CN112467142A - Aqueous solution type lithium iron phosphate anode adhesive, preparation method and application thereof - Google Patents
Aqueous solution type lithium iron phosphate anode adhesive, preparation method and application thereof Download PDFInfo
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- CN112467142A CN112467142A CN202011334662.4A CN202011334662A CN112467142A CN 112467142 A CN112467142 A CN 112467142A CN 202011334662 A CN202011334662 A CN 202011334662A CN 112467142 A CN112467142 A CN 112467142A
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- lithium iron
- iron phosphate
- aqueous solution
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 90
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 62
- 239000000853 adhesive Substances 0.000 title claims abstract description 58
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003999 initiator Substances 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 17
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 16
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 13
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- -1 acrylic ester Chemical class 0.000 claims abstract description 9
- FLUHOKZCSIYKQX-UHFFFAOYSA-N methyl prop-2-enoate phosphoric acid Chemical compound COC(C=C)=O.P(=O)(O)(O)O FLUHOKZCSIYKQX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 239000011230 binding agent Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 18
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 13
- 229910001416 lithium ion Inorganic materials 0.000 claims description 13
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 9
- 239000011883 electrode binding agent Substances 0.000 claims description 8
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 7
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 6
- 239000006256 anode slurry Substances 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 4
- 239000011976 maleic acid Substances 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 3
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims description 3
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims description 3
- NXBXJOWBDCQIHF-UHFFFAOYSA-N 2-[hydroxy-[2-(2-methylprop-2-enoyloxy)ethoxy]phosphoryl]oxyethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOP(O)(=O)OCCOC(=O)C(C)=C NXBXJOWBDCQIHF-UHFFFAOYSA-N 0.000 claims description 3
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 claims description 3
- VHSHLMUCYSAUQU-UHFFFAOYSA-N 2-hydroxypropyl methacrylate Chemical compound CC(O)COC(=O)C(C)=C VHSHLMUCYSAUQU-UHFFFAOYSA-N 0.000 claims description 3
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 claims description 3
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 3
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- WDHYRUBXLGOLKR-UHFFFAOYSA-N phosphoric acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OP(O)(O)=O WDHYRUBXLGOLKR-UHFFFAOYSA-N 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 abstract description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 abstract description 9
- 229920003169 water-soluble polymer Polymers 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 4
- 238000007334 copolymerization reaction Methods 0.000 abstract description 3
- 239000000178 monomer Substances 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 description 10
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- POLZHVHESHDZRD-UHFFFAOYSA-N 2-hydroxyethyl 2-methylprop-2-enoate;phosphoric acid Chemical group OP(O)(O)=O.CC(=C)C(=O)OCCO POLZHVHESHDZRD-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 229920006184 cellulose methylcellulose Polymers 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011267 electrode slurry Substances 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 150000008040 ionic compounds Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000011884 anode binding agent Substances 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000003013 cathode binding agent Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003232 water-soluble binding agent Substances 0.000 description 1
Images
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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
- H01M4/622—Binders being polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
- C08F220/281—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing only one oxygen, e.g. furfuryl (meth)acrylate or 2-methoxyethyl (meth)acrylate
-
- 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
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive 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
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
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Abstract
The application discloses an aqueous solution type lithium iron phosphate anode adhesive, a preparation method and application thereof, wherein the preparation method comprises the following steps: the aqueous solution type lithium iron phosphate anode adhesive is aqueous solution, and the solid content of the aqueous solution type lithium iron phosphate anode adhesive is 3-15%; the viscosity of the aqueous solution type lithium iron phosphate positive adhesive is 5000-100000 cp at 25 ℃, and the pH value is 6-8; the water solution type lithium iron phosphate anode adhesive comprises the following synthetic formula in percentage by mass: 10-20 parts of lower unsaturated carboxylic acid; 8-15 parts of acrylamide and derivatives thereof; 5-20 parts of water-soluble acrylate; 5-10 parts of (methyl) acrylate phosphate; 0.1-0.4 part of initiator. Compared with the prior art, the single-component aqueous solution system has better storage and use stability, simpler formula and simple and convenient preparation compared with a multi-component blending solution; in the aspect of components, monomers such as acrylic acid, acrylic ester, acrylamide and the like are adopted for copolymerization, and compared with water-soluble polymers such as polyvinyl alcohol, CMC and the like, the product has better thermal stability.
