CN106299269A - A kind of lithium ion battery anode glue size preparation method - Google Patents
A kind of lithium ion battery anode glue size preparation method Download PDFInfo
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- CN106299269A CN106299269A CN201610682971.8A CN201610682971A CN106299269A CN 106299269 A CN106299269 A CN 106299269A CN 201610682971 A CN201610682971 A CN 201610682971A CN 106299269 A CN106299269 A CN 106299269A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- 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
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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
- 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
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
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Abstract
The present invention provides a kind of lithium ion battery anode glue size preparation method, will solve the technical problem that the dispersibility being to improve positive active material with conductive agent, thus improve the combination property of lithium ion battery.First active substances in cathode materials, conductive agent and nmp solvent are mixed to join in de-airing mixer, protect vacuum high-temperature quickly to stir, then bleed condensation, remove part nmp solvent in slurry, it is eventually adding PVDF sol solution, fidelity sky leads to recirculated water high-speed stirred uniformly, obtains finely dispersed anode sizing agent, and the method can be greatly improved production efficiency and the stock quality of lithium ion battery anode glue size.The present invention is first by active substances in cathode materials, conductive agent and nmp solvent Hybrid Heating fidelity sky high-speed stirred, and beneficially positive active material is uniformly dispersed with conductive agent, improves the production efficiency of lithium ion battery and the combination property of battery；The NMP condenser of addition is recovered to recycling by the present invention, has saved production cost.
Description
Technical field
The invention belongs to technical field of lithium ion, relate to a kind of lithium ion battery anode glue size preparation method.
Background technology
Lithium ion battery energy density is big, has extended cycle life, and high rate performance and security performance are good, and environmental protection is current
Main energy sources product.Lithium ion battery includes positive pole, negative pole, barrier film, electrolyte and shell, and positive pole is lithium ion battery important set
Become part, the quality of cathode performance directly affects the performance of lithium ion battery, anode sizing agent anode sizing agent prepare direct shadow
Ring the combination property of lithium ion battery.
Along with developing rapidly of lithium ion battery, people propose higher requirement to performance of lithium ion battery, drive simultaneously
Active substance of lithium ion battery anode material and the fast lifting of conductive agent material property, little granule cathode active material with
Conductive agent even particle distribution, conducts electricity very well, but under tradition stirring technique, material dispersion effect is poor, conducts electricity in positive electrode
Agent can not be good filling, have impact on the performance of lithium ion battery.If the superiority of small-particulate materials can be made full use of,
Prepare and be uniformly dispersed and anode sizing agent that processing characteristics is good, the combination property of lithium ion battery will certainly be greatly improved.
Summary of the invention
It is an object of the invention to provide a kind of lithium ion battery anode glue size preparation method, will solve the technical problem that it is to carry
High positive active material and the dispersibility of conductive agent, thus improve the combination property of lithium ion battery.
The present invention can be achieved through the following technical solutions:
A kind of lithium ion battery anode glue size preparation method,
First active substances in cathode materials, conductive agent and nmp solvent, are mixed to join in de-airing mixer by a, if nickel cobalt manganese
The material cell such as acid lithium, cobalt acid lithium material, lithium manganate material, then the mass ratio of active substance, conductive agent and NMP is (95 ~ 98):
(0.5 ~ 3): (40 ~ 100), if LiFePO 4 material battery, then the mass ratio of active substance, conductive agent and NMP be (95 ~
98): (0.5 ~ 3): (97 ~ 120)；
Low rate mixing 10 ~ 20min, low rate mixing revolution 5 ~ 10r/min, rotation 500 ~ 800r/min, scrape fidelity outage speed after wall
Stir and heat, control slurry temperature 60 ~ 80 DEG C, high-speed stirred speed revolution 20 ~ 25r/min, rotation 2000 ~ 3000r/min,
Vacuum is less than-0.08MPa, high-speed stirred 2 ~ 3h；Then low rate mixing is carried out, low rate mixing revolution 10r/min, rotation 500 ~
800r/min, cooling of bleeding after being simultaneously filled with drying nitrogen in size barrel, inflation/deflation circulation is carried out, by high-temperature stirring when bleeding
Nmp solvent continuous suction condenser in size barrel condenses, until nickle cobalt lithium manganate, cobalt acid lithium material, lithium manganate material
Reach 75 ~ 80% etc. material cell slurry solid content, or LiFePO 4 material cell size solid content reaches 55 ~ 60%；
B stops agitator heating, is filled with drying nitrogen low rate mixing, low rate mixing revolution 5r/min, rotation 500r/min, and incites somebody to action
Agitator leads to recirculated water and slurry is cooled to less than 50 DEG C, adds quantitative dispersion in advance all in the viscous paste of mix homogeneously
Even Kynoar sol solution, sol solution concentration 5% ~ 10%, fidelity sky high-speed stirred, and it is passed through recirculated water, material temperature controls
Less than 50 DEG C, high-speed stirred revolution 25r/min, autobiography 2000 ~ 3000r/min, vacuum ＜-0.08MPa, the high-speed stirred time
It is 2 ~ 3h, obtains finely dispersed lithium ion battery anode glue size.
