CN113224267A - Efficient and high-solid-content ternary material slurry mixing process - Google Patents
Efficient and high-solid-content ternary material slurry mixing process Download PDFInfo
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- CN113224267A CN113224267A CN202110448987.3A CN202110448987A CN113224267A CN 113224267 A CN113224267 A CN 113224267A CN 202110448987 A CN202110448987 A CN 202110448987A CN 113224267 A CN113224267 A CN 113224267A
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- 239000002002 slurry Substances 0.000 title claims abstract description 84
- 238000002156 mixing Methods 0.000 title claims abstract description 48
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 43
- 230000008569 process Effects 0.000 title claims abstract description 39
- 238000003756 stirring Methods 0.000 claims abstract description 76
- 239000003292 glue Substances 0.000 claims abstract description 52
- 238000004898 kneading Methods 0.000 claims abstract description 49
- 239000002033 PVDF binder Substances 0.000 claims abstract description 45
- 239000007787 solid Substances 0.000 claims abstract description 33
- 239000006258 conductive agent Substances 0.000 claims abstract description 18
- 238000007580 dry-mixing Methods 0.000 claims abstract description 15
- 238000007873 sieving Methods 0.000 claims abstract description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 42
- 239000006185 dispersion Substances 0.000 claims description 34
- 238000007790 scraping Methods 0.000 claims description 26
- 238000004537 pulping Methods 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 16
- 238000010586 diagram Methods 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000007599 discharging Methods 0.000 description 4
- 230000004580 weight loss Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000012360 testing method Methods 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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
-
- 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
Abstract
The invention provides a high-efficiency and high-solid content ternary material slurry mixing process, which comprises the steps of firstly dissolving a PVDF binder to prepare a glue solution, then dry-mixing a ternary material and a conductive agent, adding the glue solution and CNT to knead, adding a part of the glue solution again to perform high-viscosity stirring after the kneading is finished, adding the rest of the glue solution to perform low-viscosity stirring after the high-viscosity stirring is finished, and sieving after the stirring is finished and defoaming is performed, thus finishing the preparation of the slurry. The efficient and high-solid-content ternary material slurry mixing process disclosed by the invention has the advantages that the glue solution is prepared in advance, and the problems that the PVDF binder cannot be fully dissolved and the viscosity is unstable in dry-method slurry mixing are solved; in addition, the main material and the conductive agent are subjected to dry mixing and kneading processes, so that the problems that the conductive agent SP in the wet process cannot be fully and uniformly dispersed in the glue solution and is easy to agglomerate are solved; the slurry prepared by the slurry mixing process has high solid content, reduces the addition of a solvent and the energy consumption of coating and drying equipment, and has the advantages of short time and low internal resistance of the pole piece.
Description
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a high-efficiency and high-solid-content ternary material slurry mixing process.
Background
At present, lithium ion batteries are rapidly developed on the aspects of vehicles, 3C and energy storage power stations, new technologies are continuously updated and iterated, and batteries with high energy density, quick charge systems and low cost are always pursued by a host factory, which provides higher requirements for battery design and manufacturing capacity and is a huge challenge faced by the battery factory, but the challenge and the opportunity coexist. The manufacturing process is the key of success, the first procedure in the lithium ion battery production and manufacturing process is a slurry mixing process, the overall performance of the battery is determined by the slurry mixing quality, the conventional ternary material slurry mixing process mainly adopts two modes of wet slurry mixing and dry slurry mixing, wherein the wet slurry mixing is the main mode, and the dry slurry mixing is only used by a few manufacturers.
The two processes have respective advantages and disadvantages, and the battery pole piece manufactured by the wet slurry mixing process has the problems of large internal resistance, poor dispersibility, low production efficiency, low solid content of slurry and the like. The dry method has high slurry mixing efficiency, but PVDF cannot be completely dissolved, and the viscosity of the slurry is unstable, so that the later coating has a large risk, as shown in FIG. 9, PVDF is added at the early stage, NMP solvent is added at the kneading stage, PVDF can be gradually dissolved to form the slurry with viscosity, serious aggregates appear, the slurry is difficult to open due to the agglomeration, and the slurry in the aggregates cannot be sufficiently wetted, rubbed and kneaded. The two processes also cause the influences of unstable battery performance, poor battery cell rate performance, fast attenuation of long-cycle capacity, poor high-temperature cycle and the like.
