CN113429907A - Preparation method of high-temperature-resistant low-transfer protective film - Google Patents
Preparation method of high-temperature-resistant low-transfer protective film Download PDFInfo
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- CN113429907A CN113429907A CN202110849158.6A CN202110849158A CN113429907A CN 113429907 A CN113429907 A CN 113429907A CN 202110849158 A CN202110849158 A CN 202110849158A CN 113429907 A CN113429907 A CN 113429907A
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- 230000001681 protective effect Effects 0.000 title claims abstract description 75
- 238000012546 transfer Methods 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000003522 acrylic cement Substances 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000178 monomer Substances 0.000 claims abstract description 16
- 239000000853 adhesive Substances 0.000 claims abstract description 15
- 230000001070 adhesive effect Effects 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 15
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 238000003851 corona treatment Methods 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000005096 rolling process Methods 0.000 claims abstract description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 60
- 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 22
- 238000000034 method Methods 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 239000012752 auxiliary agent Substances 0.000 claims description 13
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 239000004593 Epoxy Substances 0.000 claims description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 8
- 239000011737 fluorine Substances 0.000 claims description 8
- 229910052731 fluorine Inorganic materials 0.000 claims description 8
- 239000012948 isocyanate Substances 0.000 claims description 8
- 150000002513 isocyanates Chemical class 0.000 claims description 8
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 4
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- VHSHLMUCYSAUQU-UHFFFAOYSA-N 2-hydroxypropyl methacrylate Chemical compound CC(O)COC(=O)C(C)=C VHSHLMUCYSAUQU-UHFFFAOYSA-N 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 3
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 3
- LNMQRPPRQDGUDR-UHFFFAOYSA-N hexyl prop-2-enoate Chemical compound CCCCCCOC(=O)C=C LNMQRPPRQDGUDR-UHFFFAOYSA-N 0.000 claims description 3
- FZSHSWCZYDDOCK-UHFFFAOYSA-N 2-methylprop-2-enoic acid;oxolane Chemical compound C1CCOC1.CC(=C)C(O)=O FZSHSWCZYDDOCK-UHFFFAOYSA-N 0.000 claims description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 2
- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 claims description 2
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 2
- 229940119545 isobornyl methacrylate Drugs 0.000 claims description 2
- 230000009194 climbing Effects 0.000 description 18
- 239000011521 glass Substances 0.000 description 11
- 239000003292 glue Substances 0.000 description 8
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1806—C6-(meth)acrylate, e.g. (cyclo)hexyl (meth)acrylate or phenyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1812—C12-(meth)acrylate, e.g. lauryl (meth)acrylate
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/064—Copolymers with monomers not covered by C09J133/06 containing anhydride, COOH or COOM groups, with M being metal or onium-cation
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/24—Homopolymers or copolymers of amides or imides
- C09J133/26—Homopolymers or copolymers of acrylamide or methacrylamide
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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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a preparation method of a high-temperature-resistant low-transfer protective film, which comprises the following steps: 2-5 parts of soft monomer, 1-3 parts of hard monomer, 0.5-2 parts of functional monomer and 3-7 parts of solvent B are added into a reaction kettle by weight, stirred at the temperature of 63-64 ℃ and introduced with nitrogen; adding 0.015-0.03 part by weight of initiator, and reacting for 8-12 hours at constant temperature; adding 0.015-0.03 part by weight of initiator, heating to 65 ℃, and reacting at constant temperature for 6-8 hours; cooling to 50 ℃, and adding 1-4 parts by weight of solvent B to obtain the acrylic adhesive; performing corona treatment on the surface of a base material, and coating 100 parts by weight of acrylic acid adhesive, 1-50 parts by weight of assistant and 100-78 parts by weight of solvent A10; feeding the coated substrate into a continuous oven for baking, attaching a low-silicon release film, and rolling to obtain a pre-cured protective film; and curing the pre-cured protective film to obtain the high-temperature-resistant low-transfer protective film.
Description
Technical Field
The invention belongs to the field of protective films, and particularly relates to a preparation method of a high-temperature-resistant low-transfer protective film.
Background
Along with the change of science and technology, the living standard of people is continuously improved, the use of electronic products such as mobile phones, tablet computers, personal computers and the like is quite popular, the electronic equipment products need different protective films to carry out requirements such as protection and shielding in the preparation process, and the requirements for process protective films are higher and higher along with the thinning of the electronic equipment, such as high-temperature resistant protective films and the like which need shielding in the glass silk-screen process.
