CN113594403B - Granular carbon anode and preparation method and application thereof - Google Patents
Granular carbon anode and preparation method and application thereof Download PDFInfo
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- CN113594403B CN113594403B CN202110873322.7A CN202110873322A CN113594403B CN 113594403 B CN113594403 B CN 113594403B CN 202110873322 A CN202110873322 A CN 202110873322A CN 113594403 B CN113594403 B CN 113594403B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 238000005422 blasting Methods 0.000 claims abstract description 17
- 239000011812 mixed powder Substances 0.000 claims abstract description 17
- 239000011268 mixed slurry Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000000839 emulsion Substances 0.000 claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006258 conductive agent Substances 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 7
- 238000001125 extrusion Methods 0.000 claims description 14
- 239000006229 carbon black Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 5
- 239000002041 carbon nanotube Substances 0.000 claims description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 5
- 229910001416 lithium ion Inorganic materials 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 244000043261 Hevea brasiliensis Species 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 229920003052 natural elastomer Polymers 0.000 claims description 2
- 229920001194 natural rubber Polymers 0.000 claims description 2
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 2
- 239000004800 polyvinyl chloride Substances 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000002245 particle Substances 0.000 abstract description 19
- 238000003756 stirring Methods 0.000 abstract description 17
- 230000018044 dehydration Effects 0.000 abstract description 4
- 238000006297 dehydration reaction Methods 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 description 13
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 239000010405 anode material Substances 0.000 description 6
- 239000003292 glue Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000004898 kneading Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- NFMAZVUSKIJEIH-UHFFFAOYSA-N bis(sulfanylidene)iron Chemical compound S=[Fe]=S NFMAZVUSKIJEIH-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229910000339 iron disulfide Inorganic materials 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000001680 brushing effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000006256 anode slurry Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000006257 cathode slurry Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000011877 solvent mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a granular carbon anode and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) Mixing carbon material powder and copper powder to obtain mixed powder; (2) Mixing a solvent, a conductive agent slurry and a binder emulsion to obtain a mixed slurry; (3) The method optimizes the powder stirring process, saves the stirring time, omits a slurry dehydration process, saves the cost and improves the shot blasting uniformity of the carbon particle anode.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and relates to a granular carbon anode and a preparation method and application thereof.
Background
At present, in the preparation method of the lithium ion battery granular carbon anode at home and abroad, active substances, conductive agents, binders, solvents and the like are generally added into a traditional double-planet mixer to be mixed and stirred to prepare slurry, most of the solvents are removed from the slurry to obtain mixed semi-dry and wet solutes, the mixed solutes are extruded into strips by a granulator, and the strips are thrown by a shot blasting machine to form semi-dry and wet round granules.
CN101803065B discloses a primary cell having an anode comprising lithium and comprising iron disulfide (FeS) 2 ) And a cathode of carbon particles. The electrolyte comprises a lithium salt dissolved in a solvent mixture. The iron disulfide powder is preferably premixed with the carbon black and stored. A cathode slurry is prepared comprising iron disulfide powder, carbon black, a binder, and a liquid solvent. The mixture is coated onto a substrate and the solvent is evaporated, leaving a dried cathode coating on the substrate. The cathode coating is then baked at high temperature in an atmosphere under partial vacuum or in an atmosphere of nitrogen or an inert gas. The method needs to remove redundant solvent, waste is large, and in the process of removing the solvent, substances with small particle size, such as conductive agents, in the slurry can be removed, so that the solute ratio is unbalanced and the like.
CN112271285A discloses a preparation process of lithium ion battery anode slurry, which comprises the following steps: preparing anode powder; preparing polyvinylidene fluoride (PVDF) glue solution; uniformly adding a novel carbon black conductive agent ECP-600JD into a polyvinylidene fluoride glue solution, and fully stirring to obtain a carbon black conductive glue solution; uniformly adding the oil single-walled carbon nanotubes into the carbon black conductive glue solution, and stirring and dispersing to obtain composite conductive slurry; adding the anode powder into the composite conductive slurry for preliminary kneading; secondary kneading and stirring; adding the rest PVDF glue solution and appropriate NMP, and crushing and dispersing at high speed. The preparation method has the advantages of long process flow, high energy consumption and complex process.
