CN114614016A - Adhesive composition for lithium ion battery and preparation method thereof - Google Patents
Adhesive composition for lithium ion battery and preparation method thereof Download PDFInfo
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- CN114614016A CN114614016A CN202210291636.0A CN202210291636A CN114614016A CN 114614016 A CN114614016 A CN 114614016A CN 202210291636 A CN202210291636 A CN 202210291636A CN 114614016 A CN114614016 A CN 114614016A
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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
- H01M4/622—Binders being polymers
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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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- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
An adhesive composition for a lithium ion battery and a preparation method thereof belong to the technical field of lithium ion batteries, and the adhesive composition consists of hyperbranched polyesteramide aqueous solution, polyvinyl alcohol, polydiallyldimethylammonium chloride, high-concentration carboxyl hydroxyl polymer solution, methoxy polyethylene glycol ether sodium salt, polyether and dimethyl siloxane graft copolymer, a tackifier, tris (2, 4-di-tert-butylphenyl) phosphite and deionized water; the stripping strength of an electrode plate prepared by the adhesive composition for the lithium ion battery electrode is 5.8-6.2 mN/mm, the first discharge capacity of the lithium ion battery assembled by the electrode plate is 480mAh, the first stock efficiency is 92-96%, the capacity retention rate is 91.9-94.5% and the expansion rate of the electrode plate is 22.9-28.6% after 50 weeks of charge-discharge circulation.
Description
Technical Field
The invention relates to an adhesive composition for a lithium ion battery and a preparation method thereof, belonging to the technical field of lithium ion batteries.
Background
The lithium ion battery mainly comprises electrode plates (including a positive plate and a negative plate), a diaphragm, electrolyte and the like; and the electrode plates are all composed of electrode active material powder, adhesive, conductive agent and current collector. When preparing the electrode plate of the lithium ion battery, the electrode active material, the conductive agent and the adhesive solution are mixed and ground uniformly to form slurry, and then the slurry is coated on copper foil and aluminum foil serving as a current collector, and the slurry is obtained through the processes of drying, rolling and the like. Wherein the adhesive has a key role in the preparation of the electrode sheet. Polyvinylidene fluoride is the earliest commercialized binder for the lithium ion battery, but the binder has the defects of poor electronic and ionic conductivity, poor adhesion of active substances on a current collector due to easy swelling of electrolyte, unsatisfactory mechanical properties and elasticity, easy formation of lithium carbide with metal lithium, influence on the service life and safety performance of the battery, high requirement on the humidity of the environment during storage and use and the like. The water-based binder takes water as a dispersing agent, has low price, is green and environment-friendly, and is friendly to human body and environment. Therefore, more and more lithium battery production companies are targeting aqueous binders using water as a solvent,
the water-based binder is gradually replacing oil-based binders such as PVDF and the like, and becomes a new generation of commercial lithium ion battery binder.
Chinese patent CN107384261A discloses an aqueous binder for a lithium ion battery separator heat-resistant layer, which is prepared from the following raw materials in parts by weight: relative to 100 parts by weight of acrylate monomers, 3-35 parts by weight of functional monomers, 0.3-15 parts by weight of olefin unsaturated group-containing reactive emulsifier, 0.1-15 parts by weight of water-soluble initiator, 0.01-3 parts by weight of electrolyte and 100-700 parts by weight of deionized water, wherein the mass fraction of the water-based adhesive is 20-55%. The water-based adhesive prepared by the patent has poor bonding force, poor flexibility after crosslinking and curing, and brittle and easy to break after electrode plates are dried, so that the yield of battery production is reduced.
Chinese patent CN105778834A discloses an adhesive for a ceramic diaphragm of a lithium ion battery and a preparation method thereof, wherein the adhesive adopts an emulsion polymerization method, acrylic soft monomers and hard monomers with specific proportions are mixed to form stable latex bundles through the dispersion action of a complex emulsifier, and the polymerized monomers are polymerized in the latex bundles under the action of an initiator to form stable polymer emulsion. In this patent, an oxidation-reduction initiator system is used, which contains ferrous chloride, and the presence of ferric ions in the binder reduces the first coulombic efficiency and charge-discharge performance.
In summary, the adhesive for the lithium ion battery electrode still has the problems of low bonding strength, poor flexibility, low first coulombic efficiency, poor charge and discharge performance and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides an adhesive composition for a lithium ion battery and a preparation method thereof, which realize the following purposes: the adhesive composition for the lithium ion battery electrode, which has the advantages of excellent bonding strength, good flexibility, high initial coulomb rate, good charge and discharge performance and low battery attenuation rate, is prepared.