However, the existing high temperature resistant protective films on the market have different degrees of defects, such as high temperature resistance which is not satisfactory, and more transferred substances after high temperature use which can not meet the customer requirements, so that it is necessary to develop a protective film which meets the high temperature resistance and is low in precipitation.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a high-temperature-resistant low-transfer protective film, which solves the problems that the surface of glass has residual glue and wire frame prints after high-temperature conditions, the protective film has larger climbing after high-temperature processing and the like in the prior art.
In order to solve the problems of the prior art, the invention adopts the technical scheme that:
the invention provides a preparation method of a high-temperature-resistant low-transfer protective film, which comprises the following steps:
performing corona treatment on the surface of a base material, and coating 100 parts by weight of acrylic acid adhesive, 1-50 parts by weight of auxiliary agent and 100-78 parts by weight of solvent A10 to obtain a coated base material;
feeding the coated substrate into a continuous oven for baking, attaching a low-silicon release film, and rolling to obtain a pre-cured protective film;
curing the pre-cured protective film to obtain a high-temperature-resistant low-transfer protective film;
the acrylic adhesive is prepared by the following method:
2-5 parts of soft monomer, 1-3 parts of hard monomer, 0.5-2 parts of functional monomer and 3-7 parts of solvent B are added into a reaction kettle by weight, stirred at the temperature of 63-64 ℃ and introduced with nitrogen;
adding 0.015-0.03 part by weight of initiator, and reacting for 8-12 hours at constant temperature;
adding 0.015-0.03 part by weight of initiator, heating to 65 ℃, and reacting at constant temperature for 6-8 hours;
and cooling to 50 ℃, and adding 1-4 parts by weight of solvent B to obtain the acrylic adhesive.
Further, the soft monomer is one or more of butyl acrylate, isooctyl acrylate, n-hexyl acrylate and lauryl methacrylate.
Further, the hard monomer is one or more of methyl acrylate, methyl methacrylate, ethyl methacrylate, isobornyl methacrylate, tetrahydrofuran methacrylate, glycidyl methacrylate and vinyl acetate.
Further, the functional monomer is one or more of hydroxyethyl acrylate, acrylic acid, methacrylic acid, beta-hydroxypropyl methacrylate and acrylamide.
Further, the solvent A is ethyl acetate, and the solvent B is one or more of ethyl acetate and toluene; the initiator is one or more of azodiisobutyronitrile and benzoyl peroxide.
Further, the molecular weight of the acrylic adhesive is 100-.
Furthermore, the auxiliary agent is one or more of isocyanate curing agent, epoxy curing agent and fluorine-containing auxiliary agent.
Further, the base material is one of PET and PI, and the thickness of the base material is 6-200 μm.
Further, when the substrate is sent into a continuous oven for baking, the transmission speed is 10-50m/min, and the temperature of 8 sections of oven is set to be 40-60 ℃/90-100 ℃/90-100 ℃/100-.
Furthermore, the curing temperature is set to be 50-55 ℃, and the curing time is set to be 48-72 hours.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the high-temperature-resistant low-transfer protective film provided by the invention adopts the prepared acrylic adhesive as the pressure-sensitive adhesive, the hard monomer is added in the preparation of the acrylic adhesive, the molecular weight of the prepared acrylic adhesive is 200 thousands in 100-;
by the preparation method of the acrylic adhesive and the control of the process flow, the prepared acrylic adhesive has narrow molecular weight distribution and less tailing in the molecular weight distribution, and is matched with the adjustment of an auxiliary agent in the preparation process of a protective film, so that the finally prepared protective film has good adhesive residue performance, and the surface of glass has no adhesive residue after high temperature; on the basis of no residual adhesive, the molecular weight of the acrylic adhesive prepared by the invention is 200 ten thousand, the cohesive force is higher, the wire frame printing has no residue, and the climbing of the finally prepared protective film is lower.
Detailed Description
The invention is further described below. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The high-temperature-resistant low-transfer protective film prepared by the preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention needs to be subjected to a high-temperature performance test, and test items comprise adhesive residue performance, wire frame printing performance and climbing performance.
