CN115572548B - High-shear-strength insulating hot melt adhesive film for metal shell power battery and preparation method thereof - Google Patents
High-shear-strength insulating hot melt adhesive film for metal shell power battery and preparation method thereof Download PDFInfo
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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
- C09J7/10—Adhesives in the form of films or foils without carriers
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
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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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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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
- 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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- 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 relates to the technical field of hot melt adhesive films, and in particular discloses a high-shear-strength insulating hot melt adhesive film for a metal shell power battery, which comprises the following raw materials in parts by weight: 30-40 parts of polyester resin, 10-15 parts of polyolefin resin, 8-12 parts of tackifying resin, 5-10 parts of rare earth compound coupling agent modified hydroxyapatite, 3-6 parts of modified boron nitride, 3-6 parts of hydroxyl silicone oil, 2-5 parts of cross-linking agent and 45-55 parts of acetone. The hot melt adhesive film adopts polyester resin and polyolefin resin, the compatibility between raw materials of the product is enhanced by adding tackifying resin and hydroxyl silicone oil as auxiliary agents, the hydroxyl apatite and the modified boron nitride are coordinated by the rare earth compound coupling agent, the two are coordinated, the insulation property and the shearing strength of the product are enhanced, the product performance is improved, the raw materials are coordinated and promoted mutually, and the performance effect of the product is improved.
Description
Technical Field
The invention relates to the technical field of hot melt adhesive films, in particular to a high-shear-strength insulating hot melt adhesive film for a metal shell power battery and a preparation method thereof.
Background
The hot melt adhesive film is a film product with or without release paper, and can be conveniently operated continuously or intermittently. Can be widely used for bonding various fabrics, paper, high polymer materials and metals. The adhesive can be used for bonding various materials such as metal, plastic, paper, wood, ceramic, textile and the like, and good effect can be obtained when the adhesive is bonded on the surface of an uneven object; the adhesive is mainly used for bonding nameplates, plastics and hardware, bonding and fixing metal shells of electronic products, bonding and fixing reinforcing plates, laminating and bonding smart cards and chip type passports, bonding a mobile phone window frame and a front cover, bonding a camera battery groove and the like.
The invention provides a high-shear strength insulating hot melt adhesive film for a metal shell power battery and a preparation method thereof.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a high-shear-strength insulating hot melt adhesive film for a metal-shell power battery and a preparation method thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a high-shear-strength insulating hot melt adhesive film for a metal shell power battery, which comprises the following raw materials in parts by weight:
30-40 parts of polyester resin, 10-15 parts of polyolefin resin, 8-12 parts of tackifying resin, 5-10 parts of rare earth compound coupling agent modified hydroxyapatite, 3-6 parts of modified boron nitride, 3-6 parts of hydroxyl silicone oil, 2-5 parts of cross-linking agent and 45-55 parts of acetone.
Preferably, the hot melt adhesive film comprises the following raw materials in parts by weight:
35 parts of polyester resin, 12.5 parts of polyolefin resin, 10 parts of tackifying resin, 7.5 parts of rare earth compound coupling agent modified hydroxyapatite, 4.5 parts of modified boron nitride, 4.5 parts of hydroxyl silicone oil, 3.5 parts of cross-linking agent and 50 parts of acetone.
Preferably, the tackifying resin is a C5 petroleum resin; the cross-linking agent is diethylenetriamine.
Preferably, the preparation method of the rare earth compound coupling agent modified hydroxyapatite comprises the following steps:
s01: adding rare earth lanthanum sulfate into sodium alginate solution according to the weight ratio of 1:5, then adding coupling agent KH560 accounting for 10-20% of the total weight of the rare earth lanthanum sulfate and 1-5% of phosphoric acid buffer solution, and stirring and uniformly mixing;
s02: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 5-10% according to the weight ratio of 1:4, stirring and dispersing uniformly, then adding sodium dodecyl sulfate with the total amount of 10-20% of the hydroxyapatite, and stirring uniformly to obtain pre-modified hydroxyapatite;
s03: adding the pre-modified hydroxyapatite into the S01 product which is 3 to 5 times of the pre-modified hydroxyapatite, stirring for reaction, washing with water and drying after stirring is finished, thus obtaining the rare earth compound coupling agent modified hydroxyapatite.
