CN112768638A - Water-based positive electrode slurry and preparation method thereof - Google Patents
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- H—ELECTRICITY
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- 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
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H—ELECTRICITY
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- 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
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- 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
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- 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 provides aqueous anode slurry and a preparation method thereof, wherein the preparation method comprises the following steps: (1) mixing 2-5 parts of aqueous binder, 0.5-1 part of aqueous thickener and 60-70 parts of deionized water, stirring at a low speed for 30min, and stirring at a high speed for 30-60 min; (2) adding 2-5 parts of a conductive agent, and stirring at a high speed; (3) adding 92-95 parts of lithium iron phosphate powder, and stirring at a low speed for 30 min; (4) adding zirconium beads with the diameter of phi 6.5mm, stirring at a low speed for 5-10 min, and then dispersing at a high speed; (5) adding deionized water to adjust viscosity, and controlling the viscosity of the slurry to be 4500-8000 mpa & s; (6) defoaming, filtering to separate zirconium beads, and slowly stirring the obtained slurry to obtain the aqueous anode slurry. The aqueous slurry obtained by the method is uniformly dispersed, does not generate gel, and has uniform particles, good stability, strong fluidity and difficult sedimentation.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to aqueous anode slurry in a lithium ion battery and a preparation method thereof.
Background
Compared with lead-acid batteries, nickel-metal hydride batteries and nickel-cadmium batteries, lithium ion batteries have the advantages of higher energy density, small self-discharge, long cycle life and the like, and are widely applied to the fields of consumer electronics and power batteries at present. At present, the anode slurry of the lithium ion battery generally adopts fluorine-containing polymer such as PVDF (polyvinylidene fluoride) as a binder and NMP (N-methyl pyrrolidone) as a solvent, and adopts an oily slurry stirring system for production, and the production process is divided into a dry stirring process and a wet stirring process due to the difference of the processes. The dry stirring method mainly comprises the steps of uniformly mixing and stirring main materials of lithium iron phosphate, conductive carbon and PVDF, gradually adding a solvent NMP for dispersing and viscosity adjusting, and finally stabilizing the viscosity and the solid content to meet the requirements of the production process. The wet stirring is to mix the binder and solvent NMP to prepare glue solution, mix the main material with conductive agent and solvent NMP to prepare liquid material, and mix and stir the two to prepare slurry. However, the oily positive electrode slurry uses NMP as a solvent, and has the following disadvantages: firstly, the price of NMP rises quickly at present, and the production cost of the slurry is high; secondly, the NMP water absorption of the oily slurry is strong, the requirements on the environmental humidity in the slurry stirring and coating processes are high, and the cost of accessory facilities is high; thirdly, the slurry is coated on the pole piece, and waste gas is generated in the drying process, so that the environmental pollution and the harm to human bodies are caused. Therefore, research and development have been made on an aqueous positive electrode binder system for avoiding environmental pollution and reducing production costs caused by the use of an oily slurry.
The aqueous anode slurry is prepared by replacing the type of a binder with a water-based binder and replacing NMP (N-methyl pyrrolidone) as a solvent with deionized water in a water-based system. However, in a water system, the nano lithium iron phosphate is extremely difficult to disperse, nanoparticles are easy to agglomerate, the prepared slurry is easy to layer, the dispersion characteristic is poor, the slurry is easy to settle and gel, the fluidity and stability of the slurry are poor, the process difficulty of the slurry mixing and coating process is high, and the application of the nano lithium iron phosphate cathode material in the water system adhesive system is greatly limited. Meanwhile, in the existing aqueous anode slurry system, the flexibility of the pole piece prepared from the slurry is not high due to the characteristics of the product formula and the preparation process, and the practical application of the pole piece prepared from the slurry has certain limitation. However, this mode also has problems of easy sedimentation, easy gelation during stirring, and the like.
Therefore, how to provide a method for preparing an aqueous cathode slurry to avoid the disadvantages of the existing production process is a technical problem to be solved in the present invention.
Disclosure of Invention
The present invention is directed to solving the above problems, and an object of the present invention is to provide an aqueous positive electrode slurry and a method for preparing the same. The aqueous slurry obtained by the preparation method provided by the invention has the advantages of uniform dispersion, no occurrence of gel, uniform particles, good stability, strong fluidity and difficult sedimentation.