In order to realize the purpose, the invention adopts the following technical scheme:
an adhesive composition for a lithium ion battery and a preparation method thereof comprise an adhesive composition formula and an adhesive composition preparation method.
The following is a further improvement of the above technical solution:
step 1 adhesive composition
The adhesive composition comprises the following specific formula in parts by weight:
20-50 parts of hyperbranched polyesteramide aqueous solution
0.5-6 parts of polyvinyl alcohol
1-10 parts of poly (diallyldimethylammonium chloride)
3-8 parts of high-concentration carboxyl hydroxyl polymer solution
0.1-6 parts of methoxypolyethylene glycol ether sodium salt
0.1-5 parts of polyether and dimethyl siloxane graft copolymer
0-4 parts of tackifier
0.1 to 2 parts of tris (2, 4-di-tert-butylphenyl) phosphite
30-60 parts of deionized water
The mass concentration of the hyperbranched polyesteramide in the hyperbranched polyesteramide aqueous solution is 10-50%;
the hyperbranched polyamide is a copolymer of succinic anhydride and diisopropanolamine, the number average molecular weight of the hyperbranched polyamide is 1200g/mol, and a terminal functional group is a secondary alcohol;
the polyvinyl alcohol has an alcoholysis degree of 80-92%, a polymerization degree of 400-900 and a volatile component of less than or equal to 1%;
the preparation method of the high-concentration carboxyl hydroxyl polymer solution comprises the following steps: according to parts by mass, stirring and dissolving 10-20 parts of carboxylated chitosan and 2-10 parts of hydroxypropyl-beta-cyclodextrin in 60-85 parts of deionized water, slowly adding 0.3-0.9 part of polymethacryloxyethyl trimethyl ammonium chloride, and completely dissolving to obtain a transparent solution, namely a high-concentration carboxyl hydroxyl polymer solution;
the carboxylation degree of the carboxylated chitosan is 60-80%, and insoluble substances are less than 0.3%;
the tackifier is one or more of carboxymethyl cellulose, hydroxypropyl guar gum, hydroxypropyl methyl cellulose, xanthan gum and sodium alginate;
step 2 adhesive composition preparation method
According to the weight parts of each raw material in the formula of the adhesive composition, firstly adding a hyperbranched polyesteramide aqueous solution into a mixing kettle, then adding deionized water, polyvinyl alcohol, methoxy polyethylene glycol ether sodium salt, polydiallyldimethylammonium chloride, a polyether-dimethylsiloxane graft copolymer, a high-concentration carboxyhydroxy polymer solution and tris (2, 4-di-tert-butylphenyl) phosphite, mixing and stirring at the rotating speed of 3000-5500 rpm for 15-25 minutes, then adding a tackifier, and continuously stirring for 40-60 minutes to obtain the adhesive composition.
Compared with the prior art, the invention has the following beneficial effects:
1. the adhesive composition for the lithium ion battery electrode, which is prepared by the invention, has the advantages of excellent bonding strength, good flexibility, high first coulomb rate, good charge and discharge performance and low battery attenuation rate;
2. the stripping strength of an electrode plate prepared by the adhesive composition for the lithium ion battery electrode is 5.8-6.2 mN/mm, the first discharge capacity of the lithium ion battery assembled by the electrode plate is 480mAh, the first stock efficiency is 92-96%, the capacity retention rate is 91.9-94.5% and the expansion rate of the electrode plate is 22.9-28.6% after 50 weeks of charge-discharge circulation.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1: adhesive composition for lithium ion battery and preparation method thereof
The method comprises the following steps:
1. adhesive composition
The adhesive composition comprises the following specific formula in parts by weight:
40 parts of hyperbranched polyesteramide aqueous solution
2 parts of polyvinyl alcohol
5 parts of polydiallyldimethylammonium chloride
6 parts of high-concentration solution of a carboxyhydroxypolymer
3 parts of methoxy polyglycol ether sodium salt
2 parts of polyether-dimethylsiloxane graft copolymer
2 parts of tackifier
1 part of tris (2, 4-di-tert-butylphenyl) phosphite
50 parts of deionized water
The mass concentration of the hyperbranched polyesteramide in the hyperbranched polyesteramide aqueous solution is 30%;
the hyperbranched polyamide is a copolymer of succinic anhydride and diisopropanolamine, the number average molecular weight of the hyperbranched polyamide is 1200g/mol, and a terminal functional group is a secondary alcohol;
the alcoholysis degree of the polyvinyl alcohol is 85 percent, the polymerization degree is 600, and the volatile component is less than or equal to 1 percent;
the preparation method of the high-concentration carboxyl hydroxyl polymer solution comprises the following steps: according to parts by mass, stirring and dissolving 16 parts of carboxylated chitosan and 6 parts of hydroxypropyl-beta-cyclodextrin in 75 parts of deionized water, slowly adding 0.5 part of polymethacryloxyethyl trimethyl ammonium chloride, and completely dissolving to obtain a transparent solution, namely a high-concentration carboxyl hydroxyl polymer solution;
the carboxylation degree of the carboxylated chitosan is 65 percent, and insoluble substances are less than 0.3 percent;
the tackifier is carboxymethyl cellulose.
