CN110534707A - A kind of preparation method of lithium titanate slurry - Google Patents
A kind of preparation method of lithium titanate slurry Download PDFInfo
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- CN110534707A CN110534707A CN201910765566.6A CN201910765566A CN110534707A CN 110534707 A CN110534707 A CN 110534707A CN 201910765566 A CN201910765566 A CN 201910765566A CN 110534707 A CN110534707 A CN 110534707A
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- lithium titanate
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- slurry
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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
-
- 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
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
-
- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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 is a kind of preparation method of lithium titanate slurry, belongs to lithium ion battery manufacturing field.The strategy that method of the invention uses two steps to walk, first prepares solvent and portion of binder in high-speed vacuum mixer, and vacuum extraction for several times is carried out after the completion of preparation, obtains the binder solution of certain range of viscosities under room temperature；Secondly lithium titanate, portion of binder and conductive agent are ground with being vibrated in the ball mill with abrasive media, the binder solution prepared before is added drop-wise in ball mill by grinding whithin a period of time simultaneously, slurry is placed in constant-temperature vacuum tub after filtering, vacuum extraction for several times is carried out, the lithium titanate slurry of required viscosity under certain temperature is obtained.
Description
Technical field
The present invention relates to lithium ion battery manufacturing fields, more particularly to a kind of slurry using lithium titanate as negative electrode material
Preparation method.
Background technique
The negative electrode of lithium ion battery being commercialized at present is mainly compound material based on carbon, its advantage be price just
Preferably, energy density is high, but disadvantage, it is also obvious that cycle-index is no more than 3,000 times, head rushes low efficiency, meeting under high magnification charges
Expanding and leading to the problem of dendrite leads to cell safety；Lithium titanate is that high magnification charges not as a kind of " zero strain material " feature
It can expand, platform voltage height will not generate dendrite, and it can be more than 30,000 times that stability, which recycles well, and energy density is low, therefore can answer
In motorbus, bus and energy storage device.
Now industrialization lithium titanate anode production method be by lithium titanate, conductive agent, binder and solvent in groove tank
High-speed stirred 60-120min is carried out using spiral vane, 2-5 vacuum of extraction controls the viscous of final slurry to drive air away
Degree is in 4000-5000cps；The lithium titanate slurry solid content that this method is prepared is in 40-50%, and energy density is in 180-
220Wh/Kg, this method solid content is relatively low, and energy density is not high, can not match the energy density of lithium ion battery demand now；
Patent CN201210133183 " a kind of production method of lithium battery " points out for lithium titanate to be heat-treated, ball milling
Processing, with conductive agent carry out mixing and ball milling processing, glue preparation, and by the lithium titanate and conductive agent that are mixed through ball-milling treatment with
Glue carries out mixed pulp.The preparation process wants 20 hours at the soonest, takes a long time and does not meet industrialized production mode；Simultaneously
The dry ball milling of use, Ball-milling Time account for 10 hours or more, and energy consumption is higher, take a long time and do not meet industrialized production, and
Do not point out ball-milling medium.
Patent CN201611202887 " a kind of preparation method of negative electrode of lithium titanate battery slurry " is pointed out negative electrode active material
Matter, additive, conductive agent, binder carry out vacuum bakeout, then carry out dry-mixing with Vacuum mixer, then with solvent in vacuum
Mixed mud is carried out in kneader, stiff mud shape mixture is formed, then be mixed to form ooze shape mixture with wet with solvent, finally again with molten
Agent mixing dispersion finally obtains slurry.This method still disperses lithium titanate using traditional dry method, dilute by step by step
It releases and finally obtains slurry, it is cumbersome, in order to which mixing uniformity is to process control requirements height, therefore it is not particularly suited for industrial metaplasia
It produces, also there are no lithium battery enterprise using this kind of method production.