Further, one or more during positive active material is LiFePO4, nickle cobalt lithium manganate, cobalt acid lithium, LiMn2O4.
Further, conductive agent can be conductive black Super-P, graphite agent KS-15, graphite agent KS-16, nanometer
One or more in carbon fiber, CNT.
Further, Kynoar can be one or more in Solef 5130, PVDF761A, HSV900.
Advantages of the present invention with effect is:
1. the present invention is first by active substances in cathode materials, conductive agent and nmp solvent Hybrid Heating fidelity sky high-speed stirred, high temperature
In lower slurry, the granule resistance of motion is little, and beneficially positive active material is uniformly dispersed with conductive agent, solves high-specific surface area and leads
Electricity agent is difficult to a scattered difficult problem, improves conductive agent dispersion efficiency and dispersing uniformity, improves the production effect of lithium ion battery
Rate and the combination property of battery；
2. the present invention is filled with drying nitrogen to finely dispersed positive active material and conductive agent slurry high temperature, and cooling of bleeding follows
Ring, is recovered to the NMP condenser of addition recycling, has saved production cost, efficiently improve positive active material and conduction
The solid content of agent slurry, finally gives finely dispersed positive active material and conductive agent viscous paste.
The most scattered sol solution is joined in positive active material and conductive agent viscous paste and carries out height by the present invention
Speed stirring, and be passed through recirculated water, it is to avoid sol solution is reduced the viscosity of glue itself by high temperature and high speed long agitation, reduction
The addition of glue, improves lithium ion battery activity substance content, thus improves capacity of lithium ion battery.
Accompanying drawing explanation
Fig. 1 is lithium ion battery anode glue size coating pole piece SEM figure in embodiment 1.
Fig. 2 is lithium ion battery anode glue size coating pole piece SEM figure in embodiment 2.
Fig. 3 is lithium ion battery anode glue size coating pole piece SEM figure in embodiment 3.
Detailed description of the invention
The present invention is as follows.
First quantitative active substances in cathode materials, conductive agent and nmp solvent are mixed to join in de-airing mixer.If
For material cell such as nickle cobalt lithium manganate, cobalt acid lithium material, lithium manganate materials, then the mass ratio of active substance, conductive agent and NMP is
95 ~ 98:0.5 ~ 3:40 ~ 100, if LiFePO 4 material battery, then the mass ratio of active substance, conductive agent and NMP be 95 ~
98:0.5 ~ 3:97 ~ 120.
