CN116410653A - Self-repairing coating, electronic screen protective film and preparation method - Google Patents
Self-repairing coating, electronic screen protective film and preparation method Download PDFInfo
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- CN116410653A CN116410653A CN202310399992.9A CN202310399992A CN116410653A CN 116410653 A CN116410653 A CN 116410653A CN 202310399992 A CN202310399992 A CN 202310399992A CN 116410653 A CN116410653 A CN 116410653A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 134
- 238000000576 coating method Methods 0.000 title claims abstract description 134
- 230000001681 protective effect Effects 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000010410 layer Substances 0.000 claims abstract description 324
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims abstract description 120
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims abstract description 90
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims abstract description 90
- 229920001971 elastomer Polymers 0.000 claims abstract description 82
- 239000000806 elastomer Substances 0.000 claims abstract description 82
- -1 acrylic ester Chemical class 0.000 claims abstract description 28
- 229920006276 ketonic resin Polymers 0.000 claims abstract description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 14
- 239000012948 isocyanate Substances 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 11
- 239000004417 polycarbonate Substances 0.000 claims abstract description 11
- 229920000728 polyester Polymers 0.000 claims abstract description 11
- 229920005862 polyol Polymers 0.000 claims abstract description 9
- 150000003077 polyols Chemical class 0.000 claims abstract description 9
- 239000012949 free radical photoinitiator Substances 0.000 claims abstract description 6
- 238000001723 curing Methods 0.000 claims description 54
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 17
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
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- 238000000034 method Methods 0.000 claims description 12
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- 238000013007 heat curing Methods 0.000 claims description 10
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 7
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 7
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- 239000003973 paint Substances 0.000 claims description 5
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- 230000008569 process Effects 0.000 claims description 5
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 claims description 3
- VZXPHDGHQXLXJC-UHFFFAOYSA-N 1,6-diisocyanato-5,6-dimethylheptane Chemical compound O=C=NC(C)(C)C(C)CCCCN=C=O VZXPHDGHQXLXJC-UHFFFAOYSA-N 0.000 claims description 3
- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical class OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 claims description 3
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 3
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 3
- HDONYZHVZVCMLR-UHFFFAOYSA-N N=C=O.N=C=O.CC1CCCCC1 Chemical compound N=C=O.N=C=O.CC1CCCCC1 HDONYZHVZVCMLR-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- KUIDSTKCJKFHLZ-UHFFFAOYSA-N [4-(prop-2-enoyloxymethyl)cyclohexyl]methyl prop-2-enoate Chemical compound C=CC(=O)OCC1CCC(COC(=O)C=C)CC1 KUIDSTKCJKFHLZ-UHFFFAOYSA-N 0.000 claims description 3
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical group C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 3
- 125000005587 carbonate group Chemical group 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 125000004386 diacrylate group Chemical group 0.000 claims description 3
- 238000007606 doctor blade method Methods 0.000 claims description 3
- 238000005886 esterification reaction Methods 0.000 claims description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 3
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 3
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 3
- RZFODFPMOHAYIR-UHFFFAOYSA-N oxepan-2-one;prop-2-enoic acid Chemical compound OC(=O)C=C.O=C1CCCCCO1 RZFODFPMOHAYIR-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
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- 239000012748 slip agent Substances 0.000 claims description 3
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- 125000005396 acrylic acid ester group Chemical group 0.000 claims description 2
- 230000032050 esterification Effects 0.000 claims description 2
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical class OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
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- 229910052710 silicon Inorganic materials 0.000 description 12
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- 239000011521 glass Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
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- 238000001179 sorption measurement Methods 0.000 description 6
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
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- 239000002537 cosmetic Substances 0.000 description 5
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 150000002513 isocyanates Chemical class 0.000 description 4
- 239000000741 silica gel Substances 0.000 description 4
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- 229920002635 polyurethane Polymers 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- YXRKNIZYMIXSAD-UHFFFAOYSA-N 1,6-diisocyanatohexane Chemical compound O=C=NCCCCCCN=C=O.O=C=NCCCCCCN=C=O.O=C=NCCCCCCN=C=O YXRKNIZYMIXSAD-UHFFFAOYSA-N 0.000 description 2
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- 150000008366 benzophenones Chemical class 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
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Images
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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- 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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
-
- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- 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]
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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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
- C09J2475/00—Presence of polyurethane
-
- 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
- C09J2483/00—Presence of polysiloxane
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Laminated Bodies (AREA)
Abstract
The embodiment of the application provides a self-repairing coating, an electronic screen protective film and a preparation method, and relates to the field of protective films. The self-repairing coating comprises the following components in parts by weight: 60-70 parts of linear aliphatic polycarbonate polyol, 20-30 parts of hydroxyl polyester, 90-110 parts of dual-curing resin, 40-50 parts of acrylic ester, 60-70 parts of ketone-aldehyde resin, 35-45 parts of aliphatic isocyanate, 1-1.5 parts of free radical photoinitiator, 0.05-0.15 part of non-organotin catalyst, 1-5 parts of slipping agent and 170-210 parts of solvent. The electronic screen protection film comprises the following components which are overlapped from top to bottom in sequence: the self-repairing adhesive comprises a base film layer, a first pressure-sensitive adhesive layer, a self-repairing layer, a thermoplastic polyurethane elastomer layer, a second pressure-sensitive adhesive layer and a release film layer. The protective film has good offset printing and excellent self-repairing capability, can ensure the self-repairing effect for a long time, and can be used under extreme conditions.