Description
Technical Field
The application relates to the technical field of lithium ion batteries, in particular to an aqueous solution type lithium iron phosphate anode adhesive, a preparation method and application thereof.
Background
Lithium iron phosphate is a commonly used lithium ion battery anode material, however, because lithium iron phosphate has relatively poor conductivity and relatively low energy density, the market share of lithium batteries prepared by using the lithium iron phosphate anode, especially the market share of power batteries, has been suppressed by lithium batteries prepared by using ternary anode materials for a long time. However, lithium iron phosphate has an advantage of higher safety compared to a ternary cathode material. In recent years, the news about the safety accidents of lithium ion batteries, especially lithium ion power batteries, is frequently reported, so that safer lithium iron phosphate materials are more and more concerned. With the continuous and deep research of lithium iron phosphate anode lithium ion batteries, people also put higher requirements on relevant materials matched with the lithium iron phosphate anode lithium ion batteries, such as lithium iron phosphate anode adhesives.
An ideal binder for a lithium iron phosphate positive electrode should have the following characteristics:
1. the adhesive force is high enough, so that the lithium iron phosphate powder can be effectively adhered to the surface of an aluminum foil (a positive current collector);
2. the adhesive has good dispersibility, and can uniformly disperse the lithium iron phosphate powder on the premise of not adding auxiliary agents such as a dispersing agent, a thickening agent and the like when being used for preparing the anode slurry;
3. electrochemical stability, no swelling in electrolyte and good tolerance to strong redox reaction environment during charging and discharging of lithium ion battery'
4. The thermal stability can be kept stable for a long time at the working temperature of the lithium ion battery, particularly the power battery;
5. and the lithium iron phosphate has poor conductivity, so that the energy density of the lithium iron phosphate positive pole piece can be improved if the adhesive has certain conductivity.
The traditional lithium iron phosphate anode binder is a PVDF-NMP solution, belongs to a solvent type, and has the defects of poor tolerance, easy swelling and the like of an electrolyte besides causing environmental problems. In addition, the binder itself is an insulating material, and performance of the lithium iron phosphate material is further inhibited. Therefore, many studies have been made to find a suitable aqueous lithium iron phosphate positive electrode binder.
Chinese patent No. CN105153974B discloses an aqueous composite binder suitable for lithium iron phosphate and a method for preparing an aqueous positive electrode slurry by using the same. The adhesive is compounded by a main adhesive, an ionic adhesive and a flexibilizer. Wherein the primary binder is a water-soluble polymer (e.g., polyvinyl alcohol); ionic binders include polymers containing-COOLi groups (e.g., lithium polyacrylate, lithium carboxymethyl cellulose), water-soluble lithium-containing silicates (e.g., lithium silicate), or water-soluble binders capable of forming complexes with free Li + (e.g., polyethylene oxide), and the like; the flexibilizer is a long-chain water-soluble polymer (such as partially hydrolyzed polyacrylamide) with adsorption flocculation effect. Compared with the traditional adhesive, the adhesive has better bonding performance, and the performance of the lithium ion battery prepared by using the adhesive is more outstanding. However, the adhesive adopts a composite blending system, the components and the preparation process are relatively complex, and the stability of the blending system in the storage and use processes is difficult to predict and control.
Chinese patent publication No. CN109585851A discloses an aqueous binder suitable for a lithium iron phosphate positive electrode and a positive electrode slurry prepared by using the binder. The adhesive is mainly acrylic polymer (such as polyacrylic acid, acrylonitrile multipolymer, acrylate multipolymer, polyacrylamide and the like) dispersion liquid, and is assisted by polyvinyl alcohol and polyethylene oxide. The binder is mainly used for solving the problems that the positive pole piece is easy to curl in the drying process and the active substance and the current collector are stripped in the rolling, battery preparation and charge-discharge cycle processes. This patent does not describe whether the binder is a solution system or an emulsion system, and like the aforementioned patents, the binder is also a blended system, which may be less stable.
