CN107681119A - A kind of scattered method for preparing lithium battery slurry of no paddle - Google Patents
A kind of scattered method for preparing lithium battery slurry of no paddle Download PDFInfo
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- CN107681119A CN107681119A CN201610623327.3A CN201610623327A CN107681119A CN 107681119 A CN107681119 A CN 107681119A CN 201610623327 A CN201610623327 A CN 201610623327A CN 107681119 A CN107681119 A CN 107681119A
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- lithium battery
- battery slurry
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- preparing lithium
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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
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
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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 scattered method for preparing lithium battery slurry of no paddle.Using container tank revolution and autobiography at a high speed, make between solid particle therein, high velocity impact and shearing are produced between particle and tank body, all solids particle is not reassociated, and be evenly dispersed in solvent.10min is most only needed soon using a homogenization process of the invention, substantially increases the efficiency of homogenate." dead band " is not present in dispersion process, improves the mixing uniformity and dispersiveness of slurry, and whole process does not produce bubble, can be directly coated with without processing.Present invention is particularly suited for button cell and small-sized Soft Roll, cylinder, steel aluminum-shell battery production among use.
Description
Technical field
The present invention relates to technical field of lithium-ion battery, more particularly to a kind of efficiency for improving homogenate, improves and starches
The mixing uniformity and dispersiveness of material, and whole process does not produce bubble, disperses without what processing can be directly coated with without paddle
The method for preparing lithium battery slurry.
Background technology
Lithium ion battery is because with energy density is high, output voltage is high, self-discharge rate is low, service life is long, memoryless effect
It should obtain people with environment-friendly grade excellent characteristics and greatly pay close attention to.Lithium battery be widely used in notebook computer, mobile phone,
The mobile electronic terminal devices such as video camera, instrument and meter, electric tool.In addition, lithium ion battery applications electric automobile (EV),
The demand of the high-tech industries such as energy storage, military project also constantly expands.Important industry of the lithium battery as national new energy strategy, in state
Under the support of family's policy, develop with undergoing blowout.
Lithium battery slurry is typically uniformly mixed by electrode active material, conductive agent, binding agent and dispersant.Slurry body
System belongs to highly viscous solid-liquid two-phase suspension, and electrode slurry mixing dispersing technology is the important step of lithium battery production.Electrode slurry
The dispersiveness and uniformity of various materials in material, directly affect the impedance magnitude of lithium battery, degree of polarization, the degree of consistency, follow
The performances such as ring life-span, the performance for improving lithium battery is had a very big impact.
Lithium ion battery manufacturer typically carries out mixing point to lithium battery slurry using planetary vacuum dispersion machine at present
Dissipate, contain agitating paddle in planetary dispersion machine, make pulp flow around agitating paddle, rotation using the rotation and revolution of agitating paddle
Turn, collision.Easily there is " dead band " in this process, and bubble occurs, it is necessary to finally do application of vacuum, to prevent coated
There is hole in pole piece in journey.
In addition, this process is generally Multistep feeding, progressively disperse, add first low speed premix after each step dry powder material,
Solvent is set to infiltrate dry powder, then high speed is disperseed again.Slurry is scattered to need 6-8.5 hours total time.It is scattered mixing to be present in this method
The problem of not thorough low with efficiency.
The content of the invention
For above technical barrier existing for current technology, starched the invention provides one kind without the scattered lithium battery for preparing of paddle
The method of material.The efficiency of homogenate can be improved using the present invention, improve the mixing uniformity and dispersiveness of slurry, and whole process
Bubble is not produced, can be directly coated with without processing.Present invention is particularly suited for button cell and small-sized Soft Roll, cylinder, steel aluminium
Used among the production of housing battery.
To achieve these goals, the present invention uses following technical scheme：
A kind of scattered method for preparing lithium battery slurry of no paddle, homogenization process be by negative or positive electrode active material, conductive agent,
Auxiliary agent is scattered in a solvent with binding agent, is uniformly mixed using without paddle, slurry is made.In the technical program, pass through at a high speed
Dispersed ultrafine is sheared, moment microcosmic mixing is carried out to material in the presence of high shear and disperses, can thoroughly avoid
Slurry dead angle in conventional mixer, reach the uniform effect of dispersed ultrafine；The solvent in the manufacturing process of whole slurry simultaneously
Addition in batches, it is ensured that slurry viscosity is small during being mixed with of slurry, and each component can be carried out at a higher temperature
The motion of violent molecular level, so as to further from it is microcosmic it is upper carry out anode sizing agent it is ultra-fine dispersed, on a microscopic level
It ensure that battery excellent performance and uniformity.
