CN113697806A - Liquid-crystal mechanical fusion coated artificial graphite material and preparation method thereof - Google Patents
Liquid-crystal mechanical fusion coated artificial graphite material and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- 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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- H—ELECTRICITY
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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention relates to a liquid-phase mechanical fusion coated artificial graphite material and a preparation method thereof. The method comprises the following steps: mechanically crushing petroleum coke raw materials, and then improving the appearance and removing fine powder by a shaping machine to obtain shaped powder; carrying out high-temperature heat treatment on the shaped powder to obtain an artificial graphite material A; taking the artificial graphite material A, adding a liquid phase coating agent, and stirring and mixing to obtain an artificial graphite material B; carrying out low-temperature heat treatment on the artificial graphite material B, and then crushing and shaping to obtain an artificial graphite material C; and placing the artificial graphite material C into a carbonization kiln for high-temperature treatment, cooling to room temperature after the treatment, crushing and grading to obtain the liquid-phase mechanically fused and coated artificial graphite material. The liquid phase coating mode is adopted, so that the materials are uniformly mixed and are not adhered, the emission of toxic and harmful gases is obviously reduced, the reversible capacity of the prepared material reaches 355mAh/g, the first effect reaches more than 94 percent, the compatibility with the electrolyte is good, and the internal resistance is obviously reduced.
Description
Technical Field
The invention belongs to the field of preparation and electrochemistry of modified artificial graphite materials for a negative electrode of a lithium battery, and particularly relates to a liquid-phase mechanical fusion coated artificial graphite material and a preparation method thereof.
Background
In the next decade, the artificial graphite negative electrode still has an unfortunate share in the lithium battery market. The artificial graphite prepared by the traditional process has high capacity, high first effect, high compaction and stable cycle performance, but has insufficient dynamic performance, and the negative impedance occupies a large proportion in the electrochemical test of the battery. The surface modification of the graphite negative electrode material is an effective method for improving the dynamic performance and reducing the internal resistance. Generally, graphite modification mainly adopts a solid-phase coating mode and a liquid-phase coating mode, the solid-phase coating mainly adopts petroleum or coal-series asphalt and other solid organic matter mixed materials for carbonization, but the problems of uneven asphalt mixed materials and the like are faced, carbonized products are poor in bonding and coating consistency, difficult to cool and easy to oxidize after being discharged from a furnace, poor in compatibility with electrolyte and obvious in first effect reduction; the liquid phase coating mode adopts a liquid organic coating agent, and compared with the solid phase mode, the solid-liquid mixed materials are uniform and are not easy to bond, but easily volatilize toxic and harmful gases, and the environmental protection pressure is large.
Therefore, the technical scheme of the invention is provided.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a liquid-crystal mechanical fusion coated artificial graphite material and a preparation method thereof. The liquid phase coating mode is adopted, so that the materials are uniformly mixed and are not adhered, the emission of toxic and harmful gases is obviously reduced, the reversible capacity of the prepared material reaches 355mAh/g, the first effect reaches more than 94 percent, the compatibility with the electrolyte is good, and the internal resistance is obviously reduced.
The scheme of the invention is to provide a preparation method of a liquid-phase mechanical fusion coated artificial graphite material, which comprises the following steps:
(1) mechanically crushing petroleum coke raw materials, and then improving the appearance and removing fine powder by a shaping machine to obtain shaped powder;
(2) carrying out high-temperature heat treatment on the shaped powder to obtain an artificial graphite material A;
(3) taking 100 parts by weight of the artificial graphite material A, adding 5-30 parts by weight of a liquid phase coating agent, and stirring and mixing to obtain an artificial graphite material B;
(4) carrying out low-temperature heat treatment on the artificial graphite material B, and crushing and shaping after the reaction is finished to obtain an artificial graphite material C;
(5) and placing the artificial graphite material C into a carbonization kiln for high-temperature treatment, cooling to room temperature after the treatment, crushing and grading to obtain the liquid-phase mechanically fused and coated artificial graphite material.
Preferably, in the step (1), the mechanical pulverization is carried out by one of a mechanical mill, a roll mill, a jet mill and a ball mill.
Preferably, in the step (2), the particle size of the artificial graphite material A is 6-15 μm; the high-temperature heat treatment adopts one of a box furnace or an Acheson furnace; the high temperature is 2200-3200 ℃.