The specific test method for the residual adhesive performance is as follows: cutting a heat-resistant low-transfer protective film with a proper size to stick to a plain surface of glass (the glass is not subjected to any treatment such AS AR or AS), rolling 2kg of roller back and forth for 2 times, then putting the roller into an oven with a set temperature of 200 ℃, baking for 3min, taking out and cooling, then rolling 2kg of roller back and forth for 2 times, repeating the process for 5 times, then putting the roller into the oven with a set temperature of 200 ℃, baking for 35min, taking out and cooling for 30min, and observing whether punctiform residual glue exists on the surface of the glass by using a strong-light flashlight; the residual adhesive performance is not OK if there is a spot residual adhesive, and is OK if there is no spot residual adhesive.
The specific test method for the wire frame printing performance comprises the following steps: cutting a high-temperature-resistant low-transfer protective film with a proper size to be pasted with a plain surface of glass (the glass is not subjected to any treatment such AS AR or AS), rolling 2kg of roller back and forth for 2 times, then putting the roller into an oven with a set temperature of 200 ℃, baking for 3min, taking out and cooling, then rolling 2kg of roller back and forth for 2 times, repeating the process for 5 times, then putting the roller into the oven with a set temperature of 200 ℃, baking for 35min, taking out and cooling for 30min, and observing whether the periphery of the glass has a residual rubber frame which is difficult to wipe by using a strong-light flashlight; the wire frame print performance is not OK if there is a residual rubber frame that is not easily wiped, and is OK if there is no residual rubber frame that is not easily wiped.
The specific test method of climbing performance is as follows: cutting 25.4mm high temperature resistant low transfer protective film and pasting a plain surface of the glass (the glass is not processed, such AS AR or AS), rolling and pressing 2kg of roller back and forth for 2 times, then putting the roller into an oven with the set temperature of 200 ℃, baking for 3min, taking out and cooling, then rolling and pressing 2kg of roller back and forth for 2 times, repeating the process for 5 times, then putting the roller into the oven with the set temperature of 200 ℃, baking for 35min, taking out and cooling for 30min, testing the viscosity at constant temperature, climbing up when the adhesive force is greater than 50gf/in, and climbing down when the adhesive force is less than 50 gf/in.
Example 1
The preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention comprises the step of firstly preparing the acrylic adhesive.
Adding 2 parts by weight of isooctyl acrylate, 3 parts by weight of methyl methacrylate, 2 parts by weight of acrylic acid and 7 parts by weight of ethyl acetate into a reaction kettle, introducing nitrogen for a period of time at the temperature of 63-64 ℃, adding 0.03 part by weight of azobisisobutyronitrile, and keeping the temperature for reacting for 8-12 hours; adding 0.03 part by weight of azobisisobutyronitrile, raising the temperature to 65 ℃, and reacting for 6-8 hours; and cooling to 50 ℃ and adding 4 parts by weight of ethyl acetate to obtain the high-temperature-resistant acrylate pressure-sensitive adhesive.
Selecting PET as a base material, wherein the thickness of the base material is 6 microns, carrying out corona treatment on the surface of the base material, and coating 100 parts by weight of acrylic acid adhesive, 1 part by weight of isocyanate curing agent, 30 parts by weight of epoxy curing agent, 3 parts by weight of fluorine-containing auxiliary agent and 30 parts by weight of ethyl acetate to obtain the coated base material; feeding the coated substrate into a continuous oven for baking, wherein the conveying speed is 10-50m/min when the substrate is fed into the continuous oven for baking, the temperature of 8 sections of the oven is sequentially set to be 40-60 ℃/90-100 ℃/90-100 ℃/100 plus-material 120 ℃/90-100 ℃/60-80 ℃, the low-silicon release film is attached after baking is finished, and the low-silicon release film is rolled to obtain a pre-cured protective film; curing the pre-cured protective film for 48-72 hours at 50-55 ℃ to obtain the high-temperature resistant low-transfer protective film.
The high-temperature-resistant low-transfer protective film prepared by the preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention has the advantages that the residual glue performance is OK, the wire frame printing performance is OK, the climbing is 30gf/in, and the climbing is low; has the advantages of high temperature resistance and low transfer.
Example 2
The preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention comprises the step of firstly preparing the acrylic adhesive.
