CN116285482A - Reagent for removing oily electrode coating and application method thereof - Google Patents

Reagent for removing oily electrode coating and application method thereof Download PDF

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Publication number
CN116285482A
CN116285482A CN202310338227.6A CN202310338227A CN116285482A CN 116285482 A CN116285482 A CN 116285482A CN 202310338227 A CN202310338227 A CN 202310338227A CN 116285482 A CN116285482 A CN 116285482A
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reagent
electrode coating
nmp
dcm
methylpyrrolidone
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CN202310338227.6A
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CN116285482B (en
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刘应春
詹新举
王媛
李学成
盛云飞
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Wuhu Etc Battery Ltd
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Wuhu Etc Battery Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D9/00Chemical paint or ink removers
    • C09D9/005Chemical paint or ink removers containing organic solvents

Abstract

The invention discloses a reagent for removing an oily electrode coating layer and a use method thereof, and relates to the technical field of lithium ion battery detection, wherein the reagent comprises the following chemical raw materials in percentage by mass: ethylene Carbonate (EC): 5-15%, N-methylpyrrolidone (NMP): 10-20%, dichloromethane (DCM): 5-10%, ethyl Acetate (EA): 55-80%, wherein Ethylene Carbonate (EC) is used to dissolve the binder-like polymer in the electrode coating, N-methylpyrrolidone (NMP) is used to dissolve the oily substance in the electrode coating, methylene chloride (DCM) is used to protect the carbon-coated layer in the electrode coating, and Ethyl Acetate (EA) is used to dissolve the surface coating in the electrode coating. The application method for removing the oily electrode coating layer by using the reagent comprises the following steps: (1) preparing a reagent according to a relevant proportion; (2) tiling the pole piece to be wiped on dust-free cloth; (3) dripping the reagent into the area to be wiped by using a dropper; (4) after waiting for 1min, the cotton swab is used for wiping slowly, and the cotton swab is dried.