Preferably, the mass fraction of the sodium alginate solution is 10-20%; the pH value of the phosphoric acid buffer solution is 4.5-5.5.
Preferably, the temperature of the stirring reaction is 55-65 ℃, the stirring time is 30-40min, and the stirring rotating speed is 350-450r/min.
Preferably, the preparation method of the modified boron nitride comprises the following steps:
s11: adding 30-40 parts of boron nitride into 50-60 parts of ethanol, dispersing uniformly, then adding 2-5 parts of hydrochloric acid and 1-3 parts of sodium oxalate, stirring and mixing fully;
s12: adding 3-6 parts of diatomite and 1-5 parts of tween 60 into 5-10 parts of chitosan water solution, uniformly stirring, then adding 1-3 parts of sodium dimercaptopropane sulfonate, and fully stirring and mixing to obtain an additive modifier;
s13: and adding the additive modifier into the S11 product according to the weight ratio of 1:6, stirring and mixing fully, washing with water, and drying to obtain the modified boron nitride.
Preferably, the mass fraction of the chitosan aqueous solution is 10-15%.
The invention also provides a preparation method of the high-shear-strength insulating hot melt adhesive film for the metal shell power battery, which comprises the following steps:
firstly, fully mixing polyester resin, polyolefin resin, tackifying resin, hydroxyl silicone oil and acetone for one time to obtain a pre-prepared material;
adding rare earth compound coupling agent modified hydroxyapatite, modified boron nitride and cross-linking agent, and fully mixing for the second time to obtain a glue film material;
and thirdly, the adhesive film material is sent into a hot-pressing machine at 75-85 ℃ for 10-20min, the hot-pressing pressure is 10-20MPa, and the hot-melting adhesive film is obtained after the hot-pressing is finished.
Preferably, the rotating speed of the primary mixing is 550-650r/min, and the mixing time is 10-20min; the rotation speed of the secondary mixing is 1000-1200r/min, and the mixing time is 20-30min.
Compared with the prior art, the invention has the following beneficial effects:
the hot melt adhesive film adopts polyester resin and polyolefin resin, the compatibility between raw materials of the product is enhanced by adding tackifying resin and hydroxyl silicone oil as auxiliary agents, the hydroxyl apatite and the modified boron nitride are coordinated by the rare earth compound coupling agent, the two are coordinated, the insulation property and the shearing strength of the product are enhanced, the product performance is improved, the raw materials are coordinated and promoted mutually, and the performance effect of the product is improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The high-shear-strength insulating hot melt adhesive film for the metal shell power battery comprises the following raw materials in parts by weight:
30-40 parts of polyester resin, 10-15 parts of polyolefin resin, 8-12 parts of tackifying resin, 5-10 parts of rare earth compound coupling agent modified hydroxyapatite, 3-6 parts of modified boron nitride, 3-6 parts of hydroxyl silicone oil, 2-5 parts of cross-linking agent and 45-55 parts of acetone.
The hot melt adhesive film of the embodiment comprises the following raw materials in parts by weight:
35 parts of polyester resin, 12.5 parts of polyolefin resin, 10 parts of tackifying resin, 7.5 parts of rare earth compound coupling agent modified hydroxyapatite, 4.5 parts of modified boron nitride, 4.5 parts of hydroxyl silicone oil, 3.5 parts of cross-linking agent and 50 parts of acetone.
The tackifying resin of this embodiment is a C5 petroleum resin; the cross-linking agent is diethylenetriamine.
The preparation method of the rare earth compound coupling agent modified hydroxyapatite of the embodiment comprises the following steps:
s01: adding rare earth lanthanum sulfate into sodium alginate solution according to the weight ratio of 1:5, then adding coupling agent KH560 accounting for 10-20% of the total weight of the rare earth lanthanum sulfate and 1-5% of phosphoric acid buffer solution, and stirring and uniformly mixing;
s02: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 5-10% according to the weight ratio of 1:4, stirring and dispersing uniformly, then adding sodium dodecyl sulfate with the total amount of 10-20% of the hydroxyapatite, and stirring uniformly to obtain pre-modified hydroxyapatite;
s03: adding the pre-modified hydroxyapatite into the S01 product which is 3 to 5 times of the pre-modified hydroxyapatite, stirring for reaction, washing with water and drying after stirring is finished, thus obtaining the rare earth compound coupling agent modified hydroxyapatite.
