CN115011269A - Special protection film of hot melt UV coating lithium cell - Google Patents

Special protection film of hot melt UV coating lithium cell Download PDF

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Publication number
CN115011269A
CN115011269A CN202210856806.5A CN202210856806A CN115011269A CN 115011269 A CN115011269 A CN 115011269A CN 202210856806 A CN202210856806 A CN 202210856806A CN 115011269 A CN115011269 A CN 115011269A
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glue
weight
parts
protective film
coating
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CN115011269B (en
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梁展盛
李鹏
张长宇
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Dongguan Aozhongxin Material Technology Co ltd
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Dongguan Aozhongxin Material Technology Co ltd
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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
    • 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
    • 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
    • C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
    • 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
    • C09J7/24—Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/241—Polyolefin, e.g.rubber
    • C09J7/243—Ethylene or propylene polymers
    • 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
    • C09J7/35—Heat-activated
    • 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
    • C09J7/38—Pressure-sensitive adhesives [PSA]
    • C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/385—Acrylic polymers
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
    • 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
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
    • 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
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/304—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being heat-activatable, i.e. not tacky at temperatures inferior to 30°C
    • 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
    • C09J2423/00—Presence of polyolefin
    • C09J2423/10—Presence of homo or copolymers of propene
    • C09J2423/106—Presence of homo or copolymers of propene in the substrate
    • 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
    • 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

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paints Or Removers (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention provides a hot-melt UV (ultraviolet) coating protective film special for a lithium battery, which comprises a glue layer and a substrate layer, wherein the glue layer is formed by UV photocuring glue, and the glue comprises 90-110 parts by weight of modified polyacrylate, 5-50 parts by weight of active diluent, 0-10 parts by weight of tackifying resin and 0.1-5 parts by weight of photoinitiator. According to the invention, the glue with moderate molecular weight and suitable for hot-melt coating is prepared, so that the coating efficiency in the hot-melt photocuring process is improved, the prepared protective film glue film has higher appearance flatness, and the protective film has better adhesion effect when being adhered to a base material. The glue with moderate molecular weight forms a glue layer with moderate molecular weight after photocuring, and the glue layer has excellent stripping performance and better bonding performance.

Description

Special protection film of hot melt UV coating lithium cell
Technical Field
The invention belongs to the field of lithium battery protective films, and particularly relates to a hot-melt UV (ultraviolet) coating protective film special for a lithium battery, in particular to a special protective film for a lithium battery, which is specially used for surface pasting of an aluminum plastic film in the production process of a polymer lithium battery and surface protection of the aluminum plastic film.
Background
With the rapid development of the lithium battery industry, the corresponding lithium battery protective film is also rapidly developed. In the process of lithium battery production, transportation and the like, the lithium battery can be inevitably collided or polluted, and in order to avoid collision, scratch, surface pollution and the like of the lithium battery, it is necessary to cover a protective film on the surface of the lithium battery so as to prolong the service life of the lithium battery.
Generally, in the lithium battery industry, a solvent coating process is mostly adopted for producing a lithium battery protective film, the solvent coating process has good mixing dispersibility of organic components and good coating effect, but the use of an organic solvent has the disadvantages of large environmental pollution, poor production environment, large resource waste, and low production efficiency due to the addition of a solvent drying step. In recent years, with the deepening of environmental protection concepts and environmental protection policies, a solvent-free hot-melt photocuring coating process is also developed to a certain extent, but a solvent-free adhesive causes the coating process to have a poor coating effect, and the use of a film formed by photocuring is influenced. In addition, the existing lithium battery protective film also has the problems of low initial adhesion, poor peeling performance after hot pressing, easy residual glue in film tearing and the like, and influences the use effect of the lithium battery protective film.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention provides the hot-melt UV coating lithium battery special protective film, which is used for improving the hot-melt coating efficiency and preparing the lithium battery protective film with excellent stripping performance by preparing the adhesive suitable for hot-melt photocuring coating.
The invention provides a hot-melt UV coating protective film special for a lithium battery, which comprises an adhesive layer and a substrate layer,
the adhesive layer is formed by UV (ultraviolet) photocuring glue, and the glue comprises, by weight, 90-110 parts of modified polyacrylate, 5-50 parts of reactive diluent, 0-10 parts of tackifying resin and 0.1-5 parts of photoinitiator; the modified polyacrylate is isocyanate modified polyacrylate; the glass transition temperature range of the modified polyacrylate is-80 to-20 ℃.