The technical scheme has the problems of long process flow, high energy consumption or the need of removing excessive solvent, so that the development of the preparation method of the granular carbon anode, which has the advantages of simple flow, short time consumption and no need of removing the excessive solvent, is necessary.
Disclosure of Invention
The invention aims to provide a granular carbon anode and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a particulate carbon positive electrode, the method comprising the steps of:
(1) Mixing carbon material powder and copper powder to obtain mixed powder;
(2) Mixing a solvent, a conductive agent slurry and a binder emulsion to obtain a mixed slurry;
(3) And (3) carrying out screw extrusion on the mixed powder obtained in the step (1) and the mixed slurry obtained in the step (2), and carrying out shot blasting and drying treatment to obtain the granular carbon anode.
According to the invention, the mixed powder and the mixed slurry are prepared in advance and are fed through the feeding bin to be mixed, so that the powder stirring process is optimized, the stirring time is saved, the slurry dehydration process is omitted, the cost is saved, and the shot blasting uniformity of the carbon particle anode is improved.
The granular carbon anode prepared by the method has uniform granularity, higher liquid absorption rate and high specific discharge capacity.
Preferably, the carbon material powder of step (1) includes any one of carbon black powder, acetylene black, carbon fiber or carbon composite material or a combination of at least two thereof.
Preferably, the mass ratio of the carbon material powder to the copper powder is (97 to 98): 0.4 to 0.6), for example: 97, 0.4, 97.2.
Preferably, the revolution speed of the mixing in the step (1) is 9 to 11rpm, for example: 9rpm, 10rpm, 11rpm, or the like.
Preferably, the dispersion speed of the mixing in step (1) is 190 to 210rpm, for example: 190rpm, 195rpm, 200rpm, 205rpm, 210rpm, or the like.
Preferably, the mixing time in step (1) is 9 to 11min, for example: 9min, 9.5min, 10min, 10.5min, 11min, etc.
Preferably, the solvent of step (2) comprises water.
Preferably, the conductive agent slurry comprises any one of carbon nanotube slurry, conductive carbon black, conductive graphite and graphene slurry or a combination of at least two of the carbon nanotube slurry, the conductive carbon black, the conductive graphite and the graphene slurry.
Preferably, the binder emulsion comprises any one of or a combination of at least two of polytetrafluoroethylene emulsion, styrene-butadiene rubber emulsion, natural rubber emulsion or polyvinyl chloride resin.
Preferably, the revolution speed of the mixing in the step (2) is 14-16 rpm, for example: 14. 15 or 16, etc.
Preferably, the dispersion speed of the mixing in the step (2) is 490 to 510rpm, for example: 490rpm, 495rpm, 500rpm, 505rpm or 510rpm and the like.
Preferably, the mixing time in step (2) is 9 to 11min, for example: 9min, 9.5min, 10min, 10.5min or 11min and the like.
Preferably, during the screw extrusion process in the step (3), the flow rate of the mixed powder material feeding is 19 to 21L/min, for example: 19L/min, 19.5L/min, 20L/min, 20.5L/min or 21L/min, etc.
Preferably, during the screw extrusion in step (3), the flow rate of the mixed slurry is 9 to 11L/min, for example: 9L/min, 9.5L/min, 10L/min, 10.5L/min, 11L/min, etc.
Preferably, the temperature of the screw extrusion in step (3) is 20 to 30 ℃, for example: 20 ℃, 22 ℃, 25 ℃, 28 ℃ or 30 ℃ and the like.
Preferably, the solid content of the material obtained after the screw extrusion in the step (3) is 78-82%, for example: 78%, 79%, 80%, 81%, 82%, etc.
Preferably, the material extruded by the screw in the step (3) is in a strip shape.
Preferably, the temperature of the shot blasting in the step (3) is 55-65 ℃, for example: 55 deg.C, 58 deg.C, 60 deg.C, 62 deg.C or 65 deg.C.
