CN112194978A - High-heat-resistant coating slurry, high-temperature-resistant diaphragm for lithium battery and preparation method of high-temperature-resistant diaphragm - Google Patents
High-heat-resistant coating slurry, high-temperature-resistant diaphragm for lithium battery and preparation method of high-temperature-resistant diaphragm Download PDFInfo
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- CN112194978A CN112194978A CN202010864809.4A CN202010864809A CN112194978A CN 112194978 A CN112194978 A CN 112194978A CN 202010864809 A CN202010864809 A CN 202010864809A CN 112194978 A CN112194978 A CN 112194978A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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 discloses high-heat-resistant coating slurry, a high-temperature-resistant diaphragm for a lithium battery and a preparation method of the high-heat-resistant diaphragm, wherein the preparation method of the high-heat-resistant coating slurry comprises the following steps: uniformly mixing a first solvent and an inorganic ceramic material, and sanding to obtain a mixed solution; uniformly mixing polybenzimidazole, a pore-forming agent, a mixed solution and a second solvent to obtain the high-heat-resistant coating slurry, wherein the method for preparing the high-temperature-resistant diaphragm for the lithium battery comprises the following steps: and coating the high-heat-resistant coating slurry on two sides or one side of the polyolefin base film, and drying to obtain the high-temperature-resistant diaphragm for the lithium battery. According to the invention, through introducing polybenzimidazole, the polybenzimidazole is combined with the pore-forming agent, the mixed solution and the second solvent, the high temperature resistance of the diaphragm is improved synergistically, and the safety of the lithium battery is further improved.
Description
Technical Field
The invention belongs to the technical field of battery diaphragms, and particularly relates to high-heat-resistant coating slurry, a high-temperature-resistant diaphragm for a lithium battery and a preparation method of the high-temperature-resistant diaphragm.
Background
The lithium ion battery has the advantages of high power density, low self-discharge rate, no memory effect, stable discharge voltage and the like, and gradually replaces the traditional lead-acid storage battery and nickel-cadmium storage battery, thereby becoming the main choice of the secondary battery. The composition structure of the lithium ion battery comprises five major parts, namely a positive electrode, a negative electrode, an electrolyte, a diaphragm and a shell. Separators are key components of lithium ion batteries and are important determinants of battery capacity, cycling ability, and safety performance.
The demand for power cells in terms of high power output performance and safety presents a significant challenge for lithium batteries. The performance of the diaphragm determines the interface structure and the internal resistance of the battery, and further influences the key performances of the battery such as capacity, cycle performance, charge-discharge current density and the like. In the high-power discharge process, the local temperature of the battery reaches about 100 ℃, so that the cathode solid electrolyte interface protective film can be decomposed and release heat, the battery is further heated, the decomposition of substances such as organic electrolyte and the like and the melting of a diaphragm are caused, and the anode and the cathode are directly reacted and even explode. A puncture or impact experienced by the battery during use may also cause the battery voltage to drop momentarily. The sharp increase in current generates a large amount of heat, which causes the temperature to rapidly rise, thereby subjecting the battery separator to a high temperature state. Therefore, the separator is required to have better thermal dimensional stability, excellent interfacial properties and thermochemical stability for the safe operation of a power lithium battery.
The microporous film made of polyolefin material is a leading product in the current diaphragm market due to the characteristics of low production cost, excellent chemical and electrochemical stability, proper pore structure and the like. No matter polyethylene, polypropylene or other thermoplastic high polymer materials, the materials are all shrunk and deformed due to melting when the melting point is close to, and potential hidden danger is brought to the safety of the battery. Inorganic substances such as alumina, zirconia and the like are very stable in the range of 100 to 300 ℃, and micro/nano materials thereof are already marketed. The inorganic coating is covered on the surface of the polyolefin diaphragm, even if the organic basement membrane is melted in the process of charging and discharging of the battery, the inorganic coating can still keep the integrity of the diaphragm, the phenomenon of large-area positive/negative short circuit is prevented, and a feasible solution is provided for solving the safety of a high-power battery.
