CN108172750A - The preparation method of graphite negative electrode of lithium ion battery highly viscous slurry - Google Patents
The preparation method of graphite negative electrode of lithium ion battery highly viscous slurry Download PDFInfo
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- CN108172750A CN108172750A CN201711281748.3A CN201711281748A CN108172750A CN 108172750 A CN108172750 A CN 108172750A CN 201711281748 A CN201711281748 A CN 201711281748A CN 108172750 A CN108172750 A CN 108172750A
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- agitator tank
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
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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
-
- 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
-
- 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 present invention discloses a kind of preparation method of graphite negative electrode of lithium ion battery highly viscous slurry, belongs to lithium ion battery production field.The preparation method is that first conductive agent, active material and thickener are added in agitator tank, then carries out dry powder stirring successively, high-viscosity stirring, viscosity adjustment stirring, adds in liquid cement agitation, slurry vacuum defoamation.Using above-mentioned stirring flow, each link can be completed in relatively short mixing time, save the plenty of time.It is carried out in addition, whole process of the present invention does not need to the more agitator tank division of labor, it is not required that the material transferred to other use in agitator tank substantially increases production efficiency, while improves the stability and dispersion effect of slurry.
Description
Technical field
The present invention relates to a kind of preparation methods of graphite negative electrode of lithium ion battery highly viscous slurry, belong to lithium ion battery life
Production field.
Background technology
The development of new-energy automobile, key are its electrical source of power.Lithium ion battery has that energy density is big, self discharge
The advantages that small, memory-less effect, operating voltage range are wide, service life is long, non-environmental-pollution is that current new-energy automobile is main
Electrical source of power.
Lithium ion battery generally comprises positive plate, negative plate, the diaphragm being interval between positive plate and negative plate.Positive plate
Including plus plate current-collecting body and the anode diaphragm being coated on plus plate current-collecting body, negative plate includes negative current collector and is coated on cathode
Cathode membrane on collector.When prepared by electrode plates, first by active material (such as cobalt acid lithium, graphite), conductive agent (such as second
Acetylene black, carbon nanotube, carbon fiber etc.), bonding agent (such as Kynoar, polyvinylpyrrolidone, sodium carboxymethylcellulose,
SBR emulsion etc.) and solvent (such as N-Methyl pyrrolidone, water) electrode slurry is made together, then it is coated as required
It in collection liquid surface, is then dried, obtains battery pole piece.
Wherein, the performance of electrode slurry has the performance of lithium ion battery important influence.Each component in electrode slurry
Disperse more uniform, pole piece just has better processing performance, and the distribution of impedance of electrode everywhere is uniform, active in charge and discharge
The effect of substance can play bigger, and average gram volume performance will be promoted, so as to promote the performance of battery.
In practical application, traditional graphite cathode slurry preparation method is that conductive agent is carried out high rotating speed with thickener soln
Double planetary dispersion, then add in negative electrode active material, after the stirring for carrying out certain time, add binding agent through row in short-term
Between stir to get final graphite cathode slurry.Such method needs long time treatment to the dispersion of conductive agent first, time-consuming and
Dispersity is unsatisfactory；Secondly traditional handicraft is needed in slurry preparation process, and stirring system is always maintained at vacuumizing shape
State causes slurry system internal temperature easily to increase, at the same again outside plus recirculated water cooled down, therefore the requirement to equipment and
Abrasion is all very high.Lead to that slurry preparation efficiency is low, stability is poor, effect is undesirable, preparation, lithium battery to follow-up pole piece above
Performance can all impact.
Invention content
The present invention is intended to provide a kind of preparation method of graphite negative electrode of lithium ion battery highly viscous slurry, to realize shorter
Slurry each component is uniformly dispersed in time, the slurry uniformity prepared is good.
