CN108550793A - A kind of preparation method of lithium ion battery anode sizing agent - Google Patents
A kind of preparation method of lithium ion battery anode sizing agent Download PDFInfo
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- CN108550793A CN108550793A CN201810451494.3A CN201810451494A CN108550793A CN 108550793 A CN108550793 A CN 108550793A CN 201810451494 A CN201810451494 A CN 201810451494A CN 108550793 A CN108550793 A CN 108550793A
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation method of lithium ion battery anode sizing agent, this method is added in super mixer after first weighing positive active material, conductive agent, binder according to a certain ratio and is uniformly mixed；Then uniformly mixed siccative is added in high vacuum kneader, solvent is added in three times and kneading is processed, processes dough material into strips using screw extrusion apparatus and electric chopper after mediating uniformly；Strip-shaped materials are added in planetary stirring machine, solvent is added, it is uniform to slurry to vacuumize stirring；The viscosity and solid content of slurry after stirring finally are measured, the satisfactory stock discharge of viscosity is spare, and underproof adjustment viscosity is until viscosity meets the requirements.It is an advantage of the invention that：Using half siccative kneading process, the dispersion dead zone from impeller end farther out during traditional blade rotatably mixes is avoided, ensures all components being uniformly distributed in each region.
Description
Technical field
The present invention relates to a kind of lithium ion battery anode sizing agents, and in particular to a kind of lithium ion battery anode sizing agent
Preparation method.
Background technology
The electrode of lithium ion battery manufactures, and anode sizing agent is made of adhesive, conductive agent, positive electrode etc.；Negative electrode slurry
Then it is made of adhesive, graphite carbon dust etc..The preparation of positive and negative electrode slurry all includes liquid and liquid, liquid and solid material
Between the series of process process such as be mutually mixed, dissolve, disperseing, and in this process all along with temperature, viscosity, ring
The variations such as border.In positive and negative electrode slurry, the dispersibility and uniformity of particulate active are directly rung to lithium ion in battery two
The movement of interpolar, therefore the mixing dispersion of the slurry of each pole piece material is most important in lithium ion battery production, slurry dispersion
The quality of quality directly influences the performance of quality of follow-up lithium ion battery production and products thereof.
The preparation of existing pulp of lithium ion battery is all completed in double-planet dispersing apparatus.Although at present small-sized
Battery production has technically reached its maturity, but at present in the production process of lithium ion battery, and battery with two side terminals control is still
The technological difficulties that lithium ion battery makes, especially for large capacity, powerful power-type lithium ion battery.In addition, with
Lithium ion battery material is constantly progressive, and raw materials particles grain size is smaller and smaller, which not only improves performance of lithium ion battery,
It is easily created two level aggregate, to increase the difficulty of mixing dispersing technology.、
The mixing dispersion process of pulp of lithium ion battery can be divided into Macro-mixing Process and microcosmic dispersion process, the two processes
Always the whole process that can be all prepared along with pulp of lithium ion battery.And sheared according to the impeller in traditional handicraft --- cycle
Characteristic, can be divided into the effect of impeller two major classes, and the first kind is the shear action nearby generated to impeller；Second class is then logical
It crosses the flow that impeller pumps out and generates ringing.The further peptizaiton of slurry relies primarily on the shear action of impeller, and leaf
The flow of wheel determines the ability of the dispersion of impeller.And in the region from impeller end farther out, always there is one layer of slurry always
Stagnate it is motionless, this region namely it has often been said that " dead zone ", the working region of dispersing apparatus is bigger, and slurry viscosity is got over
The problem of height, " dead zone ", is more prominent, even if using different impeller and structure, dead zone is still difficult to avoid that, thus lithium from
In the preparation process of sub- cell size, obtained slurry products just will appear mixing and disperse uneven, powder granule and bonding
Agent contacts a series of problems, such as uneven, easy layering and generation hardness precipitation.A kind of slurries of the sufficiently complex of rheological characteristic of slurry exist
Newtonian fluid or pseudoplastic fluid may be shown as when low concentration；After the slightly higher generation floc sedimentation of concentration, Bingham fluid may be shown as；
Again it is possible that dilatant fluid under higher concentration.
Therefore the dispersibility and uniformity for improving pulp of lithium ion battery especially anode sizing agent are one significant
Project can be solved by improving and developing more outstanding dispersing apparatus or grope more optimal dispersing technology, this two
A aspect complements each other again mutually promotes.
