CN115011269B - 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
CN115011269B
CN115011269B CN202210856806.5A CN202210856806A CN115011269B CN 115011269 B CN115011269 B CN 115011269B CN 202210856806 A CN202210856806 A CN 202210856806A CN 115011269 B CN115011269 B CN 115011269B
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glue
parts
weight
coating
protective film
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CN115011269A (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
    • 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
    • C09J2203/326—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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paints Or Removers (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention provides a special protection film for a hot-melt UV-coated lithium battery, which comprises a glue layer and a substrate layer, wherein the glue layer is formed by curing glue through UV light, and the glue comprises, by weight, 90-110 parts of modified polyacrylate, 5-50 parts of reactive diluents, 0-10 parts of tackifying resin and 0.1-5 parts of photoinitiators. According to the invention, the glue with moderate molecular weight and suitable for hot melt coating is prepared, so that the coating efficiency in a hot melt photo-curing process is improved, the prepared protective film adhesive film has higher appearance flatness, and a better adhesion effect of the protective film when the protective film is adhered to a substrate is ensured. And the glue with moderate molecular weight forms a glue layer with moderate molecular weight after photo-curing, 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 protection films, and particularly relates to a special protection film for a hot-melt UV coated lithium battery, in particular to an aluminum plastic film surface adhesive and a special protection film for a lithium battery, which are specially used in the production process of a polymer lithium battery.
Background
With the rapid development of the lithium battery industry, the corresponding lithium battery protection film is also rapidly developed. In the process of producing and transporting lithium batteries, the lithium batteries are inevitably collided or polluted, and in order to avoid collision, scratch, surface pollution and the like of the lithium batteries, a layer of protection film is covered on the surfaces of the lithium batteries so as to prolong the service lives of the lithium batteries.
Generally, in the lithium battery industry, a solvent coating process is often adopted to produce 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 large environmental pollution, poor production environment and large resource waste, the step of drying the solvent is required to be added, and the production efficiency is low. In recent years, along with the continuous deep environmental protection concept and environmental protection policy, a solvent-free hot-melt photo-curing coating process is also developed to a certain extent, but a solvent-free adhesive makes the coating process have poor coating effect, and influences the use of a photo-curing formed adhesive film. In addition, the existing lithium battery protective film has the problems of low initial adhesion, poor stripping performance after hot pressing, easy residual adhesive of the torn film and the like, and influences the use effect of the lithium battery protective film.
Disclosure of Invention
In order to solve the defects and shortcomings in the prior art, the invention provides the special protective film for the hot-melt UV coated lithium battery, which is prepared by preparing an adhesive suitable for hot-melt photo-curing coating so as to improve the hot-melt coating efficiency and prepare the lithium battery protective film with excellent stripping performance.
The invention provides a special protective film for a hot-melt UV coated lithium battery, which comprises a glue layer and a substrate layer,
the glue layer is formed by UV light curing of 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 of the modified polyacrylate ranges from-80 ℃ to-20 ℃.
The modified polyacrylate has a lower glass transition temperature, and the lower glass transition temperature enables the modified polyacrylate to have better flexibility and cohesiveness, and further the adhesive film formed after photo-curing also has better flexibility and cohesiveness.
Preferably, the modified polyacrylate has a number average molecular weight in the range of 2 to 20 tens of thousands. 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, interfacial adhesion damage is easy to occur during stripping, the holding power is too high, and the stripping strength is low; if the molecular weight of the adhesive film is too small, the adhesive film cohesive force is insufficient, cohesive failure of the adhesive film easily occurs during peeling, the holding power is low, and the peeling strength is also low; the adhesive film with moderate molecular weight has good peeling strength during peeling, does not generate interface damage, and has good 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 adhesive layer obtained by the method has excellent stripping performance and adhesive performance.
