CN112467082A - Production stirring process for negative electrode graphite slurry of lithium ion battery - Google Patents
Production stirring process for negative electrode graphite slurry of lithium ion battery Download PDFInfo
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- CN112467082A CN112467082A CN202011306570.5A CN202011306570A CN112467082A CN 112467082 A CN112467082 A CN 112467082A CN 202011306570 A CN202011306570 A CN 202011306570A CN 112467082 A CN112467082 A CN 112467082A
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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
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- 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
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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
- H01M4/621—Binders
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- 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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Abstract
The invention relates to a production stirring process of graphite slurry of a lithium ion battery cathode, which comprises the following processing steps: (1) processing conductive adhesive, (2) primarily infiltrating graphite, (3) primarily processing viscosity reduction, (4) processing viscosity reduction for the second time, (5) homogenizing slurry, (6) adding styrene butadiene rubber into the homogenized slurry, stirring for 20-40min, and revolving for 25-35RPM (revolution speed) and rotating for 700-900RPM (revolution speed) required by equipment to obtain slurry with viscosity and solid content meeting the process requirements; (7) and (5) defoaming and processing. The stirring process provided by the invention can shorten the stirring time and improve the stirring production efficiency, and the viscosity of the prepared cathode slurry is changed within 48H and is less than 1000 mpa.s; the change in solid content of 48H is less than 0.2%; the prepared slurry production battery cell can meet the requirement that the cycle retention rate is more than 80% after 800 cycles. The invention can improve the production efficiency on the premise of ensuring the quality of the slurry.
Description
Technical Field
The invention relates to a production method of a lithium ion battery, in particular to a production stirring process of graphite slurry of a lithium ion battery cathode.
Background
In the production process of the lithium ion battery at present, slurry is prepared from a negative electrode material through a pulping process, and the slurry is uniformly coated on a copper foil through coating equipment to prepare a lithium ion negative electrode plate. Generally, the lithium ion battery negative electrode material mainly comprises graphite, conductive carbon black, a thickening agent, an adhesive and other components, and pulping is to uniformly mix the materials into liquid slurry with uniform material dispersion and small viscosity change. At present, a wet mixing stirring process is generally used for negative electrode ingredients, slurry has certain fluidity in the stirring process of the wet mixing stirring process, stirring shearing force cannot effectively act on a negative electrode material to influence the dispersion efficiency, the stirring time is generally 6-8H, the pulping efficiency is low, and the pulping stirring process needs to be optimized for improving the pulping efficiency in order to obtain the slurry in an ideal state with uniform dispersion, stable solid content and small slurry viscosity change.
Disclosure of Invention
The invention aims to solve the problems and provides a production and stirring process of graphite slurry for a negative electrode of a lithium ion battery.
The technical scheme adopted by the invention is as follows: a production stirring process for graphite slurry of a lithium ion battery cathode comprises the following processing steps:
(1) processing the conductive adhesive: firstly, dispersing and dissolving sodium carboxymethylcellulose in a solvent by stirring equipment, and stirring for 90-120min to prepare an ideal sodium carboxymethylcellulose glue solution; then adding conductive carbon black into the prepared sodium carboxymethylcellulose glue solution, and stirring for 20-30min under the condition that the vacuum degree is less than or equal to-80 kpa to prepare the conductive adhesive required by pulping;
(2) preliminary infiltration of graphite: adding 100% of graphite, 22-24% of water and 1-2% of N-methyl pyrrolidone into a stirrer, stirring for 40-70min, performing primary infiltration on the graphite by using equipment at the revolution speed of 20-30RPM and the rotation speed of 120-200RPM, and after the infiltration is finished, making the slurry into a semi-dry wet paste;
(3) first viscosity reduction processing: adding the preliminarily infiltrated graphite into conductive adhesive accounting for 20-40% of the added amount of the graphite, stirring in a stirrer at high viscosity for 40-70min, and further uniformly dispersing the graphite at revolution speed of 25-35RPM and rotation speed of 500-20000 mPa.s required by equipment to obtain negative electrode slurry with viscosity of 10000-20000 mPa.s;