The mass fraction of the sodium alginate solution in the embodiment is 10-20%; the pH value of the phosphoric acid buffer solution is 4.5-5.5.
The temperature of the stirring reaction in the embodiment is 55-65 ℃, the stirring time is 30-40min, and the stirring rotating speed is 350-450r/min.
The preparation method of the modified boron nitride comprises the following steps:
s11: adding 30-40 parts of boron nitride into 50-60 parts of ethanol, dispersing uniformly, then adding 2-5 parts of hydrochloric acid and 1-3 parts of sodium oxalate, stirring and mixing fully;
s12: adding 3-6 parts of diatomite and 1-5 parts of tween 60 into 5-10 parts of chitosan water solution, uniformly stirring, then adding 1-3 parts of sodium dimercaptopropane sulfonate, and fully stirring and mixing to obtain an additive modifier;
s13: and adding the additive modifier into the S11 product according to the weight ratio of 1:6, stirring and mixing fully, washing with water, and drying to obtain the modified boron nitride.
The mass fraction of the chitosan aqueous solution of the embodiment is 10-15%.
The preparation method of the high-shear-strength insulating hot melt adhesive film for the metal shell power battery comprises the following steps of:
firstly, fully mixing polyester resin, polyolefin resin, tackifying resin, hydroxyl silicone oil and acetone for one time to obtain a pre-prepared material;
adding rare earth compound coupling agent modified hydroxyapatite, modified boron nitride and cross-linking agent, and fully mixing for the second time to obtain a glue film material;
and thirdly, the adhesive film material is sent into a hot-pressing machine at 75-85 ℃ for 10-20min, the hot-pressing pressure is 10-20MPa, and the hot-melting adhesive film is obtained after the hot-pressing is finished.
The rotational speed of primary mixing in the embodiment is 550-650r/min, and the mixing time is 10-20min; the rotation speed of the secondary mixing is 1000-1200r/min, and the mixing time is 20-30min.
Example 1.
The high-shear-strength insulating hot melt adhesive film for the metal shell power battery comprises the following raw materials in parts by weight:
30 parts of polyester resin, 10 parts of polyolefin resin, 8 parts of tackifying resin, 5 parts of rare earth compound coupling agent modified hydroxyapatite, 3 parts of modified boron nitride, 3 parts of hydroxyl silicone oil, 2 parts of cross-linking agent and 45 parts of acetone.
The tackifying resin of this embodiment is a C5 petroleum resin; the cross-linking agent is diethylenetriamine.
The preparation method of the rare earth compound coupling agent modified hydroxyapatite of the embodiment comprises the following steps:
s01: adding rare earth lanthanum sulfate into sodium alginate solution according to the weight ratio of 1:5, then adding coupling agent KH560 accounting for 10% of the total amount of the rare earth lanthanum sulfate and 1% of phosphoric acid buffer solution, and stirring and uniformly mixing;
s02: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 5% according to the weight ratio of 1:4, stirring and dispersing uniformly, then adding sodium dodecyl sulfate with the total amount of 10% of the hydroxyapatite, and stirring uniformly to obtain pre-modified hydroxyapatite;
s03: adding the pre-modified hydroxyapatite into the S01 product which is 3 times of the pre-modified hydroxyapatite, stirring for reaction, washing with water and drying after stirring is finished, thus obtaining the rare earth compound coupling agent modified hydroxyapatite.
The mass fraction of the sodium alginate solution in the embodiment is 10%; the pH of the phosphate buffer solution was 4.5.
The temperature of the stirring reaction in this example was 55℃and the stirring time was 30min, and the stirring speed was 350r/min.