Summary of the invention:
The purpose of the invention is to improve the energy density of lithium titanate battery, and it is suitable for fast industrialization and produces；
To achieve the goals above, the following technical solution that the present invention takes:
Step (1) mixes solvent and portion of binder in vacuum high-speed mixer, stands after a certain period of time same
When extraction vacuum, the binder solution for obtaining required range of viscosities under room temperature are spare for several times；
Step (2) vibrates lithium titanate, portion of binder and conductive agent with abrasive media in the ball mill grinds, and grinding is same
When the binder solution prepared before is added drop-wise in ball mill whithin a period of time；
Slurry is placed in constant-temperature vacuum tub after step (3) filtering, vacuum extraction for several times is carried out, obtains institute under assigned temperature
Need the lithium titanate slurry of viscosity；
Further, step (1) individually mixes solvent and portion of binder in above scheme, in order to reduce viscous
The viscosity of agent solution is tied, in favor of the bubble in discharge solution, guarantees to drip in the stability and step 2 of coating into ball mill
The stability added；The purpose of extraction vacuum is to guarantee the stability of coating in order to which the bubble in solution is discharged.
The ratio of step (1) portion of binder is the 30%-75% of total binder in above scheme；Mixing time is 30-
60min；Extraction vacuum number is 1-3 times, vacuum degree 0.5-1MPa；Binder solution range of viscosities is 500-2000cps；It is preferred that
For 800-2000cps.
Step (2) is by the way of ball milling in above scheme, it is therefore an objective to which ball milling dispersion relies on the room machine of decentralized medium
Extruding force and impact force and achieve the purpose that dispersion.Therefore not needing dispersion has higher viscosity, and opposite low viscosity is high
Solid content is easier the progress of dispersion instead；And high stir disperses then to need in the non newtonian dispersion of viscosity higher, ability
There is better shearing force；Therefore ball milling can be such that slurry disperses more evenly in the dispersion of low viscosity；Low viscosity simultaneously
Be conducive to the discharge of bubble in slurry, to make rear end coating more evenly, film coated surface is more smooth, to reach higher energy
Density.The mode that binder solution is added dropwise, in order to guarantee that abrasive has higher solid content when initial grinding,
The volatilization of solvent is reduced simultaneously and reduces the generation of bubble in slurry system.
The ratio of step (2) portion of binder is the 25%-70% of total binder in above scheme；Ball-milling Time 20-
40min, preferably 30min；Ball-milling medium is one of zirconium oxide bead, zirconium silicate pearl, rare earth zirconium pearl, alumina bead or more
Kind；The binder solution time for adding of preparation is 15-30min；
The purpose of step (3) extraction vacuum is to guarantee the stabilization of coating in order to which the bubble in solution is discharged in above scheme
Property；The purpose of constant temperature is that the slurry is easy gel at low temperature.
Step (3) filtering sieve used is stainless steel mesh in above scheme, and aperture is 50-200 mesh (examination abrasive media
Partial size depending on)；Constant temperature is some temperature in 30-70 DEG C, preferably 50 DEG C；Extraction vacuum number is 1-3 times, vacuum degree
0.5-1MPa；Finally obtained lithium titanate slurry viscosity range 3000-5000cps, solid content 50%-60%；Work as lithium titanate
When lithium titanate quality ratio is 92-95% in slurry, range of viscosities at 50 DEG C of lithium titanate slurry is 4000-5000cps, solid content
For 55%-60%.
Above-mentioned preparation method, the lithium titanate particle size range are D50: 0.1 μm -1 μm.
Above-mentioned preparation method, in finally obtained lithium titanate slurry, the content of lithium titanate is in 90-95%；Total binder contains
Amount is mass fraction in 2-5%, the % in 3-5%, conductive agent content.
Above-mentioned preparation method, the conductive agent include: carbon nanotubes (CNT), graphene, acetylene black, carbon fiber (VGCF)
One of or it is a variety of.The binder includes: PVDF, polyvinyl acetate, polyvinylidene fluoride, polyethylene, CMC, CMS-Na,
One of SBR or a variety of.The solvent includes: one of NMP, deionized water, DMF, DMAC, acetone or a variety of.