Description
Technical Field
The application relates to the field of protective films, in particular to a self-repairing coating, an electronic screen protective film and a preparation method.
Background
Along with the continuous popularization and innovation of electronic products, electronic screen protection films are updated continuously, wherein mobile phones and mobile phone protection films are the most typical representatives. The primary use of the mobile phone protection film by consumers is mainly to protect the mobile phone, and the requirements of the mobile phone protection film are not limited to the protection function, and new requirements are also put forward: blue light prevention, frosting, peeping prevention, self-repairing and the like. Therefore, novel films such as a blue light protection film, a frosted protection film, a peeping protection film, a self-repairing protection film and the like are produced, wherein the self-repairing protection film is mainly applied to curved-surface mobile phones.
At present, most of film layers for realizing self-repairing functions in the self-repairing protective film are thermosetting repairing material systems, but offset printing and self-repairing capabilities and long-term stability of the protective film are poor.
Disclosure of Invention
In order to solve at least one technical problem, an object of the embodiments of the present application is to provide a self-repairing coating, an electronic screen protective film and a preparation method thereof, wherein the protective film has good offset printing and excellent self-repairing capability, can ensure a self-repairing effect for a long time, and can be used under extreme conditions.
In a first aspect, an embodiment of the present application provides a self-repairing coating, including the following components in parts by weight:
in the technical scheme, the self-repairing coating is a double-curing coating, and the self-repairing layer is obtained through heat curing and ultraviolet curing. Wherein the linear aliphatic polycarbonate polyol contains self-repairing C=C double bonds, and can generate intermolecular acting force (polar group) with the second component hydroxyl polyester, so that the self-repairing performance of the film is affected, and the self-repairing is facilitated; the self-repairing coating contains rich active hydrogen-containing groups (hydrogen bond, amino, hydroxyl and the like), so that the self-repairing layer can be recovered in a short time after being damaged by external force.
In one possible implementation, the linear aliphatic polycarbonate polyol is a polymer containing repeating carbonate groups in the molecular backbone and hydroxyl groups at the chain ends, and is selected from the group consisting of Covestro Desmophen C, covestro Desmophen C1200, desmophen C2200, desmophen C2100, asahi chemical "Duoble" from Kogyo Polymer Co., ltd TM At least one of.
In one possible implementation, the hydroxyl polyester is obtained by dehydration esterification of a dibasic acid with an excess of a polyol, optionally selected from at least one of H101, H103, H104 of the HyPer H10 series of Desmophen 670BA, desmophen 651MPA/X, of Corp.
In one possible implementation, the dual cure resin is a modified urethane acrylate, optionally selected from at least one of 1831A, 1443 of Guangdong Dingrison New Material Co., ltd., D-039 of Sante chemical Co., ltd., HUV-201A of Suzhou air Intelligence New Material Co., ltd., and dual stage cured coating DHC-92L of Guangzhou tetrahedron New Material technologies Co., ltd.