(4) second viscosity reduction processing: adding 10-20% of conductive adhesive into the slurry with the first viscosity reduced in the step 3, stirring the slurry in a stirrer for 20-40min at high viscosity, wherein the revolution speed of the equipment is 25-35RPM, and the rotation speed is 1500-2000RPM, so that the viscosity and the solid content are further reduced while the slurry is further dispersed;
(5) homogenizing the slurry: after the viscosity is reduced, 37.5 percent of sodium carboxymethylcellulose and 3 percent of water are added, the mixture is stirred for 50-70min, and the revolution of the equipment is 30-40RPM and the rotation is 1200-1500RPM, so as to obtain homogenized slurry;
(6) adding styrene butadiene rubber into the homogenized slurry, and stirring for 20-40min, wherein the revolution speed of the equipment is 25-35RPM, and the rotation speed of the equipment is 700-900RPM, so as to obtain the slurry with the viscosity and the solid content meeting the process requirements;
(7) defoaming and processing: finally defoaming and stirring for 20-30min under the condition that the vacuum degree is less than or equal to-70 kpa, and revolving (rotating back) at 10RPM required by equipment to prepare the slurry.
In the preparation process of the conductive adhesive, cooling water is required to be communicated with the tank body, and the temperature in the preparation process is controlled to be 21-25 ℃.
In the slurry preparation process, cooling water needs to be communicated with the tank body, and the temperature in the slurry preparation process is controlled to be 21-25 ℃.
The invention has the beneficial effects that: the stirring process provided by the invention can shorten the stirring time and improve the stirring production efficiency, and the viscosity of the prepared cathode slurry is changed within 48H and is less than 1000 mpa.s; the change in solid content of 48H is less than 0.2%; the prepared slurry production battery cell can meet the requirement that the cycle retention rate is more than 80% after 800 cycles. The invention can improve the production efficiency on the premise of ensuring the quality of the slurry.
Drawings
Fig. 1 is a graph showing the cycle life of a battery prepared from the slurry according to the present invention.
FIG. 2 is a graph showing the viscosity of the slurry prepared according to the present invention as a function of time in a static state.
FIG. 3 is a graph showing the change of the solid content with time in the state of standing of the slurry prepared according to the present invention.
Detailed Description
The invention comprises the following processing steps:
(1) processing the conductive adhesive: firstly, dispersing and dissolving sodium carboxymethylcellulose in a solvent by stirring equipment, and stirring for 90-120min to prepare an ideal sodium carboxymethylcellulose glue solution; then adding conductive carbon black into the prepared sodium carboxymethylcellulose glue solution, and stirring for 20-30min under the condition that the vacuum degree is less than or equal to-80 kpa to prepare the conductive adhesive required by pulping;
(2) preliminary infiltration of graphite: adding 100% of graphite, 22-24% of water and 1-2% of N-methyl pyrrolidone into a stirrer, stirring for 40-70min, performing primary infiltration on the graphite by using equipment at revolution speed of 20-30RPM and rotation speed of 120-200RPM, and after the infiltration is finished, making the slurry into a semi-dry wet paste;
(3) first viscosity reduction processing: adding the preliminarily infiltrated graphite into conductive adhesive accounting for 20-40% of the added amount of the graphite, stirring in a stirrer at high viscosity for 40-70min, and further uniformly dispersing the graphite at revolution speed of 25-35RPM and rotation speed of 500-20000 mPa.s required by equipment to obtain negative electrode slurry with viscosity of 10000-20000 mPa.s;
(4) second viscosity reduction processing: adding 10-20% of conductive adhesive into the slurry with the first viscosity reduced in the step 3, stirring the slurry in a stirrer for 20-40min at high viscosity, wherein the revolution speed of the equipment is 25-35RPM, and the rotation speed is 1500-2000RPM, so that the viscosity and the solid content are further reduced while the slurry is further dispersed;
(5) homogenizing the slurry: after the viscosity is reduced, 37.5 percent of sodium carboxymethylcellulose and 3 percent of water are added, the mixture is stirred for 50-70min, and the revolution of the equipment is 30-40RPM and the rotation is 1200-1500RPM, so as to obtain homogenized slurry;
(6) adding styrene butadiene rubber into the homogenized slurry, and stirring for 20-40min, wherein the revolution speed of the equipment is 25-35RPM, and the rotation speed of the equipment is 700-900RPM, so as to obtain the slurry with the viscosity and the solid content meeting the process requirements;
(7) defoaming and processing: finally defoaming and stirring for 20-30min under the condition that the vacuum degree is less than or equal to-70 kpa, and revolving (rotating back) at 10RPM required by equipment to prepare the slurry.