Description

Reagent for removing oily electrode coating and application method thereof
Technical Field
The invention relates to the technical field of lithium ion battery detection, in particular to a reagent for removing an oily electrode coating layer and a use method thereof.
Background
The lithium ion battery has the advantages of high energy density, good safety, no memory effect, long cycle life and the like, and is widely applied to the fields of portable electronic products, power and energy storage batteries. The lithium ion battery has certain probability of failure in the use or storage process, including capacity attenuation, short cycle life, increased internal resistance, lithium precipitation, gas production, thermal runaway and the like, and the service performance, consistency, reliability and safety of the lithium ion battery are seriously reduced. The method is a main task of lithium ion failure analysis, and has profound significance for improving the performance and developing the technology of the lithium ion battery.
In the battery failure analysis process, button cell performance test of the electrode after battery disassembly is the most common analysis mode. The internal electrode structure of lithium ion battery is generally a composite electrode with coated electrode material on both sides of current collector, and only one side of the electrode is required to be coated with slurry for making button cell. At this time, one surface of the double-sided coating layer needs to be removed completely, and the performance of the electrode is not affected.
The anode electrode coating slurry is usually an aqueous system, and pure water is used for removing the electrode coating layer during wiping. The cathode electrode coating is usually an oily system, carbon coating layers are arranged on both sides of the current collector, and the current wiping mode popular in the industry is to wipe with water or N-methylpyrrolidone (NMP); the mode is long in time consumption and low in efficiency, and the phenomenon that an electrode coating layer is not wiped cleanly and a carbon coating layer on a current collector is damaged can occur; the quality of the electrode plate obtained in the mode is low, the consistency of the button cell performance cannot be ensured, and the analysis of the cell failure is hindered.
Disclosure of Invention
The present invention is directed to a reagent for removing oily electrode coating and a method for using the same, which solve the above-mentioned drawbacks caused by the prior art.
A reagent for removing oily electrode coating layer comprises the following chemical raw materials in percentage by mass: ethylene Carbonate (EC): 5-15%, N-methylpyrrolidone (NMP): 10-20%, dichloromethane (DCM): 5-10%, ethyl Acetate (EA): 55-80%, wherein Ethylene Carbonate (EC) is used to dissolve the binder-like polymer in the electrode coating, N-methylpyrrolidone (NMP) is used to dissolve the oily substance in the electrode coating, methylene chloride (DCM) is used to protect the carbon-coated layer in the electrode coating, and Ethyl Acetate (EA) is used to dissolve the surface coating in the electrode coating.
Preferably, the reagent contains the following chemical raw materials in percentage by mass: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Acetate (EA): 70%.
Preferably, in this reagent, ethylene Carbonate (EC) is replaced by Propylene Carbonate (PC), and the chemical raw materials and the mass percentages thereof are as follows: propylene Carbonate (PC): 10%, N-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Acetate (EA): 70%.
Preferably, in the reagent, dichloromethane (DCM) is replaced by Petroleum Ether (PE), and the chemical raw materials and the mass percentages thereof are as follows: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, petroleum Ether (PE): 5%, ethyl Acetate (EA): 70%.
Preferably, in the reagent, ethyl Acetate (EA) is replaced by Ethyl Propionate (EP), and the chemical raw materials and the mass percentages thereof are as follows: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Propionate (EP): 70%.
Preferably, the reagent contains the following chemical raw materials in percentage by mass: ethylene Carbonate (EC): 15%, N-methylpyrrolidone (NMP): 20%, dichloromethane (DCM): 10%, ethyl Acetate (EA): 55%.
The application method of removing the oily electrode coating layer by using the reagent comprises the following operation steps:
step 1: preparing a reagent according to a relevant proportion;
step 2: tiling the pole piece to be wiped on dust-free cloth;
step 3: dripping the reagent into the area to be wiped by using a dropper;
step 4: after waiting for 1min, the cotton swab is used for wiping slowly, and the cotton swab is dried.
Compared with the prior art, the invention has the following advantages:
1. the electrode coating layer removing reagent provided by the invention can effectively protect the carbon coating layer on the surface of the electrode from being damaged, protect the integrity of the electrode and improve the accuracy of test data.
2. The testing method provided by the invention can be used for rapidly removing the coating layer on the surface of the oily electrode, so that the testing efficiency is improved.
3. The raw materials in the electrode coating layer removing reagent provided by the invention are common reagents in laboratories, are easy to obtain, and have low price and cost and strong economical practicability.
Drawings
FIG. 1 is a photograph of an electrode after wiping with the reagent [ 10% EC+15% NMP+5% DCM+70% EA ] of example 1.
FIG. 2 is a photograph of the electrode after wiping with the reagent [ 10% PC+15% NMP+5% DCM+70% EA ] of example 2.
FIG. 3 is a photograph of an electrode after wiping with the reagent [ 10% EC+15% NMP+5% PE+70% EA ] of example 3.
FIG. 4 is a photograph of the electrode of example 4 after wiping with reagent [ 10% EC+15% NMP+5% DCM+70% EP ].
FIG. 5 is a photograph of the electrode of example 5 after wiping with reagent [ 15% EC+20% NMP+10% DCM+55% EA ].
FIG. 6 is a photograph of the electrode of comparative example 1 after wiping with the reagent [ water ].
FIG. 7 is a photograph of an electrode after wiping with the reagent [ NMP ] of comparative example 2.
Fig. 8 is a photograph of an electrode after wiping with reagent [ 10% ec+15% nmp+75% ea ] of comparative example 3.
FIG. 9 is a photograph of the electrode of comparative example 4 after wiping with reagent [ 15% NMP+5% DCM+80% EA ].
Fig. 10 is a photograph of an electrode after wiping with reagent [ 15% ec+5% dcm+80% ea ] of comparative example 5.
FIG. 11 is a photograph of the electrode of comparative example 6 after wiping with reagent [ 30% EC+40% NMP+30% DCM ].
Detailed Description
The invention is further described in connection with the following detailed description, in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
