CN114956069A - Device for preparing artificial graphite cathode material for lithium ion battery and preparation method thereof - Google Patents
Device for preparing artificial graphite cathode material for lithium ion battery and preparation method thereof Download PDFInfo
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- 229910021383 artificial graphite Inorganic materials 0.000 title claims abstract description 45
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 39
- 239000010406 cathode material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 85
- 238000005087 graphitization Methods 0.000 claims abstract description 52
- 239000002006 petroleum coke Substances 0.000 claims abstract description 52
- 238000000227 grinding Methods 0.000 claims abstract description 45
- 238000012986 modification Methods 0.000 claims abstract description 32
- 230000004048 modification Effects 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 238000003763 carbonization Methods 0.000 claims abstract description 24
- 238000007493 shaping process Methods 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims description 70
- 239000010426 asphalt Substances 0.000 claims description 48
- 239000005539 carbonized material Substances 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000006011 modification reaction Methods 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 238000004806 packaging method and process Methods 0.000 claims description 15
- 239000010405 anode material Substances 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 14
- 238000012216 screening Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 7
- 239000007773 negative electrode material Substances 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 3
- 238000002715 modification method Methods 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 11
- 238000000576 coating method Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 229910021382 natural graphite Inorganic materials 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 239000011331 needle coke Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 239000011325 microbead Substances 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000006253 pitch coke Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- -1 transition metal nitride Chemical class 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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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
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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
- 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
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
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- 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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Abstract
The invention discloses a device for preparing an artificial graphite cathode material for a lithium ion battery and a preparation method thereof, and particularly relates to the field of battery materials. The device comprises a material coarse crushing and drying unit, a mechanical grinding and shaping unit, a modification unit, a depolymerization unit, a graphitization unit, a carbonization unit and a post-treatment unit, wherein all the units are sequentially connected. The invention has simple production process and high efficiency, and effectively reduces the production cost of the cathode material. The invention improves the surface density of the battery negative pole piece according to the particle shape adjustment of the petroleum coke, effectively improves the discharge rate and prolongs the cycle life of the material. The invention sets the proportion of different coating asphalts according to the different particle sizes of the raw materials, so that the electrical property of the artificial graphite cathode material can be best exerted.
Description
Technical Field
The invention relates to the field of battery materials, in particular to a device for preparing an artificial graphite cathode material for a lithium ion battery and a preparation method thereof.
Background
The lithium ion battery is a secondary battery, and mainly depends on the reciprocating movement of lithium ions between a positive electrode and a negative electrode to realize the charging and discharging process, so the lithium ion battery is also vividly called a rocking chair battery. With the increasing demand of various countries for green energy, lithium ion batteries have become a hot spot for scientific research and development of energy. The cathode material is one of the critical materials of the lithium ion battery, and influences the important performance indexes of the lithium ion battery, such as the capacity, the service life, the safety performance and the like. At present, the negative electrode material for the lithium ion battery mainly comprises a carbon material, a transition metal oxide, an alloy material, a silicon material, a lithium-containing transition metal nitride, a lithium titanate material and the like, wherein the carbon material mainly comprises graphite, hard carbon, soft carbon and the like.
However, among the materials used as the carbon negative electrode, only microbeads of carbon, natural graphite and artificial graphite are mature. The carbon cycling performance of the microbeads is good, but the current dosage is not very large compared with natural graphite and artificial graphite due to low capacity; the natural graphite has low intercalation potential and excellent intercalation and deintercalation performance, is a good lithium ion battery cathode material, but has general cycle performance and is mainly used on digital batteries; although the cycle performance of the artificial graphite is slightly better than that of the natural graphite, the artificial graphite has the defects of difficult processing, low capacity, large rebound and the like.
Patent CN104900878A discloses a method for producing artificial graphite cathode material of lithium ion battery, which adds single or multiple transition metal elements into main material petroleum coke in coarse powder state, and then graphitizes the main material petroleum coke, and this method has certain defects: because the petroleum coke has coarse particles, the complete uniform graphitization of the interior of the main material is difficult to ensure even at the ultrahigh-temperature graphitization temperature, and finally the negative electrode material has negative influence on the capacity exertion.
