CN106252603B - A kind of preparation method of pulp of lithium ion battery - Google Patents
A kind of preparation method of pulp of lithium ion battery Download PDFInfo
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- CN106252603B CN106252603B CN201610797575.XA CN201610797575A CN106252603B CN 106252603 B CN106252603 B CN 106252603B CN 201610797575 A CN201610797575 A CN 201610797575A CN 106252603 B CN106252603 B CN 106252603B
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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
Abstract
The invention discloses a kind of preparation methods of pulp of lithium ion battery.The preparation method takes active material, conductive agent and binder the following steps are included: 1) according to mass ratio；2) prepare glue and mixture: A) binder is added in solvent, it is uniformly mixed, obtains glue；B) active material and conductive agent are uniformly mixed, obtain mixture；3) the 40%~80% of glue is added in mixture, is uniformly dispersed, obtains highly viscous slurry；4) glue of solvent and surplus is added in highly viscous slurry, high speed dispersion obtains low viscosity slurry；5) solvent is added in low viscosity slurry, is uniformly dispersed, adjust slurry viscosity be 4000~15000mPas, then filter, deaeration to get.The preparation method can be improved pulping efficiency；Highly viscous slurry is dispersed with the redisperse conducive to active material and conductive agent, reduces the reunion of conductive agent；Low viscosity slurry high speed dispersion further increases the uniformity of slurry dispersion.
Description
Technical field
The present invention relates to field of lithium ion battery, and in particular to a kind of preparation method of pulp of lithium ion battery.
Background technique
In recent years, lithium ion battery is grown rapidly as a kind of important environmentally friendly green energy, since it has
The advantages that energy density is big, storage life is long, green safe pollution-free, has been widely used in electric car, city rail
Traffic, the mobile fields such as powered base station and scale energy storage.
Important component of the lithium ion cell positive as lithium ion battery, there is important influence to battery performance.
And in anode plate manufacturing process, it first has to active material (such as LiFePO4, cobalt acid lithium), conductive agent (such as Super
P, carbon nanotube, KS-6, carbon fiber etc.), binder (such as Kynoar) and solvent (such as N-Methyl pyrrolidone) in proportion
It carries out being mixed and made into slurry, then slurry is uniformly coated in collection liquid surface according to design requirement, be then dried, grind
Pressure, cross cutting, obtain anode plate.In anode plate manufacturing process, the dispersity of anode sizing agent directly influences subsequent pole
The security performance of the processing performance of plate and entire battery, electrode slurry disperse more uniform, are more conducive to positive electrode maximum
The performance of gram volume, and then it is also beneficial to the high rate performance of battery.
In the prior art, CN103825006A discloses a kind of preparation method of lithium ion battery anode glue size, including with
Lower step: A. weighs positive material according to the ratio of weight ratio positive electrode 90~92%, conductive agent 4~5%, binder 4~5%
Material, conductive agent and binder；B. according to the ratio of weight ratio binder 4~5%, solvent 94~96%, by binder and solvent
Mixing is configured to the mother liquor that concentration is 4~6%；C. positive electrode is tentatively mixed with conductive agent；D. raw material preliminary mixes
Afterwards, 10~15% mother liquors are added, make positive electrode and conductive agent homogeneous immersion, soft powdery is presented in material after infiltration；E. toward leaching
50~60% mother liquors are continuously added in material after profit, are uniformly mixed positive electrode with conductive agent；F. after material is kneaded, to stirring
Mix and 20~25% mother liquor is added in pot is diluted well-mixed material, the viscosity control of slurries 6000~
12000mPaS is to be coated with；According to the positive electrode of invention production, positive electrode can be mixed uniformly and good with conductive agent
Good contact improves material and disperses consistency, improves battery cycle life.But the preparation method of the lithium ion battery anode glue size
The material that chinese raw materials obtains after tentatively mixing and mother liquor incorporation time are long, influence battery production efficiency.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of pulp of lithium ion battery, can improve pulp of lithium ion battery
Preparation efficiency；It can also promote the redisperse of conductive agent and active material simultaneously, reduce conductive agent and reunite.