The preparation method of the modified boron nitride comprises the following steps:
s11: adding 30 parts of boron nitride into 50 parts of ethanol, uniformly dispersing, then adding 2 parts of hydrochloric acid and 1 part of sodium oxalate, and stirring and mixing fully;
s12: adding 3 parts of diatomite and 1 part of tween 60 into 5 parts of chitosan aqueous solution, uniformly stirring, then adding 1 part of sodium dimercaptopropane sulfonate, and fully stirring and mixing to obtain an additive modifier;
s13: and adding the additive modifier into the S11 product according to the weight ratio of 1:6, stirring and mixing fully, washing with water, and drying to obtain the modified boron nitride.
The mass fraction of the chitosan aqueous solution of this example was 10%.
The preparation method of the high-shear-strength insulating hot melt adhesive film for the metal shell power battery comprises the following steps of:
firstly, fully mixing polyester resin, polyolefin resin, tackifying resin, hydroxyl silicone oil and acetone for one time to obtain a pre-prepared material;
adding rare earth compound coupling agent modified hydroxyapatite, modified boron nitride and cross-linking agent, and fully mixing for the second time to obtain a glue film material;
and thirdly, the adhesive film material is sent into a hot-pressing machine at 75 ℃ for 10min, the hot-pressing pressure is 10MPa, and the hot-melting adhesive film is obtained after the hot-pressing is finished.
The rotational speed of the primary mixing in this example was 550r/min, and the mixing time was 10min; the rotation speed of the secondary mixing is 1000r/min, and the mixing time is 20min.
Example 2.
The high-shear-strength insulating hot melt adhesive film for the metal shell power battery comprises the following raw materials in parts by weight:
40 parts of polyester resin, 15 parts of polyolefin resin, 12 parts of tackifying resin, 10 parts of rare earth compound coupling agent modified hydroxyapatite, 6 parts of modified boron nitride, 6 parts of hydroxyl silicone oil, 5 parts of cross-linking agent and 55 parts of acetone.
The tackifying resin of this embodiment is a C5 petroleum resin; the cross-linking agent is diethylenetriamine.
The preparation method of the rare earth compound coupling agent modified hydroxyapatite of the embodiment comprises the following steps:
s01: adding rare earth lanthanum sulfate into sodium alginate solution according to the weight ratio of 1:5, then adding coupling agent KH560 accounting for 20% of the total amount of the rare earth lanthanum sulfate and 5% of phosphoric acid buffer solution, and stirring and uniformly mixing;
s02: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 10% according to the weight ratio of 1:4, stirring and dispersing uniformly, then adding sodium dodecyl sulfate with the total amount of 20% of the hydroxyapatite, and stirring uniformly to obtain pre-modified hydroxyapatite;
s03: and adding the pre-modified hydroxyapatite into the S01 product which is 5 times of the pre-modified hydroxyapatite, stirring for reaction, washing with water and drying after stirring is finished, so as to obtain the rare earth compound coupling agent modified hydroxyapatite.
The mass fraction of the sodium alginate solution in the embodiment is 20%; the pH of the phosphate buffer solution was 5.5.
The temperature of the stirring reaction in this example was 65℃and the stirring time was 40min, and the stirring speed was 450r/min.
The preparation method of the modified boron nitride comprises the following steps:
s11: adding 40 parts of boron nitride into 60 parts of ethanol, uniformly dispersing, then adding 5 parts of hydrochloric acid and 3 parts of sodium oxalate, and stirring and mixing fully;
s12: adding 6 parts of diatomite and 5 parts of tween 60 into 10 parts of chitosan aqueous solution, uniformly stirring, then adding 3 parts of sodium dimercaptopropane sulfonate, and fully stirring and mixing to obtain an additive modifier;
s13: and adding the additive modifier into the S11 product according to the weight ratio of 1:6, stirring and mixing fully, washing with water, and drying to obtain the modified boron nitride.
The mass fraction of the chitosan aqueous solution of this example was 15%.
The preparation method of the high-shear-strength insulating hot melt adhesive film for the metal shell power battery comprises the following steps of:
firstly, fully mixing polyester resin, polyolefin resin, tackifying resin, hydroxyl silicone oil and acetone for one time to obtain a pre-prepared material;
adding rare earth compound coupling agent modified hydroxyapatite, modified boron nitride and cross-linking agent, and fully mixing for the second time to obtain a glue film material;
and thirdly, the adhesive film material is sent into a hot-pressing machine at 85 ℃ for 20min, the hot-pressing pressure is 20MPa, and the hot-melt adhesive film is obtained after the hot-pressing is finished.