In patent CN105390673B, a highly graphitized material is used as a raw material, and the high-capacity graphite negative electrode is prepared through crushing, granulation, graphitization, and carbon coating. The first discharge capacity reaches 346.2, and the first discharge capacity is compacted to 1.26 and the multiplying power is 1C. Although the capacity is improved, the multiplying power can only reach 1C, and the quick charging performance can not meet the current market requirement.
Patent CN113697805A uses graphitized raw materials as raw materials, prepares the artificial graphite negative electrode material of high compaction high capacity through grinding, surface treatment, granulation, graphitization and carbon coating carbonization, though the electric capacity can reach the demand, but the low temperature performance can not be guaranteed, and the cycle discharge frequency is not feasible, can satisfy the requirement of filling soon, but can not satisfy the demand of high energy storage.
Disclosure of Invention
In order to solve the problems, the invention provides a device for preparing an artificial graphite cathode material for a lithium ion battery and a preparation method thereof, wherein petroleum coke is used as a raw material and is polymerized and carbonized with asphalt, so that the electrical conductivity, the thermal conductivity and the high temperature resistance can be obviously improved; and then the artificial graphite cathode material is formed through secondary coating and carbonization, so that the cathode material which has good low temperature property, high capacity and long cycle life and is suitable for energy storage and power lithium batteries is obtained.
At present, the battery negative electrode material is still the artificial graphite material in the application. Although natural graphite has high capacity, the disadvantages of easy expansion and quick attenuation are to be improved, and only artificial graphite has the advantages of high capacity and good cycle.
In order to achieve the above purpose, the invention provides the following technical scheme:
according to a first aspect of the present invention, there is provided an apparatus for preparing an artificial graphite anode material for a lithium ion battery, comprising:
the device comprises a material coarse crushing and drying unit, a mechanical grinding and shaping unit, a modification unit, a depolymerization unit, a graphitization unit, a carbonization unit and a post-treatment unit, wherein all the units are connected in sequence.
Further, the material coarse crushing and drying unit comprises an original material feeding bin, a feeding belt, a raw material coarse crushing unit, a coarse crushing and drying unit and a cooling screw conveyer; the stone tar raw material in the raw material feeding bin enters the raw material coarse crushing unit through the feeding belt for coarse crushing, the coarse crushed material is dried in the coarse crushing and drying unit, and the dried material enters the mechanical grinding unit through the cooling screw conveyor.
Further, the mechanical grinding and shaping unit comprises a coarse powder feeding bin, a grinding unit, a particle size grading unit, a shaping unit, a first grinding pipeline, a second grinding pipeline and a third grinding pipeline; wherein the coarse powder in the coarse crushing and drying unit enters a coarse powder feeding bin for storage and then enters a grinding unit, the ground material enters a particle size grading unit through a first grinding pipeline, the particle size under the composite condition after grading enters a shaping unit through a second grinding pipeline, and the shaped material enters a modification unit through a third grinding pipeline.
Further, the modification unit comprises a fine powder feeding bin and a modification reaction kettle, wherein the materials shaped in the mechanical grinding and shaping unit enter the fine powder feeding bin for storage, then enter the modification reaction kettle from the fine powder feeding bin for modification, and enter the depolymerization unit.
Further, the depolymerization unit comprises a modified powder feeding bin, a depolymerizer main machine, a depolymerizer, a first depolymerizing pipeline and a second depolymerizing pipeline, and the graphitization unit comprises a graphitization furnace; the material modified by the modification unit enters a modified powder feeding bin, after a depolymerizer main machine is opened, the material in the modified powder feeding bin enters a depolymerizer through a first depolymerizing pipeline for depolymerization, the depolymerized material enters a graphitization furnace through a second depolymerizing pipeline for graphitization, and the graphitized material after the graphitization treatment enters a carbonization unit; the graphitization furnace is a box-type graphitization furnace.
Further, the carbonization unit comprises a graphitized material feeding port, a mixer and a roller kiln; the graphitized material after treatment enters a mixer through a graphitized material feeding hole to be uniformly mixed, the uniformly mixed material enters a roller kiln to be carbonized, and the carbonized material enters an after-treatment unit.
