CN116799213A - Lithium ion battery positive electrode slurry dispersion auxiliary agent and preparation method and application thereof - Google Patents
Lithium ion battery positive electrode slurry dispersion auxiliary agent and preparation method and application thereof Download PDFInfo
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- CN116799213A CN116799213A CN202310842747.0A CN202310842747A CN116799213A CN 116799213 A CN116799213 A CN 116799213A CN 202310842747 A CN202310842747 A CN 202310842747A CN 116799213 A CN116799213 A CN 116799213A
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- positive electrode
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 34
- 239000006185 dispersion Substances 0.000 title claims abstract description 26
- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 11
- 239000011267 electrode slurry Substances 0.000 title claims description 26
- 238000002360 preparation method Methods 0.000 title abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000006256 anode slurry Substances 0.000 claims abstract description 9
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 229920000570 polyether Polymers 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 45
- 238000006116 polymerization reaction Methods 0.000 claims description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 9
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 9
- -1 polyoxyethylene Polymers 0.000 claims description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 5
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 4
- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 claims description 4
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 4
- UWNADWZGEHDQAB-UHFFFAOYSA-N i-Pr2C2H4i-Pr2 Natural products CC(C)CCC(C)C UWNADWZGEHDQAB-UHFFFAOYSA-N 0.000 claims description 4
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 4
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 4
- YTUUEOBZXXUZJL-UHFFFAOYSA-N 2,3-diethylpentane-1,2,3-triol Chemical compound CCC(O)(CC)C(O)(CC)CO YTUUEOBZXXUZJL-UHFFFAOYSA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 150000005215 alkyl ethers Chemical class 0.000 claims description 3
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 3
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 3
- CCIVGXIOQKPBKL-UHFFFAOYSA-N ethanesulfonic acid Chemical compound CCS(O)(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 3
- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical compound NCCS(O)(=O)=O XOAAWQZATWQOTB-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
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 3
- UICXTANXZJJIBC-UHFFFAOYSA-N 1-(1-hydroperoxycyclohexyl)peroxycyclohexan-1-ol Chemical compound C1CCCCC1(O)OOC1(OO)CCCCC1 UICXTANXZJJIBC-UHFFFAOYSA-N 0.000 claims description 2
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 claims description 2
- ZAJAQTYSTDTMCU-UHFFFAOYSA-N 3-aminobenzenesulfonic acid Chemical compound NC1=CC=CC(S(O)(=O)=O)=C1 ZAJAQTYSTDTMCU-UHFFFAOYSA-N 0.000 claims description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims description 2
- BLCKNMAZFRMCJJ-UHFFFAOYSA-N cyclohexyl cyclohexyloxycarbonyloxy carbonate Chemical compound C1CCCCC1OC(=O)OOC(=O)OC1CCCCC1 BLCKNMAZFRMCJJ-UHFFFAOYSA-N 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 claims description 2
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 2
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 2
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 2
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 2
- FFIUNPRXUCRYFU-UHFFFAOYSA-N tert-butyl pentaneperoxoate Chemical compound CCCCC(=O)OOC(C)(C)C FFIUNPRXUCRYFU-UHFFFAOYSA-N 0.000 claims description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 abstract description 12
- 229910021393 carbon nanotube Inorganic materials 0.000 abstract description 12
- 239000006258 conductive agent Substances 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000005336 cracking Methods 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 229910004764 HSV900 Inorganic materials 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium ion batteries, and in particular relates to a lithium ion battery anode slurry dispersion auxiliary agent, a preparation method and application thereof, wherein the lithium ion battery anode slurry dispersion auxiliary agent comprises the following raw material components: the total weight is 100 parts, wherein, the component A is 40-60 parts, the component B is 10-20 parts, and the component C is 30-50 parts; the component A is hydroxyl-containing polyether substance, the component B is initiator, and the component C is sulfonic group-containing organic substance. The compound carbon tube system can solve the problem of uneven dispersion of the slurry in a long-cycle, high-multiplying power, high specific energy and other (which needs to use the carbon nanotube conductive slurry as a conductive agent) cell technology platform; the solvent consumption is reduced, and the energy consumption is reduced; the solid content is improved, and the cracking of the pole piece is improved; improving the fluidity and stability of the slurry; the agglomeration probability of small particles is reduced; reducing the resistance of the membrane; and the consistency of the performance of the battery cells is improved, and the yield of the pole pieces is improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a lithium ion battery anode slurry dispersing auxiliary agent, a preparation method and application thereof.