Low rate mixing 10 ~ 20min, low rate mixing revolution 5 ~ 10r/min, rotation 500 ~ 800r/min, after scraping wall, fidelity is empty
High-speed stirred also heats, and controls slurry temperature and keeps 60 ~ 80 DEG C, high-speed stirred speed revolution 20 ~ 25r/min, and rotation 2000 ~
3000r/min, vacuum ＜-0.08MPa, carry out low rate mixing after high-speed stirred 2 ~ 3h, low rate mixing revolution 10r/min, from
Turning 500 ~ 800r/min, and cooling of bleeding after being filled with drying nitrogen in size barrel, inflation/deflation circulates and carries out, by high temperature when bleeding
Nmp solvent continuous suction condenser in stirring size barrel condenses, until nickle cobalt lithium manganate, cobalt acid lithium material, LiMn2O4
The material cell slurry solid contents such as material reach 75 ~ 80%, or LiFePO 4 material cell size solid content reaches 55 ~ 60%.
Then stop agitator heating, be filled with drying nitrogen low rate mixing, and agitator led to circulating water to slurry
Less than 50 DEG C, the viscous paste of mix homogeneously adds quantitative prior finely dispersed Kynoar (PVDF) peptization
Liquid, sol solution concentration 5% ~ 10%, fidelity sky high-speed stirred, and it is passed through recirculated water, material temperature controls below 50 DEG C, and high-speed stirred is public
Turning 25r/min, rotation 2000 ~ 3000r/min, vacuum ＜-0.08MPa, the high-speed stirred time is 2 ~ 3h, is uniformly dispersed
Lithium ion battery anode glue size.
Embodiment 1
Prepared by LiFePO4 18650-1600mAh-3.2V lithium ion battery anode glue size, first by the LiFePO4 material of 95kg
Material, the NMP of graphitic carbon black KS-15 and 100kg of conductive black Super-P, 1kg of 1kg are mixed to join in 200L blender,
Low rate mixing 10min, low rate mixing revolution 5r/min, rotation 500r/min, fidelity sky high-speed stirred heating after scraping wall, control
Slurry temperature keeps 70 ± 5 DEG C, and high-speed stirred speed is revolution 20r/min, rotation 3000r/min, vacuum ＜-0.08MPa,
Carry out low rate mixing, low rate mixing revolution 10r/min, rotation 500r/min after high-speed stirred 2h, and be filled with dry in size barrel
Bleeding after dry nitrogen cooling, inflation/deflation circulation is carried out, and continuous for the nmp solvent in high-temperature stirring size barrel suction is condensed when bleeding
Device condenses, until testing size solid content is 57 ± 1%.
Then stop agitator heating, be filled with drying nitrogen low rate mixing, and agitator led to circulating water to slurry
Less than 50 DEG C, the viscous paste of mix homogeneously adds Kynoar (PVDF) Solef that 30kg solid content is 10%
5130 sol solutions, fidelity sky high-speed stirred, and it is passed through recirculated water, material temperature controls below 50 DEG C, high-speed stirred revolution 20r/
Min, rotation 3000r/min, vacuum ＜-0.08MPa, the high-speed stirred time is 3h, obtains finely dispersed lithium ion battery
Anode sizing agent.
It is short that the method prepares lithium ion battery anode glue size mixing time, and production efficiency is high, and slurry uniformity is good, the method
The lithium ion battery anode glue size coating pole piece SEM of preparation schemes as shown in Figure 1.
Embodiment 2
Prepared by LiFePO4 18650-1700mAh-3.2V lithium ion battery anode glue size, first by the LiFePO4 material of 97kg
Material, the CNT (CNTs) of 1kg, the NMP of 90kg are mixed to join in 200L blender, low rate mixing 10min, low rate mixing
Revolution 5r/min, rotation 500r/min, fidelity sky high-speed stirred heating after scraping wall, control slurry temperature and keep 70 ± 5 DEG C, high
Speed mixing speed is revolution 25r/min, rotation 3000r/min, vacuum ＜-0.08MPa, stirs at a slow speed after high-speed stirred 3h
Mix, low rate mixing revolution 10r/min, rotation 600r/min, and cooling of bleeding after being filled with drying nitrogen in size barrel, inflation/deflation
Circulation is carried out, and is condensed by continuous for the nmp solvent in high-temperature stirring size barrel suction condenser when bleeding, until testing size
Solid content is 57 ± 1%.