In the preparation process of the conductive adhesive, cooling water is required to be communicated with the tank body, and the temperature in the preparation process is controlled to be 21-25 ℃. In the slurry preparation process, cooling water needs to be communicated with the tank body, and the temperature in the pulping process is controlled to be 21-25 ℃.
As shown in fig. 1, the cell capacity retention rate varies with the cycle number of charge and discharge cycles, and the retention rate of 800 cycles of the cell cycle life is more than 80% in the industry at present, and it can be seen from fig. 1 that the performance of the slurry cell prepared by the invention can meet the standard requirements in the industry.
As shown in fig. 2, the change curve of the internal viscosity of 48H in the static state of the slurry after the preparation of the slurry is completed, the stirring process provided by the invention can shorten the stirring time and improve the stirring production efficiency, and the internal change of the viscosity of the prepared negative electrode slurry is less than 1000 mpa.s.
As shown in FIG. 3, the change of the solid content of the slurry in 48H in a static state can meet the process requirement when the change of the solid content of the slurry is less than 0.2 percent along with the time change curve after the preparation of the slurry is finished.
The invention can improve the production efficiency on the premise of ensuring the quality of the slurry.
Claims (3)
1. A production stirring process for lithium ion battery negative electrode graphite slurry is characterized by comprising the following steps: comprises the following processing steps:
(1) processing the conductive adhesive: firstly, dispersing and dissolving sodium carboxymethylcellulose in a solvent by stirring equipment, and stirring for 90-120min to prepare an ideal sodium carboxymethylcellulose glue solution; then adding conductive carbon black into the prepared sodium carboxymethylcellulose glue solution, and stirring for 20-30min under the condition that the vacuum degree is less than or equal to-80 kpa to prepare the conductive adhesive required by pulping;
(2) preliminary infiltration of graphite: adding 100% of graphite, 22-24% of water and 1-2% of N-methyl pyrrolidone into a stirrer, stirring for 40-70min, performing primary infiltration on the graphite by using equipment at the revolution speed of 20-30RPM and the rotation speed of 120-200RPM, and after the infiltration is finished, making the slurry into a semi-dry wet paste;
(3) first viscosity reduction processing: adding the preliminarily infiltrated graphite into conductive adhesive accounting for 20-40% of the added amount of the graphite, stirring in a stirrer at high viscosity for 40-70min, and further uniformly dispersing the graphite at revolution speed of 25-35RPM and rotation speed of 500-20000 mPa.s required by equipment to obtain negative electrode slurry with viscosity of 10000-20000 mPa.s;
(4) second viscosity reduction processing: adding 10-20% of conductive adhesive into the slurry with the first viscosity reduced in the step 3, stirring the slurry in a stirrer for 20-40min at high viscosity, wherein the revolution speed of the equipment is 25-35RPM, and the rotation speed is 1500-2000RPM, so that the viscosity and the solid content are further reduced while the slurry is further dispersed;
(5) homogenizing the slurry: after the viscosity is reduced, 37.5 percent of sodium carboxymethylcellulose and 3 percent of water are added, the mixture is stirred for 50-70min, and the revolution of the equipment is 30-40RPM and the rotation is 1200-1500RPM, so as to obtain homogenized slurry;
(6) adding styrene butadiene rubber into the homogenized slurry, and stirring for 20-40min, wherein the revolution speed of the equipment is 25-35RPM, and the rotation speed of the equipment is 700-900RPM, so as to obtain the slurry with the viscosity and the solid content meeting the process requirements;
(7) defoaming and processing: finally defoaming and stirring for 20-30min under the condition that the vacuum degree is less than or equal to-70 kpa, and revolving (rotating back) at 10RPM required by equipment to prepare the slurry.