One common feature of the solutions given in the above-mentioned references is the use of polyvinyl alcohol. Polyvinyl alcohol is a water-soluble polymer widely applied in the field of adhesives, however, the thermal stability of polyvinyl alcohol is poor, and at 100-150 ℃, hydroxyl groups on a molecular chain gradually condense and dehydrate, and then gradually become brittle, so that the bonding capability is poor, and the overall thermal performance of a lithium ion battery may be adversely affected.
Disclosure of Invention
In order to solve the above technical problems, the present application provides an aqueous solution type lithium iron phosphate positive electrode binder, which has the following characteristics:
1. aqueous, non-blended systems;
2. water-soluble polymers such as polyvinyl alcohol are not used;
3. good thermal stability, electrochemical stability and dispersibility.
The technical scheme provided by the application is as follows:
the application provides a anodal adhesive of aqueous solution type lithium iron phosphate, includes: the aqueous solution type lithium iron phosphate anode adhesive is aqueous solution, and the solid content of the aqueous solution type lithium iron phosphate anode adhesive is 3-15%; the viscosity of the aqueous solution type lithium iron phosphate positive adhesive is 5000-100000 cp at 25 ℃, and the pH value is 6-8;
the water solution type lithium iron phosphate anode adhesive comprises the following synthetic formula in percentage by mass:
10-20 parts of lower unsaturated carboxylic acid;
8-15 parts of acrylamide and derivatives thereof;
5-20 parts of water-soluble acrylate;
5-10 parts of (methyl) acrylate phosphate;
0.1-0.4 part of initiator.
Further, in a preferred embodiment of the present invention, the solid content of the aqueous solution type lithium iron phosphate positive electrode binder is preferably 5% to 10%.
Further, in a preferred embodiment of the present invention, the viscosity of the aqueous solution type lithium iron phosphate positive electrode binder at 25 ℃ is preferably 10000 to 50000 cp.
The application provides a preparation method of an aqueous solution type lithium iron phosphate positive adhesive, which is characterized by comprising the following steps:
s101, adding the lower unsaturated carboxylic acid, the acrylamide and the derivative thereof, the water-soluble acrylate and the initiator into a reaction vessel, adding 300-320 parts of deionized water, and fully stirring until all materials are completely dissolved; the weight of the initiator accounts for 50-75% of the total amount of the initiator in the formula;
s102, stirring is kept, the reaction temperature is increased to 55-75 ℃, and the reaction is carried out for 2-6 hours;
s103, keeping stirring and reaction temperature, adding the (methyl) acrylate phosphate and the rest of the initiator into a reaction container, adding the deionized water until the theoretical solid content of the reaction solution reaches a preset value, and continuing to react for 1.5-4 hours;
and S104, stirring is kept, heating is stopped, after the temperature in the reaction container is reduced to the normal temperature, a measured neutralizer is added into the reaction container, the mixture is stirred fully and uniformly, the pH value of a product is 6-8, and then the material is collected, so that the aqueous solution type lithium iron phosphate positive adhesive is obtained.
Further, in a preferred embodiment of the present invention, in step S102: keeping stirring, and raising the reaction temperature to 55-75 ℃, preferably 60-65 ℃; the reaction is carried out for 2-6 h, and the preferable reaction time is 3-4.5 h.
Further, in a preferred embodiment of the present invention, in the step S103: the reaction is continued for 1.5 to 4 hours, preferably 2 to 2.5 hours.
Further, in a preferred mode of the present invention, the lower unsaturated carboxylic acid includes: acrylic acid, methacrylic acid, maleic acid, itaconic acid.
Further, in a preferred mode of the present invention, the lower unsaturated carboxylic acid is acrylic acid and/or methacrylic acid.
Further, in a preferred mode of the present invention, the acrylamide and derivatives thereof include: acrylamide, methacrylamide, N-methylolacrylamide, 2-acrylamido-2-methylpropanesulfonic acid.
Further, in a preferred embodiment of the present invention, the water-soluble acrylate includes: hydroxyethyl acrylate, hydroxyethyl methacrylate, 2-hydroxypropyl acrylate, 3-hydroxypropyl acrylate, 2-hydroxypropyl methacrylate, and 3-hydroxypropyl methacrylate.
Further, in a preferred embodiment of the present invention, the water-soluble acrylate is hydroxyethyl acrylate and/or 3-hydroxypropyl acrylate.