Background
Carbon nanotubes, which are novel carbon materials having a specific structure, have excellent mechanical and electrochemical properties, and have been attracting attention in various fields. In the application of lithium battery, when the carbon nano tube is used as the conductive agent, the unique network structure of the carbon nano tube can be effectively connected with more active substances, and the excellent conductivity can also greatly reduce the impedance. In addition, the carbon nano tube with larger length-diameter ratio has larger specific surface area, and compared with the traditional conductive agent SuperP and graphite, the carbon nano tube has the advantages that the addition amount is small enough to construct a high-efficiency three-dimensional high-conductivity network in the electrode, and the aim of improving the energy density of the battery is fulfilled. However, the carbon nanotubes are nano materials with small dimensions, have large specific surface area and high length-diameter ratio, are easy to agglomerate and are difficult to disperse. Thus, the complete dispersion of the carbon nanotubes into a non-aggregated "single state" is critical to improving the conductivity of the conductive paste. At present, the industry is used for preparing high-efficiency dispersion solution of carbon nanotubes, the solvent is mainly organic solvent N-methyl pyrrolidone (NMP), and a proper amount of dispersion auxiliary agent polyvinylpyrrolidone (PVP) is added to strengthen the dispersion effect.
The conductive paste (prepared from carbon nano tube, graphene, PVP dispersion aid, NMP solvent and the like) is used as a conductive agent to be applied to a lithium battery anode material, so that the impedance can be greatly reduced, the consumption of the conductive agent can be reduced, and the purposes of improving the performances of battery capacity, multiplying power, circulation and the like can be achieved. In order to improve the dispersion performance and the viscosity stabilizing effect of the slurry in the process of mixing the lithium ion battery anode materials, a dispersing auxiliary agent is often required to be added, so that the slurry can maintain good fluidity after being stored for one or two days. Conversely, at the same viscosity, the solid content can be increased, thus reducing the amount of NMP used, and after the solid content is increased, the baking temperature can be reduced, or if the baking temperature is unchanged, the coating speed can be faster. Thus, the productivity is improved, and the energy consumption is also saved.
However, we have found that the dispersion aid has antagonism (high viscosity rebound and easy gelation) when used with conductive paste, which results in pipe blockage or no paste removal by a flow pump, and large surface density fluctuation when coated, and difficult quality control.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a lithium ion battery anode slurry dispersing auxiliary agent, and is compounded with a carbon tube system or is applied to a long-cycle, high-multiplying-power and high-specific-energy (carbon nano tube conductive slurry is needed to be used as a conductive agent) cell technology platform for solving the problem of slurry dispersion.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the lithium ion battery anode slurry dispersing auxiliary is characterized by comprising the following raw material components: the total weight is 100 parts, wherein, the component A is 40-60 parts, the component B is 10-20 parts, and the component C is 30-50 parts;
the component A is hydroxyl-containing polyether substance, the component B is initiator, and the component C is sulfonic group-containing organic substance.
In a preferred example, the hydroxyl-containing polyether material is selected from one or a combination of two or more of trihydroxy polyether (polypropylene oxide), triethylglycerol ether, polytetrahydrofuran ether, polyoxyethylene ether, polyethylene glycol ether, propylene glycol polyoxyethylene ether, glycerol polyoxyethylene ether, allyl alcohol polyoxyalkylene ether, and polyoxyethylene alkyl ether.
In a preferred example, the initiator is selected from one or a combination of two or more of diisobutyl cyanide, azobisisobutyronitrile, azobisisoheptonitrile, cumene hydroperoxide, tert-butyl peroxybenzoate, tert-butyl peroxyvalerate, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, tert-butyl hydroperoxide/sodium metabisulfite, methyl ethyl ketone peroxide, cyclohexanone peroxide.
In a preferred example, the sulfonic acid group-containing organic substance is selected from one or a combination of two or more of toluene sulfonic acid, methyl sulfonic acid, trifluoro methane sulfonic acid, dodecyl benzene sulfonic acid, sulfamic acid, aminoethane sulfonic acid, benzene sulfonic acid, ethyl sulfonic acid, and sulfamic acid.
