CN114539940B - Preparation method of high-temperature-resistant adhesive tape for lithium battery - Google Patents
Preparation method of high-temperature-resistant adhesive tape for lithium battery Download PDFInfo
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- CN114539940B CN114539940B CN202210105745.9A CN202210105745A CN114539940B CN 114539940 B CN114539940 B CN 114539940B CN 202210105745 A CN202210105745 A CN 202210105745A CN 114539940 B CN114539940 B CN 114539940B
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/33—Applications of adhesives in processes or use of adhesives in the form of films or foils for batteries or fuel cells
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/41—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the carrier layer
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The application relates to the technical field of adhesive tapes, in particular to a preparation method of a high-temperature-resistant adhesive tape for a lithium battery, which comprises the following steps: step 1: weighing polyester and silicone oil, heating to 185-200 ℃, and mixing for 0.8-2.5h to obtain a mixture A; step 2: weighing PMDA, hexagonal boron nitride, polyethylene glycol and isopropanol, vibrating for 12-18min, heating to 50-65 ℃, adding diaminodiphenyl ether, vibrating for 8-15min, heating to 75-85 ℃, reacting at constant temperature for 1.5-3.5h, and distilling to obtain a mixture B; adding the mixture B into the mixture A in 3-5 batches, heating to 205-220 ℃, reacting for 2-3h, and preparing a film to obtain a substrate; and 3, step 3: the base material is activated through the activating solution, the adhesive is coated on the base material, and the high-temperature-resistant adhesive tape is obtained through drying and rolling.
Description
Technical Field
The application relates to the technical field of adhesive tapes, in particular to a preparation method of a high-temperature-resistant adhesive tape for a lithium battery.
Background
Common adhesive tapes can be classified according to their effects: high temperature resistant adhesive tape, double-sided adhesive tape, insulating adhesive tape, special adhesive tape, pressure sensitive adhesive tape, die cutting adhesive tape and the like, and different effects are suitable for different industry requirements. The adhesive tape is coated with a layer of adhesive on the surface to enable the adhesive tape to stick to the article.
When present lithium cell is used for cell-phone, computer and flat board, quick charge-discharge of lithium cell in the use, the security of taking into account the lithium cell generally can adopt the lithium cell sticky tape, because cell-phone, computer and flat board lithium cell when using emit the heat, therefore the lithium cell sticky tape need work under the high temperature condition for a long time, but present lithium cell sticky tape heat resistance is poor for the life of lithium cell sticky tape shortens.
Disclosure of Invention
In order to improve the high temperature resistance, the application provides a preparation method of a high temperature resistant adhesive tape for a lithium battery.
The preparation method of the high-temperature-resistant adhesive tape for the lithium battery adopts the following technical scheme:
a preparation method of a high-temperature-resistant adhesive tape for a lithium battery comprises the following steps:
step 1: weighing 55-75 parts of polyester and 3-8 parts of silicone oil according to parts by weight, heating to 185-200 ℃, and mixing for 0.8-2.5h to obtain a mixture A;
step 2: weighing 25-35 parts of PMDA, 5-11 parts of hexagonal boron nitride, 0.5-1 part of polyethylene glycol and 80-150 parts of isopropanol according to parts by weight, vibrating for 12-18min, heating to 50-65 ℃, adding 15-30 parts of diaminodiphenyl ether, vibrating for 8-15min, heating to 75-85 ℃, reacting at constant temperature for 1.5-3.5h, and distilling to obtain a mixture B; adding the mixture B into the mixture A in 3-5 batches, heating to 205-220 ℃, reacting for 2-3h, and preparing a film to obtain a substrate;
and step 3: activating the base material by the activating solution, coating the adhesive on the base material, drying and rolling to obtain the high-temperature-resistant adhesive tape.
The preparation method is simple to operate and high in production efficiency, the obtained high-temperature-resistant adhesive tape has good high-temperature-resistant performance, insulating performance and heat-conducting performance, the durability of the high-temperature-resistant adhesive tape when the high-temperature-resistant adhesive tape is used for a lithium battery is improved, meanwhile, due to the insulating performance and the heat-conducting performance of the high-temperature-resistant adhesive tape, the possibility of electric leakage of the lithium battery is reduced, the heat-conducting effect can be achieved, and the heat dissipation effect of the lithium battery when the lithium battery is used for a mobile phone or a flat plate is improved. The polyester has ageing resistance, high temperature resistance and insulating property, so that the obtained adhesive tape has insulating property and high temperature resistance, the ageing possibility and the ageing possibility of the high temperature resistant adhesive tape are reduced, the silicone oil has heat resistance, insulating property and smaller surface tension, and the insulating property and the high temperature resistance of the obtained adhesive tape are further improved.
