CN114843516B - Dispersing agent for lithium ion battery anode slurry - Google Patents

Dispersing agent for lithium ion battery anode slurry Download PDF

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CN114843516B
CN114843516B CN202210526719.3A CN202210526719A CN114843516B CN 114843516 B CN114843516 B CN 114843516B CN 202210526719 A CN202210526719 A CN 202210526719A CN 114843516 B CN114843516 B CN 114843516B
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positive electrode
electrode slurry
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dispersing agent
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CN114843516A (en
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齐文刚
王永鹤
李文龙
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Jiangsu Yite New Materials Co ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
    • H01M4/623—Binders being polymers fluorinated polymers
    • 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
    • H01M4/624—Electric conductive 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a dispersing agent for lithium battery positive electrode slurry. Based on 100 weight percent of the total weight of the dispersing agent, the dispersing agent comprises 5-15 weight percent of A component, 15-60 weight percent of polyether polyurethane containing comb structures, 0.01-1 weight percent of B component, 0.001-0.1 weight percent of C component and the balance of organic solvent. Compared with the prior art, when the solid content in the positive electrode slurry is equal, the positive electrode slurry has smaller viscosity, and when the viscosity of the positive electrode slurry is equal, the positive electrode slurry has higher solid content, and the uniform dispersion of the positive electrode slurry can be realized by using relatively less solvent; in addition, the positive electrode slurry obtained by dispersing the dispersing agent can effectively overcome the problems of wrinkling, breakage or foil scratching after being coated, has good flexibility, and can effectively improve the viscosity by adding the dispersing agent into the mixed slurry containing the commercial binder.

Description

Dispersing agent for lithium ion battery anode slurry
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a dispersing agent for positive electrode slurry of a lithium ion battery.
Background
The lithium ion battery is a high and new technology product, and compared with nickel-cadmium and nickel-hydrogen batteries, the lithium ion battery has the advantages of high voltage, large specific energy, long cycle life, good safety performance, small self-discharge, no memory effect, rapid charge and discharge, wide working temperature range and the like. The lithium iron phosphate lithium ion battery is widely developed and applied to electric tools, energy storage and electric automobiles.
The traditional lithium iron phosphate electrode mainly comprises a current collector and an electrode material attached to the current collector, wherein the current collector is aluminum, and an electrode material layer mainly comprises an active substance, a conductive additive and a binder, and the preparation method is as follows: adding lithium iron phosphate, a binder and a conductive agent into an organic solvent, uniformly stirring to prepare electrode slurry, coating the electrode slurry on an aluminum foil by an extrusion coating or transfer coating method, and drying and cold pressing to obtain the lithium iron phosphate electrode.
For lithium iron phosphate with larger granularity (more than micron level), the electrode is prepared by adopting the method, so that the lithium iron phosphate can be uniformly dispersed, and the whole electrode has better conductivity. However, for the nano-sized lithium iron phosphate material, the nano-sized lithium iron phosphate particles are more than the micro-sized lithium iron phosphate particles under the same weight, the dispersion is more difficult, and the same amount of the conductive agent (the same amount as the conductive agent used in the electrode prepared by the micro-sized lithium iron phosphate) cannot form good conductive effect among the nano-sized lithium iron phosphate particles, and the increase of the amount of the conductive agent correspondingly reduces the amount of the active substance (namely the lithium iron phosphate), thereby reducing the capacity density of the lithium iron phosphate battery.
For improving the battery capacity, there are generally two methods: firstly, the specific capacity of the electrode active material is improved; and secondly, the proportion of the electrode active material in the electrode material is increased, namely, the content of other substances such as a binder, a conductive agent and the like is reduced, or the solid content of the electrode material is increased, and the use amount of a solvent is reduced. The specific capacity of the electrode active material is a characteristic of the electrode active material itself, and improvement of the specific capacity of the electrode active material can be achieved by improving the electrode active material, and the method often has higher requirements on technology. The current common method is to reduce the amount of solvent used by reducing the content of conductive agent in the electrode material, increasing the content of electrode active material or increasing the solid content of the electrode material. The increase of the solid content and the decrease of the solvent amount of the electrode material tend to increase the viscosity of the electrode material, so that the fluidity of the electrode slurry is reduced, and the electric performance is reduced. How to balance the relationship between the two, so as to effectively improve the battery capacity is a problem to be solved in the field.