2. Adhesive composition formulation method
According to the weight parts of each raw material in the formula of the adhesive composition, firstly adding a hyperbranched polyesteramide aqueous solution into a mixing kettle, then adding deionized water, polyvinyl alcohol, methoxy polyethylene glycol ether sodium salt, polydiallyldimethylammonium chloride, a polyether-dimethylsiloxane graft copolymer, a high-concentration carboxyhydroxy polymer solution and tris (2, 4-di-tert-butylphenyl) phosphite, mixing and stirring at 3500 rpm for 20 minutes, then adding a tackifier, and continuing stirring for 50 minutes to obtain the adhesive composition.
Example 2: adhesive composition for lithium ion battery and preparation method thereof
The method comprises the following steps:
1. adhesive composition
The adhesive composition comprises the following specific formula in parts by weight:
20 parts of hyperbranched polyesteramide aqueous solution
0.5 part of polyvinyl alcohol
1 part of polydiallyldimethylammonium chloride
3 parts of a high-concentration solution of a carboxyhydroxypolymer
0.1 part of methoxy polyglycol ether sodium salt
0.1 part of polyether-dimethylsiloxane graft copolymer
0.1 part of tris (2, 4-di-tert-butylphenyl) phosphite
30 parts of deionized water
The mass concentration of the hyperbranched polyesteramide in the hyperbranched polyesteramide aqueous solution is 10%;
the hyperbranched polyamide is a copolymer of succinic anhydride and diisopropanolamine, the number average molecular weight of the hyperbranched polyamide is 1200g/mol, and a terminal functional group is a secondary alcohol;
the polyvinyl alcohol has 80% of alcoholysis degree, 400% of polymerization degree and less than or equal to 1% of volatile component;
the preparation method of the high-concentration carboxyl hydroxyl polymer solution comprises the following steps: according to parts by mass, 10 parts of carboxylated chitosan and 2 parts of hydroxypropyl-beta-cyclodextrin are stirred and dissolved in 60 parts of deionized water, and then 0.3 part of polymethacryloxyethyl trimethyl ammonium chloride is slowly added to obtain a transparent solution, namely a high-concentration carboxyl hydroxyl polymer solution;
the carboxylation chitosan has carboxylation degree of 60% and insoluble substance less than 0.3%.
2. Adhesive composition formulation method
According to the weight parts of each raw material in the formula of the adhesive composition, firstly adding a hyperbranched polyesteramide aqueous solution into a mixing kettle, then adding deionized water, polyvinyl alcohol, methoxy polyethylene glycol ether sodium salt, polydiallyldimethylammonium chloride, a polyether-dimethylsiloxane graft copolymer, a high-concentration carboxyhydroxy polymer solution and tris (2, 4-di-tert-butylphenyl) phosphite, mixing and stirring at the rotating speed of 3000 r/min for 15 minutes, and then continuously stirring for 40 minutes to obtain the adhesive composition.