The polyimide is prepared by using the iso-diol as a solvent and the PMDA and the diamino diphenyl ether as raw materials for preparing polyimide, and the polyimide has good insulating property and high temperature resistance, so that the high temperature resistant adhesive tape has good high temperature resistance and insulating property. And in the process of preparing the polyimide, hexagonal boron nitride is added, so that the hexagonal boron nitride is uniformly dispersed in the polyimide, meanwhile, polyethylene glycol is used as a dispersing agent, so that the dispersing effect is achieved, the hexagonal boron nitride is further uniformly dispersed, the hexagonal boron nitride has good insulating property, high temperature resistance and heat conductivity, the high temperature resistance and insulating property of the adhesive tape are improved, the high temperature resistant adhesive tape has heat conductivity, the high temperature resistant adhesive tape can be used in a lithium battery for a long time, the possibility of electric leakage is reduced, the heat conductivity is achieved, and the heat dissipation effect when the lithium battery is used in a mobile phone or a flat plate is improved.
The surface of the base material is activated through the activating solution, so that the activity of the surface of the base material is improved, the adhesive tape is easier to adhere to the adhesive, the adhesive has better adhesion and stripping resistance, and the phenomenon that the adhesive tape is separated from a mobile phone battery is reduced.
Preferably, the hexagonal boron nitride is modified hexagonal boron nitride, and the modified hexagonal boron nitride is prepared from the following raw materials in parts by weight:
hexagonal boron nitride: 23 to 30 portions of
Mica: 1.5 to 3.5 portions
Silane coupling agent: 0.8 to 1.3 portions of
Titanate coupling agent: 0.3 to 1.2 portions of
Polyvinylpyrrolidone: 75 to 100 portions of
Methyl pyrrolidone: 18-25
Methanol: 25-50 parts of
Ethanol: 120-160 parts.
Modified hexagonal boron nitride obtained through the technical scheme has better dispersibility, because hexagonal boron nitride has great inertia, and then be difficult to disperse in the polymer, and when filling the filled polymer, it is inhomogeneous to appear dispersing easily, make the high temperature resistance of the high temperature resistant adhesive tape that obtains, heat conductivility and insulating properties poor, and then this application obtains through above-mentioned scheme during modified hexagonal boron nitride fills the raw materials of high temperature resistant adhesive tape easily, make this high temperature resistant adhesive tape have better insulating properties, heat conductivility and high temperature resistance.
Polyvinylpyrrolidone is an organic solvent with better polarity, so that the surface activity of hexagonal boron nitride can be reduced, methyl pyrrolidone is a polar solvent, so that the inertia of hexagonal boron nitride can be reduced, and meanwhile, methanol contains hydroxyl, so that the surface activity of hexagonal boron nitride can be further improved.
The silane coupling agent can improve the compatibility of an inorganic phase and an organic phase, further improve the dispersibility of the obtained modified hexagonal boron nitride in a polymer, uniformly disperse the hexagonal boron nitride in a raw material system of the high-temperature-resistant adhesive tape, and further improve the high-temperature resistance, the heat conduction performance and the insulation performance of the high-temperature-resistant adhesive tape.
Preferably, the modified hexagonal boron nitride is prepared by the following steps:
step A: weighing 23-30 parts of hexagonal boron nitride and 75-100 parts of polyvinylpyrrolidone according to the weight parts of the agent, and oscillating for 3-8 hours to obtain pretreated hexagonal boron nitride;
and B: weighing 18-25 parts of methyl pyrrolidone and 25-50 parts of methanol according to the weight parts of the agent, adding the methyl pyrrolidone and the methanol into the pretreated hexagonal boron nitride obtained in the step A, oscillating for 15-18h, filtering and drying to obtain a mixture A;
and C: and (3) weighing 1.5-3.5 parts of mica, 0.8-1.3 parts of silane coupling agent and 0.3-1.2 parts of titanate coupling agent according to parts by weight, dissolving in 120-160 parts of ethanol, adding the mixture A obtained in the step (B), shaking for 1-1.5h, filtering, and drying filter residues to obtain the modified hexagonal boron nitride.