Putting 5 parts by weight of n-hexyl acrylate, 1 part by weight of ethyl methacrylate, 0.5 part by weight of methacrylic acid and 3 parts by weight of toluene into a reaction kettle, introducing nitrogen for a period of time under the stirring condition of 63-64 ℃, adding 0.015 part by weight of benzoyl peroxide, and keeping the temperature for reacting for 8-12 hours; adding 0.015 part of benzoyl peroxide by weight, raising the temperature to 65 ℃, and reacting for 6-8 hours; and cooling to 50 ℃ and adding 1 part by weight of toluene to obtain the high-temperature-resistant acrylate pressure-sensitive adhesive.
Selecting PI as a base material, wherein the thickness of the base material is 100 micrometers, carrying out corona treatment on the surface of the base material, and coating 100 parts by weight of acrylic acid adhesive, 1 part by weight of isocyanate curing agent, 40 parts by weight of epoxy curing agent, 3 parts by weight of fluorine-containing auxiliary agent and 30 parts by weight of ethyl acetate to obtain the coated base material; feeding the coated substrate into a continuous oven for baking, wherein the conveying speed is 10-50m/min when the substrate is fed into the continuous oven for baking, the temperature of 8 sections of the oven is sequentially set to be 40-60 ℃/90-100 ℃/90-100 ℃/100 plus-material 120 ℃/90-100 ℃/60-80 ℃, the low-silicon release film is attached after baking is finished, and the low-silicon release film is rolled to obtain a pre-cured protective film; curing the pre-cured protective film for 48-72 hours at 50-55 ℃ to obtain the high-temperature resistant low-transfer protective film.
The high-temperature-resistant low-transfer protective film prepared by the preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention has the advantages that the residual glue performance is OK, the wire frame printing performance is OK, the climbing is 30gf/in, and the climbing is low; has the advantages of high temperature resistance and low transfer.
Example 3
The preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention comprises the step of firstly preparing the acrylic adhesive.
Adding 3 parts by weight of butyl acrylate, 2 parts by weight of methyl acrylate, 1 part by weight of hydroxyethyl acrylate and 5 parts by weight of ethyl acetate into a reaction kettle, introducing nitrogen for a period of time at the temperature of 63-64 ℃, adding 0.02 part by weight of azobisisobutyronitrile, and keeping the temperature for reacting for 8-12 hours; adding 0.02 part by weight of azobisisobutyronitrile, raising the temperature to 65 ℃, and reacting for 6-8 hours; and cooling to 50 ℃ and adding 3 parts by weight of ethyl acetate to obtain the high-temperature-resistant acrylate pressure-sensitive adhesive.
Selecting PET as a base material, wherein the thickness of the base material is 30 micrometers, carrying out corona treatment on the surface of the base material, and coating 100 parts by weight of acrylic adhesive, 1.5 parts by weight of isocyanate curing agent, 40 parts by weight of epoxy curing agent, 3 parts by weight of fluorine-containing auxiliary agent and 30 parts by weight of ethyl acetate to obtain the coated base material; feeding the coated substrate into a continuous oven for baking, wherein the conveying speed is 10-50m/min when the substrate is fed into the continuous oven for baking, the temperature of 8 sections of the oven is sequentially set to be 40-60 ℃/90-100 ℃/90-100 ℃/100 plus-material 120 ℃/90-100 ℃/60-80 ℃, the low-silicon release film is attached after baking is finished, and the low-silicon release film is rolled to obtain a pre-cured protective film; curing the pre-cured protective film for 48-72 hours at 50-55 ℃ to obtain the high-temperature resistant low-transfer protective film.
The high-temperature-resistant low-transfer protective film prepared by the preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention has the advantages that the residual glue performance is OK, the wire frame printing performance is OK, the climbing is 25gf/in, and the climbing is low; has the advantages of high temperature resistance and low transfer.
Example 4
The preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention comprises the step of firstly preparing the acrylic adhesive.
Adding 4 parts by weight of butyl acrylate, 2 parts by weight of methyl acrylate, 1.5 parts by weight of beta-hydroxypropyl methacrylate and 6 parts by weight of ethyl acetate into a reaction kettle, introducing nitrogen for a period of time under the stirring condition of 63-64 ℃, adding 0.025 part by weight of azobisisobutyronitrile, and keeping the temperature for reacting for 8-12 hours; adding 0.025 parts by weight of azobisisobutyronitrile, raising the temperature to 65 ℃, and reacting for 6-8 hours; and cooling to 50 ℃ and adding 2 parts by weight of ethyl acetate to obtain the high-temperature-resistant acrylate pressure-sensitive adhesive.