Further, the post-treatment unit comprises a carbonized material bin, a carbonized material mixer, screening equipment, demagnetizing equipment and packaging equipment; the carbonized material is stored in a carbonized material bin, and then is mixed, screened, demagnetized and packaged by a carbonized material mixer, a screening device, a demagnetizing device and a packaging device in sequence.
According to a second aspect of the present invention, there is provided a method for preparing an artificial graphite anode material for a lithium ion battery using the above unit, comprising:
step one, raw material treatment
Firstly, coarsely crushing petroleum coke and drying to obtain coarse petroleum coke, and then performing fine powder shaping treatment on the coarse petroleum coke to obtain fine powder petroleum coke; carrying out fine pulverization treatment on the asphalt to obtain fine powder asphalt;
step two, modification
Performing modification treatment on the fine petroleum coke powder and the fine asphalt powder to obtain a granulation material;
step three, depolymerization
Depolymerizing the granulated material to obtain a cathode precursor product;
step four, graphitization treatment
Placing the cathode precursor product in a box-type graphitization furnace for high-temperature graphitization treatment to obtain a graphitized material;
step five, carbonizing
Adding 1.5-3% of crushed asphalt into the graphitized material, uniformly mixing in a mixer, and then entering a roller kiln for carbonization under the protection of nitrogen at 900-1200 ℃ to obtain a carbonized material;
step six, post-treatment
And mixing, screening, demagnetizing and packaging the carbonized material to obtain the artificial graphite cathode material for the lithium ion battery.
Further, in the first step, the petroleum coke is coarsely crushed by a shear type crusher;
and/or the grain size of the coarse powder petroleum coke is less than or equal to 5 mm;
and/or the water content of the petroleum coke is less than 3 percent after the petroleum coke is coarsely crushed and dried.
Further, the petroleum coke is 2# A low-sulfur petroleum coke, NB/SH/T05272015 petroleum coke or 3# A petroleum coke;
and/or the asphalt is solid asphalt with the softening point of 150-350 ℃ obtained by purifying oil asphalt;
and/or the proportion of the fine petroleum coke to the fine asphalt is (85-97) to (3-15).
Further, in the second step, the modification reaction kettle is filled with an inert gas in advance, and the inert gas is used for exhausting air in the reaction kettle and includes, but is not limited to, nitrogen as an example.
Further, in the second step, the modification method is that the fine petroleum coke powder and the fine asphalt powder in the modification reaction kettle are stirred for 2 hours at the temperature of 200-400 ℃, the temperature is raised to 650 ℃, and under the protection of inert gas, the mixture is statically modified for 6 hours in a temperature curve of 650 ℃ to obtain the granulating material.
Further, the modification reaction kettle is a vertical heating reaction kettle or a horizontal cooling kettle.
Furthermore, in the fourth step, the high-temperature graphitization treatment method is to gradually increase the temperature of the box-type graphitization furnace, raise the temperature to 2300 ℃ until 3000 ℃ and treat for 8 h.
The box-type graphitization furnace adopted by the invention heats the granulated material, the material can be gradually heated, the spacing between graphite layers is gradually reduced along with the temperature rise, the material is obviously changed when reaching 2300 ℃, the material is slowly changed when reaching 3000 ℃, and the graphitization process is completed.
The invention adopts the box-type graphitization furnace with slow temperature rise process, the electrifying period can reach 90-98h, the furnace core temperature can reach 2800-.
Furthermore, the carbonization equipment is vertical carbonization furnace equipment.
According to a third aspect of the present invention, there is provided an artificial graphite anode material prepared by the above-described preparation method.
The invention has the following advantages:
the invention ensures that the prepared artificial graphite cathode material has stable mechanical strength and can obviously improve the conductivity, the thermal conductivity and the high temperature resistance through the granulation process.
The artificial graphite cathode material for the lithium ion battery prepared by the invention has the advantages of good low temperature property, high capacity and long cycle life, and is suitable for energy storage and power lithium batteries.
