur coke is about 4000 yuan/ton, which is far lower than that of needle coke, and the production cost can be reduced; but the high-sulfur coke has high content of impurities and volatile components, which can reduce the performance of the artificial graphite, and the proper pre-carbonization process is selected in the invention, so that the content of the volatile components and the sulfur in the high-sulfur coke can be reduced; then crushing and screening the intermediate material 1 with proper particle size distribution, so that the tap density of the artificial graphite can be improved, and the electrical property of the artificial graphite is further improved.
Preferably, in S1, the pre-carbonization temperature is 900-1200 ℃ and the pre-carbonization time is 4-5h.
Preferably, in S1, the particle diameter D of the intermediate charge 1 10 ≥3μm、D 50 8-10 μm, D 90 ≤18μm、D 99 ≤35μm。
Preferably, in S2, the amount of the intermediate material 1 is 7-8% of the weight of the binder; the binder is asphalt; the binder is preferably medium temperature coal tar pitch.
Preferably, in S2, the granulation temperature is 900-1200 ℃ and the granulation time is 5-6h.
Preferably, in S2, the particle size D of the intermediate charge 2 10 ≥7.5μm、D 50 16.3-18.7 μm, D 90 ≤28μm、D 99 ≤48μm。
The tap density and graphitization degree of the artificial graphite can be further improved by selecting a proper granulation process and screening the intermediate material 2 with proper particle size distribution.
Preferably, in S3, the graphitization temperature is 2800-3200 ℃, and the graphitization time is 7-8h.
Preferably, the pre-carbonization, granulation, graphitization is performed in an inert gas atmosphere.
Preferably, pre-carbonizing and granulating in a nitrogen atmosphere; graphitization was performed in an argon atmosphere.
Preferably, the precarbonization and granulation are carried out in a tunnel kiln.
The tunnel kiln is used for replacing the traditional vertical kettle, the yield of batch production can be improved, and the tunnel kiln can be used for pre-carbonizing and granulating at a higher temperature, so that the purity of raw materials is improved, and the contents of impurities such as sulfur element, volatile component and the like are reduced; thereby improving the electrical property of the artificial graphite.
Preferably, in S3, the screen is 100-500 mesh.
Has the advantages that:
the invention selects the high-sulfur coke as the raw material, which can reduce the production cost; proper pre-carbonization and granulation processes are selected, so that the volatile content and the sulfur content in the high-sulfur coke can be reduced; the intermediate material 1 and the intermediate material 2 with proper particle size distribution are screened, so that the tap density of the artificial graphite can be improved, and the electrical property of the artificial graphite is further improved; replace traditional vertical cauldron with the tunnel cave, can improve batch production's output, use the tunnel cave moreover and can carry out carbonization and granulation in advance under higher temperature, improve the purity of raw materials, reduce the content of impurity such as sulphur element, volatile, prolong the energy storage life, improve the electrical property of artificial graphite.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
A method for preparing artificial graphite by using high-sulfur coke comprises the following steps:
s1, putting coarsely crushed high-sulfur coke into a tunnel kiln, pre-carbonizing at 1100 ℃ for 4.5 hours in a nitrogen atmosphere, and then crushing to obtain an intermediate material 1 with 10wt% of volatile matter;
particle diameter D of intermediate Material 1 10 ≥3μm、D 50 Is 8-10 μm, D 90 ≤18μm、D 99 ≤35μm；
S2, shaping the intermediate material 1, then uniformly mixing the intermediate material with asphalt, and granulating for 5.5 hours at 1100 ℃ in a tunnel kiln in a nitrogen atmosphere to obtain an intermediate material 2; the using amount of the intermediate material 1 is 7.5 percent of the weight of the asphalt;
particle diameter D of intermediate Material 2 10 ≥7.5μm、D 50 16.3-18.7 μm, D 90 ≤28μm、D 99 ≤48μm；
And S3, shaping the intermediate material 2, graphitizing for 7.5h at 3000 ℃ in an argon atmosphere in a graphitizing furnace, demagnetizing, and sieving by using a 100-500-mesh vibrating screen to obtain the artificial graphite.
Example 2
A method for preparing artificial graphite by using high-sulfur coke comprises the following steps:
s1, putting coarsely crushed high-sulfur coke into a tunnel kiln, pre-carbonizing for 5 hours at 900 ℃ in a nitrogen atmosphere, and then crushing to obtain an intermediate material 1 with 13wt% of volatile components;
particle diameter D of intermediate Material 1 10 ≥3μm、D 50 8-10 μm, D 90 ≤18μm、D 99 ≤35μm；
S2, shaping the intermediate material 1, then uniformly mixing the intermediate material with asphalt, and granulating for 6 hours at 900 ℃ in a tunnel kiln in a nitrogen atmosphere to obtain an intermediate material 2; the using amount of the intermediate material 1 is 7 percent of the weight of the asphalt;
particle diameter D of intermediate Material 2 10 ≥7.5μm、D 50 16.3-18.7 μm, D 90 ≤28μm、D 99 ≤48μm；
And S3, shaping the intermediate material 2, graphitizing for 8 hours at 2800 ℃ in an argon atmosphere in a graphitizing furnace, demagnetizing, and sieving by using a 100-500-mesh vibrating screen to obtain the artificial graphite.
