CN112635715A - Lithium ion battery anode slurry, and homogenizing method and application thereof - Google Patents
Lithium ion battery anode slurry, and homogenizing method and application thereof Download PDFInfo
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- CN112635715A CN112635715A CN202011510117.6A CN202011510117A CN112635715A CN 112635715 A CN112635715 A CN 112635715A CN 202011510117 A CN202011510117 A CN 202011510117A CN 112635715 A CN112635715 A CN 112635715A
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000006256 anode slurry Substances 0.000 title claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 111
- 238000003756 stirring Methods 0.000 claims abstract description 105
- 239000002904 solvent Substances 0.000 claims abstract description 53
- 239000011230 binding agent Substances 0.000 claims abstract description 45
- 239000006258 conductive agent Substances 0.000 claims abstract description 37
- 238000005507 spraying Methods 0.000 claims abstract description 30
- 239000010405 anode material Substances 0.000 claims abstract description 20
- 239000011267 electrode slurry Substances 0.000 claims description 22
- 239000002033 PVDF binder Substances 0.000 claims description 11
- 238000000265 homogenisation Methods 0.000 claims description 10
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 9
- 239000007774 positive electrode material Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 239000006230 acetylene black Substances 0.000 claims description 4
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003273 ketjen black Substances 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 3
- 239000006245 Carbon black Super-P Substances 0.000 claims description 3
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 claims description 3
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 2
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 claims description 2
- 229940015043 glyoxal Drugs 0.000 claims description 2
- 229910002102 lithium manganese oxide Inorganic materials 0.000 claims description 2
- VLXXBCXTUVRROQ-UHFFFAOYSA-N lithium;oxido-oxo-(oxomanganiooxy)manganese Chemical compound [Li+].[O-][Mn](=O)O[Mn]=O VLXXBCXTUVRROQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000013557 residual solvent Substances 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims 1
- 238000007599 discharging Methods 0.000 abstract description 4
- 239000002002 slurry Substances 0.000 description 15
- 239000003292 glue Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000008595 infiltration Effects 0.000 description 4
- 238000001764 infiltration Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000011883 electrode binding agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- -1 for example Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/51—Methods thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/53—Mixing liquids with solids using driven stirrers
-
- 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
- H01M4/04—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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides lithium ion battery anode slurry, a homogenizing method and application thereof, wherein the homogenizing method comprises the following steps: and in the stirring process, sequentially adding conductive agent powder and binder powder, simultaneously adding part of solvent in a spraying manner, then adding anode material powder, and simultaneously adding the rest of solvent in a spraying manner to prepare the lithium ion battery anode slurry. According to the invention, the conductive agent, the binder and the anode material are all added in a powder form, the solvent is sprayed while the powder is added, the added solvent and the powder are continuously sprayed while stirring, and the powder is continuously kneaded to be uniformly stirred and dispersed, so that in the preferable range of the invention, the viscosity of the anode slurry of the lithium ion battery is 15000-22000 mpa · s, and when the average fineness is 4-8 μm, the total time from feeding to discharging is about 3.5h, the stirring time is shortened, and the cost is saved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, relates to a lithium ion battery anode slurry, and particularly relates to a lithium ion battery anode slurry, a homogenizing method and application thereof.
Background
The positive binder of the lithium iron phosphate cylindrical battery mostly adopts PVDF5130, and before slurry preparation, the positive binder PVDF5130 and a solvent NMP are dissolved to form a glue solution, and then positive slurry is prepared. The preparation process is mainly that the adhesive and the solvent are mixed to form glue solution, and then the glue solution and other materials are added into a stirring cylinder to be stirred according to different sequences and different qualities, so that the preparation of the slurry is completed.
