CN115678448B - Acrylic acid pressure-sensitive adhesive for cell blue film and humidity and heat aging resistance, and preparation method and application thereof - Google Patents
Acrylic acid pressure-sensitive adhesive for cell blue film and humidity and heat aging resistance, and preparation method and application thereof Download PDFInfo
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- CN115678448B CN115678448B CN202211271201.6A CN202211271201A CN115678448B CN 115678448 B CN115678448 B CN 115678448B CN 202211271201 A CN202211271201 A CN 202211271201A CN 115678448 B CN115678448 B CN 115678448B
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 230000032683 aging Effects 0.000 title abstract description 36
- 239000003999 initiator Substances 0.000 claims abstract description 34
- 239000002390 adhesive tape Substances 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims abstract description 21
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims abstract description 14
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 12
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims abstract description 11
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 11
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000010410 layer Substances 0.000 claims description 57
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 32
- 239000000758 substrate Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 13
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- -1 polyethylene terephthalate Polymers 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- MABAWBWRUSBLKQ-UHFFFAOYSA-N ethenyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)C=C MABAWBWRUSBLKQ-UHFFFAOYSA-N 0.000 claims description 5
- PJUIMOJAAPLTRJ-UHFFFAOYSA-N monothioglycerol Chemical compound OCC(O)CS PJUIMOJAAPLTRJ-UHFFFAOYSA-N 0.000 claims description 5
- 229940035024 thioglycerol Drugs 0.000 claims description 5
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 claims description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 4
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 2
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 4
- 239000000853 adhesive Substances 0.000 abstract description 11
- 230000001070 adhesive effect Effects 0.000 abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 7
- 230000000630 rising effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 24
- 230000008859 change Effects 0.000 description 12
- 239000000126 substance Substances 0.000 description 10
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 9
- 229910000077 silane Inorganic materials 0.000 description 9
- 239000011268 mixed slurry Substances 0.000 description 8
- 239000004925 Acrylic resin Substances 0.000 description 6
- 229920000178 Acrylic resin Polymers 0.000 description 6
- 239000006087 Silane Coupling Agent Substances 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 6
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011265 semifinished product Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000003313 weakening effect Effects 0.000 description 4
- 229910002803 Si-O-Fe Inorganic materials 0.000 description 3
- 229910002802 Si–O–Fe Inorganic materials 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 229920001400 block copolymer Polymers 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 240000007126 Citrus medica var. sarcodactylis Species 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011417 postcuring Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 239000005028 tinplate Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The application provides an acrylic pressure-sensitive adhesive for a cell blue film and humidity and heat aging resistance, and a preparation method and application thereof, wherein the preparation raw materials of the acrylic pressure-sensitive adhesive comprise the following components in parts by weight: 15-25 parts of isooctyl acrylate, 50-60 parts of n-butyl acrylate, 6-10 parts of hydroxypropyl acrylate and/or hydroxyethyl acrylate, 2-5 parts of methacrylic acid, 5-10 parts of acrylic acid, 0.5-2 parts of vinyl silane, 2-10 parts of vinyl acetate, 0.1-0.4 part of chain transfer agent, 0.25-0.5 part of initiator and 20-40 parts of solvent. The acrylic acid pressure-sensitive adhesive provided by the application is matched with a certain curing agent and color paste to prepare the cell blue film adhesive tape, and the cell blue film adhesive tape is attached to a square aluminum shell cell, so that the edge folding angle of at least 240h can be kept from rising, the peeling force rises to be lower than 40% after aging at 85 ℃ and 85%RH and 500h, no residual adhesive is generated, and the aging resistance is excellent.
Description
Technical Field
The application belongs to the technical field of pressure-sensitive adhesives, and relates to an acrylic pressure-sensitive adhesive for a cell blue film and humidity and heat aging resistance, and a preparation method and application thereof.
Background
Currently, with the rapid popularization of new energy automobiles and the continuous expansion of the power battery industry scale, the production standard, quality and safety control of lithium batteries are also becoming strict and mature. The blue film is used as an important process in the production process of the lithium battery cell, plays roles in protecting and insulating the cell, and also improves the performance requirement of the blue film. At present, the requirements of the traditional anti-warping performance, peeling force, initial adhesion, holding adhesion and the like of the blue film are met, and the ageing resistance in a high-temperature and high-humidity environment is also provided, wherein the change of the peeling force before and after ageing is required to be less than 40%.
In a high humidity environment, water vapor can weaken the adhesive bonding interface, so that the interface bonding force is weakened. And under the condition of high temperature and high humidity, the post-curing strengthening effect of the adhesive at high temperature and the weakening effect of the adhesive interface at high humidity exist at the same time, and the strengthening effect is far greater than the weakening effect. In order to simulate the working environment of the battery cell, a high-temperature high-humidity aging test is adopted to detect the change condition of the stripping force of the blue film of the battery cell. After the existing cell blue film is subjected to high-temperature high-humidity aging test, the stripping force can be greatly improved, even by more than 100%, and the existing cell blue film is accompanied by the problems of residual glue and the like, and does not meet the current performance requirements of the blue film.
