CN115141376B - Dispersing agent for lithium ion battery anode slurry and application thereof - Google Patents
Dispersing agent for lithium ion battery anode slurry and application thereof Download PDFInfo
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- 239000002270 dispersing agent Substances 0.000 title claims abstract description 59
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 22
- 239000006256 anode slurry Substances 0.000 title abstract description 6
- 239000011267 electrode slurry Substances 0.000 claims abstract description 26
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 12
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 5
- 239000006258 conductive agent Substances 0.000 claims description 17
- 239000011230 binding agent Substances 0.000 claims description 13
- 239000003960 organic solvent Substances 0.000 claims description 13
- 239000007774 positive electrode material Substances 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 239000002033 PVDF binder Substances 0.000 claims description 5
- 239000002041 carbon nanotube Substances 0.000 claims description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims description 4
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 4
- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 claims description 2
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- RLGQACBPNDBWTB-UHFFFAOYSA-N cetyltrimethylammonium ion Chemical group CCCCCCCCCCCCCCCC[N+](C)(C)C RLGQACBPNDBWTB-UHFFFAOYSA-N 0.000 claims description 2
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical group CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 claims description 2
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical group CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000004220 aggregation Methods 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 description 43
- 238000003756 stirring Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 239000003292 glue Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 239000002202 Polyethylene glycol Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 229920001223 polyethylene glycol Polymers 0.000 description 5
- 229920001451 polypropylene glycol Polymers 0.000 description 5
- 238000004537 pulping Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 125000003158 alcohol group Chemical group 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- XJMWHXZUIGHOBA-UHFFFAOYSA-N azane;propanoic acid Chemical compound N.CCC(O)=O XJMWHXZUIGHOBA-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229920002113 octoxynol Polymers 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- -1 1, 3-dimethylbutyl Chemical group 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000004491 isohexyl group Chemical group C(CCC(C)C)* 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
-
- 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
-
- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- 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
-
- 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
Abstract
The invention discloses a dispersing agent for lithium ion battery anode slurry, which has the following structural formula: RO (C) 2 H 4 O) m (C 3 H 6 O) n CH 2 CH 2 COOM wherein R represents a C2-C18 alkyl group and M represents H, NH 4 + Or an organic ammonium group, n is 1 to 50, and m is 1 to 50. The dispersing agent is specially designed according to the characteristics of the positive electrode slurry of the lithium battery, and can reduce the risk of secondary aggregation of solid particles in the positive electrode slurry on the premise of ensuring that the conductivity of the lithium battery is not affected, improve the fluidity of the positive electrode slurry, further reduce the resistance of a pole piece, improve the gram capacity of the battery and reduce the alternating current internal resistance of the battery.
Description
Technical Field
The invention relates to a dispersing agent for lithium ion battery anode slurry, in particular to an ionic dispersing agent, and belongs to the technical field of lithium batteries.
Background
The lithium ion battery has the advantages of large specific energy, long cycle life, low self-discharge rate, no memory effect, environmental friendliness and the like, and has wide application in the fields of aviation, national defense, automobiles, 3C and the like.
A lithium ion battery is a rechargeable battery that operates primarily by virtue of movement of lithium ions between a positive electrode and a negative electrode. During charge and discharge, li + To-and-fro intercalation and deintercalation between two electrodes, li during charging + The positive electrode is de-intercalated, the negative electrode is intercalated by the electrolyte, the negative electrode is in a lithium-rich state, and the negative electrode is in the opposite direction during discharge.
The lithium ion battery consists of a positive electrode, a negative electrode, a diaphragm and electrolyte, and when the lithium ion battery is formed, the prepared slurry is required to be coated on an aluminum foil to prepare the positive electrode and the negative electrode respectively, so that the viscosity of the slurry is directly related to the coating quality, the current requirements on the capacity of the lithium ion battery are higher and higher, and the common solution is to increase the proportion of electrode active substances in the slurry, so that the solid content of the slurry is too high, the viscosity and the fluidity are poor, the coating effect of the electrode is influenced, and the efficiency of the preparation process of the lithium ion battery is further influenced.