However, the above method has the following disadvantages: 1) the PVDF5130 positive electrode binder is prepared into a glue solution, so that the process is complicated, the occupied area is large, and the consumed time is long; 2) the PVDF5130 glue solution participates in the preparation of the lithium iron phosphate anode slurry, the viscosity fluctuation is large and unstable, the solid content of the slurry is only about 59%, and the energy consumption of solvent evaporation in the coating and drying process is large; 3) after a large amount of solvent, powder and glue solution are added into the stirring cylinder, the powder is wrapped by the glue solution, the soaking is insufficient, the powder is not stirred and is not uniformly dispersed, the prepared positive plate has high rigidity and is not soft, and the cold-pressed positive plate is easy to crack; 4) the thick semi-dry semi-wet material layer which is easily formed on the inner wall of the stirring cylinder and the upper layer of the stirring paddle due to insufficient stirring is bonded on the inner wall of the stirring cylinder or the upper layer of the stirring paddle, cannot be stirred and dispersed, and the cylinder needs to be manually scraped; 5) the feeding sequence of one portion by one portion comprises about 6 hours from feeding to discharging, the homogenization takes long time, and the manufacturing cost is increased.
CN107910546A discloses a method for preparing a uniform slurry for a positive electrode of a lithium ion battery, which comprises: 1) weighing the following raw materials in parts by weight: 85-95 parts of a positive ternary material, 2-10 parts of a binder polyvinylidene fluoride, 0.5-5 parts of conductive carbon black powder and 0.1-5 parts of a surfactant; 2) measuring an organic solvent; 3) dissolving the weighed polyvinylidene fluoride powder serving as the binder into a weighed organic solvent, and stirring for 1-5 hours to obtain a PVDF solution; 4) adding the weighed conductive carbon black powder into the PVDF solution prepared in the step, and stirring for 1-10 hours to prepare a conductive adhesive; 5) adding the NCM dry powder into the conductive adhesive prepared in the step 4), adding the rest organic solvent, adding the surfactant, and stirring to obtain uniform slurry for the positive electrode of the lithium ion battery. According to the invention, the preparation process is adjusted and improved, and the prepared slurry can greatly improve the performance of the lithium battery. However, it has a problem of long homogenization time.
CN111834623A discloses a homogenizing method of silicon-based negative electrode slurry of a lithium ion battery, which comprises: adding a pure silicon system negative electrode material, diluted PAA binder glue solution and a conductive material into a double-planet stirrer, and stirring at a high speed; pouring graphite powder, and stirring to uniformly wet the graphite; adding PAA binder glue solution to adjust the solid content of the slurry to 60-65 wt%, stirring the slurry and kneading; adding PAA binder glue solution or deionized water to adjust the viscosity of the slurry to 3000-9000 mPa & s; adding Styrene Butadiene Rubber (SBR) dispersion, and stirring at a slow speed to be uniform. However, it has problems of insufficient wetting of the powder with the solvent, long homogenization time, and the like.
CN103230748A a method for mixing electrode slurry, comprising: 1) firstly, adding powdery raw materials to be mixed into a slurry stirring device for dry mixing to form uniform powdery slurry; 2) then automatically adding a certain amount of deionized water through a pipeline for wet mixing, so that the powdery dry materials are uniformly dispersed in the deionized water; 3) adding PTFE solution, quickly stirring until the slurry reaches the set viscosity, and then entering the next production procedure. The invention ensures that the slurry is mixed more uniformly and has better performance. However, the method still has the problems of insufficient infiltration of the solvent and the powder, long homogenization time and the like.
The existing homogenizing methods all have the problems of long homogenizing time, insufficient infiltration and the like, so that the problems which need to be solved urgently at present are solved by ensuring that the homogenizing method has the characteristics of short homogenizing time, sufficient infiltration and the like under the condition of simple operation.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the lithium ion battery anode slurry, the homogenizing method and the application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a homogenizing method of lithium ion battery anode slurry, which comprises the following steps:
and in the stirring process, sequentially adding conductive agent powder and binder powder, simultaneously adding part of solvent in a spraying manner, then adding anode material powder, and simultaneously adding the rest of solvent in a spraying manner to prepare the lithium ion battery anode slurry.
According to the invention, the conductive agent, the binder and the anode material are added in a powder form, and the solvent is sprayed while the powder is added, so that the powder is infiltrated and deposited at the bottom of the stirring cylinder as soon as possible, and the floating or adhesion on the inner wall of the stirring kettle and the stirring paddle is reduced. The added solvent and the powder are continuously sprayed and stirred while being kneaded to ensure that the powder is uniformly stirred and dispersed, the stirring time is shortened, and the cost is saved.