Accordingly, there is a need in the art to develop an acrylic pressure sensitive adhesive for use in cell blue films that is resistant to wet heat aging.
Disclosure of Invention
Aiming at the defects of the prior art, the application aims to provide an acrylic pressure-sensitive adhesive for a cell blue film and humidity and heat aging resistance, and a preparation method and application thereof. The acrylic acid pressure-sensitive adhesive provided by the application is matched with a certain curing agent and color paste to prepare the cell blue film adhesive tape, and the cell blue film adhesive tape is attached to a square aluminum shell cell, can keep at least 240h edge folding angle from rising, can keep the stripping force from rising to be lower than 40% after aging at 85 ℃ and 85%RH and 500h, can preferably be lower than 30% after aging, does not generate residual glue, has excellent ageing resistance, has simple and feasible production process, and can be applied to cell blue films of new energy batteries.
In order to achieve the aim of the application, the application adopts the following technical scheme:
in a first aspect, the application provides an acrylic pressure-sensitive adhesive for a cell blue film and humidity and heat aging resistance, which is prepared from the following raw materials in parts by weight: 15-25 parts of isooctyl acrylate, 50-60 parts of n-butyl acrylate, 6-10 parts of hydroxypropyl acrylate and/or hydroxyethyl acrylate, 2-5 parts of methacrylic acid, 5-10 parts of acrylic acid, 0.5-2 parts of vinyl silane, 2-10 parts of vinyl acetate, 0.1-0.4 part of chain transfer agent, 0.25-0.5 part of initiator and 20-40 parts of solvent.
According to the application, the specific raw materials are selected, and the content of each component is controlled, so that the prepared acrylic pressure-sensitive adhesive has the advantages of humidity resistance and heat aging resistance, and can keep stable stripping force and small change.
In the present application, the acrylic pressure-sensitive adhesive may be prepared from the raw materials in an amount of 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, or the like.
In the preparation raw materials of the acrylic pressure-sensitive adhesive, the dosage of the n-butyl acrylate can be 50 parts, 51 parts, 52 parts, 53 parts, 54 parts, 55 parts, 56 parts, 57 parts, 58 parts, 59 parts or 60 parts and the like.
In the present application, the hydroxy propyl acrylate and/or hydroxy ethyl acrylate may be used in an amount of 6 parts, 7 parts, 8 parts, 9 parts or 10 parts, etc. in the raw materials for preparing the acrylic pressure-sensitive adhesive.
In the present application, the acrylic pressure-sensitive adhesive may be prepared using 2 parts, 3 parts, 4 parts, 5 parts, etc. of methacrylic acid.
In the present application, the acrylic pressure-sensitive adhesive may be prepared from 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, or the like.
In the present application, the vinyl silane may be used in an amount of 0.5 part, 1 part, 1.5 parts, 2 parts, or the like in the raw material for the preparation of the acrylic pressure-sensitive adhesive.
In the present application, the acrylic pressure-sensitive adhesive may be prepared from 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts or 10 parts of vinyl acetate.
In the present application, the chain transfer agent may be used in an amount of 0.1 part, 0.2 part, 0.3 part, 0.4 part, or the like in the raw material for the preparation of the acrylic pressure-sensitive adhesive.
In the present application, the initiator may be used in an amount of 0.25 parts, 0.3 parts, 0.35 parts, 0.4 parts, 0.45 parts, 0.5 parts, or the like in the raw materials for preparing the acrylic pressure-sensitive adhesive.
In the present application, the acrylic pressure-sensitive adhesive may be prepared from 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, or the like.
Preferably, the acrylic pressure-sensitive adhesive comprises the following raw materials in parts by weight: 15-20 parts of isooctyl acrylate, 52-58 parts of n-butyl acrylate, 7-9 parts of hydroxypropyl acrylate and/or hydroxyethyl acrylate, 3-5 parts of methacrylic acid, 6-8 parts of acrylic acid, 1-1.5 parts of vinyl silane, 4-8 parts of vinyl acetate, 0.15-0.3 part of chain transfer agent, 0.3-0.4 part of initiator and 20-40 parts of solvent.
Preferably, the vinylsilane comprises any one or a combination of at least two of vinyltriisopropoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane or vinyltris (β -methoxyethoxy) silane, preferably vinyltriisopropoxysilane and/or vinyltris (β -methoxyethoxy) silane.
Preferably, the chain transfer agent includes thiol compounds such as thioglycerol and/or mercaptoethanol.
Preferably, the initiator comprises azobisisobutyronitrile.