In one possible implementation, the acrylate is at least one of a-NOD-N, A-HD-N,1, 4-cyclohexanedimethanol diacrylate, polyethylene glycol diacrylate, ethoxylated trimethylolpropane triacrylate, caprolactone acrylate, available from new middle village chemical industries, inc;
and/or the ketone-aldehyde resin is KR-1021 of An Feng technical Co., ltd;
and/or the aliphatic isocyanate is at least one of isophorone diisocyanate, hexamethylene diisocyanate, 4' -diisocyanate, methylcyclohexane diisocyanate, trimethylhexamethylene diisocyanate and xylylene diisocyanate;
and/or the free radical photoinitiator is a benzophenone derivative;
and/or the non-organotin catalyst is at least one of TMG 160, TMG 720, TMG 634, TMG 612, TMG 330 of Shanghai, haimanhai, schmidt chemical Co., ltd;
and/or the slip agent is a silicone acrylate, optionally winning digao TEGO Rad2250;
and/or the solvent is at least one of methyl isobutyl ketone, ethyl acetate, methyl acetate, propyl acetate, methyl isobutyl ketone, toluene, xylene, cyclohexane, 120# solvent, cyclohexanone and isopropanol.
In a second aspect, an embodiment of the present application provides an electronic screen protection film, which includes: the self-repairing coating comprises a base film layer, a first pressure-sensitive adhesive layer, a self-repairing layer, a thermoplastic polyurethane elastomer layer (TPU layer), a second pressure-sensitive adhesive layer and a release film layer, wherein the self-repairing layer is obtained by coating, thermally curing and ultraviolet curing the self-repairing coating provided in the first aspect.
In the technical scheme, the thermoplastic polyurethane elastomer (TPU) has good elasticity and large tensile fracture rate, is a high polymer material with very good resilience after external force is withdrawn, and when the TPU layer is taken as a base material to form a protective film formed by a self-repairing layer, the protective film is subjected to the action of external force to crack, the external force is withdrawn, the TPU molecules can be recovered, and the action can be promoted to occur at high temperature, so that the effect of automatic repairing is achieved.
In one possible implementation manner, the first pressure-sensitive adhesive layer comprises the following components in parts by weight:
in the technical scheme, the first pressure-sensitive adhesive layer is a PU adhesive system and is used for protecting the repair layer, and the stripping force is small.
In one possible implementation manner, the second pressure-sensitive adhesive layer comprises the following components in parts by weight:
in the technical scheme, the second pressure-sensitive adhesive layer corresponding to the glue is a silica gel pressure-sensitive adhesive, and has high stripping force and high hardness.
In a third aspect, an embodiment of the present application provides a method for preparing an electronic screen protection film provided in the second aspect, including the following steps:
a first pressure-sensitive adhesive layer is arranged on the base film layer;
the two sides of the thermoplastic polyurethane elastomer layer are respectively provided with a self-repairing layer, a second pressure-sensitive adhesive layer and a release film layer, so that the first pressure-sensitive adhesive layer and the self-repairing layer are laminated and compounded together.
In one possible implementation, it includes the steps of:
coating glue corresponding to the first pressure-sensitive adhesive layer on the base film layer, thermally curing to obtain the first pressure-sensitive adhesive layer, and coating the first pressure-sensitive adhesive layer with a first release film;
coating a coating corresponding to the thermoplastic polyurethane elastomer layer on the second release film, thermally curing to obtain the thermoplastic polyurethane elastomer layer, and coating the thermoplastic polyurethane elastomer layer with a third release film;
tearing the second release film on the thermoplastic polyurethane elastomer layer, coating a layer of self-repairing coating on the thermoplastic polyurethane elastomer layer, and obtaining the self-repairing layer through heat curing and ultraviolet curing;
tearing off the first release film on the first pressure-sensitive adhesive layer, and coating and curing the self-repairing layer by using the first pressure-sensitive adhesive layer;
tearing the third release film on the thermoplastic polyurethane elastomer layer, coating a layer of glue corresponding to the second pressure-sensitive layer on the thermoplastic polyurethane elastomer layer, thermally curing to obtain a second pressure-sensitive adhesive layer, and coating the second pressure-sensitive adhesive layer with the release film layer;
or alternatively, the process may be performed,
coating glue corresponding to the first pressure-sensitive adhesive layer on the base film layer, thermally curing to obtain the first pressure-sensitive adhesive layer, and coating the first pressure-sensitive adhesive layer with a first release film;
coating a coating corresponding to the thermoplastic polyurethane elastomer layer on the second release film, thermally curing to obtain the thermoplastic polyurethane elastomer layer, and coating the thermoplastic polyurethane elastomer layer with a third release film;
and tearing the third release film on the thermoplastic polyurethane elastomer layer, coating a layer of glue corresponding to the second pressure-sensitive layer on the thermoplastic polyurethane elastomer layer, thermally curing to obtain a second pressure-sensitive adhesive layer, and coating the second pressure-sensitive adhesive layer with the release film layer.