Example 3: adhesive composition for lithium ion battery and preparation method thereof
The method comprises the following steps:
1. adhesive composition
The adhesive composition comprises the following specific formula in parts by weight:
50 parts of hyperbranched polyesteramide aqueous solution
6 parts of polyvinyl alcohol
10 parts of polydiallyldimethylammonium chloride
8 parts of a high-concentration solution of a carboxyhydroxypolymer
6 parts of methoxy polyglycol ether sodium salt
5 parts of a polyether-dimethylsiloxane graft copolymer
4 parts of tackifier
2 parts of tris (2, 4-di-tert-butylphenyl) phosphite
60 parts of deionized water
The mass concentration of the hyperbranched polyesteramide in the hyperbranched polyesteramide aqueous solution is 50%;
the hyperbranched polyamide is a copolymer of succinic anhydride and diisopropanolamine, the number average molecular weight of the hyperbranched polyamide is 1200g/mol, and a terminal functional group is a secondary alcohol;
the polyvinyl alcohol has an alcoholysis degree of 92 percent, a polymerization degree of 900 and a volatile component of less than or equal to 1 percent;
the preparation method of the high-concentration carboxyl hydroxyl polymer solution comprises the following steps: in parts by mass, 20 parts of carboxylated chitosan and 10 parts of hydroxypropyl-beta-cyclodextrin are stirred and dissolved in 85 parts of deionized water, and then 0.9 part of polymethacryloxyethyltrimethyl ammonium chloride is slowly added to obtain a transparent solution, namely a high-concentration carboxyl hydroxyl polymer solution;
the carboxylation degree of the carboxylated chitosan is 80 percent, and insoluble substances are less than 0.3 percent;
the tackifier is sodium alginate.
2. Adhesive composition formulation method
According to the weight parts of the raw materials in the formula of the adhesive composition, firstly adding an aqueous solution of hyperbranched polyesteramide into a mixing kettle, then adding deionized water, polyvinyl alcohol, methoxy polyethylene glycol ether sodium salt, polydiallyldimethylammonium chloride, a graft copolymer of polyether and dimethyl siloxane, a high-concentration carboxyl hydroxyl polymer solution and tris (2, 4-di-tert-butylphenyl) phosphite, mixing and stirring at a rotating speed of 5500 revolutions per minute for 25 minutes, then adding a tackifier, and continuously stirring for 40-60 minutes to obtain the adhesive composition.
Comparative example 1:
on the basis of example 1, the modification was made in that 40 parts of an aqueous hyperbranched polyesteramide solution were replaced with 40 parts of an aqueous 30% strength by mass polyvinyl alcohol solution in equal amounts, and the other conditions were not changed.
Comparative example 2:
on the basis of example 1, the procedure was modified in that 6 parts of the highly concentrated carboxyhydroxypolymer solution were replaced by 6 parts of the hyperbranched polyesteramide aqueous solution in equal amounts, and the other conditions were not changed.
Comparative example 3:
on the basis of example 1, 5 parts of polydiallyldimethylammonium chloride were replaced by 5 parts of an aqueous hyperbranched polyesteramide solution in equal amounts, and the other conditions were unchanged.
Performance evaluation:
1. preparation of positive and negative electrode plates of lithium ion battery
The binder composition for lithium ion batteries obtained in the above examples 1, 2 and 3 and comparative examples 1, 2 and 3 was prepared by respectively weighing 100 parts of the binder composition for lithium ion batteries, adding 92 parts of a lithium iron phosphate powder material in batches, mixing, grinding into a slurry, uniformly coating the slurry on a clean aluminum foil, drying at 90 ± 10 ℃, and compacting to obtain a lithium iron phosphate positive electrode sheet;
the binder compositions for lithium ion batteries obtained in the above examples 1, 2 and 3 and comparative examples 1, 2 and 3 were prepared by respectively weighing 80 parts, adding 95 parts of graphite negative electrode material in batches, mixing and grinding into slurry, uniformly coating on a clean copper foil, drying at 90 ± 10 ℃, and compacting to obtain a graphite negative electrode sheet.
2. Assembled lithium ion battery
Cutting the manufactured positive and negative electrode plates of the lithium ion battery into electrode plates with a certain area according to the size of the battery capacity specification, manufacturing a lithium iron phosphate/graphite winding type lithium ion battery by using a Cellgard-2400 battery diaphragm, packaging the lithium ion battery by using an aluminum plastic film, carrying out vacuum drying at the temperature of 80 +/-10 ℃ for 10-72 hours, transferring the lithium ion battery into a dry glove box filled with argon, and injecting electrolyte, wherein the electrolyte comprises LiPF 6/Ethyl Methyl Carbonate (EMC) + Ethylene Carbonate (EC) + diethyl carbonate (DEC), and the EMC: EC: DEC =1:1:1 (volume ratio), so as to obtain the lithium ion battery.