Disclosure of Invention
In view of the above, the invention aims to provide an efficient and high-solid-content ternary material slurry mixing process to avoid the problems of insufficient dissolution of dry slurry mixing PVDF, unstable viscosity, low production efficiency of wet slurry mixing, low solid content and poor dispersibility.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
an efficient and high-solid-content ternary material slurry mixing process comprises the following steps:
(1) preparing PVDF glue solution;
(2) dry-mixing a conductive agent SP and a ternary material to obtain a dry mixture;
(3) adding Carbon Nano Tubes (CNT) and part of PVDF glue solution into the dry mixture for kneading and scraping to obtain first pre-pulping;
(4) adding part of PVDF glue solution in the first pre-pulping process, stirring at high viscosity, and scraping to obtain a second pre-pulping process;
(5) adding all the residual PVDF glue solution into the second pre-prepared pulp, stirring at low viscosity, and scraping to obtain third pre-prepared pulp;
(6) and vacuumizing the third pre-pulping to remove bubbles, and sieving by using a sieve to obtain the required pulp.
Preferably, the dry mixing in step (2) comprises the following specific operation steps: firstly adding 50% of ternary material, then adding conductive agent SP, and finally adding the rest 50% of ternary material, wherein the revolution (reversal) speed of the stirrer is 15-25rpm, the dispersion speed is 500-1500rpm, and the stirring time is 20-45 min.
Preferably, the dry mixing material in the step (2) is kept still for 10min after the dry mixing is finished, and then the step (3) is carried out.
Preferably, the kneading in step (3) comprises the following specific steps: the kneading temperature is less than or equal to 35 ℃, low-speed kneading is carried out firstly, the revolution speed of the stirrer is 10-20rpm, the low-speed kneading time is 10-20min, then high-speed kneading is carried out, the revolution speed of the stirrer is 20-30rpm, the dispersion speed is 500-1000rpm, and the high-speed kneading time is 25-45 min.
Preferably, the solids content of the first pre-pulping is from 86% to 89%.
Preferably, the revolution speed of the stirrer during high-viscosity stirring in the step (4) is 20-30rpm, the dispersion speed is 1500-2500rpm, the stirring time is 70-110min, the stirring temperature is less than or equal to 35 ℃, and the vacuum degree is-90 kpa.
Preferably, the solids content of the second pre-pulping is 81-85%.
Preferably, the low viscosity stirring in step (5) comprises the following specific operation steps: the low-viscosity stirring temperature is less than or equal to 35 ℃, the vacuum degree is-90 kpa, primary stirring is firstly carried out, the revolution speed of the stirrer is 20-30rpm, the dispersion speed is 3000rpm, the primary stirring time is 10-30min, secondary stirring is carried out, the revolution speed of the stirrer is 30-40rpm, the dispersion speed is 3000rpm 4000rpm, and the secondary stirring time is 80-120 min.
Preferably, in the step (6), the revolution (reverse rotation) speed of the stirrer during vacuum defoaming is 15rpm, the temperature is less than or equal to 35 ℃, the vacuum degree is-90 kpa, the time is 60min, and the mesh number of the screen is 150 meshes.
Preferably, the specific operation steps for preparing the PVDF glue solution in the step (1) are as follows: preparing glue solution by using a certain amount of adhesive polyvinylidene fluoride (PVDF) and N-methyl pyrrolidone (NMP) according to the solid content of 6%, adding an NMP solution, adding PVDF, mixing and stirring at a low speed, wherein the revolution speed of a stirrer is 10-20rpm, the dispersion speed is 500 plus 1500rpm, the time is 10min, stirring at a medium speed, the revolution speed of the stirrer is 20-30rpm, the dispersion speed is 2000 plus 3000rpm, the time is 20min, stirring at a high speed, the revolution speed of the stirrer is 30-40rpm, the dispersion speed is 3000 plus 4000rpm, and the time is 240min to obtain PVDF glue solution, and stirring and storing the PVDF glue solution at a low speed for later use under a vacuum condition, wherein the revolution speed of the stirrer is 15rpm, and the time is more than 180 min.