Preferably, in the step (3), the rotating speed of stirring and mixing is 300-1100 r/min, and the linear speed of stirring and mixing is 5-30 m/s; the stirring and mixing time is 5-60 min, and the stirring and mixing temperature is 50-300 ℃. The stirring and mixing adopts high-speed stirring equipment suitable for solid-liquid phases, and a stirring shaft is a whole body and penetrates through the whole stirring kettle from top to bottom; the stirring kettle can be in a conical shape or a barrel shape; the stirring paddle is in the form of a knife or a punch.
Preferably, in the step (3), the liquid phase coating agent is a stripping byproduct of ethylene cracking tar, and is one or a mixture of more of heterocyclic aromatic hydrocarbon, ketone, hydrocarbon, resin, asphalt and heavy oil; the viscosity of the liquid phase coating agent is 100-2000 mm2And/s, the carbon residue value is 7-28%.
In the step (4), the low-temperature heat treatment equipment comprises a heating kettle and a cooling kettle; the heating kettle can be a roller furnace, a vertical reaction kettle or a horizontal reaction kettle, the temperature is controlled to be 350-700 ℃, the rotating speed is controlled to be 10-30r/min, and the time is controlled to be 4-24 h; when the heating kettle is started, nitrogen or other inert gases are introduced for whole-process protection, and exhaust gas is introduced into an environment-friendly device for absorption; the cooling kettle does not limit the type of equipment, and the discharging temperature is controlled to be less than or equal to 100 ℃ in a water cooling mode.
Preferably, in the step (4), the crushing and shaping equipment is an impact type grading mill, and fine powder is removed at the same time; the particle size of the artificial graphite material C is 10-25 μm.
Preferably, in the step (5), the temperature of the high-temperature treatment is 800-1300 ℃; the high-temperature treatment mode comprises the steps of heating for 4-8 hours, keeping the temperature for 4-8 hours and cooling for 4-8 hours; wherein, the loading manner adopts an automatic manner to load materials, and is implemented in a closed space, so as to avoid the overflow of volatile gas.
Preferably, in the step (5), a pin mill is adopted for crushing, and the frequency is 5-30 Hz; the grading mode adopts double-layer screen meshes for screening and grading, the upper layer screen mesh is 100-200 meshes, and the lower layer screen mesh is 300-400 meshes.
Based on the same technical concept, the invention also provides a liquid-phase mechanical fusion coated artificial graphite material prepared by the method.
The invention further provides a test method for the liquid-phase mechanical fusion coated artificial graphite material, which comprises the following steps:
(i) mixing the liquid-phase mechanically fused and coated artificial graphite material, the adhesive, the conductive agent and the solvent, and mixing the mixture together by a defoaming stirrer to prepare slurry A;
(ii) and uniformly coating the slurry A on a copper foil by using a scraper, drying, rolling, continuously drying in vacuum for 10-24h, punching into small pieces by using a cutting machine, and adding electrolyte to assemble a button cell for testing.
In the step (i), the adhesive is one or more of sodium carboxymethylcellulose, styrene butadiene rubber, polyvinylidene fluoride and polyacrylonitrile; the conductive agent is one or more of acetylene black, ketjen black, graphene and carbon nanotubes; the solvent is one of deionized water and N-methyl pyrrolidone.
In the step (ii), the coating thickness of the slurry A is 50-250 μm, the rolling thickness is 30-200 μm, and the electrolyte and the button cell accessories are commercially available conventional products.
The invention has the beneficial effects that:
the liquid-phase mechanical fusion coating artificial graphite material has the advantages of uniform coating, non-bonding of discharged particles, low temperature of discharged particles out of a roller kiln and easy subsequent processing; and through detection, the following steps are detected: the liquid-phase mechanical fusion coated artificial graphite material has less reversible capacity loss, the maximum material capacity is more than 355mAh/g, the compatibility with electrolyte is good, and the first effect can reach 95.5%; in the aspect of compaction, compared with the solid phase coated on 2T powder, the solid phase coated on the 2T powder can be improved by 0.02-0.05 g/cm3(ii) a The internal resistance is obviously reduced by 5-22%. Namely, the liquid-phase mechanical fusion coated artificial graphite material has the advantages of low specific surface area, high tap density, high powder pressure, good surface appearance, high charging and discharging efficiency, good cycle performance and excellent storage performance, and is charged into a furnace in a closed mode, so that the environmental protection pressure caused by the fact that toxic volatile gas is coated in a liquid phase is relieved.