The modified polyacrylate has lower glass transition temperature, so that the modified polyacrylate has better flexibility and cohesiveness, and further, a glue film formed after photocuring also has better flexibility and cohesiveness.
Preferably, the number average molecular weight of the modified polyacrylate ranges from 2 to 20 ten thousand. The stripping performance of the adhesive film is closely related to the molecular weight, if the molecular weight of the adhesive film is too large, interface adhesion damage is easy to occur during stripping, the permanent adhesive force is too high, and the stripping strength is low; if the molecular weight of the adhesive film is too small, the cohesive force of the adhesive film is insufficient, the cohesive failure in the adhesive film is easy to occur during stripping, the permanent adhesive force is lower, and the stripping strength is also lower; and the adhesive film with moderate molecular weight has good peeling strength when peeled off, can not generate interface damage and also has better pressure-sensitive adhesive performance. Therefore, the modified polyacrylate is controlled in a moderate molecular weight range, so that the adhesive layer formed by curing the modified polyacrylate also has a moderate molecular weight range, and the obtained adhesive layer has excellent stripping performance and adhesive performance.
Preferably, the reactive diluent comprises at least one of pentaerythritol acrylate, pentaerythritol acrylate derivatives, trimethylol acrylate derivatives, 2-ethylhexyl acrylate, isobornyl acrylate, tripropylene glycol diacrylate, 1, 6-hexanediol diacrylate, dipropylene glycol diacrylate, trimethylolpropane diallyl ether, trimethylolpropane monoallyl ether.
Preferably, the reactive diluent comprises at least one of 2-ethylhexyl acrylate, trimethylolpropane monoallyl ether, pentaerythritol acrylate. The reactive diluent and the isocyanate modified polyacrylate jointly participate in the photocuring process of the glue, the selection of the reactive diluent influences the molecular weight of a glue layer obtained after curing, and the scheme ensures that the heavier molecular weight obtained after curing is moderate and the excellent peeling strength of the glue layer is ensured by selecting the proper diluent.
Preferably, the modified polyacrylate is prepared by the following steps:
step one, uniformly mixing an acrylate monomer and a thermal initiator to form a mixed solution;
step two, heating part of the mixed solution in the step one to 60-90 ℃, carrying out heat preservation reaction for 0.5-2 h, adding the rest of the mixed solution, and continuing the heat preservation reaction for 2-6 h to obtain polyacrylate;
step three, heating the polyacrylate obtained in the step two, evacuating and dewatering, cooling to 65-70 ℃, adding an isocyanate monomer, carrying out heat preservation reaction for 1.5-3 hours, adding a catalyst, carrying out heat preservation reaction for 3-6 hours, adding a polymerization inhibitor, and uniformly mixing to obtain modified polyacrylate;
the acrylate monomer comprises a non-functional acrylate monomer and a hydroxyl-containing acrylate monomer, and the glass transition temperature range of the non-functional acrylate monomer is-80 to-20 ℃; the proportion of the non-functional acrylate monomer in the acrylate monomer is not less than 83 wt%, and the proportion of the hydroxyl-containing acrylate monomer in the acrylate monomer is not less than 1 wt%.
Preferably, the acrylate monomer further comprises a functional acrylate monomer, the ratio of the functional acrylate monomer in the acrylate monomer is not less than 0.1 wt%, and the functional acrylate monomer contains a polar group.
In the preparation method of the polyacrylate, on one hand, the molecular weight controllability of the polyacrylate in the reaction process is stronger by the operation of feeding materials step by step, and the prepared polyacrylate has moderate molecular weight; on the other hand, the problem that the acrylate monomer is easy to implode in the polymerization process is solved by the operation of feeding step by step, and the like, so that the modified polyacrylate prepared by the preparation method in the scheme has smaller molecular weight distribution range span, and therefore, the adhesive layer formed by the modified polyacrylate prepared by the preparation method in the scheme also has proper molecular weight and smaller molecular weight distribution range span, and further has excellent stripping performance.
Preferably, the non-functional acrylate monomer is selected from at least one of methyl acrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, methyl methacrylate, ethyl methacrylate, lauryl acrylate, butyl methacrylate, 2-ethylhexyl methacrylate.