Compared with the prior art, the efficient and high-solid-content ternary material slurry mixing process has the following advantages:
the efficient and high-solid-content ternary material slurry mixing process disclosed by the invention has the advantages that the glue solution is prepared in advance, and the problems that the PVDF binder cannot be fully dissolved and the viscosity is unstable in dry-method slurry mixing are solved; in addition, the main material and the conductive agent are subjected to dry mixing and kneading processes, so that the problems that the conductive agent SP in the wet process cannot be fully and uniformly dispersed in the glue solution and is easy to agglomerate are solved; the slurry prepared by the slurry mixing process has high solid content, reduces the addition of a solvent and the energy consumption of coating and drying equipment, and has the advantages of short time and low internal resistance of the pole piece.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a schematic diagram of the fineness of the slurry prepared in example 2 of the present invention;
FIG. 3 is a schematic view showing the discharge state of the slurry prepared in example 2 of the present invention;
FIG. 4 is a schematic view showing a state in which a slurry obtained in example 2 of the present invention is sieved;
FIG. 5 is a graph showing the 48h viscosity and solids profile of the slurry prepared in example 2 of the present invention;
FIG. 6 is a schematic diagram of the coating adhesion and weight loss rate change curves of the slurry electrode plate prepared in example 2 of the present invention;
FIG. 7 is a schematic view showing a state of a slurry at a kneading stage of a comparative example of the present invention;
FIG. 8 is a schematic view showing the state of a slurry at the kneading stage in example 2 of the present invention;
FIG. 9 is a schematic diagram showing the state of slurry at the kneading stage of conventional dry mixing.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The invention is described in detail below with reference to the following embodiments and accompanying drawings, fig. 1 is a schematic process flow diagram of the invention, and the mass ratio of the positive electrode system of the invention is: mTernary material:MConductive agent SP:MCNT conductive paste:MPVDF513097:1:0.5: 1.5; and in the slurry mixing stage, if the temperature is less than or equal to 35 ℃, the cooling water is closed, otherwise, the cooling water is opened for cooling.
Example 1
1. Preparing glue solution by using binders polyvinylidene fluoride (PVDF 5130) and N-methyl pyrrolidone (NMP) according to the solid content of 6%, firstly adding an NMP solution, then adding the PVDF 5130 binder, mixing and stirring at a low speed (revolution 10rpm, dispersion 500rpm, time 10min) to obtain glue solution 1, then stirring at a medium speed (revolution 20rpm, dispersion 2000rpm, time 20min) to obtain glue solution 2, finally stirring at a high speed (revolution 30rpm, dispersion 3000rpm, time 240min) to obtain glue solution 3, namely PVDF glue solution, and storing the PVDF glue solution under a vacuum condition by stirring at a low speed (revolution 15rpm, time more than 180 min).
2. And (3) dry-mixing the conductive agent SP and the ternary material, adding 50% of the ternary material, adding the conductive agent SP, and adding 50% of the ternary material again for mixing (revolution (inversion) at 15rpm, dispersion at 500rpm, and time 20 min).
3. And standing for 10min after mixing is finished, adding CNT and part of PVDF glue solution, kneading, controlling the solid content of kneading to be 86%, firstly kneading at a low speed (revolution at 10rpm for 10min and the temperature of no more than 35 ℃), scraping pulp after the low speed kneading is finished, then continuously stirring and kneading (revolution at 20rpm, dispersion at 500rpm for 25min and the temperature of no more than 35 ℃), and scraping pulp after the kneading is finished.
4. Adding the prepared glue solution in advance, performing high-viscosity stirring, controlling the solid content of the slurry to be 81%, revolving at 20rpm, dispersing at 1500rpm for 70min, controlling the temperature to be less than or equal to 35 ℃, and scraping the slurry to obtain slurry 1 after the high-viscosity stirring is finished.
5. Adding the rest of all the glue solution, stirring at low viscosity, revolving at 20rpm, dispersing at 2000rpm for 10min at the temperature of less than or equal to 35 ℃, keeping the vacuum degree at-90 kpa, scraping the pulp after stirring, continuing stirring after scraping the pulp, revolving at 30rpm, dispersing at 3000rpm for 80min at the temperature of less than or equal to 35 ℃, keeping the vacuum degree at-90 kpa, and scraping the pulp after stirring at low viscosity to obtain the pulp 2. And detecting the solid content, fineness and viscosity of the slurry.
6. After stirring, vacuumizing to remove bubbles, revolving at 15rpm (rotating the stirring paddle) for 60min at the temperature of less than or equal to 35 ℃ and the vacuum degree of-90 kpa, and filtering and discharging by using a 150-mesh screen.