Tearing the second release film on the thermoplastic polyurethane elastomer layer, coating a layer of self-repairing coating on the thermoplastic polyurethane elastomer layer, and obtaining the self-repairing layer through heat curing and ultraviolet curing;
and tearing off the first release film on the first pressure-sensitive adhesive layer, and coating and curing the self-repairing layer by using the first pressure-sensitive adhesive layer.
In the technical scheme, the second release film is used as a carrier for coating the coating corresponding to the thermoplastic polyurethane elastomer layer, and after the thermoplastic polyurethane elastomer layer is formed, the third release film is used for coating, so that the appearance of the thermoplastic polyurethane elastomer layer is effectively protected; the first release film is used for protecting the first pressure-sensitive adhesive layer and preventing foreign matters from adhering to influence the appearance and the viscosity of the first pressure-sensitive adhesive layer; the self-repairing coating is coated on the thermoplastic polyurethane elastomer layer to form a self-repairing layer, and an upper protecting layer consisting of a low-viscosity first pressure-sensitive adhesive layer and a base film layer is used for covering to protect the self-repairing layer, and then curing is carried out to enable unreacted thermosetting micromolecules in each layer to continuously react in the curing process; the release film layer is used for protecting the second pressure-sensitive adhesive layer and preventing foreign matters from adhering to influence the appearance and the viscosity of the second pressure-sensitive adhesive layer.
In one possibilityIn the implementation mode of (2), the heat curing temperature is 110-155 ℃, and the energy of ultraviolet light curing is 1000-2000mJ/cm 2 ；
And/or coating in a doctor blade coating or slot coating mode in all steps.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments of the present application will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of an electronic screen protection film according to an embodiment of the present application.
Icon: 100-an electronic screen protective film; 110-a base film layer; 120-a first pressure sensitive adhesive layer; 130-a self-healing layer; 140-a thermoplastic polyurethane elastomer layer; 150-a second pressure sensitive adhesive layer; 160-release film layer.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The self-repairing coating, the electronic screen protective film and the preparation method of the self-repairing coating are specifically described below.
The embodiment of the application provides a self-repairing coating, which comprises the following components in parts by weight: 60-70 parts of linear aliphatic polycarbonate polyol, 20-30 parts of hydroxyl polyester, 90-110 parts of dual-curing resin, 40-50 parts of acrylic ester, 60-70 parts of ketone-aldehyde resin, 35-45 parts of aliphatic isocyanate, 1-1.5 parts of free radical photoinitiator, 0.05-0.15 part of non-organotin catalyst, 1-5 parts of slipping agent and 170-210 parts of solvent. Illustratively, the self-healing coating comprises the following components in parts by weight: 60 parts, 62 parts, 65 parts, 68 parts or 70 parts of linear aliphatic polycarbonate polyol, 20 parts, 23 parts, 25 parts, 27 parts or 30 parts of hydroxyl polyester, 90 parts, 100 parts or 110 parts of dual-curing resin, 40 parts, 41 parts, 43 parts, 45 parts, 47 parts or 50 parts of acrylic ester, 60 parts, 62 parts, 65 parts, 68 parts or 70 parts of ketone-aldehyde resin, 35 parts, 38 parts, 40 parts or 45 parts of aliphatic isocyanate, 1 part, 1.2 parts, 1.35 parts or 1.5 parts of free radical photoinitiator, 0.05 part, 0.1 part or 0.15 part of non-organotin catalyst, 1 part, 3 parts or 5 parts of slipping agent, 170 parts, 180 parts, 190 parts, 200 parts or 210 parts of solvent.
In the embodiment of the application, the specific selection of each component is as follows:
the linear aliphatic polycarbonate polyol is a polymer containing repeated carbonate groups (-O-COO-) in the molecular main chain and hydroxyl groups (-OH) at the chain end, and can be selected from Covestro Desmophen C of Kogyo Polymer (China) Co., ltd., covestro Desmophen C of Kogyo Polymer (China) Co., ltd., desmophen C2200 of Kogyo Polymer (Linear polycarbonate diol), desmophen C2100 of Kogyo Polymer (Linear polycarbonate diol) Co., ltd., xup, and Duozhen of Asahi chemical TM At least one of "(polycarbonate diol).
