CN109728299A - A kind of preparation method and battery slurry of battery slurry - Google Patents
A kind of preparation method and battery slurry of battery slurry Download PDFInfo
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- CN109728299A CN109728299A CN201811572756.8A CN201811572756A CN109728299A CN 109728299 A CN109728299 A CN 109728299A CN 201811572756 A CN201811572756 A CN 201811572756A CN 109728299 A CN109728299 A CN 109728299A
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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
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of preparation method of battery slurry and its battery slurries.Electrode material or ceramic material powder are direct plungeed into the synthetic reaction system of adhesive, adhesive synthesis prepares a step with slurry and completes, optimize process flow, not only significantly shorten the production time, reduce production cost, and guarantee that slurry has good dispersing uniformity, improve the performances such as the adhesive strength of slurry.Gained battery slurry of the invention, appearance is thick-pasty, and slurry is uniformly dispersed, soilless sticking or depositional phenomenon；It can be swimmingly coated on the collection liquid surfaces such as copper foil, aluminium foil or organic polymer material membrane surface, even uniform after coating, peel strength is high, shows being well combined between combination and slurry and Nian Jie substrate between paste powder.Gained ceramic diaphragm slurry of the invention, heat resistance is good, coats modified wet process PE basement membrane with the slurry, percent thermal shrinkage is not higher than 3% at 150 DEG C.
Description
Technical field
The present invention relates to a kind of preparation method of battery slurry and a kind of lithium ion batteries prepared using this method
Electrode slurry and ceramic diaphragm slurry.
Background technique
Lithium ion battery is a kind of new energy battery currently to attract attention, and application field is extensive, especially in new energy
The fields such as automobile and high-end electronic product are even more indispensable.And with the Quick Extended in lithium ion battery applications field, peace
Quan Xing, validity more and more attention has been paid to.At the same time, how the production technology of lithium ion battery is optimized, is being guaranteed
Improving production efficiency under the premise of safely and effectively, faster and better to meet the needs of lithium ion battery industry scale enlargement, at
For each lithium ion battery manufacturer and its upstream materials and module manufacturer emphasis of interest.
The main building block of lithium ion battery includes shell, electrode material, electrolyte, diaphragm etc..Wherein, electrode material
It is divided into positive electrode and negative electrode material, is the core composition material of lithium ion battery.In recent years, people are to lithium ion cell positive
A large amount of research and probe has been carried out with the type, proportion and production technology of negative electrode material etc..For example, Authorization Notice No. is
The Chinese invention patent of CN105552307B discloses a kind of lithium-sulfur cell negative electrode material and preparation method thereof, negative electrode material by
Stable state lithium powder, carbon material and adhesive composition, can effectively inhibit the Li dendrite generated in use process, improve safety
Property, while reducing producting process difficulty；The Chinese invention of Publication No. CN108270011A discloses a kind of lithium ion battery
Negative electrode material and preparation method thereof deposits one layer of conductive materials on negative electrode material surface using chemical plating method, to improve cathode
The electric conductivity of material, and alleviate volume expansion problem of the material in cyclic process；The China of Publication No. CN108258230A
A kind of disclosure of the invention lithium ion battery hollow silicon-carbon cathode material, had both efficiently solved the expansion issues of material, simultaneously will
Nano-silicon homogeneously disperses, and ensure that the transmission rate of electronics and lithium ion；The Chinese invention of Publication No. CN108376762A is public
It has opened a kind of dual carbon and has introduced silicate anodal material, preparation method and application, provided a kind of new type lithium ion battery just
The application idea of pole material.
Diaphragm is also one of significant components of lithium ion battery.The material of diaphragm is usually the materials such as polyethylene, polypropylene
Single layer or laminated film, film chemical stability and solvent resistance made of this kind of material are good, can be in electrolyte environment
It keeps stablizing.However, this kind of film is there is also all kinds of defects, as tensile strength is low, poor heat resistance cause it is heated it is easily Texturized,
Low, liquid wellability difference of puncture-resistant intensity etc., therefore, it is necessary before being applied to lithium battery for carrying out enhancing modification to diaphragm
Step.
Currently, the most popular method of diagram modification be membrane surface coat one layer of ceramic material, with improve its hot property,
Mechanical performance and liquid wellability.In general, ceramic material needs uniformly mixed with lithium ion battery ceramic diaphragm adhesive specially,
After being prepared into ceramic diaphragm slurry, membrane surface can be coated in.To reach good modified effect, people are to ceramic material
The substitute of coating processes and ceramic material has carried out a series of research.For example, in Publication No. CN108269957A
State's invention patent disclose it is a kind of with high wellability, the lithium battery diaphragm of high thermal stability and preparation method thereof, it is heavy with chemistry
Area method replaces general coating method to effectively improve the dispersibility of ceramic material by ceramic material uniform deposition in membrane surface.