How to solve the above problems in the prior art is a problem to be solved by the person skilled in the art.
Disclosure of Invention
The invention aims to: the invention aims to provide a dispersing agent for positive electrode slurry of a lithium ion battery, which ensures that the positive electrode slurry prepared by the dispersing agent has higher solid content, smaller viscosity, even dispersion when using less solvent, better flexibility and capability of overcoming the problems of wrinkling, broken tape or scratch foil leakage after coating.
The technical scheme is as follows: in order to solve the problems in the prior art, the invention provides a dispersing agent for lithium ion battery anode slurry, which comprises the following components in percentage by weight based on 100 weight percent: 5 to 15wt% (e.g., 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15 wt%) of component A, 15 to 60wt% (e.g., 15wt%, 17wt%, 18wt%, 20wt%, 22wt%, 24wt%, 25wt%, 26wt%, 28wt%, 30wt%, 32wt%, 34wt%, 35wt%, 36wt%, 38wt%, 40wt%, 42wt%, 44wt%, 45wt%, 46wt%, 48wt%, 50wt%, 52wt%, 54wt%, 56wt%, 58wt%, 60 wt%) of polyether-type polyurethane containing comb structure, polyurethane 0.01 to 1wt% (e.g., 0.01wt%, 0.05wt%, 0.1wt%, 0.12wt%, 0.14wt%, 0.16wt%, 0.18wt%, 0.2wt%, 0.25wt%, 0.3wt%, 0.35wt%, 0.4wt%, 0.45wt%, 0.5wt%, 0.55wt%, 0.6wt%, 0.65wt%, 0.7wt%, 0.75wt%, 0.8wt%, 0.85wt%, 0.9wt%, 0.95wt%, 1 wt%) of the B component, 0.001 to 0.1wt% (e.g., 0.001wt%, 0.004wt%, 0.006wt%, 0.008wt%, 0.01wt%, 0.05wt%, 0.1 wt%) of the C component, the balance of the organic solvent is organic solvent,
wherein,
the component A is one or a combination of at least two of polyvinylpyrrolidone, polyacrylamide, hydroxyethyl cellulose and polyoxyethylene copolymer;
the component B is one or a combination of at least two of hexamethylenediamine, tertiary amine and ethanolamine; and
the component C is selected from one or a combination of at least two of polysiloxane, polyether compound and modified organosilicon.
In some embodiments of the invention, the a-component is preferably polyvinylpyrrolidone.
In some embodiments of the invention, the polyether urethanes containing comb structures are compounds of formula I:
wherein,
n represents an integer of 0 to 100 (e.g., 0, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 12, 14, 16, 18, 20, 22, 24, 26, 28, 30, 32, 34, 36, 38, 40, 42, 44, 46, 48, 50, 52, 54, 56, 58, 60, 62, 64, 66, 68, 70, 72, 74, 76, 78, 80, 82, 84, 86, 88, 90, 92, 94, 96, 98, 100);
A 1 represents an H atom, an alkyl group having 1 to 5 (e.g., 1, 2, 3, 4, 5) carbon atoms, an alkoxy group having 1 to 4 (e.g., 1, 2, 3, 4) carbon atoms, or an alkenyl group having 2 to 5 (e.g., 2, 3, 4, 5) carbon atoms;
A 2 representation of
A 3 Representation of
X 1 、X 2 And X 3 Each independently represents
* Representing the attachment site in the bonded structure.
The polyurethane compound shown in the general formula I has a comb-shaped structure, the tail end of the polyurethane compound is a multi-branched structure formed by polytetrahydrofuran and polyethylene glycol block copolymer, so that space resistance for further condensation among solid particles is formed, in addition, the polar structure of the polyurethane compound has stronger affinity with a solvent, and the wetting degree of the solid particles by the solvent is increased. When the composite material is used as a dispersing agent to be applied to positive electrode slurry after being combined with the component A, the component B and the component C, the composite material can play a good role in dispersing, greatly reduce the viscosity of the positive electrode slurry, improve the uniformity and flexibility of the positive electrode slurry during coating, and avoid the problems of wrinkling, breakage and foil leakage during coating.
In some embodiments of the invention, the B component is preferably ethanolamine.
In some embodiments of the invention, the C component is preferably a polysiloxane.