Invention content
The purpose that the present invention is is to provide a kind of preparation method of lithium ion battery anode sizing agent, which utilizes
Powder is pre-mixed mediates two big optimization designs with half-dried high viscous material cutting.
The present invention is achieved like this, a kind of preparation method of lithium ion battery anode sizing agent, it is characterised in that adopt
Using the following method slurry is prepared with step：
（1）Super mixer is added after three kinds of positive active material, conductive agent, binder dry powder are weighed according to a certain ratio
In be uniformly mixed；
（2）Uniformly mixed dry powder is added in high vacuum kneader, solvent is added in three times and mediates and processes, after mediating uniformly
Dough material is processed into strips using screw extrusion apparatus and electric chopper；
（3）Strip-shaped materials are added in planetary stirring machine, solvent is added, it is uniform to slurry to vacuumize stirring；
（4）The viscosity and solid content of slurry after stirring are measured, the satisfactory stock discharge of viscosity is spare, underproof tune
Whole viscosity is until viscosity meets the requirements.
Further, the step（1）Middle positive active material is nickle cobalt lithium manganate（NCM）Or itself and LiMn2O4（LMO）
Mixture, conductive agent is carbon nanotube（CNTs）With carbon nano-fiber（CNFs）One or both of, binder is poly- inclined
Vinyl fluoride（PVDF）.
Further, the step（1）In three kinds of dry powder according to a certain ratio be specially nickle cobalt lithium manganate:LiMn2O4:Carbon
Nanotube:Carbon nano-fiber:Kynoar=（80%~95%）：（0%~15%）：（0.5%~2.5%）：（0.5%~2.5%）：（1%
~3%）.
Further, the step（1）It is 20 ~ 25m/s that linear velocity is stirred when high speed mixer dry powder blend, when mixing
Between be 5 ~ 30min.Stirring linear velocity and incorporation time be 5 ~ 30min be the present invention Optimal Parameters, this parameter area it
The most short mixed effect of the incorporation time of interior dry powder is best.
Further, the step（2）Middle solvent is N-Methyl pyrrolidone（NMP）, N- methyl is added in when kneading three times
The amount of pyrrolidones is the 1% ~ 10% of dry powder total amount, and it is 0.5 ~ 2h of first time, second of 1 ~ 3h, third to mediate process time three times
Secondary 0.5 ~ 2h.
Further, the step（2）It when middle material is mediated, is not vacuumized when mediating for the first time, second true when mediating
Reciprocal of duty cycle≤- 0.085MPa, vacuum degree≤- 0.085MPa when third time is mediated.
Further, the step（2）Middle mediate finishes a diameter of 10 ~ 30mm of strip-shaped materials of extrusion, and length is 30 ~
50mm。
Further, the step（3）It is middle that strip-shaped materials are added in planetary stirring machine, N-Methyl pyrrolidone is added
Amount be dry powder total amount 10% ~ 30%, stirring linear velocity be 5 ~ 15m/s, mixing time be 0.5 ~ 3h, vacuum degree for≤-
0.085MPa。
Further, the step（4）The viscosity of middle end product slurry be 4500 ~ 10000MPa s, solid content 60% ~
80%。
It is an advantage of the invention that：（1）Use dry powder premix, half siccative three-level is mediated, slurry homogenizes the even of three-level mixing
Paste-making method has fully ensured that the dispersibility and consistency of slurry.（2）Using half siccative kneading process, traditional blade rotation is avoided
Dispersion dead zone in rotatable mixing from impeller end farther out ensures all components being uniformly distributed in each region.（3）The present invention
Whole slurry preparation process takes 4 ~ 10h, and the time of 2 ~ 5h can be saved compared with the preparation method of traditional gluing+batch mixing, improves
Yield.
Description of the drawings
Fig. 1 is traditional anode sizing agent preparation method schematic diagram.
Fig. 2 is anode sizing agent preparation method schematic diagram of the present invention.
Specific implementation mode
The embodiment of the present invention is described in further detail below in conjunction with description of the drawings, but the present embodiment is not used to limit
The system present invention, every similar structure using the present invention and its similar variation, should all be included in protection scope of the present invention.
Comparative example chooses the battery core anode proportioning of certain model, and dispensing homogenate is carried out according to Fig. 1, and flow is as follows：
（1）The anode proportioning NCM required according to the model battery core：LMO：CNTs：CNFs：PVDF=（80%~95%）：（0%~15%）：
（0.5%~2.5%）：（0.5%~2.5%）：（1%~3%）.It weighs PVDF dry powder and planetary agitator tank is added in 70% total amount nmp solvent
Middle gluing disperses 10 ~ 15m/s of linear velocity, 3 ~ 4h of time, and gluing, which finishes, vacuumizes 2 ~ 4h of standing, vacuum degree≤- 0.085MPa.