Preferably, the reactive diluent comprises at least one of pentaerythritol acrylate, pentaerythritol acrylate derivative, trimethylol acrylate derivative, 2-ethylhexyl acrylate, isobornyl acrylate, tetrapropylene glycol diacrylate, 1, 6-hexanediol diacrylate, dipropylene glycol diacrylate, trimethylol propane diallyl ether, trimethylol propane 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 participate in the photo-curing process of the glue together, the molecular weight of the glue layer obtained after curing can be influenced by the selection of the reactive diluent, and the proper diluent is selected in the scheme, so that the obtained heavy molecular weight after curing is moderate, and the excellent peeling strength of the glue layer is ensured.
Preferably, the modified polyacrylate is prepared as follows:
step one, uniformly mixing an acrylic ester monomer and a thermal initiator to form a mixed solution;
step two, taking part of the mixed solution in the step one, heating to 60-90 ℃ firstly, carrying out heat preservation reaction for 0.5-2 hours, then adding the rest of the mixed solution into the mixed solution, and carrying out heat preservation reaction for 2-6 hours to obtain polyacrylate;
step three, heating the polyacrylate in the step two, evacuating to remove water, cooling to 65-70 ℃, adding isocyanate monomer into the polyacrylate, reacting for 1.5-3 hours at a temperature, adding catalyst, reacting for 3-6 hours at a temperature, adding polymerization inhibitor, and uniformly mixing to obtain modified polyacrylate;
the acrylic ester monomer comprises a nonfunctional acrylic ester monomer and a hydroxyl-containing acrylic ester monomer, and the glass transition temperature of the nonfunctional acrylic ester monomer ranges from-80 ℃ to-20 ℃; the proportion of the non-functional acrylate monomer in the acrylate monomer is not less than 83wt%, and the proportion of the hydroxyl-containing acrylate monomer in the acrylate monomer is not less than 1wt%.
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 0.1wt%, and the functional acrylate monomer contains a polar group.
In the scheme, in the preparation method of the polyacrylate, on one hand, the operation of stepwise feeding ensures that the molecular weight controllability of the polyacrylate in the reaction process is stronger, and the prepared polyacrylate has moderate molecular weight; on the other hand, the operation of step-by-step feeding avoids the problems of easy sudden aggregation and the like of acrylate monomers in the polymerization process, so that the modified polyacrylate prepared by the preparation method in the scheme has smaller span of molecular weight distribution range, 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 span of molecular weight distribution range, 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, 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 iso-octoate, potassium oleate, tetrabutyl titanate, tetraisopropyl titanate.
Preferably, the polymerization inhibitor is at least one selected from the group consisting of 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 rosin ester, 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 special protection film for the hot-melt UV coated 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 formed by the steps until the mixture is uniformly mixed to form glue;
and secondly, after the glue is cooled to a proper coating temperature, coating the glue on a substrate, and then performing photo-curing and rolling to obtain the special protective film for the lithium battery.
Preferably, the melting temperature of the mixture in step one is from 90 to 130 ℃ and the coating temperature in step two is from 60 to 90 ℃.
Preferably, the preparation method of the special protection film for the hot-melt UV coated lithium battery comprises the following specific steps:
step one, under the condition of avoiding light, heating modified polyacrylate, reactive diluent, tackifying resin and photoinitiator to 90-130 ℃ under the protection of nitrogen, and carrying out melt mixing until the components are uniformly mixed to form glue;
and secondly, cooling the glue in the first step to 60-90 ℃, coating on the substrate layer, and then curing and forming 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 step one further comprises adding 0 to 10 parts by weight of a halogen-free organic pigment.
Preferably, the material of the substrate layer comprises at least one of polyethylene terephthalate film and 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 a hot melt photo-curing process is improved, the prepared protective film adhesive film has higher appearance flatness, and the protective film is ensured to have 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 photo-curing, and the glue layer has excellent stripping performance and better bonding performance. In the scheme, the glue used in the hot-melt photo-curing coating process is solvent-free, so that a solvent drying step can be omitted, the environmental protection and the safety of the production process are ensured, and the production efficiency is improved.
Drawings
FIG. 1 is a schematic structural diagram of a special protective film for a hot-melt UV coated lithium battery;
the reference numerals are: 1, an adhesive layer; 2, a substrate layer.
