CN118360015A - Preparation method of self-repairing dispersion functional positive electrode binding material, positive electrode slurry and preparation method thereof, and preparation method of positive electrode plate - Google Patents
Preparation method of self-repairing dispersion functional positive electrode binding material, positive electrode slurry and preparation method thereof, and preparation method of positive electrode plate Download PDFInfo
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- CN118360015A CN118360015A CN202410803395.2A CN202410803395A CN118360015A CN 118360015 A CN118360015 A CN 118360015A CN 202410803395 A CN202410803395 A CN 202410803395A CN 118360015 A CN118360015 A CN 118360015A
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- 239000000463 material Substances 0.000 title claims abstract description 78
- 239000011267 electrode slurry Substances 0.000 title claims abstract description 54
- 239000006185 dispersion Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 239000002033 PVDF binder Substances 0.000 claims abstract description 35
- 239000000178 monomer Substances 0.000 claims abstract description 34
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000003999 initiator Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000001694 spray drying Methods 0.000 claims abstract description 7
- 239000012467 final product Substances 0.000 claims abstract description 4
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 22
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- 239000011343 solid material Substances 0.000 claims description 14
- 229920000858 Cyclodextrin Polymers 0.000 claims description 13
- 239000001116 FEMA 4028 Substances 0.000 claims description 13
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 13
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 13
- 229960004853 betadex Drugs 0.000 claims description 13
- 239000006258 conductive agent Substances 0.000 claims description 13
- 239000011888 foil Substances 0.000 claims description 12
- 229940074391 gallic acid Drugs 0.000 claims description 11
- 235000004515 gallic acid Nutrition 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 7
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- -1 tert-butylisononanoate peroxide Chemical class 0.000 claims description 4
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 3
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 claims description 3
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 claims description 3
- WVSFUMAHZBOQGJ-UHFFFAOYSA-N phosphono 2-methylprop-2-eneperoxoate Chemical compound CC(=C)C(=O)OOP(O)(O)=O WVSFUMAHZBOQGJ-UHFFFAOYSA-N 0.000 claims description 3
- FSDNTQSJGHSJBG-UHFFFAOYSA-N piperidine-4-carbonitrile Chemical compound N#CC1CCNCC1 FSDNTQSJGHSJBG-UHFFFAOYSA-N 0.000 claims description 3
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 3
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 2
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 2
- RIOOIQBUNJDFON-UHFFFAOYSA-N methyl 2-methylprop-2-enoate oxolane Chemical compound O1CCCC1.COC(C(=C)C)=O RIOOIQBUNJDFON-UHFFFAOYSA-N 0.000 claims description 2
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 claims description 2
- 238000005336 cracking Methods 0.000 abstract description 16
- 230000008569 process Effects 0.000 abstract description 5
- 238000010924 continuous production Methods 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 16
- 239000002002 slurry Substances 0.000 description 14
- 239000003292 glue Substances 0.000 description 8
- 238000004132 cross linking Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- JJZFJUJKZUIFKN-UHFFFAOYSA-N 1,2-ditert-butyl-3-propan-2-ylbenzene Chemical group CC(C)C1=CC=CC(C(C)(C)C)=C1C(C)(C)C JJZFJUJKZUIFKN-UHFFFAOYSA-N 0.000 description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000007774 positive electrode material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000002313 adhesive film Substances 0.000 description 3
- 229920002313 fluoropolymer Polymers 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 2
- 239000006256 anode slurry Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000009920 chelation Effects 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000007922 dissolution test Methods 0.000 description 2
- 239000004811 fluoropolymer Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
- 101000588031 Heliothis armigera entomopoxvirus Spindolin Proteins 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- VTJUKNSKBAOEHE-UHFFFAOYSA-N calixarene Chemical compound COC(=O)COC1=C(CC=2C(=C(CC=3C(=C(C4)C=C(C=3)C(C)(C)C)OCC(=O)OC)C=C(C=2)C(C)(C)C)OCC(=O)OC)C=C(C(C)(C)C)C=C1CC1=C(OCC(=O)OC)C4=CC(C(C)(C)C)=C1 VTJUKNSKBAOEHE-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 239000011883 electrode binding agent Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium ion batteries, and discloses a preparation method of a self-repairing dispersion functional positive electrode binding material, which comprises the following steps: (1) Uniformly mixing PVDF powder with a proper amount of initiator, grafting monomer and self-repairing functional monomer through a pulverizer; (2) Extruding PVDF modified products from the uniformly mixed samples under the high-temperature and high-pressure reaction condition of a double-screw extruder with the length-diameter ratio L/D of 40; (3) The final product is obtained by spray drying the obtained PVDF modified product, and the positive electrode slurry and the preparation method thereof and the preparation method of the positive electrode plate are also disclosed. The preparation method of the positive electrode bonding material has the advantages of simple process, low cost, short time, high efficiency, no pollution and continuous production, reduces the crystallinity of the original bonding material through mechanical deformation, greatly improves the solubility of the bonding material, improves the flexibility of the obtained pole piece, increases the stripping force of the pole piece through grafting the effective monomer, and reduces the influence of pole piece cracking.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of a self-repairing dispersion functional positive electrode binding material, positive electrode slurry, a preparation method of the positive electrode slurry and a preparation method of a positive electrode plate.