Preferably, the positive active material be cobalt acid lithium, nickle cobalt lithium manganate, LiMn2O4, LiFePO4, rich lithium manganese,
Mixture more than one or both of orthophosphates, nickel manganese binary material.
Preferably, the negative electrode active material is more than one or both of graphite, soft or hard carbon, silicon-carbon compound
Mixture.
Preferably, the conductive agent is carbon black, CNT, vapour deposition carbon fiber or one kind in graphene or two
The mixture of the kind above.
Preferably, the binding agent is in sodium carboxymethylcellulose, acrylate, epoxy resin, polyurethane, PVDF
One or more kinds of mixtures.
Preferably, the solvent is one kind in water, NMP, acetone.
Preferably, the auxiliary agent is mass ratio 1:0.8:3 poly- 3,4 ethylenedioxy thiophene, titanium carbide and polyaniline bag
The indium oxide covered.In the technical program, poly- 3, the addition of the indium oxide of 4 ethylenedioxy thiophenes, titanium carbide and polyaniline-coated
Each component can be made to be uniformly dispersed in slurry, and improve the performance of slurry, so as to improve the performance of battery.
Preferably, the preparation method of the indium oxide of polyaniline-coated is：Indium oxide is dissolved in diethylene glycol (DEG) and obtains reactant
System, sodium hydroxide is then slowly added into, 140-160 DEG C is warming up in 2-2.5h after stirring 1-3h, is cooled down after reacting 1-3h；From
The sediment that gains in depth of comprehension arrive uses volume ratio 1 successively:2 ethanol washs with methyl acetate mixed solution, acetone, deionized water, vacuum
It is dried to obtain base core nano indium oxide；Then by the nano oxidized chlorine ultrasonic disperse of base core in absolute ethyl alcohol, addition contains polyphenyl
The ethanol solution of amine, concentrated ammonia liquor is added dropwise, stirring reaction 1-1.5h at 85-95 DEG C, the sediment being centrifugally separating to obtain is successively
Washed with absolute ethyl alcohol, deionized water, crushed after roasting and obtain polyaniline-coated nano indium oxide.
Preferably, the parts by weight of each component are respectively during homogenate：400-520 part negative or positive electrodes active material,
6.4-11 parts conductive agent, 10-15 parts auxiliary agent, 6.4-16.8 parts binding agent and 439-781 part solvents.
Preferably, it the described method comprises the following steps：
(1) positive active material or negative electrode active material, conductive agent, adhesive powder and auxiliary agent are weighed, is added in homogenate tank, and
The solvent of 1/3 amount is added, it is 45-75wt% to make its solid content；
(2) homogenate tank is put into instrument, makes tank body autobiography and revolution simultaneously, rotation rotating speed is 500-1500rpm, and revolve round the sun rotating speed
For 55-60rpm, rotational time 1-5min；
(3) rotating speed is heightened to 2500-3500rpm, and revolved round the sun rotating speed 20-35rpm, and 2-5 points of frozen water cooling is put into after time 2-10min
Clock；
(4) repeat step (3) 1-3 times；Then the solvent of surplus is added, it is 30-60wt% to make its solid content, in 1500-
Continue to disperse under 2500rpm, time 1-3min, obtain lithium battery slurry.
The homogenization process positive pole and negative pole of the present invention is suitable, wherein the positive active material is cobalt acid lithium
(LiCoO2), nickle cobalt lithium manganate [LiNixCoyMn(1-x-y)O2], LiMn2O4 (LiMn2O4), LiFePO4 (LiFePO4), rich lithium manganese
(xLi2MnO3·yLiMO2), orthophosphates (LiCoPO4And LiNiPO4), nickel manganese binary material (LiNi0.5Mn1.5O4) at least
It is a kind of；The negative electrode active material is at least one of graphite, soft or hard carbon, silicon-carbon cathode composite；The conductive agent be carbon black,
CNT, vapour deposition at least one of carbon fiber or graphene；The binding agent is sodium carboxymethylcellulose (CMC), third
At least one of olefin(e) acid ester, epoxy resin, polyurethane, PVDF (polyvinylidene fluoride).The solvent is in water, NMP, acetone
One kind.