The hydroxyl polyester is obtained by dehydration esterification reaction of dibasic acid and excessive polyalcohol, and can be selected from at least one of Desmophen 670BA of Korschpolymer (China), desmophen 651MPA/X of Korschpolymer (China), hyPer H10 series H101 of Suzhou Haibut resin technology Co., ltd, hyPer H10 series H103 of Suzhou Haibut resin technology Co., ltd, and HyPer H10 series H104 of Suzhou Haibut resin technology Co., ltd.
The dual-curing resin is a polymer capable of performing thermal curing and photo curing, and specifically can be modified polyurethane acrylic ester, has high hardness, and can be selected from at least one of 1831A of Guangdong Dingrison New Material Co., ltd, 1443 of Guangdong Dingrison New Material Co., ltd-039 of Sante chemical Co., ltd, HUV-201A of Suzhou avionics New Material Co., ltd, and dual-stage curing coating DHC-92L of Guangzhou tetrahedron New Material science and technology Co., ltd.
The acrylic acid ester is the general name of acrylic acid and its homolog esters, and its molecular structure has high polarity and complete saturation, and can be selected from at least one of A-NOD-N of Xinzhongcun chemical industry Co., ltd., A-HD-N of Xinzhongcun chemical industry Co., ltd., 1, 4-cyclohexanedimethanol diacrylate of Guangdong Dauchun Jun chemical industry Co., ltd., polyethylene glycol diacrylate (n=4) of Guangdong Dauchun Jun chemical industry Co., ltd., ethoxylated trimethylolpropane triacrylate of Guangdong Dauchun chemical industry Co., ltd., and caprolactone acrylate of Shanghai chemical Co., ltd.
The ketone-aldehyde resin is a neutral, non-saponified cyclohexanone with high brightness and light resistance, and can be selected from KR-1021 of An Feng industrial technology Co.
The aliphatic isocyanate refers to an isocyanate product except aromatic, the isocyanate product has-N=C-O functional groups, the polyurethane material prepared from the aliphatic isocyanate has good ageing resistance, high temperature resistance, yellowing resistance, light resistance and other performances, and the aliphatic isocyanate can be at least one of isophorone diisocyanate, hexamethylene diisocyanate, 4' -diisocyanate, methylcyclohexane diisocyanate, trimethylhexamethylene diisocyanate, xylylene diisocyanate and the like.
The free radical photoinitiator may be a benzophenone derivative.
The non-organotin catalyst is a catalyst other than organotin catalyst, and is selected from at least one of Valikat Bi2810, TMG 160 of Shanghamikava, TMG 720 of Shanghamikava, TMG 634 of Haimanhamikava, TMG 612 of Haimanhamikava, and TMG 330 of Haimanhamikava.
The slipping agent is a slipping auxiliary agent with high compatibility and high crosslinking agent, can effectively improve the water contact angle of film formation, can be specifically organic silicon acrylic ester, and can be selected as winning Di-high TEGO Rad2250.
The solvent is at least one of methyl isobutyl ketone, ethyl acetate, methyl acetate, propyl acetate, methyl isobutyl ketone, toluene, xylene, cyclohexane, 120# solvent, cyclohexanone and isopropanol.
Referring to fig. 1, the embodiment of the present application further provides an electronic screen protection film 100, which includes a structure that is stacked from top to bottom: a base film layer 110, a first pressure-sensitive adhesive layer 120, a self-healing layer 130, a thermoplastic polyurethane elastomer layer 140, a second pressure-sensitive adhesive layer 150, and a release film layer 160; when in use, the base film layer 110 and the first pressure-sensitive adhesive layer 120 form an upper protective layer, and when in use, the release film layer 160 of the electronic screen protective film 100 is torn off, the second pressure-sensitive adhesive layer 150 is adhered to an electronic screen (such as a curved screen of a curved mobile phone), and then the upper protective layer is torn off.
The self-repairing layer 130 is obtained by coating, thermally curing, and ultraviolet curing with the self-repairing coating.
Wherein, the thermoplastic polyurethane elastomer layer 140 is obtained by coating and thermally curing a corresponding coating, and as an embodiment, the thermoplastic polyurethane elastomer layer 140 comprises the following components in parts by weight: 100 parts by weight of an aliphatic urethane acrylic resin (AA 4835 of European Asian Co., ltd.), 10 to 20 parts by weight of TPU particles (5715 of Lu Borun), 80 to 100 parts by weight of a ketone-aldehyde resin (KR-1021 of An Feng Co., ltd.), 25 to 30 parts by weight of butanone, 50 to 55 parts by weight of cyclohexanone, 0.3 to 0.5 parts by weight of a polyester modified hydroxyl-functional polydimethylsiloxane-containing solution (Pick chemical, BYK-371), 10 to 20 parts by weight of a high-functionality HDI trimer (Kogyo Co., aliphatic polyisocyanate series, N3700) were mixed to obtain a TPU composite glue.
