CN113817419A - Protective film for glass PVD (physical vapor deposition) process and preparation method thereof - Google Patents
Protective film for glass PVD (physical vapor deposition) process and preparation method thereof Download PDFInfo
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- CN113817419A CN113817419A CN202111312792.2A CN202111312792A CN113817419A CN 113817419 A CN113817419 A CN 113817419A CN 202111312792 A CN202111312792 A CN 202111312792A CN 113817419 A CN113817419 A CN 113817419A
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- Prior art keywords
- film
- glass
- protective film
- layer
- release
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- 239000011521 glass Substances 0.000 title claims abstract description 79
- 230000001681 protective effect Effects 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005240 physical vapour deposition Methods 0.000 title abstract description 56
- 239000010410 layer Substances 0.000 claims abstract description 87
- 239000012790 adhesive layer Substances 0.000 claims abstract description 52
- 239000004800 polyvinyl chloride Substances 0.000 claims abstract description 32
- 229920000915 polyvinyl chloride Polymers 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 229920006346 thermoplastic polyester elastomer Polymers 0.000 claims abstract description 10
- 229920006284 nylon film Polymers 0.000 claims abstract 2
- 239000003795 chemical substances by application Substances 0.000 claims description 46
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 36
- 239000003292 glue Substances 0.000 claims description 29
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 28
- 239000011259 mixed solution Substances 0.000 claims description 26
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 22
- 239000004014 plasticizer Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 14
- 239000010703 silicon Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 238000013329 compounding Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 238000005096 rolling process Methods 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 238000002834 transmittance Methods 0.000 claims description 12
- 239000002216 antistatic agent Substances 0.000 claims description 7
- 239000004593 Epoxy Substances 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 5
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims description 4
- 239000002608 ionic liquid Substances 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 229920000768 polyamine Polymers 0.000 claims description 4
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 3
- KNDQHSIWLOJIGP-UMRXKNAASA-N (3ar,4s,7r,7as)-rel-3a,4,7,7a-tetrahydro-4,7-methanoisobenzofuran-1,3-dione Chemical compound O=C1OC(=O)[C@@H]2[C@H]1[C@]1([H])C=C[C@@]2([H])C1 KNDQHSIWLOJIGP-UMRXKNAASA-N 0.000 claims description 2
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 claims description 2
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 2
- CFEKOKRYQRODRZ-UHFFFAOYSA-N 2-cyclohexylethane-1,1-diamine Chemical compound NC(N)CC1CCCCC1 CFEKOKRYQRODRZ-UHFFFAOYSA-N 0.000 claims description 2
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 claims description 2
- 150000008065 acid anhydrides Chemical class 0.000 claims description 2
- 125000002723 alicyclic group Chemical group 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 150000004982 aromatic amines Chemical class 0.000 claims description 2
- YMHQVDAATAEZLO-UHFFFAOYSA-N cyclohexane-1,1-diamine Chemical compound NC1(N)CCCCC1 YMHQVDAATAEZLO-UHFFFAOYSA-N 0.000 claims description 2
- OYOFUEDXAMRQBB-UHFFFAOYSA-N cyclohexylmethanediamine Chemical compound NC(N)C1CCCCC1 OYOFUEDXAMRQBB-UHFFFAOYSA-N 0.000 claims description 2
- IUNMPGNGSSIWFP-UHFFFAOYSA-N dimethylaminopropylamine Chemical compound CN(C)CCCN IUNMPGNGSSIWFP-UHFFFAOYSA-N 0.000 claims description 2
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 claims description 2
- GKQPCPXONLDCMU-CCEZHUSRSA-N lacidipine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C1=CC=CC=C1\C=C\C(=O)OC(C)(C)C GKQPCPXONLDCMU-CCEZHUSRSA-N 0.000 claims description 2
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 2
- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 9
- 230000009194 climbing Effects 0.000 abstract description 6
- 239000012528 membrane Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- ZNJRWJSLGMRLAZ-UHFFFAOYSA-N C1(CCC(N1)=O)=O.[Li].FC(F)F.FC(F)F Chemical group C1(CCC(N1)=O)=O.[Li].FC(F)F.FC(F)F ZNJRWJSLGMRLAZ-UHFFFAOYSA-N 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 3