Preferably, the temperature of the drying treatment in step (3) is 145-155 ℃, for example: 145 ℃, 148 ℃, 150 ℃, 152 ℃, 155 ℃ and the like.
Preferably, the drying treatment time is 3 to 4 hours, for example: 3h, 3.2h, 3.5h, 3.8h or 4h and the like.
In a second aspect, the present invention provides a particulate carbon positive electrode produced by the method of the first aspect.
Preferably, the particulate carbon positive electrode has a spherical structure.
Preferably, the particulate carbon positive electrode has a diameter of 1.8 to 2mm, for example: 1.8mm, 1.85mm, 1.9mm, 1.95mm, 2mm, or the like.
In a third aspect, the invention provides a lithium ion battery comprising a particulate carbon cathode as described in the second aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the mixed powder and the mixed slurry are prepared in advance and are fed through the feeding bin to be mixed, so that the powder stirring process is optimized, the stirring time is saved, the slurry dehydration process is omitted, the cost is saved, and the shot blasting uniformity of the carbon particle anode is improved.
(2) The carbon anode has a liquid absorption amount per unit volume of more than 3.53g, a discharge capacity of more than 0.980Ah, and a particle powder falling rate of less than 0.65%.
Drawings
FIG. 1 is a schematic view of an apparatus of a screw extruder described in example 1 of the present invention, including 1-a driving system, 2-a feeding system, 3-a temperature control system, 4-a vacuum system, 5-an extrusion hole, 6-a first feeding chamber, and 7-a second feeding chamber.
Fig. 2 is a schematic diagram of the shot blasting machine according to example 1 of the present invention, 8-granular carbon cathode material, 9-heating device, and 10-turntable.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitation of the present invention.
Example 1
The embodiment provides a preparation method of a granular carbon anode, which adopts a screw extruder shown in fig. 1 and a shot blasting machine shown in fig. 2 for preparation, wherein the screw extruder comprises a screw, one end of the screw is provided with an extrusion hole 5, the screw is provided with a feeding system 2, a temperature control system 3 and a vacuum system 4, the feeding system comprises a first feeding bin and a second feeding bin which are independent, and the screw extruder further comprises a driving system 1 connected with the screw;
the shot blasting machine comprises a rotary table 10 and a heating device 9 positioned below the rotary table 10;
the preparation method comprises the following specific steps:
(1) Adding 97.4kg of carbon black powder and 0.5kg of copper powder into a first feeding bin 6 of a screw extruder, preliminarily premixing the carbon powder and the copper powder, revolving at 10rpm, dispersing at 200rpm, mixing and stirring for 10min to obtain mixed powder;
(2) Adding 13.1kg of water, 10kg of carbon nanotube slurry and 4kg of polytetrafluoroethylene emulsion into a second feeding bin 7 of a screw extruder, mixing and stirring, and stirring for 10min according to revolution speed of 15rpm and dispersion speed of 500rpm to obtain mixed slurry;
(3) The driving system 1 is started, after the vacuum system 4 is vacuumized, the screw circulating cooling water of the temperature control system 3 is started, the temperature of the inner cavity of the screw is kept at 25 ℃, the feeding system 2 is started, meanwhile, the mixed powder in the first feeding bin 6 is opened to be fed at the flow rate of 20L/min, the mixed conductive slurry liquid in the second feeding bin 7 is fed at the flow rate of 10L/min, the mixed powder and the mixed slurry are continuously kneaded and sheared under the screw operated by the screw extruder, the mixture is fed forwards in a grinding mode, and the kneaded slurry is in a dough shape and has the solid content of 80%. Under the condition of continuous conveying of the screw, the screw is finally and continuously arranged at the end part of the screw
Extruding the mixture in the extrusion hole 5, performing shot blasting on the granular carbon anode material 8 at 60 ℃ by adjusting a heating device 9 of a shot blasting machine to form a rapeseed-shaped granular carbon anode material with uniform size, and baking the granular carbon anode material at 150 ℃ for 3.5 hours to obtain the granular carbon anode.