Preferably, the solvent comprises ethyl acetate.
In a second aspect, the present application provides a method for preparing the acrylic pressure-sensitive adhesive according to the first aspect, the method comprising the steps of:
a) Adding a solvent into a reactor, and preheating;
b) Mixing isooctyl acrylate, n-butyl acrylate, hydroxypropyl acrylate and/or hydroxyethyl acrylate, methacrylic acid, acrylic acid, chain transfer agent and partial initiator according to the formula amount to obtain a mixture, and adding the mixture into the preheated solvent in the step a) for reaction;
c) Continuously adding part of initiator to react;
d) Continuously adding vinyl silane to react;
e) Continuously adding the rest initiator and vinyl acetate to react;
f) And cooling to obtain the acrylic pressure-sensitive adhesive.
In the present application, in step b), various monomers are reacted to form an acrylate, and the vinyl silane and acrylate form a block copolymer having the following chemical structure:
wherein R, R 'and R' each represent a different alkyl group.
Silane has the characteristics of high temperature resistance, oxidation resistance, low surface energy, good flexibility and the like, and is a great hot spot for research in the field of functional materials. The application adopts vinyl silane, and introduces the silane into a polyacrylate molecular chain through copolymerization of C=C and acrylic ester, and the silane is tightly combined in a covalent bond mode. In a high-temperature and high-humidity environment, silane can migrate to the surface with more water to generate silanol substances through hydrolysis reaction, and then the silanol substances and-OH on the surface of tin (or aluminum) (the material of the battery core is generally steel or aluminum) are subjected to dehydration condensation reaction to form Si-O-Fe (Al) chemical bonds, so that the high-temperature aging resistance of the acrylic pressure-sensitive adhesive can be improved. Part of unreacted silanol has a hydrophobic effect, and hydrogen atoms on-OH and oxygen atoms on the surface of tin (or aluminum) form intermolecular hydrogen bonds, so that the hydrophobicity can be further improved, and the weakening effect of water vapor on an adhesive interface is reduced. Therefore, the block copolymer formed by vinyl silane and acrylic ester has the advantages of wet heat aging resistance, can keep stable stripping force and has small change. The action mechanism is as follows:
however, as the amount of silane increases, the opposite effect occurs. On one hand, a network structure is formed between the silane coupling agent and the acrylic resin to form an interpenetrating potential, so that the adhesive force of the polymer is increased; on the other hand, an excessive amount of the silane coupling agent may cause self-polymerization to form local crosslinking, affecting the flexibility of the acrylic resin of the main body, and further causing a decrease in the anti-warping property. Therefore, the silane coupling agent should be added in an appropriate amount within a certain range, and the amount thereof should not be too large.
Preferably, the preheating of step a) is performed under an inert atmosphere.
Preferably, the inert atmosphere comprises nitrogen.
Preferably, the temperature of the preheating in step a) is 70-75 ℃, e.g. 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃ or 75 ℃, etc., and the time of the preheating is 30-40min, e.g. 30min, 33min, 35min, 38min or 40min, etc.
Preferably, the part of the initiator in step b) is 1/4 of the total amount of initiator.
Preferably, the adding the mixture to the preheated solvent in step a) in step b) specifically includes: the mixture is added dropwise to the preheated solvent of step a) at a constant speed over a period of 1.5-2 hours (e.g., 1.5 hours, 1.8 hours, or 2 hours, etc.), and the reaction temperature is maintained at 78-82 ℃, e.g., 78 ℃, 79 ℃, 80 ℃, 81 ℃, 82 ℃, etc.
Preferably, the temperature of the reaction in step b) is 78-82 ℃, e.g. 78 ℃, 79 ℃, 80 ℃, 81 ℃ or 82 ℃, etc., and the time of the reaction is 0.5-1.5h, e.g. 0.5h, 0.8h, 1h, 1.2h or 1.5h, etc.
Preferably, the part of the initiator in step c) is 1/4 of the total amount of initiator.
Preferably, the temperature of the reaction in step c) is 80-82 ℃, e.g. 80 ℃, 81 ℃ or 82 ℃, etc., and the time of the reaction is 0.5-1.5h, e.g. 0.5h, 0.8h, 1h, 1.2h or 1.5h, etc.
Preferably, the temperature of the reaction in step d) is 80-82 ℃, e.g. 80 ℃, 81 ℃ or 82 ℃, etc., and the time of the reaction is 1.5-2 hours, e.g. 1.5 hours, 1.8 hours or 2 hours, etc.
Preferably, the temperature of the reaction in step e) is 82-84 ℃, e.g. 82 ℃, 83 ℃ or 84 ℃ etc., and the time of the reaction is 1.5-2 hours, e.g. 1.5 hours, 1.8 hours or 2 hours etc.
