CN109326779A - A kind of preparation method of high multiplying power lithium ion battery slurry - Google Patents
A kind of preparation method of high multiplying power lithium ion battery slurry Download PDFInfo
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- 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
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Abstract
The present invention provides a kind of preparation method of high multiplying power lithium ion battery slurry, includes the following steps: step a, mixed slurry: binder and electrocondution slurry are stirred uniformly obtained slurry mix;Step b, active material and conductive dry powder mixed powder: are stirred uniformly obtained powder mixture;Step c, solubilizer stirs: it is uniform that slurry mix and powder mixture are mixed and added into stirring solvent, obtains high multiplying power lithium ion battery slurry.The electrocondution slurry of binder and difficult dispersion with divergent function is stirred dispersion by the present invention in advance, will be held miscible granular solids active material, conductive dry powder blend together, and be remerged and mix together with stirring solvent.Such method is conducive to keep lithium ion battery anode glue size obtained fully dispersed uniformly, improves and efficiency is mixed, so that the time required for reduction is stirred while stirring evenly, and the high rate capability of lithium ion cell positive can be effectively improved.
Description
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of preparation side of high multiplying power lithium ion battery slurry
Method.
Background technique
Lithium ion battery is successfully opened as a kind of novel high-capacity long-life environment-friendly battery since the beginning of the nineties in last century
Since hair, has in electric bicycle, electric car, battery-operated motor cycle, electric tool, energy-storage system, 3C Product field and answered extensively
With compared with ni-Cd, nickel-metal hydride battery, lithium ion battery has high specific energy, operating voltage height, temperature limit wide, puts certainly
Electric rate is low, many advantages, such as having extended cycle life, is pollution-free.And lithium ion battery in the production process, the technological design of slurry
There is larger impact to the performance of lithium ion battery, excellent reasonable technological design can directly promote the electrical property of battery, improve
The efficiency of production.
At present industrial common Li-ion positive electrode slurry conductive agent be SUPER-P and KS-6, CNT, graphene,
One of ECP600JD mix and match.Because CNT, graphene, ECP600JD have respective conductive characteristic, and have simultaneously
The characteristics of hardly possible dispersion, so the time usually prepared is longer, slurry equality obtained is poor, and cannot achieve three kinds even four
The conductive material of kind different characteristics is mixed, to effectively improve the high rate capability of lithium ion battery.
Currently used Li-ion positive electrode slurry preparation method are as follows: binder PVDF and partial solvent NMP is mixed
Gluing solution is made, then by active material, conductive particle SUPER-P, electrocondution slurry CNT are successively mixed evenly, thus
Realize homogenate.Its advantage is that: wet blending process is used, the dissolution of gluing solution completely, sequentially adds various types of materials mixing, obtains
Slurry equality is good.CN201710505746.1 provides a kind of pulp of lithium ion battery and its closes paste-making method, by electrode material,
Binder carries out mixed processing in sealable slurry tank, obtains the first mixed material;It is successively added in the first mixed material
CNT conducting resinl dilution of the viscosity less than 3000cP.s and the first conjunction slurry solvent mixed processing obtain the second mixed material;Second
Slurry solvent is closed in addition second in mixed material, carries out mixed processing and obtains pulp of lithium ion battery.Pass through between each step of this method
Synergistic effect significantly improves the production efficiency for closing slurry;Pulp of lithium ion battery obtained is with good stability simultaneously and disperses
Property.The disadvantage is that: mixing time is too long, usually prepares the time of one pot of slurry in 8h or so, and every pot of slurrying, all material all need
Redistribution is wanted, multiple mixing time is longer, and has stringent sequencing between each step, and flexibility is inadequate, is unfavorable for producing
It can efficiency.
Summary of the invention
The technical problem to be solved in the present invention is that being lacked for present on the preparation method of existing Li-ion positive electrode slurry
It falls into, proposes a kind of high multiplying power lithium ion anode sizing agent and preparation method.