Example 2
The embodiment provides a preparation method of a granular carbon anode, which adopts the same screw extruder and shot blasting machine as those in the embodiment 1, and comprises the following specific steps:
(1) Adding 97.38kg of carbon black powder and 0.52g of copper powder into a first feeding bin 6 of a screw extruder, preliminarily premixing the carbon powder and the copper powder, revolving at 9rpm, dispersing at 210rpm, and mixing and stirring for 11min to obtain mixed powder;
(2) Adding 9.99g of water, 10.01g of carbon nano tube slurry and 4.02g of polytetrafluoroethylene emulsion into a second feeding bin 7 of a screw extruder, mixing and stirring, and stirring for 9min according to revolution of 16rpm and dispersion of 500rpm to obtain mixed slurry;
(3) Starting a driving system 1, after a vacuum system 4 is vacuumized, starting screw circulating cooling water of a temperature control system 3 to keep the temperature of an inner cavity of the screw at 25 ℃, starting a feeding system 2, simultaneously opening mixed powder in a first feeding bin 6 to feed at a flow rate of 20L/min, feeding mixed conductive slurry liquid in a second feeding bin 7 at a flow rate of 10L/min, and continuously kneading and shearing the mixed powder and the mixed slurry under the screw operated by a screw extruderCutting, grinding and conveying forward, wherein the kneaded slurry is in a dough shape and has a solid content of 81%. Under the condition of continuous conveying of the screw rotation, the screw is finally and continuously arranged at the end part of the screw
Extruding the mixture in the extrusion hole 5, performing shot blasting on the granular carbon anode material 8 at 62 ℃ by adjusting a heating device 9 of a shot blasting machine to form a rapeseed-shaped granular carbon anode material with uniform size, and baking the granular carbon anode material for 4 hours at 145 ℃ to obtain the granular carbon anode.
Example 3
The difference between this example and example 1 is that the flow rate of the first feeding bin 6 is 15L/min, and the other conditions and parameters are exactly the same as those in example 1.
Example 4
The difference between this example and example 1 is that the flow rate of the first feeding bin 6 is 25L/min, and the other conditions and parameters are the same as those in example 1.
Example 5
The difference between the embodiment and the embodiment 1 is that the flow rate of the blanking from the second feeding bin 7 is 5L/min, and the other conditions and parameters are the same as those of the embodiment 1.
Example 6
The difference between this example and example 1 is that the flow rate of the second feeding bin 7 is 15L/min, and the other conditions and parameters are exactly the same as those in example 1.
Example 7
The difference between the embodiment and the embodiment 1 is that the flow rate of the feeding material from the first feeding bin 6 is the same as the flow rate of the feeding material from the second feeding bin 7, and the flow rates are both 15L/min, and other conditions and parameters are completely the same as those of the embodiment 1.
Comparative example 1
The comparative example is different from example 1 only in that active materials, conductive agents, bonding agents, solvents and the like are added into a traditional double-planet mixer to be mixed and stirred to prepare slurry, and other conditions and parameters are completely the same as those of example 1.
And (4) performance testing:
preparing 200mL container, weighing, brushing 20 mesh net at the bottom of the container, allowing the solvent to pass through and the carbon particle anode to pass through, weighing 30 + -0.5 g of baked particle anode, putting into the container, and weighing. Weighing 100mL of absolute ethyl alcohol, pouring the absolute ethyl alcohol into a container filled with a carbon particle anode, after the absolute ethyl alcohol flows out of the container, the absolute ethyl alcohol does not flow out in strands, dripping for more than or equal to 1 second at intervals, weighing the total amount after liquid absorption, obtaining the liquid absorption amount of the carbon particle anode according to the difference of front and back weight meditation, assembling the prepared carbon particle anode into a cell with the standard capacity of 1Ah, controlling variables, carrying out a normal-temperature discharge test on the obtained battery, obtaining the performance comparison of the carbon particle anode according to the discharge result, weighing 200g of the baked carbon particle anode, passing through a 60-mesh brush net with the aperture of 250 mu m, vibrating and brushing, collecting and weighing falling powder, obtaining the particle powder falling rate according to weight calculation, wherein the test result is shown in Table 1:
TABLE 1
| Liquid absorption per unit volume/g | Discharge capacity/Ah | Particle dusting rate/%) | |
| Example 1 | 3.65 | 1.012 | 0.32％ |
| Example 2 | 3.64 | 1.009 | 0.35％ |
| Example 3 | 3.61 | 0.999 | 0.45％ |
| Example 4 | 3.60 | 0.993 | 0.48％ |
| Example 5 | 3.58 | 0.986 | 0.51％ |
| Example 6 | 3.55 | 0.981 | 0.57％ |
| Example 7 | 3.53 | 0.980 | 0.65％ |
| Comparative example 1 | 3.45 | 0.962 | 0.96％ |
As can be seen from table 1, the carbon anodes of the present invention have a liquid absorption per unit volume of 3.53g or more, a discharge capacity of 0.980Ah or more, and a particle chipping rate of 0.65% or less, as obtained in examples 1 to 7.