Detailed Description
In order that those skilled in the art will better understand the present invention, a technical solution of the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments.
Preparation of modified polyacrylate:
(1) The process I is carried out in such a way that,
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 and reacting for 1 hour, then dripping the rest mixed solution into the mixed solution within 4 hours, and continuing to preserving heat and reacting for 3 hours to obtain polyacrylate;
and thirdly, heating the polyacrylate in the second step, evacuating to remove water, cooling to 68 ℃, adding 3.5 parts by weight of isocyanate ethyl acrylate to react for 2 hours, continuously adding 0.02 part by weight of dibutyltin dilaurate to react for 4 hours, finally adding 0.05 part by weight of hydroquinone to react, cooling to about 50 ℃, and discharging from a kettle to obtain the modified polyacrylate.
(2) The treatment II is carried out in such a way that,
step one, after 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 are uniformly mixed, heating to 78 ℃, and carrying out heat preservation reaction for 8 hours to obtain polyacrylate;
and step two, heating the polyacrylate in the step one, evacuating to remove water, cooling to 68 ℃, adding 3.5 parts by weight of isocyanate ethyl acrylate into the polyacrylate to react for 2 hours, continuously adding 0.02 part by weight of dibutyltin dilaurate into the polyacrylate to react for 4 hours, finally adding 0.05 part by weight of hydroquinone into the polyacrylate, cooling to about 50 ℃, and discharging the polyacrylate from the kettle to obtain the modified polyacrylate.
(3) The treatment III is carried out in such a way that,
the modified polyacrylate of the treatment group is commercially available isocyanate modified polyacrylate, and the molecular weight of the modified polyacrylate is 10 ten thousand.
(4) The treatment IV is carried out, wherein,
the modified polyacrylate of the treatment group is commercially available isocyanate modified polyacrylate, and the molecular weight of the modified polyacrylate is 30 ten thousand.
Example 1
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin in the treatment I, 5 parts by weight of acrylic acid-2-ethylhexyl ester, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylic ester, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenylpropionyl-1 into a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the materials after melt mixing to 90 ℃ to obtain the glue with a liquid state suitable for coating. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 2
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin in the treatment I, 10 parts by weight of trimethylolpropane diallyl ether, 10 parts by weight of pentaerythritol acrylic ester, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenylpropanone-1 into a glue melting tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 3
Under the condition of avoiding light, adding 100 parts by weight of 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-phenylpropanone-1 into a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 4
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin in the treatment I, 5 parts by weight of acrylic acid-2-ethylhexyl ester, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylic ester, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenylpropionyl-1 into a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the materials after melt mixing to 90 ℃ to obtain the glue with a liquid state suitable for coating. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a BOPP release film having a thickness of 60. Mu.m, the glue coating thickness was 15. Mu.m, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 5
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin, 5 parts by weight of isobornyl acrylate, 10 parts by weight of tetra-propylene 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-phenylpropionyl-1 in the treatment I into a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the materials after melt mixing to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 6
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin, 10 parts by weight of trimethylol acrylic ester, 10 parts by weight of isobornyl acrylic ester, 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 in a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 7
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin, 5 parts by weight of dipropylene glycol diacrylate, 5 parts by weight of trimethylolpropane acrylate 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-phenylpropionyl-1 into a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 8
Under the light-shielding condition, 100 parts by weight of the modified acrylic resin in the treatment I and 5 parts by weight of the acrylic resin are mixedAdding 2-ethylhexyl acrylate, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylic ester, 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-phenylpropanone-1 into a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all the materials, and naturally cooling the materials after the melt mixing to 90 ℃ to obtain the glue which is suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 9
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin in the treatment I, 5 parts by weight of acrylic acid-2-ethylhexyl ester, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylic ester, 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-phenylpropionyl-1 into a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the materials after melt mixing to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 10