The stirring of the present invention is performed in a planetary mixer.
As a preferred embodiment of the present invention, the homogenization method specifically comprises:
sequentially adding conductive agent powder and binder powder under the condition of stirring, and simultaneously adding partial solvent in a spraying mode, wherein the conductive agent powder, the binder powder and the solvent are continuously added and simultaneously added;
(II) after the conductive agent powder and the binder powder are added, stirring for a certain time;
(III) adding the anode material powder under the stirring condition, simultaneously adding the residual solvent in a spraying mode, and continuously adding the anode material powder and the solvent, wherein the adding is completed simultaneously;
and (IV) after the addition is finished, continuously stirring for a certain time under a certain vacuum degree to prepare the lithium ion battery anode slurry.
In a preferred embodiment of the present invention, in the step (i), the revolution speed of the stirring is 8 to 12rpm, for example, 8.0rpm, 8.5rpm, 9.0rpm, 9.5rpm, 10.0rpm, 10.5rpm, 11.0rpm, 11.5rpm or 12.0 rpm.
Preferably, the rotation speed of the stirring is 180-220 rpm, for example, the rotation speed is 180rpm, 185rpm, 190rpm, 195rpm, 200rpm, 205rpm, 210rpm, 215rpm or 220 rpm.
According to the invention, when the conductive agent powder, the binder powder and the solvent are adopted, the revolution speed is 8-12 rpm, and the rotation speed is 180-220 rpm, so that the conductive agent powder, the binder powder and the solvent are soaked and fully stirred, the mixing effect is good, and the conductive agent powder and the binder powder are prevented from being agglomerated on the stirring paddle and the inner wall.
Preferably, the solvent is added in an amount of 50-60% of the total amount of the solvent, for example, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, or 60% of the total amount of the solvent.
Preferably, the stirring time is 20-40 min, for example, 20min, 22min, 24min, 26min, 28min, 30min, 32min, 34min, 36min, 38min or 40 min.
In a preferred embodiment of the present invention, in the step (ii), the revolution speed of the stirring is 8 to 12rpm, for example, 8.0rpm, 8.5rpm, 9.0rpm, 9.5rpm, 10.0rpm, 10.5rpm, 11.0rpm, 11.5rpm or 12.0 rpm.
Preferably, the rotation speed of the stirring is 900 to 1100rpm, for example, 900, 950, 1000, 1050 or 1100 rpm.
Preferably, the certain time is 10-20 min, for example, 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min or 20 min.
After the conductive agent powder, the binder powder and the solvent are mixed, the autorotation speed is increased and the mixture is stirred for a period of time, so that the conductive agent powder, the binder powder and the solvent are dispersed more uniformly.
In a preferred embodiment of the present invention, in the step (iii), the revolution speed of the stirring is 8 to 12rpm, for example, 8.0rpm, 8.5rpm, 9.0rpm, 9.5rpm, 10.0rpm, 10.5rpm, 11.0rpm, 11.5rpm or 12.0 rpm.
Preferably, the rotation speed of the stirring is 1300-1700 rpm, for example, the rotation speed is 1300rpm, 1350rpm, 1400rpm, 1450rpm, 1500rpm, 1550rpm, 1600rpm, 1650rpm or 1700 rpm.
Preferably, the stirring time is 90-120 min, for example, 90min, 95min, 100min, 105min, 110min, 115min or 120 min.
According to the invention, when the anode material powder is added, the revolution speed is 8-12 rpm, and the rotation speed is 1300-1700 rpm, so that the rotation speed is increased, the anode material powder is dispersed more uniformly in the stirring kettle, and the anode material is prevented from being aggregated into blocks.
In a preferred embodiment of the present invention, in the step (iv), the revolution speed of the stirring is 20 to 30rpm, for example, the revolution speed is 20rpm, 21rpm, 22rpm, 23rpm, 24rpm, 25rpm, 26rpm, 27rpm, 28rpm, 29rpm or 30 rpm.