Further, in a preferred mode of the present invention, the (meth) acrylate phosphate ester includes: 2- (phosphonooxy) ethyl 2-methyl-2-acrylate, 2-hydroxyethyl 2-methyl-2-acrylate phosphate, bis (methacryloyloxyethyl) hydrogen phosphate.
Further, in a preferred embodiment of the present invention, the (meth) acrylate phosphate is 2-methyl-2-propenoic acid-2-hydroxyethyl ester phosphate.
Further, in a preferred mode of the present invention, the initiator includes: ammonium persulfate, sodium persulfate, potassium persulfate.
The application provides an application of an aqueous solution type lithium iron phosphate anode adhesive, which comprises the steps of preparing an electrical material by using the aqueous solution type lithium iron phosphate anode adhesive; the electrical material includes: lithium iron phosphate anode slurry, a lithium iron phosphate anode plate and a lithium ion battery.
The invention provides an aqueous solution type lithium iron phosphate anode adhesive, which comprises the following components: the aqueous solution type lithium iron phosphate anode adhesive is aqueous solution, and the solid content of the aqueous solution type lithium iron phosphate anode adhesive is 3-15%; the viscosity of the aqueous solution type lithium iron phosphate positive adhesive is 5000-100000 cp at 25 ℃, and the pH value is 6-8; the water solution type lithium iron phosphate anode adhesive comprises the following synthetic formula in percentage by mass: 10-20 parts of lower unsaturated carboxylic acid; 8-15 parts of acrylamide and derivatives thereof; 5-20 parts of water-soluble acrylate; 5-10 parts of (methyl) acrylate phosphate; 0.1-0.4 part of initiator.
The invention has the beneficial effects that:
compared with a multi-component blending solution, the aqueous solution system adopting a single component has better storage and use stability, simpler formula and simple and convenient preparation. In the aspect of components, monomers such as acrylic acid, acrylic ester, acrylamide and the like are adopted for copolymerization, and compared with water-soluble polymers such as polyvinyl alcohol, CMC and the like, the product has better thermal stability;
the dispersibility is good, and when the binder is used for preparing the lithium iron phosphate anode slurry, the uniformly dispersed slurry can be obtained without adding auxiliary agents such as a dispersing agent, a thickening agent and the like;
water-soluble acrylate containing hydroxyl (such as hydroxyethyl acrylate) is added into the formula as sizing material, so that the thermal property of the product is maintained, and the product is endowed with good bonding capability;
the unsaturated carboxylic acid in the adhesive component and the neutralized carboxylate thereof are ionic compounds, have certain conductivity and can make up for the defect of insufficient conductivity of the lithium iron phosphate to a certain extent;
good electrochemical stability, the binder is difficult to swell in an electrolyte and is capable of remaining stable during continuous charge and discharge.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flow chart of the preparation of the aqueous solution type lithium iron phosphate positive binder according to the present invention;
fig. 2 is a first charge-discharge curve obtained by testing after lithium iron phosphate positive electrode sheets are prepared by using the aqueous solution type lithium iron phosphate positive adhesive of the present invention and assembled into a button cell.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It will be understood that when an element is referred to as being "fixed" or "disposed" on another element, it can be directly on the other element or be indirectly disposed on the other element; when an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It will be understood that the terms "length," "width," "upper," "lower," "front," "rear," "first," "second," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like, as used herein, refer to an orientation or positional relationship indicated in the drawings that is solely for the purpose of facilitating the description and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the application.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "plurality" or "a plurality" means two or more unless specifically limited otherwise.
It should be understood that the structures, ratios, sizes, and the like shown in the drawings are only used for matching the disclosure of the specification, so as to be understood and read by those skilled in the art, and are not used to limit the practical limit conditions of the present application, so that the modifications of the structures, the changes of the ratio relationships, or the adjustment of the sizes, do not have the technical essence, and the modifications, the changes of the ratio relationships, or the adjustment of the sizes, are all within the scope of the technical contents disclosed in the present application without affecting the efficacy and the achievable purpose of the present application.