Example 2
1. Preparing glue solution by using binders polyvinylidene fluoride (PVDF 5130) and N-methyl pyrrolidone (NMP) according to the solid content of 6%, firstly adding an NMP solution, then adding the PVDF 5130 binder, mixing and stirring at a low speed (revolution 15rpm, dispersion 1000rpm, time 10min) to obtain glue solution 1, then stirring at a medium speed (revolution 25rpm, dispersion 2500rpm, time 20min) to obtain glue solution 2, finally stirring at a high speed (revolution 35rpm, dispersion 3500rpm, time 240min) to obtain glue solution 3, namely PVDF glue solution, and storing the PVDF glue solution under a vacuum condition by stirring at a low speed (revolution 15rpm, time more than 180 min).
2. And (3) dry-mixing the conductive agent SP and the ternary material, adding 50% of the ternary material, adding the conductive agent SP, and adding 50% of the ternary material again for mixing (revolution (inversion) at 20rpm, dispersion at 1000rpm, and time 35 min).
3. And standing for 10min after mixing is finished, adding CNT and part of PVDF glue solution, kneading, controlling the solid content of kneading to be 87.5%, firstly kneading at low speed (revolution is 15rpm, time is 15min, and temperature is less than or equal to 35 ℃), scraping pulp after the low speed kneading is finished, then continuously stirring and kneading (revolution is 25rpm, dispersion is 600rpm, time is 35min, and temperature is less than or equal to 35 ℃), and scraping pulp after the kneading is finished.
4. Adding the prepared glue solution, performing high-viscosity stirring, controlling the solid content of the slurry to be 83.2%, revolving at 25rpm, dispersing at 2000rpm for 90min, controlling the temperature to be less than or equal to 35 ℃, and scraping the slurry to obtain slurry 1 after the high-viscosity stirring is finished, wherein the vacuum degree is-90 kpa.
5. Adding the rest all glue solution, stirring at low viscosity, revolving at 25rpm, dispersing at 2800rpm for 20min at the temperature of less than or equal to 35 ℃, keeping the vacuum degree at-90 kpa, scraping the pulp after stirring, then continuously stirring at the speed of less than or equal to 35 ℃ after scraping the pulp, revolving at 35rpm, dispersing at 3500rpm for 100min at the temperature of less than or equal to 35 ℃, keeping the vacuum degree at-90 kpa, and scraping the pulp after low-viscosity stirring to obtain the pulp 2. And detecting the solid content, fineness and viscosity of the slurry.
6. After stirring, vacuumizing to remove bubbles, revolving at 15rpm (rotating the stirring paddle) for 60min at the temperature of less than or equal to 35 ℃ and the vacuum degree of-90 kpa, and filtering and discharging by using a 150-mesh screen.
Example 3
1. Preparing glue solution by using a certain amount of binder polyvinylidene fluoride (PVDF 5130) and N-methyl pyrrolidone (NMP) according to the solid content of 6%, firstly adding an NMP solution, then adding the PVDF 5130 binder, mixing and stirring at a low speed (revolution 20rpm, dispersion 1500rpm, time 10min) to obtain glue solution 1, then stirring at a medium speed (revolution 30rpm, dispersion 3000rpm, time 20min) to obtain glue solution 2, finally stirring at a high speed (revolution 40rpm, dispersion 4000rpm, time 240min) to obtain glue solution 3, namely PVDF glue solution, and storing the PVDF glue solution under a vacuum condition by stirring at a low speed (revolution 15rpm, time more than 180 min).
2. And (3) dry-mixing the conductive agent SP and the ternary material, adding 50% of the ternary material, adding the conductive agent SP, and adding 50% of the ternary material again for mixing (revolution (inversion) at 25rpm, dispersion at 1500rpm, and time 45 min).
3. And standing for 10min after mixing is finished, adding CNT and part of PVDF glue solution, kneading, controlling the solid content of kneading to be 89%, performing low-speed kneading (revolution at 20rpm for 20min and the temperature of no more than 35 ℃), performing slurry scraping after the low-speed kneading is finished, then continuing stirring and kneading (revolution at 30rpm, dispersion at 1000rpm for 45min and the temperature of no more than 35 ℃), and performing slurry scraping after the kneading is finished.