Then stop agitator heating, be filled with drying nitrogen low rate mixing, and agitator led to circulating water to slurry
Less than 50 DEG C, the viscous paste of mix homogeneously adds Kynoar (PVDF) Solef that 20kg solid content is 10%
5130 sol solutions, fidelity sky high-speed stirred, and it is passed through recirculated water, material temperature controls below 50 DEG C, high-speed stirred revolution 25r/
Min, rotation 3000r/min, vacuum ＜-0.08MPa, the high-speed stirred time is 2h, obtains finely dispersed lithium ion battery
Anode sizing agent.
It is short that the method prepares lithium ion battery anode glue size mixing time, and production efficiency is high, and slurry uniformity is good, the method
The lithium ion battery anode glue size coating pole piece SEM of preparation schemes as shown in Figure 2.
Embodiment 3
Prepared by nickle cobalt lithium manganate ternary 18650-2200mAh-3.7V lithium ion battery anode glue size, first by the iron phosphate of 98kg
Lithium material, the CNT (CNTs) of 0.5kg, the NMP of 40kg are mixed to join in 200L blender, low rate mixing 20min, slowly
Speed stirring revolution 10r/min, rotation 800r/min, fidelity sky high-speed stirred heating after scraping wall, control slurry temperature and keep 75
± 5 DEG C, high-speed stirred speed is revolution 20r/min, and rotation 2000r/min, vacuum ＜-0.08MPa, high-speed stirred 3h is laggard
Row low rate mixing, low rate mixing revolution 10r/min, rotation 800r/min, and it is cold to bleed after being filled with drying nitrogen in size barrel
But, inflation/deflation circulation is carried out, and is condensed, directly by continuous for the nmp solvent in high-temperature stirring size barrel suction condenser when bleeding
It is 79 ± 1% to testing size solid content.
Then stop agitator heating, be filled with drying nitrogen low rate mixing, and agitator led to circulating water to slurry
Less than 50 DEG C, the viscous paste of mix homogeneously adds Kynoar (PVDF) the 761A peptization that 15kg solid content is 10%
Liquid, fidelity sky high-speed stirred, and it is passed through recirculated water, material temperature controls below 50 DEG C, high-speed stirred revolution 20r/min, rotation
2000r/min, vacuum ＜-0.08MPa, the high-speed stirred time is 2h, obtains finely dispersed lithium ion battery anode glue size.
It is short that the method prepares lithium ion battery anode glue size mixing time, and production efficiency is high, and slurry uniformity is good, the method
The lithium ion battery anode glue size coating pole piece SEM of preparation schemes as shown in Figure 3.
Claims (4)
1. a lithium ion battery anode glue size preparation method, is characterized in that:
First active substances in cathode materials, conductive agent and nmp solvent, are mixed to join in de-airing mixer by a, if nickel cobalt manganese
The material cell such as acid lithium, cobalt acid lithium material, lithium manganate material, then the mass ratio of active substance, conductive agent and NMP is 95 ~ 98:
0.5 ~ 3:40 ~ 100, if LiFePO 4 material battery, then the mass ratio of active substance, conductive agent and NMP be 95 ~ 98:0.5 ~
3:97 ~ 120；
Low rate mixing 10 ~ 20min, low rate mixing revolution 5 ~ 10r/min, rotation 500 ~ 800r/min, scrape fidelity outage speed after wall
Stir and heat, control slurry temperature 60 ~ 80 DEG C, high-speed stirred speed revolution 20 ~ 25r/min, rotation 2000 ~ 3000r/min,
Vacuum is less than-0.08MPa, high-speed stirred 2 ~ 3h；Then low rate mixing is carried out, low rate mixing revolution 10r/min, rotation 500 ~
800r/min, cooling of bleeding after being simultaneously filled with drying nitrogen in size barrel, inflation/deflation circulation is carried out, by high-temperature stirring when bleeding
Nmp solvent continuous suction condenser in size barrel condenses, until nickle cobalt lithium manganate, cobalt acid lithium material, lithium manganate material
Reach 75 ~ 80% etc. material cell slurry solid content, or LiFePO 4 material cell size solid content reaches 55 ~ 60%；
B stops agitator heating, is filled with drying nitrogen low rate mixing, low rate mixing revolution 5r/min, rotation 500r/min, and incites somebody to action
Agitator leads to recirculated water and slurry is cooled to less than 50 DEG C, adds quantitative dispersion in advance all in the viscous paste of mix homogeneously
Even Kynoar sol solution, sol solution concentration 5% ~ 10%, fidelity sky high-speed stirred, and it is passed through recirculated water, material temperature controls
Less than 50 DEG C, high-speed stirred revolution 25r/min, autobiography 2000 ~ 3000r/min, vacuum ＜-0.08MPa, the high-speed stirred time
It is 2 ~ 3h, obtains finely dispersed lithium ion battery anode glue size.