As shown in fig. 1 to 2, an embodiment of the present application provides an aqueous solution type lithium iron phosphate positive electrode binder, including: the aqueous solution type lithium iron phosphate anode adhesive is aqueous solution, and the solid content of the aqueous solution type lithium iron phosphate anode adhesive is 3-15%; the viscosity of the aqueous solution type lithium iron phosphate positive adhesive is 5000-100000 cp at 25 ℃, and the pH value is 6-8; the water solution type lithium iron phosphate anode adhesive comprises the following synthetic formula in percentage by mass: 10-20 parts of lower unsaturated carboxylic acid; 8-15 parts of acrylamide and derivatives thereof; 5-20 parts of water-soluble acrylate; 5-10 parts of (methyl) acrylate phosphate; 0.1-0.4 part of initiator.
Specifically, in the embodiment of the present invention, the solid content of the aqueous solution type lithium iron phosphate positive electrode binder is preferably 5% to 10%.
Specifically, in the embodiment of the invention, the viscosity of the aqueous solution type lithium iron phosphate positive electrode binder at 25 ℃ is preferably 10000-50000 cp.
The application provides a preparation method of an aqueous solution type lithium iron phosphate anode adhesive, which comprises the following steps:
s101, adding the lower unsaturated carboxylic acid, the acrylamide and the derivative thereof, the water-soluble acrylate and the initiator into a reaction vessel, adding 300-320 parts of deionized water, and fully stirring until all materials are completely dissolved; the weight of the initiator accounts for 50-75% of the total amount of the initiator in the formula;
s102, stirring is kept, the reaction temperature is increased to 55-75 ℃, and the reaction is carried out for 2-6 hours;
s103, keeping stirring and reaction temperature, adding the (methyl) acrylate phosphate and the rest of the initiator into a reaction container, adding the deionized water until the theoretical solid content of the reaction solution reaches a preset value, and continuing to react for 1.5-4 hours;
and S104, stirring is kept, heating is stopped, after the temperature in the reaction container is reduced to the normal temperature, a measured neutralizer is added into the reaction container, the mixture is stirred fully and uniformly, the pH value of a product is 6-8, and then the material is collected, so that the aqueous solution type lithium iron phosphate positive adhesive is obtained.
Specifically, in the embodiment of the present invention, in the S102 step: keeping stirring, and raising the reaction temperature to 55-75 ℃, preferably 60-65 ℃; the reaction is carried out for 2-6 h, and the preferable reaction time is 3-4.5 h.
Specifically, in the embodiment of the present invention, in the step S103: the reaction is continued for 1.5 to 4 hours, preferably 2 to 2.5 hours.
Specifically, in an embodiment of the present invention, the lower unsaturated carboxylic acid includes: acrylic acid, methacrylic acid, maleic acid, itaconic acid.
Specifically, in the embodiment of the present invention, the lower unsaturated carboxylic acid is acrylic acid and/or methacrylic acid.
Specifically, in embodiments of the present invention, the acrylamide and derivatives thereof include: acrylamide, methacrylamide, N-methylolacrylamide, 2-acrylamido-2-methylpropanesulfonic acid.
Specifically, in embodiments of the present invention, the water-soluble acrylate comprises: hydroxyethyl acrylate, hydroxyethyl methacrylate, 2-hydroxypropyl acrylate, 3-hydroxypropyl acrylate, 2-hydroxypropyl methacrylate, and 3-hydroxypropyl methacrylate.
Specifically, in the embodiment of the invention, the water-soluble acrylate is hydroxyethyl acrylate and/or 3-hydroxypropyl acrylate.
Specifically, in embodiments of the present invention, the (meth) acrylate phosphate ester comprises: 2- (phosphonooxy) ethyl 2-methyl-2-acrylate, 2-hydroxyethyl 2-methyl-2-acrylate phosphate, bis (methacryloyloxyethyl) hydrogen phosphate.
Specifically, in the examples of the present invention, the (meth) acrylate phosphate is 2-methyl-2-propenoic acid-2-hydroxyethyl ester phosphate.
Specifically, in an embodiment of the present invention, the initiator includes: ammonium persulfate, sodium persulfate, potassium persulfate.