Based on one general inventive concept, another object of the present invention is to provide a method for preparing the above-mentioned lithium ion battery positive electrode slurry dispersion aid, comprising the steps of:
step 1: sequentially adding 40-60 parts of component A, 10-20 parts of component B and 30-50 parts of component C into a (100L) reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at a stirring speed of 30-50 rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 40-90 ℃, and performing prepolymerization reaction for 2-4 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 60-100 ℃, and carrying out polymerization reaction at the stirring rotation speed of 40-50 rpm for 3-5 h;
step 4: after the polymerization reaction is finished, the mixture is subjected to demagnetizing filtration, sampling and detection, and warehousing if the mixture is qualified.
Based on one general inventive concept, another object of the present invention is to provide an application of the above-mentioned dispersion aid for positive electrode slurry of lithium ion battery, and to adapt the dispersion aid to conductive slurry of carbon tube system to obtain positive electrode slurry of lithium ion battery.
In a preferred example, the lithium ion battery positive electrode slurry contains the following solid components in mass fraction: liFePO 4 95 to 99 weight percent, 0.3 to 1.0 weight percent of conductive carbon black, 0.8 to 2.5 weight percent of conductive slurry, 1.5 to 2.5 weight percent of polyvinylidene fluoride and 0.1 to 0.5 weight percent of dispersing auxiliary agent.
Compared with the prior art, the lithium ion battery anode slurry dispersing auxiliary can be compounded with a carbon tube system, and can solve the problem of uneven slurry dispersion in a long-cycle, high-multiplying-power and high-specific-energy battery core technology platform (the carbon nano tube conductive slurry is required to be used as a conductive agent);
the specific advantages and positive effects mainly comprise the following aspects:
(1) The solvent consumption is reduced, and the energy consumption is reduced;
(2) The solid content is improved, and the cracking of the pole piece is improved;
(3) Improving the fluidity and stability of the slurry;
(4) The agglomeration probability of small particles is reduced;
(5) Reducing the resistance of the membrane;
(6) And the consistency of the performance of the battery cells is improved, and the yield of the pole pieces is improved.
Detailed Description
The invention will be further described with reference to specific embodiments for the purpose of making the objects, technical solutions and advantages of the invention more apparent, but the invention is not limited to these examples. It should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below. In the present invention, unless otherwise specified, all parts and percentages are by mass, the equipment and materials employed, etc. are commercially available or are conventional in the art. The methods in the following examples are conventional in the art unless otherwise specified.
The terms "comprising," "including," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range.
Example 1
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight, sequentially adding 50 parts of trihydroxy polyether (polypropylene oxide), 10 parts of diisobutylcyanide and 40 parts of methylbenzenesulfonic acid into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at 40rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 65 ℃, and performing prepolymerization reaction for 3 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 60-100 ℃, and stirring at 45rpm for 4h to perform polymerization reaction;
step 4: after the polymerization reaction is finished, demagnetizing, filtering, sampling, detecting, and warehousing to obtain the dispersing auxiliary 1.
Example 2
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight, sequentially adding 50 parts of polyethylene glycol ether, 10 parts of diisobutylcyanide and 40 parts of ethylsulfonic acid into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at 50rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 90 ℃, and performing prepolymerization reaction for 2 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 100 ℃, and carrying out polymerization reaction at the stirring rotation speed of 40rpm for 5 hours;
step 4: after the polymerization reaction is finished, demagnetizing, filtering, sampling, detecting, and warehousing to obtain the dispersing auxiliary 2.
Example 3
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight, sequentially adding 50 parts of glycerol polyoxyethylene ether, 10 parts of azodiisobutyronitrile and 40 parts of benzenesulfonic acid into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at a stirring rotating speed of 30rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 40 ℃, and performing prepolymerization reaction for 4 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 60 ℃, and carrying out polymerization reaction at the stirring rotation speed of 50rpm for 3 hours;
step 4: after the polymerization reaction is finished, demagnetizing, filtering, sampling, detecting, and warehousing to obtain the dispersing auxiliary 3.
Example 4
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight, sequentially adding 50 parts of polytetrahydrofuran ether, 10 parts of cumene hydroperoxide and 40 parts of dodecylbenzene sulfonic acid into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at a stirring rotating speed of 40rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 80 ℃, and performing prepolymerization reaction for 3.5h;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the tank of the reaction kettle at 85 ℃, and stirring at 42rpm for polymerization reaction for 3.5h;
step 4: after the polymerization reaction is finished, demagnetizing, filtering, sampling, detecting, and warehousing to obtain the dispersing auxiliary 4.