The invention has simple production process and high efficiency, and effectively reduces the production cost of the cathode material. The invention improves the surface density of the battery negative pole piece according to the particle shape adjustment of the petroleum coke, effectively improves the discharge rate and prolongs the cycle life of the material. The invention sets the proportion of different coating asphalts according to different particle sizes of raw materials, so that the electrical property of the artificial graphite cathode material can be best exerted.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.
FIG. 1 is a diagram of an apparatus for preparing an artificial graphite anode material for a lithium ion battery according to the present invention;
FIG. 2 is a diagram of a material crushing and drying unit provided by the invention;
FIG. 3 is a diagram of a mechanical polishing and shaping unit provided by the invention;
FIG. 4 is a diagram of a modification unit provided by the invention;
FIG. 5 is a diagram of a disaggregation unit provided by the present invention;
FIG. 6 is a diagram of a graphitizing unit provided by the present invention;
FIG. 7 is a diagram of a carbonization unit provided by the invention;
FIG. 8 is a diagram of a post-processing unit provided by the present invention;
fig. 9 is a process flow chart of the invention for preparing the artificial graphite cathode material for the lithium ion battery.
FIG. 10 is an electron microscope image of fine petroleum coke powder provided by the present invention;
FIG. 11 is an electron micrograph of a granulated material according to the present invention.
In the figure, 1-a material rough breaking and drying unit, 11-an original material feeding bin, 12-a feeding belt, 13-a raw material rough breaking unit, 14-a rough crushing and drying unit and 15-a cooling screw conveyer;
2-mechanical grinding and shaping unit, 21-coarse powder feeding bin, 22-grinding unit, 23-particle size grading unit, 24-shaping unit, 25-first grinding pipeline, 26-second grinding pipeline and 27-third grinding pipeline;
3-modification unit, 31-fine powder feeding bin and 32-modification reaction kettle;
4-depolymerization unit, 41-modified powder feeding bin, 42-depolymerizer host, 43-depolymerizer, 44-first depolymerizing pipeline, 45-second depolymerizing pipeline;
5-graphitization unit, 51-graphitization furnace;
6-a carbonization unit, 61-a graphitized material feeding port, 62-a roller kiln and 63-a mixer;
7-post-treatment unit, 71-carbonized material bin, 72-carbonized material mixer, 73-screening equipment, 74-demagnetizing equipment and 75-packaging equipment.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example provides an apparatus for preparing an artificial graphite anode material for a lithium ion battery, as shown in fig. 1.
An apparatus for preparing an artificial graphite anode material for a lithium ion battery, comprising:
the device comprises a material coarse crushing and drying unit 1, a mechanical grinding and shaping unit 2, a modification unit 3, a depolymerization unit 4, a graphitization unit 5, a carbonization unit 6 and a post-treatment unit 7, wherein the units are sequentially connected.
Further, the material coarse crushing and drying unit 1 comprises an original material feeding bin 11, a feeding belt 12, a raw material coarse crushing unit 13, a coarse crushing and drying unit 14 and a cooling screw conveyer 15; wherein, the raw material of the stone tar in the raw material feeding bin 11 enters the raw material coarse crushing unit 13 through the feeding belt 12 for coarse crushing, the coarse crushed material is dried in the coarse crushing and drying unit 14, and the dried material enters the mechanical grinding unit after being cooled by the cooling screw conveyer 15, as shown in fig. 2.
Further, the mechanical grinding and shaping unit 2 comprises a coarse powder feeding bin 21, a grinding unit 22, a particle size grading unit 23, a shaping unit 24, a first grinding pipeline 25, a second grinding pipeline 26 and a third grinding pipeline 27; wherein, the coarse powder in the coarse crushing and drying unit 1 enters a coarse powder feeding bin for storage 21 and then enters a grinding unit 22, the ground material enters a particle size grading unit 23 through a first grinding pipeline 25, the particle size under the composite condition after grading enters a shaping unit 24 through a second grinding pipeline 26, and the shaped material enters a modification unit through a third grinding pipeline 27, as shown in fig. 3.