In order to achieve the goal above, technical solution used by the preparation method of pulp of lithium ion battery of the invention is:
A kind of preparation method of pulp of lithium ion battery, comprising the following steps:
1) according to mass ratio, active material: conductive agent: binder=92~95:2~5:2~6 ratio takes active matter
Matter, conductive agent and binder；
2) prepare glue and mixture:
A) binder of formula ratio is added in the solvent for being equivalent to 14~19 times of binder quality, is uniformly mixed, obtains
Glue；
B) active material of formula ratio and conductive agent are uniformly mixed, obtain mixture；
3) in step 2) B) obtained in step 2) A is added in mixture) gained glue 40%~80%, dispersion is equal
It is even, obtain highly viscous slurry；
4) the resulting highly viscous slurry quality 0.1~0.265 of step 3) is added in the highly viscous slurry that step 3) obtains
The glue of solvent again and surplus, high speed dispersion obtain low viscosity slurry；
5) resulting 0~0.08 times of low viscosity slurry quality of step 4) is added in the low viscosity slurry that step 4) obtains
Solvent is uniformly dispersed, control slurry viscosity be 4000~15000mPas, then filter, deaeration to get.
The preparation of the preparation method of pulp of lithium ion battery of the invention, glue and mixture can carry out simultaneously, improve
The efficiency of slurrying；In mixture, for the first time be added part glue, the viscosity of slurry is higher, the frictional force between particle compared with
Greatly, the redisperse for being conducive to active material and conductive agent, reduces the reunion of conductive agent, while being conducive to shorten subsequent low viscosity slurry
Expect high speed dispersion and adjusts the time dispersed during viscosity；Solvent is added after the remaining glue of second of addition, is carried out low viscous
Slurry high speed dispersion is spent, the uniformity of slurry dispersion is further increased.
The preparation method of pulp of lithium ion battery of the invention can shorten the preparation time of slurry, improve production efficiency,
Production energy consumption is reduced, it is with good economic efficiency.
Step 2) A) in, the binder is Kynoar；The solvent is N-Methyl pyrrolidone.
Preferably, step 2) A) in, the mixing carries out under vacuum conditions, and mixed temperature is 20 DEG C~40
℃.Vacuum degree≤- 0.085MPa of vacuum condition.The mixing using stirring mode, the revolving speed of stirring is 1200~
1800r/min, mixing time are 80~300min.
Preferably, the glue being prepared in step 2) A) 6~10h is stood to reuse.
Preferably, step 2) B) in, the conductive agent be one of Super P, carbon nanotube, KS-6, graphene or
Any combination.The active material is LiFePO4.The mixing carries out under vacuum conditions, and vacuum degree≤-
0.085MPa.Mixing is using the agitating mode for being, the revolving speed of stirring are as follows: revolution 10~20r/min, 300~800r/min of rotation,
Mixing time is 30~50min.
Preferably, in step 3), the temperature of slurry is 30 DEG C~50 DEG C during the dispersion.What the dispersion used
Be stirring mode, the revolving speed of stirring are as follows: revolution 20~30r/min, 100~500r/min of rotation, mixing time be 300~
500min。
Preferably, in step 4), the high speed dispersion carries out under vacuum conditions, during high speed dispersion, slurry
Temperature be 30 DEG C~50 DEG C.Vacuum degree≤- 0.085MPa of vacuum condition.The high speed dispersion using stirring side
Formula, the revolving speed of stirring are as follows: 15~25r/min of revolution, 1500~2500r/min of rotation, mixing time is 160~200min.