Example 5
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight, sequentially adding 50 parts of polyoxyethylene alkyl ether, 10 parts of diisobutyl cyanide and 40 parts of aminoethyl sulfonic acid into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at a stirring rotating speed of 45rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 45 ℃, and performing prepolymerization reaction for 2.5h;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 70 ℃, stirring at 48rpm, and carrying out polymerization reaction for 4.2h;
step 4: after the polymerization reaction is finished, demagnetizing, filtering, sampling, detecting, and warehousing to obtain the dispersing auxiliary 5.
Example 6
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight of the total weight, sequentially adding 50 parts of glycerol polyoxyethylene ether, 10 parts of cumene hydroperoxide and 40 parts of sulfamic acid into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at a stirring rotating speed of 38rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 55 ℃, and performing prepolymerization reaction for 3 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 65 ℃, and carrying out polymerization reaction at the stirring rotation speed of 45rpm for 3.5h;
step 4: after the polymerization reaction is finished, demagnetizing, filtering, sampling, detecting, and warehousing to obtain the dispersing auxiliary 6.
Example 7
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight, sequentially adding 50 parts of allyl alcohol polyoxyalkylene ether, 10 parts of diisobutyl cyanide and 40 parts of trifluoromethanesulfonic acid into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at a stirring speed of 42rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 60 ℃, and performing prepolymerization reaction for 2.2 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 78 ℃, and carrying out polymerization reaction at the stirring rotation speed of 42rpm for 4.8 hours;
step 4: after the polymerization reaction is finished, demagnetizing, filtering, sampling, detecting, and warehousing to obtain the dispersing auxiliary 7.
Example 8
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight, sequentially adding 50 parts of polyoxyethylene ether, 10 parts of tert-butyl peroxybenzoate and 40 parts of dodecylbenzenesulfonic acid into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at a stirring speed of 30rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 40 ℃, and performing prepolymerization reaction for 2 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 60 ℃, and carrying out polymerization reaction at the stirring rotation speed of 50rpm for 5 hours;
step 4: after the polymerization reaction is finished, demagnetizing, filtering, sampling, detecting, and warehousing to obtain the dispersing auxiliary 8.
Example 9
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight, sequentially adding 50 parts of triethylglycerol ether, 10 parts of diisobutylcyanide and 40 parts of aminobenzenesulfonic acid into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at 50rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 40-90 ℃, and performing prepolymerization reaction for 4 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 100 ℃, and carrying out polymerization reaction at the stirring rotation speed of 40rpm for 3 hours;
step 4: after the polymerization reaction is finished, the mixture is demagnetized, filtered, sampled and detected, and qualified and put in storage to obtain the dispersing auxiliary 9.
Comparative example 1
A lithium ion battery positive electrode slurry dispersing auxiliary comprises the following preparation steps:
step 1: based on 100 parts by weight, sequentially adding 50 parts of hydroxyethyl acrylate, 10 parts of potassium persulfate initiator and 40 parts of phosphorus pentoxide into a 100L reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at a stirring rotating speed of 40rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 65 ℃, and performing prepolymerization reaction for 3 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 80 ℃, and carrying out polymerization reaction at the stirring rotation speed of 45rpm for 4 hours;
step 4: after the polymerization reaction is finished, the mixture is subjected to demagnetizing filtration, sampling detection and qualified warehousing, and the dispersing auxiliary 10 is obtained.
In order to illustrate the suitability of the dispersing aid and the carbon tube conductive liquid, the dispersing aids prepared in examples 1-9 and comparative example 1 are respectively mixed with conductive paste G6 widely used in the lithium battery industry according to the weight ratio of 3:7, and the mixture is kept stand in an environment with humidity less than or equal to 10% and temperature of 25+/-2 ℃, and the slurry mobility of 1h, 2h, 4h and 24h after mixing is observed to judge whether the dispersing aid and the carbon tube are matched; the results are shown in Table 1 below.