To achieve the goals above, the present invention realizes by the following technical solutions.
A kind of preparation method of high multiplying power lithium ion battery slurry, includes the following steps:
Step a, binder and electrocondution slurry mixed slurry: are stirred uniformly obtained slurry mix;
Step b, active material and conductive dry powder mixed powder: are stirred uniformly obtained powder mixture;
Step c, solubilizer stirs: it is uniform that slurry mix and powder mixture are mixed and added into stirring solvent, obtains
High multiplying power lithium ion battery slurry.
Further, PVDF (Kynoar) powder that the binder is 1.5~3 parts of mass fraction, the conduction
Slurry includes 7.5~25 parts of mass fraction of CNT (carbon nanotube) slurry and 5~17 parts of mass fraction of graphene slurry.
Further, the iron phosphate powder that the active material is 92.5~97.5 parts of mass fraction, it is described conductive dry
Powder includes 0.3~1.5 part of mass fraction of SUPER-P (conductive black) and 0.2~1.5 part of mass fraction of ECP600JD (super
Lead carbon black).
Further, the NMP (N-Methyl pyrrolidone) that the solvent is 43~97.5 parts of mass fraction.
Further, CNT (carbon nanotube) slurry is the sticky state slurry of solid content 4%~7%, dispersant
1~20 μm of≤1.3%, CNT length of material, 2~20nm of outer diameter.
Further, the graphene slurry be solid content 4%~7% sticky state slurry, dispersant≤
1.4%, graphene is 1~7 μm of diameter, the few layer of graphene of 2~10nm of thickness.
Further, the ECP600JD (superconduction carbon black) is one kind of Ketjen black, specific surface area 800m2/ g or more.
Further, the stirring in the step 1 is carried out using double-planet stirred tank, stirring 40~60rpm of revolution, from
Turn 1000~3000rpm, mixing time is 3~4 hours.
Further, the stirring in the step 2 is carried out using dry powder ball mill, 50~200rpm of revolving speed stirring, stirring
Time was at 0.5~1 hour.
Further, the stirring in the step 3 is carried out using double-planet stirred tank, stirring 40~60rpm of revolution, from
Turn 1000~2500rpm, mixing time is 2~3 hours.
Beneficial effects of the present invention:
The present invention in step a, by the electrocondution slurry CNT of binder PVDF material and difficult dispersion with divergent function and
Graphene is stirred in advance, obtains fully dispersed uniform slurry mix.In stepb, miscible graininess will be held
Solid active agents, conductive dry powder SUPER-P, ECP600JD are mixed, and obtain finely dispersed powder mixture.Again will
Slurry mix, powder mixture are stirred together with solvent, can compress the mixing time for reducing step b and step c, from
And it is easy to keep lithium ion battery anode glue size obtained fully dispersed uniformly.
There is the accounting of binder PVDF powder and electrocondution slurry, active material and conductive dry powder and solvent in the present invention
It is uniformly mixed in each step conducive to mixture, reduces and mix to the uniformly required time.Step a and step b can simultaneously into
Row, preparation process flexibility is big, reduces preparation time for optimization and provides essential condition.
Step a and step c is stirred using double-planet stirred tank in the present invention, and step b is mixed using dry powder ball mill, will be held
Miscible granular solids active material, conductive dry powder SUPER-P, ECP600JD are mixed with dry powder ball mill, and hardly possible is stirred
The step a of dispersion is using the revolution that the better double-planet stirred tank of mixing effect stirs and uses mixing effect best and walks around certainly
Speed makes resource obtain rationalizing utilization.
Conductive dry powder in electrocondution slurry and step b, can divide multiple batches of be transferred in step c stirred tank in step a of the present invention
The preparation of anode slurry of high-rate is carried out, pulping efficiency can be greatly improved in production process.