Preparation example 1:
4g of 2-acrylamide-2-methylpropanesulfonic acid, 15g of acrylic acid, 6g of acrylamide, 12g of hydroxyethyl acrylate, 0.15g of ammonium persulfate and 300g of deionized water are put into a 500mL three-necked bottle provided with a reflux condenser tube and an electric stirring device, and the materials are fully stirred until the materials are completely dissolved. Stirring is kept, the temperature is raised to 60 ℃, and then the reaction is carried out for 4 hours under the condition of heat preservation. 6g of 2-methyl-2-acrylic acid-2-hydroxyethyl phosphate, 0.07g of ammonium persulfate and 54g of deionized water are added, and after the reaction is continued for 2 hours, the heating is stopped. And (3) after the temperature in the three-necked bottle is reduced to the normal temperature, adding metered lithium hydroxide, controlling the pH value of the product to be 6-8, and collecting the product.
The product was a light yellow clear viscous aqueous solution with a viscosity of about 20000cp (25 ℃). A small amount of the binder was dried in an oven to obtain a sheet having a length of about 10mm, a width of about 3mm and a thickness of about 3 mm. The volume of the sheet increased by less than 5% after immersion in the electrolyte and incubation at 60 ℃ for 72 h.
Preparation example 2:
as compared with preparation example 1, 15g of acrylic acid was replaced with 12g of acrylic acid and 3g of maleic acid, 6g of acrylamide was replaced with 5g of acrylamide and 1g of N-methylolacrylamide, and hydroxyethyl acrylate was replaced with 3-hydroxypropyl acrylate, and the rest was the same as in example 1.
The product was a pale yellow clear viscous aqueous solution with a viscosity of about 30000cp (25 ℃). A small amount of the binder was dried in an oven to obtain a sheet having a length of about 10mm, a width of about 3mm and a thickness of about 3 mm. The volume of the sheet increased by less than 5% after immersion in the electrolyte and incubation at 60 ℃ for 72 h.
The application provides an application of an aqueous solution type lithium iron phosphate anode adhesive, which comprises the steps of preparing an electrical material by using the aqueous solution type lithium iron phosphate anode adhesive; the electrical material includes: lithium iron phosphate anode slurry, a lithium iron phosphate anode plate and a lithium ion battery.
Application example 3:
preparing the lithium iron phosphate anode slurry by using the aqueous solution type lithium iron phosphate anode adhesive prepared in the preparation example 1, wherein the slurry formula comprises the following components:
binder (dry weight basis), 7.2 g;
conductive agent (acetylene black), 0.9 g;
172g of lithium iron phosphate;
deionized water, and metering, wherein the solid content of the slurry is controlled to be 55-60%.
The preparation method of the slurry comprises the following steps:
deionized water and a binder were added to a beating apparatus (sand mill) and stirred for 20min at a rotation speed of 500 rpm. Then adding the conductive agent, stirring for 30min at the rotating speed of 500 rpm. Then, the lithium iron phosphate was added in several portions, and the rotation speed was increased to 2500 rpm. And after all the lithium iron phosphate is added, keeping the rotating speed and stirring for 6 hours. Stopping stirring, pouring out the slurry and filtering by using a 200-mesh screen to obtain the finished slurry.
The slurry is uniform gray black dispersion liquid in appearance, no powder agglomeration exists, no obvious settlement exists after the slurry is kept still for 12 hours, and the viscosity of the slurry is about 3400 cp.
And (3) blade-coating the slurry on the surface of an aluminum foil, and drying to obtain the lithium iron phosphate positive pole piece, wherein the thickness of the dried coating is 100-120 mu m. The button cell is assembled by using the pole piece (the negative electrode is simple substance lithium, and the diaphragm is a polyolefin wet diaphragm). The button cell has good charge-discharge efficiency and cycle performance, under the condition of 0.1C, the charge-discharge efficiency reaches more than 95%, the first charge specific capacity and the first discharge specific capacity are not lower than 145mAh/g, and after 100 cycles, the discharge capacity is kept at about 140 mAh/g.