Preferably, the hydroxyl-containing acrylate monomer is selected from at least one of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate.
Preferably, the functional acrylate monomer is selected from at least one of acrylic acid, methacrylic acid, glycidyl acrylate, and glycidyl methacrylate.
Preferably, the isocyanate monomer is isocyanate ethyl acrylate.
Preferably, the catalyst is selected from at least one of triethylenediamine, bis (dimethylaminoethyl) ether, dimethylethanolamine, N-methylmorpholine, 2-dimorpholinodiethyl ether, 1, 4-dimethylpiperazine, N-dimethylbenzylamine, dibutyltin dilaurate, stannous octoate, potassium isooctanoate, potassium oleate, tetrabutyl titanate, tetraisopropyl titanate.
Preferably, the polymerization inhibitor is at least one selected from p-hydroxyanisole, hydroquinone, p-methoxyphenol and 2, 6-di-tert-butylphenol.
Preferably, the tackifying resin comprises at least one of polymerized rosin, hydrogenated rosin resin, pentaerythritol ester of rosin, terpene resin, terpene phenolic resin, C5 petroleum resin, hydrogenated C5 petroleum resin. The tackifying resin can improve the initial adhesion of the adhesive layer and the adhered base material.
Preferably, the protective film special for the hot-melt UV coating lithium battery is prepared by the following preparation method:
step one, mixing modified polyacrylate, reactive diluent, tackifying resin and photoinitiator, and heating, melting and mixing the mixture until the mixture is uniformly mixed to form glue;
and step two, after the glue is cooled to a proper coating temperature, coating the glue on the substrate, then carrying out photocuring, and simultaneously rolling to obtain the special protective film for the lithium battery.
Preferably, the melting temperature of the mixture in the first step is 90-130 ℃, and the coating temperature in the second step is 60-90 ℃.
Preferably, the preparation method of the protective film special for the hot-melt UV coated lithium battery comprises the following specific steps:
under the condition of keeping out of the sun, heating modified polyacrylate, reactive diluent, tackifying resin and photoinitiator to 90-130 ℃ under the protection of nitrogen, melting and mixing until the components are uniformly mixed to form glue;
and step two, cooling the glue in the step one to 60-90 ℃, coating the glue on the substrate layer, then carrying out curing molding on the viscous glue by utilizing UV light to form a glue layer on the substrate layer, and simultaneously rolling to obtain the special protective film for the lithium battery.
Preferably, the glue formed in the first step further comprises adding 0-10 parts by weight of a halogen-free organic pigment.
Preferably, the material of the substrate layer comprises at least one of a polyethylene terephthalate film and a polypropylene film.
Preferably, the substrate layer is corona treated.
In the scheme, the glue with moderate molecular weight and suitable for hot-melt coating is prepared, so that the coating efficiency in the hot-melt photocuring process is improved, the prepared protective film glue film has higher appearance flatness, and the protective film has better adhesion effect when being adhered to a substrate. In addition, the glue with moderate molecular weight forms a glue layer with moderate molecular weight after photocuring, and the glue layer has excellent stripping performance and better bonding performance. In the scheme, the glue adopted by the hot-melting photocuring coating process is solvent-free, so that the solvent drying step can be omitted, the environmental protection and safety of the production process are ensured, and the production efficiency is improved.
Drawings
FIG. 1 is a schematic structural diagram of a protective film for a hot-melt UV coated lithium battery according to the present invention;
the reference signs are: 1, a glue layer; 2, a base material layer.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Preparation of modified polyacrylate:
(1) in the processing I, the first step of the process,
uniformly mixing 100 parts by weight of 2-ethylhexyl acrylate, 3 parts by weight of hydroxypropyl acrylate, 0.3 part by weight of acrylic acid and 0.5 part by weight of azobisisobutyronitrile to form a mixed solution;
step two, heating part of the mixed solution in the step one to 78 ℃, preserving heat for reaction for 1 hour, dropwise adding the rest of the mixed solution in the mixed solution within 4 hours, and continuing preserving heat for reaction for 3 hours to obtain polyacrylate;
and step three, heating the polyacrylate obtained in the step two, evacuating and dehydrating, adding 3.5 parts by weight of isocyanate ethyl acrylate after cooling to 68 ℃ for reacting for 2 hours, continuously adding 0.02 part by weight of dibutyltin dilaurate into the mixture for continuously reacting for 4 hours, finally adding 0.05 part by weight of hydroquinone into the mixture, cooling to about 50 ℃, and taking the mixture out of the kettle to obtain the modified polyacrylate.
