CN112885987A - Preparation method of lithium battery negative electrode slurry - Google Patents
Preparation method of lithium battery negative electrode slurry Download PDFInfo
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- CN112885987A CN112885987A CN202110134107.5A CN202110134107A CN112885987A CN 112885987 A CN112885987 A CN 112885987A CN 202110134107 A CN202110134107 A CN 202110134107A CN 112885987 A CN112885987 A CN 112885987A
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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
- H01M4/1397—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
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
Abstract
The invention provides a preparation method of lithium battery cathode slurry, which comprises the following steps: mixing a negative electrode active substance and a conductive agent, adding a solvent, stirring and pre-infiltrating to obtain a first mixture with a solid content of 70-85%; adding a solvent into the first mixture for dry mixing to obtain a second mixture; adding a solvent into the mixture II for kneading to form a semi-dry muddy mixture III with the solid content of 60-70%; adding a solvent into the mixture III, stirring and dispersing to form a mixed slurry IV with the solid content of 50-60%; adding a binder into the mixed slurry IV, and uniformly stirring and dispersing; adding a solvent into the mixed slurry IV for dilution and dispersion, and finally adding the solvent to adjust the slurry to the required viscosity; the method can effectively control the distribution of adsorption sites of the solvent and the dispersant in the discharged slurry, maintain proper viscosity and maintain the stable space state of the slurry.
Description
Technical Field
The invention belongs to the technical field of preparation of lithium battery negative electrode slurry, and particularly relates to a preparation method of lithium battery negative electrode slurry.
Background
The lithium ion battery cell is a secondary battery cell capable of being repeatedly charged and discharged, and is fully utilized in many fields at present. And the lithium ion battery pulping is in the first stage of the whole process, so that the quality of the pulp performance is more important. At present, the mainstream stirring process at home and abroad gradually begins to change from wet stirring to dry stirring. The dry stirring process has the advantages of short stirring time, relatively good slurry dispersibility and the like, and various battery manufacturers start to change to the method. However, the deep exploration of the principle of the method is lack of how to understand and utilize the effect of each step of the dry stirring.
In the conventional dry process, an active substance, a conductive agent and a dispersant are generally added and mixed together in a dry mixing stage, and a certain proportion of solvent is added for kneading and subsequent dispersion after the dry mixing is finished. The graphite particles are dispersed by the CMC steric hindrance repulsive force adsorbed on the surface. If the graphite surface is adsorbed by a large number of COO units in CMC, although the dispersibility is good, the COO units among the linked graphite particles are less, the capability of maintaining the overall stability is reduced, and the filter element is easy to settle and block. How to make the trade-off between the two is of paramount importance.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of lithium battery cathode slurry, which can effectively control the distribution of adsorption sites of a solvent and a dispersant in the slurry after shipment, maintain proper viscosity and maintain the stable space state of the slurry.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of negative electrode slurry of a lithium battery comprises the following steps:
(1) mixing a negative electrode active substance and a conductive agent, adding a solvent, stirring and pre-infiltrating to obtain a first mixture with a solid content of 70-85%;
(2) adding a solvent into the first mixture for dry mixing to obtain a second mixture;
(3) adding a solvent into the mixture II for kneading to form a semi-dry muddy mixture III with the solid content of 60-70%;
(4) adding a solvent into the mixture III, stirring and dispersing to form a mixed slurry IV with the solid content of 50-60%;
(5) adding a binder into the mixed slurry IV, and uniformly stirring and dispersing;
(6) and adding a solvent into the mixed slurry IV for dilution and dispersion, and finally adding the solvent to adjust the slurry to the required viscosity.
Further, in the step (1), the stirring time is 20-30 min.
In the step (2), the dry mixing stirring time is 10-15 min.
In the step (3), the kneading time is 20-60 min.
In the step (4), the stirring and dispersing time is 2-3 h.
In the step (5), the viscosity of the slurry is 2000-8000 mPa.s.
The weight ratio of the negative electrode active material to the conductive agent to the dispersing agent to the binder is 96-98: 0-2: 0.5-1: 0.1-1.
The negative active material is artificial graphite or natural graphite.
The solvent is deionized water.
The dispersant is CMC.
The binder is styrene-butadiene rubber emulsion (SBR) or acrylic resin emulsion (PAA); and (3) when the binder is acrylic resin emulsion, adding the binder and deionized water into the third mixture in the step (4) to form a fourth mixed slurry with the solid content of 50-60%, and omitting the step (5).
According to the preparation method of the lithium battery cathode slurry, the cathode active material and the conductive agent are mixed and added with the solvent for stirring and pre-infiltrating, so that the solvent is guaranteed to preferentially occupy partial sites of the cathode active material, then the dispersing agent is added for dry mixing and subsequent kneading, then the binder and the solvent are added for stirring and dispersing, and finally the solvent is added for adjusting the slurry to be proper in viscosity. Compared with the prior art, the preparation method provided by the invention can control the distribution of adsorption sites of the solvent and the dispersant in the discharged slurry, the viscosity of the discharged slurry is proper, the dispersion is good, the stability of the slurry is excellent, and the dispersion time of the slurry is shortened to 3.5-4.5 h.