Selecting PI as a base material, wherein the thickness of the base material is 60 micrometers, carrying out corona treatment on the surface of the base material, and coating 100 parts by weight of acrylic adhesive, 1 part by weight of isocyanate curing agent, 40 parts by weight of epoxy curing agent, 5 parts by weight of fluorine-containing auxiliary agent and 30 parts by weight of ethyl acetate to obtain the coated base material; feeding the coated substrate into a continuous oven for baking, wherein the conveying speed is 10-50m/min when the substrate is fed into the continuous oven for baking, the temperature of 8 sections of the oven is sequentially set to be 40-60 ℃/90-100 ℃/90-100 ℃/100 plus-material 120 ℃/90-100 ℃/60-80 ℃, the low-silicon release film is attached after baking is finished, and the low-silicon release film is rolled to obtain a pre-cured protective film; curing the pre-cured protective film for 48-72 hours at 50-55 ℃ to obtain the high-temperature resistant low-transfer protective film.
The high-temperature-resistant low-transfer protective film prepared by the preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention has the advantages that the residual glue performance is OK, the wire frame printing performance is OK, the climbing is 25gf/in, and the climbing is low; has the advantages of high temperature resistance and low transfer.
Example 5
The preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention comprises the step of firstly preparing the acrylic adhesive.
Adding 3 parts by weight of lauryl methacrylate, 2 parts by weight of methyl acrylate, 1 part by weight of hydroxyethyl acrylate and 5 parts by weight of ethyl acetate into a reaction kettle, introducing nitrogen for a period of time at the temperature of 63-64 ℃, adding 0.02 part by weight of azobisisobutyronitrile, and keeping the temperature to react for 8-12 hours; adding 0.02 part by weight of azobisisobutyronitrile, raising the temperature to 65 ℃, and reacting for 6-8 hours; and cooling to 50 ℃ and adding 3 parts by weight of ethyl acetate to obtain the high-temperature-resistant acrylate pressure-sensitive adhesive.
Selecting PET as a base material, wherein the thickness of the base material is 6 microns, carrying out corona treatment on the surface of the base material, and coating 100 parts by weight of acrylic adhesive, 1 part by weight of isocyanate curing agent, 44 parts by weight of epoxy curing agent, 5 parts by weight of fluorine-containing auxiliary agent and 100 parts by weight of ethyl acetate to obtain the coated base material; feeding the coated substrate into a continuous oven for baking, wherein the conveying speed is 10-50m/min when the substrate is fed into the continuous oven for baking, the temperature of 8 sections of the oven is sequentially set to be 40-60 ℃/90-100 ℃/90-100 ℃/100 plus-material 120 ℃/90-100 ℃/60-80 ℃, the low-silicon release film is attached after baking is finished, and the low-silicon release film is rolled to obtain a pre-cured protective film; curing the pre-cured protective film for 48-72 hours at 50-55 ℃ to obtain the high-temperature resistant low-transfer protective film.
The high-temperature-resistant low-transfer protective film prepared by the preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention has the advantages that the residual glue performance is OK, the wire frame printing performance is OK, the climbing is 26gf/in, and the climbing is low; has the advantages of high temperature resistance and low transfer.
Example 6
The preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention comprises the step of firstly preparing the acrylic adhesive.
Putting 4 parts by weight of isooctyl acrylate, 2 parts by weight of methyl acrylate, 1.5 parts by weight of acrylamide and 6 parts by weight of ethyl acetate into a reaction kettle, introducing nitrogen for a period of time under the stirring condition of 63-64 ℃, adding 0.025 part by weight of azobisisobutyronitrile, and keeping the temperature for reacting for 8-12 hours; adding 0.025 parts by weight of azobisisobutyronitrile, raising the temperature to 65 ℃, and reacting for 6-8 hours; and cooling to 50 ℃ and adding 2 parts by weight of ethyl acetate to obtain the high-temperature-resistant acrylate pressure-sensitive adhesive.