4. Adding the prepared glue solution, performing high-viscosity stirring, controlling the solid content of the slurry to be 85%, revolving at 30rpm, dispersing at 2500rpm for 110min, controlling the temperature to be less than or equal to 35 ℃, and scraping the slurry to obtain slurry 1 after the high-viscosity stirring is finished, wherein the vacuum degree is-90 kpa.
5. Adding the rest of all the glue solution, stirring at low viscosity, revolving at 30rpm, dispersing at 3000rpm for 30min at the temperature of less than or equal to 35 ℃, keeping the vacuum degree at-90 kpa, scraping the pulp after stirring, continuing stirring after scraping the pulp, revolving at 40rpm, dispersing at 4000rpm for 120min at the temperature of less than or equal to 35 ℃, keeping the vacuum degree at-90 kpa, and scraping the pulp after stirring at low viscosity to obtain the pulp 2. And detecting the solid content, fineness and viscosity of the slurry.
6. After stirring, vacuumizing to remove bubbles, revolving at 15rpm (rotating the stirring paddle) for 60min at the temperature of less than or equal to 35 ℃ and the vacuum degree of-90 kpa, and filtering and discharging by using a 150-mesh screen.
Comparative example 1
1. And (3) dry-mixing the conductive agent SP and the ternary material, adding 50% of the ternary material, adding the conductive agent SP, and adding 50% of the ternary material again for mixing (revolution (inversion) at 15rpm, dispersion at 500rpm, and time 20 min).
2. And after the mixing is finished, standing for 10min, adding NMP for kneading, controlling the solid content in the kneading to be 86%, firstly kneading at a low speed (revolution at 10rpm for 10min and the temperature to be less than or equal to 35 ℃), scraping the slurry after the low speed kneading is finished, then continuously stirring and kneading (revolution at 20rpm for 500rpm and the time to be 25min and the temperature to be less than or equal to 35 ℃), scraping the slurry after the kneading is finished, wherein the slurry state in the kneading process is shown in figure 7, the NMP is directly added, the slurry cannot be agglomerated, and the effective kneading cannot be carried out, and figure 8 is a schematic diagram of the slurry state in the kneading stage of the embodiment 2 of the invention, and the PVDF glue solution is added for kneading, the slurry is agglomerated.
FIG. 2 is the fineness data of the slurry prepared in example 2 of the present invention, and it can be seen that the discharge fineness of the slurry is 20-30 μm, which corresponds to the discharge fineness of the ternary material slurry. The fineness is determined by the particle size of the material, which shows that the slurry prepared by the process has good dispersibility and does not have obvious aggregates and hard blocks.
Fig. 3 is a schematic diagram of a discharge state of slurry prepared in example 2 of the present invention, and fig. 4 is a schematic diagram of a sieving state of a 150-mesh sieve of slurry prepared in example 2 of the present invention, wherein normal sieving of 150 meshes indicates that the slurry has good fluidity, no obvious dispersion unevenness, no agglomeration and no sedimentation risk, and good dispersion effect.
FIG. 5 is the data of the viscosity and solid content change of the slurry prepared in example 2 of the present invention within 48h at 25 ℃, and it can be seen from the data that the viscosity rises by 3227mpa.s and the solid content rises by 1.95% after the slurry is discharged to stand for 48h, and NMP is gradually volatilized after standing for a long time in a beaker, so that the solvent is reduced, the viscosity is increased, and the solid content correspondingly rises. The stability of viscosity and solid content is beneficial to smooth coating, and the large fluctuation of surface density and thickness can not occur.
Fig. 6 is data of the coating adhesion and the weight loss rate change of the slurry pole piece prepared in example 2, and it can be seen from the data that the coating adhesion of the pole piece is maintained above 2N/30mm, and the weight loss rate is below 0.3%, which meets the specification requirements of a ternary system positive pole piece, which indicates that the slurry prepared by the invention has good process feasibility, and the higher the adhesion of the pole piece is, the better the adhesion of the slurry and a current collector is, which is beneficial to improving the cycle performance and the rate capability of a battery cell at a later stage. The lower the weight loss rate is, the less the solvent used by the slurry is, the solid content is correspondingly improved, the coating thickness of the pole piece is correspondingly reduced, and the charging and discharging performance of the battery cell is facilitated.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. An efficient and high-solid-content ternary material slurry mixing process is characterized by comprising the following steps:
(1) preparing PVDF glue solution;
(2) dry-mixing a conductive agent SP and a ternary material to obtain a dry mixture;
(3) adding the carbon nano tube and part of PVDF glue solution into the dry mixture for kneading and scraping to obtain first pre-pulping;
(4) adding part of PVDF glue solution in the first pre-pulping process, stirring at high viscosity, and scraping to obtain a second pre-pulping process;
(5) adding all the residual PVDF glue solution into the second pre-prepared pulp, stirring at low viscosity, and scraping to obtain third pre-prepared pulp;
(6) and vacuumizing the third pre-pulping to remove bubbles, and sieving by using a sieve to obtain the required pulp.