As shown in fig. 1 to 11, a reagent for removing an oily electrode coating layer comprises the following chemical raw materials in percentage by mass: ethylene Carbonate (EC): 5-15%, N-methylpyrrolidone (NMP): 10-20%, dichloromethane (DCM): 5-10%, ethyl Acetate (EA): 55-80%, wherein Ethylene Carbonate (EC) is used to dissolve the binder-like polymer in the electrode coating, N-methylpyrrolidone (NMP) is used to dissolve the oily substance in the electrode coating, methylene chloride (DCM) is used to protect the carbon-coated layer in the electrode coating, and Ethyl Acetate (EA) is used to dissolve the surface coating in the electrode coating.
The application method of removing the oily electrode coating layer by using the reagent comprises the following operation steps:
step 1: preparing a reagent according to a relevant proportion;
step 2: tiling the pole piece to be wiped on dust-free cloth;
step 3: dripping the reagent into the area to be wiped by using a dropper;
step 4: after waiting for 1min, the cotton swab is used for wiping slowly, and the cotton swab is dried.
Example 1: the electrode was wiped using reagents [ 10% ec+15% nmp+5% dcm+70% ea ]
In this embodiment, the chemical raw materials and the mass percentages of the chemical raw materials contained in the reagent are as follows: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Acetate (EA): 70%. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the slurry coating on the surface of the electrode is completely removed, and the carbon coating on the current collector remains intact, thereby reaching the technical requirements.
Example 2: the electrode was wiped using the reagent [ 10% pc+15% nmp+5% dcm+70% ea ]
In this example, in this reagent, ethylene Carbonate (EC) was replaced with Propylene Carbonate (PC) (or a carbonate substance such as dimethyl carbonate), and the following chemical raw materials were contained in mass percent: propylene Carbonate (PC): 10%, N-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Acetate (EA): 70%. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the slurry coating on the surface of the electrode is completely removed, and the carbon coating on the current collector remains intact, thereby reaching the technical requirements.
Example 3: the electrode was wiped using the reagent [ 10% ec+15% nmp+5% pe+70% ea ]
In this example, in this reagent, dichloromethane (DCM) was replaced with Petroleum Ether (PE) (or chloroform, etc.), and the following chemical raw materials were contained in mass percent: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, petroleum Ether (PE): 5%, ethyl Acetate (EA): 70%. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the slurry coating on the surface of the electrode is completely removed, and the carbon coating on the current collector remains intact, thereby reaching the technical requirements.
Example 4: the electrode was wiped using reagents [ 10% ec+15% nmp+5% dcm+70% ep ]
In this example, ethyl Acetate (EA) was replaced with Ethyl Propionate (EP), and the chemical materials and mass percentages thereof contained were as follows: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Propionate (EP): 70%. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the slurry coating on the surface of the electrode is completely removed, and the carbon coating on the current collector remains intact, thereby reaching the technical requirements.
Example 5: the electrode was wiped using the reagent [ 15% ec+20% nmp+10% dcm+55% ea ]
In this embodiment, the chemical raw materials and the mass percentages of the chemical raw materials contained in the reagent are as follows: ethylene Carbonate (EC): 15%, N-methylpyrrolidone (NMP): 20%, dichloromethane (DCM): 10%, ethyl Acetate (EA): 55%. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the slurry coating on the surface of the electrode is completely removed, and the carbon coating on the current collector remains intact, thereby reaching the technical requirements.
Comparative example 1: wiping an electrode with a reagent [ water ]
In this embodiment, the chemical raw materials and the mass percentages of the chemical raw materials contained in the reagent are as follows: water: 100%. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the aluminum foil is completely exposed on the surface of the electrode, the carbon coating layer on the current collector is completely wiped, and the carbon coating layer is not reserved; the technical requirements are not met.
Comparative example 2: wiping an electrode with a reagent [ NMP ]
In this embodiment, the chemical raw materials and the mass percentages of the chemical raw materials contained in the reagent are as follows: n-methylpyrrolidone (NMP): 100%. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the carbon coating on the current collector is destroyed; the technical requirements are not met.
Comparative example 3: the electrode was wiped with reagent [ 10% ec+15% nmp+75% ea ]
In this embodiment, the chemical raw materials and the mass percentages of the chemical raw materials contained in the reagent are as follows: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, ethyl Acetate (EA): 75%, i.e. Dichloromethane (DCM) was omitted. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the carbon coating on the current collector is destroyed; failing to meet the technical requirements
Comparative example 4: the electrode was wiped using the reagent [ 15% NMP+5% DCM+80% EA ]
In this embodiment, the chemical raw materials and the mass percentages of the chemical raw materials contained in the reagent are as follows: n-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Acetate (EA): 80%, i.e. the Ethylene Carbonate (EC) was eliminated. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the electrode coating cannot be removed; failing to meet the technical requirements
Comparative example 5: the electrode was wiped using reagents [ 15% ec+5% dcm+80% ea ]
In this embodiment, the chemical raw materials and the mass percentages of the chemical raw materials contained in the reagent are as follows: ethylene Carbonate (EC): 15%, dichloromethane (DCM): 5%, ethyl Acetate (EA): 80% of the N-methylpyrrolidone (NMP) was eliminated. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the electrode coating cannot be removed; failing to meet the technical requirements
Comparative example 6: the electrode was wiped with reagent [ 30% ec+40% nmp+30% dcm ]
In this embodiment, the chemical raw materials and the mass percentages of the chemical raw materials contained in the reagent are as follows: ethylene Carbonate (EC): 30%, N-methylpyrrolidone (NMP): 40%, dichloromethane (DCM): 30%, i.e. Ethyl Acetate (EA) was eliminated. The reagent is prepared according to the relevant proportion and the electrode is wiped.
Wiping results: the carbon coating on the current collector is destroyed; the technical requirements are not met.
Accordingly, the above disclosed embodiments are illustrative in all respects, and not exclusive. All changes that come within the scope of the invention or equivalents thereto are intended to be embraced therein.