One of the purposes of the invention is to provide a preparation method of aqueous positive electrode slurry, which comprises the following steps:
(1) mixing 2-5 parts of aqueous binder, 0.5-1 part of aqueous thickener and 60-70 parts of deionized water in parts by weight, stirring at a low speed for 30min, scraping the wall of the wall-sticking object, and then stirring at a high speed for 30-60 min to form a glue solution A;
(2) adding 2-5 parts of a conductive agent into the glue solution A, and stirring at a high speed to form a glue solution B;
(3) adding 92-95 parts of lithium iron phosphate powder into the glue solution B for three times, wherein the three times of adding amount sequentially account for 50%, 30% and 20% of the total amount of the lithium iron phosphate, and stirring at a low speed for 30min after adding the lithium iron phosphate each time to form a glue solution C;
(4) adding a certain amount of zirconium beads into the glue solution C, wherein the diameter of the zirconium beads is phi 6.5mm, stirring at a low speed for 5-10 min to disperse the zirconium beads in the slurry, and then dispersing at a high speed to obtain a glue solution D;
(5) adding deionized water into the glue solution D to adjust the viscosity, and controlling the viscosity of the slurry to be 4500-8000 mpa & s;
(6) and (5) defoaming the slurry obtained in the step (5), filtering to separate zirconium beads, and slowly stirring the slurry obtained by filtering to obtain the aqueous anode slurry.
Further, the aqueous binder in step (1) includes at least one of SBR (styrene butadiene emulsion), PTFE (polytetrafluoroethylene emulsion), PAA (polyacrylate).
Further, the aqueous thickener in step (1) comprises at least one of lithium carboxymethyl cellulose, sodium carboxymethyl cellulose and potassium carboxymethyl cellulose.
Further, the conductive agent in the step (2) includes at least one of graphene, conductive carbon black, conductive graphite, and carbon nanotubes.
Further, the deionized water has the conductivity of less than 2 mu s/cm.
Further, the zirconium beads are TZP zirconium beads with the density of 6.0g/cm3。
Further, the rotation speed of the low-speed stirring in the step (1) is as follows: the revolution speed is 8-12 r/min, the dispersion speed is 500-800 r/min, and the high-speed stirring rotating speed is as follows: the revolution speed is 28-35 r/min, and the dispersion speed is 2500-3500 r/min.
Further, the rotation speed of the high-speed stirring in the step (2) is as follows: the revolution speed is 28-35 r/min, the dispersion speed is 2500-3500 r/min, and the stirring time is 60-120 min.
Further, the rotation speed of the low-speed stirring in the step (3) is as follows: the revolution speed is 8 to 12r/min, and the dispersion speed is 500 to 800 r/min.
Further, the rotation speed of the low-speed stirring in the step (4) is as follows: the revolution speed is 8-12 r/min, and the dispersion speed is 500-800 r/min; the rotating speed of the high-speed dispersion is as follows: the revolution speed is 28-35 r/min, the dispersion speed is 2500-3500 r/min, and the dispersion time is 200-250 min.
Further, the conditions of the defoaming treatment in the step (6) are as follows: the vacuum degree is-0.08 to-0.09 MPa, and the stirring speed is as follows: the revolution speed is 8-12 r/min, the dispersion speed is 500-800 r/min, and the stirring treatment time is 20 min.
Further, in the step (6), the filtering is performed by adopting a filter screen of 180-200 meshes.
The invention also aims to provide the aqueous positive electrode slurry prepared by the method.
The invention has the following beneficial effects:
(1) the invention provides a water-based anode slurry, which adopts a water-based binder and a water solvent, and avoids the problems of high environmental requirement, difficult control of water content, high cost, large loss and the like caused by taking PVDF binder (oily) and NMP as solvents;
(2) according to the preparation method of the water-based anode slurry, zirconium beads with special sizes are used as grinding dispersion media of the glue solution and the main material, so that the main material and the binder are combined more uniformly and are not easy to gel;
(3) the slurry obtained by the invention has uniform particles, good stability and difficult sedimentation.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is described in detail below with reference to the following embodiments, and it should be noted that the following embodiments are only for explaining and illustrating the present invention and are not intended to limit the present invention. The invention is not limited to the embodiments described above, but rather, may be modified within the scope of the invention.