The conductive material that lithium ion battery anode glue size produced by the present invention contains includes that SUPER-P, CNT, graphene are taken
Point-line-face conductive network with formation, and the high-specific surface area of conductive dry powder ECP600JD material possesses strong liquid suction function,
Guarantee that the internal resistance of cell will not increase because of the variation of volume.
A kind of anode slurry of high-rate provided by the invention and preparation method thereof compared with the existing technology and
Speech, mixing time is shorter, and stirring is more uniform, and can effectively improve the high rate capability of lithium ion cell positive.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is preparation process figure of the present invention;
Fig. 2 is embodiment and comparative example 5C charging voltage capacity ratio chart;
Fig. 3 is embodiment and comparative example 5C discharge voltage capacity ratio chart.
Specific embodiment
In order to be more clear the purpose of the present invention, technical solution and advantageous effects, below in conjunction with attached drawing and implementation
Mode, the present invention will be described in further detail.It should be understood that embodiment described in this specification is used for the purpose of
It explains the present invention, is not intended to the limitation present invention.
Such as Fig. 1, the present invention provides a kind of preparation method of high multiplying power lithium ion battery slurry, includes the following steps: step
A, binder and electrocondution slurry mixed slurry: are stirred uniformly obtained slurry mix;Step b, mixed powder: will be active
Substance and conductive dry powder are stirred uniformly obtained powder mixture;Step c, solubilizer stirs: by slurry mix and dry powder
It is uniform that mixture is mixed and added into stirring solvent, obtains high multiplying power lithium ion battery slurry.This method will be with divergent function
Binder and the electrocondution slurry of difficult dispersion are stirred dispersion in advance, will hold miscible granular solids active material, conduction
Dry powder blend together, is remerged and is mixed together with stirring solvent.Such method is conducive to make lithium ion cell positive obtained
Slurry is fully dispersed uniformly, improves and efficiency is mixed, so that reducing the time required for stirring while stirring evenly.
Preferably, PVDF (Kynoar) powder that the binder is 1.5~3 parts of mass fraction, the conductive paste
Material includes 7.5~25 parts of mass fraction of CNT (carbon nanotube) slurry and 5~17 parts of mass fraction of graphene slurry, described
The iron phosphate powder that active material is 92.5~97.5 parts of mass fraction, the conduction dry powder includes mass fraction 0.3~1.5
The SUPER-P (conductive black) and 0.2~1.5 part of mass fraction of ECP600JD (superconduction carbon black) of part, the solvent are quality
The NMP (N-Methyl pyrrolidone) that 43~97.5 parts of number, conductive material include that SUPER-P, CNT, graphene arrange in pairs or groups to be formed
Point-line-face conductive network, and the high-specific surface area of conductive dry powder ECP600JD material possesses strong liquid suction function, guarantees battery
Internal resistance will not increase because of the variation of volume.Binder PVDF powder and electrocondution slurry, active material and conductive dry powder, Yi Jirong
The accounting of agent is conducive to mixture and is uniformly mixed in each step, reduces and mixes to the uniformly required time.
Preferably, CNT (carbon nanotube) slurry be solid content 4%~7% sticky state slurry, dispersant≤
1~20 μm of 1.3%, CNT length of material, 2~20nm of outer diameter, the graphene slurry is that the sticky state of solid content 4%~7% is starched
Material, dispersant≤1.4%, graphene are 1~7 μm of diameter, the few layer of graphene of 2~10nm of thickness, the ECP600JD
(superconduction carbon black) is one kind of Ketjen black, specific surface area 800m2/ g or more.The difficulty that is stirred of slurry and binder is maximum
, the solid contents of two kinds of slurries, dispersing agent, the size of material and ECP600JD specific surface area can guarantee slurry and binder into
Row stirs evenly sufficiently.