The utility model has the advantages that compared to the prior art, creatively using the strategy walked step by step, portion of binder is used by the present invention
Solvent, which first dissolves, forms binder solution, and lithium titanate, binder and conductive agent are ground in the ball mill, replace height to stir with ball milling
The mode of dispersion, ball milling can be such that slurry disperses more evenly in the dispersion of low viscosity；Low viscosity is conducive to starch simultaneously
The discharge of bubble in material, to make rear end coating more evenly, film coated surface is more smooth, to reach higher energy density.It will
Binder solution is added in grinding system in a manner of being added dropwise, and the final uniformity for promoting slurry, the slurry is identical viscous
There is higher solid content under degree, to improve the energy density of battery, finally obtained lithium titanate energy of slurry density is more existing
10-20% or more is promoted in conventional production method.This method is easy to operate, and preparation efficiency is high, low in cost, is conducive to industry
The popularization of change produces.Advantages of the present invention: the lithium titanate slurry solid content being prepared can accomplish 50-60%；Energy density
Reach 220-260Wh/Kg, improves 10%-20% compared to present production method；Meet national security, cleaning, efficiently new
The developing direction of the energy.
Specific implementation method:
Below with reference to specific embodiment, the present invention is described in further detail, and described is explanation of the invention
Rather than limit, in following embodiments, unless otherwise specified, the % is mass percent, and described part is parts by weight.
A kind of preparation method of the lithium titanate slurry of embodiment 1, comprising the following steps:
Step (1): 100g solvent NMP and 3g binder SBR is mixed into (revolving speed in vacuum high-speed mixer
1000rpm/min；Time 30min), 30min is stood after the completion and concurrently sets vacuum degree 0.6MPa, and 3 vacuum of extraction are true every time
Empty time 10min, binder solution viscosity 1880cps at 25 DEG C；
Step (2): by partial size D50It is 0.8 μm of lithium titanate 90g, 1g binder CMC and 6g conductive agent acetylene black in ball mill
Middle vibrated with zirconium oxide bead is ground, and zirconium oxide bead additive amount is the 30% of ball mill total volume；Grinding will be prepared before simultaneously
Binder solution is at the uniform velocity added drop-wise in ball mill, time for adding 30min, milling time 30min；
Step (3): being placed in 50 DEG C of vacuum tubs of constant temperature for slurry with after 100 mesh net filtrations, stands 30min, and extraction 3 times
Vacuum, each vacuum time 10min obtain final lithium titanate slurry.
A kind of preparation method of the lithium titanate slurry of embodiment 2, comprising the following steps:
Step (1): 75g solvent DMF, 5g acetone and 2g binder PVDF are mixed in vacuum high-speed mixer
(revolving speed 1000rpm/min；Time 30min), 30min is stood after the completion concurrently sets vacuum degree 0.6MPa, 2 vacuum of extraction,
Each vacuum time 10min, binder solution viscosity 1150cps at 25 DEG C；
Step (2): by partial size D50It is conductive for 0.6 μm of lithium titanate 92g, 2g binder CMC and 2g conductive agent acetylene black and 2g
Agent graphene uses the oscillation grinding of zirconium silicate pearl in the ball mill, and zirconium silicate pearl additive amount is the 30% of ball mill total volume；Grinding
The binder solution prepared before is at the uniform velocity added drop-wise in ball mill simultaneously, time for adding 25min, milling time 30min；
Step (3): being placed in 50 DEG C of vacuum tubs of constant temperature for slurry with after 100 mesh net filtrations, stands 30min, and extraction 3 times
Vacuum, each vacuum time 10min obtain final lithium titanate slurry.
A kind of preparation method of the lithium titanate slurry of embodiment 3, comprising the following steps:
Step (1): by 60g solvent DMAC, 10g deionized water and 1g binder polyvinyl acetate in vacuum high-speed mixer
In mixed (revolving speed 1000rpm/min；Time 30min), 30min is stood after the completion and concurrently sets vacuum degree 0.6MPa, is taken out
Put 2 vacuum, each vacuum time 10min, binder solution viscosity 950cps at 25 DEG C；
Step (2): by partial size D50It is led for 0.4 μm of lithium titanate 95g, 2g binder CMS-Na and 1g conductive agent carbon fiber and 1g
Electric agent carbon nanotubes uses the oscillation grinding of rare earth zirconium pearl in the ball mill, and rare earth zirconium pearl additive amount is the 30% of ball mill total volume；
The binder solution prepared before is at the uniform velocity added drop-wise in ball mill by grinding simultaneously, time for adding 15min, milling time 30min；
Step (3): being placed in 50 DEG C of vacuum tubs of constant temperature for slurry with after 100 mesh net filtrations, stands 30min, and extraction 3 times
Vacuum, each vacuum time 10min obtain final lithium titanate slurry.