Example 1
A preparation method of aqueous cathode slurry comprises the following steps:
(1) mixing 2 parts of aqueous binder, 0.5 part of aqueous thickening agent and 60 parts of deionized water (the conductivity is less than 2 mu s/cm) according to the parts by weight, stirring at a low speed for 30min, wherein the rotating speed is as follows: revolution speed is 8r/min, dispersion speed is 500r/min, after wall-sticking objects are scraped, high-speed stirring is carried out for 30min, and the rotating speed is as follows: the revolution speed is 28r/min, the dispersion speed is 2500r/min, and glue solution A is formed;
(2) adding 2 parts of conductive agent into the glue solution A, and stirring at a high speed at the following rotation speed: the revolution speed is 28r/min, the dispersion speed is 2500r/min, and the stirring time is 60min, so as to form glue solution B;
(3) and adding 92 parts of lithium iron phosphate powder into the glue solution B for three times, wherein the three times of adding amount sequentially account for 50%, 30% and 20% of the total amount of the lithium iron phosphate, and stirring at a low speed for 30min after adding the lithium iron phosphate each time, wherein the rotating speed is as follows: the revolution speed is 8r/min, the dispersion speed is 500r/min, and glue solution C is formed;
(4) adding a certain amount of zirconium beads into the glue solution C, wherein the zirconium beads are TZP zirconium beads and have the density of 6.0g/cm3The diameter is phi 6.5mm, the mixture is stirred for 5min at a low speed, and the rotating speed is as follows: the revolution speed is 8r/min, the dispersion speed is 500r/min, so that the zirconium beads are dispersed in the slurryInside, high-speed dispersion is carried out again, and the rotational speed is: the revolution speed is 28r/min, the dispersion speed is 2500r/min, and the dispersion time is 200min, so as to obtain glue solution D;
(5) adding deionized water (the conductivity is less than 2 mu s/cm) into the glue solution D to adjust the viscosity, and controlling the viscosity of the slurry to be 5500-6000mpa & s;
(6) stirring the slurry obtained in the step (5) at the vacuum degree of-0.08 MPa at the stirring speed of: and (3) stirring for 20min at the revolution speed of 8r/min and the dispersion speed of 500r/min, defoaming, filtering by using a 180-mesh filter screen to separate zirconium beads, and slowly stirring the slurry obtained by filtering to obtain the aqueous anode slurry.
Wherein the aqueous binder is styrene-butadiene emulsion; the aqueous thickening agent is sodium carboxymethyl cellulose; the conductive agent is conductive carbon black.
Example 2
A preparation method of aqueous cathode slurry comprises the following steps:
(1) mixing 5 parts of aqueous binder, 1 part of aqueous thickening agent and 70 parts of deionized water (the conductivity is less than 2 mu s/cm) according to the parts by weight, stirring at a low speed for 30min, wherein the rotating speed is as follows: revolution is carried out at 12r/min, dispersion is carried out at 800r/min, wall-sticking objects are scraped, high-speed stirring is carried out for 60min, and the rotating speed is as follows: revolution is carried out for 35r/min, dispersion is carried out for 3500r/min, and glue solution A is formed;
(2) adding 5 parts of conductive agent into the glue solution A, and stirring at a high speed at the following rotation speed: revolution is carried out at 35r/min, dispersion is carried out at 3500r/min, and stirring time is 120min, thus forming glue solution B;
(3) and adding 95 parts of lithium iron phosphate powder into the glue solution B for three times, wherein the three times of adding amount sequentially account for 50%, 30% and 20% of the total amount of the lithium iron phosphate, and stirring at a low speed for 30min after adding the lithium iron phosphate each time, wherein the rotating speed is as follows: revolution is carried out for 12r/min, dispersion is carried out for 800r/min, and glue solution C is formed;
(4) adding a certain amount of zirconium beads into the glue solution C, wherein the zirconium beads are TZP zirconium beads and have the density of 6.0g/cm3The diameter is phi 6.5mm, the mixture is stirred for 10min at low speed, and the rotating speed is as follows: revolution is carried out at 12r/min, dispersion is carried out at 800r/min, zirconium beads are dispersed in the slurry, and then high-speed dispersion is carried out, wherein the rotating speed is as follows: revolution is carried out at 35r/min, dispersion is carried out at 3500r/min, and dispersion time is 250min, so as to obtain glue solution D;
(5) adding deionized water (the conductivity is less than 2 mu s/cm) into the glue solution D to adjust the viscosity, and controlling the viscosity of the slurry to be 4500-5000 mpa.s;
(6) stirring the slurry obtained in the step (5) at the vacuum degree of-0.09 MPa at the stirring speed: revolution is carried out for 12r/min, dispersion is carried out for 800r/min, stirring treatment is carried out for 20min, defoaming is carried out, then a 180-mesh filter screen is adopted for filtering and separating out zirconium beads, and slurry obtained by filtering is slowly stirred, so that the water-based anode slurry is obtained.