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 is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an electron microscope image of the liquid phase mechanically fused coated artificial graphite material described in example 1.
FIG. 2 is a charge-discharge curve diagram of the liquid-phase mechanically fused coated artificial graphite material of example 1.
FIG. 3 is the electrochemical impedance spectrum of the liquid phase mechanofusion coated artificial graphite material described in example 1.
FIG. 4 is an X-ray diffraction pattern of the liquid phase mechanofusion coated artificial graphite material described in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
The embodiment provides a preparation method of a liquid-crystal mechanical fusion coated artificial graphite material, which comprises the following steps:
(1) crushing 1t of petroleum coke raw material by a mechanical mill, and then improving the appearance and removing fine powder by a shaping machine to obtain shaped powder;
(2) feeding the shaped powder into an Acheson graphitizing furnace, controlling the temperature by regulating and controlling the power transmission quantity, and carrying out high-temperature heat treatment at 3100-3200 ℃ to obtain an artificial graphite material A with the average particle size of 6 microns;
(3) the artificial graphite material A and a heterocyclic aromatic hydrocarbon liquid phase coating agent (the viscosity is 100 mm)2The carbon residue value is 7%) is mixed in a mechanical fusion machine according to the weight ratio of 100:5, and the mixture is stirred and mixed for 10min under the conditions of 300r/min and 50 ℃ to obtain an artificial graphite material B;
(4) carrying out low-temperature heat treatment on the artificial graphite material B by adopting a horizontal reaction kettle at the temperature of 500 ℃ and the rotating speed of 19r/min, introducing nitrogen for full protection, and absorbing the discharged tail gas by an environment-friendly device; discharging the material after the reaction at 80 ℃ through a cooling kettle, crushing the material by using a graded impact mill, and removing fine powder to obtain an artificial graphite material C with the particle size of 12 mu m;
(5) and (3) loading the artificial graphite material C into a carbonization kiln through an automatic loading device, carrying out high-temperature heat treatment, controlling the temperature to be 800 ℃, heating for 4 hours, keeping the temperature for 4 hours, cooling for 4 hours to room temperature, crushing by using a rod pin type mill, controlling the frequency to be 10Hz, then carrying out double-layer screening by using a 150+ 300-mesh screen, and taking the lower-layer material to obtain the liquid-phase mechanically fused and coated artificial graphite material.
The obtained liquid-phase mechanical fusion coated artificial graphite material is subjected to inspection and test, and specifically comprises the following steps:
(i) mixing the liquid-phase mechanically fused and coated artificial graphite material, styrene butadiene rubber, sodium carboxymethylcellulose, acetylene black and deionized water according to a ratio of 90:4:4:2:100, and mixing the materials together by a defoaming stirrer to prepare slurry A;
(ii) and uniformly coating the slurry A on a copper foil by using a scraper, wherein the coating thickness is 210 mu m, drying, rolling and pressing to obtain a rolled thickness of 156 mu m, continuously drying in vacuum for 12h, punching into a 16cm small wafer by using a cutting machine, and adding electrolyte to assemble a button cell for testing.
The results are shown in Table 1.
In addition, clearly evident states of lithium intercalation and deintercalation stages of graphite can be observed from fig. 2, and the first efficiency is calculated from the lithium intercalation and deintercalation capacities.
As can be seen from FIG. 3, the electrochemical impedance of the material prepared by the present invention is significantly better than that of the comparative example, which can be calculated or observed by the electrochemical impedance spectroscopy.
As can be seen from fig. 4, distinct and well-defined characteristic peaks of graphite can be observed without any negative influence on the microstructure.