In some embodiments of the present invention, in the dispersant, the organic solvent is selected from one or a combination of at least two of N-methylpyrrolidone, dimethyl carbonate, diethyl carbonate, ethyl acetate, methyl propionate, preferably the organic solvent is N-methylpyrrolidone.
In some embodiments of the present invention, a dispersant for a lithium ion battery positive electrode slurry comprises, based on 100wt% total weight, the following components: 5 to 15 weight percent of polyvinylpyrrolidone, 15 to 60 weight percent of polyether polyurethane containing comb structures, 0.01 to 1 weight percent of ethanolamine, 0.001 to 0.1 weight percent of polysiloxane and the balance of organic solvent.
In some embodiments of the present invention, a dispersant for a lithium ion battery positive electrode slurry comprises, based on 100wt% total weight, the following components: 5 to 15 weight percent of polyvinylpyrrolidone, 15 to 60 weight percent of polyether polyurethane with comb-shaped structure shown in the general formula I, 0.01 to 1 weight percent of ethanolamine, 0.001 to 0.1 weight percent of polysiloxane and the balance of organic solvent:
wherein,
n represents 0 to 100;
A 1 represents an H atom, an alkyl group having 1 to 5 carbon atoms, an alkoxy group having 1 to 4 carbon atoms, or an alkenyl group having 2 to 5 carbon atoms;
A 2 representation of
A 3 Representation of
X 1 、X 2 And X 3 Each independently represents
* Representing the carbon atoms in the bonded structure.
In some embodiments of the invention, A 2 Representation of
In some embodiments of the invention, X 1 、X 2 And X 3 Each independently represents
In another aspect, the present invention provides a positive electrode slurry comprising the dispersant of the present invention, which is formed by mixing a solid dry material and an organic solvent.
In some embodiments of the present invention, the total weight is 100wt%, the solid dry material in the positive electrode slurry includes 85 to 98wt% (e.g., 85wt%, 86wt%, 87wt%, 88wt%, 89wt%, 90wt%, 91wt%, 92wt%, 93wt%, 94wt%, 95wt%, 96wt%, 97wt%, 98 wt%) of lithium iron phosphate, 0.5 to 8wt% (e.g., 0.5wt%, 0.8wt%, 1wt%, 1.5wt%, 2wt%, 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt%, 5wt%, 5.5wt%, 6wt%, 6.5wt%, 7wt%, 7.5wt%, 8 wt%) of a conductive agent, and 0.1 to 1wt% (e.g., 0.1wt% >, 0.1 wt%; 0.12wt%, 0.14wt%, 0.16wt%, 0.18wt%, 0.2wt%, 0.25wt%, 0.3wt%, 0.35wt%, 0.4wt%, 0.45wt%, 0.5wt%, 0.55wt%, 0.6wt%, 0.65wt%, 0.7wt%, 0.75wt%, 0.8wt%, 0.85wt%, 0.9wt%, 0.95wt%, 1 wt%) of a dispersant, and 1 to 8wt% (e.g., 1wt%, 1.5wt%, 2wt%, 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5wt%, 5wt%, 5.5wt%, 6wt%, 6.5wt%, 7wt%, 7.5wt%, 8 wt%) of a binder.
In some embodiments of the invention, the weight of the organic solvent in the positive electrode slurry is 35 to 50wt% (e.g., 35wt%, 36wt%, 37wt%, 38wt%, 39wt%, 40wt%, 41wt%, 42wt%, 43wt%, 44wt%, 45wt%, 46wt%, 47wt%, 48wt%, 49wt%, 50 wt%) of the total weight of the positive electrode slurry.
In the present invention, the higher the solid content in the positive electrode slurry, the more advantageous the improvement in battery capacity. When the dispersing agent is applied to the positive electrode slurry, the dispersing agent can ensure high solid content and lower viscosity, and can overcome the problems of wrinkling, belt breakage or scratch foil leakage after being coated, thus being suitable for industrial use.
In some embodiments of the invention, the conductive agent is selected from one or a combination of at least two of a graphite conductive agent, conductive carbon black, graphene and metal powder, preferably the graphite conductive agent is selected from one or a combination of at least two of KS-6, KS-15, SFG-6, SFG-15, preferably the conductive carbon black comprises one or a combination of at least two of acetylene black, super P, super S, 350G, carbon fiber, carbon nanotube, ketjen black, activated carbon, preferably the metal powder is selected from one or a combination of at least two of zinc powder, copper powder, aluminum powder, silver powder, gold powder, tungsten powder, tin powder.