Under the light-shielding condition, 100 parts by weight of the modified acrylic resin in the treatment III and 5 parts by weight of acrylic acid-2-ethylAdding hexyl ester, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylic ester, 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 for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Example 11
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin in treatment III, 5 parts by weight of acrylic acid-2-ethylhexyl ester, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylic ester, 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-phenylpropionyl-1 into a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the materials after melt mixing to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Comparative example 1
Under the condition of light shielding, 100 parts by weight of the modified acrylic resin in the treatment I, 10 parts by weight of 2-ethylhexyl acrylate and 20 parts by weight ofAdding trimethylolpropane diallyl ether, 10 parts by weight of pentaerythritol acrylic ester, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenyl acetone-1 into a melt adhesive groove, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a BOPP release film having a thickness of 60. Mu.m, the glue coating thickness was 15. Mu.m, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Comparative example 2
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin in the treatment I, 10 parts by weight of acrylic acid-2-ethylhexyl ester, 20 parts by weight of trimethylolpropane diallyl ether, 10 parts by weight of pentaerythritol acrylic ester, 3 parts by weight of terpene resin and 1 part by weight of 2-hydroxy-2-methyl-phenylpropanone-1 into a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a BOPP release film having a thickness of 60. Mu.m, the glue coating thickness was 15. Mu.m, the coating speed was 100m/min, and the UV radiation amount was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Comparative example 3
Under the condition of light-shielding, 100 parts by weight of modified acrylic resin (commercially available with 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 and 5 parts by weight ofAdding pentaerythritol acrylic ester, 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 melt adhesive groove, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm thick PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation dose was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Comparative example 4
Under the condition of avoiding light, adding 100 parts by weight of modified acrylic resin, 5 parts by weight of acrylic acid-2-ethylhexyl ester, 10 parts by weight of trimethylolpropane diallyl ether, 5 parts by weight of pentaerythritol acrylic ester, 3 parts by weight of terpene resin, 2 parts by weight of blue pigment and 1 part by weight of 2-hydroxy-2-methyl-phenylpropionyl-1 in a melt adhesive tank, introducing nitrogen for protection, heating to 100 ℃, stirring for 30min at a stirring speed of 500r/min, completely melting and uniformly mixing all materials, and naturally cooling the melted and mixed materials to 90 ℃ to obtain the glue suitable for coating in a liquid state. And then conveying the glue completely melted by the hot melting process to a coating head by using a pump, coating the glue on the substrate layer 2, curing the glue by using a UV lamp to form a glue layer 1, and rolling to obtain the protective film. Wherein the substrate layer 2 used in this example was a 50 μm thick PET release film, the glue coating thickness was 15 μm, the coating speed was 100m/min, and the UV radiation dose was 200mJ/cm 2 (wavelength 300-400 nm), the irradiation time of the glue curing is 20s.
Test case
1. Experimental construction mode
The protective films prepared in examples 1 to 11 and comparative examples 1 to 4 were subjected to initial adhesion of rolling balls, peeling force of steel plates, peeling force of aluminum plastic films after high temperature and high pressure, and high temperature and high pressure glue stain tests.
Ball primary adhesion test: the protective films prepared using examples 1 to 11 and comparative examples 1 to 4 were subjected to initial adhesion test of the rolling ball according to the method in national standard GB/T4852-2002.
Peel force test: the protective films prepared using examples 1 to 11 and comparative examples 1 to 4 were subjected to peel strength test according to the method in national standard GB/T2792-2014.
2. Experimental results
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. In general, the steel plate peeling force for the battery protective film adhesive tape is preferably in the range of 0.1 to 0.3N/25mm, and the aluminum plastic film peeling force after high temperature and high pressure is preferably in the range of 0.3 to 0.5N/25mm. Test results show that the protective film prepared by the preferred scheme of the invention meets the range of the better performance requirements of the protective film in terms of initial adhesion and stripping performance, and has good appearance.
TABLE 1 results of test on the properties of the protective films prepared in examples 1 to 11 and comparative examples 1 to 4
As can be seen from Table 1, the protective films in examples 1 to 4 have good initial adhesion and peeling properties, and the prepared hot melt coating protective film has uniform thickness and good appearance. The protective films of examples 5 to 7 were low in both initial adhesion and peeling force and were prone to degluing, which did not meet the performance requirements for the protective films. The protective films of examples 8 to 10 were low in initial adhesion and peeling force, and their properties were not within the range of properties required for the present invention. The protective film in example 11 has good initial adhesion and peeling properties.