The present invention is made between solid particle therein, produced between particle and tank body using container tank revolution and autobiography at a high speed
Raw high velocity impact and shearing, make all solids particle not reassociate, and are evenly dispersed in solvent；The invention provides one kind
The pervasive method of lithium battery slurry is prepared, a homogenization process most only needs 10min soon, substantially increases the efficiency of homogenate, disperses
During " dead band " is not present, the mixing uniformity and dispersiveness of slurry are improved, and whole process does not produce bubble, without place
Reason can be directly coated with.
Embodiment
Below by specific embodiment, technical scheme is described in further detail.It should be appreciated that this hair
Bright implementation is not limited to the following examples, and any formal accommodation and/or change made to the present invention will all fall
Enter the scope of the present invention.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments, it is the normal of this area unless otherwise instructed
Rule method.
Embodiment 1
A kind of scattered method for preparing lithium battery slurry of no paddle, the described method comprises the following steps：
(1) 400 parts of negative electrode active material Delaniums, 6.4 parts of conductive agent carbon blacks, 6.4 parts of adhesive powder CMC and 10 parts are weighed
Auxiliary agent, add in homogenate tank, and add 146.3 parts of aqueous solvent, it is 45wt% to make its solid content；
(2) homogenate tank is put into instrument, makes tank body autobiography and revolution simultaneously, rotation rotating speed is 500rpm, and revolution rotating speed is
55rpm, rotational time 1min；
(3) rotating speed is heightened to 2500rpm, and revolved round the sun rotating speed 20rpm, and frozen water is put into after time 2min and is cooled down 2 minutes；
(4) repeat step (3) 1 times；Then 292.7 parts of aqueous solvent is added, it is 30wt% to make its solid content, at 1500 rpm
Continue to disperse, time 1min, obtain lithium battery slurry.
Auxiliary agent is mass ratio 1:0.8:The indium oxide of 3 poly- 3,4 ethylenedioxy thiophene, titanium carbide and polyaniline-coated.
The preparation method of the indium oxide of polyaniline-coated is：Indium oxide is dissolved in diethylene glycol (DEG) and obtains reaction system, Ran Houhuan
It is slow to add sodium hydroxide, 140 DEG C are warming up in 2h after stirring 1h, is cooled down after reacting 1h；Obtained sediment is centrifuged to use successively
Volume ratio 1:2 ethanol washs with methyl acetate mixed solution, acetone, deionized water, and it is nano oxidized that vacuum drying obtains base core
Indium；Then the nano oxidized chlorine ultrasonic disperse of base core is added into the ethanol solution containing polyaniline in absolute ethyl alcohol, be added dropwise
Concentrated ammonia liquor, stirring reaction 1h at 85 DEG C, the sediment being centrifugally separating to obtain are washed with absolute ethyl alcohol, deionized water successively, are calcined
Crush afterwards and obtain polyaniline-coated nano indium oxide.Fineness test is carried out to obtained slurry, is as a result 23.
Embodiment 2
A kind of scattered method for preparing lithium battery slurry of no paddle, the described method comprises the following steps：
(1) 480 parts of positive active material richness lithium manganese, 8 parts of conductive agent graphenes, 12 parts of adhesive powder acrylate and 12 are weighed
Part auxiliary agent, add in homogenate tank, and add 200 parts of solvent NMP, it is 55wt% to make its solid content；
(2) homogenate tank is put into instrument, makes tank body autobiography and revolution simultaneously, rotation rotating speed is 900rpm, and revolution rotating speed is
58pm, rotational time 3min；
(3) rotating speed is heightened to 3000rpm, and revolved round the sun rotating speed 25rpm, and frozen water is put into after time 5min and is cooled down 4 minutes；
(4) repeat step (3) 2 times；Then add 400 parts of solvent NMP, it is 45wt% to make its solid content, under 2000rpm after
It is continuous scattered, time 2min, obtain lithium battery slurry.
Auxiliary agent is mass ratio 1:0.8:The indium oxide of 3 poly- 3,4 ethylenedioxy thiophene, titanium carbide and polyaniline-coated.