In some embodiments of the invention, the binder is selected from one or a combination of at least two of polyvinylidene fluoride, sodium carboxymethyl cellulose, styrene-butadiene rubber, sodium alginate, polyacrylic acid, and polyethylene oxide.
In some embodiments of the invention, the binder is selected from polyvinylidene fluoride having a molecular weight of 60 to 100 tens of thousands.
In some embodiments of the present invention, in the positive electrode slurry, the organic solvent is selected from one or a combination of at least two of N-methylpyrrolidone, dimethyl carbonate, diethyl carbonate, ethyl acetate, methyl propionate, preferably N-methylpyrrolidone.
In the present invention, the positive electrode slurry may be uniformly dispersed by uniformly mixing lithium iron phosphate, a conductive agent, a dispersing agent, and a binder in a solvent, by stirring and/or ultrasonic dispersion. The stirring may be conventional mechanical stirring, magnetic stirring or stirring with a shear dispersing emulsifying machine. The mixing sequence of the lithium iron phosphate, the conductive agent, the dispersing agent, the binder and the solvent is not particularly limited, and the conductive agent, the binder and the solvent can be uniformly mixed firstly, then the lithium iron phosphate is added, and finally the dispersing agent is added to uniformly mix, or the lithium iron phosphate, the conductive agent and the binder can be uniformly mixed firstly, then the solvent is added, and finally the dispersing agent is added to uniformly mix. The stirring can be primary stirring and secondary stirring, wherein the primary stirring speed is 100-500 rpm, the stirring time is 5-30 min, the secondary stirring speed is more than or equal to 2000 rpm, and the stirring time is 10-300 min.
The beneficial effects are that: compared with the prior art, when the solid content in the positive electrode slurry is equal, the positive electrode slurry has smaller viscosity, and when the viscosity in the positive electrode slurry is equal, the positive electrode slurry has higher solid content and can be prepared in a shorter time, and even dispersion of the positive electrode slurry can be realized by using relatively less solvent, so that the time of a production process is effectively saved, and the production efficiency is improved; in addition, the positive electrode slurry obtained by dispersing the dispersing agent of the invention effectively solves the problems of wrinkling, breakage or scratching foil leakage after being coated, has good flexibility, is suitable for industrial production, and can effectively improve the viscosity by adding the dispersing agent of the invention into the mixed slurry containing the commercial binder.
Detailed Description
The invention will be described below in connection with specific embodiments. The following examples are illustrative of the present invention and are not intended to limit the present invention. Other combinations and various modifications within the spirit of the invention may be made without departing from the spirit or scope of the invention.
The synthetic method of polyether polyurethane with the structure of the general formula I comprises the following steps:
step 1, synthesis of intermediate Z-1:
1mol of isophorone diisocyanate (IPDI) is fully dissolved in 300mL of tetrahydrofuran, 0.5g of dibutyltin dilaurate is added under the nitrogen environment, the temperature is controlled at 30 ℃, 1mol of hydroxyethyl acrylate is dropwise added into a reaction system at a constant speed within 2-3 h, the temperature is controlled at 30 ℃, and the titration method monitors that NCO reaction is complete. Eluting the solvent, dissolving the product in a mixed solvent of n-hexane and anhydrous ethyl acetate (the weight ratio of n-hexane to anhydrous ethyl acetate is 4:1), separating by a column, and performing rotary evaporation to obtain a compound of Z-1.
Step 2, synthesis of intermediate monomer Z-2 compound:
1mol of C-1 compound (purchased from Wanhua chemical group Co., ltd.) was dissolved in 1000mL of anhydrous tetrahydrofuran, 3.1mol of p-isopropylphenyl isocyanate was added, 0.1g of dibutyltin dilaurate was added under nitrogen atmosphere, and the temperature was controlled to 25℃and the completion of NCO reaction was monitored by titration. Eluting the solvent, dissolving the product in a mixed solvent of n-hexane and anhydrous ethyl acetate (the weight ratio of n-hexane to anhydrous ethyl acetate is 4:1), separating by a column, and performing rotary evaporation to obtain a compound of Z-2.