Compared with the embodiment 1 and the embodiment 3-4, the blanking flow rate of the first feeding bin can influence the performance of the prepared granular carbon electrode, the blanking flow rate of the first feeding bin is controlled to be 19-21L/min, the granular carbon anode with better effect can be prepared, if the blanking flow rate of the first feeding bin is too high, excessive powder is mismatched with the supply liquid amount of the second feeding bin, the pipeline opening is easily blocked by the powder, the solid content is too large, the equipment is seriously abraded, if the blanking flow rate of the first feeding bin is too low, the powder is too little, the slurry entering the pipeline opening is too thin, and the slurry kneading and shearing effects cannot be achieved.
Compared with the embodiment 1 and the embodiment 5-6, the embodiment 1 can obtain that the flow rate of the second feeding bin blanking affects the performance of the prepared granular carbon electrode, the flow rate of the second feeding bin blanking is controlled to be 9-11L/min, a granular carbon anode with a good effect can be prepared, if the flow rate of the second feeding bin blanking is too high, powder and excessive liquid enter a pipeline opening, the slurry is too thin, the slurry running-in and shearing effects cannot be achieved, if the flow rate of the second feeding bin blanking is too low, the powder and the supplied liquid are not matched too little, the powder is easy to block the pipeline opening, the solid content is larger, and the equipment is seriously worn.
Compared with the embodiment 7, the embodiment 1 has the advantages that the feeding speed of the mixed powder is higher than that of the mixed slurry by controlling the feeding flow rates of the first feeding bin and the second feeding bin, so that the slurry can be well and uniformly mixed to obtain the slurry with proper solid content, and further the granular carbon anode with excellent performance is prepared.
Compared with the embodiment 1 and the comparative example 1, the invention has the advantages that the mixed powder and the mixed slurry are prepared in advance and are fed through the feeding bin to be mixed, so that the powder stirring process is optimized, the stirring time is saved, the slurry dehydration procedure is omitted, the cost is saved, the shot blasting uniformity of the carbon particle anode is improved, the liquid absorption rate and the discharge capacity of the prepared particle carbon anode are improved, and the powder falling rate of the particle carbon anode is reduced.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed herein fall within the scope and disclosure of the present invention.
Claims (22)
1. A method for producing a particulate carbon positive electrode, comprising the steps of:
(1) Mixing carbon material powder and copper powder to obtain mixed powder;
(2) Mixing a solvent, a conductive agent slurry and a binder emulsion to obtain a mixed slurry;
(3) Carrying out screw extrusion on the mixed powder obtained in the step (1) and the mixed slurry obtained in the step (2), and carrying out shot blasting and drying treatment to obtain the granular carbon anode;
and (4) in the screw extrusion process in the step (3), the blanking flow rate of the mixed powder is 19 to 21L/min, and in the screw extrusion process in the step (3), the blanking flow rate of the mixed slurry is 9 to 11L/min.
2. The production method according to claim 1, wherein the carbon material powder of step (1) comprises carbon black powder and/or carbon fiber.