2. The production stirring process of the lithium ion battery negative electrode graphite slurry according to claim 1, characterized in that: in the preparation process of the conductive adhesive, cooling water is required to be communicated with the tank body, and the temperature in the preparation process is controlled to be 21-25 ℃.
3. The production stirring process of the lithium ion battery negative electrode graphite slurry according to claim 1, characterized in that: in the slurry preparation process, cooling water needs to be communicated with the tank body, and the temperature in the slurry preparation process is controlled to be 21-25 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011306570.5A CN112467082A (en) | 2020-11-20 | 2020-11-20 | Production stirring process for negative electrode graphite slurry of lithium ion battery |
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| CN202011306570.5A CN112467082A (en) | 2020-11-20 | 2020-11-20 | Production stirring process for negative electrode graphite slurry of lithium ion battery |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113346083A (en) * | 2021-05-31 | 2021-09-03 | 湖北亿纬动力有限公司 | Negative electrode slurry and preparation method and application thereof |
| CN113380973A (en) * | 2021-06-15 | 2021-09-10 | 湖南美尼科技有限公司 | Preparation method of silicon-based negative electrode slurry |
| CN115055071A (en) * | 2022-06-16 | 2022-09-16 | 汕尾天贸新能源科技有限公司 | Production stirring process for negative electrode graphite slurry of lithium ion battery |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103117392A (en) * | 2013-02-27 | 2013-05-22 | 江苏乐能电池股份有限公司 | Slurry compounding process of lithium ion battery slurry |
| WO2016169289A1 (en) * | 2015-04-20 | 2016-10-27 | 田东 | Method for preparing lithium ion battery negative electrode slurry |
| WO2017032154A1 (en) * | 2015-08-25 | 2017-03-02 | 田东 | Method for preparing graphite cathode slurry for lithium battery |
| CN106848204A (en) * | 2015-12-05 | 2017-06-13 | 中山天贸电池有限公司 | A kind of method for mixing of graphite material at negative |
-
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- 2020-11-20 CN CN202011306570.5A patent/CN112467082A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103117392A (en) * | 2013-02-27 | 2013-05-22 | 江苏乐能电池股份有限公司 | Slurry compounding process of lithium ion battery slurry |
| WO2016169289A1 (en) * | 2015-04-20 | 2016-10-27 | 田东 | Method for preparing lithium ion battery negative electrode slurry |
| WO2017032154A1 (en) * | 2015-08-25 | 2017-03-02 | 田东 | Method for preparing graphite cathode slurry for lithium battery |
| CN106848204A (en) * | 2015-12-05 | 2017-06-13 | 中山天贸电池有限公司 | A kind of method for mixing of graphite material at negative |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113346083A (en) * | 2021-05-31 | 2021-09-03 | 湖北亿纬动力有限公司 | Negative electrode slurry and preparation method and application thereof |
| CN113380973A (en) * | 2021-06-15 | 2021-09-10 | 湖南美尼科技有限公司 | Preparation method of silicon-based negative electrode slurry |
| CN115055071A (en) * | 2022-06-16 | 2022-09-16 | 汕尾天贸新能源科技有限公司 | Production stirring process for negative electrode graphite slurry of lithium ion battery |
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Application publication date: 20210309 |