Comparative example 1
Step (1): 60g solvent NMP is added in vacuum high speed agitator, sequentially adds partial size D50For 0.8 μm of lithium titanate
100g, 2g binder CMC, 3g binder SBR, 5g conductive agent acetylene black, setting speed 1500rpm/min, mixing time
30min adds 60g solvent NMP, setting speed 1000rpm/min, mixing time 10min；
Step (2): standing 30min and concurrently set vacuum degree 0.6MPa, 3 vacuum of extraction, each vacuum time 10min,
Obtain final lithium titanate slurry.
Embodiment 1-3 and the specific testing result of comparative example are as follows:
In summary using the strategy walked step by step, portion of binder is first dissolved with solvent, then replaces height to stir point with ball milling
Scattered mode, the relatively now conventional production method of finally obtained lithium titanate energy of slurry density promote 10-20% or more.
Claims (9)
1. a kind of preparation method of lithium titanate slurry, which comprises the following steps:
Step (1): solvent and portion of binder are mixed in vacuum high-speed mixer, are stood while being taken out after a certain period of time
Vacuum for several times is put, it is spare in the binder solution of 800-2000cps to obtain range of viscosities under room temperature；
Step (2): lithium titanate, portion of binder and conductive agent being vibrated with abrasive media in the ball mill and ground, and grinding is simultaneously
The binder solution prepared before is added drop-wise in ball mill whithin a period of time；
Step (3): being placed in constant-temperature vacuum tub for slurry after filtering, carries out vacuum extraction for several times, needed for obtaining under assigned temperature
The lithium titanate slurry of viscosity.
2. a kind of preparation method of lithium titanate slurry according to claim 1, it is characterised in that: part is viscous in step (1)
The ratio for tying agent is the 30%-75% of total binder.
3. a kind of preparation method of lithium titanate slurry according to claim 1, it is characterised in that: ball milling is situated between in step (2)
Matter is one of zirconium oxide bead, zirconium silicate pearl, rare earth zirconium pearl or a variety of；Binder solution time for adding is 15-30min.
4. a kind of preparation method of lithium titanate slurry according to claim 1, it is characterised in that: step (3) constant temperature is 30-
Some temperature in 70 DEG C, preferably 50 DEG C.
5. a kind of preparation method of lithium titanate slurry according to claim 1, it is characterised in that: the lithium titanate partial size
Range is D50: 0.4 μm -1.0 μm.
6. a kind of preparation method of lithium titanate slurry according to claim 1, it is characterised in that: the lithium titanate slurry 50
DEG C when range of viscosities be 3000-5000cps, solid content 50%-60%, energy density 220-260Wh/Kg.
7. a kind of preparation method of lithium titanate slurry according to claim 6, it is characterised in that: the titanium that step (3) obtains
The content of lithium titanate is in 90-95% in sour lithium slurry；Total binder content is in 3-5%, and conductive agent content is in 2-5%, the %
For mass fraction.
8. a kind of preparation method of lithium titanate slurry according to claim 7, it is characterised in that: the conductive agent are as follows: receive
One of rice carbon pipe (CNT), graphene, acetylene black, carbon fiber (VGCF) are a variety of；The binder are as follows: PVDF, poly-vinegar acid
One of ethylene, polyethylene, CMC, CMS-Na, SBR are a variety of；The solvent are as follows: NMP, deionized water, DMF, DMAC, third
One of ketone is a variety of.
9. a kind of preparation method of lithium titanate slurry according to claim 7, it is characterised in that: metatitanic acid in lithium titanate slurry
Lithium mass ratio is 92-95%, and range of viscosities at 50 DEG C of finally obtained lithium titanate slurry is 4000-5000cps, and solid content is
55%-60%.
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Cited By (1)
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Application publication date: 20191203 |