Disclosure of Invention
In order to solve the problem of severe thermal shrinkage of the separator, the invention aims to provide a preparation method of high-heat-resistance coating slurry.
It is another object of the present invention to provide a high heat-resistant coating paste obtained by the above preparation method.
Another object of the present invention is to provide a method of preparing a high temperature resistant separator for a lithium battery.
The invention also aims to provide the high-temperature-resistant separator for the lithium battery obtained by the method.
The purpose of the invention is realized by the following technical scheme.
A preparation method of high heat-resistant coating slurry comprises the following steps:
1) uniformly mixing a first solvent and an inorganic ceramic material, and sanding to obtain a mixed solution, wherein the inorganic ceramic material accounts for 20-70 wt% of the mixed solution, and the balance is the first solvent;
in the step 1), the first solvent and the inorganic ceramic material are uniformly mixed by stirring for 20-60 minutes.
In the step 1), the sanding time is 10-40 minutes.
In the step 1), the inorganic ceramic material is alumina, boehmite, magnesium hydroxide, silica or barium sulfate, and the first solvent is ethanol, isopropanol or dichloromethane.
2) Uniformly mixing polybenzimidazole, a pore-forming agent, a mixed solution and a second solvent to obtain the high-heat-resistance coating slurry, wherein the ratio of the polybenzimidazole, the pore-forming agent, the mixed solution and the second solvent is (7-40): (30-80): (15-40): (5-30).
In the step 2), the second solvent is N-methylpyrrolidone (NMP), dimethyl sulfoxide (DMSO), Dimethylformamide (DMF), or Dimethylacetamide (DMAC).
In the step 2), the polybenzimidazole, the pore-forming agent, the mixed solution and the second solvent are uniformly mixed by stirring for 30-90 minutes.
In the step 2), the pore-forming agent is triethyl phosphate or dimethyl carbonate.
The high heat-resistant coating slurry obtained by the preparation method.
The method for preparing the high-temperature-resistant diaphragm for the lithium battery comprises the steps of coating the high-temperature-resistant coating slurry on two sides or one side of a polyolefin base film, and drying to obtain the high-temperature-resistant diaphragm for the lithium battery.
In the above technical solution, the coating is roll coating.
In the technical scheme, the coating thickness is 1-8 microns.
In the technical scheme, the drying temperature is 40-90 ℃, and the drying time is 10-40 s.
The high-temperature-resistant diaphragm for the lithium battery obtained by the method.
According to the invention, through introducing polybenzimidazole, the polybenzimidazole is combined with the pore-forming agent, the mixed solution and the second solvent, the high temperature resistance of the diaphragm is improved synergistically, and the safety of the lithium battery is further improved.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
Benzimidazole procurement by Nanfengen New materials science and technology Limited
The mixer is double planet power mixer, the model: HY-DLH43L, manufacturer: guangzhou Hongyang mechanical science and technology Co Ltd
The sanding equipment is full ceramic nanometer grinding machine, model: PT-5L, a Producer of Dongguan City Deno mechanical Equipment Co., Ltd
Example 1
A preparation method of high heat-resistant coating slurry comprises the following steps:
1) mixing a first solvent and an inorganic ceramic material, stirring for 20 minutes until the mixture is uniformly mixed, and sanding for 20 minutes to obtain a mixed solution, wherein the inorganic ceramic material accounts for 30 wt% of the mixed solution, the balance is the first solvent, the inorganic ceramic material is alumina, and the first solvent is ethanol;
2) mixing polybenzimidazole, a pore-forming agent, a mixed solution and a second solvent, and stirring for 40 minutes until the mixture is uniform to obtain high-heat-resistant coating slurry, wherein the ratio of the polybenzimidazole, the pore-forming agent, the mixed solution and the second solvent is 9: 30: 17: 7, the second solvent is N-methyl pyrrolidone (NMP), and the pore-forming agent is triethyl phosphate.