The first pressure-sensitive adhesive layer 120 is obtained by coating and thermally curing corresponding glue, and as an embodiment, the components of the first pressure-sensitive adhesive layer 120 corresponding to the glue include, in parts by weight: 45-50 parts of polyurethane resin, 3-5 parts of isocyanate curing agent, 0.3-2 parts of antistatic agent and 45-50 parts of solvent. The first pressure-sensitive adhesive is a PU adhesive system and is used for protecting the repair layer, the peeling force is small, the steel plate is 2-4gf/25mm, the film tearing force before baking is 0.5-2gf/25mm, and the film tearing force after baking is 1.5-4gf/25mm.
The second pressure-sensitive adhesive layer 150 is obtained by coating and thermally curing corresponding glue, and as an embodiment, the components of the second pressure-sensitive adhesive layer 150 corresponding to the glue include, in parts by weight: 100 parts of silica gel resin, 0.5-2 parts of reactive polysiloxane, 0.5-2 parts of silane coupling agent, 1-3 parts of platinum catalyst and 80-200 parts of solvent. The second pressure-sensitive adhesive is a silica gel system and is used for attaching an AF cover plate to a client, and the AF cover plate has a high water contact angle (118-120 degrees), so that the second pressure-sensitive adhesive is required to have a larger AF stripping force (more than or equal to 40gf/25 mm).
Wherein, the base film layer 110 may be a PET film; the release film layer 160 may be a fluorine release film.
The embodiment of the application provides a preparation method of the electronic screen protective film 100, which comprises the following steps:
disposing a first pressure-sensitive adhesive layer 120 on the base film layer 110;
the self-repairing layer 130, the second pressure-sensitive adhesive layer 150 and the release film layer 160 are respectively arranged on two sides of the thermoplastic polyurethane elastomer layer 140, so that the first pressure-sensitive adhesive layer 120 and the self-repairing layer 130 are laminated and compounded together.
As an embodiment, it specifically comprises the following steps:
(1) Coating the first pressure-sensitive adhesive layer 120 on the base film layer 110 with glue corresponding to the glue, thermally curing to obtain the first pressure-sensitive adhesive layer 120, and coating the first pressure-sensitive adhesive layer 120 with a first release film.
(2) And coating the coating corresponding to the thermoplastic polyurethane elastomer layer 140 on the second release film, thermally curing to obtain the thermoplastic polyurethane elastomer layer 140, and coating the thermoplastic polyurethane elastomer layer 140 by using a third release film.
(3) Tearing the second release film on the thermoplastic polyurethane elastomer layer 140, coating a layer of self-repairing coating on the thermoplastic polyurethane elastomer layer 140, and performing heat curing and ultraviolet curing to obtain a self-repairing layer 130; in the above technical solution, the dual-cured self-repairing layer 130 may be heated and cured by ultraviolet light, or may be performed simultaneously or separately, for example, heated and cured by ultraviolet light.
It should be noted that the sequence of the step (1) and the step (2) to the step (3) is not required to be specific, and the steps may be performed sequentially or simultaneously.
(4) The first release film on the first pressure-sensitive adhesive layer 120 is peeled off, and the self-repairing layer 130 is covered with the first pressure-sensitive adhesive layer 120 and cured.
After curing, the thermosetting molecules in each film layer continue to react, so that each cured film layer is actually the corresponding film layer in the protective film.
(5) And tearing the third release film on the thermoplastic polyurethane elastomer layer 140, coating a layer of glue corresponding to the second pressure-sensitive layer on the thermoplastic polyurethane elastomer layer 140, thermally curing to obtain a second pressure-sensitive adhesive layer 150, and coating the second pressure-sensitive adhesive layer 150 with a release film layer 160.