Background
Polyvinylidene fluoride (PVDF) -based fluoropolymers have been widely used in the preparation of electrode materials for the last decades because of their remarkable thermal stability, chemical inertness, low surface energy, unique electrical properties, etc. However, the weak van der Waals force is used for providing a bonding network, so that the electrode particles are declustered, the pole pieces are easy to crack, the capacity is easy to attenuate, and the defect is more remarkable particularly in a battery with high energy density. Therefore, the PVDF can be subjected to grafting modification to improve the surface hydrophilicity of the PVDF and develop a novel fluorinated polymer with adjustable structure and performance, so that the material diversity requirements of different applications are met.
Patent CN102153704a discloses a modification of PVDF by co-radiation grafting of an N-vinyl pyrrolidone (NVP) monomer with PVDF powder; patent US 5576106 discloses a method of grafting unsaturated functional monomers onto the surface of powdered fluoropolymers by radiation grafting.
Although the grafting method mentioned above can obtain a high grafting ratio, a large amount of solvent is used in the grafting process, and the subsequent treatment is troublesome.
Patent CN102603986a discloses a surface solid phase grafting modified PVDF and its preparation method. However, the process needs strong alkali pretreatment and nitrogen protection, and the preparation efficiency is low.
Therefore, a new PVDF modification method with high efficiency, long-term use, difficult pollution and high grafting rate is necessary to be developed to solve the problems of electrode particle deagglomeration and pole piece cracking caused by insufficient adhesion of the anode material in the existing lithium battery.
Disclosure of Invention
The invention aims to provide a preparation method of a self-repairing dispersion functional positive electrode binding material, positive electrode slurry, a preparation method of the positive electrode slurry and a preparation method of a positive electrode plate.
The technical scheme of the invention is as follows:
A preparation method of a self-repairing dispersion functional positive electrode binding material comprises the following steps:
(1) Uniformly mixing PVDF powder with a proper amount of initiator, grafting monomer and self-repairing functional monomer through a pulverizer;
(2) Extruding PVDF modified products from the uniformly mixed samples under the high-temperature and high-pressure reaction condition of a double-screw extruder with the length-diameter ratio L/D of 40;
(3) And spray drying the PVDF modified product to obtain a final product.
Further, in the step (1), the mass parts of each reaction component are: PVDF 100 parts; 10-20 parts of grafting monomer; 0.5 parts of an initiator; 5 parts of self-repairing functional monomer.
Further, the PVDF is preferably a PVDF binder, such as, for example, furanolin (2032).
Further, in the step (1), the grafting monomer is any one or a combination of at least two of phosphoric acid methacrylate (PM-2), glycidyl Methacrylate (GMA), isopropyl methacrylate (IBOA), tetrahydrofuran methyl methacrylate (THFFA), vinyl Acetate (VA), N-vinyl pyrrolidone (NVP), 1, 6-hexanediol diacrylate (HDDA), neopentyl glycol diacrylate (NPGDA), dipropylene glycol diacrylate (DPGDA), tripropylene glycol diacrylate (TPGDA) and trimethylolpropane triacrylate (TMPTA).
Further, the grafting monomer is preferably phosphoric methacrylate (PM-2).
Further, in the step (1), the self-repairing functional monomer is any one or a combination of at least two of beta-cyclodextrin, calixarene, column arene and gallic acid.
Further, the self-repairing functional monomer is preferably beta-cyclodextrin and gallic acid.
Further, in the step (1), the initiator is any one of di-t-butyl peroxide (DTBP), di-t-butylcumene peroxide (BIBP), benzoyl Peroxide (BPO), tert-butyl peroxybenzoate (TBPB), lauroyl Peroxide (LPO), dicumyl peroxide (DCP), and t-butylisononanoate peroxide (TBPIN).
Further, the initiator is preferably di-t-butylcumene peroxide (BIBP).