In view of the above problems, the current solution in the industry is to add a dispersant to the slurry to improve the dispersion effect of the slurry, and the existing dispersants include polyvinylpyrrolidone, phosphite, triton-X and the like, which can solve the fluidity problem of the slurry to a certain extent, but the functions of the slurry on the problems of viscosity, gel and the like are still not strong enough, and in addition, the safety of the dispersants is not high.
Disclosure of Invention
Aiming at the problems of poor viscosity and fluidity of slurry for lithium ion batteries, and influence on electrode coating effect, further increase of electrode sheet resistance and reduction of gram capacity, the invention provides a dispersing agent for positive electrode slurry of lithium ion batteries and application thereof.
The technical scheme for solving the technical problems is as follows:
a dispersing agent for positive electrode slurry of a lithium ion battery has the following structural formula: RO (C) 2 H 4 O) m (C 3 H 6 O) n CH 2 CH 2 COOM wherein R represents a C2-C18 alkyl group and M represents H, NH 4 + Or an organic ammonium group, n is 1 to 50, and m is 1 to 50.
Preferably, R represents a C4-C16 alkyl group, more preferably a C6-C12 alkyl group, most preferably a C8-C10 alkyl group.
Preferably, the organic ammonium group is cetyl trimethylammonium group, tetraethylammonium group or tetrabutylammonium group.
Preferably, n is 10 to 40 and m is 10 to 40; further preferably, n is 10 to 25 and m is 10 to 25.
The alkyl groups described in the present invention may be linear or branched, and may be, for example, C2 alkyl-ethyl; c3 alkyl-propyl, such as n-propyl or isopropyl; c4 alkyl-butyl such as n-butyl, isobutyl, tert-butyl or 2-butyl; c5 alkyl-pentyl, such as n-pentyl, isopentyl or neopentyl; c6 alkyl-hexyl, such as n-hexyl, isohexyl and 1, 3-dimethylbutyl.
The dispersing agent is prepared by polymerizing polypropylene glycol, polyethylene glycol and alcohol corresponding to R to form a precursor, and then performing condensation reaction on terminal alcohol hydroxyl of the precursor and 1-hydroxy ammonium propionate, wherein the dispersing agent can be obtained by referring to the following reaction process:
ROH+HO-(CH 2 CH 2 O) m -H→RO-(CH 2 CH 2 O) m -H (1)
OH-(CH 2 CH 2 CH 2 O) n -H+CH 2 OHCH 2 COOM→OH-(CH 2 CH 2 CH 2 O) n -CH 2 CH 2 COOM (2)
RO-(CH 2 CH 2 O) n -H+OH-(CH 2 CH 2 CH 2 O) n -CH 2 CH 2 COOM→RO-(CH 2 CH 2 O) n (CH 2 CH 2 CH 2 O) m -CH 2 CH 2 COOM (3)
(1) Under the catalysis of concentrated sulfuric acid, polyethylene glycol and ROH are subjected to condensation dehydration reaction under the stirring condition of 30-35 ℃ in the presence of an organic solvent, and the molar ratio of the polyethylene glycol to the ROH is (0.6-0.8): 1, generating polyethylene glycol monoethers;
(2) The polypropylene glycol and the 1-hydroxy ammonium propionate are subjected to condensation dehydration reaction under the condition of stirring at 25-30 ℃ in the presence of an organic solvent under the catalysis of concentrated sulfuric acid, and the molar ratio of the polypropylene glycol to the 1-hydroxy ammonium propionate is 1: (1.1-1.2) to produce hydroxyl-terminated polypropylene glycol ammonium propionate;
(3) Stirring and reacting hydroxyl-terminated polypropylene glycol ammonium propionate and polyethylene glycol monoether in a dry container with tetrahydrofuran as solvent in the presence of concentrated sulfuric acid at 35-40deg.C for 12-24 hr in inert atmosphere to obtain RO- (CH) at a molar ratio of 1:1 2 CH 2 O) n (CH 2 CH 2 CH 2 O) m -CH 2 CH 2 COOM is obtained through a further hydrolysis reaction when M represents H.