(2) In the treatment II, the step of treating,
uniformly mixing 100 parts by weight of 2-ethylhexyl acrylate, 3 parts by weight of hydroxypropyl acrylate, 0.3 part by weight of acrylic acid and 0.5 part by weight of azobisisobutyronitrile, heating to 78 ℃, and carrying out heat preservation reaction for 8 hours to obtain polyacrylate;
and step two, heating the polyacrylate obtained in the step one, evacuating and dehydrating, adding 3.5 parts by weight of isocyanate ethyl acrylate after cooling to 68 ℃ for reacting for 2 hours, continuously adding 0.02 part by weight of dibutyltin dilaurate into the mixture for continuously reacting for 4 hours, finally adding 0.05 part by weight of hydroquinone into the mixture, cooling to about 50 ℃, and taking the mixture out of the kettle to obtain the modified polyacrylate.
(3) In the treatment step III, the reaction mixture is subjected to a treatment step,
the modified polyacrylate of this treatment group was a commercially available isocyanate modified polyacrylate with a molecular weight of 10 ten thousand.
(4) And (IV) treating the mixture,
the modified polyacrylates of this treatment group were commercially available isocyanate-modified polyacrylates having a molecular weight of 30 ten thousand.
Example 1
Under the condition of keeping out of the sun, 100 parts by weight of the modified acrylic resin in the treatment I, 5 parts by weight of 2-ethylhexyl acrylate, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylate, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a glue melting tank, nitrogen is introduced for protection and the mixture is heated to 100 ℃, the mixture is stirred for 30min at the stirring speed of 500r/min, all the materials are completely melted and uniformly mixed, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue suitable for coating in a liquid state. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 2
Under the condition of keeping out of the sun, 100 parts by weight of the modified acrylic resin in the treatment I, 10 parts by weight of trimethylolpropane diallyl ether, 10 parts by weight of pentaerythritol acrylate, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a glue melting tank, nitrogen is introduced for protection, the mixture is heated to 100 ℃, the mixture is stirred for 30min at the stirring speed of 500r/min, all the materials are completely melted and uniformly mixed, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue suitable for coating in a liquid state. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 3
Under the condition of keeping out of the sun, 100 parts by weight of the modified acrylic resin in the treatment I, 5 parts by weight of 2-ethylhexyl acrylate, 5 parts by weight of trimethylolpropane diallyl ether, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a glue melting tank, nitrogen is introduced for protection, the mixture is heated to 100 ℃, the mixture is stirred for 30min at the stirring speed of 500r/min, all the materials are completely melted and uniformly mixed, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue in a liquid state and suitable for coating. And then conveying the glue which is completely melted to a coating head by using a pump, coating on the substrate layer 2, irradiating the glue by using a UV lamp for curing to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 4
Under the condition of keeping out of the sun, 100 parts by weight of the modified acrylic resin in the treatment I, 5 parts by weight of 2-ethylhexyl acrylate, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylate, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a glue melting tank, nitrogen is introduced for protection and the mixture is heated to 100 ℃, the mixture is stirred for 30min at the stirring speed of 500r/min, all the materials are completely melted and uniformly mixed, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue suitable for coating in a liquid state. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a BOPP release film with the thickness of 60 μm, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 5
Under the condition of keeping out of the light, the100 parts by weight of the modified acrylic resin in the treatment I, 5 parts by weight of isobornyl acrylate, 10 parts by weight of tripropylene glycol diacrylate, 5 parts by weight of 1, 6-hexanediol diacrylate, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a melt glue tank, nitrogen is introduced for protection and the mixture is heated to 100 ℃, the mixture is stirred for 30min at a stirring speed of 500r/min, all the materials are completely melted and uniformly mixed, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue suitable for coating in a liquid state. And then conveying the glue which is completely melted to a coating head by using a pump, coating on the substrate layer 2, irradiating the glue by using a UV lamp for curing to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 6
Under the condition of keeping out of the sun, 100 parts by weight of the modified acrylic resin in the treatment I, 10 parts by weight of trihydroxymethyl acrylate, 10 parts by weight of isobornyl acrylate, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a glue melting tank, nitrogen is introduced for protection, the mixture is heated to 100 ℃, the mixture is stirred for 30min at the stirring speed of 500r/min, all the materials are completely melted and uniformly mixed, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue suitable for coating in a liquid state. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 7
Under the condition of keeping out of the light, 100 parts by weight of the modified acrylic resin in the treatment I and 5 parts by weight of dipropylene glycol are addedAdding alcohol diacrylate, 5 parts by weight of trihydroxy methacrylate derivative, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 into a glue melting tank, introducing nitrogen for protection, heating to 100 ℃, stirring at a stirring speed of 500r/min for 30min to completely melt and uniformly mix all the materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain glue in a liquid state suitable for coating. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 8