In order to achieve the above-mentioned object of the invention, the present invention uses technical solution as described below：
A kind of preparation method of graphite negative electrode of lithium ion battery highly viscous slurry, includes the following steps：
(1) dry powder stirs：After the dry powder material of conductive agent, active material and thickener CMC being added in into agitator tank, control
Agitator tank stirs；
(2) high-viscosity stirring：Into agitator tank plus water, adjustment solid content to 67%-78%, control agitator tank stir；
(3) viscosity adjustment stirring, including：3a. sides add waterside control agitator tank stirring to agitator tank, by slurry in agitator tank
Solid content be adjusted to 58%-62%；3b. adds in thickener CMC, control agitator tank stirring into agitator tank；3c. sides are to agitator tank
Add waterside control agitator tank stirring, the solid content of slurry in agitator tank is adjusted to 51%-55%, viscosity is adjusted to 2000-4000cp；
(4) liquid cement agitation is added in：Glue SBR, control agitator tank stirring are added in into slurry；
(5) slurry vacuum defoamation：Agitator tank is evacuated to -0.09MPa--0.1MPa, control agitator tank stirring.
As specific technical solution, the concrete operations of the control agitator tank stirring described in step (1) are：Described in control
Agitator tank revolution rotating speed is 15-25 revs/min, and it is 0-200 revs/min to control the stirring disk rotating speed of the agitator tank, stirring 8 to
12 minutes.
As specific technical solution, the concrete operations of the control agitator tank stirring described in step (2) are：Described in control
Agitator tank revolution rotating speed is 35-60 revs/min, and the stirring disk rotating speed for controlling the agitator tank is 800-1200 revs/min, stirring
15 to 25 minutes.
As specific technical solution, the concrete operations of the step 3a are：It is 60- to control the agitator tank revolution rotating speed
70 revs/min, it is 1000-1200 revs/min to control the stirring disk rotating speed of the agitator tank, in 3 to 5 minutes inner edges to agitator tank
Add waterside control agitator tank stirring, by the solid content of slurry in agitator tank be adjusted to continue after 58%-62% to control agitator tank after
Continuous stirring 8 to 12 minutes.
As specific technical solution, the concrete operations of the step 3b are：After thickener CMC being added in into agitator tank,
It is 60-70 revs/min to control agitator tank revolution rotating speed, control the stirring disk rotating speed of the agitator tank turn for 1000-1200/
Minute, it stirs 1-3 minutes.
As specific technical solution, the concrete operations of step 3c are：It is 60-70 to control the agitator tank revolution rotating speed
Rev/min, the stirring disk rotating speed for controlling the agitator tank is 1000-1200 revs/min, is added in 3 to 5 minutes inner edges to agitator tank
The solid content of slurry in agitator tank is adjusted to continue that agitator tank is controlled to continue after 51%-55% by waterside control agitator tank stirring
Stirring 8 to 12 minutes, the viscosity for obtaining slurry are 2000-4000cp.
As specific technical solution, the concrete operations of the control agitator tank stirring described in step (4) are：Described in control
Agitator tank revolution rotating speed is 20-40 revs/min, and the stirring disk rotating speed for controlling the agitator tank is 500-800 revs/min, stirring
15 to 25 minutes.
As specific technical solution, the concrete operations of the control agitator tank stirring described in step (5) are：Described in control
Agitator tank revolution rotating speed is 8-12 revs/min, is stirred 4 to 6 minutes.
It is by 2 parts of conductive agents, 95 parts of active material stones as specific technical solution, in the step (1) by mass parts
Ink, 0.1 to 0.5 part of thickener CMC are added in agitator tank, are by 0.5 to 0.9 part of thickener in the step 3b by mass parts
CMC is added in agitator tank, is to add in 2 parts of glue SBR in slurry by mass parts in the step (4).
The slurry preparation method of the present invention is that first conductive agent, active material and thickener are added in agitator tank, then
Dry powder stirring is carried out successively, high-viscosity stirring, viscosity adjustment stirring, adds in liquid cement agitation, slurry vacuum defoamation.It is stirred using above-mentioned
Flow is mixed, each link can be completed in relatively short mixing time, even if plus the time used in intermediate linking link, it is whole
Also it is only 95-115min the time required to a flow, compared to the mixing time 600-900min of current wet processing, saves big
Measure the time.It is carried out in addition, whole process of the present invention does not need to the more agitator tank division of labor, it is not required that the material transferred to other use in agitator tank
Material, substantially increases production efficiency.Furthermore the present invention first carries out cathode conductive agent, active material and thickener powder body material
It is dispersed with stirring, avoids conductive agent and generate reunion in the slurry, disperseed using high-viscosity stirring early period, agitating paddle is to the machine of slurry
Tool active force is big, can play good dispersion effect, then adjust and stir using viscosity, each component is made thoroughly to be dispersed, improve
The stability and dispersion effect of slurry.