Preferably, the rotation speed of the stirring is 2000 to 3000rpm, for example, 2000rpm, 2100rpm, 2200rpm, 2300rpm, 2400rpm, 2500rpm, 2600rpm, 2700rpm, 2800rpm, 2900rpm, or 3000 rpm.
Preferably, the vacuum is greater than or equal to 0.085MPa, for example, 0.085MPa, 0.090MPa, 0.095MPa, 0.0100MPa, 0.0200MPa or 0.030 MPa.
Preferably, the stirring time is 40-80 min, for example, 40min, 44min, 48min, 52min, 56min, 60min, 64min, 68min, 72min, 76min or 80 min.
According to the invention, after the conductive agent, the binder, the anode material and the solvent are added, the rotation speed and the revolution speed are improved, and the stirring kettle has a certain vacuum degree, so that the anode slurry is further uniformly mixed, and the influence of bubbles generated in the stirring process on the mixing effect is avoided.
In a preferred embodiment of the present invention, in the steps (I), (II) and (III), the revolution speeds of the stirring are equal.
As a preferred technical solution of the present invention, the conductive agent powder, the binder powder and the positive electrode material powder are all added by spraying.
As a further preferable technical solution, the method for homogenizing the lithium ion battery positive electrode slurry specifically comprises the following steps:
under the stirring condition, the revolution speed is 8-12 rpm, the rotation speed is 180-220 rpm, the conductive agent powder and the binder powder are sequentially added in a spraying manner, meanwhile, 50-60% of solvent is added in a spraying manner, the conductive agent powder, the binder powder and the solvent are continuously added and are added simultaneously, and the stirring time is 20-40 min;
(II) after the conductive agent powder and the binder powder are added, stirring for 10-20 min, wherein the revolution speed is 8-12 rpm, and the rotation speed is 900-1100 rpm;
(III) under the stirring condition, the revolution speed is 8-12 rpm, the rotation speed is 1300-1700 rpm, the anode material powder is added in a spraying mode, the rest solvent is added in a spraying mode, the anode material powder and the solvent are continuously added, the adding is completed simultaneously, and the stirring time is 90-120 min;
and (IV) after the addition is finished, continuously stirring for 40-80 min under the condition that a certain vacuum degree is not less than 0.085Mpa, wherein the revolution speed is 20-30 rpm, the rotation speed is 2000-3000 rpm, and the prepared lithium ion battery anode slurry has the viscosity of 15000-22000 Mpa & s and the average fineness of 4-8 mu m.
In a second aspect, the invention provides a lithium ion battery anode slurry, which is prepared by the lithium ion battery anode slurry homogenizing method of the first aspect.
In a preferred embodiment of the present invention, the lithium ion battery positive electrode slurry has a viscosity of 11000 to 22000mpa · s, for example, a viscosity of 11000mpa · s, 12000mpa · s, 13000mpa · s, 14000mpa · s, 15000mpa · s, 16000mpa · s, 17000mpa · s, 18000mpa · s, 19000mpa · s, 20000mpa · s, 21000mpa · s, or 22000mpa · s; more preferably 15000 to 22000mpa · s.
Preferably, the average fineness of the lithium ion battery positive electrode slurry is 3 to 13 μm, for example, the average fineness is 3.0, 4.0 μm, 4.5 μm, 5.0 μm, 5.5 μm, 6.0 μm, 6.5 μm, 7.0 μm, 7.5 μm, 8.0 μm, 9.0 μm, 10.0 μm, 11.0 μm, 12.0 μm or 13.0 μm, and more preferably 4 to 8 μm.
Preferably, the conductive agent powder comprises any one of Super-P, Ketjen black or acetylene black or a combination of at least two of the Super-P, the Ketjen black and the acetylene black.
Preferably, the binder powder comprises any one or a combination of at least two of polyvinylidene fluoride, polyvinylidene fluoride or styrene butadiene rubber.
It should be noted that the molecular weight of the binder is not specifically required and limited, and those skilled in the art can reasonably select the molecular weight of the binder according to the requirements of the slurry, for example, the binder is polyvinylidene fluoride with a weight of 10-15 w.
Preferably, the positive electrode material powder comprises any one of lithium iron phosphate, lithium cobaltate, lithium nickel cobalt manganese oxide, or lithium manganese oxide or a combination of at least two of the two.