The action principle of the dispersing agent for the lithium ion battery anode slurry claimed by the invention is as follows:
the hydrophilic group and the lipophilic group can effectively reduce the surface tension of a solid-liquid interface from a microscopic interface, improve the wetting permeability, improve the solid content and the coating convenience of electrode active substances, and are favorable for uniform dispersion of particles such as electrode active substances, conductive carbon and the like, thereby improving the performance of a battery.
The dispersant provided by the invention has the beneficial effects that:
(1) The dispersing agent is specially designed according to the characteristics of the positive electrode slurry of the lithium battery, and can reduce the risk of secondary aggregation of solid particles in the positive electrode slurry on the premise of ensuring that the conductivity of the lithium battery is not affected, improve the fluidity of the positive electrode slurry, further reduce the resistance of a pole piece, improve the gram capacity of the battery and reduce the alternating current internal resistance of the battery;
(2) The dispersing agent is convenient to use, does not need to be matched with a special pulping process, and can achieve the dispersing and viscosity reducing effects of the slurry by adding the dispersing agent according to a proportion on the basis of the original pulping process, and the process cost is not required to be increased additionally.
The invention also discloses a lithium ion battery anode slurry which comprises the dispersing agent.
Preferably, the positive electrode slurry further contains a positive electrode active material and a conductive agent.
Preferably, the positive electrode active material is one or more of lithium cobaltate, lithium iron phosphate, nickel cobalt manganese ternary material and nickel cobalt lithium aluminate ternary material; the conductive agent is one or two of carbon black and carbon nano tube.
Preferably, the positive electrode slurry further comprises a binder and an organic solvent, wherein the binder is polyvinylidene fluoride, and the organic solvent is N-methylpyrrolidone.
The invention also discloses a positive pole piece of the lithium ion battery, and the surface of the positive pole piece is coated with the positive pole slurry of the lithium ion battery.
The invention also discloses a lithium ion battery, which comprises the positive electrode plate.
Detailed Description
The principles and features of the present invention are described below in connection with examples, which are set forth only to illustrate the present invention and not to limit the scope of the invention.
The structural formula of the dispersing aid used in the examples is presented below:
example 1: effect in wet pulping process
The specific preparation steps of the lithium battery positive electrode slurries of the experimental groups 1-5 and the control group 1 are as follows:
1) Mixing and stirring the binder and the organic solvent uniformly to obtain a glue solution A;
2) Respectively adding the dispersing agents A-F into the glue solution A and uniformly stirring to obtain a glue solution B;
3) Adding a conductive agent into the glue solution B to obtain conductive agent slurry;
4) And adding the positive electrode active material into the conductive agent slurry to obtain positive electrode slurry.
The weight ratio of the raw materials in the method is as follows: conductive agent: dispersing agent: binder = 92:4:3:1; the positive electrode active material is lithium iron phosphate produced by Hunan Yu energy-saving new energy battery material Co, the conductive agent is formed by mixing conductive carbon black and carbon nano tubes according to a mass ratio of 1:1, the binder is polyvinylidene fluoride, the organic solvent is N-methyl pyrrolidone, and the dispersing agents used in examples 1-5 are a dispersing agent A, a dispersing agent B, a dispersing agent C, a dispersing agent D and a dispersing agent E respectively.
The control group 1 was not added with dispersant, and the other components of the slurry were the same as those of the experimental groups 1 to 5.