The comparative example 1, which does not contain tackifying resin, has lower initial adhesion and peeling force of the protective film, and its performance is not within the performance range required by the present invention. The protective film of comparative example 2 had good initial adhesion and peeling properties, consistent with the properties required by the present invention. The protective film of comparative example 3 was low in initial adhesion and peeling force due to too large molecular weight of the modified polyacrylate, and was uneven in adhesive surface and poor in flatness when coated. The modified acrylic ester adopted in comparative example 4 is synthesized by a one-step feeding method, so that the formed protective film has lower initial adhesion and stripping force and poorer flatness.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and 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 modifications or equivalent substitutions can be made to the technical solution of the present invention, but these modifications or substitutions are all within the scope of the present invention.

Claims (6)

1. A special protection film of hot melt UV coating lithium cell, its characterized in that: the adhesive comprises an adhesive layer and a substrate layer, wherein the adhesive layer is formed by Ultraviolet (UV) light curing of glue, and the glue comprises, by weight, 90-110 parts of modified polyacrylate, 5-50 parts of reactive diluent, 3-10 parts of tackifying resin and 0.1-5 parts of photoinitiator;
the reactive diluents include 2-ethylhexyl acrylate, trimethylolpropane diallyl ether and pentaerythritol acrylate;
the modified polyacrylate is isocyanate modified polyacrylate;
the tackifying resin is terpene resin;
the preparation method of the modified polyacrylate comprises the following steps:
step one, uniformly mixing an acrylic ester monomer and a thermal initiator to form a mixed solution;
step two, taking part of the mixed solution in the step one, heating to 60-90 ℃ firstly, carrying out heat preservation reaction for 0.5-2 hours, then adding the rest of the mixed solution into the mixed solution, and carrying out heat preservation reaction for 2-6 hours to obtain polyacrylate;
step three, heating the polyacrylate in the step two, evacuating to remove water, cooling to 65-70 ℃, adding isocyanate monomer into the polyacrylate, reacting for 1.5-3 hours at a temperature, adding catalyst, reacting for 3-6 hours at a temperature, adding polymerization inhibitor, and uniformly mixing to obtain modified polyacrylate;
the acrylic ester monomer comprises a hydroxyl-containing acrylic ester monomer and a non-functional acrylic ester monomer, and the glass transition temperature of the non-functional acrylic ester monomer ranges from-80 ℃ to-20 ℃;
the proportion of the non-functional acrylate monomer in the acrylate monomer is not less than 83wt%, and the proportion of the hydroxyl-containing acrylate monomer in the acrylate monomer is not less than 1wt%.
2. The hot-melt UV-coated lithium battery-dedicated protective film according to claim 1, wherein: the glass transition temperature of the modified polyacrylate ranges from-80 ℃ to-20 ℃.
3. The hot-melt UV-coated lithium battery-dedicated protective film according to claim 1, wherein: the number average molecular weight of the modified polyacrylate ranges from 2 ten thousand to 20 ten thousand.
4. The hot-melt UV-coated lithium battery-dedicated protective film according to claim 1, wherein: the acrylate monomer further comprises a functional acrylate monomer, wherein the ratio of the functional acrylate monomer in the acrylate monomer is not less than 0.1wt%, and the functional acrylate monomer is at least one selected from acrylic acid, methacrylic acid, glycidyl acrylate and glycidyl methacrylate.
5. The special protection film for hot-melt UV-coated lithium batteries according to any one of claims 1 to 4, 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 formed by the steps until the mixture is uniformly mixed to form the glue;
and secondly, after the glue is cooled to a proper coating temperature, coating the glue on the base material, and then performing photo-curing and rolling simultaneously to obtain the special protective film for the lithium battery.
6. The protective film for hot-melt UV-coated lithium battery according to claim 5, 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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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

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* 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

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