The preparation method has the advantages of simple operation and high production efficiency, and the obtained modified hexagonal boron nitride has better dispersibility, can be well filled in the high-temperature-resistant adhesive tape, improves the high-temperature resistance, the insulating property and the heat-conducting property of the high-temperature-resistant adhesive tape, can reduce the possibility of electric leakage when the high-temperature-resistant adhesive tape is used for a mobile phone battery, and has better high-temperature resistance and heat-conducting property.
In the step A, polyvinylpyrrolidone is used as an organic solution and has good polarity, so that the polar interaction of hexagonal boron nitride can be improved, hexagonal boron nitride is pretreated in a vibration mode, and the hexagonal boron nitride starts to be stripped, the methylpyrrolidone in the step is a polar solvent with strong selectivity and good stability, so that the stripping effect of the hexagonal boron nitride can be improved, and the methanol contains hydroxyl, so that the hexagonal boron nitride is hydroxylated in the stripping process, the surface activity of the hexagonal boron nitride is improved, the inertia of the hexagonal boron nitride is reduced, and the obtained modified boron nitride can be well dispersed in the solution.
Furthermore, the silane coupling agent and the titanate coupling agent act synergistically, so that the dispersibility of the obtained modified hexagonal boron nitride in the polymer can be improved, the modified hexagonal boron nitride of the prepared high-temperature-resistant adhesive tape is uniformly dispersed, the insulating property and the high-temperature resistance of the high-temperature-resistant adhesive tape are improved, and the mica also has the insulating property, the high-temperature resistance and the heat-conducting property and improves the insulating property, the high-temperature resistance and the heat-conducting property of the high-temperature-resistant adhesive tape.
Preferably, the preparation of the hexagonal boron nitride comprises the following steps:
step A: weighing 20-25 parts of ammonium borate and 3-8 parts of melamine according to parts by weight, uniformly mixing, introducing nitrogen, reacting for 3-5 hours at 380-420 ℃, and cooling to obtain a mixture I;
and B, step B: weighing 80-100 parts by weight of sodium hydroxide, adding into the mixture I obtained in the step A, soaking for 5-10min, filtering, reacting the filter residue at 2000-2200 ℃ for 8-13h under the protection of nitrogen, cooling, and sieving by 50-100 meshes to obtain the hexagonal boron nitride.
The preparation method has the advantages of simple operation and high production efficiency, the purity of the hexagonal boron nitride obtained by the scheme is high, and the hexagonal boron nitride obtained by modification has good high-temperature resistance, insulating property and heat conductivity.
Preferably, the activating solution is ammonia water and hexametaphosphoric acid in a weight ratio of 10-15.
The ratio of above parts by weight is the ratio of the preferred parts by weight of this application, and the aqueous ammonia is weak alkaline, can activate the base film surface, and sodium hexametaphosphate has stability for the base film can activate in the aqueous ammonia well, and the aqueous ammonia can reduce the activity on base film surface, makes the adhesive can closely with the base film adhesion.
Preferably, the adhesive is acrylic glue or silica gel glue.
The acrylic glue has the excellent characteristics of room temperature curing, convenient operation, high bonding strength, water resistance, heat resistance, cold resistance, aging resistance, acid and alkali resistance and the like; make the substrate can carry out coating ya keli glue at normal atmospheric temperature, improve the convenience of coating, and adopt silica gel glue to have high temperature resistant, electrical insulation, weatherability, fire-retardant, corrosion-resistant etc. excellent characteristics, and then with substrate zonulae occludens for high temperature resistant adhesive tape can adhere well on the lithium cell.
Preferably, the silicone oil is phenyl silicone oil or methyl hydrogen-containing silicone oil.
The phenyl silicone oil and the methyl hydrogen-containing silicone oil have excellent heat resistance, electric insulation performance, weather resistance, smaller surface tension and the like, so that the high-temperature-resistant adhesive tape can be used as a defoaming agent, and the possibility of generating bubbles in the raw materials of the high-temperature-resistant adhesive tape is reduced.
Preferably, the polyester consists of PBT and PET.
The PBT polybutylene terephthalate is milk white semitransparent to opaque semi-crystalline thermoplastic polyester and has high temperature resistance and insulating property. The PET has certain crystal orientation capability, so that the PET has high film forming property, high temperature resistance and insulating property, and meanwhile, the PBT and the PET act synergistically, so that the high-temperature-resistant adhesive tape has high insulating property and high temperature resistance.