Example 2
(1) Crushing 1t of petroleum coke raw material by a mechanical mill, and then improving the appearance and removing fine powder by a shaping machine to obtain shaped powder;
(2) feeding the shaped powder into an Acheson graphitizing furnace, controlling the temperature by regulating and controlling the power transmission, and carrying out high-temperature heat treatment at 2400-2500 ℃ to obtain an artificial graphite material A with the average particle size of 15 microns;
(3) the artificial graphite material A and a heterocyclic aromatic hydrocarbon liquid phase coating agent (the viscosity is 1000 mm)2The carbon residue value is 28%) according to the weight ratio of 100:30, stirring and mixing for 60min under the conditions of 800r/min and 300 ℃ to obtain an artificial graphite material B;
(4) carrying out low-temperature heat treatment on the artificial graphite material B by adopting a horizontal reaction kettle at the temperature of 550 ℃ and the rotating speed of 24r/min, introducing nitrogen for full protection, and absorbing the discharged tail gas by an environment-friendly device; discharging the material after the reaction at 80 ℃ through a cooling kettle, crushing the material by using a graded impact mill, and removing fine powder to obtain an artificial graphite material C with the granularity of 20 mu m;
(5) and (3) loading the artificial graphite material C into a carbonization kiln through an automatic loading device, carrying out high-temperature heat treatment, controlling the temperature to be 1300 ℃, heating for 8 hours, keeping the temperature for 8 hours, cooling for 8 hours to room temperature, crushing by using a rod pin type mill, controlling the frequency to be 15Hz, then carrying out double-layer screening by using a 150+ 350-mesh screen, and taking the lower-layer material to obtain the liquid-phase mechanically fused and coated artificial graphite material.
The obtained liquid-phase mechanical fusion coated artificial graphite material is subjected to inspection and test, and specifically comprises the following steps:
(i) mixing the liquid-phase mechanically fused and coated artificial graphite material, styrene butadiene rubber, sodium carboxymethylcellulose, acetylene black and deionized water according to a ratio of 90:4:4:2:100, and mixing the materials together by a defoaming stirrer to prepare slurry A;
(ii) and uniformly coating the slurry A on copper foil by using a scraper, wherein the coating thickness is 195 micrometers, drying, rolling to a thickness of 132 micrometers, continuously drying in vacuum for 12 hours, punching into a 16cm small wafer by using a cutting machine, and adding electrolyte to assemble a button cell for testing.
The results are shown in Table 1.
Example 3
(1) Crushing 1t of petroleum coke raw material by a mechanical mill, and then improving the appearance and removing fine powder by a shaping machine to obtain shaped powder;
(2) feeding the shaped powder into an Acheson graphitizing furnace, controlling the temperature by regulating and controlling the power transmission, and carrying out high-temperature heat treatment at 2800-2900 ℃ to obtain an artificial graphite material A with the average particle size of 11 mu m;
(3) the artificial graphite material A and a heterocyclic aromatic hydrocarbon liquid phase coating agent (with the viscosity of 600 mm) are mixed2/s, carbon residue value of 18%) in a mechanical fusion machine in a weight ratio of 100:15,stirring and mixing for 35min at 500r/min and 170 ℃ to obtain an artificial graphite material B;
(4) carrying out low-temperature heat treatment on the artificial graphite material B by adopting a horizontal reaction kettle at the temperature of 450 ℃ and the rotating speed of 24r/min, introducing nitrogen for full protection, and absorbing the discharged tail gas by an environment-friendly device; discharging the material after the reaction at 80 ℃ through a cooling kettle, crushing the material by using a graded impact mill, and removing fine powder to obtain an artificial graphite material C with the particle size of 16 mu m;
(5) and (3) loading the artificial graphite material C into a carbonization kiln through an automatic loading device, carrying out high-temperature heat treatment, controlling the temperature to be 1100 ℃, heating for 6h, keeping the temperature for 6h, cooling for 6h to room temperature, crushing by using a rod pin type mill, controlling the frequency to be 12Hz, then carrying out double-layer screening by using a 150+ 325-mesh screen, and taking the lower-layer material to obtain the liquid-phase mechanically fused and coated artificial graphite material.
The obtained liquid-phase mechanical fusion coated artificial graphite material is subjected to inspection and test, and specifically comprises the following steps:
(i) mixing the liquid-phase mechanically fused and coated artificial graphite material, styrene butadiene rubber, sodium carboxymethylcellulose, acetylene black and deionized water according to the proportion of 85:6:5:4:100, and mixing together by a defoaming stirrer to prepare slurry A;
(ii) uniformly coating the slurry A on a copper foil by using a scraper, wherein the coating thickness is 232 mu m, drying and rolling the copper foil, the rolling thickness is 161 mu m, continuously drying the copper foil in vacuum for 12h, punching the copper foil into a 16cm small wafer by using a cutting machine, and adding electrolyte to assemble a button cell for testing.