Drawings
FIG. 1 is a flow chart showing the preparation of a negative electrode slurry for a lithium battery in example 1;
FIG. 2 is a flowchart of the preparation of negative electrode slurry for lithium battery in example 2;
FIG. 3 is a graph showing the change in viscosity of lithium battery negative electrode pastes prepared in example 1 and comparative example 1 over 72 hours;
fig. 4 is a graph showing the change in viscosity of the negative electrode pastes for lithium batteries prepared in example 2 and comparative example 2 over 72 hours.
Detailed Description
The present invention will be described in detail with reference to examples.
Comparative example 1
A preparation method of lithium battery negative electrode slurry comprises the following steps:
the method comprises the following steps: weighing 97.7 parts of artificial graphite, 1.2 parts of CMC powder and 1.1 parts of SBR emulsion according to the mass parts, adding the artificial graphite and the CMC powder into a double-planet stirring tank, carrying out dry mixing, and stirring for 20 min;
step two: adding deionized water after the first step for kneading, and stirring for 20min to form semi-dry mud-like slurry with the solid content of 67% (mass percentage);
step three: adding primary deionized water into the material obtained in the step two, stirring and dispersing for 2 hours, and reducing the solid content to 55.16%;
step four: adding the material obtained in the step four into the SBR emulsion with the formula amount and stirring;
step five: and (4) adding deionized water into the material obtained in the step three for dispersion, and adding deionized water to adjust the viscosity to 3000-6000mPa & s.
Example 1
A preparation method of lithium battery negative electrode slurry comprises the following steps:
the method comprises the following steps: weighing 97.7 parts of artificial graphite, 1.2 parts of CMC powder and 1.1 parts of SBR emulsion according to the mass parts, adding the artificial graphite into a double-planet stirring tank, adding a small amount of deionized water until the solid content in the tank is 77.5%, stirring for 20min, and pre-infiltrating;
step two: adding CMC after the first step for dry mixing, and stirring for 10min
Step three: adding deionized water into the material obtained in the step two for kneading for 20min to form semi-dry mud-like slurry with the solid content of 67% (mass percentage);
step four: adding primary deionized water into the material obtained in the step three, stirring and dispersing for 2 hours, and reducing the solid content to 55.16%;
step five: adding the material obtained in the step four into the SBR emulsion with the formula amount and stirring;
step six: and D, adding deionized water into the material obtained in the step five for dispersion, and adding deionized water to adjust the viscosity to 3000-6000 mPa.
Comparative example 2
A preparation method of lithium battery negative electrode slurry comprises the following steps:
the method comprises the following steps: weighing 95.5 parts of artificial graphite, 1 part of conductive agent, 0.4 part of CMC powder and 3.1 parts of PAA according to the mass parts; adding artificial graphite, a conductive agent and CMC powder into a double-planet stirring tank, carrying out dry mixing, and stirring for 30 min;
step two: adding deionized water after the first step for kneading, and stirring for 60min to form semi-dry mud-like slurry with solid content of 68% (mass percentage);
step three: adding the material obtained in the second step into PAA emulsion, stirring and dispersing with deionized water for 3 hours, and reducing the solid content to 52%;
step four: and (4) adding deionized water into the material obtained in the step three for dispersion, and adding deionized water to adjust the viscosity to 3000-6000 mPa.
Example 2
A preparation method of lithium battery negative electrode slurry comprises the following steps:
the method comprises the following steps: weighing 95.5 parts of artificial graphite, 1 part of conductive agent, 0.4 part of CMC powder and 3.1 parts of PAA according to the mass parts; adding artificial graphite and a conductive agent into a double-planet stirring tank, adding a small amount of deionized water until the solid content in the tank is 73%, stirring for 20min, and pre-infiltrating;
step two: adding CMC powder after the first step for dry mixing, and stirring for 10 min;
step three: adding deionized water for kneading, and stirring for 60min to form semi-dry slurry with solid content of 68% (mass percentage);
step four: adding the PAA emulsion and deionized water into the material obtained in the third step, stirring and dispersing for 3 hours, and reducing the solid content to 52%;
step five: and D, adding deionized water into the material obtained in the step four for dispersion, and adding deionized water to adjust the viscosity of the material to 3000-6000mPa & s.
The slurry prepared according to the stirring steps in the embodiments 1 and 2 of the invention has moderate delivery viscosity under the same solid content, is beneficial to coating, and does not block a steel shell filter element during filtering; the slurry has good dispersibility and excellent standing stability, and the slurry does not have any settlement in 96 hours and has good state; compared with the comparative examples 1 and 2, the slurry has the advantages of higher shipment viscosity, poorer standing stability, easy blockage of filter elements and no contribution to mass production of production lines under the condition of the same solid content.