Further, in the step (2), the twin-screw extruder is provided with six sections, wherein the temperatures of the first section to the sixth section are in order: 30 ℃, 80 ℃, 160 ℃, 150 ℃.
Further, in the step (2), the feed inlet of the twin-screw extruder is in the first section, the feed speed is 30rpm, the screw speed is 40rpm, and the average residence time of the materials in the twin-screw extruder is 1.5-3min.
The other technical scheme of the invention is as follows:
A positive electrode slurry comprising a solid material and an organic solvent; wherein the solid materials comprise the following components in parts by weight: 2 parts of self-repairing dispersion functional positive electrode binding material prepared by the method; 1 part of a conductive agent; 97 parts of lithium iron phosphate.
Further, the weight portion of the organic solvent accounts for 40% of the total weight of the positive electrode slurry.
Further, the organic solvent is one or a combination of at least two of N-methyl pyrrolidone, ethyl acetate, methyl propionate, dimethyl carbonate, diethyl carbonate and ethyl methyl carbonate.
Further, the organic solvent is preferably N-methylpyrrolidone.
Further, the conductive agent is one or a combination of at least two of KS-6, KS-15, SFG-6, SFG-15, acetylene black, super P, super S, 350G, carbon fiber, carbon nanotube and active carbon.
Further, the conductive agent is preferably Super P.
The third technical scheme of the invention is as follows:
a method of preparing a positive electrode slurry as hereinbefore described, the method comprising:
(1) Adding and mixing the self-repairing dispersion functional positive electrode binding material, the conductive agent and the organic solvent;
(2) And adding the lithium iron phosphate, stirring and dispersing to obtain the positive electrode slurry.
Further, a high-speed deaerator is preferable for stirring uniformly.
The fourth technical scheme of the invention is as follows:
a preparation method of a positive electrode plate comprises the following steps:
(1) Uniformly coating the uniformly dispersed positive electrode slurry on a substrate by taking aluminum foil as a positive electrode substrate;
(2) And (3) placing the substrate coated with the positive electrode slurry in an oven, and drying at 105 ℃ to obtain the positive electrode plate.
Further, the wet thickness of the positive electrode slurry after coating was 200, 300 μm.
The invention provides a preparation method of a self-repairing dispersion functional positive electrode binding material, positive electrode slurry, a preparation method of the positive electrode slurry and a preparation method of a positive electrode plate, and has the beneficial effects that:
(1) The positive electrode binding material has the advantages of simple preparation process, low cost, short time, high efficiency, no pollution and continuous production, and has industrial production conditions;
(2) According to the preparation method of the self-repairing dispersion functional positive electrode binding material, the crystallinity of the original binding material is reduced through mechanical deformation, the solubility of the binding material is greatly improved, the flexibility of the obtained pole piece is also improved, and meanwhile, the stripping force of the pole piece is increased and the influence of pole piece cracking is reduced through the arrangement of the grafting monomer;
(3) The positive electrode slurry prepared by the invention has good charge repulsive force due to the grafting of the phosphate group, and has a certain steric hindrance effect due to the PVDF long chain, so that the viscosity and the stability of the slurry are greatly improved;
(4) The anode slurry prepared by the invention realizes dynamic crosslinking due to a reversible crosslinking system of host-guest interaction of beta-cyclodextrin and gallic acid, and can recover broken bonds between polymer chains in a continuous cycle period, thereby introducing a self-repairing effect; meanwhile, the beta-cyclodextrin has a unique space network structure, so that the stability of the slurry is further maintained.
(5) The positive electrode plate prepared by the invention has the advantages that the beta-cyclodextrin hyperbranched network structure and the positive electrode material are contacted more firmly through multidimensional hydrogen bond interaction, and meanwhile, the binding force between the positive electrode material and the base material is increased through the chelation of the carboxyl of gallic acid and the aluminum material; the binding force is tighter in the whole dynamic crosslinking process, so that the structure of the electrode film can be stabilized, and the cycle performance is enhanced.
Drawings
FIG. 1 is an enlarged view showing the degree of cracking when the wet-thickness 300um dry pole pieces of examples 1-3 and comparative example 1 were taken out and after the glove box was left for 48 hours.
Detailed Description
The invention designs a preparation method of a self-repairing dispersion functional positive electrode binding material, which comprises the following steps:
(1) Uniformly mixing PVDF powder with a proper amount of initiator, grafting monomer and self-repairing functional monomer through a pulverizer;
(2) Extruding PVDF modified products from the uniformly mixed samples under the high-temperature and high-pressure reaction condition of a double-screw extruder with the length-diameter ratio L/D of 40;
(3) And spray drying the PVDF modified product to obtain a final product.