Preferably, the temperature reduction in step f) is to a temperature of 50-55deg.C, such as 50deg.C, 51deg.C, 52 deg.C, 53 deg.C, 54 deg.C or 55deg.C, etc.
As a preferred technical scheme of the application, the preparation method comprises the following steps:
a) Will dissolveThe agent is added into the reactor, at N 2 Preheating at 70-75deg.C for 30-40min in the atmosphere;
b) Mixing isooctyl acrylate, n-butyl acrylate, hydroxypropyl acrylate and/or hydroxyethyl acrylate, methacrylic acid, acrylic acid, chain transfer agent and partial initiator to obtain a mixture, dripping the mixture into the preheated solvent in the step a) at a constant speed within 1.5-2h, keeping the reaction temperature at 78-82 ℃, and continuing to react for 0.5-1.5h at 78-82 ℃ after dripping is finished; wherein, part of the initiator is 1/4 of the total amount of the initiator;
c) Continuously adding part of initiator, and reacting for 0.5-1.5h at 80-82 ℃; wherein, part of the initiator is 1/4 of the total amount of the initiator;
d) Continuously adding vinyl silane, and reacting for 1.5-2h at 80-82 ℃;
e) Continuously adding the rest initiator and vinyl acetate, and reacting for 1.5-2h at 82-84 ℃;
f) Cooling to 50-55 ℃, discharging to obtain the acrylic pressure-sensitive adhesive.
The application provides a battery cell blue film adhesive tape capable of resisting wet heat aging, which comprises a release film layer, a first acrylic acid pressure sensitive adhesive layer, a first substrate layer, a second acrylic acid pressure sensitive adhesive layer and a second substrate layer which are sequentially laminated;
the preparation raw materials of the first acrylic pressure-sensitive adhesive layer and the second acrylic pressure-sensitive adhesive layer comprise: the acrylic pressure sensitive adhesive, curing agent and blue film color paste of the first aspect.
Namely, the cell blue film adhesive tape of the present application has a double-layer structure. The thickness of the release film layer, the first acrylic pressure-sensitive adhesive layer, the first substrate layer, the second acrylic pressure-sensitive adhesive layer and the second substrate layer in the cell blue film adhesive tape is not particularly limited, and can be adjusted according to the requirements of customers.
Preferably, the materials of the first substrate layer and the second substrate layer each comprise polyethylene terephthalate (PET).
Preferably, the mass ratio of the acrylic pressure-sensitive adhesive to the curing agent to the blue film color paste is 100 (0.8-1.2): (3-8), for example 100:0.8:3, 100:0.8:5, 100:0.8:8, 100:1:3, 100:1:5, 100:1:8, 100:1.2:3, 100:1.2:5 or 100:1.2:8, etc., and more preferably 100 (0.9-1.1): (4-6).
Preferably, the curing agent comprises an isocyanate-based curing agent.
Preferably, the preparation raw materials of the first acrylic pressure sensitive adhesive layer and the second acrylic pressure sensitive adhesive layer further comprise a solvent.
Preferably, the solvent comprises ethyl acetate.
It should be noted that the preparation method of the battery cell blue film adhesive tape is not particularly limited, and the preparation method can be exemplified by the following method:
(1) Mixing an acrylic pressure-sensitive adhesive, a curing agent, a blue film color paste and an optional solvent to obtain first mixed slurry, coating the first mixed slurry on one surface of a first substrate layer by using a scraper to form a first acrylic pressure-sensitive adhesive layer, and attaching a release film on one surface of the first acrylic pressure-sensitive adhesive layer, which is far away from the first substrate layer, so as to obtain a semi-finished product;
(2) Mixing an acrylic pressure-sensitive adhesive, a curing agent, a blue film color paste and an optional solvent to obtain second mixed slurry, coating the second mixed slurry on one surface of a second substrate layer by using a scraper to form a second acrylic pressure-sensitive adhesive layer, and then bonding and curing the second acrylic pressure-sensitive adhesive layer with the semi-finished product in the step (1) to obtain the cell blue film adhesive tape, wherein the first substrate layer and the second acrylic pressure-sensitive adhesive layer are adjacently arranged.
Preferably, the curing is first baked at 70-90 ℃ (e.g., 70 ℃, 75 ℃, 80 ℃,85 ℃, or 90 ℃ etc.) for 3-8min (e.g., 3min, 5min, or 8min, etc.), and then cured at 45-55 ℃ (e.g., 45 ℃, 48 ℃, 50 ℃, 53 ℃, or 55 ℃ etc.) for 70-80h (e.g., 70h, 72h, 74h, 76h, 78h, or 80h, etc.).