- 239000003522 acrylic cement Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- KFYRJJBUHYILSO-YFKPBYRVSA-N (2s)-2-amino-3-dimethylarsanylsulfanyl-3-methylbutanoic acid Chemical compound C[As](C)SC(C)(C)[C@@H](N)C(O)=O KFYRJJBUHYILSO-YFKPBYRVSA-N 0.000 description 1
- KNLXUOXPWXEJME-GVXVVHGQSA-N (2s,4as,8ar)-1,1,4a-trimethyl-2,3,4,5,6,7,8,8a-octahydronaphthalen-2-ol Chemical compound C1CCC[C@H]2C(C)(C)[C@@H](O)CC[C@@]21C KNLXUOXPWXEJME-GVXVVHGQSA-N 0.000 description 1
- GTACSIONMHMRPD-UHFFFAOYSA-N 2-[4-[2-(benzenesulfonamido)ethylsulfanyl]-2,6-difluorophenoxy]acetamide Chemical compound C1=C(F)C(OCC(=O)N)=C(F)C=C1SCCNS(=O)(=O)C1=CC=CC=C1 GTACSIONMHMRPD-UHFFFAOYSA-N 0.000 description 1
- WYMDDFRYORANCC-UHFFFAOYSA-N 2-[[3-[bis(carboxymethyl)amino]-2-hydroxypropyl]-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)CN(CC(O)=O)CC(O)=O WYMDDFRYORANCC-UHFFFAOYSA-N 0.000 description 1
- VQVIHDPBMFABCQ-UHFFFAOYSA-N 5-(1,3-dioxo-2-benzofuran-5-carbonyl)-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(C(C=2C=C3C(=O)OC(=O)C3=CC=2)=O)=C1 VQVIHDPBMFABCQ-UHFFFAOYSA-N 0.000 description 1
- 101710130081 Aspergillopepsin-1 Proteins 0.000 description 1
- 102100031007 Cytosolic non-specific dipeptidase Human genes 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- -1 m-aminomethane Chemical compound 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- 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
- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
- C09J133/12—Homopolymers or copolymers of methyl methacrylate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/24—Plastics; Metallised plastics based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/241—Polyolefin, e.g.rubber
- C09J7/243—Ethylene or propylene polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—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
-
- 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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
-
- 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
- C09J2427/00—Presence of halogenated polymer
- C09J2427/006—Presence of halogenated polymer in the substrate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2477/00—Presence of polyamide
- C09J2477/006—Presence of polyamide in the substrate
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Laminated Bodies (AREA)
Abstract
The invention provides a protective film for a glass PVD (physical vapor deposition) process and a preparation method thereof, wherein the protective film sequentially comprises a base material layer, an adhesive layer and a release film layer from top to bottom; the material of the substrate layer is a flexible film; the flexible film includes any one of a polyvinyl chloride film, a nylon film, or a thermoplastic polyester elastomer film. The protective film disclosed by the invention has good heat resistance and acid resistance, is small in viscosity climbing after a high-temperature process, is easy to strip, is not layered in the high-temperature process, has no upwarp at the edge, can effectively protect glass, prevents acid liquor from permeating, prevents the glass from being scratched or polluted, and can be applied to a PVD (physical vapor deposition) process of curved glass.
Description
Technical Field
The invention belongs to the technical field of acrylic protective films, and relates to a protective film for a glass PVD (physical vapor deposition) process and a preparation method thereof.
Background
The non-plating surface needs to be protected in the glass PVD (physical vapor deposition) process, the high-temperature baking is carried out for 1h at the temperature of 180-190 ℃ in the process, the material is required to be soft, no adhesive residue exists after high-temperature evaporation, the material and the glass are not separated, the glass cannot be corroded by acid liquor, and the glass can be effectively protected. After cooling at high temperature, the glass is easy to separate from the surface of the glass. The protective film in the prior art is usually an acrylic protective film or a PU protective film which takes PET, PE and the like as base materials, however, the PET base material has poor flexibility and high stiffness, and the edge of glass can not be effectively protected because the PET base material and a curved surface are easy to warp at high temperature; the PE base material has poor high temperature resistance, and the base material is easy to melt and adhere to the surface of glass when being placed in an oven in an overlapping way. Meanwhile, the traditional acrylic protective film is poor in scratch resistance, easy to powder and not beneficial to die cutting processing. The silica gel protective film has a large amount of silicon transfer and can contaminate the PVD glass.