The preparation method of the indium oxide of polyaniline-coated is：Indium oxide is dissolved in diethylene glycol (DEG) and obtains reaction system, Ran Houhuan
It is slow to add sodium hydroxide, 150 DEG C are warming up in 2.5h after stirring 2h, is cooled down after reacting 2h；Centrifuge obtained sediment successively
With volume ratio 1:2 ethanol washs with methyl acetate mixed solution, acetone, deionized water, and vacuum drying obtains base core nano oxygen
Change indium；Then the nano oxidized chlorine ultrasonic disperse of base core is added into the ethanol solution containing polyaniline in absolute ethyl alcohol, dripped
Enriching ammoniacal liquor, stirring reaction 1.5h at 90 DEG C, the sediment being centrifugally separating to obtain are washed with absolute ethyl alcohol, deionized water successively,
Crushed after roasting and obtain polyaniline-coated nano indium oxide.Fineness test is carried out to obtained slurry, is as a result 22.
Embodiment 3
A kind of scattered method for preparing lithium battery slurry of no paddle, the described method comprises the following steps：
(1) weigh 520 parts of positive active material cobalt acid lithiums, 11 parts of conductive agent CNTs, 16.8 parts of adhesive powder PVDF with
15 parts of auxiliary agents, add in homogenate tank, and add 260.3 parts of solvent acetone, it is 75wt% to make its solid content；
(2) homogenate tank is put into instrument, makes tank body autobiography and revolution simultaneously, rotation rotating speed is 1500rpm, and revolution rotating speed is
60rpm, rotational time 5min；
(3) rotating speed is heightened to 3500rpm, and revolved round the sun rotating speed 35rpm, and frozen water is put into after time 10min and is cooled down 5 minutes；
(4) repeat step (3) 3 times；Then 520.7 parts of solvent acetone is added, it is 60wt% to make its solid content, in 2500rpm
Under continue to disperse, time 3min, obtain lithium battery slurry.
Auxiliary agent is mass ratio 1:0.8:The indium oxide of 3 poly- 3,4 ethylenedioxy thiophene, titanium carbide and polyaniline-coated.
The preparation method of the indium oxide of polyaniline-coated is：Indium oxide is dissolved in diethylene glycol (DEG) and obtains reaction system, Ran Houhuan
It is slow to add sodium hydroxide, 160 DEG C are warming up in 2.5h after stirring 3h, is cooled down after reacting 3h；Centrifuge obtained sediment successively
With volume ratio 1:2 ethanol washs with methyl acetate mixed solution, acetone, deionized water, and vacuum drying obtains base core nano oxygen
Change indium；Then the nano oxidized chlorine ultrasonic disperse of base core is added into the ethanol solution containing polyaniline in absolute ethyl alcohol, dripped
Enriching ammoniacal liquor, stirring reaction 1.5h at 95 DEG C, the sediment being centrifugally separating to obtain are washed with absolute ethyl alcohol, deionized water successively,
Crushed after roasting and obtain polyaniline-coated nano indium oxide.Fineness test is carried out to obtained slurry, is as a result 20.
Comparative example 1：
It is homogenized using there is the planetary dispersion machine of oar.Equipment cleaning will be homogenized totally and dried up, 1.2Kg is added into slurry tank
Deionized water, then add CMC dry powder 16g, open revolution carry out stirring at low speed, stirring motor frequency 10Hz, after 10 minutes
Scraper is carried out, then opens revolution and rotation stirring simultaneously.Vacuum stirring is proceeded by when not having CMC dry powder in liquid, is stirred
Mix speed and be gradually increased to revolve round the sun 35Hz, rotation 35Hz.Glue is made after 1.5 hours in stirring.
18g conductive agents are added into the slurry tank containing glue, open low speed revolution rotation, after mixing 10 minutes, increase turns
Speed extremely revolution 35, rotation 35Hz.1Kg graphite is added, opens low speed revolution rotation, mixing carries out scraper after 10 minutes, starts to take out
It is stirred under vacuum, mixing speed is gradually increased to revolve round the sun 35Hz, rotation 35Hz.Logical cooling water stirs 2 hours.Then solid content is added
For 50% SBR solution 64g, and 1Kg pure water is added, be stirred under vacuum (revolution 35Hz, rotation 35Hz) the 30 minutes time, stirred
Testing size fineness, it is as a result 26 after mixing end.
By verification experimental verification, no paddle dispersion method prepares lithium battery anode and cathode slurry, compared to there is paddle planet dispersion method, its
Process is simple, efficiency high (more than ten times), and slurry good dispersion.
Claims (10)
1. a kind of scattered method for preparing lithium battery slurry of no paddle, it is characterised in that homogenization process is that negative or positive electrode is lived
Property material, conductive agent, auxiliary agent and binding agent it is scattered in a solvent, using uniformly being mixed without paddle, slurry is made.