Specific embodiment
It is described further with reference to specific embodiment：
Embodiment 1：
The preparation method for the graphite negative electrode of lithium ion battery highly viscous slurry that embodiment 1 provides, includes the following steps：
(1) dry powder stirs：2 parts of conductive agents, 95 parts of active material graphite, 0.5 part of thickener CMC are put into and stirred by mass parts
The machine of mixing is stirred, and control agitator tank revolution rotating speed is 15-25 revs/min, and the stirring disk rotating speed for controlling agitator tank is 0-200
Rev/min, it stirs 8 to 12 minutes；
(2) high-viscosity stirring：Add water, adjustment solid content to 67%-78%, control agitator tank revolution rotating speed into agitator tank
It it is 35-60 revs/min, the stirring disk rotating speed for controlling agitator tank is 800-1200 revs/min, is stirred 15 to 25 minutes；
(3) viscosity adjustment stirring, including：3a. control agitator tank revolution rotating speeds are 60-70 revs/min, control agitator tank
It is 1000-1200 revs/min to stir disk rotating speed, adds waterside control agitator tank stirring to agitator tank in 3 to 5 minutes inner edges, will stir
The solid content for mixing slurry in tank is adjusted to 58%-62%, continues that agitator tank is controlled to continue stirring 8 to 12 minutes later；3b. is to stirring
After adding in 0.5 part of thickener CMC in tank, control agitator tank revolution rotating speed is 60-70 revs/min, controls the agitator disk of agitator tank
Rotating speed is 1000-1200 revs/min, is stirred 1-3 minutes；3c. control agitator tank revolution rotating speeds are 60-70 revs/min, and control is stirred
The stirring disk rotating speed for mixing tank is 1000-1200 revs/min, waterside control agitator tank is added to stir to agitator tank in 3 to 5 minutes inner edges
It mixes, the solid content of slurry in agitator tank is adjusted to 51%-55%, continue that agitator tank is controlled to continue stirring 8 to 12 minutes later, obtain
Viscosity to slurry is 2000-4000cp.
(4) liquid cement agitation is added in：It is added in into slurry and presses mass parts by 2 parts of glue SBR, control agitator tank revolution rotating speed
It it is 20-40 revs/min, the stirring disk rotating speed for controlling agitator tank is 500-800 revs/min, is stirred 15 to 25 minutes；
(5) slurry vacuum defoamation：Agitator tank is evacuated to -0.09MPa--0.1MPa, control agitator tank revolution rotating speed is
It 8-12 revs/min, stirs 4 to 6 minutes, obtains finished product.
Embodiment 2：
The preparation method for the graphite negative electrode of lithium ion battery highly viscous slurry that embodiment 2 provides, includes the following steps：
(1) dry powder stirs：2 parts of conductive agents, 95 parts of active material graphite, 0.3 part of thickener CMC are put into and stirred by mass parts
The machine of mixing is stirred, and control agitator tank revolution rotating speed is 15-25 revs/min, and the stirring disk rotating speed for controlling agitator tank is 0-200
Rev/min, it stirs 8 to 12 minutes；
(2) high-viscosity stirring：Add water, adjustment solid content to 67%-78%, control agitator tank revolution rotating speed into agitator tank
It it is 35-60 revs/min, the stirring disk rotating speed for controlling agitator tank is 800-1200 revs/min, is stirred 15 to 25 minutes；
(3) viscosity adjustment stirring, including：3a. control agitator tank revolution rotating speeds are 60-70 revs/min, control agitator tank
It is 1000-1200 revs/min to stir disk rotating speed, adds waterside control agitator tank stirring to agitator tank in 3 to 5 minutes inner edges, will stir
The solid content for mixing slurry in tank is adjusted to 58%-62%, continues that agitator tank is controlled to continue stirring 8 to 12 minutes later；3b. is to stirring
After adding in 0.7 part of thickener CMC in tank, control agitator tank revolution rotating speed is 60-70 revs/min, controls the agitator disk of agitator tank
Rotating speed is 1000-1200 revs/min, is stirred 1-3 minutes；3c. control agitator tank revolution rotating speeds are 60-70 revs/min, and control is stirred
The stirring disk rotating speed for mixing tank is 1000-1200 revs/min, waterside control agitator tank is added to stir to agitator tank in 3 to 5 minutes inner edges
It mixes, the solid content of slurry in agitator tank is adjusted to 51%-55%, continue that agitator tank is controlled to continue stirring 8 to 12 minutes later, obtain
Viscosity to slurry is 2000-4000cp.