The Chinese invention of Publication No. CN108232087A discloses a kind of preparation method of battery separator, uses polymer powder generation
For ceramic material powder, the dispersibility of slurry is improved to a certain extent.
Currently, the electrode material and ceramic diaphragm material of lithium ion battery are in application process, the material that needs a person with the qualifications of a general is prepared into
After slurry, the coating of electrode slice or diaphragm and the production and assembly of subsequent lithium battery can be applied to.The general preparation side of slurry
Method is after mixing the powder of electrode material or ceramic material with adhesive specially, to be prepared into slurry by high-speed stirred.The party
Method is easy to operate, technical maturity, receives the extensive use of each lithium ion battery manufacturer.However, being prepared by the above method
Slurry, shadow of the dispersing uniformity by many factors such as beating equipment, beating time, powder dosage and adhesive viscosities
It rings.And under normal conditions, the dosage of powder is much larger than the dosage of adhesive, therefore it is equal in adhesive to further increase powder
The difficulty of even dispersion.To guarantee that slurry is uniformly dispersed, it need to usually improve beating equipment, extend beating time, to production cost
Control causes adverse effect.Therefore, the preparation process of slurry is optimized, improves the dispersing uniformity of slurry, with preparation
Performance more preferably pulp of lithium ion battery or ceramic diaphragm slurry, while production cost is further controlled, become
The urgent need of lithium ion battery manufacturer and popular research field.
Summary of the invention
The present invention is intended to provide a kind of preparation method of battery slurry and a kind of battery prepared using this method are used
Slurry.The powder of electrode material or ceramic material is put into the synthetic system of adhesive, it is same in the synthesis process of adhesive
Step carries out the dispersion of powder, and battery slurry is made in a step.The battery slurry prepared by this method, be uniformly dispersed degree
Well, adhesive property and electrical property are not less than the slurry of universal method preparation.The present invention prepares the synthesis of adhesive and slurry
Be combined into one, the battery slurry preparation method provided is easy to operate, easily controllable, and eliminate high speed mashing equipment and
Technique greatlys save production time and production cost.
The technical solution of the present invention is as follows:
A kind of preparation method of battery slurry, the preparation suitable for electrode slurry and ceramic diaphragm slurry, it is characterised in that: will
Electrode material or ceramic material are added directly into the synthetic reaction system of adhesive, the dispersion of electrode material or ceramic material with
The synthetic reaction of adhesive is synchronous to be carried out, and is directly prepared into electrode slurry or ceramic diaphragm slurry, electrode material or ceramic material with
Ingredient in the synthetic reaction system of adhesive is added by following mass parts:
Electrode material or ceramic material, 30-90 parts,
Adhesive reaction object, 2-12 parts,
Conductive agent, 0-2 parts,
Auxiliary agent, 0-2 parts,
Solvent, 10-70 parts.
Further, electrode material or ceramic material are in synchronous addition during feeding intake of the synthesis material of adhesive.
Further, the electrode material includes positive electrode or/and negative electrode material.
Further, the positive electrode is one or both of sulphur, LiFePO4, lithium-contained composite metal oxide
More than；Preferably lithium-contained composite metal oxide or/and LiFePO4.
Further, the lithium-contained composite metal oxide is one or more of lithium and following metallic element
The oxide of the compound system of composition: cobalt, manganese, nickel, vanadium, molybdenum, chromium, aluminium；Preferably lithium and one or both of nickel, cobalt, manganese
The composite oxides of composition described above.
Further, the negative electrode material is graphite, graphene, carbon nanotube, elemental lithium, lithium titanate, nano-silicon, silicon
One or more of carbon complex, polyacetylene, polyparaphenylene, polypyrrole；Preferably graphite or/and silicon-carbon is compound
Object.
Further, the ceramic material be one or both of metal oxide, silica, silicate with
On；Preferably metal oxide.
Further, the electrode material or ceramic material, form are the powder that partial size D50 is not more than 30 μm.
Further, the adhesive is acrylate adhesive, polyimide adhesive, polyethenol series bonding
One or more of agent；Preferably acrylate adhesive.
Further, the conductive agent is one or more of graphite, carbon nanotube, graphene, acetylene black；It is preferred that
For acetylene black.