Further, the modification unit 3 includes a fine powder feeding bin 31 and a modification reaction kettle 32, wherein the material shaped in the mechanical grinding and shaping unit 2 enters the fine powder feeding bin 31 for storage, and then enters the modification reaction kettle 32 from the fine powder feeding bin for modification, and the modified material enters the depolymerization unit 4, as shown in fig. 4.
Further, the depolymerization unit 4 includes a modified powder feeding bin 41, a depolymerization machine main unit 42, a depolymerization machine 43, a first depolymerization pipeline 44 and a second depolymerization pipeline 45 as shown in fig. 5, and the graphitization unit 5 includes a graphitization furnace 51 as shown in fig. 6; the modified material of the modification unit 3 enters a modified powder feeding bin 41, after a depolymerizer host 42 is opened, the material in the modified powder feeding bin 41 enters a depolymerizer 43 through a first depolymerizing pipeline 44 for depolymerization, the depolymerized material enters a graphitization furnace 51 through a second depolymerizing pipeline 45 for graphitization, and the treated graphitized material enters a carbonization unit 6; the graphitization furnace is a box-type graphitization furnace.
Further, the carbonization unit 6 comprises a graphitized material feeding port 61, a roller kiln 62 and a mixer 63; the treated graphitized material enters a mixer 63 through a graphitized material feeding port 61 to be uniformly mixed, the mixed material enters a roller kiln 62 to be carbonized, and the carbonized material enters the post-treatment unit 7, as shown in fig. 7.
Further, the post-treatment unit comprises a carbonized material bin 71, a carbonized material mixer 72, a screening device 73, a demagnetizing device 74 and a packaging device 75; the carbonized material enters the carbonized material bin 71 for storage, and then sequentially passes through the carbonized material mixer 72, the sieving device 73, the demagnetizing device 74 and the packaging device 75 from the carbonized material bin 71 to be mixed, sieved, demagnetized and packaged, as shown in fig. 8.
Example 2
This example provides a method for preparing an artificial graphite anode material for a lithium ion battery using the apparatus of example 1, the process is shown in fig. 9,
step one, pretreatment of raw materials
Firstly, crushing petroleum coke to the particle size of less than or equal to 5mm by using a shear type crusher, and drying until the water content is less than 3% to obtain coarse powder petroleum coke;
selecting coating asphalt as solid asphalt with the softening point of 250 +/-5 ℃ obtained by purifying oil asphalt;
coarse petroleum coke powder is subjected to coarse crushing, drying and mechanical grinding and shaping to form fine powder, and the fine powder petroleum coke with the particle size of 10.0 +/-1.0 mu m is obtained; performing fine pulverization treatment on the coated asphalt to obtain fine powder asphalt with the particle size of 5.0 +/-1.0 mu m, and mixing the fine powder petroleum coke: adding the fine powder asphalt 97:3 into the modification unit 3;
step two, modification
The modification reaction kettle is filled with inert gas nitrogen in advance, and the inert gas is used for exhausting air in the reaction kettle;
feeding fine petroleum coke and fine asphalt into a pretreatment nitrogen-filled modification reaction kettle through a fine powder feeding bin, stirring the fine petroleum coke and the fine asphalt at 300 ℃ for 2 hours, heating to 650 ℃, and statically modifying for 6 hours and 8 hours in a 650 ℃ temperature curve under the protection of inert gas to prepare a modified material with the particle size of 17.0 +/-2.0 microns;
step three, depolymerization treatment
Storing the modified material in a modified powder feeding bin 41, opening a depolymerizer host 42, and allowing the modified material in the modified powder feeding bin 41 to enter a depolymerizer 43 through a first depolymerizing pipeline 44 for depolymerization to obtain a depolymerized precursor product;
step four, graphitization treatment
Cooling the depolymerized precursor product through a secondary kettle, putting the depolymerized precursor product into a box-type graphitization furnace, gradually heating to 2300 ℃ until the temperature reaches 3000 ℃, and treating for 8 hours to obtain a graphitization precursor;
step four, carbonizing
Adding the graphitized precursor and 1.5-3% of crushed asphalt into a mixer, uniformly mixing, then feeding into a roller kiln, performing high-temperature carbonization treatment for 4 hours at 1050 ℃, and performing secondary coating carbonization treatment to obtain a carbonized material;
step five, post-treatment
And storing the carbonized material in a carbonized material bin 71, mixing the carbonized material in a carbonized material mixer 72, a screening device 73, a demagnetizing device 74 and a packaging device 75, and mixing, screening, demagnetizing and packaging to obtain the artificial graphite cathode material for the lithium ion battery.