In view of the above, the aqueous solution type lithium iron phosphate positive adhesive, the preparation method and the application thereof provided by the embodiment of the invention adopt a single-component aqueous solution system, have better storage and use stability compared with a multi-component blending solution, and have simpler formula and simple and convenient preparation. In the aspect of components, monomers such as acrylic acid, acrylic ester, acrylamide and the like are adopted for copolymerization, and compared with water-soluble polymers such as polyvinyl alcohol, CMC and the like, the product has better thermal stability; unsaturated carboxylic acid in the aqueous solution type lithium iron phosphate positive adhesive component and neutralized carboxylate thereof are ionic compounds, have certain conductivity, and can make up for the defect of insufficient conductivity of the lithium iron phosphate to a certain extent; the aqueous solution type lithium iron phosphate cathode binder is difficult to swell in an electrolyte and can keep stable in the continuous charging and discharging process.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The aqueous solution type lithium iron phosphate anode adhesive is characterized by being an aqueous solution, wherein the solid content of the aqueous solution type lithium iron phosphate anode adhesive is 3-15%;
the viscosity of the aqueous solution type lithium iron phosphate positive adhesive is 5000-100000 cp at 25 ℃, and the pH value is 6-8;
the water solution type lithium iron phosphate anode adhesive comprises the following synthetic formula in percentage by mass:
10-20 parts of lower unsaturated carboxylic acid;
8-15 parts of acrylamide and derivatives thereof;
5-20 parts of water-soluble acrylate;
5-10 parts of (methyl) acrylate phosphate;
0.1-0.4 part of initiator.
2. The preparation method of the aqueous solution type lithium iron phosphate positive adhesive according to claim 1, comprising the following steps:
s101, adding the lower unsaturated carboxylic acid, the acrylamide and the derivative thereof, the water-soluble acrylate and the initiator into a reaction vessel, adding 300-320 parts of deionized water, and fully stirring until all materials are completely dissolved; the weight of the initiator accounts for 50-75% of the total amount of the initiator in the formula;
s102, stirring is kept, the reaction temperature is increased to 55-75 ℃, and the reaction is carried out for 2-6 hours;
s103, keeping stirring and reaction temperature, adding the (methyl) acrylate phosphate and the rest of the initiator into a reaction container, adding the deionized water until the theoretical solid content of the reaction solution reaches a preset value, and continuing to react for 1.5-4 hours;
and S104, stirring is kept, heating is stopped, after the temperature in the reaction container is reduced to the normal temperature, a measured neutralizer is added into the reaction container, the mixture is stirred fully and uniformly, the pH value of a product is 6-8, and then the material is collected, so that the aqueous solution type lithium iron phosphate positive adhesive is obtained.
3. The aqueous solution type lithium iron phosphate positive binder according to claim 1, wherein the lower unsaturated carboxylic acid comprises: acrylic acid, methacrylic acid, maleic acid, itaconic acid.
4. The aqueous solution type lithium iron phosphate positive electrode binder according to claim 3, wherein the lower unsaturated carboxylic acid is acrylic acid and/or methacrylic acid.
5. The aqueous solution type lithium iron phosphate positive adhesive according to claim 1, wherein the acrylamide and the derivative thereof comprise: acrylamide, methacrylamide, N-methylolacrylamide, 2-acrylamido-2-methylpropanesulfonic acid.
6. The aqueous solution type lithium iron phosphate positive adhesive according to any one of claims 1, wherein the water-soluble acrylate comprises: hydroxyethyl acrylate, hydroxyethyl methacrylate, 2-hydroxypropyl acrylate, 3-hydroxypropyl acrylate, 2-hydroxypropyl methacrylate, and 3-hydroxypropyl methacrylate.
7. The aqueous solution type lithium iron phosphate positive adhesive according to claim 6, wherein the water-soluble acrylate is hydroxyethyl acrylate and/or 3-hydroxypropyl acrylate.
8. The aqueous solution type lithium iron phosphate positive binder according to claim 1, wherein the (meth) acrylate phosphate comprises: 2- (phosphonooxy) ethyl 2-methyl-2-acrylate, 2-hydroxyethyl 2-methyl-2-acrylate phosphate, bis (methacryloyloxyethyl) hydrogen phosphate.
9. The aqueous solution type lithium iron phosphate positive adhesive according to claim 1, wherein the initiator comprises: ammonium persulfate, sodium persulfate, potassium persulfate.
10. The use of the aqueous solution type lithium iron phosphate positive binder according to any one of claims 1 to 9, wherein the aqueous solution type lithium iron phosphate positive binder is used to prepare an electrical material, and the electrical material comprises: lithium iron phosphate anode slurry, a lithium iron phosphate anode plate and a lithium ion battery.
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Application publication date: 20210309 |