Under the condition of keeping out of the sun, 100 parts by weight of the modified acrylic resin in the treatment I, 5 parts by weight of 2-ethylhexyl acrylate, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylate, 3 parts by weight of hydrogenated rosin resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a glue melting tank, nitrogen is introduced for protection and the heating is carried out to 100 ℃, the stirring speed of 500r/min is carried out for 30min, all the materials are completely melted and uniformly mixed, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue in a liquid state suitable for coating. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 9
100 parts by weight of the modified acrylic resin in Process I, 5 parts by weight of 2-ethylhexyl acrylate, and 10 parts by weight of trimethylolpropane diallyl under the protection from lightAdding ether, 5 parts by weight of pentaerythritol acrylate, 3 parts by weight of hydrogenated petroleum resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 into a glue melting tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min to completely melt and uniformly mix all the materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain glue in a liquid state suitable for coating. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 10
Under the condition of keeping out of the sun, 100 parts by weight of the modified acrylic resin in the treatment III, 5 parts by weight of 2-ethylhexyl acrylate, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylate, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a glue melting tank, nitrogen is introduced for protection and the mixture is heated to 100 ℃, the mixture is stirred for 30min at the stirring speed of 500r/min, all the materials are completely melted and uniformly mixed, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue suitable for coating in a liquid state. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Example 11
100 parts by weight of the modified acrylic resin in Process III, 5 parts by weight of 2-ethylhexyl acrylate, 10 parts by weight of trimethylolpropane diallyl ether, and 5 parts by weight of a quaternary phosphonium salt were added under exclusion of lightPentaerythritol acrylate, 3 parts by weight of hydrogenated petroleum resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a glue melting tank, nitrogen is introduced for protection, the mixture is heated to 100 ℃, the mixture is stirred for 30min at the stirring speed of 500r/min, all the materials are melted completely and mixed uniformly, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue suitable for coating in a liquid state. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a release film with a thickness of 50 μm PET, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Comparative example 1
Under the condition of keeping out of the sun, adding 100 parts by weight of the modified acrylic resin in the treatment I, 10 parts by weight of 2-ethylhexyl acrylate, 20 parts by weight of trimethylolpropane diallyl ether, 10 parts by weight of pentaerythritol acrylate, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 into a glue melting tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min to completely melt and uniformly mix all the materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain glue in a liquid state suitable for coating. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a BOPP release film with the thickness of 60 μm, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Comparative example 2
Under the condition of keeping out of the light, 100 parts by weight of the modified acrylic resin in the treatment I, 10 parts by weight of 2-ethylhexyl acrylate, 20 parts by weight of trimethylolpropane diallyl ether, 10 parts by weight of pentaerythritol acrylate and 3 parts by weight of terpene tree are addedAdding 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 and grease into a glue melting tank, introducing nitrogen for protection, heating to 100 ℃, stirring at a stirring speed of 500r/min for 30min to completely melt and uniformly mix all the materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain glue suitable for coating in a liquid state. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a BOPP release film with the thickness of 60 μm, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Comparative example 3
Under the condition of keeping out of the sun, 100 parts by weight of modified acrylic resin (which is commercially available and has the molecular weight of 30 ten thousand) in the treatment IV, 5 parts by weight of 2-ethylhexyl acrylate, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylate, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 are added into a glue melting tank, nitrogen is introduced for protection and heating to 100 ℃, stirring is carried out for 30min at the stirring speed of 500r/min, all the materials are completely melted and uniformly mixed, and then the melted and mixed materials are naturally cooled to 90 ℃ to obtain glue suitable for coating in a liquid state. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a PET release film with a thickness of 50 μm, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Comparative example 4
100 parts by weight of the modified acrylic resin in Process II, 5 parts by weight of 2-ethylhexyl acrylate, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylate, 3 parts by weight of a terpene resin, and 2 parts by weight of blue were added under the exclusion of lightAdding 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 and a color pigment into a glue melting tank, introducing nitrogen for protection, heating to 100 ℃, stirring at a stirring speed of 500r/min for 30min to completely melt and uniformly mix all the materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain glue suitable for coating in a liquid state. And then, conveying the glue which is completely melted by the pump to a coating head, coating on the substrate layer 2, irradiating the glue by a UV lamp to be cured to form a glue layer 1, and simultaneously rolling to obtain the protective film. The substrate layer 2 adopted in the embodiment is a PET release film with a thickness of 50 μm, the glue coating thickness is 15 μm, the coating speed is 100m/min, and the UV radiation amount is 200mJ/cm 2 (wavelength 300-400nm), the irradiation time for curing the glue is 20 s.