A kind of 2. scattered method for preparing lithium battery slurry of no paddle according to claim 1, it is characterised in that it is described just
Pole active material is cobalt acid lithium, nickle cobalt lithium manganate, LiMn2O4, LiFePO4, rich lithium manganese, orthophosphates, in nickel manganese binary material
One or more kinds of mixtures.
3. the scattered method for preparing lithium battery slurry of a kind of no paddle according to claim 1, it is characterised in that described negative
Pole active material is mixture more than one or both of graphite, soft or hard carbon, silicon-carbon compound.
4. the scattered method for preparing lithium battery slurry of a kind of no paddle according to claim 1, it is characterised in that described to lead
Electric agent is carbon black, CNT, the mixture of vapour deposition one or both of carbon fiber or graphene above.
5. the scattered method for preparing lithium battery slurry of a kind of no paddle according to claim 1, it is characterised in that described viscous
Knot agent is mixture more than one or both of sodium carboxymethylcellulose, acrylate, epoxy resin, polyurethane, PVDF.
6. the scattered method for preparing lithium battery slurry of a kind of no paddle according to claim 1, it is characterised in that described molten
Agent is one kind in water, NMP, acetone.
7. the scattered method for preparing lithium battery slurry of a kind of no paddle according to claim 1, it is characterised in that described to help
Agent is mass ratio 1:0.8:The indium oxide of 3 poly- 3,4 ethylenedioxy thiophene, titanium carbide and polyaniline-coated.
A kind of 8. scattered method for preparing lithium battery slurry of no paddle according to claim 7, it is characterised in that polyaniline
The preparation method of the indium oxide of cladding is：Indium oxide is dissolved in diethylene glycol (DEG) and obtains reaction system, is then slowly added into sodium hydroxide,
140-160 DEG C is warming up in 2-2.5h after stirring 1-3h, is cooled down after reacting 1-3h；Centrifuge obtained sediment and use volume successively
Than 1:2 ethanol washs with methyl acetate mixed solution, acetone, deionized water, and vacuum drying obtains base core nano indium oxide；So
The nano oxidized chlorine ultrasonic disperse of base core is added the ethanol solution containing polyaniline, dense ammonia is added dropwise in absolute ethyl alcohol afterwards
Water, stirring reaction 1-1.5h at 85-95 DEG C, the sediment being centrifugally separating to obtain are washed with absolute ethyl alcohol, deionized water successively, are roasted
Crushed after burning and obtain polyaniline-coated nano indium oxide.
9. a kind of scattered method for preparing lithium battery slurry of no paddle according to claim 1 or 2 or 3, it is characterised in that
The parts by weight of each component are respectively during homogenate：400-520 part negative or positive electrodes active material, 6.4-11 parts conductive agent, 10-15
Part auxiliary agent, 6.4-16.8 parts binding agent and 439-781 part solvents.
10. the scattered method for preparing lithium battery slurry of a kind of no paddle according to claim 9, it is characterised in that described
Method comprises the following steps：
(1) positive active material or negative electrode active material, conductive agent, adhesive powder and auxiliary agent are weighed, is added in homogenate tank, and
The solvent of 1/3 amount is added, it is 45-75wt% to make its solid content；
(2) homogenate tank is put into instrument, makes tank body autobiography and revolution simultaneously, rotation rotating speed is 500-1500rpm, and revolve round the sun rotating speed
For 55-60rpm, rotational time 1-5min；
(3) rotating speed is heightened to 2500-3500rpm, and revolved round the sun rotating speed 20-35rpm, and 2-5 points of frozen water cooling is put into after time 2-10min
Clock；
(4) repeat step (3) 1-3 times；Then the solvent of surplus is added, it is 30-60wt% to make its solid content, in 1500-
Continue to disperse under 2500rpm, time 1-3min, obtain lithium battery slurry.
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Cited By (1)
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| CN109742404A (en) * | 2019-02-20 | 2019-05-10 | 湖南科霸汽车动力电池有限责任公司 | Lithium battery anode slurry and preparation method thereof suitable for nickel foam substrate |
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| CN109742404A (en) * | 2019-02-20 | 2019-05-10 | 湖南科霸汽车动力电池有限责任公司 | Lithium battery anode slurry and preparation method thereof suitable for nickel foam substrate |
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Application publication date: 20180209 |