CN212532828U discloses a special protection film of optical glass coating, release the type membrane including low PET membrane, viscose layer and PET: PET has the viscose layer from the surface coating of type membrane, low appear PET membrane with PET has the laminating of the one side on viscose layer from the type membrane coating, and this utility model's beneficial effect lies in: through special development of the film material and the acrylic adhesive and strict selection of the release film, the high-temperature-resistant acrylic adhesive has excellent temperature resistance, no precipitate after high temperature, no pollution and good die cutting performance. However, the utility model uses the PET substrate, and its flexibility is poor, the deflection is high, under the high temperature condition and between the curved surface easy appear the phenomenon of upwarping, can't effectively protect the glass edge.
Therefore, in the field, it is desired to develop a protective film which has good heat resistance and acid resistance, has small viscosity climbing after a high-temperature process, is easy to peel off, has no edge lifting in the high-temperature process, can effectively protect glass, and can prevent the glass from being scratched or polluted, so as to be used for a glass PVD process.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a protective film for a glass PVD process and a preparation method thereof. The protective film disclosed by the invention has good heat resistance and acid resistance, is small in viscosity climbing after a high-temperature process, is easy to strip, is not layered in the high-temperature process, has no upwarp at the edge, can effectively protect glass, prevents acid liquor from permeating, prevents the glass from being scratched or polluted, and can be applied to a PVD (physical vapor deposition) process of curved glass. In addition, the acrylic adhesive is low in high-temperature viscosity climbing, easy to tear off after high temperature, free of organic silicon and excellent in ring testing resistance.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a protective film for a glass PVD (physical vapor deposition) process, which comprises a base material layer, an adhesive layer and a release film layer from top to bottom in sequence;
the material of the substrate layer is a flexible film;
the flexible film includes any one of a polyvinyl chloride (PVC) film, a nylon (PA) film, or a thermoplastic polyester elastomer (TPEE) film.
In the invention, flexible films such as a PVC film, a PA film, a TPEE film and the like are used as substrate layers of the protective film, the substrate is softer in the high-temperature process, is tightly attached to an attached object and does not warp, and the surface of glass can be better protected, so that the glass is not corroded in the pickling and washing process.
Preferably, the flexible film has a thickness of 10-150 μm, such as 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, 110 μm, 120 μm, 130 μm, 140 μm, 150 μm, or the like.
Preferably, the PVC film has a plasticizer content of 16% to 30%, such as 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, or 30%, and the like.
As the preferred technical scheme, when the plasticizer content of the PVC film is within the range of 16-30%, the PVC film is soft, good attachment to the curved screen can be achieved, delamination does not occur in the high-temperature process, the edge does not warp, glass can be effectively protected, and acid liquor permeation is prevented. If the plasticizer content of the PVC film is higher than 30%, precipitation may occur during a high temperature process.
Preferably, the flexible film has a light transmittance of > 80%, e.g., 81%, 83%, 85%, 89%, 90%, 92%, or 95%, etc., and the flexible film has a haze of < 60%, e.g., 55%, 50%, or 45%, etc.
Preferably, the heat shrinkage rate of the flexible film in the MD direction and the TD direction is less than 3% under the condition of 150 ℃ and 20 min.
Preferably, the adhesive layer comprises the following raw materials in parts by weight:
according to the invention, the acrylic glue is matched with the PA film, the TPEE film or the PVC film with low plasticizer content and the like, the viscosity of the glue layer is stable, so that the glue layer and the curved screen can be firmly jointed, the base material is soft in the high-temperature process, the thermal shrinkage rate is low, the glue layer is tightly jointed with an adherend and does not warp, the glass surface can be well protected, and the glass surface is not corroded in the pickling and washing process.
In the preparation raw materials of the adhesive layer, the dosage of the curing agent can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts or 8 parts and the like.