Preferably, the weight part ratio of the PBT to the PET is 1.2-1.5.
The proportion is the ratio of the better parts by weight of the application, and the PBT and the PET have better high-temperature resistance and insulating property under the proportion.
Preferably, the film forming method in step 3 is: the obtained raw material is extruded at 180-195 ℃ and then calendered.
The base film obtained by the scheme has better high temperature resistance, heat conductivity and insulating property.
In summary, the present application has the following beneficial effects:
1. according to the application, in the process of preparing polyimide, the hexagonal boron nitride is added, so that the hexagonal boron nitride is uniformly dispersed in the polyimide, meanwhile, the polyethylene glycol is used as a dispersing agent and has a dispersing effect, and further the hexagonal boron nitride is uniformly dispersed.
2. The surface activity of the hexagonal boron nitride is further improved through pretreatment, the inertia of the hexagonal boron nitride is reduced, and the obtained modified boron nitride can be well dispersed in a solution. Furthermore, the dispersibility of the obtained modified hexagonal boron nitride in the polymer can be improved through the synergistic effect of the silane coupling agent and the titanate coupling agent, so that the modified hexagonal boron nitride of the prepared high-temperature-resistant adhesive tape is uniformly dispersed, and the insulating property and the high-temperature-resistant property of the high-temperature-resistant adhesive tape are improved.
Detailed Description
The following preparations and examples provide further details of the source of part of the starting materials for the present application:
titanate coupling agent, manufacturer: dongguan city Dinghai plastic chemical Co., ltd, model: 201;
acrylic glue, manufacturer: the technology company, toguan, zhu-Yi New Material, inc., brand: zhuoli;
silica gel glue, manufacturer: dongguan Yihe new material science and technology limited company, model:
YH-308AB；
hexagonal boron nitride (commercially available hexagonal boron nitride in table 1), manufacturer: zhengzhou City Yuanfeng chemical Co., ltd.
Preparation examples
Preparation of hexagonal boron nitride
Preparation example 1
A hexagonal boron nitride comprising the steps of:
step A: weighing 2.3Kg of ammonium borate and 0.5Kg of melamine, putting the ammonium borate and the melamine into a reaction kettle, uniformly mixing, introducing nitrogen, reacting for 4 hours at 400 ℃, and cooling to obtain a mixture I;
and B: and B, weighing 9Kg of sodium hydroxide, adding the sodium hydroxide into the mixture I obtained in the step A, soaking for 8min, filtering, introducing nitrogen, reacting the filter residue at 2100 ℃ for 10h, cooling, and sieving by a 80-mesh sieve to obtain the hexagonal boron nitride.
Preparation example 2
A hexagonal boron nitride comprising the steps of:
step A: weighing 2Kg of ammonium borate and 0.5Kg of melamine, putting the ammonium borate and the melamine into a reaction kettle, uniformly mixing, introducing nitrogen, reacting for 3 hours at 400 ℃, and cooling to obtain a mixture I;
and B: and B, weighing 9Kg of sodium hydroxide, adding the sodium hydroxide into the mixture I obtained in the step A, soaking for 5min, filtering, introducing nitrogen, reacting the filter residue at 2000 ℃ for 8h, cooling, and sieving by a 50-mesh sieve to obtain the hexagonal boron nitride.
Preparation example 3
A hexagonal boron nitride comprising the steps of:
step A: weighing 2.5Kg of ammonium borate and 0.8Kg of melamine, putting the ammonium borate and the melamine into a reaction kettle, uniformly mixing, introducing nitrogen, reacting for 5 hours at 420 ℃, and cooling to obtain a mixture I;
and B: and B, weighing 10Kg of sodium hydroxide, adding the sodium hydroxide into the mixture I obtained in the step A, soaking for 10min, filtering, introducing nitrogen, reacting the filter residue at 2200 ℃ for 13h, cooling, and sieving by a 100-mesh sieve to obtain the hexagonal boron nitride.