As another embodiment, the following steps may also be used:
(1) Coating glue corresponding to the first pressure-sensitive adhesive layer 120 on the base film layer 110, thermally curing to obtain the first pressure-sensitive adhesive layer 120, and coating the first pressure-sensitive adhesive layer with a first release film;
(2) Coating a coating corresponding to the thermoplastic polyurethane elastomer layer 140 on the second release film, thermally curing to obtain the thermoplastic polyurethane elastomer layer 140, and coating the thermoplastic polyurethane elastomer layer with a third release film;
(3) And tearing the third release film on the thermoplastic polyurethane elastomer layer 140, coating a layer of glue corresponding to the second pressure-sensitive layer 150 on the thermoplastic polyurethane elastomer layer 140, thermally curing to obtain a second pressure-sensitive adhesive layer 150, and coating the second pressure-sensitive adhesive layer 150 with a release film layer 160.
(4) Tearing the second release film on the thermoplastic polyurethane elastomer layer 140, coating a layer of self-repairing coating on the thermoplastic polyurethane elastomer layer 140, and performing heat curing and ultraviolet curing to obtain a self-repairing layer 130;
(5) And tearing off the first release film on the first pressure-sensitive adhesive layer 120, and coating and curing the self-repairing layer 130 by using the first pressure-sensitive adhesive layer 120.
In the above preparation process, the first release film, the second release film and the third release film are typically silicon-based release films, and the release film in the protective film is typically a fluorine-based release film.
In all the above steps, the heat curing temperatures are 110-155 ℃ respectively; the energy of ultraviolet light solidification is 1000-2000mJ/cm 2 . The coating can be performed in a doctor blade coating or slot coating mode in all steps.
The features and capabilities of the present application are described in further detail below in connection with the examples.
Example 1
The embodiment provides a self-repairing protection film for curved mobile phone, the protection film includes top-down stack setting in proper order: the adhesive comprises a base film layer, a first pressure-sensitive adhesive layer, a self-repairing layer, a thermoplastic polyurethane elastomer layer, a second pressure-sensitive adhesive layer and a release film layer, wherein the base film layer and the first pressure-sensitive adhesive=an upper protective layer.
The material components of the first pressure-sensitive adhesive layer corresponding to the glue are as follows: 48 parts by weight of polyurethane resin (KT-9005, korean KT), 1 part by weight of antistatic agent (GT-100F, shanghai Gu Tong technology Co., ltd.), 3.8 parts by weight of isocyanate curing agent (NA-220, shanghai Gu Tong technology Co., ltd.) and 46.6 parts by weight of ethyl acetate, and the above materials are uniformly mixed and stirred.
The self-repairing layer corresponds to the self-repairing paint and comprises the following material components: 65 parts by weight of a linear aliphatic polycarbonate polyol
C1100, guangzhou-Hao Yi New Material science and technology Co., ltd.), 25 parts by weight of a hydroxy polyester
670BA, guangzhou Hao, new Material technologies Co., ltd.), 100 parts by weight of a dual-cure resin (DSU-1831A, guangdong Dingdi Sen New Material Co., ltd.), 45 parts by weight of an acrylic ester (A-NOD-N, new Zhongcun chemical Co., ltd.), 65 parts by weight of a ketone-aldehyde resin (KR-1021, an Feng, utility Co., ltd.), 1.35 parts by weight of a radical photo-initiatorAgent (benzophenone derivative), 0.1 part by weight of a non-organotin catalyst (TMG 160, shanghai Mannheim Gaoshimi chemical Co., ltd.) 40 parts by weight of an aliphatic isocyanate (>
N3700, guangzhou-Hao, new Material science and technology Co., ltd.), 3 parts by weight of a slipping agent (Digao TEGO Rad2250, winning, 150 parts by weight of methyl isobutyl ketone and 40 parts by weight of ethyl acetate, and the above materials are uniformly mixed and stirred.
The thermoplastic polyurethane elastomer layer corresponds to the material composition of the coating: 100 parts by weight of aliphatic polyurethane acrylic resin (AA 4835 of European Asia corporation), 15 parts by weight of TPU particles (5715 of Lu Borun), 90 parts by weight of ketone-aldehyde resin (KR-1021 of An Feng practical Co.), 28 parts by weight of butanone, 52 parts by weight of cyclohexanone, 0.4 part by weight of polyester modified hydroxyl-functional polydimethylsiloxane solution (Pick chemical, BYK-371), 15 parts by weight of high-functionality HDI trimer (Kogyo Co., aliphatic polyisocyanate series, N3700) and uniformly mixing and stirring the above materials.