Compared with the prior art, the application has the following beneficial effects:
(1) The application adopts vinyl silane, and introduces the silane into a polyacrylate molecular chain through copolymerization of C=C and acrylic ester, and the silane is tightly combined in a covalent bond mode. In a high-temperature and high-humidity environment, silane can migrate to the surface with more water to generate hydrolysis reaction to generate silanol substances, and then the silanol substances and-OH on the surface of tin (or aluminum) are subjected to dehydration condensation reaction to form Si-O-Fe (Al) chemical bonds, so that the high-temperature aging resistance of the acrylic pressure-sensitive adhesive can be improved. Meanwhile, due to the existence of Si-O-Fe (Al) chemical bonds, the pressure-sensitive adhesive is not easy to generate cohesive failure at high temperature, and no residual adhesive or ghost is left when the pressure-sensitive adhesive is peeled off from a metal plate after ageing.
(2) After the silane is hydrolyzed, part of unreacted silanol has a hydrophobic effect, hydrogen atoms on-OH and oxygen atoms on the surface of the tin plate form intermolecular hydrogen bonds, so that the hydrophobicity can be further improved, and the weakening effect of water vapor on an adhesive interface is reduced. Therefore, the block copolymer formed by vinyl silane and acrylic ester has the advantages of wet heat aging resistance, can keep stable stripping force and has small change.
(3) The acrylic acid pressure-sensitive adhesive provided by the application is matched with a certain curing agent and color paste to prepare the cell blue film adhesive tape, and the cell blue film adhesive tape is attached to a square aluminum shell cell, so that the edge folding angle of at least 240h can be kept not to rise, the peeling force rises to be lower than 40% after aging at 85 ℃ and 85%RH and 500h, no residual glue is generated, the aging resistance is excellent, the production process is convenient and easy to implement, and the current use requirement on a new energy cell blue film can be met.
Drawings
Fig. 1 is an infrared spectrum of an acrylic pressure-sensitive adhesive provided in example 1 of the present application.
Detailed Description
The technical scheme of the application is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the application and are not to be construed as a specific limitation thereof.
The raw material information used in the examples and comparative examples of the present application is as follows:
isooctyl acrylate, n-butyl acrylate, hydroxypropyl acrylate, methacrylic acid, acrylic acid, vinyl acetate, available from the commercial company, bard, analytical purity;
vinyl triisopropoxysilane available from ark (fingered citron chemical materials limited under the model AC-76;
vinyl triethoxysilane, model KH151, available from shandong, new materials inc;
vinyl tri (beta-methoxyethoxy) silane, model ZQ-172, available from Hubeixing, new Material technology Co., ltd;
the initiator was azobisisobutyronitrile, the chain transfer agent was thioglycerol, available from alaa Ding Shiji (Shanghai) limited, analytically pure;
ethyl acetate, sigma aldrich (Shanghai) trade limited, analytically pure;
a curing agent, available from kesijugao polymer (chinese) limited, model Desmodur L75;
color paste, available from Hangzhou Fucai New Material technology Co., ltd, model number JQ1313.
Examples 1 to 6
In examples 1-6, an acrylic pressure-sensitive adhesive for cell blue film and humidity and heat aging resistance is provided, and the raw materials for preparing the acrylic pressure-sensitive adhesive are shown in table 1 in parts by weight.
TABLE 1
In table 1, "/" indicates that no corresponding raw material was added.
The preparation method comprises the following steps:
a) Adding ethyl acetate solvent into a four-necked flask, and adding the ethyl acetate solvent into the four-necked flask in N 2 Preheating for 30min at 75 ℃ in the atmosphere;
b) Uniformly mixing isooctyl acrylate, n-butyl acrylate, hydroxypropyl acrylate, methacrylic acid, acrylic acid, chain transfer agent (thioglycerol) and partial initiator (1/4 of the total amount of the initiator, azodiisobutyronitrile) according to the formula amount to obtain a mixture, uniformly dripping the mixture into the preheated solvent in the step a) within 2h, keeping the reaction temperature at 80 ℃, and continuing to react for 1h at 80 ℃ after dripping is finished;
c) Part of the initiator (1/4 of the total amount of initiator, azobisisobutyronitrile) was added and reacted at 80℃for 1h;
d) Continuously adding vinyl silane, and reacting for 2 hours at 80 ℃;
e) Continuously adding the rest initiator and vinyl acetate, and reacting for 1.5h at 84 ℃;
f) Cooling to 50 ℃, discharging to obtain the acrylic pressure-sensitive adhesive.
The infrared spectrogram of the acrylic pressure-sensitive adhesive provided in example 1 of the present application is shown in FIG. 1, and it can be seen that 1728cm -1 The peak characteristic of carbonyl groups of acrylic acid and methacrylic acid is 1640cm -1 There was no characteristic peak of c=c, and 1117cm -1 The stretching vibration peak of Si-O bond indicates that all C=C of vinylsilane participates in the reaction, and the copolymerization generates the chemical bond of Si-O-C, which indicates that the vinylsilane and the acrylic ester form a copolymer.