Further, the auxiliary agent is polyoxyethylene stearic acid ester, sulfonate, sulfate, stearmide, carboxymethyl fibre
Tie up one or more of plain salt, polyacrylate, polyacrylamide, polyvinyl alcohol, organic alcohols, organic silicon；It is excellent
It is selected as polyoxyethylene stearic acid ester, dodecyl sodium sulfate, lauryl sodium sulfate, Stepanol MG, stearmide, carboxylic
Sodium carboxymethylcellulose pyce, Sodium Polyacrylate, polyacrylamide, polyvinyl alcohol, isopropanol, ethylene glycol, 1,2- propylene glycol, 1,3- the third two
Alcohol, glycerine, pentaerythrite, triethylamine, acetic anhydride, maleic anhydride, three second methoxy silane of γ-aminopropyl, γ-aminopropyl three
Ethoxysilane, γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silicon
Alkane, gamma-mercaptopropyltriethoxysilane, γ-mercaptopropyl trimethoxysilane, N- (β-aminoethyl)-γ-aminopropyl trimethoxy
One of silane, N- β-(aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, γ-aminopropyltriethoxy diethoxy silane
Or it is two or more.
Further, the solvent is water, alcohol, inorganic acid, organic acid, ester, ketone, aldehyde, ether, amine, aliphatic hydrocarbon, fragrance
One or more of hydrocarbon, halogenated hydrocarbons；Preferably water, ethyl alcohol, ethylene glycol, normal propyl alcohol, isopropanol, n-butanol, the tert-butyl alcohol,
Cyclohexanol, ethylene glycol, 1,2- propylene glycol, 1,3- propylene glycol, glycerine, pentaerythrite, phosphoric acid, acetic acid, formic acid, ethyl acetate,
Methyl acetate, Ethyl formate, n-butyl acetate, tert-butyl acetate, ethyl acetoacetate, olein, diethylene glycol list
Methyl ether acetate, propylene glycol methyl ether acetate, tributyl citrate, acetone, methyl ethyl ketone, cyclohexanone, acetaldehyde, glyoxal, penta 2
Aldehyde, salicylide, propandiol butyl ether, dioxane, hexamethylene, normal octane, benzene,toluene,xylene, ethylbenzene, methylene chloride, trichlorine
Methane, carbon tetrachloride, dichloroethanes, trichloroethanes, tetrahydrofuran, 1-Methyl-2-Pyrrolidone, N,N-dimethylformamide,
One or more of DMAC N,N' dimethyl acetamide.
A kind of battery slurry prepared according to the above method, including electrode slurry or ceramic diaphragm slurry.
The beneficial effects of the present invention are:
(1) electrode material or ceramic material powder are direct plungeed into the synthetic reaction system of adhesive by preparation method of the invention
In, adhesive synthesis prepares a step with slurry and completes, and optimizes process flow, not only significantly shortens the production time, reduces
Production cost, and guarantee that slurry has good dispersing uniformity, improve the performances such as the adhesive strength of slurry.
(2) present invention gained battery slurry, appearance are thick-pasty, and slurry is uniformly dispersed, and soilless sticking or deposition are existing
As.
(3) present invention gained battery slurry can swimmingly be coated on the collection liquid surfaces such as copper foil, aluminium foil or organic poly-
Close object material membrane surface, even uniform after coating.
(4) present invention gained battery slurry, the diaphragm coated on the collectors such as copper foil, aluminium foil or organic polymer material
Behind surface, peel strength is high, shows being well combined between combination and slurry and Nian Jie substrate between paste powder.
(5) present invention gained ceramic diaphragm slurry, heat resistance is good, coats modified wet process PE base with the slurry
Film, percent thermal shrinkage is not higher than 3% at 150 DEG C.
Detailed description of the invention
Fig. 1 is the peel strength curve according to embodiment 1-3 negative electrode slurry, ceramic slurry and the anode sizing agent prepared respectively
Figure.
Specific embodiment
It will be described in more detail below by embodiment, but protection scope of the present invention is not limited in these implementations
Example.