Selecting PI as a base material, wherein the thickness of the base material is 60 micrometers, carrying out corona treatment on the surface of the base material, and coating 100 parts by weight of acrylic adhesive, 0.4 part by weight of isocyanate curing agent, 0.4 part by weight of epoxy curing agent, 0.2 part by weight of fluorine-containing auxiliary agent and 10 parts by weight of ethyl acetate to obtain the coated base material; feeding the coated substrate into a continuous oven for baking, wherein the conveying speed is 10-50m/min when the substrate is fed into the continuous oven for baking, the temperature of 8 sections of the oven is sequentially set to be 40-60 ℃/90-100 ℃/90-100 ℃/100 plus-material 120 ℃/90-100 ℃/60-80 ℃, the low-silicon release film is attached after baking is finished, and the low-silicon release film is rolled to obtain a pre-cured protective film; curing the pre-cured protective film for 48-72 hours at 50-55 ℃ to obtain the high-temperature resistant low-transfer protective film.
The high-temperature-resistant low-transfer protective film prepared by the preparation method of the high-temperature-resistant low-transfer protective film provided by the embodiment of the invention has the advantages that the residual glue performance is OK, the wire frame printing performance is OK, the climbing is 25gf/in, and the climbing is low; has the advantages of high temperature resistance and low transfer.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the high-temperature-resistant low-transfer protective film is characterized by comprising the following steps of:
performing corona treatment on the surface of a base material, and coating 100 parts by weight of acrylic acid adhesive, 1-50 parts by weight of auxiliary agent and 100-78 parts by weight of solvent A10 to obtain a coated base material;
feeding the coated substrate into a continuous oven for baking, attaching a low-silicon release film, and rolling to obtain a pre-cured protective film;
curing the pre-cured protective film to obtain a high-temperature-resistant low-transfer protective film;
the acrylic adhesive is prepared by the following method:
2-5 parts of soft monomer, 1-3 parts of hard monomer, 0.5-2 parts of functional monomer and 3-7 parts of solvent B are added into a reaction kettle by weight, stirred at the temperature of 63-64 ℃ and introduced with nitrogen;
adding 0.015-0.03 part by weight of initiator, and reacting for 8-12 hours at constant temperature;
adding 0.015-0.03 part by weight of initiator, heating to 65 ℃, and reacting at constant temperature for 6-8 hours;
and cooling to 50 ℃, and adding 1-4 parts by weight of solvent B to obtain the acrylic adhesive.
2. The method for preparing a high temperature resistant low-transfer protective film according to claim 1, wherein the soft monomer is one or more of butyl acrylate, isooctyl acrylate, n-hexyl acrylate and lauryl methacrylate.
3. The method for preparing a high temperature resistant low-transfer protective film according to claim 1, wherein the hard monomer is one or more of methyl acrylate, methyl methacrylate, ethyl methacrylate, isobornyl methacrylate, tetrahydrofuran methacrylate, glycidyl methacrylate and vinyl acetate.
4. The method for preparing a high temperature resistant low-transfer protective film according to claim 1, wherein the functional monomer is one or more of hydroxyethyl acrylate, acrylic acid, methacrylic acid, beta-hydroxypropyl methacrylate, and acrylamide.
5. The method for preparing a high temperature resistant low-transfer protective film according to claim 1, wherein the solvent A is ethyl acetate, and the solvent B is one or more of ethyl acetate and toluene; the initiator is one or more of azodiisobutyronitrile and benzoyl peroxide.
6. The method as claimed in claim 1, wherein the molecular weight of the acrylic adhesive is 100-200 ten thousand.
7. The method for preparing a high temperature resistant low-transfer protective film according to claim 1, wherein the auxiliary agent is one or more of an isocyanate curing agent, an epoxy curing agent and a fluorine-containing auxiliary agent.
8. The method for preparing the high temperature resistant low-transfer protective film according to claim 1, wherein the substrate is one of PET and PI, and the thickness of the substrate is 6-200 μm.
9. The method as claimed in claim 1, wherein the substrate is transported at a speed of 10-50m/min when being baked in a continuous oven, and the temperature of the 8-section oven is set to 40-60 ℃/90-100 ℃/90-100 ℃/100-.
10. The method for preparing a high temperature resistant low-transfer protective film according to claim 1, wherein the curing temperature is set to 50-55 ℃ and the curing time is 48-72 hours.
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| CN116589941A (en) * | 2023-01-06 | 2023-08-15 | 江苏荣骐光电材料科技有限公司 | Preparation method of special low-viscosity protective film for high Wen Ruanbao-resistant lithium battery |
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| CN110628363A (en) * | 2019-09-29 | 2019-12-31 | 新纶科技（常州）有限公司 | Preparation method of adhesive and preparation method of adhesive tape |
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