In step 5), the vacuum degree that is dispersed in is -0.09MPa~-0.1MPa, under the conditions of slurry temperature is 20~30 DEG C
It carries out.Mode of the dispersion using stirring, the revolving speed of stirring are as follows: revolution 8~15r/min, 400~600r/ of rotation
Min, mixing time are 30~40min.It is 20~30 DEG C, vacuum degree≤- 0.085MPa that slurry viscosity, which is measured, in the temperature of slurry
Under conditions of carry out.The filtering uses three-level filter system filter slurry, and filter core is 100 mesh~150 mesh.The deaeration is true
Empty deaeration, the vacuum degree of vacuum defoamation are -0.09MPa~-0.1MPa.It is de- in vacuum in order to accelerate the spilling of bubble in slurries
During bubble, slurries can also be stirred at low speed.Preferably, inclined heated plate is 45~65min.
Detailed description of the invention
Fig. 1 is the SEM figure in embodiment 1 after lithium ion battery anode glue size coating；
Fig. 2 is the SEM figure in comparative example 1 after lithium ion battery anode glue size coating；
Fig. 3 is the SEM figure in comparative example 2 after lithium ion battery anode glue size coating.
Specific embodiment
Of the invention is described further below in conjunction with specific embodiment.
In specific embodiment, the step 1) A of sizing material is prepared) and prepare the step 1) B of mixture) without sequencing.
In order to improve preparation efficiency, step 1) A in each embodiment) and step 1) B) carry out simultaneously.Step 1) A) stir setting for use
Standby is glue making machine, stirs the equipment used in remaining step as double-planet de-airing mixer.
Embodiment 1
The preparation method of the pulp of lithium ion battery of the present embodiment, comprising the following steps:
1) lithium-iron phosphate active material 93.5g, Super P conductive agent 3g, Kynoar 3.5g are taken；
2) prepare glue and mixture:
A the Kynoar of formula ratio) is added to 49g (being equivalent to 14 times of Kynoar quality) N- crassitude
It is -0.085MPa in vacuum degree, revolving speed is to stir 300min under 1200r/min, and mixing is equal controlled at 40 DEG C in ketone
It is even, glue is obtained, it is spare to stand 8h；
B) lithium-iron phosphate active material of formula ratio and Super P conductive agent are added and closed in slurry kettle, be in vacuum degree-
0.085MPa, revolution revolving speed are 10r/min, and rotation revolving speed is to be dispersed with stirring 30min under 800r/min, are uniformly mixed, must mix
Material；
3) in step 2) B) obtained in 60% step 2) A is added in mixture) resulting glue, control the temperature of slurry
It is 50 DEG C, vacuum degree is -0.085MPa, revolution revolving speed is 20r/min, rotation revolving speed is to stir 400min under 100r/min,
It is uniformly dispersed, obtains highly viscous slurry；
4) it is molten that 25g (0.195 times that is equivalent to highly viscous slurry quality) is added in the highly viscous slurry that step 3) obtains
The glue of agent and surplus, control slurry temperature be 50 DEG C, vacuum degree be -0.085MPa, revolution revolving speed be 15r/min, oneself
Speed of walking around is high speed dispersion 200min under 1500r/min, obtains low viscosity slurry；
5) solvent 7g (0.04 times that is equivalent to low viscosity slurry quality) is added in the low viscosity slurry that step 4) obtains,
It is -0.1MPa in vacuum degree, temperature is 25 DEG C, and revolution revolving speed is 15r/min, rotation revolving speed is stirring under 600r/min
30min obtains the slurry that the viscosity at 30 DEG C is 10000mPas, filter core is used to cross filter pulp for the three-level filter system of 150 mesh
Material, under conditions of stirring at low speed, slurry is vacuumized, vacuum degree be -0.1MPa under vacuum defoamation 65min to get.