Example 3
This example provides a method for preparing an artificial graphite anode material for a lithium ion battery using the apparatus of example 1, the process is shown in fig. 9,
step one, pretreatment of raw materials
Firstly, needle coke is crushed into particles with the particle size less than or equal to 5mm by a shearing type crusher, and the particles are dried until the water content is less than 3 percent to obtain coarse powder petroleum coke;
selecting coating asphalt as solid asphalt with the softening point of 250 +/-5 ℃ obtained by purifying oil asphalt;
coarse needle coke is crushed, dried and mechanically ground into fine powder to obtain fine powder with the particle size of 9.0 +/-1.0 microns; carrying out fine pulverization treatment on the coated asphalt to obtain fine powder asphalt with the particle size of 5.0 +/-1.0 mu m, and mixing the needle coke raw coke fine powder: adding the asphalt fine powder of 85:15 into the modification unit 3;
step two, modification
The modification reaction kettle is filled with inert gas nitrogen in advance, and the inert gas is used for exhausting air in the reaction kettle;
feeding fine petroleum coke powder and fine asphalt powder into a fine powder feeding bin, pretreating, charging into a nitrogen modification reaction kettle, stirring the fine petroleum coke powder and the fine asphalt powder for 2 hours at 300 ℃, heating to 680 ℃, and statically modifying for 6 hours and 8 hours in a 680 ℃ temperature curve under the protection of inert gas to prepare a modified material with the particle size of 16.0 +/-2.0 mu m;
step three, depolymerization treatment
Storing the modified material in a modified powder feeding bin 41, opening a depolymerizer host 42, and allowing the modified material in the modified powder feeding bin 41 to enter a depolymerizer 43 through a first depolymerizing pipeline 44 for depolymerization to obtain a depolymerized precursor product;
step four, graphitization treatment
Cooling the depolymerized precursor product through a secondary kettle, putting the depolymerized precursor product into a box-type graphitization furnace, gradually heating to 2300 ℃ until the temperature reaches 3000 ℃, and treating for 8 hours to obtain a graphitization precursor;
step four, carbonizing
Adding the graphitized precursor and 1.5-3% of crushed asphalt into a mixer, uniformly mixing, then entering a roller kiln for high-temperature carbonization treatment for 6 hours at 1100 ℃, and performing secondary coating carbonization treatment to obtain a carbonized material;
step five, post-treatment
And storing the carbonized material in a carbonized material bin 71, mixing the carbonized material in a carbonized material mixer 72, a screening device 73, a demagnetizing device 74 and a packaging device 75, and mixing, screening, demagnetizing and packaging to obtain the artificial graphite cathode material for the lithium ion battery.