Embodiment 1
It is passed through high pure nitrogen into reaction vessel, purified water 200g, emulsifier neopelex 0.1g and auxiliary agent is added
Sodium carboxymethylcellulose 0.1g is put into reaction vessel, is opened stirring to sodium carboxymethylcellulose and is completely dissolved；Then it is stirring
Under the conditions of Isooctyl acrylate monomer 2.001g, acrylamide 1.557g, hydroxy-ethyl acrylate 0.223g and acrylic acid 1.779g is added,
After adjusting pH value to neutrality with alkali, initiator potassium persulfate 0.0331g is added, continues to stir；Divide more several times gradually to reaction
In container bottle plus negative electrode material silicon-carbon compound 50.0g and conductive agent acetylene black 0.5600g is put into, it is abundant to continue stirring until powder
After being scattered in reaction system, continues to stir 1h, then heat to 60 DEG C, isothermal reaction 8h.To after the reaction was completed, by reaction system
It is cooled to room temperature, stops stirring, remove high pure nitrogen, collect product, obtain acrylate-silicon-carbon cathode slurry.
Embodiment 2
Polyvinyl alcohol (abbreviation PVA) is put into the reaction vessel equipped with thermometer, mechanical stirring device and reflux condensing tube
20.0g.Purified water 200.0g is taken, is injected in reaction vessel.Temperature in reaction vessel is increased to 90 ± 5 DEG C, condensing reflux stirs
It mixes until PVA is all soluble in water.The temperature in reaction vessel is then reduced to 60 ± 5 DEG C, uses phosphoric acid regulation system
PH value is 4.5 ± 0.5.It is kept stirring, weighs 160.0g ceramic material alumina powder, several times step by step input reaction vessel
It is interior.A clean beaker is taken, throws N hydroxymethyl acrylamide 5.0g thereto, after purified water 5.0g dissolution is added, adds propylene
Sour 1.0g, stirs evenly.The solution is put into reaction vessel, 4 h are stirred.0.015 g of initiator ammonium persulfate is taken again, is used
After the dissolution of 5g purified water, put into reaction vessel.Keeping temperature in reaction vessel is 60 ± 5 DEG C, stirs 12-18h.Reaction is held
Temperature is cooled to room temperature in device, is collected product, is obtained modified polyvinylalcohol-aluminium oxide ceramics slurry.
Embodiment 3
Solvent 1-Methyl-2-Pyrrolidone (abbreviation NMP) 40.0g and auxiliary agent PVA 2.0g are weighed, 150 DEG C are warming up to after mixing,
It is condensed back to stir to PVA and be completely dissolved, PVA-NMP solution cooling is spare.2,2'- bis- (three is put into reaction vessel
Methyl fluoride) -4,4'- benzidine (abbreviation TFMB) 3.90g and PVA-NMP solution 30.0g, is stirred completely molten to TFMB
Solution.Anode material nickel cobalt manganic acid lithium powder 70.0g is weighed, is put into reaction vessel several times, then put into conductive agent acetylene black
0.790g is kept stirring.It weighs in 4,4'- biphenyl ether dianhydride (abbreviation ODPA) 3.75g investment reaction vessel, and with remaining
On PVA-NMP solution eluant container wall in remaining ODPA to reaction solution, 18h is stirred.Pentaerythritol phosphate is weighed again (referred to as
PEPA) 0.125g is put into reaction vessel, stirs 6 h.Acetic anhydride and each 1.0 g of triethylamine, investment reaction are finally weighed respectively
In container, 24 h are stirred.It is high pure nitrogen atmosphere that aforesaid operations step, which is answered in whole holding reaction vessel, and warm in reaction vessel
Degree is maintained at 4 ± 1 DEG C.Stop stirring, remove High Purity Nitrogen, collects product, obtain polyimides-nickle cobalt lithium manganate anode sizing agent.
Slurry obtained by above-described embodiment, dispersion is highly uniform, without any reunion or depositional phenomenon.It will change obtained by embodiment 2
Property polyvinyl alcohol-aluminium oxide ceramics slurry coat modified wet process PE basement membrane, the percent thermal shrinkage at 150 DEG C is not higher than 3%.
The membrane surface in the collectors such as copper foil, aluminium foil or organic polymer material is respectively coated in they, it will be seen from figure 1 that stripping
From intensity height, show being well combined between combination and slurry and Nian Jie substrate between paste powder.
Claims (10)
1. a kind of preparation method of battery slurry, which is characterized in that electrode material or ceramic material are added directly into bonding
In the synthetic reaction system of agent, the dispersion of electrode material or ceramic material and the synthetic reaction of adhesive it is synchronous carry out, directly system
At the ingredient in the synthetic reaction system of electrode slurry or ceramic diaphragm slurry, electrode material or ceramic material and adhesive by such as
Lower mass parts addition:
Electrode material or ceramic material, 30-90 parts,
Adhesive reaction object, 2-12 parts,
Conductive agent, 0-2 parts,
Auxiliary agent, 0-2 parts,
Solvent, 10-70 parts.