In the step (1), the mass portions of the reaction components are as follows: PVDF 100 parts; 10-20 parts of grafting monomer; 0.5 parts of an initiator; 5 parts of self-repairing functional monomer, wherein PVDF is a PVDF binder Funolin (2032), a grafting monomer is phosphoric acid methacrylate (PM-2), an initiator is di-tert-butylcumene peroxide (BIBP), and the self-repairing functional monomer is beta-cyclodextrin and gallic acid.
The invention also designs positive electrode slurry which comprises solid materials and organic solvents; wherein the solid materials comprise the following components in parts by weight: 2 parts of self-repairing dispersion functional positive electrode binding material prepared by the method; 1 part of a conductive agent; 97 parts of lithium iron phosphate, wherein the organic solvent is N-methyl pyrrolidone and the conductive agent is Super P.
The preparation method of the positive electrode slurry comprises the following steps:
(1) Adding and mixing the self-repairing dispersion functional positive electrode binding material, the conductive agent and the organic solvent;
(2) And adding the lithium iron phosphate, stirring and dispersing to obtain the positive electrode slurry.
The invention also designs a preparation method of the positive pole piece, which comprises the following steps:
(1) Uniformly coating the uniformly dispersed positive electrode slurry on a substrate by taking aluminum foil as a positive electrode substrate;
(2) And (3) placing the substrate coated with the positive electrode slurry in an oven, and drying at 105 ℃ to obtain the positive electrode plate.
In order to make the above objects, features and advantages of the present invention more comprehensible, the following embodiments accompanied with examples are further described. The invention is not limited to the embodiments listed but includes any other known modification within the scope of the claims that follow.
Reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
In example 1, the preparation method of the self-repairing dispersion functional positive electrode binding material and the positive electrode slurry is as follows:
(1) 100 parts of PVDF powder, 10 parts of phosphoric methacrylate (PM-2), 0.5 part of di-tert-butylcumene peroxide (BIBP), 2 parts of beta-cyclodextrin and 3 parts of gallic acid are weighed and uniformly mixed.
(2) Preheating a double-screw extruder, adding the uniformly mixed powder into a feed inlet for extrusion reaction, and performing spray drying treatment on the obtained modified PVDF to obtain the self-repairing dispersed functional positive electrode binding material P1.
(3) 7G of positive electrode binding material P1 is weighed in 93g of N-methyl pyrrolidone, magnetically stirred in a water bath kettle at 60 ℃ and the time required for looking at the complete solvent is counted at the rotating speed of 300 rpm.
Specifically, 7% of the self-repairing dispersion functional positive electrode binding material P1 solution is dried in an air-blast drying oven at 80 ℃ for 2 hours, then the temperature is increased by 90 ℃ for two hours to prepare a glue film, and the glue film is cut into strips with the width of 15mm and the length of 80mm and placed in a horizontal peeling strength machine for a stretching experiment.
(4) The solid material proportion of the lithium iron phosphate positive electrode slurry is as follows: 2wt% of self-repairing dispersed functional positive electrode binding material P1,1wt% of conductive agent Super P and 97wt% of lithium iron phosphate. The positive electrode slurry consists of a solid material and N-methyl pyrrolidone, wherein the weight of the N-methyl pyrrolidone accounts for 40% of the total weight of the positive electrode slurry.
In the embodiment, specifically, the self-repairing dispersion function positive electrode binding material P1, super P and N-methyl pyrrolidone are mixed together, stirred for 20 seconds in a deaerator at a rotation speed of 800rpm/min, and then added with lithium iron phosphate, and stirred for 20 minutes in the deaerator at a rotation speed of 2000rpm/min, so as to obtain positive electrode slurry.
In this example, specifically, the positive electrode slurry was uniformly coated on the surface of the aluminum foil at thicknesses of 200um and 300um, respectively.
In this embodiment, specifically, the uniformly dispersed slurry is uniformly coated on the substrate with a thickness of 200um &300um by using aluminum foil as the substrate of the positive electrode sheet.
In the embodiment, specifically, the manufactured positive electrode sheet is placed in an oven and dried at 105 ℃ for 30min &1h.
In this embodiment, specifically, the rolled pole piece dried by 200 μm wet thickness is tested for peel strength and folding endurance.
Further, the pole piece dried by the wet thickness of 300um is placed under an electronic magnifying glass to observe the cracking degree in the same ratio, and placed in a glove box for 48 hours to observe the cracking state.