Preferably, the stirring in the step a is carried out using double-planet stirred tank, stirring 40~60rpm of revolution, rotation
1000~3000rpm, mixing time are 3~4 hours.Stirring in the step b is carried out using dry powder ball mill, and revolving speed 50~
200rpm stirring, mixing time was at 0.5~1 hour.Stirring in the step c is carried out using double-planet stirred tank, and stirring is public
Turn 40~60rpm, 1000~2500rpm of rotation, mixing time is 2~3 hours.Step a and step c uses double-planet stirred tank
Stirring, step b will hold miscible granular solids active material using dry powder ball mill mixing, conductive dry powder SUPER-P,
ECP600JD is mixed with dry powder ball mill, and the step a that hardly possible is dispersed with stirring is stirred using the better double-planet stirred tank of mixing effect
It mixes and the revolution for using mixing effect best and rotation revolving speed, resource is made to obtain rationalizing and use.
A kind of anode slurry of high-rate provided by the invention and preparation method thereof compared with the existing technology and
Speech, mixing time is shorter, and stirring is full and uniform, can effectively improve the high rate capability of lithium ion cell positive.
The present invention successively carries out test of many times, and it is further detailed as reference pair invention progress now to lift A partial experiment result
Description, below with reference to specific
Embodiment 1
Sa, electrocondution slurry CNT 400kg that addition solid content is 5% in the double-planet stirred tank of 500L, solid content are
5% electrocondution slurry graphene 280kg, binder PVDF dry powder 40kg, by revolution 45rpm, after rotation 1500rpm stirs 3h,
Positive conductive slurry mix is made, with the 15rpm that revolves, rotation 100rpm is mixed slowly.
Sb, in the dry powder ball mill of 2000L, active compound lithium iron phosphate material 1600kg, conductive dry powder is added
After stirring 1h by revolving speed 150rpm, anode powder mixture is made in SUPER-P 16kg, conductive dry powder ECP600JD8kg.
Sc, by electrocondution slurry mixture 120kg obtained, positive powder mixture 400kg obtained, nmp solvent 290kg
In the double-planet stirred tank of 500L, by revolution 45rpm, rotation 1200rpm, after 2.5h is mixed, solid content 50% is made
Lithium ion battery anode glue size.
Embodiment 2
Sa, electrocondution slurry CNT 300kg that addition solid content is 5% in the double-planet stirred tank of 400L, solid content are
5% electrocondution slurry graphene 220kg, binder PVDF dry powder 27kg, by revolution 45rpm, after rotation 1500rpm stirs 3h,
Positive conductive slurry mix is made, with the 15rpm that revolves, rotation 80rpm is mixed slowly.
Sb, in the double-planet stirred tank of 1000L, active material nickel-cobalt-manganese ternary material 800kg, conductive dry powder is added
It is dry that anode is made from after revolving speed 1000rpm stirring 0.5h by revolution 45rpm in SUPER-P8kg, conductive dry powder ECP600JD4kg
Powder mixture.
Sc, electrocondution slurry mixture 60kg obtained, positive powder mixture 200kg obtained, nmp solvent 85kg are existed
In the double-planet stirred tank of 500L, by revolution 45rpm, rotation 1200rpm, after 2h is mixed, the lithium of solid content 65% is made
Ion battery anode sizing agent.
Comparative example
S1, in the double-planet stirred tank of 500L, be added binder PVDF 3.4kg dry powder and solvent NMP 290kg revolution
3h is mixed in 40rpm, rotation 800rpm, obtains PVDF adhesive solution.
S2, in PVDF gluing solution, be added active compound lithium iron phosphate 370kg, conductive dry powder SUPER-P 3kg,
It is mixed after ECP600JD 8kg, by revolution 35rpm, rotation 1200rpm, stirs 4h, obtain thick mixed slurry.
S3, in obtained thick mixed slurry, be added solid content be 5% electrocondution slurry CNT80kg, solid content 5%
Electrocondution slurry graphene 80kg, revolve 35rpm, rotation 1400rpm, stir 3h, guarantee slurry solid content 50%, led
The wet blending process pulp of lithium ion battery of electric material.