Step 3. Synthesis of the Compound of formula I:
100g Z-1 compound and 1g of azobisisobutyronitrile were sufficiently dissolved in 100g of toluene to obtain a solution to be titrated D. 100g of toluene is added into a reaction bottle, the temperature is controlled to 70 ℃ under stirring, the solution D to be titrated is dripped into the reaction system at a constant speed within 3-4 h, the reaction is carried out for 1h at 70 ℃, and the infrared detection is carried out for 1640cm -1 After the absorption peak disappeared, the reaction was complete to give the compound of Z-3:
controlling the temperature of the system to be 25-35 ℃, adding the compound of Z-2, reacting for 48 hours at room temperature, monitoring the NCO reaction by a titration method to completely react, eluting the solvent to obtain the compound of I-1:
the following examples each use specific amounts of components to prepare a dispersant for positive electrode slurry pertaining to the present invention, and dispersants not listed as falling within the scope of the present invention have the same effect of use.
Example 1
Based on 100 weight percent of the total weight, the dispersing agent comprises 5 weight percent of polyvinylpyrrolidone, 15 weight percent of polyether polyurethane of the formula I-1, 0.08 weight percent of ethanolamine and 0.01 weight percent of polysiloxane which are fully and uniformly mixed in 79.91 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 1 of the embodiment.
Example 2
Based on 100 weight percent of the total weight, the dispersing agent comprises 10 weight percent of polyvinylpyrrolidone, 20 weight percent of polyether polyurethane of the formula I-1, 0.1 weight percent of ethanolamine and 0.02 weight percent of polysiloxane which are fully and uniformly mixed in 69.88 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 2 of the embodiment.
Example 3
Based on 100 weight percent of the total weight, the dispersing agent comprises 15 weight percent of polyvinylpyrrolidone, 35 weight percent of polyether polyurethane of the formula I-1, 0.15 weight percent of ethanolamine and 0.01 weight percent of polysiloxane which are fully and uniformly mixed in 49.84 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 3 of the embodiment.
Example 4
Based on 100 weight percent of the total weight, the dispersing agent comprises 5 weight percent of polyvinylpyrrolidone, 40 weight percent of polyether polyurethane of the formula I-1, 0.1 weight percent of ethanolamine and 0.02 weight percent of polysiloxane which are fully and uniformly mixed in 54.88 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 4 of the embodiment.
Example 5
Based on 100 weight percent of the total weight, the dispersing agent comprises 10 weight percent of polyvinylpyrrolidone, 50 weight percent of polyether polyurethane of the formula I-1, 0.15 weight percent of ethanolamine and 0.01 weight percent of polysiloxane which are fully and uniformly mixed in 39.84 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 5 of the embodiment.
Example 6
Based on 100 weight percent of the total weight, the dispersing agent comprises 15 weight percent of polyvinylpyrrolidone, 60 weight percent of polyether polyurethane of the formula I-1, 0.1 weight percent of ethanolamine and 0.02 weight percent of polysiloxane which are fully and uniformly mixed in 24.88 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 6 of the embodiment.
Example 7
Based on 100 weight percent of the total weight, the dispersing agent comprises 5 weight percent of polyvinylpyrrolidone, 25 weight percent of polyether polyurethane of the formula I-1, 0.2 weight percent of ethanolamine and 0.01 weight percent of polysiloxane which are fully and uniformly mixed in 69.79 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 7 of the embodiment.
Example 8
Based on 100 weight percent of the total weight, the dispersing agent comprises 10 weight percent of polyvinylpyrrolidone, 30 weight percent of polyether polyurethane of the formula I-1, 0.4 weight percent of ethanolamine and 0.02 weight percent of polysiloxane which are fully and uniformly mixed in 59.58 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 8 of the embodiment.
Example 9
Based on 100 weight percent of the total weight, the dispersing agent comprises 15 weight percent of polyvinylpyrrolidone, 45 weight percent of polyether polyurethane of the formula I-1, 0.5 weight percent of ethanolamine and 0.02 weight percent of polysiloxane which are fully and uniformly mixed in 39.48 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 9 of the embodiment.
Example 10
Based on 100 weight percent of the total weight, the dispersant comprises 10 weight percent of polyacrylamide, 20 weight percent of polyether polyurethane of the formula I-1, 0.1 weight percent of ethanolamine and 0.02 weight percent of polysiloxane which are fully and uniformly mixed in 69.88 weight percent of N-methylpyrrolidone, so as to obtain the dispersant 10 of the embodiment.