Example 2, the preparation method of the self-repairing dispersion functional positive electrode binding material and the positive electrode slurry is as follows:
(1) 100 parts of PVDF powder, 15 parts of phosphoric methacrylate (PM-2), 0.5 part of di-tert-butylcumene peroxide (BIBP), 2 parts of beta-cyclodextrin and 3 parts of gallic acid are weighed and uniformly mixed.
(2) Preheating a double-screw extruder, adding the uniformly mixed powder into a feed inlet for extrusion reaction, and performing spray drying treatment on the obtained modified PVDF to obtain the self-repairing dispersed functional positive electrode binding material P2.
(3) 7G of self-repairing dispersion functional positive electrode binding material P2 is weighed, and is magnetically stirred in a water bath kettle at 60 ℃ for the time required for looking at the complete solvent at the rotating speed of 300rpm in 93g of N-methyl pyrrolidone.
Specifically, 7% of the self-repairing dispersion functional positive electrode binding material P2 solution is dried for 2 hours in an 80 ℃ air blast drying box, then is dried for two hours at 90 ℃ to prepare a glue film, and the glue film is cut into strips with the width of 15mm and the length of 80mm and is placed in a horizontal peeling strength machine for a stretching experiment.
(4) The solid material proportion of the lithium iron phosphate positive electrode slurry is as follows: 2wt% of self-repairing dispersed functional positive electrode binding material P2,1wt% of conductive agent Super P and 97wt% of lithium iron phosphate. The positive electrode slurry consists of a solid material and N-methyl pyrrolidone, wherein the weight of the N-methyl pyrrolidone accounts for 40% of the total weight of the positive electrode slurry.
In the embodiment, specifically, the self-repairing dispersion function positive electrode binding material P2, super P and N-methyl pyrrolidone are mixed together, stirred for 20 seconds in a deaerator at a rotation speed of 800rpm/min, and then added with lithium iron phosphate, and stirred for 20 minutes in the deaerator at a rotation speed of 2000rpm/min, so as to obtain positive electrode slurry.
In this example, specifically, the positive electrode slurry was uniformly coated on the surface of the aluminum foil at thicknesses of 200um and 300um, respectively.
In this embodiment, specifically, the uniformly dispersed slurry is uniformly coated on the substrate with a thickness of 200um &300um by using aluminum foil as the substrate of the positive electrode sheet.
In the embodiment, specifically, the manufactured positive electrode sheet is placed in an oven and dried at 105 ℃ for 30min &1h.
In this embodiment, specifically, the rolled pole piece dried by 200 μm wet thickness is tested for peel strength and folding endurance.
In this embodiment, specifically, the pole piece dried to a wet thickness of 300um is placed under an electronic magnifier to observe the cracking degree in the same ratio, and placed in a glove box for 48 hours to observe the cracking state.
Example 3, the preparation method of the self-repairing dispersion functional positive electrode binding material and the positive electrode slurry is as follows:
(1) 100 parts of PVDF powder, 20 parts of phosphoric methacrylate (PM-2), 0.5 part of di-tert-butylcumene peroxide (BIBP), 2 parts of beta-cyclodextrin and 3 parts of gallic acid are weighed and uniformly mixed.
(2) Preheating a double-screw extruder, adding the uniformly mixed powder into a feed inlet for extrusion reaction, and performing spray drying treatment on the obtained modified PVDF to obtain the self-repairing dispersed functional positive electrode binding material P3.
(3) 7G of self-repairing dispersion functional positive electrode binding material P3 is weighed, and is magnetically stirred in a water bath kettle at 60 ℃ for the time required for looking at the complete solvent at the rotating speed of 300rpm in 93g of N-methyl pyrrolidone.
Specifically, 7% of the self-repairing dispersion functional positive electrode binding material P3 solution is dried in an air-blasting drying oven at 80 ℃ for 2 hours, then the temperature is increased by 90 ℃ for two hours to prepare a glue film, and the glue film is cut into strips with the width of 15mm and the length of 80mm and placed in a horizontal peeling strength machine for a stretching experiment.
(4) The solid material proportion of the lithium iron phosphate positive electrode slurry is as follows: 2wt% of self-repairing dispersed functional positive electrode binding material P3,1wt% of conductive agent Super P and 97wt% of lithium iron phosphate. The positive electrode slurry consists of a solid material and N-methyl pyrrolidone, wherein the weight of the N-methyl pyrrolidone accounts for 40% of the total weight of the positive electrode slurry.