In the raw materials for preparing the adhesive layer, the antistatic agent can be used in an amount of 0 part, 0.2 part, 0.5 part, 0.7 part, 0.9 part or 1 part.
In the preparation raw materials of the adhesive layer, the amount of the leveling agent can be 0.1 part, 0.3 part, 0.5 part, 0.7 part, 1 part, 1.2 parts, 1.3 parts or 1.5 parts, etc.
Preferably, the number average molecular weight of the acrylic glue is 200000-700000, such as 200000, 300000, 400000, 500000, 600000 or 700000.
As the preferable technical scheme of the invention, the glue with relatively large molecular weight (200000-.
Preferably, the hydroxyl value of the acrylic glue is 34-88mgKOH/g, such as 34mgKOH/g, 40mgKOH/g, 50mgKOH/g, 60mgKOH/g, 70mgKOH/g, 80mgKOH/g, 88mgKOH/g, and the like.
Preferably, the viscosity of the acrylic glue at 23 + -2 ℃ is 17000 + -7000 cps, such as 10000cps, 12000cps, 15000cps, 18000cps, 20000cps or 24000 cps.
Preferably, the curing agent comprises an epoxy curing agent, which may be a difunctional polymer or a trifunctional polymer.
Preferably, the epoxy curing agent includes any one of aliphatic polyamine, alicyclic polyamine, aromatic amine, or acid anhydride.
Preferably, the epoxy curing agent includes any one of ethylenediamine EDA, diethylenetriamine DETA, triethylenetetramine TETA, polyethylenepolyamine PEPA, dipropylenetriamine DPTA, dimethylaminopropylamine DMAPA, diethylaminopropylamine DEAPA, trimethylhexamethylenediamine TMD, diaminomethylcyclohexane, hexahydropyridine HHP, isophoronediamine IPDA, diaminocyclohexane DAHM, diaminomethylcyclohexylmethane dammm, m-phenylenediamine, m-xylylenediamine, diaminodiphenylmethane, diaminodiphenylsulfone, m-aminomethane, benzophenone tetracarboxylic dianhydride, tetrahydrophthalic anhydride, or nadic anhydride.
Preferably, the antistatic agent comprises quaternary ammonium salt and/or ionic liquid, and can be added according to application requirements.
Preferably, the ionic liquid comprises any one of 1-ethyl-3-methylimidazole bis (trifluoromethyl) sulfonyl imide salt, lithium bis (trifluoromethyl) sulfonyl imide or lithium bis (trifluoromethyl) sulfonyl imide.
Preferably, the leveling agent comprises a hydroxyl-containing silicone-based leveling agent, such as BYK3700 or BYK3560, bibk chemical, germany, or the like.
Preferably, the release film layer is made of a PET single-silicon release film.
Preferably, the thickness of the release film layer is 12-75 μm, such as 12 μm, 15 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, or 75 μm, and the like.
Preferably, the release film layer has a release force of 10-30g/25mm, such as 10g/25mm, 15g/25mm, 20g/25mm, 25g/25mm, or 30g/25mm, and the like.
In a second aspect, the present invention provides a method for preparing the protective film for a PVD process of glass according to the first aspect, the method comprising the following steps:
(1) mixing the raw material of the adhesive layer with a solvent to obtain a mixed solution;
(2) and (2) coating the mixed solution obtained in the step (1) on a release film layer, drying, then compounding with a substrate layer, rolling and curing to obtain the protective film for the glass PVD process.
Preferably, the solvent in step (1) comprises any one of ethyl acetate, toluene, butanone, isopropanol or methanol.
Preferably, the solid content of the mixed solution in the step (1) is 20% to 50%, such as 20%, 30%, 40%, or 50%.
Preferably, the drying temperature in step (2) is 80-120 ℃, such as 80 ℃, 90 ℃, 100 ℃, 110 ℃ or 120 ℃, and the like, and the drying is carried out until the thickness of the adhesive layer is 5-30 μm, such as 5 μm, 10 μm, 15 μm, 20 μm, 25 μm or 30 μm, and the like.