Example 3
A method for preparing artificial graphite by using high-sulfur coke comprises the following steps:
s1, putting coarsely crushed high-sulfur coke into a tunnel kiln, pre-carbonizing for 4 hours at 1200 ℃ in a nitrogen atmosphere, and then crushing to obtain an intermediate material 1 with 11wt% of volatile matter;
particle diameter D of intermediate Material 1 10 ≥3μm、D 50 8-10 μm, D 90 ≤18μm、D 99 ≤35μm；
S2, shaping the intermediate material 1, then uniformly mixing the intermediate material with asphalt, and granulating for 5 hours at 1200 ℃ in a tunnel kiln in a nitrogen atmosphere to obtain an intermediate material 2; the using amount of the intermediate material 1 is 8 percent of the weight of the asphalt;
particle diameter D of intermediate Material 2 10 ≥7.5μm、D 50 16.3-18.7 mu m, D 90 ≤28μm、D 99 ≤48μm；
And S3, shaping the intermediate material 2, graphitizing for 7 hours at 3200 ℃ in an argon atmosphere in a graphitizing furnace, demagnetizing, and screening by using a 100-500-mesh vibrating screen to obtain the artificial graphite.
Comparative example 1
The intermediate charge 1 was replaced with needle coke having the same particle size distribution, and the procedure was otherwise the same as in example 1.
Comparative example 2
Particle diameter D of intermediate Material 1 10 ≥1μm、D 50 Is 10-12 μm, D 90 ≤20μm、D 99 Less than or equal to 40 mu m; the rest is the same as example 1.
Comparative example 3
Particle diameter D of intermediate Material 2 10 ≥5μm、D 50 20-22 μm, D 90 ≤35μm、D 99 Less than or equal to 50 mu m; the rest is the same as example 1.
The artificial graphite prepared in examples 1 to 3 and comparative examples 1 to 3 were used to measure tap density, and button cells were prepared from the artificial graphite of each group and tested for performance, and the results are shown in table 1.
The preparation method of the button cell comprises the following steps: taking the artificial graphite prepared in the examples 1-3 and the comparative examples 1-3, and preparing anode slurry according to the weight ratio of the artificial graphite to the conductive agent to the binder of 95; respectively uniformly scraping and coating the negative electrode slurry on copper foil, and drying in vacuum at 60 ℃ to obtain a negative electrode plate; and respectively assembling the lithium sheet serving as a positive electrode and the 1mol/LLIPF6 solution serving as an electrolyte solution to obtain the button cell.
TABLE 1 test results
As can be seen from Table 1, the artificial graphite prepared by using high-sulfur coke and combining with a proper preparation process has the performance close to that of the artificial graphite prepared by using needle coke, and the cost is low; and the intermediate material 1 and the intermediate material 2 with proper particle size distribution are selected, so that the tap density of the artificial graphite can be improved, and the performance of the lithium ion battery can be improved.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A method for preparing artificial graphite by using high-sulfur coke is characterized by comprising the following steps:
s1, carrying out pre-carbonization treatment on the coarsely crushed high-sulfur coke, and then crushing to obtain an intermediate material 1 with 10-13wt% of volatile matter;
s2, shaping the intermediate material 1, then uniformly mixing the intermediate material with a binder, and granulating to obtain an intermediate material 2;
and S3, shaping the intermediate material 2, then graphitizing, and demagnetizing and screening to obtain the artificial graphite.
2. The method for preparing artificial graphite from high-sulfur coke according to claim 1, wherein the pre-carbonization temperature is 900 to 1200 ℃ and the pre-carbonization time is 4 to 5 hours in S1.
3. The method for preparing artificial graphite from high-sulfur coke according to claim 1 or 2, wherein in S1, the particle diameter D of the intermediate charge 1 10 ≥3μm、D 50 8-10 μm, D 90 ≤18μm、D 99 ≤35μm。
4. The method for preparing artificial graphite from high-sulfur coke according to claim 1 or 2, wherein in S2, the amount of the intermediate charge 1 is 7-8% by weight of the binder; the binder is asphalt.
5. The method for preparing artificial graphite from high-sulfur coke according to claim 1 or 2, wherein the granulation temperature is 900 to 1200 ℃ and the granulation time is 5 to 6 hours in S2.
6. The method for preparing artificial graphite from high-sulfur coke according to claim 1 or 2, wherein in S2, the particle diameter D of intermediate charge 2 10 ≥7.5μm、D 50 16.3-18.7 μm, D 90 ≤28μm、D 99 ≤48μm。
7. The method for preparing artificial graphite from high sulfur coke according to claim 1 or 2, wherein in S3, the graphitization temperature is 2800 to 3200 ℃ and the graphitization time is 7 to 8 hours.
8. The method for preparing artificial graphite from high-sulfur coke according to claim 1 or 2, wherein the pre-carbonization, granulation, and graphitization are performed in an inert gas atmosphere.
9. The method for preparing artificial graphite from high-sulfur coke according to claim 1 or 2, wherein the pre-carbonization and granulation are performed in a tunnel kiln.
10. The method for preparing artificial graphite from high-sulfur coke according to claim 1 or 2, wherein in S3, the mesh is 100 to 500 mesh.
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