The rotational speed of the primary mixing in this embodiment is 650r/min, and the mixing time is 20min; the rotation speed of the secondary mixing is 1200r/min, and the mixing time is 30min.
Example 3.
The high-shear-strength insulating hot melt adhesive film for the metal shell power battery comprises the following raw materials in parts by weight:
35 parts of polyester resin, 12.5 parts of polyolefin resin, 10 parts of tackifying resin, 7.5 parts of rare earth compound coupling agent modified hydroxyapatite, 4.5 parts of modified boron nitride, 4.5 parts of hydroxyl silicone oil, 3.5 parts of cross-linking agent and 50 parts of acetone.
The tackifying resin of this embodiment is a C5 petroleum resin; the cross-linking agent is diethylenetriamine.
The preparation method of the rare earth compound coupling agent modified hydroxyapatite of the embodiment comprises the following steps:
s01: adding rare earth lanthanum sulfate into sodium alginate solution according to the weight ratio of 1:5, then adding coupling agent KH560 accounting for 15% of the total amount of the rare earth lanthanum sulfate and 3% of phosphoric acid buffer solution, and stirring and uniformly mixing;
s02: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 7.5% according to the weight ratio of 1:4, stirring and dispersing uniformly, then adding sodium dodecyl sulfate with the total amount of the hydroxyapatite to 15%, and stirring uniformly to obtain pre-modified hydroxyapatite;
s03: adding the pre-modified hydroxyapatite into the S01 product which is 4 times of the pre-modified hydroxyapatite, stirring for reaction, washing with water and drying after stirring is finished, thus obtaining the rare earth compound coupling agent modified hydroxyapatite.
The mass fraction of the sodium alginate solution in the embodiment is 15%; the pH value of the phosphate buffer solution is 5.0.
The temperature of the stirring reaction in this example was 60℃and the stirring time was 35min, and the stirring speed was 400r/min.
The preparation method of the modified boron nitride comprises the following steps:
s11: adding 45 parts of boron nitride into 55 parts of ethanol, uniformly dispersing, then adding 3.5 parts of hydrochloric acid and 2 parts of sodium oxalate, and stirring and mixing fully;
s12: adding 4.5 parts of diatomite and 3 parts of tween 60 into 7.5 parts of chitosan water solution, uniformly stirring, then adding 2 parts of sodium dimercaptopropane sulfonate, and fully stirring and mixing to obtain an additive modifier;
s13: and adding the additive modifier into the S11 product according to the weight ratio of 1:6, stirring and mixing fully, washing with water, and drying to obtain the modified boron nitride.
The mass fraction of the chitosan aqueous solution of this example was 12.5%.
The preparation method of the high-shear-strength insulating hot melt adhesive film for the metal shell power battery comprises the following steps of:
firstly, fully mixing polyester resin, polyolefin resin, tackifying resin, hydroxyl silicone oil and acetone for one time to obtain a pre-prepared material;
adding rare earth compound coupling agent modified hydroxyapatite, modified boron nitride and cross-linking agent, and fully mixing for the second time to obtain a glue film material;
and thirdly, the adhesive film material is sent into a hot-pressing machine at 80 ℃ for 15min, the hot-pressing pressure is 15MPa, and the hot-melting adhesive film is obtained after the hot-pressing is finished.
The rotational speed of the primary mixing in this embodiment is 600r/min, and the mixing time is 15min; the rotational speed of the secondary mixing is 1100r/min and the mixing time is 25min.
Comparative example 1.
The difference from example 3 is that the rare earth compound coupling agent is not added to modify the hydroxyapatite.
Comparative example 2.
The difference from example 3 is that the rare earth compound coupling agent modified hydroxyapatite is replaced by hydroxyapatite.
Comparative example 3.
The difference from example 3 is that the hydroxyapatite is not pre-modified in the preparation method of the rare earth compound coupling agent modified hydroxyapatite.
Comparative example 4.
The difference from example 3 is that rare earth lanthanum sulfate is not added in the preparation of the rare earth compound coupling agent modified hydroxyapatite.
Comparative example 5.