(4) liquid cement agitation is added in：It is added in into slurry and presses mass parts by 2 parts of glue SBR, control agitator tank revolution rotating speed
It it is 20-40 revs/min, the stirring disk rotating speed for controlling agitator tank is 500-800 revs/min, is stirred 15 to 25 minutes；
(5) slurry vacuum defoamation：Agitator tank is evacuated to -0.09MPa--0.1MPa, control agitator tank revolution rotating speed is
It 8-12 revs/min, stirs 4 to 6 minutes, obtains finished product.
Embodiment 3：
The preparation method for the graphite negative electrode of lithium ion battery highly viscous slurry that embodiment 3 provides, includes the following steps：
(1) dry powder stirs：2 parts of conductive agents, 95 parts of active material graphite, 0.1 part of thickener CMC are put into and stirred by mass parts
The machine of mixing is stirred, and control agitator tank revolution rotating speed is 15-25 revs/min, and the stirring disk rotating speed for controlling agitator tank is 0-200
Rev/min, it stirs 8 to 12 minutes；
(2) high-viscosity stirring：Add water, adjustment solid content to 67%-78%, control agitator tank revolution rotating speed into agitator tank
It it is 35-60 revs/min, the stirring disk rotating speed for controlling agitator tank is 800-1200 revs/min, is stirred 15 to 25 minutes；
(3) viscosity adjustment stirring, including：3a. control agitator tank revolution rotating speeds are 60-70 revs/min, control agitator tank
It is 1000-1200 revs/min to stir disk rotating speed, adds waterside control agitator tank stirring to agitator tank in 3 to 5 minutes inner edges, will stir
The solid content for mixing slurry in tank is adjusted to 58%-62%, continues that agitator tank is controlled to continue stirring 8 to 12 minutes later；3b. is to stirring
After adding in 0.9 part of thickener CMC in tank, control agitator tank revolution rotating speed is 60-70 revs/min, controls the agitator disk of agitator tank
Rotating speed is 1000-1200 revs/min, is stirred 1-3 minutes；3c. control agitator tank revolution rotating speeds are 60-70 revs/min, and control is stirred
The stirring disk rotating speed for mixing tank is 1000-1200 revs/min, waterside control agitator tank is added to stir to agitator tank in 3 to 5 minutes inner edges
It mixes, the solid content of slurry in agitator tank is adjusted to 51%-55%, continue that agitator tank is controlled to continue stirring 8 to 12 minutes later, obtain
Viscosity to slurry is 2000-4000cp.
(4) liquid cement agitation is added in：It is added in into slurry and presses mass parts by 2 parts of glue SBR, control agitator tank revolution rotating speed
It it is 20-40 revs/min, the stirring disk rotating speed for controlling agitator tank is 500-800 revs/min, is stirred 15 to 25 minutes；
(5) slurry vacuum defoamation：Agitator tank is evacuated to -0.09MPa--0.1MPa, control agitator tank revolution rotating speed is
It 8-12 revs/min, stirs 4 to 6 minutes, obtains finished product.
Above example be only it is fully open is not intended to limit the present invention, all creation purports based on the present invention, without creating
Property labour equivalence techniques feature replacement, should be considered as the application exposure range.