In the embodiment, specifically, the self-repairing dispersion function positive electrode binding material P3, super P and N-methyl pyrrolidone are mixed together, stirred for 20 seconds in a deaerator at a rotation speed of 800rpm/min, and then added with lithium iron phosphate, and stirred for 20 minutes in the deaerator at a rotation speed of 2000rpm/min, so as to obtain positive electrode slurry.
In this example, specifically, the positive electrode slurry was uniformly coated on the surface of the aluminum foil at thicknesses of 200um and 300um, respectively.
In this embodiment, specifically, the uniformly dispersed slurry is uniformly coated on the substrate with a thickness of 200um &300um by using aluminum foil as the substrate of the positive electrode sheet.
In the embodiment, specifically, the manufactured positive electrode sheet is placed in an oven and dried at 105 ℃ for 30min &1h.
In this embodiment, specifically, the rolled pole piece dried by 200 μm wet thickness is tested for peel strength and folding endurance.
In this embodiment, specifically, the pole piece dried to a wet thickness of 300um is placed under an electronic magnifier to observe the cracking degree in the same ratio, and placed in a glove box for 48 hours to observe the cracking state.
Comparative example 1, the positive electrode binder and positive electrode slurry were prepared as follows:
(1) 7g of the positive electrode binding material, funuolin (2032), is weighed into 93g of N-methyl pyrrolidone, and magnetically stirred in a water bath kettle at 60 ℃ for the time required for looking at the complete solvent at the rotating speed of 300 rpm.
Further, 7% positive electrode binding material solution is dried in a blowing drying oven at 80 ℃ for 2 hours, then dried at 90 ℃ for two hours to prepare a glue film, and the glue film is cut into strips with the width of 15mm and the length of 80mm and placed in a horizontal peeling strength machine for stretching experiments.
(2) The solid material proportion of the lithium iron phosphate positive electrode slurry is as follows: 2wt% of a positive electrode binding material, namely, fusolin (2032), 1wt% of a conductive agent Super P and 97wt% of lithium iron phosphate. The positive electrode slurry consists of a solid material and N-methyl pyrrolidone, wherein the weight of the N-methyl pyrrolidone accounts for 40% of the total weight of the positive electrode slurry.
In the embodiment, specifically, the positive electrode binding materials of furol (2032), super P and N-methyl pyrrolidone are mixed together, stirred at a rotation speed of 800rpm/min for 20 seconds in a deaerator, and then added with lithium iron phosphate and stirred at a rotation speed of 2000rpm/min for 20 minutes in the deaerator, so as to obtain positive electrode slurry.
In this example, specifically, the positive electrode slurry was uniformly coated on the surface of the aluminum foil at thicknesses of 200um and 300um, respectively.
In this embodiment, specifically, the uniformly dispersed slurry is uniformly coated on the substrate with a thickness of 200um &300um by using aluminum foil as the substrate of the positive electrode sheet.
In the embodiment, specifically, the manufactured positive electrode sheet is placed in an oven and dried at 105 ℃ for 30min &1h.
In this embodiment, specifically, the rolled pole piece dried by 200 μm wet thickness is tested for peel strength and folding endurance.
In this embodiment, specifically, the pole piece dried to a wet thickness of 300um is placed under an electronic magnifier to observe the cracking degree in the same ratio, and placed in a glove box for 48 hours to observe the cracking state.
In this example, specifically, the dissolution test results of examples 1 to 3and comparative example 1 described above are shown in table 1 below.
TABLE 1 results of dissolution test of examples 1-3 and comparative example 1
In this example, it is specifically understood from examples 1 to 3 and comparative example 1 that: 1. compared with the dissolution time of the positive electrode binding material Funuolin (2032), the self-repairing dispersion functional positive electrode binding material provided by the invention has the advantages that when the grafting monomer reaches more than 15 parts, the dissolution time is not reduced any more, and is reduced by 37.5% at most; 2. the 7% solution viscosity of the self-repairing dispersion functional positive electrode binding material is reduced by 30% -40% compared with that of the positive electrode binding material Funoline (2032).
In this example, specifically, the adhesive film performance test results of the above examples 1 to 3 and comparative example 1 are shown in the following table 2.
TABLE 2 adhesive film Performance test results for examples 1-3 and comparative example 1
In this example, it is specifically understood from examples 1 to 3 and comparative example 1 that: 1. the flexibility of the self-repairing dispersion function positive electrode binding material is improved, the elongation of the adhesive film is approximately twice that of the positive electrode binding material Funoline (2032), and the reduction of the elastic modulus further indicates that the toughness of the self-repairing dispersion function positive electrode binding material is improved; 2. when the grafting monomer is 15 parts, the flexibility of the self-repairing dispersion functional positive electrode binding material is improved to be close to a saturated state.