Preferably, the solvent comprises any one of N-methyl pyrrolidone, acetone, ethanol, methyl acetone or glyoxal monobutyl ether or a combination of at least two thereof.
In a third aspect, the invention provides a lithium ion battery comprising the lithium ion battery positive electrode slurry according to the second aspect.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the conductive agent, the binder and the anode material are added in a powder form, and the solvent is sprayed while the powder is added, so that the powder is infiltrated and deposited at the bottom of the stirring cylinder as soon as possible, and the floating or adhesion on the inner wall of the stirring kettle and the stirring paddle is reduced. And continuously spraying and stirring the added solvent and the powder while adding, and continuously kneading to uniformly stir and disperse the powder, wherein in the preferred range of the invention, the viscosity of the lithium ion battery anode slurry is 15000-22000 mpa · s, the total time from feeding to discharging is about 3.5h when the average fineness is 4-8 mu m, the stirring time is shortened, and the cost is saved.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
Example 1
The embodiment provides a method for homogenizing lithium ion battery anode slurry, which specifically comprises the following steps:
under the stirring condition, the revolution speed is 10rpm, the rotation speed is 200rpm, Super P conductive agent powder and polyvinylidene fluoride binder powder are sequentially added in a spraying manner, 55% of N-methyl pyrrolidone solvent is added in a spraying manner, the conductive agent powder, the binder powder and the solvent are continuously added and are added simultaneously, and the stirring time is 30 min;
(II) after the conductive agent powder and the binder powder are added, stirring for 15min, wherein the revolution speed is 10pm, and the rotation speed is 1000 rpm;
(III) under the stirring condition, the revolution speed is 10rpm, the rotation speed is 1500rpm, the lithium iron phosphate anode material powder is added in a spraying manner, the rest solvent is added in a spraying manner, the anode material powder and the solvent are continuously added, the addition is completed simultaneously, and the stirring time is 105 min;
(IV) after the addition is finished, under a certain vacuum degree of 0.085Mpa, continuously stirring for 60min, wherein the revolution speed is 25rpm, the rotation speed is 2500rpm, and the lithium ion battery anode slurry is prepared, wherein the viscosity is 17000Mpa & s, and the average fineness is 6 mu m.
The total time of homogenization was 3.5 h.
Example 2
The embodiment provides a method for homogenizing lithium ion battery anode slurry, which specifically comprises the following steps:
under the stirring condition, the revolution speed is 8rpm, the rotation speed is 220rpm, Ketjen black conductive agent powder and polyvinylidene fluoride binder powder are sequentially added in a spraying manner, 60% acetone solvent is added in a spraying manner, the conductive agent powder, the binder powder and the solvent are continuously added and are added simultaneously, and the stirring time is 20 min;
(II) after the conductive agent powder and the binder powder are added, stirring for 20min, wherein the revolution speed is 12pm, and the rotation speed is 900 rpm;
(III) under the stirring condition, the revolution speed is 8rpm, the rotation speed is 1300rpm, the nickel cobalt lithium manganate positive electrode material powder is added in a spraying manner, meanwhile, the rest solvent is added in a spraying manner, the positive electrode material powder and the solvent are continuously added, the addition is finished simultaneously, and the stirring time is 120 min;
and (IV) after the addition is finished, continuously stirring for 80min under a certain vacuum degree of 0.090Mpa, wherein the revolution speed is 30rpm, the rotation speed is 2000rpm, and the prepared lithium ion battery anode slurry has the viscosity of 17500Mpa & s and the average fineness of 7 mu m.
The total homogenization time amounted to 4.0 h.