A method for preparing a high-temperature-resistant diaphragm for a lithium battery comprises the steps of coating the high-temperature-resistant coating slurry prepared in the embodiment on one surface of a polyolefin base film in a roll coating mode, wherein the coating thickness is 2 micrometers, and drying at 50 ℃ for 15 seconds to obtain the high-temperature-resistant diaphragm for the lithium battery, wherein the polyolefin base film is a polyethylene film.
Example 2
A preparation method of high heat-resistant coating slurry comprises the following steps:
1) mixing a first solvent and an inorganic ceramic material, stirring for 20 minutes until the mixture is uniformly mixed, and sanding for 25 minutes to obtain a mixed solution, wherein the inorganic ceramic material in the mixed solution accounts for 50 wt% and the balance is the first solvent, the inorganic ceramic material is boehmite, and the first solvent is isopropanol;
2) mixing polybenzimidazole, a pore-forming agent, a mixed solution and a second solvent, and stirring for 40 minutes until the mixture is uniform to obtain high-heat-resistant coating slurry, wherein the ratio of the polybenzimidazole, the pore-forming agent, the mixed solution and the second solvent is 22: 41: 21: 13, the second solvent is Dimethylformamide (DMF), and the pore-forming agent is dimethyl carbonate.
A method for preparing a high-temperature-resistant diaphragm for a lithium battery comprises the steps of coating the high-temperature-resistant coating slurry prepared in the embodiment on one surface of a polyolefin base film in a roll coating mode, wherein the coating thickness is 3 micrometers, and drying at 60 ℃ for 10 seconds to obtain the high-temperature-resistant diaphragm for the lithium battery, wherein the polyolefin base film is a polyethylene film.
Example 3
A preparation method of high heat-resistant coating slurry comprises the following steps:
1) mixing a first solvent and an inorganic ceramic material, stirring for 30 minutes until the mixture is uniformly mixed, and sanding for 25 minutes to obtain a mixed solution, wherein the inorganic ceramic material accounts for 60 wt% of the mixed solution, the balance is the first solvent, the inorganic ceramic material is magnesium hydroxide, and the first solvent is dichloromethane;
2) mixing polybenzimidazole, a pore-forming agent, a mixed solution and a second solvent, and stirring for 50 minutes until the mixture is uniform to obtain high-heat-resistance coating slurry, wherein the ratio of the polybenzimidazole, the pore-forming agent, the mixed solution and the second solvent is 33: 45: 23: 21, the second solvent is Dimethylacetamide (DMAC), and the pore-forming agent is dimethyl carbonate.
The method for preparing the high-temperature-resistant diaphragm for the lithium battery comprises the steps of coating the high-temperature-resistant coating slurry prepared in the embodiment on two sides of a polyolefin base film in a roll coating mode, wherein the coating thickness of each side is 2 micrometers, and drying at 50 ℃ for 15 seconds to obtain the high-temperature-resistant diaphragm for the lithium battery, wherein the polyolefin base film is a polypropylene film.
The high-temperature-resistant diaphragm for the lithium battery obtained in the embodiment 1-3 is tested, and the test result is as follows:
the decomposition voltage of the high temperature-resistant separator for lithium battery obtained in example 1 was 4.7VThe thermal shrinkage at 130 ℃ for 1 hour is 0.9%, the thermal shrinkage at 150 ℃ for 1 hour is 1.7%, the film breaking temperature is 230 ℃, the liquid absorption rate is 170%, and the ionic conductivity: 1.1X 10-3s/cm-1. Lithium iron phosphate is used as a positive electrode, graphite is used as a negative electrode, a lithium hexafluorophosphate solution with the solute concentration of 1mol/L is used as an electrolyte (the solvent of the electrolyte is a mixed solution of EC (ethylene carbonate) and DMC (dimethyl carbonate), the mass ratio of the EC to DMC is 1: 1.), a battery is assembled, the capacity retention rate is 98% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 99.43% after the battery is cycled for 20 circles.