In this example, specifically, the slurry properties of examples 1 to 3 and comparative example 1 described above were tested as shown in the following Table 3.
TABLE 3 results of slurry Performance test for examples 1-3 and comparative example 1
In this embodiment, specifically, the method for detecting viscosity includes: the sample was placed in a constant temperature water bath at 25℃for 1h, measured using an NDJ-5S digital rotary viscometer, using rotor number 4, at 12rpm, and at 25 ℃.
In this example, it is specifically understood from examples 1 to 3 and comparative example 1 that: 1. the slurry viscosity gradually decreases with the increase of the amount of the grafting monomer, and when the grafting monomer is 20 parts, the slurry viscosity is reduced by 62% compared with the viscosity of the comparison sample; 2. the slurry prepared from the self-repairing dispersion functional positive electrode binding material has better stability, only increases by about 30 percent in 24 hours, and increases by nearly 130 percent in 24 hours in viscosity of the slurry prepared from the positive electrode binding material Funulin (2032).
In this example, the peel strength and the folding endurance test results of the wet thickness 200um dry pole pieces of examples 1 to 3 and comparative example 1 are shown in table 4 below.
Table 4 test results of peel strength and folding endurance of wet thickness 200um dry pole pieces of examples 1-3 and comparative example 1
In this embodiment, specifically, the method for detecting the peel force includes: the pole piece rolled to a compaction density of 2.4g/m3 is cut into sample strips of 15mm multiplied by 200mm, and the sample strips are tested by using a 180-degree horizontal peel strength tester at a speed of 150mm/min and a test temperature of 23 ℃.
In this embodiment, specifically, the method for testing the folding endurance is as follows: the pole piece is rolled to a compaction density of 2.4g/m < 3 > pole piece, and is cut into a sample strip with 15mm multiplied by 200mm, and the sample strip is folded once respectively to the coating surface and the aluminum foil surface for one time until the sample strip is cracked.
In this example, it is specifically understood from examples 1 to 3 and comparative example 1 that: 1. the peel strength of the positive electrode plate prepared by the self-repairing dispersion functional positive electrode binding material is obviously increased, and when the grafting monomer is 10 parts, the peel strength is about 5 times that of the positive electrode plate prepared by the positive electrode binding material Funulin (2032); 2. the peel force and folding endurance were reduced with the addition of the grafting monomer, which was the optimum grafting amount at 15 parts.
Referring to FIG. 1, FIG. 1 is an enlarged view showing the cracking degree of the wet-thickness 300um dry pole pieces of examples 1-3 and comparative example 1 when taken out and after the glove box is placed for 48 hours.
In this example, it is specifically understood from examples 1 to 3 and comparative example 1 that: 1. the cracking prevention effect of the positive electrode plate prepared by the self-repairing dispersion functional positive electrode bonding material is far better than that of the positive electrode plate prepared by the positive electrode bonding material Funulin (2032); 2. the cracking resistance is slightly reduced with the increase of the grafting monomer; 3. when the self-repairing dispersion functional positive electrode bonding material is placed in a glove box for 48 hours, the cracks of the positive electrode plate prepared by the self-repairing dispersion functional positive electrode bonding material are less or even disappear, and the cracks of the positive electrode plate prepared by the positive electrode bonding material Funuolin (2032) are not improved.
In summary, the preparation method of the self-repairing dispersion functional positive electrode binding material, the positive electrode slurry, the preparation method of the positive electrode slurry and the preparation method of the positive electrode plate have the beneficial effects that:
(1) According to the preparation method of the self-repairing dispersion functional positive electrode binding material, the crystallinity of the original binding material is reduced through mechanical deformation and grafting of the monomer, the solubility of the binding material is greatly improved, the flexibility of the obtained pole piece is also improved, and the influence of cracking of the pole piece is reduced;
(2) The positive electrode slurry prepared by the invention has good charge repulsive force due to the grafting of the phosphate group, and has a certain steric hindrance effect due to the PVDF long chain, so that the viscosity and the stability of the slurry are greatly improved;
(3) The anode slurry prepared by the invention realizes dynamic crosslinking due to a reversible crosslinking system of host-guest interaction of beta-cyclodextrin and gallic acid, and can recover broken bonds between polymer chains in a continuous cycle period, thereby introducing a self-repairing effect; meanwhile, the beta-cyclodextrin has a unique space network structure, so that the stability of the slurry is further maintained.