Example 3
The embodiment provides a method for homogenizing lithium ion battery anode slurry, which specifically comprises the following steps:
under the stirring condition, the revolution speed is 12rpm, the rotation speed is 180rpm, acetylene black conductive agent powder and styrene butadiene rubber binder powder are sequentially added in a spraying manner, 50% methyl acetone solvent is added in a spraying manner, the conductive agent powder, the binder powder and the solvent are continuously added and are added simultaneously, and the stirring time is 40 min;
(II) after the conductive agent powder and the binder powder are added, stirring for 10min, wherein the revolution speed is 8pm, and the rotation speed is 1100 rpm;
(III) under the stirring condition, the revolution speed is 12rpm, the rotation speed is 1700rpm, lithium cobaltate anode material powder is added in a spraying mode, the rest solvent is added in a spraying mode, the anode material powder and the solvent are continuously added, the adding is completed simultaneously, and the stirring time is 90 min;
(IV) after the addition is finished, under a certain vacuum degree of 0.095Mpa, continuously stirring for 40min, wherein the revolution speed is 20rpm, the rotation speed is 3000rpm, and the lithium ion battery anode slurry is prepared, wherein the viscosity is 18000Mpa & s, and the average fineness is 6 mu m.
The total time of homogenization amounted to 3.0 h.
Example 4
This example provides a method for homogenizing lithium ion battery positive electrode slurry, which is different from example 1 in that in step (i), the rotation speed of the stirring is 150rpm, the rest of the operation steps and operation parameters are identical to those of example, and the total time of homogenizing is also identical to example 1.
The prepared lithium ion battery positive electrode slurry has the viscosity of 14000mpa · s and the average fineness of 10 μm.
Example 5
This example provides a method for homogenizing lithium ion battery positive electrode slurry, which is different from example 1 in that in step (i), the rotation speed of the stirring is 240rpm, the rest of the operation steps and operation parameters are identical to those of example, and the total time of homogenizing is also identical to example 1.
The prepared lithium ion battery anode slurry has the viscosity of 13000mpa · s and the average fineness of 12 mu m.
Example 6
This example provides a method for homogenizing lithium ion battery positive electrode slurry, which is different from example 1 in that the rotation speed of the stirring in step (ii) is 700rpm, the rest of the operation steps and operation parameters are identical to those of example, and the total time of homogenizing is also identical to that of example 1.
The prepared lithium ion battery positive electrode slurry has the viscosity of 14000mpa · s and the average fineness of 10 μm.
Example 7
This example provides a method for homogenizing lithium ion battery positive electrode slurry, which is different from example 1 in that in step (ii), the rotation speed of the stirring is 1400rpm, the rest of the operation steps and operation parameters are identical to those of example, and the total homogenizing time is also identical to that of example 1.
The prepared lithium ion battery anode slurry has the viscosity of 13000mpa · s and the average fineness of 12 mu m.
Example 8
This example provides a method for homogenizing lithium ion battery positive electrode slurry, which is different from example 1 in that in step (iv), the revolution speed of the stirring is 10rpm, the rest of the operation steps and operation parameters are identical to those of example, and the total time of homogenizing is also identical to that of example 1.
The prepared lithium ion battery positive electrode slurry has the viscosity of 12000mpa · s and the average fineness of 13 μm.
Example 9
This example provides a method for homogenizing lithium ion battery positive electrode slurry, which is different from example 1 in that in step (iv), the revolution speed of the stirring is 40rpm, the rest of the operation steps and operation parameters are identical to those of example, and the total time of homogenizing is also identical to that of example 1.
The prepared lithium ion battery anode slurry has the viscosity of 11000mpa · s and the average fineness of 3 μm.
It can be seen from examples 4 to 9 that, although the time for homogenization was the same as in example 1, the effects of increasing or decreasing the rotation speed in step (i), the rotation speed in step (ii), and the revolution speed in step (iv) to prepare the positive electrode slurry with the viscosity and average fineness were not as good as the effects of controlling the rotation speed in step (i) to 180 to 220rpm, the rotation speed in step (ii) to 900 to 1100rpm, and the revolution speed in step (iv) to 20 to 30 rpm.
In conclusion, the conductive agent, the binder and the positive electrode material are added in a powder form, and the solvent is sprayed while the powder is added, so that the powder is infiltrated and deposited at the bottom of the stirring cylinder as soon as possible, the floating or adhesion of the powder on the inner wall of the stirring kettle and the stirring paddle is reduced, the conductive agent and the binder are added firstly, the positive electrode material is added, the infiltration of the conductive agent, the binder, the positive electrode material and other powder is facilitated, and the problem of unbalanced ratio caused by the floating and adhesion of the powder on the inner wall of the stirring kettle and the stirring paddle is reduced. And continuously spraying and stirring the added solvent and the powder while adding, and continuously kneading to uniformly stir and disperse the powder, wherein within the preferable parameter range of the invention, the viscosity of the lithium ion battery anode slurry is 15000-22000 mpa · s, the total time from feeding to discharging is about 3.5h when the average fineness is 4-8 mu m, the stirring time is shortened, and the cost is saved.