Preparation example of modified hexagonal boron nitride
Preparation example 4
The preparation method of the modified hexagonal boron nitride comprises the following steps:
step A: weighing 2.6Kg of hexagonal boron nitride and 9.0Kg of polyvinylpyrrolidone in preparation example 2, and placing them in 30000Hz ultrasonic wave to vibrate for 5h to obtain pretreated hexagonal boron nitride;
and B: weighing 2.2Kg of methyl pyrrolidone and 4.0Kg of methanol, adding the methyl pyrrolidone and the methanol into the pretreated hexagonal boron nitride obtained in the step A, placing the mixture into 30000Hz ultrasonic waves to vibrate for 16 hours, filtering and drying to obtain a mixture A;
and C: and B, weighing 0.2Kg of mica, 0.1Kg of silane coupling agent and 0.08Kg of titanate coupling agent, dissolving in 13Kg of ethanol, adding the mixture A obtained in the step B, placing the mixture A into 30000Hz ultrasonic waves, oscillating for 1.2h, filtering by using a Buchner funnel and a suction pump in a matched manner, and drying filter residues in an oven at 50 ℃ to obtain the modified hexagonal boron nitride.
Preparation examples 5 to 7
Preparation examples 5 to 7 differed from preparation example 4 in that: the dosage of the raw materials is different from the oscillation time in each step, and is specifically shown in table 1;
TABLE 1 dosage (Kg) of raw materials and shaking time in each step for preparation examples 4-7
Preparation of comparative example
Preparation of comparative example 1
Production comparative example 1 differs from production example 4 in that the production method of production comparative example 1 is as follows:
step A: weighing 2.6Kg of hexagonal boron nitride and 15.2Kg of polyvinylpyrrolidone in preparation example 2, and placing the hexagonal boron nitride and the polyvinylpyrrolidone in 30000Hz ultrasonic waves to vibrate for 21h to obtain a mixture A;
and B: and B, weighing 0.2Kg of mica, 0.1Kg of silane coupling agent and 0.08Kg of titanate coupling agent, dissolving in 13Kg of ethanol, adding the mixture A obtained in the step A, placing the mixture A into 30000Hz ultrasonic waves, oscillating for 1.2h, filtering by using a Buchner funnel and a suction pump in a matched manner, and drying filter residues in an oven at 50 ℃ to obtain the modified hexagonal boron nitride.
Preparation of comparative example 2
Production comparative example 2 differs from production example 4 in that the production method of production comparative example 2 is as follows:
step A: weighing 6.2Kg of methyl pyrrolidone, 9.0Kg of methanol and 2.6Kg of hexagonal boron nitride, placing the mixture into 30000Hz ultrasonic waves for oscillation for 21 hours, filtering and drying to obtain a mixture A;
and B, step B: and B, weighing 0.2Kg of mica, 0.1Kg of silane coupling agent and 0.08Kg of titanate coupling agent, dissolving in 13Kg of ethanol, adding the mixture A obtained in the step A, placing the mixture A into 30000Hz ultrasonic waves, oscillating for 1.2h, filtering by using a Buchner funnel and a suction pump in a matched manner, and drying filter residues in an oven at 50 ℃ to obtain the modified hexagonal boron nitride.
Preparation of comparative example 3
Preparation of comparative example 2 differs from preparation example 4 in that the preparation method of comparative example 2 is as follows:
step A: weighing 15.2Kg of methyl pyrrolidone and 2.6Kg of hexagonal boron nitride, placing the mixture into 30000Hz ultrasonic waves for oscillation for 16 hours, filtering and drying to obtain a mixture A;
and C: and (3) weighing 0.2Kg of mica, 0.1Kg of silane coupling agent and 0.08Kg of titanate coupling agent, dissolving the mica, the silane coupling agent and the titanate coupling agent in 13Kg of ethanol, adding the mixture A obtained in the step (B), placing the mixture A into 30000Hz ultrasonic waves, oscillating the mixture A for 1.2h, filtering the mixture A by using a Buchner funnel and a suction pump in a matched manner, and drying filter residues in an oven at the temperature of 50 ℃ to obtain the modified hexagonal boron nitride.