Embodiment 2
The preparation method of the pulp of lithium ion battery of the present embodiment, comprising the following steps:
1) active material 92g, KS-6 conductive agent 2g, binder 2g are taken；
The active material is LiFePO4, and binder is Kynoar；
2) prepare glue and mixture:
A) binder of formula ratio is added in 38g (being equivalent to 19 times of binder quality) solvent, controlled at 20
DEG C, it is -0.09MPa in vacuum degree, revolving speed is to stir 80min under 1200r/min, is uniformly mixed, obtains glue, it is spare to stand 6h；
The solvent is N-Methyl pyrrolidone；
B) active material of formula ratio and KS-6 conductive agent are added and closed in slurry kettle, is -0.09MPa, revolution in vacuum degree
Revolving speed is 25r/min, and rotation revolving speed is to be dispersed with stirring 45min under 300r/min, is uniformly mixed, obtains mixture；
3) in step 2) B) obtained in 80% step 2) A is added in mixture) resulting glue, control the temperature of slurry
It is 30 DEG C, vacuum degree is -0.09MPa, revolution revolving speed is 25r/min, rotation revolving speed is to stir 500min under 300r/min,
It is uniformly dispersed, obtains highly viscous slurry；
4) 14g (0.11 times that is equivalent to highly viscous slurry quality) solvent is added in the highly viscous slurry that step 3) obtains
With the glue of surplus, control slurry temperature be 40 DEG C, vacuum degree be -0.09MPa, revolve revolving speed be 18r/min, walk around certainly
Speed is high speed dispersion 180min under 1500r/min, obtains low viscosity slurry；
5) solvent 7g is added in the low viscosity slurry that step 4) obtains and (is equivalent to the 0.047 of low viscosity slurry quality
Times), it is -0.09MPa in vacuum degree, temperature is 30 DEG C, and revolution revolving speed is 8r/min, rotation revolving speed is stirring under 400r/min
30min obtains the slurry that the viscosity at 20 DEG C is 4000mPas, filter core is used to cross filter pulp for the three-level filter system of 100 mesh
Material, under conditions of stirring at low speed, vacuumizes slurry, the vacuum defoamation 45min in the case where vacuum degree is -0.09MPa, i.e.,
?.
Embodiment 3
The preparation method of the pulp of lithium ion battery of the present embodiment, comprising the following steps:
1) active material 95g, graphene conductive agent 5g, binder 6g are taken；
The active material is LiFePO4, and binder is Kynoar；
2) prepare glue and mixture:
A) binder of formula ratio is added in 96g (being equivalent to 16 times of binder quality) solvent, controlled at 30
DEG C, it is -0.095MPa in vacuum degree, revolving speed is to stir 280min under 1800r/min, is uniformly mixed, obtains glue, it is standby to stand 10h
With；
The solvent is N-Methyl pyrrolidone；
B) active material of formula ratio and graphene conductive agent are added and closed in slurry kettle, is -0.095MPa in vacuum degree, it is public
Speed of walking around is 18r/min, and rotation revolving speed is to be dispersed with stirring 50min under 700r/min, is uniformly mixed, obtains mixture；
3) in step 2) B) obtained in 50% step 2) A is added in mixture) resulting glue, control the temperature of slurry
It is 35 DEG C, vacuum degree is -0.095MPa, revolution revolving speed is 30r/min, rotation revolving speed is to stir 300min under 500r/min,
It is uniformly dispersed, obtains highly viscous slurry；
4) it is molten that 40g (0.265 times that is equivalent to highly viscous slurry quality) is added in the highly viscous slurry that step 3) obtains
The glue of agent and surplus, control slurry temperature be 40 DEG C, vacuum degree be -0.095MPa, revolution revolving speed be 25r/min, oneself
Speed of walking around is high speed dispersion 160min under 2500r/min, obtains low viscosity slurry；
5) slurry that the viscosity at 25 DEG C is 12500mPas is measured in the low viscosity slurry that step 4) obtains, using filter
Core is that the three-level filter system filter slurry of 120 mesh vacuumizes slurry under conditions of stirring at low speed, in vacuum degree
For vacuum defoamation 45min under -0.095MPa to get.