The difference from example 3 is that no modified boron nitride was added.
Comparative example 6.
The difference from example 3 is that no additive modifier was added in the preparation of the modified boron nitride.
Comparative example 7.
The difference from example 3 is that the modified boron nitride is replaced by boron nitride.
The results of the performance measurements of examples 1-3 and comparative examples 1-7 are as follows
From examples 1 to 3 and comparative examples 1 to 7,
the product of the embodiment 3 has excellent breakdown resistance and high shear strength, and simultaneously has stable performance under the cycle of-40 to 85 ℃ of high and low temperature resistance, and has excellent breakdown resistance effect;
the rare earth compound coupling agent is adopted to modify the hydroxyapatite and the modified boron nitride, so that the hydroxyapatite and the modified boron nitride have synergistic effect, and the breakdown resistance and the shearing strength of the product are enhanced;
as can be seen from comparative examples 1 to 4, the shearing strength of the product is obviously reduced without adding the rare earth compound coupling agent to modify the hydroxyapatite, and meanwhile, the breakdown resistance is deteriorated under the conventional condition, particularly, the breakdown resistance is obviously reduced under the high and low temperature resistant cycle of-40 to 85 ℃;
in addition, the hydroxyapatite is used for replacing the rare earth compound coupling agent to modify the hydroxyapatite, the performance effect improvement of the product is not obvious, the preparation methods of the hydroxyapatite and the rare earth compound coupling agent are different, and the performance effect of the product is different, so that the performance effect improvement of the product is obvious only by adopting the hydroxyapatite prepared by the method to replace the rare earth compound coupling agent;
as can be seen from comparative examples 5 to 7, the modified boron nitride is not added, and is replaced by boron nitride, meanwhile, no modifier is added in the preparation of boron nitride, the performance effect of the product is in a trend of deterioration, and only the modified boron nitride prepared by the method and the rare earth compound coupling agent modified hydroxyapatite are used cooperatively, so that the insulation, breakdown resistance and shear strength performance effect of the product are enhanced cooperatively, and meanwhile, the performance stability of the product is still excellent in an acid environment.
The invention further optimizes the aging of the product at the temperature of 50 ℃ for 2000 hours:
as can be seen from the ageing-resistant experiment, the product of the invention has stable performance after ageing resistance, the stability of the product of the comparative example is obviously deteriorated, and the performance stability of the product is obvious by adopting the raw material proportion of the invention.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (8)
1. The high-shear-strength insulating hot melt adhesive film for the metal shell power battery is characterized by comprising the following raw materials in parts by weight:
30-40 parts of polyester resin, 10-15 parts of polyolefin resin, 8-12 parts of tackifying resin, 5-10 parts of rare earth compound coupling agent modified hydroxyapatite, 3-6 parts of modified boron nitride, 3-6 parts of hydroxyl silicone oil, 2-5 parts of cross-linking agent and 45-55 parts of acetone; the preparation method of the rare earth compound coupling agent modified hydroxyapatite comprises the following steps:
s01: adding rare earth lanthanum sulfate into sodium alginate solution according to the weight ratio of 1:5, then adding coupling agent KH560 accounting for 10-20% of the total weight of the rare earth lanthanum sulfate and 1-5% of phosphoric acid buffer solution, and stirring and uniformly mixing;
s02: adding hydroxyapatite into hydrochloric acid solution with the mass fraction of 5-10% according to the weight ratio of 1:4, stirring and dispersing uniformly, then adding sodium dodecyl sulfate with the total amount of 10-20% of the hydroxyapatite, and stirring uniformly to obtain pre-modified hydroxyapatite;
s03: adding the pre-modified hydroxyapatite into the S01 product which is 3 to 5 times of the pre-modified hydroxyapatite, stirring for reaction, washing with water and drying after stirring is finished to obtain the rare earth compound coupling agent modified hydroxyapatite; the preparation method of the modified boron nitride comprises the following steps:
s11: adding 30-40 parts of boron nitride into 50-60 parts of ethanol, dispersing uniformly, then adding 2-5 parts of hydrochloric acid and 1-3 parts of sodium oxalate, stirring and mixing fully;
s12: adding 3-6 parts of diatomite and 1-5 parts of tween 60 into 5-10 parts of chitosan water solution, uniformly stirring, then adding 1-3 parts of sodium dimercaptopropane sulfonate, and fully stirring and mixing to obtain an additive modifier;
s13: and adding the additive modifier into the S11 product according to the weight ratio of 1:6, stirring and mixing fully, washing with water, and drying to obtain the modified boron nitride.