Example 11
Based on 100 weight percent of the total weight, the dispersing agent comprises 10 weight percent of polyvinylpyrrolidone, 20 weight percent of polyether polyurethane of the formula I-1, 0.1 weight percent of hexamethylenediamine and 0.02 weight percent of polysiloxane which are fully and uniformly mixed in 69.88 weight percent of N-methylpyrrolidone, so as to obtain the dispersing agent 11 of the embodiment.
Example 12
Based on 100 weight percent of the total weight, the dispersing agent comprises 10 weight percent of polyvinylpyrrolidone, 20 weight percent of polyether polyurethane of the formula I-1, 0.1 weight percent of ethanolamine and 0.02 weight percent of polysiloxane which are fully and uniformly mixed in 69.88 weight percent of dimethyl carbonate, so as to obtain the dispersing agent 12 of the embodiment.
Comparative example 1
Based on 100 weight percent of the total weight, the dispersant comprises 30 weight percent of polyvinylpyrrolidone, 0.1 weight percent of ethanolamine and 0.02 weight percent of polysiloxane which are fully and uniformly mixed in 69.88 weight percent of N-methylpyrrolidone, so as to obtain the dispersant 13 of the comparative example.
To illustrate the dispersing effect of the dispersing agent of the present invention, the dispersing agents prepared in examples 1 to 12 were added to a mixed slurry of a commercially available binder-N-methylpyrrolidone (for example, HSV 900-N-methylpyrrolidone mixed slurry, suwei 5130-N-methylpyrrolidone mixed slurry), the viscosity number of the mixed slurry after the addition of the dispersing agent of the present invention was examined, and whether or not there was a color change was observed.
Wherein the weight ratio of the components in each example is kept consistent, and the weight ratio of the total weight of the binder and the dispersant to the N-methyl pyrrolidone is 1:49.
TABLE 1 viscosity number and color Change detection results
Wherein,
the viscosity detection method comprises the following steps: the sample to be tested is thermostatted for 1h in a thermostatic water bath at 25 ℃ and is detected by using an NDJ-5S digital rotary viscometer, wherein, the rotor: no. 4; rotational speed: 6rpm, detection temperature: 25 ℃.
From the test results shown in table 1, it is apparent that the viscosity of the mixed slurry can be effectively improved when the dispersant of the present invention is added to a commercially available binder-N-methylpyrrolidone mixed slurry, and the viscosity value is greatly improved and the effect is remarkably improved when the component a is preferably polyvinylpyrrolidone, the component B is preferably ethanolamine, and the solvent is preferably N-methylpyrrolidone. In contrast, the dispersant 13 prepared in comparative example 1 was able to slightly improve the viscosity of the commercially available binder-N-methylpyrrolidone mixed slurry, and the effect improvement was not remarkable, and it was found that the dispersant of the present invention had an excellent dispersing effect and was able to remarkably improve the viscosity of the mixed slurry.
The following examples each use specific amounts of components to prepare positive electrode slurries belonging to the present invention, and the positive electrode slurries not listed within the scope of the present invention have the same effect of use.
Example 13
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 41.75wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry matter in the positive electrode slurry comprised 94.75wt% of lithium iron phosphate, 2.5wt% of Super P, 0.15wt% of dispersant 2, and 2.6wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and after adding dispersant 2, the mixture was stirred at 2000 rpm for 70 minutes to obtain positive electrode slurry 1.
Example 14
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 41.9wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry matter in the positive electrode slurry comprised 94.1wt% of lithium iron phosphate, 2.8wt% of Super P, 0.2wt% of dispersant 3, and 2.9wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and after adding dispersant 3, the mixture was stirred at 2000 rpm for 60 minutes to obtain positive electrode slurry 2.
Example 15
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 41.7wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry matter in the positive electrode slurry comprised 93.9wt% of lithium iron phosphate, 2.9wt% of Super P, 0.3wt% of dispersant 4, and 2.9wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and after adding dispersant 4, the mixture was stirred at 2000 rpm for 70 minutes to obtain positive electrode slurry 3.
Example 16
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 41.7wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry material in the positive electrode slurry comprises 93.75wt% of lithium iron phosphate, 3wt% of Super P, 0.25wt% of dispersing agent 5 and 3wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and after adding dispersant 5, the mixture was stirred at 2000 rpm for 70 minutes to obtain positive electrode slurry 4.