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 are within the scope and disclosure of the present invention.
Claims (10)
1. A homogenizing method of lithium ion battery anode slurry is characterized by comprising the following steps:
and in the stirring process, sequentially adding conductive agent powder and binder powder, simultaneously adding part of solvent in a spraying manner, then adding anode material powder, and simultaneously adding the rest of solvent in a spraying manner to prepare the lithium ion battery anode slurry.
2. A method for homogenizing according to claim 1, characterized in that it comprises in particular:
sequentially adding conductive agent powder and binder powder under the condition of stirring, and simultaneously adding partial solvent in a spraying mode, wherein the conductive agent powder, the binder powder and the solvent are continuously added and simultaneously added;
(II) after the conductive agent powder and the binder powder are added, stirring for a certain time;
(III) adding the anode material powder under the stirring condition, simultaneously adding the residual solvent in a spraying mode, and continuously adding the anode material powder and the solvent, wherein the adding is completed simultaneously;
and (IV) after the addition is finished, continuously stirring for a certain time under a certain vacuum degree to prepare the lithium ion battery anode slurry.
3. The homogenizing method according to claim 2, wherein in the step (I), the revolution speed of the stirring is 8 to 12 rpm;
preferably, the rotation speed of the stirring is 180-220 rpm;
preferably, the addition amount of the solvent accounts for 50-60% of the total addition amount of the solvent;
preferably, the stirring time is 20-40 min.
4. A method for homogenizing according to claim 2 or 3, wherein in the step (II), the revolution speed of the stirring is 8 to 12 rpm;
preferably, the rotation speed of the stirring is 900-1100 rpm;
preferably, the certain time is 10-20 min.
5. The homogenizing method according to any one of claims 2 to 4, wherein in the step (III), the revolution speed of the stirring is 8 to 12 rpm;
preferably, the rotation speed of the stirring is 1300-1700 rpm;
preferably, the stirring time is 90-120 min.
6. The homogenizing method according to any one of claims 2 to 5, wherein in the step (IV), the revolution speed of the stirring is 20 to 30 rpm;
preferably, the rotation speed of the stirring is 2000-3000 rpm;
preferably, the vacuum degree is more than or equal to 0.085 MPa;
preferably, the stirring time is 40-80 min.
7. A method of homogenizing according to any one of claims 2-6 wherein in steps (I), (II) and (III) the agitation revolution speed is equal;
preferably, the conductive agent powder, the binder powder and the positive electrode material powder are all added by spraying.
8. A lithium ion battery positive electrode slurry, which is prepared by the homogenization method of the lithium ion battery positive electrode slurry according to any one of claims 1 to 7.
9. The lithium ion battery positive electrode slurry according to claim 8, wherein the viscosity of the lithium ion battery positive electrode slurry is 11000 to 22000 mpa-s, and more preferably 15000 to 22000 mpa-s;
preferably, the average fineness of the lithium ion battery positive electrode slurry is 3-13 μm, and further preferably 4-8 μm;
preferably, the conductive agent powder comprises any one or a combination of at least two of Super-P, Ketjen black or acetylene black;
preferably, the binder powder comprises any one or a combination of at least two of polyvinylidene fluoride, polyvinylidene fluoride or styrene butadiene rubber;
preferably, the positive electrode material powder comprises any one or a combination of at least two of lithium iron phosphate, lithium cobaltate, lithium nickel cobalt manganese oxide and lithium manganese oxide;
preferably, the solvent comprises any one of N-methyl pyrrolidone, acetone, ethanol, methyl acetone or glyoxal monobutyl ether or a combination of at least two thereof.
10. A lithium ion battery comprising the lithium ion battery positive electrode slurry of claim 9.
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