2. the preparation method of battery slurry according to claim 1, which is characterized in that electrode material or ceramic material exist
Synchronous in the process be added that feed intake of the synthesis material of adhesive.
3. the preparation method of battery slurry according to claim 1, which is characterized in that the electrode material includes just
Pole material or/and negative electrode material.
4. the preparation method of battery slurry according to claim 1, which is characterized in that the negative electrode material is stone
Ink, graphene, carbon nanotube, elemental lithium, lithium titanate, nano-silicon, silicon-carbon compound, polyacetylene, polyparaphenylene, in polypyrrole
One or more；The ceramic material be one or both of metal oxide, silica, silicate with
On；The positive electrode is one or more of sulphur, LiFePO4, lithium-contained composite metal oxide.
5. the preparation method of battery slurry according to claim 4, which is characterized in that the lithium-contained composite metal oxygen
Compound be one or more of lithium and following metallic element form compound system oxide: cobalt, manganese, nickel, vanadium,
Molybdenum, chromium, aluminium.
6. the preparation method of battery slurry according to claim 1, which is characterized in that the electrode material or ceramics
Material, form are the powder that partial size D50 is not more than 30 μm.
7. the preparation method of battery slurry according to claim 1, which is characterized in that the adhesive is acrylic acid
One or more of ester adhesive, polyimide adhesive, polyethenol series adhesive.
8. the preparation method of battery slurry according to claim 1, which is characterized in that the conductive agent be graphite,
One or more of carbon nanotube, graphene, acetylene black.
9. the preparation method of battery slurry according to claim 1, which is characterized in that the auxiliary agent is poly- for stearic acid
Ethylene oxide ester, sulfonate, sulfate, stearmide, carboxymethyl cellulose salt, polyacrylate, polyacrylamide, polyethylene
One or more of alcohol, organic alcohols, organic silicon；The solvent be water, alcohol, inorganic acid, organic acid, ester, ketone,
One or more of aldehyde, ether, amine, aliphatic hydrocarbon, aromatic hydrocarbon, halogenated hydrocarbons.
10. the battery slurry that preparation method described in claim 1 obtains, which is characterized in that including electrode slurry or ceramics
Diaphragm slurry.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110190235A (en) * | 2019-06-14 | 2019-08-30 | 湖南高瑞电源材料有限公司 | A kind of aqueous solution type lithium battery ceramic diaphragm adhesive specially and its preparation method and application |
| CN110911641A (en) * | 2019-11-26 | 2020-03-24 | 陕西科技大学 | Long-chain association coated graphite type three-dimensional network electrode and preparation method thereof |
| CN111540893A (en) * | 2020-05-14 | 2020-08-14 | 杭州欣驰能源科技有限公司 | Preparation method of graphene modification-based lithium battery electrode material |
| CN111564666A (en) * | 2020-05-14 | 2020-08-21 | 杭州欣驰能源科技有限公司 | Graphene battery and preparation method thereof |
| CN113488696A (en) * | 2021-06-04 | 2021-10-08 | 天津市捷威动力工业有限公司 | High-wettability electrolyte for cylindrical lithium ion battery |
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| CN110190235A (en) * | 2019-06-14 | 2019-08-30 | 湖南高瑞电源材料有限公司 | A kind of aqueous solution type lithium battery ceramic diaphragm adhesive specially and its preparation method and application |
| CN110911641A (en) * | 2019-11-26 | 2020-03-24 | 陕西科技大学 | Long-chain association coated graphite type three-dimensional network electrode and preparation method thereof |
| CN110911641B (en) * | 2019-11-26 | 2020-10-30 | 陕西科技大学 | Long-chain association coated graphite type three-dimensional network electrode and preparation method thereof |
| CN111540893A (en) * | 2020-05-14 | 2020-08-14 | 杭州欣驰能源科技有限公司 | Preparation method of graphene modification-based lithium battery electrode material |
| CN111564666A (en) * | 2020-05-14 | 2020-08-21 | 杭州欣驰能源科技有限公司 | Graphene battery and preparation method thereof |
| CN113488696A (en) * | 2021-06-04 | 2021-10-08 | 天津市捷威动力工业有限公司 | High-wettability electrolyte for cylindrical lithium ion battery |
| CN113488696B (en) * | 2021-06-04 | 2022-08-02 | 天津市捷威动力工业有限公司 | High-wettability electrolyte for cylindrical lithium ion battery |
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| CN109728299B (en) | 2022-01-28 |
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