Wherein the aqueous binder is polytetrafluoroethylene emulsion; the aqueous thickening agent is carboxymethyl cellulose potassium; the conductive agent is conductive graphite.
Example 3
A preparation method of aqueous cathode slurry comprises the following steps:
(1) mixing 4 parts of aqueous binder, 0.8 part of aqueous thickening agent and 65 parts of deionized water (the conductivity is less than 2 mu s/cm) according to the parts by weight, stirring at a low speed for 30min, wherein the rotating speed is as follows: revolution is carried out for 10r/min, dispersion is carried out for 600r/min, after wall-sticking objects are scraped, high-speed stirring is carried out for 45min, and the rotating speed is as follows: revolution is carried out for 32r/min, dispersion is carried out for 3000r/min, and glue solution A is formed;
(2) adding 3 parts of conductive agent into the glue solution A, and stirring at a high speed at the rotating speed of: revolution is carried out at 32r/min, dispersion is carried out at 3000r/min, and stirring time is 100min, so as to form glue solution B;
(3) adding 94 parts of lithium iron phosphate powder into the glue solution B for three times, wherein the three times of adding amount are respectively 50%, 30% and 20% of the total amount of the lithium iron phosphate, and stirring at a low speed for 30min after adding the lithium iron phosphate each time, wherein the rotating speed is as follows: revolution is carried out for 10r/min, dispersion is carried out for 600r/min, and glue solution C is formed;
(4) adding a certain amount of zirconium beads into the glue solution C, wherein the zirconium beads are TZP zirconium beads and have the density of 6.0g/cm3The diameter is phi 6.5mm, the stirring is carried out for 8min at a low speed, and the rotating speed is as follows: revolution is carried out for 10r/min, dispersion is carried out for 600r/min, zirconium beads are dispersed in the slurry, and then high-speed dispersion is carried out, wherein the rotating speed is as follows: revolution is carried out at 32r/min, dispersion is carried out at 3000r/min, and dispersion time is 220min, so as to obtain glue solution D;
(5) adding deionized water (the conductivity is less than 2 mu s/cm) into the glue solution D to adjust the viscosity, and controlling the viscosity of the slurry to 7000-and 8000-mpa.s;
(6) stirring the slurry obtained in the step (5) at the vacuum degree of-0.09 MPa at the stirring speed: revolution is carried out for 10r/min, dispersion is carried out for 600r/min, stirring treatment is carried out for 20min, defoaming is carried out, then a filter screen with 200 meshes is adopted for filtering and separating out zirconium beads, and slurry obtained by filtering is slowly stirred, so that the water-based anode slurry is obtained.
Wherein the water-based binder is polyacrylate; the aqueous thickener is lithium carboxymethyl cellulose; the conductive agent is graphene.
Comparative example 1
The slurry was prepared directly according to the method of example 1, wherein the steps of adding zirconium beads and separating the zirconium beads were not employed, and other conditions were not changed.
Comparative example 2
The slurry was prepared according to the method of example 1, wherein the diameter of the zirconium beads added in step (4) was Φ 3mm, and the other conditions were not changed.
Comparative example 3
The slurry was prepared according to the method of example 1, wherein the diameter of the zirconium beads added in step (4) was Φ 10mm, and the other conditions were not changed.
Comparative example 4
The slurry preparation was carried out according to the method of example 1, wherein in step (4), instead of adding zirconium beads, zirconium beads were optionally added in step (6), and after defoaming treatment, zirconium beads were separated.
Examples of the experiments
The slurries obtained in examples 1 to 3 and comparative examples 1 to 4 were subjected to the performance test, and the results are shown in Table 1.