Examples
Example 1
The preparation method of the high-temperature-resistant adhesive tape comprises the following steps:
step 1: weighing 25.2Kg of PBT, 34.8Kg of PET and 5Kg of methyl hydrogen-containing silicone oil, putting into an internal mixer, heating to 190 ℃, and mixing for 2h to obtain a mixture A;
step 2: weighing 30Kg of PMDA, 8Kg of hexagonal boron nitride, 0.7Kg of polyethylene glycol and 120Kg of isopropanol, putting the weighed materials into ultrasonic waves, vibrating the materials for 15min, heating the materials to 60 ℃, adding 25Kg of diaminodiphenyl ether, putting the materials into the ultrasonic waves, vibrating the materials for 10min, transferring the materials into a reaction kettle, heating the materials to 60 ℃, reacting the materials at constant temperature for 2h, heating the materials to 100 ℃, and distilling a micromolecule product and the isopropanol to obtain a mixture B; adding the mixture B into the mixture A in 4 batches, uniformly mixing every time one batch is added, adding the other batch, heating to 210 ℃ after the mixture is completely added, reacting for 2.5 hours, putting the obtained raw materials into an extruder, extruding at 190 ℃, and calendering by a calender to obtain a base material;
and step 3: activating the substrate in activating solution for 15min, coating the acrylic glue on the substrate by adopting a mixed wheel gluing mode, wherein the coating weight is 120g/m 2 And (5) carrying out air drying at 50 ℃ in an air dryer, and rolling to obtain the high-temperature-resistant adhesive tape.
Examples 2 to 8
Examples 2-8 differ from example 1 in that: the dosage of the raw materials is different from the temperature, the reaction time, the mixing time and the oscillation time in each step;
TABLE 2 amounts (Kg) of starting materials of examples 1-8
TABLE 3 temperature, reaction time, mixing time and shaking time in the respective steps
Comparative example
Comparative example 1
Comparative example 1 differs from examples 1-10 in that: the preparation method of comparative example 1 was: step 1: weighing 25.2Kg of PBT, 34.8Kg of PET and 5Kg of methyl hydrogen-containing silicone oil, putting into an internal mixer, heating to 190 ℃, mixing and reacting for 4.5h, putting the obtained raw materials into an extruder, extruding at 190 ℃, and calendering by a calender to obtain a base material; step 2: activating the substrate in activating solution for 15min, coating the acrylic glue on the substrate by adopting a mixed wheel gluing mode, wherein the coating weight is 120g/m 2 And (5) carrying out air drying at 50 ℃ in an air dryer, and rolling to obtain the high-temperature-resistant adhesive tape.
Comparative example 2
Comparative example 2 differs from examples 1-10 in that:
step 1: weighing 25.2Kg of PBT, 34.8Kg of PET and 5Kg of methyl hydrogen-containing silicone oil, putting into an internal mixer, heating to 190 ℃, and mixing for 2h to obtain a mixture A;
step 2: weighing 50Kg of polyimide, 8Kg of hexagonal boron nitride and 0.7Kg of polyethylene glycol, heating to 60 ℃, and reacting at constant temperature for 2 hours to obtain a mixture B; adding the mixture B into the mixture A in 4 batches, uniformly mixing every time after adding the mixture B, adding the mixture B into the mixture A again, heating to 210 ℃ after completely adding the mixture B, reacting for 2.5 hours, putting the obtained raw materials into an extruder, extruding at 190 ℃, and calendering by a calender to obtain a base material;
and step 3: activating the base material in activating liquid for 15min, and coating acrylic glue on the base material in a mixed wheel gluing mode, wherein the coating weight is 120g/m 2 Air-drying at 50 deg.C, and rolling to obtain high temperature resistant adhesive tape
Performance test
The following performance tests were performed for examples 1-10 and comparative examples 1-2, as shown in Table 4.