Comparative examples 1 to 5
In comparative examples 1 to 5, an acrylic pressure-sensitive adhesive for a cell blue film was provided, and the preparation raw materials of the acrylic pressure-sensitive adhesive were as shown in table 2 in parts by weight.
TABLE 2
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
| Isooctyl acrylate | 20 | 20 | 20 | 20 | 20 |
| Acrylic acid n-butyl ester | 55 | 55 | 55 | 55 | 55 |
| Hydroxypropyl acrylate | 8 | 8 | 8 | 8 | 8 |
| Methacrylic acid | 4 | 4 | 4 | 4 | 4 |
| Acrylic acid | 7 | 7 | 7 | 7 | 7 |
| Thioglycerol | 0.20 | 0.20 | 0.20 | 0.20 | 0.20 |
| Azobisisobutyronitrile | 0.35 | 0.35 | 0.35 | 0.35 | 0.35 |
| Vinyl triisopropoxysilane | 0 | 3 | 5 | 1 | 1 |
| Vinyl acetate | 6 | 6 | 6 | 0 | 13 |
| Acetic acid ethyl ester | 30 | 30 | 30 | 30 | 30 |
The preparation method is the same as that of the example.
Application examples 1 to 6 and comparative application examples 1 to 5
In application examples 1 to 6, a cell blue film tape comprising a release film layer (thickness: 30 μm), a first acrylic pressure-sensitive adhesive layer (thickness: 30 μm), a first base material layer (thickness: 25 μm), a second acrylic pressure-sensitive adhesive layer (thickness: 19 μm) and a second base material layer (thickness: 36 μm) laminated in this order was provided, respectively;
the preparation raw materials of the first acrylic acid pressure-sensitive adhesive layer and the second acrylic acid pressure-sensitive adhesive layer comprise the following components in parts by weight: 100 parts of acrylic pressure-sensitive adhesive (acrylic pressure-sensitive adhesive provided in examples 1-6 and comparative examples 1-5 respectively), 1 part of curing agent (Desmodur L75), 5 parts of blue film color paste (JQ 1313) and 200 parts of solvent (ethyl acetate);
the first substrate layer and the second substrate layer are both made of PET.
The preparation method comprises the following steps:
(1) Mixing the formula amount of acrylic pressure-sensitive adhesive, a curing agent, blue film color paste and a solvent to obtain first mixed slurry, coating the first mixed slurry on one surface of a first substrate layer by using a scraper to form a first acrylic pressure-sensitive adhesive layer, and attaching a release film on one surface of the first acrylic pressure-sensitive adhesive layer, which is far away from the first substrate layer, so as to obtain a semi-finished product;
(2) Mixing the formula amount of acrylic pressure-sensitive adhesive, a curing agent, blue film color paste and a solvent to obtain second mixed slurry, coating the second mixed slurry on one surface of a second substrate layer by using a scraper to form a second acrylic pressure-sensitive adhesive layer, then bonding with the semi-finished product in the step (1), firstly baking at 80 ℃ for 5min, and then curing at 50 ℃ for 72h to obtain the cell blue film adhesive tape, wherein the first substrate layer and the second acrylic pressure-sensitive adhesive layer are adjacently arranged.
Comparative application example 6
The comparative application example differs from application example 1 only in that the preparation raw materials of the first acrylic pressure-sensitive adhesive layer and the second acrylic pressure-sensitive adhesive layer each comprise the following components in parts by weight: 100 parts of acrylic pressure-sensitive adhesive, 0.6 part of curing agent (Desmodur L75), 5 parts of blue film color paste (JQ 1313) and 200 parts of solvent (ethyl acetate).
Comparative application example 7
The comparative application example differs from application example 1 only in that the preparation raw materials of the first acrylic pressure-sensitive adhesive layer and the second acrylic pressure-sensitive adhesive layer each comprise the following components in parts by weight: 100 parts of acrylic pressure-sensitive adhesive, 1.5 parts of curing agent (Desmodur L75), 5 parts of blue film color paste (JQ 1313) and 200 parts of solvent (ethyl acetate).
The performance test was performed on the cell blue film tapes provided in application examples 1 to 6 and comparative application examples 1 to 7, as follows:
(1) 180 ° peel force: measured according to GB/T2792-1998 standard (peeling speed 300 mm/min);
(2) Initial adhesion: the measurement is carried out according to the GB/T4852-2002 standard, and the requirements are that: initial adhesion ball >9#;
(3) Holding force: the measurement was carried out according to GB/T4851-1998 standard (80 ℃);
(4) Adhesive tape thickness (excluding release film): after drying, the thickness of the adhesive tape is (110+/-2) mu m;
(5) Anti-warping performance: sticking a blue film adhesive tape around the square aluminum shell battery cell, sticking the folded corner edge with a width of about 5mm, checking the adhesive tape 1 time every 24 hours, checking whether the folded corner edge is tilted or not, and recording the time when the folded corner edge of the adhesive tape is tilted;
(6) Resistance to thermal aging under humidity: according to GB/T2792-1998 standard, sticking a blue film adhesive tape on an Al plate, pressing the adhesive tape back and forth for 3 times, standing for 2 hours, standing for 500 hours in an environment of 85 ℃ and 85%RH, taking out, standing for 24 hours, and then testing 180 DEG stripping force, wherein: the rate of change of peel force before and after testing on Al plates was <40% and no residual glue could occur, at least 3 samples per formulation were tested.