Embodiment 1, embodiment 2 and comparative example are prepared into slurry time comparison such as table 1:
Table 1
Grouping | Embodiment 1 | Embodiment 2 | Comparative example |
Preparation time | 5.5 hour | 5 hours | 10 hours |
The slurry of slurry and comparative example preparation prepared by embodiment 1, prepares according to lithium ion battery, carries out identical work
The coating of skill, to lithium ion battery is made after roller, cross cutting, lamination, storage, fluid injection, lithium ion battery cell obtained is evolved
After identical common process chemical conversion, then high power charging-discharging test is carried out, compares 5C charge-discharge performance, test result such as Fig. 2, figure
3.It is suitable from the high rate capability of embodiment and comparative example known to obtained charging/discharging voltage capacity ratio curve.
To sum up, the high rate capability of embodiment and comparative example is suitable, but preparation time is significantly reduced, and prepares slurry
Time is minimum only to be needed 5 hours.
The foregoing describe basic principles and main features of the invention and advantages of the present invention.The technical staff of the industry answers
The understanding, the present invention is not limited to the above embodiments, and the above embodiments and description only describe of the invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these change and change
Into all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent
It defines.
Claims (10)
1. a kind of preparation method of high multiplying power lithium ion battery slurry, which comprises the steps of:
Step a, binder and electrocondution slurry mixed slurry: are stirred uniformly obtained slurry mix;
Step b, active material and conductive dry powder mixed powder: are stirred uniformly obtained powder mixture;
Step c, solubilizer stirs: it is uniform that slurry mix and powder mixture are mixed and added into stirring solvent, obtains high power
Rate pulp of lithium ion battery.
2. the preparation method of high multiplying power lithium ion battery slurry according to claim 1, which is characterized in that the binder is
1.5~3 parts of mass fraction of Kynoar powder, the electrocondution slurry include 7.5~25 parts of mass fraction of carbon nanotube
Slurry and 5~17 parts of mass fraction of graphene slurry.
3. the preparation method of high multiplying power lithium ion battery slurry according to claim 1, which is characterized in that the active material
For 92.5~97.5 parts of iron phosphate powder of mass fraction, the conduction dry powder includes 0.3~1.5 part of mass fraction of conduction
Carbon black and 0.2~1.5 part of mass fraction of superconduction carbon black.
4. the preparation method of high multiplying power lithium ion battery slurry according to claim 1, which is characterized in that the solvent is matter
The N-Methyl pyrrolidone of 43~97.5 parts of number of amount.
5. the preparation method of high multiplying power lithium ion battery slurry according to claim 2, which is characterized in that the carbon nanotube
Sticky state slurry of the slurry for solid content 4%~7%, dispersant≤1.3%, 1~20 μm of carbon nano-tube material length, outside
2~20nm of diameter.
6. the preparation method of high multiplying power lithium ion battery slurry according to claim 2, which is characterized in that the graphene slurry
Material is the sticky state slurry of solid content 4%~7%, and dispersant≤1.4%, graphene is 1~7 μm of diameter, thickness 2~
The few layer of graphene of 10nm.
7. the preparation method of high multiplying power lithium ion battery slurry according to claim 3, which is characterized in that the superconduction carbon black
For one kind of Ketjen black, specific surface area 800m2/ g or more.
8. the preparation method of high multiplying power lithium ion battery slurry according to claim 1, which is characterized in that in the step a
Stirring using double-planet stirred tank carry out, stirring revolution 40~60rpm, 1000~3000rpm of rotation, mixing time be 3~4
Hour.
9. the preparation method of high multiplying power lithium ion battery slurry according to claim 1, which is characterized in that in the step b
Stirring using dry powder ball mill carry out, 50~200rpm of revolving speed stirring, mixing time was at 0.5~1 hour.
10. the preparation method of high multiplying power lithium ion battery slurry according to claim 1, which is characterized in that in the step c
Stirring using double-planet stirred tank carry out, stirring revolution 40~60rpm, 1000~2500rpm of rotation, mixing time be 2~3
Hour.
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