Detection method/test method
1. Fire rating
Detecting the fire-proof grade according to the national standard GB/T5464-1999, and recording related data;
2. high temperature resistance
According to the test method for high-temperature resistance and aging of the adhesive tape of the national standard GB/T32368-2015, detection is carried out, when the phenomena of cracking, substrate falling and curling are unqualified, the conditions are qualified when the phenomena are not generated, and specific data are shown in Table 4;
3. coefficient of thermal conductivity
Testing according to national standard GB/T2588-2008, and testing the heat conductivity coefficient at 25 ℃ by using a NETZSCH HY 009 heat conductivity tester;
4. resistance testing
Performed according to GB/1410-2006; detecting the volume resistance by using a volume surface resistivity tester LST-121, which is specifically shown in Table 4;
TABLE 4 Experimental data for examples 1-10 and comparative examples 1-2
It can be seen from the combination of examples 1 to 10 and comparative examples 1 to 2 and the combination of table 3 that the fire-retardant rating, the high-temperature resistance, the thermal conductivity and the volume resistance of examples 1 to 10 are better than those of comparative examples 1 to 2, which indicates that the preparation method of the present application has better insulating property, thermal conductivity and high-temperature resistance than those of comparative examples 1 to 2, and further indicates that the high-temperature resistant adhesive tape obtained by the present application has better high-temperature resistance, so that the durability of the adhesive tape used for a lithium battery is improved, and meanwhile, the heat dissipation effect of the lithium battery can be improved, and the possibility of electric leakage of the lithium battery is reduced.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (7)
1. The preparation method of the high-temperature-resistant adhesive tape for the lithium battery is characterized by comprising the following steps of:
step 1: weighing 55-75 parts of polyester and 3-8 parts of silicone oil according to parts by weight, heating to 185-200 ℃, and mixing for 0.8-2.5 hours to obtain a mixture A;
and 2, step: weighing 25-35 parts of PMDA, 5-11 parts of modified hexagonal boron nitride, 0.5-1 part of polyethylene glycol and 80-150 parts of isopropanol according to parts by weight, vibrating for 12-18min, heating to 50-65 ℃, adding 15-30 parts of diaminodiphenyl ether, vibrating for 8-15min, heating to 75-85 ℃, reacting at constant temperature for 1.5-3.5h, and distilling to obtain a mixture B; adding the mixture B into the mixture A in 3-5 batches, heating to 205-220 ℃, reacting for 2-3h, and preparing a film to obtain a substrate;
and step 3: activating a base material by using an activating solution, coating an adhesive on the base material, drying and rolling to obtain a high-temperature-resistant adhesive tape;
the modified hexagonal boron nitride is prepared by the following steps:
step A: weighing 23-30 parts of hexagonal boron nitride and 75-100 parts of polyvinylpyrrolidone according to parts by weight, and oscillating for 3-8 hours to obtain pretreated hexagonal boron nitride;
and B: weighing 18-25 parts of methyl pyrrolidone and 25-50 parts of methanol according to parts by weight, adding into the pretreated hexagonal boron nitride obtained in the step A, oscillating for 15-18h, filtering and drying to obtain a mixture A;
step C: weighing 1.5-3.5 parts of mica, 0.8-1.3 parts of silane coupling agent and 0.3-1.2 parts of titanate coupling agent according to parts by weight, dissolving in 120-160 parts of ethanol, adding the mixture A obtained in the step B, shaking for 1-1.5h, filtering, and drying filter residues to obtain modified hexagonal boron nitride;
the preparation of the hexagonal boron nitride comprises the following steps:
a, step a: weighing 20-25 parts of ammonium borate and 3-8 parts of melamine according to parts by weight, uniformly mixing, introducing nitrogen, reacting for 3-5 hours at 380-420 ℃, and cooling to obtain a mixture I;
step b: and b, weighing 80-100 parts by weight of sodium hydroxide, adding the sodium hydroxide into the mixture I obtained in the step a, soaking for 5-10min, filtering, reacting the filter residue at 2000-2200 ℃ for 8-13h under the protection of nitrogen, cooling, and sieving by a 50-100-mesh sieve to obtain the hexagonal boron nitride.
2. The preparation method of the high-temperature-resistant adhesive tape for the lithium battery according to claim 1, wherein the adhesive tape comprises the following steps: the activating solution is ammonia water and sodium hexametaphosphate in a weight ratio of 10-15.
3. The preparation method of the high-temperature-resistant adhesive tape for the lithium battery according to claim 1, wherein the adhesive tape comprises the following steps: the adhesive is acrylic glue or silica gel glue.
4. The preparation method of the high-temperature-resistant adhesive tape for the lithium battery according to claim 1, wherein the adhesive tape comprises the following steps: the silicone oil is phenyl silicone oil or methyl hydrogen-containing silicone oil.
5. The preparation method of the high-temperature-resistant adhesive tape for the lithium battery according to claim 1, wherein the adhesive tape comprises the following steps: the polyester consists of PBT and PET.
6. The preparation method of the high-temperature-resistant adhesive tape for the lithium battery according to claim 5, wherein the adhesive tape comprises the following steps: the weight ratio of the PBT to the PET is 1.2-1.5.
7. The preparation method of the high-temperature-resistant adhesive tape for the lithium battery as claimed in any one of claims 1 to 6, wherein the adhesive tape comprises the following steps: the film preparation method in the step 3 comprises the following steps: the obtained raw material is extruded at 180-195 ℃ and then calendered.
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