Test example
1. Experimental construction mode
The protective films prepared in examples 1-11 and comparative examples 1-4 are used for rolling ball initial viscosity, steel plate stripping force, high-temperature high-pressure post-aluminum plastic film stripping force and high-temperature high-pressure glue stain tests.
Testing initial adhesion force of the rolling ball: the initial tack test of the rolling balls was performed on the protective films prepared in examples 1 to 11 and comparative examples 1 to 4 according to the method of the national standard GB/T4852-2002.
And (3) testing the peeling force: the peel strength test was performed on the protective films prepared in examples 1 to 11 and comparative examples 1 to 4 according to the method in the national standard GB/T2792-2014.
2. Results of the experiment
The results of the performance tests on the protective films prepared in examples 1 to 11 and comparative examples 1 to 4 are shown in table 1. Generally, the preferable range of the steel plate peeling force for the battery protective film adhesive tape is 0.1 to 0.3N/25mm, and the preferable range of the aluminum plastic film peeling force after high temperature and high pressure is 0.3 to 0.5N/25 mm. The test result shows that the protective film prepared by the preferred scheme of the invention meets the better performance requirement range of the protective film in initial adhesion and stripping performance, and has good appearance.
TABLE 1 results of performance test on the protective films prepared in examples 1 to 11 and comparative examples 1 to 4
Figure BDA0003755780070000121
As can be seen from Table 1, the protective films of examples 1-4 have good initial adhesion and peeling properties, and the prepared hot-melt coating protective films have uniform thickness and good appearance. The protective films of examples 5-7 had low initial adhesion and peel strength, and had a degumming phenomenon, which did not meet the performance requirements required for protective films. The protective films of examples 8 to 10 had low initial adhesion and peeling strength, and their performances were out of the range of performances required by the present invention. The protective film of example 11 had better initial adhesion and peeling properties.
Comparative example 1, which does not contain a tackifier resin, has low initial adhesion and peel strength of the protective film, and the properties thereof are out of the range of the properties required in the present invention. The protective film of comparative example 2 had better initial adhesion and release properties, meeting the performance requirements of the present invention. The protective film of comparative example 3 had a low initial adhesion and peeling force due to the too large molecular weight of the modified polyacrylate, and had a rough adhesive surface and poor flatness when coated. The modified acrylate used in comparative example 4 was synthesized by a one-step feeding method, resulting in a lower initial adhesion and peeling force of the formed protective film and a poorer flatness of the protective film.
Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention.

Claims (10)

1. The utility model provides a special protection film of hot melt UV coating lithium cell which characterized in that: comprises an adhesive layer and a substrate layer,
the adhesive layer is formed by performing UV light curing on glue, and the glue comprises, by weight, 90-110 parts of modified polyacrylate, 5-50 parts of reactive diluent, 0-10 parts of tackifying resin and 0.1-5 parts of photoinitiator;
the reactive diluent comprises at least one of pentaerythritol acrylate, pentaerythritol acrylate derivatives, trimethylolpropane acrylate derivatives, 2-ethylhexyl acrylate, isobornyl acrylate, tripropylene glycol diacrylate, 1, 6-hexanediol diacrylate, dipropylene glycol diacrylate, trimethylolpropane diallyl ether and trimethylolpropane monoallyl ether;
the modified polyacrylate is isocyanate modified polyacrylate.