Example 17
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 41.75wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry matter in the positive electrode slurry comprised 94.75wt% of lithium iron phosphate, 2.5wt% of Super P, 0.15wt% of dispersant 10, and 2.6wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and after adding dispersant 10, the mixture was stirred at 2000 rpm for 120 minutes to obtain positive electrode slurry 5.
Example 18
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 41.9wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry matter in the positive electrode slurry comprised 94.1wt% of lithium iron phosphate, 2.8wt% of Super P, 0.2wt% of dispersant 11, and 2.9wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and dispersant 11 was added thereto and then stirred at 2000 rpm for 140 minutes to obtain positive electrode slurry 6.
Example 19
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 41.7wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry matter in the positive electrode slurry comprised 93.9wt% of lithium iron phosphate, 2.9wt% of Super P, 0.3wt% of dispersant 12, and 2.9wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and dispersant 12 was added thereto and then stirred at 2000 rpm for 150 minutes, to thereby obtain positive electrode slurry 7.
Example 20
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 37.35wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry matter in the positive electrode slurry comprised 94.1wt% of lithium iron phosphate, 2.8wt% of Super P, 0.2wt% of dispersant 3, and 2.9wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and dispersant 3 was added thereto and then stirred at 2000 rpm for 160 minutes, to thereby obtain positive electrode slurry 8.
Example 21
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 35.8wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry material in the positive electrode slurry included 93.75wt% of lithium iron phosphate, 3wt% of Super P, 0.25wt% of dispersant 4, and 3wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and after the addition of the dispersant 4, the mixture was stirred at 2000 rpm for 170 minutes to obtain a positive electrode slurry 9.
Comparative example 2
The lithium iron phosphate battery positive electrode slurry is formed by mixing solid dry materials and N-methyl pyrrolidone (wherein the weight of the N-methyl pyrrolidone is 41.7wt% of the total weight of the positive electrode slurry). Based on 100 weight percent of the total weight: the solid dry material in the positive electrode slurry included 93.75wt% of lithium iron phosphate, 3wt% of Super P, 0.25wt% of dispersant 13, and 3wt% of polyvinylidene fluoride.
Polyvinylidene fluoride and Super P were stirred in N-methylpyrrolidone at 400 rpm for 20 minutes, lithium iron phosphate was added thereto at 200 rpm for 10 minutes, and the mixture was further added with dispersant 13 and then stirred at 2000 rpm for 270 minutes, whereby positive electrode slurry 10 was obtained.
As can be seen from the comparison of the positive electrode slurries 1 to 9 prepared in examples 13 to 21 with the positive electrode slurry 10 prepared in comparative example 2, the positive electrode slurries prepared by the dispersant of the present invention can be uniformly dispersed using less solvent and can be prepared in a shorter period of time.
The solid content and viscosity of each of the positive electrode slurries 1 to 10 were measured, and the measurement results are shown in table 2.
TABLE 2 solid contents and viscosities of cathode pastes 1 to 10
Wherein,
the method for detecting the solid content comprises the following steps: the percentage of the weight ratio of the sample after being dried at 120 ℃ for 4 hours to the weight ratio of the sample before being dried;
the viscosity detection method comprises the following steps: the sample to be tested is thermostatted for 1h in a thermostatic water bath at 25 ℃ and is detected by using an NDJ-5S digital rotary viscometer, wherein, the rotor: no. 4; rotational speed: 6rpm, detection temperature: 25 ℃.
As is clear from comparison of example 16 and comparative example 2, the positive electrode slurry prepared using the dispersant of the present invention had the same solid content as the positive electrode slurry prepared in comparative example 2, but the positive electrode slurry prepared using the dispersant of example 2 of the present invention had significantly smaller viscosity; as can be seen from the comparison of example 21 and comparative example 2, when the viscosities of the positive electrode slurry prepared by the dispersant of the present invention are comparable to those of the positive electrode slurry prepared by comparative example 2, the positive electrode slurry prepared by the dispersant of the present invention has a relatively high solid content, and uniform dispersion of the positive electrode slurry can be achieved using relatively less solvent.