TABLE 1 slurry fluidity State results after dispersing aid and conductive slurry G6 were blended
The dispersion aids prepared in examples 1-9 and comparative example 1 are respectively mixed with lithium iron phosphate E80, conductive paste G6, conductive agent carbon black SP and binder HSV900 (according to the proportion of lithium iron phosphate E80 to conductive paste G6 to conductive agent carbon black SP to binder HSV900 to dispersion aid=95% to 2% to 0.8% to 2% to 0.2 percent), the mixture is prepared into N-methyl pyrrolidone solvent to obtain positive electrode slurry, the positive electrode slurry is kept stand in the environment with humidity less than or equal to 10% and temperature of 25+/-2 ℃, and whether the dispersion aid is matched with a carbon tube is judged by testing the viscosity of the positive electrode slurry for 1h, 2h, 4h and 24 h; the results are shown in Table 2 below.
Table 2 results of testing viscosity stability of positive electrode slurry to which dispersion aid was added
The above embodiments are merely preferred embodiments of the present invention, and any simple modification, modification and substitution changes made to the above embodiments according to the technical substance of the present invention are all within the scope of the technical solution of the present invention.
Claims (7)
1. The lithium ion battery anode slurry dispersing auxiliary is characterized by comprising the following raw material components: the total weight is 100 parts, wherein, the component A is 40-60 parts, the component B is 10-20 parts, and the component C is 30-50 parts;
the component A is hydroxyl-containing polyether substance, the component B is initiator, and the component C is sulfonic group-containing organic substance.
2. The positive electrode slurry dispersion aid for lithium ion batteries according to claim 1, wherein the hydroxyl-containing polyether substance is one or a combination of two or more selected from the group consisting of trihydroxy polyether (polypropylene oxide), triethylglycerol ether, polytetrahydrofuran ether, polyoxyethylene ether, polyethylene glycol ether, propylene glycol polyoxyethylene ether, glycerol polyoxyethylene ether, allyl alcohol polyoxyalkylene ether and polyoxyethylene alkyl ether.
3. The positive electrode slurry dispersion aid for lithium ion batteries according to claim 1, wherein the initiator is one or a combination of two or more selected from diisobutyl cyanide, azobisisobutyronitrile, azobisisoheptonitrile, cumene hydroperoxide, tert-butyl peroxybenzoate, tert-butyl peroxyvalerate, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, tert-butyl hydroperoxide/sodium metabisulfite, methyl ethyl ketone peroxide and cyclohexanone peroxide.
4. The positive electrode slurry dispersion aid for lithium ion batteries according to claim 1, wherein the sulfonic acid group-containing organic substance is selected from one or a combination of two or more of methyl benzenesulfonic acid, methyl sulfonic acid, trifluoromethanesulfonic acid, dodecylbenzenesulfonic acid, sulfamic acid, aminoethanesulfonic acid, benzenesulfonic acid, ethylsulfonic acid, and aminobenzenesulfonic acid.
5. The method for preparing the lithium ion battery positive electrode slurry dispersion auxiliary agent as defined in claim 1, which is characterized by comprising the following steps:
step 1: sequentially adding 40-60 parts of component A, 10-20 parts of component B and 30-50 parts of component C into a reaction kettle, introducing nitrogen to prevent the introduction of moisture in the air, and starting stirring at a stirring speed of 30-50 rpm;
step 2: after stirring uniformly, starting a temperature control system, keeping the temperature in the tank of the reaction kettle at 40-90 ℃, and performing prepolymerization reaction for 2-4 hours;
step 3: continuously heating to the polymerization temperature of 80 ℃, keeping the temperature in the reaction kettle at 60-100 ℃, and carrying out polymerization reaction at the stirring rotation speed of 40-50 rpm for 3-5 h;
step 4: after the polymerization reaction is finished, the mixture is subjected to demagnetizing filtration, sampling and detection, and warehousing if the mixture is qualified.
6. The application of the lithium ion battery anode slurry dispersing auxiliary in claim 1, wherein the dispersing auxiliary is matched with conductive slurry of a carbon tube system to obtain the lithium ion battery anode slurry.
7. The use of a lithium ion battery positive electrode slurry dispersion aid according to claim 1, wherein the lithium ion battery positive electrode slurry comprises the following solid components in percentage by mass: liFePO 4
95 to 99 weight percent, 0.3 to 1.0 weight percent of conductive carbon black, 0.8 to 2.5 weight percent of conductive slurry, 1.5 to 2.5 weight percent of polyvinylidene fluoride and 0.1 to 0.5 weight percent of dispersing auxiliary agent.
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CN117659331B (en) * | 2024-01-31 | 2024-04-05 | 江苏一特新材料有限责任公司 | Preparation method of three-dimensional network anti-cracking dispersion material and preparation method of positive electrode plate |
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