Example 4
This example provides a method for preparing an artificial graphite anode material for a lithium ion battery using the apparatus of example 1, the process is shown in fig. 9,
step one, pretreatment of raw materials
Firstly, crushing the asphalt coke into particles with the particle size of less than or equal to 5mm by using a shearing type crusher, and drying until the water content is less than 3 percent to obtain coarse powder petroleum coke;
selecting coating asphalt as solid asphalt with the softening point of 250 +/-5 ℃ obtained by purifying oil asphalt;
coarse petroleum coke powder is subjected to coarse crushing, drying and mechanical grinding and shaping to form fine powder, and the fine powder petroleum coke with the particle size of 8.5 +/-0.5 mu m is obtained; performing fine pulverization treatment on the coated asphalt to obtain fine powder asphalt with the particle size of 5.0 +/-1.0 mu m, and mixing the fine powder petroleum coke: adding 92:8 fine powder asphalt into the modification unit 3;
step two, modification
The modification reaction kettle is filled with inert gas nitrogen in advance, and the inert gas is used for exhausting air in the reaction kettle;
feeding fine petroleum coke and fine asphalt into a fine powder feeding bin, pretreating, filling the fine petroleum coke and the fine asphalt into a nitrogen modification reaction kettle, stirring the fine petroleum coke and the fine asphalt at 300 ℃ for 2 hours, heating to 650 ℃, and statically modifying for 6 hours and 8 hours in a 650 ℃ temperature curve under the protection of inert gas to obtain a modified material with the particle size of 16.0 +/-1.0 mu m;
step three, depolymerization treatment
Storing the modified material in a modified powder feeding bin 41, opening a depolymerizer host 42, and allowing the modified material in the modified powder feeding bin 41 to enter a depolymerizer 43 through a first depolymerizing pipeline 44 for depolymerization to obtain a depolymerized precursor product;
step four, graphitization treatment
Cooling the depolymerized precursor product through a secondary kettle, putting the depolymerized precursor product into a box-type graphitization furnace, gradually heating to 2300 ℃ until the temperature reaches 3000 ℃, and treating for 8 hours to obtain a graphitization precursor;
step four, carbonizing
Adding the graphitized precursor and 1.5-3% of crushed asphalt into a mixer, uniformly mixing, then entering a roller kiln for high-temperature carbonization treatment for 8 hours at 1000 ℃, and performing secondary coating carbonization treatment to obtain a carbonized material;
step five, post-treatment
And storing the carbonized material in a carbonized material bin 71, mixing the carbonized material in a carbonized material mixer 72, a screening device 73, a demagnetizing device 74 and a packaging device 75, and mixing, screening, demagnetizing and packaging to obtain the artificial graphite cathode material for the lithium ion battery.
Test examples
The artificial graphite anode materials prepared in examples 2 to 4 were tested, and the test results are shown in table 1.
TABLE 1
As can be seen from table 1, the device of the present invention is used to test and verify different raw materials such as needle coke, petroleum coke, pitch coke, etc. to obtain products with better performance indexes, the quality of the products is higher than the high standard, and the products can meet the market demand, and the device and the process design of the present invention have certain advantages in the test cost.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, it is intended that all such modifications and alterations be included within the scope of this invention as defined in the appended claims.
Claims (10)
1. An apparatus for preparing an artificial graphite negative electrode material for a lithium ion battery, comprising: the device comprises a material coarse crushing and drying unit, a mechanical grinding and shaping unit, a modification unit, a depolymerization unit, a graphitization unit, a carbonization unit and a post-treatment unit, wherein all the units are connected in sequence.
2. The device for preparing the artificial graphite anode material for the lithium ion battery as claimed in claim 1, wherein the material coarse crushing and drying unit comprises an original material feeding bin, a feeding belt, a raw material coarse crushing unit, a coarse crushing and drying unit and a cooling screw conveyer; the petroleum coke raw material in the raw material feeding bin enters the raw material coarse crushing unit through the feeding belt for coarse crushing, the coarse crushed material is dried in the coarse crushing and drying unit, and the dried material enters the mechanical grinding unit through the cooling screw conveyor.
3. The apparatus for preparing an artificial graphite anode material for lithium ion batteries according to claim 2, wherein the mechanical grinding and shaping unit comprises a coarse powder feeding bin, a grinding unit, a particle size grading unit, a shaping unit, a first grinding pipeline, a second grinding pipeline and a third grinding pipeline; wherein the coarse powder in the coarse crushing and drying unit enters a coarse powder feeding bin for storage and then enters a grinding unit, the ground material enters a particle size grading unit through a first grinding pipeline, the particle size under the composite condition after grading enters a shaping unit through a second grinding pipeline, and the shaped material enters a modification unit through a third grinding pipeline.
4. The device for preparing the artificial graphite anode material for the lithium ion battery as claimed in claim 3, wherein the modification unit comprises a fine powder feeding bin and a modification reaction kettle, wherein the material shaped in the mechanical grinding and shaping unit enters the fine powder feeding bin for storage, then enters the modification reaction kettle from the fine powder feeding bin for modification, and the modified material enters the depolymerization unit.