Claims (7)

1. A reagent for removing oily electrode coating, characterized in that: the reagent comprises the following chemical raw materials in percentage by mass: ethylene Carbonate (EC): 5-15%, N-methylpyrrolidone (NMP): 10-20%, dichloromethane (DCM): 5-10%, ethyl Acetate (EA): 55-80%, wherein Ethylene Carbonate (EC) is used to dissolve the binder-like polymer in the electrode coating, N-methylpyrrolidone (NMP) is used to dissolve the oily substance in the electrode coating, methylene chloride (DCM) is used to protect the carbon-coated layer in the electrode coating, and Ethyl Acetate (EA) is used to dissolve the surface coating in the electrode coating.
2. The reagent for removing oily electrode coating layer according to claim 1, wherein: the reagent comprises the following chemical raw materials in percentage by mass: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Acetate (EA): 70%.
3. The reagent for removing oily electrode coating layer according to claim 1, wherein: in the reagent, ethylene Carbonate (EC) is replaced by Propylene Carbonate (PC), and the chemical raw materials and the mass percentages thereof are as follows: propylene Carbonate (PC): 10%, N-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Acetate (EA): 70%.
4. The reagent for removing oily electrode coating layer according to claim 1, wherein: in the reagent, dichloromethane (DCM) is replaced by Petroleum Ether (PE), and the chemical raw materials and the mass percentages thereof are as follows: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, petroleum Ether (PE): 5%, ethyl Acetate (EA): 70%.
5. The reagent for removing oily electrode coating layer according to claim 1, wherein: in the reagent, ethyl Acetate (EA) is replaced by Ethyl Propionate (EP), and the chemical raw materials and the mass percentages thereof are as follows: ethylene Carbonate (EC): 10%, N-methylpyrrolidone (NMP): 15%, dichloromethane (DCM): 5%, ethyl Propionate (EP): 70%.
6. The reagent for removing oily electrode coating layer according to claim 1, wherein: the reagent comprises the following chemical raw materials in percentage by mass: ethylene Carbonate (EC): 15%, N-methylpyrrolidone (NMP): 20%, dichloromethane (DCM): 10%, ethyl Acetate (EA): 55%.
7. An agent for removing oily electrode coating layer according to any one of claims 1 to 6, wherein: the application method for removing the oily electrode coating layer by using the reagent comprises the following operation steps:
step 1: preparing a reagent according to a relevant proportion;
step 2: tiling the pole piece to be wiped on dust-free cloth;
step 3: dripping the reagent into the area to be wiped by using a dropper;
step 4: after waiting for 1min, the cotton swab is used for wiping slowly, and the cotton swab is dried.
CN202310338227.6A 2023-03-31 2023-03-31 Reagent for removing oily electrode coating and application method thereof Active CN116285482B (en)

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CN116285482B CN116285482B (en) 2023-12-01

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111509185A (en) * 2020-04-23 2020-08-07 惠州锂威新能源科技有限公司 Protection assembly and method for removing pole piece coating residues
CN112054265A (en) * 2020-09-30 2020-12-08 合肥国轩高科动力能源有限公司 Method for recycling and reusing anode material of waste ternary lithium ion battery
CN113675539A (en) * 2020-04-30 2021-11-19 北京小米移动软件有限公司 Electrode tab mounting process, wiping piece and battery

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111509185A (en) * 2020-04-23 2020-08-07 惠州锂威新能源科技有限公司 Protection assembly and method for removing pole piece coating residues
CN113675539A (en) * 2020-04-30 2021-11-19 北京小米移动软件有限公司 Electrode tab mounting process, wiping piece and battery
CN112054265A (en) * 2020-09-30 2020-12-08 合肥国轩高科动力能源有限公司 Method for recycling and reusing anode material of waste ternary lithium ion battery

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