Preferably, the curing temperature in the step (2) is 40-50 ℃, such as 40 ℃, 45 ℃ or 50 ℃, and the like, and the curing time is 40-72h, such as 40h, 45h, 50h, 55h, 60h, 65h, 70h or 72h, and the like.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the invention, flexible films such as a PVC film, a PA film or a TPEE film are used as a substrate layer of the protective film, the substrate is soft, the heat shrinkage rate is low, the flexible film is tightly attached to a curved surface attached object in a high-temperature process and does not warp, the surface of glass can be well protected, and the glass is not corroded in the pickling and washing process. As a preferred technical scheme, the high-molecular-weight acrylic glue is matched with the flexible film, so that the prepared protective film has good heat resistance and acid resistance, the viscosity climbing is small after the high-temperature process, the protective film is easy to peel off (the peeling force between the protective film and the glass is 328.66-688.22g/25mm), the protective film is not layered in the high-temperature process, the edge does not warp, the glass can be effectively protected, the glass is prevented from being scratched or polluted, and the high-molecular-weight acrylic glue is suitable for the PVD process of the curved glass.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a protective film for a glass PVD (physical vapor deposition) process, which comprises a substrate layer, an adhesive layer and a release film layer from top to bottom in sequence; the material of substrate layer is the PVC membrane.
Wherein the thickness of the PVC film is 70 μm, the plasticizer content is 20%, the light transmittance is 90.1%, the haze is 46.2%, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3% under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
wherein the number average molecular weight of the acrylic glue is 350000, the hydroxyl value is 62mgKOH/g, and the viscosity is 17000 +/-7000 cps at 23 +/-2 ℃; the curing agent is fully developed NE-100X; the antistatic agent is lithium bistrifluoromethane succinimide; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 microns, then compounding with a smooth surface of a PVC film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
Example 2
The embodiment provides a protective film for a glass PVD (physical vapor deposition) process, which comprises a substrate layer, an adhesive layer and a release film layer from top to bottom in sequence; the material of substrate layer is the PVC membrane.
Wherein the thickness of the PVC film is 70 μm, the plasticizer content is 24%, the light transmittance is 90.1%, the haze is 46.2%, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3% under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
wherein the number average molecular weight of the acrylic glue is 500000, the hydroxyl value is 40mgKOH/g, and the viscosity is 17000 +/-7000 cps at 23 +/-2 ℃; the curing agent is fully developed NE-100X; the antistatic agent is lithium bistrifluoromethane succinimide; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 microns, then compounding with a smooth surface of a PVC film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
Example 3
The embodiment provides a protective film for a glass PVD (physical vapor deposition) process, which comprises a substrate layer, an adhesive layer and a release film layer from top to bottom in sequence; the material of substrate layer is the PVC membrane.
Wherein the thickness of the PVC film is 80 μm, the plasticizer content is 24%, the light transmittance is 89.9%, the haze is 44.3%, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3% under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
100 parts of acrylic glue;
2 parts of a curing agent;
and 1 part of a leveling agent.
Wherein the number average molecular weight of the acrylic glue is 500000, the hydroxyl value is 40mgKOH/g, and the viscosity is 17000 +/-7000 cps at 23 +/-2 ℃; the curing agent is fully developed NE-100X; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 microns, then compounding with a smooth surface of a PVC film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
Example 4
The embodiment provides a protective film for a glass PVD (physical vapor deposition) process, which comprises a substrate layer, an adhesive layer and a release film layer from top to bottom in sequence; the material of substrate layer is the PVC membrane.
Wherein the thickness of the PVC film is 50 μm, the plasticizer content is 16%, the light transmittance is 90.3%, the haze is 46.2%, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3% under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
wherein the number average molecular weight of the acrylic glue is 350000, the hydroxyl value is 62mgKOH/g, and the viscosity is 17000 +/-7000 cps at 23 +/-2 ℃; the curing agent is fully developed NE-100X; the antistatic agent is lithium bistrifluoromethane succinimide; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 microns, then compounding with a smooth surface of a PVC film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
Example 5
The embodiment provides a protective film for a glass PVD (physical vapor deposition) process, which comprises a substrate layer, an adhesive layer and a release film layer from top to bottom in sequence; the material of substrate layer is the PVC membrane.