TABLE 1
As can be seen from table 1, only under the preparation process of the corresponding embodiment of the present invention, the obtained aqueous cathode slurry has the best properties, good and continuous fluidity, high filtration speed, no agglomeration, no gelation, and good stability. The process of example 1 is changed, and the process of comparative examples 1 to 4 is adopted to prepare the slurry, so that the obtained slurry has poor flowability, long filtering time or a small amount of agglomeration, and the equivalent effect in the example cannot be realized.
Claims (10)
1. A preparation method of aqueous positive electrode slurry is characterized by comprising the following steps:
(1) mixing 2-5 parts of aqueous binder, 0.5-1 part of aqueous thickener and 60-70 parts of deionized water in parts by weight, stirring at a low speed for 30min, scraping the wall of the wall-sticking object, and then stirring at a high speed for 30-60 min to form a glue solution A;
(2) adding 2-5 parts of a conductive agent into the glue solution A, and stirring at a high speed to form a glue solution B;
(3) adding 92-95 parts of lithium iron phosphate powder into the glue solution B for three times, wherein the three times of adding amount sequentially account for 50%, 30% and 20% of the total amount of the lithium iron phosphate, and stirring at a low speed for 30min after adding the lithium iron phosphate each time to form a glue solution C;
(4) adding a certain amount of zirconium beads into the glue solution C, wherein the diameter of the zirconium beads is phi 6.5mm, stirring at a low speed for 5-10 min to disperse the zirconium beads in the slurry, and then dispersing at a high speed to obtain a glue solution D;
(5) adding deionized water into the glue solution D to adjust the viscosity, and controlling the viscosity of the slurry to be 4500-8000 mpa & s;
(6) and (5) defoaming the slurry obtained in the step (5), filtering to separate zirconium beads, and slowly stirring the slurry obtained by filtering to obtain the aqueous anode slurry.
2. The method according to claim 1, wherein the aqueous binder in step (1) comprises at least one of styrene-butadiene emulsion, polytetrafluoroethylene emulsion, and polyacrylate; the aqueous thickening agent comprises at least one of lithium carboxymethyl cellulose, sodium carboxymethyl cellulose and potassium carboxymethyl cellulose; the conductive agent in the step (2) comprises at least one of graphene, conductive carbon black, conductive graphite and carbon nano tubes.
3. The method according to claim 1, wherein the rotation speed of the low-speed stirring in the step (1) is: the revolution speed is 8-12 r/min, the dispersion speed is 500-800 r/min, and the high-speed stirring rotating speed is as follows: the revolution speed is 28-35 r/min, and the dispersion speed is 2500-3500 r/min.
4. The method according to claim 1, wherein the high-speed stirring in the step (2) is performed at a rotation speed of: the revolution speed is 28-35 r/min, the dispersion speed is 2500-3500 r/min, and the stirring time is 60-120 min; the rotating speed of the low-speed stirring in the step (3) is as follows: the revolution speed is 8 to 12r/min, and the dispersion speed is 500 to 800 r/min.
5. The method according to claim 1, wherein the rotation speed of the low-speed stirring in the step (4) is: the revolution speed is 8-12 r/min, and the dispersion speed is 500-800 r/min; the rotating speed of the high-speed dispersion is as follows: the revolution speed is 28-35 r/min, the dispersion speed is 2500-3500 r/min, and the dispersion time is 200-250 min.
6. The process according to claim 1, wherein the zirconium beads in step (4) are TZP zirconium beads having a density of 6.0g/cm3。
7. The method according to claim 1, wherein the deionized water added in the steps (1) and (5) is deionized water having an electric conductivity of < 2 μ s/cm.
8. The production method according to claim 1, wherein the conditions of the defoaming treatment in the step (6) are: the vacuum degree is-0.08 to-0.09 MPa, and the stirring speed is as follows: the revolution speed is 8-12 r/min, the dispersion speed is 500-800 r/min, and the stirring treatment time is 20 min.
9. The preparation method according to claim 1, wherein the filtering in the step (6) is filtering with a 180-200 mesh filter screen.
10. An aqueous positive electrode slurry prepared by the method of any one of claims 1 to 9.
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| CN112768638B (en) | 2022-02-22 |
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