(4) The positive electrode plate prepared by the invention has the advantages that the beta-cyclodextrin hyperbranched network structure and the positive electrode material are contacted more firmly through multidimensional hydrogen bond interaction, and meanwhile, the binding force between the positive electrode material and the base material is increased through the chelation of the carboxyl of gallic acid and the aluminum material; the binding force is tighter in the whole dynamic crosslinking process, so that the structure of the electrode film can be stabilized, and the cycle performance is enhanced.
In the embodiment, the self-repairing and dispersing function positive electrode binding material prepared by the extrusion method has the advantages of simple manufacturing process, low cost, short time, high efficiency, no pollution, continuous production and industrial production conditions.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (9)
1. The preparation method of the self-repairing dispersion functional positive electrode binding material is characterized by comprising the following steps of:
(1) Uniformly mixing PVDF powder with a proper amount of initiator, grafting monomer and self-repairing functional monomer through a pulverizer;
(2) Extruding PVDF modified products from the uniformly mixed samples under the high-temperature and high-pressure reaction condition of a double-screw extruder with the length-diameter ratio L/D of 40;
(3) Spray drying the PVDF modified product to obtain a final product;
The self-repairing functional monomer is at least one of beta-cyclodextrin and gallic acid.
2. The method for preparing the self-repairing dispersion functional positive electrode binding material according to claim 1, which is characterized in that: in the step (1), the mass portions of the reaction components are as follows: PVDF 100 parts; 10-20 parts of grafting monomer; 0.5 parts of an initiator; 5 parts of self-repairing functional monomer.
3. The method for preparing the self-repairing dispersion functional positive electrode binding material according to claim 1, which is characterized in that: in the step (1), the grafting monomer is any one or a combination of at least two of phosphoric acid methacrylate, glycidyl methacrylate, isopropyl methacrylate, tetrahydrofuran methyl methacrylate, vinyl acetate, N-vinyl pyrrolidone, 1, 6-hexanediol diacrylate, neopentyl glycol diacrylate, dipropylene glycol diacrylate, tripropylene glycol diacrylate and trimethylolpropane triacrylate.
4. The method for preparing the self-repairing dispersion functional positive electrode binding material according to claim 1, which is characterized in that: in the step (1), the initiator is any one of di-tert-butyl peroxide, di-tert-butylcumene peroxide, benzoyl peroxide, tert-butyl peroxybenzoate, lauroyl peroxide, dicumyl peroxide and tert-butylisononanoate peroxide.
5. The method for preparing the self-repairing dispersion functional positive electrode binding material according to claim 1, which is characterized in that: in the step (2), the twin-screw extruder is provided with six sections, wherein the temperatures of the first section to the sixth section are in sequence: 30 ℃, 80 ℃, 160 ℃, 150 ℃.
6. The method for preparing the self-repairing dispersion functional positive electrode binding material according to claim 1, which is characterized in that: in the step (2), the feed inlet of the double-screw extruder is arranged in the first section, the feed speed is 30rpm, the screw rotating speed is 40rpm, and the average residence time of the materials in the double-screw extruder is 1.5-3min.
7. The positive electrode slurry is characterized by comprising solid materials and an organic solvent; wherein the solid materials comprise the following components in parts by weight: 2 parts of self-repairing dispersed functional positive electrode binding material prepared by the method according to any one of claims 1-6; 1 part of a conductive agent; 97 parts of lithium iron phosphate.
8. A method of preparing the positive electrode slurry according to claim 7, comprising:
(1) Adding and mixing the self-repairing dispersion functional positive electrode binding material, the conductive agent and the organic solvent;
(2) And adding the lithium iron phosphate, stirring and dispersing to obtain the positive electrode slurry.
9. The preparation method of the positive plate is characterized by comprising the following steps:
(1) Uniformly coating the uniformly dispersed positive electrode slurry on a substrate by taking aluminum foil as a positive electrode substrate;
(2) And (3) placing the substrate coated with the positive electrode slurry in an oven, and drying at 105 ℃ to obtain the positive electrode plate.
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| CN116606519A (en) * | 2023-05-24 | 2023-08-18 | 安徽大学 | PVDF composite material with high adhesive force and preparation method thereof |
| CN117946338A (en) * | 2024-01-29 | 2024-04-30 | 安徽大学 | PVDF material with high compatibility and adhesion and preparation method thereof |
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| CN108300340A (en) * | 2017-01-13 | 2018-07-20 | 国立大学法人大阪大学 | Glued construction body and its manufacturing method |
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