Embodiment 4
The preparation method of the pulp of lithium ion battery of the present embodiment, comprising the following steps:
1) lithium-iron phosphate active material 93g, carbon nanotube conducting agent 4g, Kynoar 3g are taken；
2) prepare glue and mixture:
A the Kynoar of formula ratio) is added to 45g (being equivalent to 15 times of Kynoar quality) N- crassitude
It is -0.1MPa in vacuum degree controlled at 35 DEG C in ketone, revolving speed is to stir 120min under 1400r/min, it is uniformly mixed,
Glue is obtained, it is spare to stand 7h；
B) lithium-iron phosphate active material of formula ratio and carbon nanotube conducting agent are added and closed in slurry kettle, be in vacuum degree-
0.1MPa, revolution revolving speed are 15r/min, and rotation revolving speed is to be dispersed with stirring 40min under 500r/min, are uniformly mixed, must mix
Material；
3) in step 2) B) obtained in 40% step 2) A is added in mixture) resulting glue, control the temperature of slurry
It is 45 DEG C, vacuum degree is -0.1MPa, revolution revolving speed is 23r/min, rotation revolving speed is to stir 350min under 250r/min, point
It dissipates uniformly, obtains highly viscous slurry；
4) it is molten that 11.6g (0.1 times that is equivalent to highly viscous slurry quality) is added in the highly viscous slurry that step 3) obtains
The glue of agent and surplus, control slurry temperature be 30 DEG C, vacuum degree be -0.1MPa, revolve revolving speed be 20r/min, rotation
Revolving speed is high speed dispersion 170min under 1800r/min, obtains low viscosity slurry；
5) solvent 12.376g is added in the low viscosity slurry that step 4) obtains and (is equivalent to low viscosity slurry quality
0.08 times), it is -0.1MPa in vacuum degree, temperature is 20 DEG C, and revolution revolving speed is 10r/min, rotation revolving speed is under 450r/min,
35min is stirred, the slurry that the viscosity at 30 DEG C is 15000mPas is obtained, uses filter core for the three-level filter system mistake of 150 mesh
Filter pulp material vacuumizes slurry under conditions of stirring at low speed, the vacuum defoamation 50min in the case where vacuum degree is -0.09MPa,
To obtain the final product.
Experimental example 1
Pulp of lithium ion battery made from the method for Examples 1 to 4 and comparative example 1~2 is respectively adopted, lithium-ion electric is made
Then pond pole piece is assembled then using it as positive plate with negative electrode tab, diaphragm, electrolyte and battery case, activate through chemical conversion
After corresponding battery is made.Test the energy density and AC internal Resistance of each lithium ion battery.Lithium ion battery energy density
Test method are as follows: the discharge capacity after made battery 0.5C constant-current charge to 3.65V, then when with 0.5C constant-current discharge to 2.5V,
Calculate the energy density of battery；The AC internal Resistance test method of lithium ion battery are as follows: battery is with 0.5C constant-current charge to 30%
The AC internal Resistance of battery is tested when SOC.Test result is shown in Table 1.
Table 1 using the lithium ion battery of the electrodes of lithium-ion batteries of Examples 1 to 4 and comparative example 1~2 energy density and
AC internal Resistance test result
| Project | Energy density (Wh/kg) | Internal resistance (m Ω) |
| Embodiment 1 | 138.2 | 0.315 |
| Embodiment 2 | 135.8 | 0.308 |
| Embodiment 3 | 137.6 | 0.295 |
| Embodiment 4 | 136.4 | 0.304 |
| Comparative example 1 | 133.7 | 0.325 |
| Comparative example 2 | 132.4 | 0.329 |
The anode sizing agent obtained using preparation process of the invention, the coating of pole plate works well in coating process, and Fig. 1 is
The SEM of pole piece after coating is characterized, and by can see active material distribution uniform in pole piece in figure, and conductive agent is without obvious group
Poly- phenomenon is conducive to the performance of positive electrode maximum gram volume；Fig. 2 and Fig. 3 is respectively pole after comparative example 1 and the coating of comparative example 2
The SEM of piece is characterized, by being observed that in pole piece that there are certain conductive agent agglomerations in figure.In addition, using the present invention
The anode sizing agent of preparation, obtained battery after die cut, assembling and chemical conversion, energy density and internal resistance of cell test result are such as
Shown in table 1, by can see in table, the lithium ion battery in energy density distribution in embodiment is above conventional cathode slurry
(comparative example 1 and comparative example 2) obtained lithium ion battery, and it is then made lower than conventional cathode slurry production process in internal resistance
The lithium ion battery obtained.