2. The high shear strength insulating hot melt adhesive film for a metal shell power battery according to claim 1, wherein the hot melt adhesive film comprises the following raw materials in parts by weight:
35 parts of polyester resin, 12.5 parts of polyolefin resin, 10 parts of tackifying resin, 7.5 parts of rare earth compound coupling agent modified hydroxyapatite, 4.5 parts of modified boron nitride, 4.5 parts of hydroxyl silicone oil, 3.5 parts of cross-linking agent and 50 parts of acetone.
3. The high shear strength insulating hot melt adhesive film for a metal shell power cell of claim 1, wherein said tackifying resin is a C5 petroleum resin; the cross-linking agent is diethylenetriamine.
4. The high shear strength insulating hot melt adhesive film for a metal shell power battery according to claim 1, wherein the mass fraction of the sodium alginate solution is 10-20%; the pH value of the phosphoric acid buffer solution is 4.5-5.5.
5. The high shear strength insulating hot melt adhesive film for metal shell power cells according to claim 1, wherein the stirring reaction temperature is 55-65 ℃, the stirring time is 30-40min, and the stirring rotation speed is 350-450r/min.
6. The high shear strength insulating hot melt adhesive film for metal shell power cells according to claim 1, wherein the mass fraction of the chitosan aqueous solution is 10-15%.
7. A method for preparing the high shear strength insulating hot melt adhesive film for metal shell power cells as defined in any one of claims 1 to 6, comprising the steps of:
firstly, fully mixing polyester resin, polyolefin resin, tackifying resin, hydroxyl silicone oil and acetone for one time to obtain a pre-prepared material;
adding rare earth compound coupling agent modified hydroxyapatite, modified boron nitride and cross-linking agent, and fully mixing for the second time to obtain a glue film material;
and thirdly, the adhesive film material is sent into a hot-pressing machine at 75-85 ℃ for 10-20min, the hot-pressing pressure is 10-20MPa, and the hot-melting adhesive film is obtained after the hot-pressing is finished.
8. The method for preparing a high shear strength insulating hot melt adhesive film for a metal-shell power battery according to claim 7, wherein the rotational speed of the primary mixing is 550-650r/min, and the mixing time is 10-20min; the rotation speed of the secondary mixing is 1000-1200r/min, and the mixing time is 20-30min.
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| JPH06293504A (en) * | 1993-04-02 | 1994-10-21 | Nippon Sherwood Kk | Coating method for hydroxylapatite |
| JP5958610B1 (en) * | 2015-06-23 | 2016-08-02 | 東洋インキＳｃホールディングス株式会社 | Hot melt adhesive sheet, method for producing adhesive structure using the same, and method for peeling |
| CN108129075A (en) * | 2017-12-31 | 2018-06-08 | 安徽普发照明有限公司 | The semiconductor lighting high heat sink material of thermal matching energy |
| CN109012622A (en) * | 2018-09-27 | 2018-12-18 | 天津理工大学 | A kind of preparation method and application of the porous composite adsorbing material of nanometer hydroxyapatite/sodium alginate |
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| JPH06293504A (en) * | 1993-04-02 | 1994-10-21 | Nippon Sherwood Kk | Coating method for hydroxylapatite |
| JP5958610B1 (en) * | 2015-06-23 | 2016-08-02 | 東洋インキＳｃホールディングス株式会社 | Hot melt adhesive sheet, method for producing adhesive structure using the same, and method for peeling |
| CN108129075A (en) * | 2017-12-31 | 2018-06-08 | 安徽普发照明有限公司 | The semiconductor lighting high heat sink material of thermal matching energy |
| CN109012622A (en) * | 2018-09-27 | 2018-12-18 | 天津理工大学 | A kind of preparation method and application of the porous composite adsorbing material of nanometer hydroxyapatite/sodium alginate |
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