Claims (9)
1. a kind of preparation method of graphite negative electrode of lithium ion battery highly viscous slurry, which is characterized in that include the following steps：
(1) dry powder stirs：After the dry powder material of conductive agent, active material and thickener CMC being added in into agitator tank, control stirring
Tank stirs；
(2) high-viscosity stirring：Into agitator tank plus water, adjustment solid content to 67%-78%, control agitator tank stir；
(3) viscosity adjustment stirring, including：3a. sides add waterside control agitator tank stirring to agitator tank, and slurry in agitator tank is consolidated
Content is adjusted to 58%-62%；3b. adds in thickener CMC, control agitator tank stirring into agitator tank；3c. sides add water to agitator tank
Side control agitator tank stirring, is adjusted to 51%-55%, viscosity is adjusted to 2000-4000cp by the solid content of slurry in agitator tank；
(4) liquid cement agitation is added in：Glue SBR, control agitator tank stirring are added in into slurry；
(5) slurry vacuum defoamation：Agitator tank is evacuated to -0.09MPa--0.1MPa, control agitator tank stirring.
2. according to the preparation method described in right 1, which is characterized in that the control agitator tank described in step (1) stirs specific
It operates and is：It is 15-25 revs/min to control the agitator tank revolution rotating speed, and the stirring disk rotating speed for controlling the agitator tank is 0-200
Rev/min, it stirs 8 to 12 minutes.
3. according to the preparation method described in right 1, the concrete operations of the control agitator tank stirring described in step (2) are：Control
The agitator tank revolution rotating speed is 35-60 revs/min, and the stirring disk rotating speed for controlling the agitator tank is 800-1200 revs/min,
Stirring 15 to 25 minutes.
4. according to the preparation method described in right 1, the concrete operations of the step 3a are：The agitator tank revolution rotating speed is controlled to be
60-70 revs/min, it is 1000-1200 revs/min to control the stirring disk rotating speed of the agitator tank, in 3 to 5 minutes inner edges to stirring
It mixes tank and adds waterside control agitator tank stirring, the solid content of slurry in agitator tank is adjusted to continue control stirring after 58%-62%
Tank continues stirring 8 to 12 minutes.
5. according to the preparation method described in right 4, the concrete operations of the step 3b are：Thickener CMC is added in into agitator tank
Afterwards, it is 60-70 revs/min to control the agitator tank revolution rotating speed, and the stirring disk rotating speed for controlling the agitator tank is 1000-1200
Rev/min, it stirs 1-3 minutes.
6. according to the preparation method described in right 6, the concrete operations of step 3c are：It is 60- to control the agitator tank revolution rotating speed
70 revs/min, it is 1000-1200 revs/min to control the stirring disk rotating speed of the agitator tank, in 3 to 5 minutes inner edges to agitator tank
Add waterside control agitator tank stirring, by the solid content of slurry in agitator tank be adjusted to continue after 51%-55% to control agitator tank after
Continuous stirring 8 to 12 minutes, the viscosity for obtaining slurry are 2000-4000cp.
7. according to the preparation method described in right 1, the concrete operations of the control agitator tank stirring described in step (4) are：Control
The agitator tank revolution rotating speed is 20-40 revs/min, and the stirring disk rotating speed for controlling the agitator tank is 500-800 revs/min,
Stirring 15 to 25 minutes.
8. according to the preparation method described in right 1, the concrete operations of the control agitator tank stirring described in step (5) are：Control
The agitator tank revolution rotating speed is 8-12 revs/min, is stirred 4 to 6 minutes.
9. be according to the preparation method described in 1 to 8 any one of right, in the step (1) by mass parts by 2 parts of conductive agents,
95 parts of active material graphite, 0.1 to 0.5 part of thickener CMC are added in agitator tank, are by 0.5 in the step 3b by mass parts
It is added in agitator tank to 0.9 part of thickener CMC, is to add in 2 parts of glue SBR in slurry by mass parts in the step (4).
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| CN111816878A (en) * | 2020-07-22 | 2020-10-23 | 骆驼集团新能源电池有限公司 | Stirring method for lithium ion battery cathode slurry |
| CN112382744A (en) * | 2020-11-11 | 2021-02-19 | 贵州梅岭电源有限公司 | Preparation method of negative electrode slurry for 3D printing |
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Application publication date: 20180615 |