（2）Conductive agent dry powder is weighed according to proportioning, is added（1）In glue in and add 10 ~ 15% NMP, open vacuum
Stirring progress conductive agent is pre-dispersed, 10 ~ 15m/s of linear velocity, 2 ~ 3h of time, vacuum degree≤- 0.085MPa.
（3）Active material dry powder is weighed according to proportioning, is added（2）In in scattered conductive agent slurry and add 10 ~ 15%
NMP opens stirring and carries out active material dispersion, 10 ~ 15m/s of linear velocity, 4 ~ 6h of time.
（4）The viscosity of slurry is measured whether within the scope of 4500 ~ 10000MPas, it is off-limits add NMP adjust it is viscous
Degree, vacuumizes 10 ~ 30min of defoaming after qualified, vacuum degree≤- 0.085MPa discharges spare.
The battery core model anode proportioning of embodiment, embodiment is identical as comparative example, as shown in Fig. 2, preparation method is as follows：
（1）It is added in super mixer and is mixed after positive active material, conductive agent, binder are weighed according to a certain ratio
It is even.
（2）Uniformly mixed siccative is added in high vacuum kneader, solvent is added in three times and mediates and processes, mediates equal
Dough material is processed into strips using screw extrusion apparatus and electric chopper after even.
（3）Strip-shaped materials are added in planetary stirring machine, solvent is added, it is uniform to slurry to vacuumize stirring.
（4）The viscosity and solid content of slurry after stirring are measured, the satisfactory stock discharge of viscosity is spare, unqualified
Adjustment viscosity until viscosity meet the requirements.
Wherein, the positive active material is nickle cobalt lithium manganate（NCM）Or itself and LiMn2O4（LMO）Mixture, lead
Electric agent is carbon nanotube（CNTs）With carbon nano-fiber（CNFs）, binder is Kynoar（PVDF）.
Wherein, dry powder quality ratio NCM：LMO：CNTs：CNFs：PVDF=（80%~95%）：（0%~15%）：（0.5%~
2.5%）：（0.5%~2.5%）：（1%~3%）.
Wherein, when the dry powder blend super mixer stirring linear velocity be 20 ~ 25m/s, incorporation time be 5 ~
30min。
Wherein, the solvent is N-Methyl pyrrolidone（NMP）, it is dry powder total amount that NMP amounts, which are added, in when kneading three times
1% ~ 10%, it is 0.5 ~ 2h of first time, second of 1 ~ 3h, 0.5 ~ 2h of third time to mediate process time three times.
Wherein, it when the material is mediated, is not vacuumized when mediating for the first time, vacuum degree when mediating for second≤-
0.085MPa, vacuum degree≤- 0.085MPa when third time is mediated.
Wherein, the kneading finishes a diameter of 10 ~ 30mm of strip-shaped materials of extrusion, and length is 30 ~ 50mm.
Wherein, described that strip-shaped materials are added in planetary stirring machine, 10% ~ 30% that NMP amounts are dry powder total amount is added,
Stirring linear velocity is 5 ~ 15m/s, and mixing time is 0.5 ~ 3h, and vacuum degree is≤- 0.085MPa.
Wherein, the viscosity of the end product slurry is 4500 ~ 10000MPa s, solid content 60% ~ 80%.
The finished product slurry parameters index of above-mentioned comparative example and embodiment is compared, as shown in table 1：
1 comparative example of table and embodiment finished product slurry parameter comparison
Comparative example and embodiment finished product slurry parameter comparison the result shows that, according to finished product slurry made of the method for the present invention and tradition
Method is compared, and slurry processing time shortens, and dispersibility is improved by a relatively large margin.
Claims (9)
1. a kind of preparation method of lithium ion battery anode sizing agent, it is characterised in that prepare slurry using following methods and step
Material：
（1）Super mixer is added after three kinds of positive active material, conductive agent, binder dry powder are weighed according to a certain ratio
In be uniformly mixed；
（2）Uniformly mixed dry powder is added in high vacuum kneader, solvent is added in three times and mediates and processes, after mediating uniformly
Dough material is processed into strips using screw extrusion apparatus and electric chopper；
（3）Strip-shaped materials are added in planetary stirring machine, solvent is added, it is uniform to slurry to vacuumize stirring；
（4）The viscosity and solid content of slurry after stirring are measured, the satisfactory stock discharge of viscosity is spare, underproof tune
Whole viscosity is until viscosity meets the requirements.