And respectively taking the freshly prepared slurry for testing, standing the slurry after 24 hours, stirring the slurry for 1 minute, testing, using a force ND-10 rotary viscometer, using a No. 2 rotor, inserting the rotor into the slurry to be tested, testing the rotating speed at 100rpm for 60 seconds, and obtaining the viscosity value of the slurry by using a multipoint average value taking mode, wherein the testing result is shown in Table 1.
Table 1 slurry viscosities and solids contents of experimental groups 1-5 and control group 1
As can be seen from the data in Table 1, after the dispersants of the present invention are added in the experimental groups 1 to 5, the solid content of the freshly prepared slurry is improved by 3 to 5% compared with that of the control group 1, the slurry of the control group 1 is gelled after 24 hours, and the slurries of the experimental groups 1 to 5 are still good in fluidity, which indicates that the dispersants of the present invention have good dispersing effect on the positive electrode slurry obtained by the wet pulping process.
Example 2: effect in dry pulping process
The specific preparation process of the lithium battery positive electrode slurries of the experimental groups 6-10 and the control group 2 is as follows:
1) Dry-mixing the binder, the conductive agent and the positive electrode active material to obtain uniformly mixed powder;
2) Adding part of organic solvent into the powder, and uniformly stirring to obtain initial slurry A;
3) Adding the dispersing agent into the initial slurry A, and uniformly stirring;
4) And on the basis of the step 3), adding the rest organic solvent, and uniformly stirring to obtain the positive electrode slurry.
Wherein, the weight ratio of each raw material is that the positive electrode active material: conductive agent: dispersing agent: binder=94:3.5:1.5:1; the positive electrode active material is lithium cobaltate, the conductive agent is formed by mixing conductive carbon black and carbon nano tubes according to the mass ratio of 1:1, the binder is polyvinylidene fluoride, the organic solvent is N-methyl pyrrolidone, and the dispersing agents used in examples 6-10 are a dispersing agent A, a dispersing agent B, a dispersing agent C, a dispersing agent D and a dispersing agent E respectively.
And respectively taking the freshly prepared slurry for testing, standing the slurry after 24 hours, stirring the slurry for 1 minute, testing, using a force ND-10 rotary viscometer, using a No. 2 rotor, inserting the rotor into the slurry to be tested, testing the rotating speed at 100rpm for 60 seconds, and obtaining the viscosity value of the slurry by using a multipoint average value taking mode, wherein the testing result is shown in Table 2.
Table 2 slurry viscosities and solids contents of experimental groups 6-10 and control group 2
As can be seen from the data in Table 2, after the dispersion aid of the present invention was added to the positive electrode slurries of the experimental groups 6 to 10, the solid content of the freshly prepared slurries was increased by 4 to 7% as compared with the comparative group 2, the initial viscosity was slightly increased, the slurries of the comparative group 2 were gelled after 24 hours, and the slurries of the experimental groups 6 to 10 were still excellent in fluidity, indicating that the dispersant of the present invention also has excellent dispersion effect on the positive electrode slurries obtained by the dry method.
Example 3: comparative experiment Effect with existing dispersant
The preparation methods of the lithium battery positive electrode slurries of the experimental groups 11-12 and the control groups 3-5 are as follows:
1) Mixing and stirring the binder and the organic solvent uniformly to obtain a glue solution A;
2) Adding a dispersing agent into the glue solution A and uniformly stirring to obtain a glue solution B;
3) Adding a conductive agent into the glue solution B to obtain conductive agent slurry;
4) And adding the positive electrode active material into the conductive agent slurry to obtain positive electrode slurry.