Lithium ion battery anode glue size preparation method the most according to claim 1, it is characterised in that: positive active material is
One or more in LiFePO4, nickle cobalt lithium manganate, cobalt acid lithium, LiMn2O4.
Lithium ion battery anode glue size preparation method the most according to claim 1, it is characterised in that: conductive agent can be conduction
One or several in white carbon black Super-P, graphite agent KS-15, graphite agent KS-16, carbon nano-fiber, CNT
Kind.
Lithium ion battery anode glue size preparation method the most according to claim 1, it is characterised in that: Kynoar can be
One or more in Solef 5130, PVDF761A, HSV900.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107611338A (en) * | 2017-08-25 | 2018-01-19 | 金川集团股份有限公司 | The preparation method of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property |
| CN110993883A (en) * | 2019-10-28 | 2020-04-10 | 广东电网有限责任公司 | Electrode plate and preparation method and application thereof |
| 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 |
| CN112121660A (en) * | 2020-08-26 | 2020-12-25 | 风帆有限责任公司 | Method for preparing anode slurry of lithium ion battery |
| CN112151801A (en) * | 2020-09-21 | 2020-12-29 | 深圳市拓邦锂电池有限公司 | Lithium ion battery anode slurry and preparation method thereof |
| CN112234199A (en) * | 2020-09-15 | 2021-01-15 | 深圳市拓邦锂电池有限公司 | Lithium ion battery positive electrode slurry, preparation method thereof and lithium ion battery positive electrode plate |
| CN112490392A (en) * | 2020-11-27 | 2021-03-12 | 天科新能源有限责任公司 | Method for reducing agglomeration phenomenon of lithium ion battery anode slurry |
| CN112542585A (en) * | 2020-11-05 | 2021-03-23 | 杭州力奥科技有限公司 | Pulping process for anode lithium iron phosphate |
| CN113422049A (en) * | 2021-06-25 | 2021-09-21 | 湖北亿纬动力有限公司 | Lithium iron phosphate positive pole piece and preparation method and application thereof |
| EP3951921A1 (en) * | 2020-08-05 | 2022-02-09 | SK Innovation Co., Ltd. | Fabrication method of positive electrode for secondary battery and secondary battery including the positive electrode |
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| CN107611338A (en) * | 2017-08-25 | 2018-01-19 | 金川集团股份有限公司 | The preparation method of Snap-type cell positive slurry used in a kind of check and evaluation material electrical property |
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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 |
| EP3951921A1 (en) * | 2020-08-05 | 2022-02-09 | SK Innovation Co., Ltd. | Fabrication method of positive electrode for secondary battery and secondary battery including the positive electrode |
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| CN112542585A (en) * | 2020-11-05 | 2021-03-23 | 杭州力奥科技有限公司 | Pulping process for anode lithium iron phosphate |
| CN112490392A (en) * | 2020-11-27 | 2021-03-12 | 天科新能源有限责任公司 | Method for reducing agglomeration phenomenon of lithium ion battery anode slurry |
| CN113422049A (en) * | 2021-06-25 | 2021-09-21 | 湖北亿纬动力有限公司 | Lithium iron phosphate positive pole piece and preparation method and application thereof |
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| CN106299269B (en) | 2018-11-02 |
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