3. The production method according to claim 1, wherein the mass ratio of the carbon material powder to the copper powder is (97 to 98): 0.4 to 6).
4. The method according to claim 1, wherein the revolution speed of the mixing in the step (1) is 9 to 11rpm.
5. The method according to claim 1, wherein the dispersion speed of the mixing in the step (1) is 190 to 210rpm.
6. The method according to claim 1, wherein the mixing in step (1) is carried out for 9 to 11min.
7. The method of claim 1, wherein the solvent of step (2) comprises water.
8. The method of claim 1, wherein the conductive agent slurry comprises any one of a carbon nanotube slurry, a conductive carbon black slurry, a conductive graphite slurry, a graphene slurry, or a combination of at least two thereof.
9. The method of claim 1, wherein the binder emulsion comprises any one of or a combination of at least two of a polytetrafluoroethylene emulsion, a styrene-butadiene rubber emulsion, a natural rubber emulsion, or a polyvinyl chloride resin emulsion.
10. The method according to claim 1, wherein the revolution speed of the mixing in the step (2) is 14 to 169rpm.
11. The method according to claim 1, wherein the dispersion speed of the mixing in the step (2) is 490 to 510rpm.
12. The method according to claim 1, wherein the mixing in step (2) is carried out for 9 to 11min.
13. The method according to claim 1, wherein the screw extrusion temperature in the step (3) is 20 to 30 ℃.
14. The preparation method according to claim 1, wherein the solid content of the material obtained after the screw extrusion in the step (3) is 78 to 82%.
15. The method according to claim 1, wherein the material extruded by the screw in the step (3) is in the form of a strand.
16. The preparation method according to claim 1, wherein the temperature of the shot blasting in the step (3) is 55 to 65 ℃.
17. The method according to claim 1, wherein the temperature of the drying treatment in the step (3) is 145 to 155 ℃.
18. The production method according to claim 1, wherein the drying treatment is carried out for 3 to 4 hours.
19. A particulate carbon positive electrode produced by the method of any one of claims 1 to 18.
20. The particulate carbon positive electrode of claim 19, wherein the particulate carbon positive electrode is a spherical structure.
21. The granular carbon positive electrode according to claim 19, wherein the granular carbon positive electrode has a diameter of 1.8 to 2mm.
22. A lithium ion battery comprising the particulate carbon positive electrode of any one of claims 19-21.
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| CN105144324A (en) * | 2013-01-25 | 2015-12-09 | 康宁股份有限公司 | Method for manufacturing carbon electrode material using a twin screw extruder |
| CN109285990A (en) * | 2018-11-12 | 2019-01-29 | 武汉中原长江科技发展有限公司 | A kind of anode of lithium-thionyl chloride energy-type cells and preparation method thereof and lithium-thionyl chloride energy-type cells |
| CN109326779A (en) * | 2018-09-14 | 2019-02-12 | 桑顿新能源科技有限公司 | A kind of preparation method of high multiplying power lithium ion battery slurry |
| CN111525092A (en) * | 2020-04-28 | 2020-08-11 | 惠州亿纬锂能股份有限公司 | Pole piece, preparation method thereof and application of pole piece in battery |
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| CN112778762B (en) * | 2020-12-31 | 2023-01-10 | 上海聚威新材料股份有限公司 | Conductive PPS composite material and preparation method thereof |
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| CN105144324A (en) * | 2013-01-25 | 2015-12-09 | 康宁股份有限公司 | Method for manufacturing carbon electrode material using a twin screw extruder |
| CN109326779A (en) * | 2018-09-14 | 2019-02-12 | 桑顿新能源科技有限公司 | A kind of preparation method of high multiplying power lithium ion battery slurry |
| CN109285990A (en) * | 2018-11-12 | 2019-01-29 | 武汉中原长江科技发展有限公司 | A kind of anode of lithium-thionyl chloride energy-type cells and preparation method thereof and lithium-thionyl chloride energy-type cells |
| CN111525092A (en) * | 2020-04-28 | 2020-08-11 | 惠州亿纬锂能股份有限公司 | Pole piece, preparation method thereof and application of pole piece in battery |
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