The results of the performance test are shown in Table 3.
TABLE 3 Table 3
As shown in Table 3, the 180 DEG stripping force of the cell blue film adhesive tapes provided in application examples 1-6 is 12.1-16.3N/25mm, the stripping force is moderate, the adhesive tape is applicable to the lamination process of most cell blue films, the initial adhesion, the holding adhesion and the anti-warping performance are qualified, no residual adhesive exists after aging for 500 hours at 85 ℃ and 85%RH, the stripping force change rate is less than 40%, wherein the stripping force change rate of the cell blue film adhesive tapes provided in application examples 1 and 3 is less than 30%, the moisture and heat aging resistance performance is excellent, and the comprehensive performance meets the current performance requirements on the cell blue film.
As is clear from Table 3, in comparative application example 1, since the acrylic pressure-sensitive adhesive was not added with a vinyl silane coupling agent, it was a pure acrylic resin, and the prepared adhesive tape had poor wet heat aging resistance, a peel force after aging was increased by >85%, and was accompanied with a residual adhesive, and failed.
In comparative application examples 2 and 3, since the vinyl silane coupling agent added to the acrylic pressure-sensitive adhesive is excessive, on one hand, it causes a decrease in the surface tension of the adhesive tape, and thus a decrease in the peel force thereof; on the other hand, the phenomenon of self-polymerization of the silane coupling agent is aggravated, local crosslinking is formed, the bonding with the acrylic resin of the main body is not tight, the flexibility of the acrylic resin is affected, and the anti-warping performance and the wet heat aging resistance of the adhesive tape are further reduced. Therefore, the time for raising is shorter, 192h and 120h are respectively, the change rate of the stripping force after aging is 48.5 percent and 62.3 percent respectively, the lifting speed of the stripping force is faster, and the product is disqualified.
In comparative application examples 4 and 5, the amount of the functional monomer vinyl acetate in the acrylic pressure-sensitive adhesive was changed, and the polar group-OH was introduced into the acrylic pressure-sensitive adhesive system, which can enhance the interaction with the adherend surface, and can improve the adhesion of the pressure-sensitive adhesive to the adherend surface. In comparative application example 4, since the acrylic pressure-sensitive adhesive does not contain vinyl acetate, the peeling force of the adhesive tape at normal temperature is low, 8.5N/25mm, and the anti-lifting performance thereof is not acceptable. Similarly, in comparative application example 5, the peel force of the tape was 18.2N/25mm, which was basically acceptable, due to the higher amount of vinyl acetate in the acrylic pressure-sensitive adhesive. Since an appropriate amount of vinyl silane was added to the acrylic pressure-sensitive adhesives of comparative application examples 4 and 5, the aging resistance was good and nearly acceptable.
In comparative application examples 6 and 7, the cohesion is affected by changing the amount of the curing agent, which results in a change in the crosslinking density of the system. The curing agent used in comparative application example 6 has the advantages of low crosslinking density, low cohesive force, poor holding power, residual adhesive after the adhesive tape is aged, quick lifting of stripping force and disqualification. The curing agent used in comparative application example 7 was in a large amount, so that the crosslinking density of the system was high, most of the functional groups of the acrylic resin, such as-OH, were reacted, resulting in a stiff film, a greatly reduced anti-warping property, and a reduced peeling force. However, the crosslinking density is high, so that the cohesive force of the system is high, and the humidity and heat aging resistance is enhanced.
In summary, the battery cell blue film adhesive tape provided in application examples 1-6 has the advantages that the 180-degree peeling force, the initial adhesion, the holding adhesion and the anti-warping performance are qualified, no residual adhesive exists after the battery cell blue film adhesive tape is aged at 85 ℃ for 85%RH and 500 hours, the peeling force change rate is less than 40%, the peeling force change rate of the battery cell blue film adhesive tape provided in application examples 1 and 3 is less than 30%, the humidity and heat aging resistance performance is more excellent, and the comprehensive performance meets the current performance requirements on the battery cell blue film.
The applicant states that the present application is described by the above examples for the cell blue film, the acrylic pressure-sensitive adhesive resistant to wet heat aging, and the preparation method and application thereof, but the present application is not limited to the above examples, i.e., it does not mean that the present application must be practiced depending on the above examples. It should be apparent to those skilled in the art that any modification of the present application, equivalent substitution of selected raw materials, addition of auxiliary components, selection of specific modes, etc. fall within the scope of the present application and the scope of disclosure.