2. The protective film for a hot-melt UV-coated lithium battery as claimed in claim 1, wherein: the reactive diluent comprises at least one of 2-ethylhexyl acrylate, trimethylolpropane monoallyl ether and pentaerythritol acrylate.
3. The protective film for a hot-melt UV-coated lithium battery as claimed in claim 1, wherein: the glass transition temperature range of the modified polyacrylate is-80 to-20 ℃.
4. The protective film for a hot-melt UV-coated lithium battery as claimed in claim 1, wherein: the number average molecular weight of the modified polyacrylate ranges from 2 to 20 ten thousand.
5. The protective film for a hot-melt UV-coated lithium battery as claimed in claim 1, wherein: the preparation steps of the modified polyacrylate are as follows:
step one, uniformly mixing an acrylate monomer and a thermal initiator to form a mixed solution;
step two, heating part of the mixed solution in the step one to 60-90 ℃, preserving heat and reacting for 0.5-2 hours, adding the rest of the mixed solution, and continuing preserving heat and reacting for 2-6 hours to obtain polyacrylate;
step three, heating the polyacrylate obtained in the step two, evacuating to remove water, cooling to 65-70 ℃, adding an isocyanate monomer, performing heat preservation reaction for 1.5-3 hours, adding a catalyst, performing heat preservation reaction for 3-6 hours, adding a polymerization inhibitor, and mixing uniformly to obtain modified polyacrylate;
the acrylate monomer comprises a hydroxyl-containing acrylate monomer and a non-functional acrylate monomer, and the glass transition temperature of the non-functional acrylate monomer is-80 to-20 ℃;
the proportion of the non-functional acrylate monomer in the acrylate monomer is not less than 83 wt%, and the proportion of the hydroxyl-containing acrylate monomer in the acrylate monomer is not less than 1 wt%.
6. The protective film for a lithium battery specified by claim 5, wherein: the acrylate monomer also comprises a functional acrylate monomer, wherein the ratio of the functional acrylate monomer in the acrylate monomer is not less than 0.1 wt%, and the functional acrylate monomer contains a polar group.
7. The protective film for a lithium battery specified by claim 5, wherein: the tackifying resin comprises at least one of polymerized rosin, hydrogenated rosin resin, rosin pentaerythritol ester, terpene resin, terpene phenolic resin, C5 petroleum resin and hydrogenated C5 petroleum resin.
8. The protective film for a lithium battery as claimed in claim 7, wherein: the tackifying resin is terpene resin.
9. The protective film for the hot-melt UV-coated lithium battery as claimed in claim 1 to 8, which is prepared by the following preparation method:
step one, mixing the modified polyacrylate, the reactive diluent, the tackifying resin and the photoinitiator, and heating, melting and mixing the mixture until the mixture is uniformly mixed to form the glue;
and step two, after the glue is cooled to a proper coating temperature, coating the glue on the substrate, then carrying out photocuring, and simultaneously rolling to obtain the special protective film for the lithium battery.
10. The protective film for a lithium battery specified by claim 9, wherein: the melting temperature of the mixture in the first step is 90-130 ℃, and the coating temperature in the second step is 60-90 ℃.
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Publication number Priority date Publication date Assignee Title
CN116273757A (en) * 2023-03-14 2023-06-23 瑞浦兰钧能源股份有限公司 Repairing method of battery blue film

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Publication number Priority date Publication date Assignee Title
WO2020165692A1 (en) * 2019-02-11 2020-08-20 3M Innovative Properties Company Uv curable adhesive
CN114702922A (en) * 2022-03-29 2022-07-05 东莞澳中新材料科技股份有限公司 Glue for battery protective film adhesive tape and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020165692A1 (en) * 2019-02-11 2020-08-20 3M Innovative Properties Company Uv curable adhesive
CN114702922A (en) * 2022-03-29 2022-07-05 东莞澳中新材料科技股份有限公司 Glue for battery protective film adhesive tape and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116273757A (en) * 2023-03-14 2023-06-23 瑞浦兰钧能源股份有限公司 Repairing method of battery blue film

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