From the comparison of example 17 with example 13, the comparison of example 18 with example 14, and the comparison of example 19 with example 15, it is understood that the positive electrode slurry prepared according to the present invention has a better viscosity when the a-component is preferably polyvinylpyrrolidone, the B-component is preferably ethanolamine, and the organic solvent is N-methylpyrrolidone.
In summary, compared with the prior art, the positive electrode slurry of the present invention has a smaller viscosity when the solid content in the positive electrode slurry is equal, and has a higher solid content when the viscosity in the positive electrode slurry is equal. Namely, the positive electrode slurry prepared by the dispersing agent has smaller viscosity and higher solid content.
The positive electrode pastes 1 to 10 were coated on the positive electrode sheet, and dried to prepare a positive electrode sheet core, and whether the surface of the core had problems of wrinkles, belt breakage or scratch foil leakage was observed, and the detection results are shown in table 3.
TABLE 3 coating effect detection results
Note that: pass is "v", fail is "x".
As shown in the results of Table 3, the dispersant of the present invention was applied to the positive electrode slurry, and the dispersant had good effect after coating, and had no problems of wrinkling, breakage or scratching and foil leakage, and had good flexibility.
In conclusion, the positive electrode slurry prepared by the dispersing agent has higher solid content and lower viscosity, and can be uniformly dispersed by using relatively less solvent, so that the time of a production process is effectively saved, and the production efficiency is improved; in addition, after the positive electrode slurry obtained by dispersing the dispersing agent is coated, the problems of wrinkling, breakage or foil scratching and foil leakage can be effectively solved, the dispersing agent has good flexibility, the dispersing agent is suitable for industrial production, and the viscosity of the dispersing agent can be effectively improved by adding the dispersing agent into the commercially available adhesive-N-methylpyrrolidone mixed slurry.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and to implement it, but not limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.

Claims (6)

1. The dispersing agent for the lithium ion battery positive electrode slurry is characterized by comprising the following components in percentage by weight based on 100 weight percent: 5 to 15 weight percent of A component, 15 to 60 weight percent of polyether polyurethane containing comb structure, 0.01 to 1 weight percent of B component, 0.001 to 0.1 weight percent of C component, and the balance of organic solvent,
the polyether polyurethane containing the comb structure is a compound shown in a general formula I:
wherein,
the component A is one or a combination of at least two of polyvinylpyrrolidone, polyacrylamide, hydroxyethyl cellulose and polyoxyethylene copolymer;
the component B is selected from one or a combination of at least two of hexamethylenediamine and ethanolamine;
the component C is selected from one or a combination of at least two of polysiloxane, polyether compound and modified organic silicon;
n represents an integer of 0 to 100;
A 1 represents an H atom, an alkyl group having 1 to 5 carbon atoms, or an alkoxy group having 1 to 4 carbon atoms;
A 2 representation of
A 3 Representation of
X 1 、X 2 And X 3 Each independently representsAnd
* Representing the attachment site in the bonded structure.
2. The dispersant for lithium ion battery positive electrode slurry according to claim 1, wherein the polyether polyurethane containing a comb structure is a compound as follows:
3. the dispersant for lithium ion battery positive electrode slurry according to claim 1, wherein the organic solvent is selected from one or a combination of at least two of N-methylpyrrolidone, dimethyl carbonate, diethyl carbonate, ethyl acetate, methyl propionate.
4. A positive electrode slurry of a lithium ion battery comprising the dispersing agent according to any one of claims 1 to 3, wherein the positive electrode slurry is formed by mixing a solid dry material and an organic solvent, and the solid dry material in the positive electrode slurry comprises 85 to 98wt% of lithium iron phosphate, 0.5 to 8wt% of a conductive agent, 0.1 to 1wt% of the dispersing agent and 1 to 8wt% of a binder, based on 100wt% of the total weight of the solid dry material; the weight of the organic solvent is 35-50 wt% of the total weight of the positive electrode slurry.
5. The positive electrode slurry for a lithium ion battery according to claim 4, wherein the conductive agent is selected from one or a combination of at least two of a graphite conductive agent, conductive carbon black, graphene and metal powder.
6. The positive electrode slurry for lithium ion battery according to claim 4, wherein the binder is selected from one or a combination of at least two of polyvinylidene fluoride, sodium carboxymethyl cellulose, styrene-butadiene rubber, sodium alginate, polyacrylic acid and polyethylene oxide.
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