Wherein the thickness of the PVC film is 150 μm, the plasticizer content is 30%, the light transmittance is 88.5%, the haze is 52.2%, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3% under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
wherein the number average molecular weight of the acrylic glue is 600000, the hydroxyl value is 36mgKOH/g, and the viscosity is 17000 +/-7000 cps at 23 +/-2 ℃; the curing agent is fully developed NE-100X; the antistatic agent is lithium bistrifluoromethane succinimide; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 microns, then compounding with a smooth surface of a PVC film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
Example 6
The embodiment provides a protective film for a glass PVD (physical vapor deposition) process, which comprises a substrate layer, an adhesive layer and a release film layer from top to bottom in sequence; the material of substrate layer is the PA membrane.
Wherein the thickness of the PA film is 50 μm, no plasticizer is used, the light transmittance is 81%, the haze is 12%, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3% under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
100 parts of acrylic glue;
3 parts of a curing agent;
and 1 part of a leveling agent.
Wherein the number average molecular weight of the acrylic glue is 200000, the hydroxyl value is 72mgKOH/g, and the viscosity at 23 +/-2 ℃ is 17000 +/-7000 cps; the curing agent is fully developed NE-100X; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 micrometers, then compounding with a smooth surface of a PA film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
Example 7
The embodiment provides a protective film for a glass PVD (physical vapor deposition) process, which comprises a substrate layer, an adhesive layer and a release film layer from top to bottom in sequence; the base material layer is made of a TPEE film.
Wherein, the thickness of the TPEE film is 30 μm, no plasticizer is used, the light transmittance is 80.4 percent, the haze is 10.6 percent, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3 percent under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
100 parts of acrylic glue;
3 parts of a curing agent;
and 1 part of a leveling agent.
Wherein the number average molecular weight of the acrylic glue is 200000, the hydroxyl value is 72mgKOH/g, and the viscosity at 23 +/-2 ℃ is 17000 +/-7000 cps; the curing agent is fully developed NE-100X; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 microns, then compounding with a smooth surface of a TPEE film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
Example 8
The present example is the same as example 1 except that the plasticizer content of the PVC film was 10%, and the other conditions were the same as example 1.
Example 9
This example is similar to example 1 except that the plasticizer content of the PVC film was 35%, and the heat shrinkage rates in both MD and TD were > 3% at 150 ℃ for 20min, and the other conditions were the same as example 1.
Example 10
The embodiment provides a protective film for a glass PVD (physical vapor deposition) process, which comprises a substrate layer, an adhesive layer and a release film layer from top to bottom in sequence; the material of substrate layer is the PVC membrane.
Wherein the thickness of the PVC film is 70 μm, the plasticizer content is 24%, the light transmittance is 90.1%, the haze is 46.2%, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3% under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
100 parts of acrylic glue;
8 parts of a curing agent;
and 1 part of a leveling agent.
Wherein the number average molecular weight of the acrylic glue is 100000, the hydroxyl value is 78mgKOH/g, and the viscosity is 17000 +/-7000 cps at 23 +/-2 ℃; the curing agent is fully developed NE-100X; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 microns, then compounding with a smooth surface of a PVC film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
Comparative example 1
The comparative example provides a protective film for a glass PVD (physical vapor deposition) process, and the protective film sequentially comprises a base material layer, an adhesive layer and a release film layer from top to bottom; the material of substrate layer is PE membrane.
The PE film has the thickness of 70 mu m, no plasticizer, light transmittance of 90.3 percent and haze of 6.2 percent, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3 percent under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
100 parts of acrylic glue;
2 parts of a curing agent;
and 1 part of a leveling agent.
Wherein the number average molecular weight of the acrylic glue is 10000, the hydroxyl value is 66mgKOH/g, and the viscosity is 17000 +/-7000 cps at 23 +/-2 ℃; the curing agent is fully developed NE-100X; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 micrometers, then compounding with a smooth surface of a PE film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
Comparative example 2
The comparative example provides a protective film for a glass PVD (physical vapor deposition) process, and the protective film sequentially comprises a base material layer, an adhesive layer and a release film layer from top to bottom; the material of substrate layer is the PET membrane.