Claims (6)
1. a kind of preparation method of lithium ion battery anode glue size, it is characterised in that: the following steps are included:
1) according to mass ratio, active material: conductive agent: binder=92 ~ 95:2 ~ 5:2 ~ 6 ratio takes active material, conductive agent
And binder；
2) prepare glue and mixture:
A) binder of formula ratio is added in the solvent for being equivalent to 14~19 times of binder quality, is uniformly mixed, obtains glue；
B) active material of formula ratio and conductive agent are uniformly mixed, obtain mixture；
3) step 2 A is added in the mixture obtained in step 2 B)) gained glue 40% ~ 80%, be uniformly dispersed, obtain high viscous
Spend slurry；
4) resulting 0.1 ~ 0.265 times of highly viscous slurry quality of step 3) molten is added in the highly viscous slurry that step 3) obtains
The glue of agent and surplus, high speed dispersion obtain low viscosity slurry；
5) resulting 0 ~ 0.08 times of low viscosity slurry quality of the solvent of step 4) is added in the low viscosity slurry that step 4) obtains,
Be uniformly dispersed, adjust slurry viscosity be 4000 ~ 15000mPas, then filter, deaeration to get；
In step 4), the high speed dispersion carries out under vacuum conditions, and during high speed dispersion, the temperature of slurry is 30 DEG C
~50℃；In step 5), it is described be dispersed in vacuum degree be -0.09MPa~-0.1MPa, under the conditions of slurry temperature is 20 ~ 30 DEG C into
Row；In step 5), the filtering uses three-level filter system filter slurry, and filter core is 100 mesh~150 mesh；It is described in step 5)
Deaeration is vacuum defoamation, and the vacuum degree of vacuum defoamation is -0.09MPa~-0.1MPa.
2. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that: step 2 A) in,
The binder is Kynoar；The solvent is N-Methyl pyrrolidone.
3. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that: step 2 A) in,
The mixing carries out under vacuum conditions, and mixed temperature is 20 DEG C ~ 40 DEG C.
4. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that: step 2 B) in,
The conductive agent is one of Super P, carbon nanotube, KS-6, graphene or any combination.
5. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that: step 2 B) in,
The active material is LiFePO4.
6. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that: in step 3), institute
The temperature for stating slurry during dispersing is 30 DEG C ~ 50 DEG C.
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| CN103187555A (en) * | 2011-12-30 | 2013-07-03 | 万向电动汽车有限公司 | Manufacturing method of lithium ion power battery cathode piece and lithium ion power battery with cathode piece |
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| CN101694872A (en) * | 2009-10-21 | 2010-04-14 | 保定风帆新能源有限公司 | Mixing preparation method of pulp of lithium ion battery |
| CN102201574A (en) * | 2011-04-14 | 2011-09-28 | 武汉理工大学 | Oxygen-vacancy-containing lithium ferrous silicate and carbon composite anode material and preparation method |
| CN102738446A (en) * | 2011-04-15 | 2012-10-17 | 比克国际(天津)有限公司 | Lithium ion battery slurry, preparation method of the lithium ion battery slurry, and lithium ion battery |
| CN103187555A (en) * | 2011-12-30 | 2013-07-03 | 万向电动汽车有限公司 | Manufacturing method of lithium ion power battery cathode piece and lithium ion power battery with cathode piece |
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