2. a kind of preparation method of lithium ion battery anode sizing agent according to claim 1, it is characterised in that：The step
Suddenly（1）Middle positive active material is nickle cobalt lithium manganate or the mixture of itself and LiMn2O4, and conductive agent is carbon nanotube and carbon nanometer
One or both of fiber, binder are Kynoar.
3. a kind of preparation method of lithium ion battery anode sizing agent according to claim 2, it is characterised in that：The step
Suddenly（1）In three kinds of dry powder according to a certain ratio be specially nickle cobalt lithium manganate:LiMn2O4:Carbon nanotube:Carbon nano-fiber:It is poly- inclined
Vinyl fluoride=（80%~95%）：（0%~15%）：（0.5%~2.5%）：（0.5%~2.5%）：（1%~3%）.
4. a kind of preparation method of lithium ion battery anode sizing agent according to claim 1, it is characterised in that：The step
Suddenly（1）It is 20 ~ 25m/s that linear velocity is stirred when high speed mixer dry powder blend, and incorporation time is 5 ~ 30min.
5. a kind of preparation method of lithium ion battery anode sizing agent according to claim 1, it is characterised in that：The step
Suddenly（2）Middle solvent is N-Methyl pyrrolidone, the amount that N-Methyl pyrrolidone is added in when kneading three times be dry powder total amount 1% ~
10%, it is 0.5 ~ 2h of first time, second of 1 ~ 3h, 0.5 ~ 2h of third time to mediate process time three times.
6. a kind of preparation method of lithium ion battery anode sizing agent according to claim 5, it is characterised in that：The step
Suddenly（2）It when middle material is mediated, is not vacuumized when mediating for the first time, vacuum degree≤- 0.085MPa when mediating for the second time is pinched for the third time
Vacuum degree≤- 0.085MPa when conjunction.
7. a kind of preparation method of lithium ion battery anode sizing agent according to claim 6, it is characterised in that：The step
Suddenly（2）Middle to mediate a diameter of 10 ~ 30mm of strip-shaped materials for finishing extrusion, length is 30 ~ 50mm.
8. a kind of preparation method of lithium ion battery anode sizing agent according to claim 1, it is characterised in that：The step
Suddenly（3）It is middle by strip-shaped materials be added planetary stirring machine in, be added N-Methyl pyrrolidone amount be dry powder total amount 10% ~
30%, stirring linear velocity is 5 ~ 15m/s, and mixing time is 0.5 ~ 3h, and vacuum degree is≤- 0.085MPa.
9. a kind of preparation method of lithium ion battery anode sizing agent according to claim 1, it is characterised in that：The step
Suddenly（4）The viscosity of middle end product slurry is 4500 ~ 10000MPa s, solid content 60% ~ 80%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113299911A (en) * | 2021-05-28 | 2021-08-24 | 江西安驰新能源科技有限公司 | Preparation method of lithium iron phosphate anode slurry for lithium ion battery |
| CN114335507A (en) * | 2021-12-16 | 2022-04-12 | 安徽博石高科新材料股份有限公司 | Surface pressing type mixing and secondary sintering method of lithium battery positive electrode material |
| CN117276651A (en) * | 2023-01-16 | 2023-12-22 | 江苏大学 | Carbon-based solid lithium battery solid electrolyte membrane, preparation method and battery core |
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| CN106207129A (en) * | 2016-08-31 | 2016-12-07 | 中航锂电（洛阳）有限公司 | A kind of preparation method of anode slurry of high-rate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113299911A (en) * | 2021-05-28 | 2021-08-24 | 江西安驰新能源科技有限公司 | Preparation method of lithium iron phosphate anode slurry for lithium ion battery |
| CN114335507A (en) * | 2021-12-16 | 2022-04-12 | 安徽博石高科新材料股份有限公司 | Surface pressing type mixing and secondary sintering method of lithium battery positive electrode material |
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| CN117276651A (en) * | 2023-01-16 | 2023-12-22 | 江苏大学 | Carbon-based solid lithium battery solid electrolyte membrane, preparation method and battery core |
| CN117276651B (en) * | 2023-01-16 | 2024-06-11 | 江苏宏鑫达新能源科技有限公司 | Carbon-based solid lithium battery solid electrolyte membrane, preparation method and battery core |
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Application publication date: 20180918 |