The PET film has the thickness of 50 mu m, no plasticizer, light transmittance of 90.2 percent and haze of 1.5 percent, and the heat shrinkage rates in the MD direction and the TD direction are both less than 3 percent under the conditions of 150 ℃ and 20 min; the release film layer is made of PET single-silicon release film, the thickness of the release film layer is 50 micrometers, and the release force is 10g/25 mm.
The adhesive layer comprises the following raw materials in parts by weight:
100 parts of acrylic glue;
2 parts of a curing agent;
and 1 part of a leveling agent.
Wherein the number average molecular weight of the acrylic glue is 10000, the hydroxyl value is 66mgKOH/g, and the viscosity is 17000 +/-7000 cps at 23 +/-2 ℃; the curing agent is fully developed NE-100X; the leveling agent was birk 3700.
The preparation method comprises the following steps:
(1) mixing the raw materials for preparing the adhesive layer with ethyl acetate serving as a solvent, and stirring at normal temperature for 40min to obtain a mixed solution with the solid content of 30%;
(2) and (2) coating the mixed solution obtained in the step (1) on a release surface of a release film layer, drying at 100 ℃ until the thickness of the adhesive layer is 20 microns, then compounding with a smooth surface of a PET film, rolling, and curing at 45 ℃ for 72 hours to obtain the protective film for the glass PVD process.
The protective films for the PVD process of glasses of examples 1 to 10 and comparative examples 1 to 2 were subjected to the following performance test methods:
(1) peel strength of protective film from steel plate SUS 304: the test was carried out according to the method of GB/T2792-: peeling at 180 degrees for 300 mm/min;
(2) aged peel force of protective film and glass at 180 ℃ for 1 h: the test was carried out according to the method of GB/T2792-: a sample with the width of 25mm is taken and stuck on the surface of glass, the sample is taken out and cooled to room temperature for testing after being baked in an oven at the temperature of 180 ℃ for 1h, and the sample is peeled off at the temperature of 180 ℃ for 300 mm/min;
(3) residual gum at 180 ℃ 1h & appearance: attaching the sample on the surface of glass with bubbles, baking in an oven at 180 ℃ for 1h, taking out, and observing the appearance; after cooling to room temperature, uncovering the protective film, and observing whether the pollution such as adhesive residue exists or not in a darkroom with strong light;
(4) smoke conditions at 180 ℃ for 1 h: placing 5A 4 samples in a sealed oven at 180 ℃ for 1h, opening the oven, and observing smoke-free fog by strong light flashlight irradiation;
(5) the resistance value of the rubber surface is as follows: testing by adopting an SIMCO impedance tester;
(6) acid prevention: attaching the sample to the surface of the glass, performing simulated immersion for 20min by using acetic acid, 2% dilute sulfuric acid or 2% dilute nitric acid and the like, and observing whether poor attachment occurs.
The results of the performance tests are shown in table 1.
TABLE 1
As can be seen from Table 1, the protective films prepared in the embodiments 1 to 7 of the present invention have low viscosity climbing after high temperature baking, are easy to peel (peeling force between the protective films and glass: 328.66-688.22g/25mm), have good adhesion to glass, have no adhesive residue, have no edge curl, can provide good protection for glass in a PVD process, have no smoke during use, do not affect health of workers, and can be widely applied to the PVD process.
The protective film provided in example 8 was too brittle and easily broken on the glass surface after baking, and the protective film provided in example 9 showed significant haze after baking at high temperature, which indicates that too high or too low plasticizer content of the PVC film resulted in the degradation of the protective film. The protective film provided in example 10 exhibited slight adhesive residue.
After the protective film provided by the comparative example 1 is baked, the protective film is melted on the surface of the glass, and the edge of the protective film provided by the comparative example 2 is warped after being attached to the surface of the glass.
The applicant states that the present invention is illustrated by the above embodiments of the protective film for PVD process of glass and the preparation method thereof, but the present invention is not limited to the above embodiments, i.e. it does not mean that the present invention is implemented only by relying on the above embodiments. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. The protective film for the glass PVD process is characterized by sequentially comprising a base material layer, an adhesive layer and a release film layer from top to bottom;
the material of the substrate layer is a flexible film;
the flexible film includes any one of a polyvinyl chloride film, a nylon film, or a thermoplastic polyester elastomer film.