The above detailed description of the method for preparing a negative electrode slurry for a lithium battery with reference to the embodiments is illustrative and not restrictive, and several embodiments may be enumerated within the scope of the limitations, so that variations and modifications thereof may be made without departing from the spirit of the present invention.
Claims (10)
1. The preparation method of the lithium battery negative electrode slurry is characterized by comprising the following steps of:
(1) mixing a negative electrode active substance and a conductive agent, adding a solvent, stirring and pre-infiltrating to obtain a first mixture with a solid content of 70-85%;
(2) adding a solvent into the first mixture for dry mixing to obtain a second mixture;
(3) adding a solvent into the mixture II for kneading to form a semi-dry muddy mixture III with the solid content of 60-70%;
(4) adding a solvent into the mixture III, stirring and dispersing to form a mixed slurry IV with the solid content of 50-60%;
(5) adding a binder into the mixed slurry IV, and uniformly stirring and dispersing;
(6) and adding a solvent into the mixed slurry IV for dilution and dispersion, and finally adding the solvent to adjust the slurry to the required viscosity.
2. The preparation method according to claim 1, wherein in the step (1), the stirring time is 20-30 min.
3. The preparation method according to claim 1, wherein in the step (2), the dry mixing is performed for 10 to 15 min.
4. The production method according to claim 1, wherein in the step (3), the kneading time is 20 to 60 min.
5. The preparation method according to claim 1, wherein in the step (4), the stirring and dispersing time is 2-3 h.
6. The production method according to any one of claims 1 to 5, wherein the weight ratio of the negative electrode active material, the conductive agent, the dispersant, and the binder is 96 to 98: 1-2: 0.5-1: 0.1-1.
7. The production method according to any one of claims 1 to 5, wherein the negative electrode active material is artificial graphite or natural graphite.
8. The method according to any one of claims 1 to 5, wherein the solvent is deionized water.
9. The method according to any one of claims 1 to 5, wherein the dispersant is CMC.
10. The method according to any one of claims 1 to 5, wherein the binder is styrene-butadiene rubber emulsion or acrylic resin emulsion; and (3) when the binder is acrylic resin emulsion, adding the binder and deionized water into the third mixture in the step (4) to form a fourth mixed slurry with the solid content of 50-60%, and omitting the step (5).
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| CN202110134107.5A CN112885987A (en) | 2021-01-29 | 2021-01-29 | Preparation method of lithium battery negative electrode slurry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457541A (en) * | 2021-07-01 | 2021-10-01 | 江西安驰新能源科技有限公司 | Efficient slurry mixing system and efficient slurry mixing process thereof |
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| CN105470512A (en) * | 2016-01-15 | 2016-04-06 | 河南比得力高新能源科技有限公司 | Preparation process for power lithium ion battery slurry |
| CN106981620A (en) * | 2017-04-07 | 2017-07-25 | 惠州拓邦电气技术有限公司 | A kind of preparation method of lithium ion battery cathode slurry |
| CN109037676A (en) * | 2017-06-09 | 2018-12-18 | 宁德时代新能源科技股份有限公司 | Lithium ion battery cathode slurry and preparation method thereof |
| KR20190062955A (en) * | 2017-11-29 | 2019-06-07 | 주식회사 엘지화학 | Method of manufacturing positive electrode slurry for lithium-sulfur battery |
| CN110364736A (en) * | 2019-07-12 | 2019-10-22 | 大连恒超锂业科技有限公司 | A kind of cathode of lithium battery slurry and preparation method thereof |
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- 2021-01-29 CN CN202110134107.5A patent/CN112885987A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105470512A (en) * | 2016-01-15 | 2016-04-06 | 河南比得力高新能源科技有限公司 | Preparation process for power lithium ion battery slurry |
| CN106981620A (en) * | 2017-04-07 | 2017-07-25 | 惠州拓邦电气技术有限公司 | A kind of preparation method of lithium ion battery cathode slurry |
| CN109037676A (en) * | 2017-06-09 | 2018-12-18 | 宁德时代新能源科技股份有限公司 | Lithium ion battery cathode slurry and preparation method thereof |
| KR20190062955A (en) * | 2017-11-29 | 2019-06-07 | 주식회사 엘지화학 | Method of manufacturing positive electrode slurry for lithium-sulfur battery |
| CN110364736A (en) * | 2019-07-12 | 2019-10-22 | 大连恒超锂业科技有限公司 | A kind of cathode of lithium battery slurry and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457541A (en) * | 2021-07-01 | 2021-10-01 | 江西安驰新能源科技有限公司 | Efficient slurry mixing system and efficient slurry mixing process thereof |
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Application publication date: 20210601 |