The decomposition voltage of the high temperature-resistant separator for a lithium battery obtained in example 2 was 4.7V, the thermal shrinkage at 130 ℃ for 1 hour was 0.6%, the thermal shrinkage at 150 ℃ for 1 hour was 1.4%, the film rupture temperature was 240 ℃, the liquid absorption rate was 180%, and the ionic conductivity: 1.1X 10- 3s/cm-1. The lithium iron phosphate is used as a positive electrode, graphite is used as a negative electrode, a lithium hexafluorophosphate solution with the solute concentration of 1mol/L is used as an electrolyte to assemble the battery, the capacity retention rate is 99% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 98.48% after the battery is cycled for 20 circles.
The decomposition voltage of the high-temperature-resistant separator for a lithium battery obtained in example 3 was 4.7V, the thermal shrinkage at 130 ℃ for 1 hour was 0.4%, the thermal shrinkage at 150 ℃ for 1 hour was 1.2%, the film rupture temperature was 245 ℃, the liquid absorption rate was 184%, and the ionic conductivity: 1.1X 10- 3s/cm-1. The lithium iron phosphate is used as a positive electrode, graphite is used as a negative electrode, a lithium hexafluorophosphate solution with the solute concentration of 1mol/L is used as an electrolyte to assemble the battery, the capacity retention rate is 99% after the battery is cycled for 100 circles under the multiplying power of 0.5C, and the average coulombic efficiency is 99.57% after the battery is cycled for 20 circles.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The preparation method of the high heat-resistant coating slurry is characterized by comprising the following steps:
1) uniformly mixing a first solvent and an inorganic ceramic material, and sanding to obtain a mixed solution, wherein the inorganic ceramic material accounts for 20-70 wt% of the mixed solution, and the balance is the first solvent;
2) uniformly mixing polybenzimidazole, a pore-forming agent, a mixed solution and a second solvent to obtain the high-heat-resistance coating slurry, wherein the ratio of the polybenzimidazole, the pore-forming agent, the mixed solution and the second solvent is (7-40): (30-80): (15-40): (5-30).
2. The method according to claim 1, wherein in the step 1), the first solvent and the inorganic ceramic material are uniformly mixed by stirring for 20 to 60 minutes, and the sanding time is 10 to 40 minutes.
3. The production method according to claim 1, wherein in the step 1), the inorganic ceramic material is alumina, boehmite, magnesium hydroxide, silica or barium sulfate, and the first solvent is ethanol, isopropanol or dichloromethane;
in the step 2), the second solvent is N-methylpyrrolidone, dimethyl sulfoxide, dimethylformamide or dimethylacetamide, and the pore-forming agent is triethyl phosphate or dimethyl carbonate.
4. The method according to claim 1, wherein in the step 2), the polybenzimidazole, the pore-forming agent, the mixed solution and the second solvent are uniformly mixed by stirring for 30 to 90 minutes.
5. The high heat-resistant coating slurry obtained by the preparation method according to any one of claims 1 to 4.
6. A method for preparing a high temperature-resistant separator for a lithium battery, characterized in that the high temperature-resistant coating slurry according to claim 5 is coated on both sides or one side of a polyolefin-based film and dried to obtain a high temperature-resistant separator for a lithium battery.
7. The method of claim 6, wherein the coating is roll coating.
8. The method of claim 6, wherein the coating has a thickness of 1 to 8 microns.
9. The method according to claim 6, wherein the drying temperature is 40 to 90 ℃ and the drying time is 10 to 40 s.
10. A high temperature resistant separator for a lithium battery obtained by the method of any one of claims 6 to 9.
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Application publication date: 20210108 |