Claims (18)
1. The battery cell blue film adhesive tape is characterized by comprising a release film layer, a first acrylic acid pressure sensitive adhesive layer, a first substrate layer, a second acrylic acid pressure sensitive adhesive layer and a second substrate layer which are sequentially laminated;
the preparation raw materials of the first acrylic pressure-sensitive adhesive layer and the second acrylic pressure-sensitive adhesive layer comprise: acrylic pressure-sensitive adhesive, curing agent and blue film color paste;
the mass ratio of the acrylic pressure-sensitive adhesive to the curing agent to the blue film color paste is 100 (0.8-1.2) to 3-8;
the acrylic pressure-sensitive adhesive comprises the following raw materials in parts by weight: 15-25 parts of isooctyl acrylate, 50-60 parts of n-butyl acrylate, 6-10 parts of hydroxypropyl acrylate and/or hydroxyethyl acrylate, 2-5 parts of methacrylic acid, 5-10 parts of acrylic acid, 0.5-2 parts of vinyl silane, 2-10 parts of vinyl acetate, 0.1-0.4 part of chain transfer agent, 0.25-0.5 part of initiator and 20-40 parts of solvent.
2. The cell blue film tape according to claim 1, wherein the vinyl silane comprises any one or a combination of at least two of vinyl triisopropoxy silane, vinyl trimethoxy silane, vinyl triethoxy silane, or vinyl tri (β -methoxyethoxy) silane.
3. The cell blue film tape according to claim 1, wherein the chain transfer agent comprises thioglycerol and/or mercaptoethanol.
4. The cell blue film tape according to claim 1, wherein the initiator comprises azobisisobutyronitrile.
5. The cell blue film tape according to claim 1, wherein the solvent comprises ethyl acetate.
6. The cell blue film adhesive tape according to claim 1, wherein the acrylic pressure sensitive adhesive is prepared by the following method:
a) Adding a solvent into a reactor, and preheating;
b) Mixing isooctyl acrylate, n-butyl acrylate, hydroxypropyl acrylate and/or hydroxyethyl acrylate, methacrylic acid, acrylic acid, chain transfer agent and partial initiator according to the formula amount to obtain a mixture, and adding the mixture into the preheated solvent in the step a) for reaction;
c) Continuously adding part of initiator to react;
d) Continuously adding vinyl silane to react;
e) Continuously adding the rest initiator and vinyl acetate to react;
f) And cooling to obtain the acrylic pressure-sensitive adhesive.
7. The cell blue film tape according to claim 6, wherein the preheating in step a) is performed at a temperature of 70-75 ℃ for a period of 30-40min.
8. The cell blue film tape according to claim 6, wherein the portion of the initiator in step b) is 1/4 of the total amount of initiator.
9. The cell blue film tape according to claim 6, wherein in step b) the mixture is added to the preheated solvent in step a), specifically comprising: dropwise adding the mixture into the preheated solvent in the step a) at a constant speed within 1.5-2h, and keeping the reaction temperature at 78-82 ℃.
10. The cell blue film tape according to claim 6, wherein the temperature of the reaction in step b) is 78-82 ℃ and the reaction time is 0.5-1.5h.
11. The cell blue film tape according to claim 6, wherein the partial initiator in step c) is 1/4 of the total initiator.
12. The cell blue film tape according to claim 6, wherein the temperature of the reaction in step c) is 80-82 ℃ and the reaction time is 0.5-1.5h.
13. The cell blue film tape according to claim 6, wherein the temperature of the reaction in step d) is 80-82 ℃ and the reaction time is 1.5-2h.
14. The cell blue film tape according to claim 6, wherein the temperature of the reaction in step e) is 82-84 ℃ and the reaction time is 1.5-2h.
15. The cell blue film tape according to claim 6, wherein the cooling in step f) is to 50-55 ℃.
16. The cell blue film tape according to claim 1, wherein the first substrate layer and the second substrate layer are both comprised of polyethylene terephthalate.
17. The cell blue film tape according to claim 1, wherein the first and second acrylic pressure sensitive adhesive layers are prepared from materials further comprising a solvent.
18. The cell blue film tape according to claim 17, wherein said solvent comprises ethyl acetate.
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| CN115160960A (en) * | 2022-08-08 | 2022-10-11 | 苏州赛伍应用技术股份有限公司 | High-solid low-viscosity acrylic polymer and preparation method and application thereof |
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| CN103952105A (en) * | 2014-03-28 | 2014-07-30 | 广东达美新材料有限公司 | Fluorosilicone modified aqueous pressure-sensitive adhesive used for polyethylene protection film, and preparation method thereof |
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