The results are shown in Table 1.
Carrying out electrochemical performance test on the batteries prepared in the three examples, and testing the first reversible capacity, the first coulombic efficiency, the powder compaction, the internal resistance and the cycle performance of the batteries; meanwhile, a solid phase coating method was used as a comparative example, the particle size of the graphitized material was 7 μm, the coating amount was the same as that of the first example, and the test results are shown in table 1.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (9)
1. A preparation method of a liquid-phase mechanical fusion coated artificial graphite material is characterized by comprising the following steps:
(1) mechanically crushing petroleum coke raw materials, and then improving the appearance and removing fine powder by a shaping machine to obtain shaped powder;
(2) carrying out high-temperature heat treatment on the shaped powder to obtain an artificial graphite material A;
(3) taking 100 parts by weight of the artificial graphite material A, adding 5-30 parts by weight of a liquid phase coating agent, and stirring and mixing to obtain an artificial graphite material B;
(4) carrying out low-temperature heat treatment on the artificial graphite material B, and crushing and shaping after the reaction is finished to obtain an artificial graphite material C;
(5) and placing the artificial graphite material C into a carbonization kiln for high-temperature treatment, cooling to room temperature after the treatment, crushing and grading to obtain the liquid-phase mechanically fused and coated artificial graphite material.
2. The method for preparing liquid-phase mechanically fused coated artificial graphite material according to claim 1, wherein in the step (1), the mechanical pulverization is carried out by one of mechanical milling, roller milling, jet milling or ball milling.
3. The method for preparing the liquid-phase mechanical fusion coated artificial graphite material according to claim 1, wherein in the step (2), the particle size of the artificial graphite material A is 6-15 μm; the high-temperature heat treatment adopts one of a box furnace or an Acheson furnace; the high temperature is 2200-3200 ℃.
4. The method for preparing the liquid-phase mechanical fusion coated artificial graphite material according to claim 1, wherein in the step (3), the rotation speed of stirring and mixing is 300-1100 r/min, and the linear speed of stirring and mixing is 5-30 m/s; the stirring and mixing time is 5-60 min, and the stirring and mixing temperature is 50-300 ℃.
5. The method for preparing the liquid-phase mechanically fused coated artificial graphite material according to claim 1, wherein in the step (3), the liquid-phase coating agent is a stripping byproduct of ethylene cracking tar, and is one or more of heterocyclic aromatic hydrocarbon, ketone, hydrocarbon, resin, asphalt and heavy oil; the viscosity of the liquid phase coating agent is 100-2000 mm2And/s, the carbon residue value is 7-28%.
6. The method for preparing liquid-phase mechanofusion coated artificial graphite material according to claim 1, wherein in the step (4), the crushing and shaping device is an impact type classifying mill, and fine powder is removed; the particle size of the artificial graphite material C is 10-25 μm.
7. The method for preparing the liquid-phase mechanical fusion coated artificial graphite material according to claim 1, wherein in the step (5), the temperature of the high-temperature treatment is 800-1300 ℃; the high-temperature treatment mode comprises the steps of heating for 4-8 hours, heat preservation for 4-8 hours and cooling for 4-8 hours.
8. The method for preparing the liquid-phase mechanical fusion coated artificial graphite material according to claim 1, wherein in the step (5), the crushing mode adopts a pin mill with the frequency of 5-30 Hz; the grading mode adopts double-layer screen meshes for screening and grading, the upper layer screen mesh is 100-200 meshes, and the lower layer screen mesh is 300-400 meshes.
9. The liquid-phase mechanically fused and coated artificial graphite material prepared by the method of any one of claims 1 to 8.
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| CN110642247A (en) * | 2019-09-30 | 2020-01-03 | 广东凯金新能源科技股份有限公司 | Artificial graphite negative electrode material, preparation method thereof and lithium ion battery |
| CN113213470A (en) * | 2021-05-07 | 2021-08-06 | 上海杉杉新材料有限公司 | Artificial graphite secondary particle, coating agent, preparation method and application thereof |
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- 2021-08-26 CN CN202110988702.5A patent/CN113697806A/en active Pending
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| CN104085883A (en) * | 2014-07-09 | 2014-10-08 | 深圳市贝特瑞新能源材料股份有限公司 | Artificial graphite negative electrode material for lithium ion battery and preparation method thereof |
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