5. The apparatus for preparing artificial graphite cathode material for lithium ion battery according to claim 4, wherein the depolymerization unit comprises a modified powder feeding bin, a depolymerization machine host, a depolymerization machine, a first depolymerization pipeline, a second depolymerization pipeline, and the graphitization unit comprises a graphitization furnace; the material modified by the modification unit enters a modified powder feeding bin, after a depolymerizer main machine is opened, the material in the modified powder feeding bin enters a depolymerizer through a first depolymerizing pipeline for depolymerization, the depolymerized material enters a graphitization furnace through a second depolymerizing pipeline for graphitization, and the graphitized material after the graphitization treatment enters a carbonization unit; the graphitization furnace is a box-type graphitization furnace.
6. The device for preparing the artificial graphite cathode material for the lithium ion battery as claimed in claim 5, wherein the carbonization unit comprises a graphitized material feeding port, a mixer and a roller kiln; the graphitized material after treatment enters a mixer through a graphitized material feeding hole to be uniformly mixed, the uniformly mixed material enters a roller kiln to be carbonized, and the carbonized material enters an after-treatment unit.
7. The device for preparing the artificial graphite cathode material for the lithium ion battery according to claim 6, wherein the post-treatment unit comprises a carbonized material bin, a carbonized material mixer, a screening device, a demagnetizing device and a packaging device; the carbonized material is stored in a carbonized material bin, and then is mixed, screened, demagnetized and packaged by a carbonized material mixer, a screening device, a demagnetizing device and a packaging device in sequence.
8. The method for preparing the artificial graphite cathode material for the lithium ion battery by using the device for preparing the artificial graphite cathode material for the lithium ion battery according to any one of claims 1 to 7 is characterized by comprising the following steps of:
step one, raw material treatment
Firstly, coarsely crushing petroleum coke and drying to obtain coarse petroleum coke, and then performing fine powder shaping treatment on the coarse petroleum coke to obtain fine powder petroleum coke; carrying out fine pulverization treatment on the asphalt to obtain fine powder asphalt;
step two, modification
Performing modification treatment on the fine petroleum coke powder and the fine asphalt powder to obtain a granulation material;
step three, depolymerization
Depolymerizing the granulated material to obtain a cathode precursor product;
step four, graphitization treatment
Placing the cathode precursor product in a box-type graphitization furnace for high-temperature graphitization treatment to obtain a graphitized material;
step five, carbonizing
Adding 1.5-3% of crushed asphalt into the graphitized material, uniformly mixing in a mixer, and then entering a roller kiln for carbonization under the protection of nitrogen at 900-1200 ℃ to obtain a carbonized material;
step six, post-treatment
And mixing, screening, demagnetizing and packaging the carbonized material to obtain the artificial graphite cathode material for the lithium ion battery.
9. The method for preparing the artificial graphite anode material for the lithium ion battery as claimed in claim 8, wherein the petroleum coke is 2# A low-sulfur petroleum coke, NB/SH/T05272015 petroleum coke or 3# A petroleum coke;
and/or the asphalt is solid asphalt with the softening point of 150-350 ℃ obtained by purifying oil asphalt;
and/or the proportion of the fine petroleum coke and the fine asphalt is (85-97) to (3-15);
and/or in the second step, inert gas is filled into the modification reaction kettle in advance;
and/or in the second step, the modification method is that fine petroleum coke and fine asphalt in the modification reaction kettle are stirred for 2 hours at the temperature of 200-400 ℃, the temperature is raised to 650 ℃, and under the protection of inert gas, static modification is carried out for 6 hours in a temperature curve of 650 ℃;
and/or in the fourth step, the high-temperature graphitization treatment method is that the temperature of the box-type graphitization furnace is gradually increased, the temperature is increased to 2300 ℃ until the temperature is 3000 ℃, and the constant temperature is kept for 8 hours.
10. An artificial graphite negative electrode material, characterized in that it is produced by the method of claim 8 or 9.
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