Wherein, the weight ratio of each raw material is that the positive electrode active material: conductive agent: dispersing agent: binder = 93:3:3:1; the positive electrode active material is lithium iron phosphate produced by Hunan Yu energy new energy battery material Co-Ltd, the conductive agent is formed by mixing conductive carbon black and carbon nano tubes according to the mass ratio of 1:1, the binder is polyvinylidene fluoride, the organic solvent is N-methyl pyrrolidone, the dispersing agents of the experiment groups 11 and 12 are respectively dispersing agent A and dispersing agent D, the dispersing agent of the comparison group 3 is polyvinylpyrrolidone, the dispersing agent of the comparison group 4 is triethyl phosphite, and the dispersing agent of the comparison group 5 is triton X.
And respectively taking the freshly prepared slurry for testing, stirring the slurry after standing for 24 hours for 1min, testing, using a force ND-10 rotary viscometer, using a No. 2 rotor, inserting the rotor into the slurry to be tested, testing the rotating speed at 100rpm for 60s, and obtaining the viscosity value of the slurry by using a multipoint average method, wherein the testing result is shown in Table 3.
TABLE 3 slurry viscosities and solids contents of experimental groups 11-12 and control groups 3-5
As can be seen from the data in Table 3, the solid content of the obtained positive electrode slurry is relatively higher than that of other existing dispersants, and the viscosity of the slurry obtained after 24 hours of standing is obviously reduced, so that the effect of improving the fluidity of the slurry is remarkable.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (13)
1. A dispersing agent for positive electrode slurry of a lithium ion battery has the following structural formula: RO (C) 2 H 4 O) m (C 3 H 6 O) n CH 2 CH 2 COOM wherein R represents a C2-C18 alkyl group and M represents H, NH 4 + Or organic ammonium group, n is 1-50, m is 1-50, and the positive electrode active substance in the positive electrode slurry is one or more of lithium cobaltate, lithium iron phosphate, nickel cobalt manganese ternary material and nickel cobalt lithium aluminate ternary material.
2. A dispersant as claimed in claim 1 wherein R represents a C4-C16 alkyl group.
3. A dispersant as claimed in claim 2 wherein R represents a C6-C12 alkyl group.
4. A dispersant as claimed in claim 3 wherein R represents a C8-C10 alkyl group.
5. The dispersant of any one of claims 1 to 4, wherein said organic ammonium group is cetyl trimethylammonium group, tetraethylammonium group or tetrabutylammonium group.
6. The dispersant of any one of claims 1 to 4, wherein n is 10 to 40 and m is 10 to 40.
7. The dispersant of claim 6 wherein n is 10 to 25 and m is 10 to 25.
8. The dispersant of claim 5 wherein n is 10 to 40 and m is 10 to 40.
9. The dispersant of claim 8 wherein n is 10 to 25 and m is 10 to 25.
10. A lithium ion battery positive electrode slurry comprising the dispersant of any one of claims 1 to 9, further comprising a positive electrode active material and a conductive agent.
11. The positive electrode slurry according to claim 10, wherein the conductive agent is one or both of carbon black and carbon nanotubes.
12. The positive electrode slurry according to any one of claims 10 to 11, further comprising a binder and an organic solvent, wherein the binder is polyvinylidene fluoride, and the organic solvent is N-methylpyrrolidone.
13. A positive electrode sheet of a lithium ion battery, characterized in that the surface of the positive electrode sheet is coated with the positive electrode slurry according to any one of claims 10 to 12.
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JP2001160395A (en) * | 1999-12-03 | 2001-06-12 | Mitsubishi Chemicals Corp | Material for positive electrode of lithium secondary battery |
CN102064326A (en) * | 2010-12-16 | 2011-05-18 | 东莞新能源电子科技有限公司 | Dispersing agent for positive and negative electrode materials of lithium ion battery |
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CN102064326A (en) * | 2010-12-16 | 2011-05-18 | 东莞新能源电子科技有限公司 | Dispersing agent for positive and negative electrode materials of lithium ion battery |
CN103208631A (en) * | 2012-01-17 | 2013-07-17 | 万向电动汽车有限公司 | Lithium battery positive electrode slurry and preparation method thereof |
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