2. The protective film for a glass PVD process of claim 1, wherein a thickness of the flexible film is 10-150 μm;
preferably, the polyvinyl chloride film has a plasticizer content of 16% to 30%;
preferably, the light transmittance of the flexible film is > 80%, and the haze of the flexible film is < 60%;
preferably, the heat shrinkage rate of the flexible film in the MD direction and the TD direction is less than 3% under the condition of 150 ℃ and 20 min.
3. The protective film for the PVD process of glass as recited in claim 1 or 2, wherein the adhesive layer is prepared from the following raw materials in parts by weight:
4. the protective film for a glass PVD process as defined in claim 3, wherein the number average molecular weight of the acrylic glue is 200000-700000;
preferably, the hydroxyl value of the acrylic glue is 34-88 mgKOH/g;
preferably, the viscosity of the acrylic glue at 23 +/-2 ℃ is 17000 +/-7000 cps.
5. The protective film for a glass PVD process of claim 3 or 4, wherein the curing agent comprises an epoxy curing agent;
preferably, the epoxy curing agent comprises any one of aliphatic polyamine, alicyclic polyamine, aromatic amine or acid anhydride;
preferably, the epoxy curing agent includes any one of ethylenediamine, diethylenetriamine, triethylenetetramine, polyethylenepolyamine, dipropylenetriamine, dimethylaminopropylamine, diethylaminopropylamine, trimethylhexamethylenediamine, diaminomethylcyclohexane, hexahydropyridine, isophoronediamine, diaminocyclohexane, diaminomethylcyclohexylmethane, m-phenylenediamine, m-xylylenediamine, diaminodiphenylmethane, diaminodiphenylsulfone, m-aminomethane, phenonetetracarboxylic dianhydride, tetrahydrophthalic anhydride, or nadic anhydride.
6. The protective film for a glass PVD process of any of claims 3-5, wherein the antistatic agent comprises a quaternary ammonium salt and/or an ionic liquid;
preferably, the ionic liquid comprises any one of 1-ethyl-3-methylimidazole bis (trifluoromethyl) sulfonyl imide salt, lithium bis (trifluoromethyl) sulfonyl imide or lithium bis (trifluoromethyl) sulfonyl imide;
preferably, the leveling agent includes a hydroxyl group-containing silicone-based leveling agent.
7. The protective film for the PVD process of glass as recited in any of claims 1 to 6, wherein the release film layer is made of a PET single silicon release film;
preferably, the thickness of the release film layer is 12-75 μm;
preferably, the release force of the release film layer is 10-30g/25 mm.
8. The method for preparing a protective film for a glass PVD process according to any of claims 1-7, wherein the method comprises the following steps:
(1) mixing the raw material of the adhesive layer with a solvent to obtain a mixed solution;
(2) and (2) coating the mixed solution obtained in the step (1) on a release film layer, drying, then compounding with a substrate layer, rolling and curing to obtain the protective film for the glass PVD process.
9. The method according to claim 8, wherein the solvent of step (1) comprises any one of ethyl acetate, toluene, methyl ethyl ketone, isopropyl alcohol or methanol;
preferably, the solid content of the mixed solution in the step (1) is 20-50%.
10. The preparation method according to claim 8 or 9, wherein the drying temperature in the step (2) is 80-120 ℃, and the drying is carried out until the thickness of the adhesive layer is 5-30 μm;
preferably, the curing temperature in the step (2) is 40-50 ℃, and the curing time is 40-72 h.
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| CN111154428A (en) * | 2019-12-18 | 2020-05-15 | 苏州高泰电子技术股份有限公司 | Antistatic UV (ultraviolet) anti-sticking adhesive tape and preparation method thereof |
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| CN111154428A (en) * | 2019-12-18 | 2020-05-15 | 苏州高泰电子技术股份有限公司 | Antistatic UV (ultraviolet) anti-sticking adhesive tape and preparation method thereof |
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| CN114921188A (en) * | 2022-05-27 | 2022-08-19 | 苏州赛伍应用技术股份有限公司 | Low-tear-film-voltage environment-friendly acrylic PVC protective film and preparation method thereof |
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Application publication date: 20211221 |
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