2. The high-efficiency and high-solid ternary material slurry mixing process according to claim 1, wherein the dry mixing in the step (2) comprises the following specific operation steps: firstly adding 50% of ternary material, then adding conductive agent SP, and finally adding the rest 50% of ternary material, wherein the revolution speed of the stirrer is 15-25rpm, the dispersion speed is 500-1500rpm, and the stirring time is 20-45 min.
3. The high-efficiency and high-solid-content ternary material slurry mixing process according to claim 1, characterized in that: and (3) standing the dry mixed material in the step (2) for 10min after the dry mixing is finished, and then performing the step (3).
4. The high-efficiency and high-solid content ternary material slurry mixing process according to claim 1, wherein the specific kneading operation in the step (3) comprises the following steps: the kneading temperature is less than or equal to 35 ℃, low-speed kneading is carried out firstly, the revolution speed of the stirrer is 10-20rpm, the low-speed kneading time is 10-20min, then high-speed kneading is carried out, the revolution speed of the stirrer is 20-30rpm, the dispersion speed is 500-1000rpm, and the high-speed kneading time is 25-45 min.
5. The high-efficiency and high-solid-content ternary material slurry mixing process according to claim 1, characterized in that: the solid content of the first pre-pulping is 86-89%.
6. The high-efficiency and high-solid-content ternary material slurry mixing process according to claim 1, characterized in that: in the step (4), the revolution speed of the stirrer during high-viscosity stirring is 20-30rpm, the dispersion speed is 1500-2500rpm, the stirring time is 70-110min, the stirring temperature is less than or equal to 35 ℃, and the vacuum degree is-90 kpa.
7. The high-efficiency and high-solid-content ternary material slurry mixing process according to claim 1, characterized in that: the solid content of the second pre-pulping is 81-85%.
8. The high-efficiency and high-solid content ternary material slurry mixing process according to claim 1, wherein the specific operation steps of low-viscosity stirring in the step (5) are as follows: the low-viscosity stirring temperature is less than or equal to 35 ℃, the vacuum degree is-90 kpa, primary stirring is firstly carried out, the revolution speed of the stirrer is 20-30rpm, the dispersion speed is 3000rpm, the primary stirring time is 10-30min, secondary stirring is carried out, the revolution speed of the stirrer is 30-40rpm, the dispersion speed is 3000rpm 4000rpm, and the secondary stirring time is 80-120 min.
9. The high-efficiency and high-solid-content ternary material slurry mixing process according to claim 1, characterized in that: in the step (6), the revolution speed of the stirrer is 15rpm during vacuum defoaming, the temperature is less than or equal to 35 ℃, the vacuum degree is-90 kpa, the time is 60min, and the mesh number of the screen is 150 meshes.
10. The high-efficiency and high-solid-content ternary material slurry mixing process according to claim 1, characterized in that: the specific operation steps for preparing the PVDF glue solution in the step (1) are as follows: preparing a glue solution by using a certain amount of adhesives PVDF and NMP according to the solid content of 6%, firstly adding NMP solution, then adding PVDF, mixing and stirring at a low speed, wherein the revolution speed of a stirrer is 10-20rpm, the dispersion speed is 500-1500rpm, the time is 10min, then stirring at a medium speed, the revolution speed of the stirrer is 20-30rpm, the dispersion speed is 2000-3000rpm, the time is 20min, finally stirring at a high speed, the revolution speed of the stirrer is 30-40rpm, the dispersion speed is 3000-4000rpm, and the time is 240min to obtain PVDF glue solution, stirring and storing the PVDF glue solution at a low speed under a vacuum condition for later use, wherein the revolution speed of the stirrer is 15rpm, and the time is more than 180 min.
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| CN111162280A (en) * | 2019-12-31 | 2020-05-15 | 河南新太行电源股份有限公司 | High-nickel cathode material of lithium ion battery and preparation process thereof |
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