3. Measurement of adhesive Strength
Electrode sheets prepared from the adhesives obtained in examples 1, 2 and 3 were cut into a 10cm × 2cm long strip, a steel sheet 1mm thick was bonded to the collector side with a double-sided tape, a transparent adhesive tape was attached to the coating layer side, and the sheet was peeled in a 180 ° direction at a speed of 100mm/min with a tensile tester to measure the peel stress.
4. Measurement of flexibility of adhesive after curing
A mandrel with the diameter phi of 3mm is placed on one side of the current collector of the rolled pole piece of the example and the comparative example, and
and (3) a bending test, wherein the state of the pole piece is observed through an optical microscope, the pole piece is good and marked as O, and the pole piece is good and is marked as X when the pole piece is peeled or cracked.
5. Evaluation of Battery Performance
And testing the first coulombic efficiency of the charge-discharge cycle and the capacity retention rate after 50 cycles of the prepared lithium iron phosphate/graphite winding type lithium ion battery by adopting a constant current method, and recording the ratio of the thickness increase value of the pole piece in the lithium-embedded state of the pole piece to the thickness of the pole piece before charge and discharge as the expansion rate (%) of the pole piece after 50 cycles of charge and discharge.
The results of the above tests are shown in the following table:
Claims (3)
1. an adhesive composition for a lithium ion battery, characterized in that: the adhesive composition for the lithium ion battery comprises the following components in parts by weight:
20-50 parts of hyperbranched polyesteramide aqueous solution
0.5-6 parts of polyvinyl alcohol
1-10 parts of poly (diallyldimethylammonium chloride)
3-8 parts of high-concentration carboxyl hydroxyl polymer solution
0.1-6 parts of methoxy polyethylene glycol ether sodium salt
0.1-5 parts of polyether and dimethyl siloxane graft copolymer
0-4 parts of tackifier
0.1 to 2 parts of tris (2, 4-di-tert-butylphenyl) phosphite
30-60 parts of deionized water;
the preparation method of the high-concentration carboxyl hydroxyl polymer solution comprises the following steps: according to parts by mass, 10-20 parts of carboxylated chitosan and 2-10 parts of hydroxypropyl-beta-cyclodextrin are stirred and dissolved in 60-85 parts of deionized water, and then 0.3-0.9 part of polymethacryloxyethyl trimethyl ammonium chloride is slowly added to obtain a transparent solution, namely a high-concentration carboxyl hydroxyl polymer solution.
2. The adhesive composition for lithium ion batteries according to claim 1, characterized in that:
the polyvinyl alcohol has an alcoholysis degree of 80-92%, a polymerization degree of 400-900 and a volatile component of less than or equal to 1%;
the carboxylation degree of the carboxylated chitosan is 60-80%, and insoluble substances are less than 0.3%;
the tackifier is one or more of carboxymethyl cellulose, hydroxypropyl guar gum, hydroxypropyl methyl cellulose, xanthan gum and sodium alginate.
3. The method for preparing an adhesive composition according to claim 1, characterized in that:
according to the weight parts of the raw materials in the formula of the adhesive composition, firstly adding an aqueous solution of hyperbranched polyesteramide into a mixing kettle, then adding deionized water, polyvinyl alcohol, methoxy polyethylene glycol ether sodium salt, polydiallyldimethylammonium chloride, a graft copolymer of polyether and dimethyl siloxane, a high-concentration carboxyl hydroxyl polymer solution and tris (2, 4-di-tert-butylphenyl) phosphite, mixing and stirring at the rotating speed of 3000-5500 rpm for 15-25 minutes, then adding a tackifier, and continuously stirring for 40-60 minutes to obtain the adhesive composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210291636.0A CN114614016A (en) | 2022-03-24 | 2022-03-24 | Adhesive composition for lithium ion battery and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210291636.0A CN114614016A (en) | 2022-03-24 | 2022-03-24 | Adhesive composition for lithium ion battery and preparation method thereof |
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| Publication Number | Publication Date |
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| CN114614016A true CN114614016A (en) | 2022-06-10 |
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| CN202210291636.0A Withdrawn CN114614016A (en) | 2022-03-24 | 2022-03-24 | Adhesive composition for lithium ion battery and preparation method thereof |
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2022
- 2022-03-24 CN CN202210291636.0A patent/CN114614016A/en not_active Withdrawn
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Application publication date: 20220610 |