The material components of the second pressure-sensitive adhesive layer corresponding to the glue are as follows: 100 parts by weight of a silica gel resin (30500 HP, jiangsu Kunshan Pureka nanotechnology Co., ltd.), 0.6 part by weight of a vinylsilane mixture (S-506, jiangsu Kunshan Pureka nanotechnology Co., ltd.), 0.6 part by weight of a reactive polysiloxane (H-7316, jiangsu Kunshan Pureka nanotechnology Co., ltd.), 1.2 parts by weight of a platinum catalyst (SYL-OFF) TM 4000, shi chemical), 70 parts by weight of 120# solvent and 30 parts by weight of ethyl acetate, and uniformly mixing and stirring the above material components.
The preparation method comprises the following steps:
(1) Coating a 50-mu m-thick PET film (base film layer) with glue corresponding to the first pressure-sensitive adhesive layer, baking at 120 ℃ for 2 minutes to obtain a 10-mu m-thick first pressure-sensitive adhesive layer, and coating the first pressure-sensitive adhesive layer with a 50-mu m silicon-based release film (first release film).
(2) A thermoplastic polyurethane elastomer layer-corresponding coating material was applied to a silicon-based release film (second release film) having a thickness of 50 μm, and the film was baked at 120℃for 2 minutes to obtain a thermoplastic polyurethane elastomer layer having a thickness of 75 μm, and the thermoplastic polyurethane elastomer layer was coated with a silicon-based release film (third release film) having a thickness of 75 μm.
(3) Tearing the second release film on the thermoplastic polyurethane elastomer layer, coating self-repairing paint on the thermoplastic polyurethane elastomer layer, baking at 115 ℃ for 2 minutes at 1000mJ/cm 2 To give a 35 μm thick self-healing layer under UV energy.
(4) And tearing off the first release film on the first pressure-sensitive adhesive layer, attaching the self-repairing layer by using the first pressure-sensitive adhesive layer, and curing for 5 days in the environment of 40 ℃.
(5) And (3) tearing the third release film on the thermoplastic polyurethane elastomer layer, coating glue corresponding to the second pressure-sensitive layer on the thermoplastic polyurethane elastomer layer, baking at 150 ℃ for 2 minutes to obtain a second pressure-sensitive adhesive layer with the thickness of 15 mu m, and coating the second pressure-sensitive adhesive layer with a fluorine release film (release film layer).
When the fluorine-containing self-repairing protective film is used, the fluorine-containing release film of the self-repairing protective film is torn off, the second pressure-sensitive adhesive layer is adhered to the curved surface screen of the curved surface mobile phone, and the upper protective layer is torn off.
Example 2
The present embodiment provides a protective film, which is different from embodiment 1 in that the material composition of the second pressure-sensitive adhesive layer corresponding to the glue is: 50 parts by weight of a silicone resin (AP-7360F, an Pin), 50 parts by weight of a silicone resin (AP-7380F, jiangsu Kunshan Purey nanotechnology Co., ltd.), 1 part by weight of a vinyl silane mixture (297, an Pin), 0.8 part by weight of a reactive polysiloxane (H-7316, jiangsu Kunshan Purey nanotechnology Co., ltd.), 1.44 parts by weight of a platinum catalyst (Dow chemical), 50 parts by weight of toluene and 50 parts by weight of ethyl acetate.
Example 3
This example provides a protective film which differs from example 1 in the preparation steps, as follows:
(1) Coating a 50-mu m-thick PET film (base film layer) with glue corresponding to the first pressure-sensitive adhesive layer, baking at 120 ℃ for 2 minutes to obtain a 10-mu m-thick first pressure-sensitive adhesive layer, and coating the first pressure-sensitive adhesive layer with a 50-mu m silicon-based release film (first release film).
(2) A thermoplastic polyurethane elastomer layer-corresponding coating material was applied to a silicon-based release film (second release film) having a thickness of 50 μm, and the film was baked at 120℃for 2 minutes to obtain a thermoplastic polyurethane elastomer layer having a thickness of 75 μm, and the thermoplastic polyurethane elastomer layer was coated with a silicon-based release film (third release film) having a thickness of 75 μm.
(3) And (3) tearing the third release film on the thermoplastic polyurethane elastomer layer, coating glue corresponding to the second pressure-sensitive layer on the thermoplastic polyurethane elastomer layer, baking at 150 ℃ for 2 minutes to obtain a second pressure-sensitive adhesive layer with the thickness of 15 mu m, and coating the second pressure-sensitive adhesive layer with a fluorine release film (release film layer).
(4) Tearing the second release film on the thermoplastic polyurethane elastomer layer, coating self-repairing paint on the thermoplastic polyurethane elastomer layer, baking at 115 ℃ for 2 minutes at 1000mJ/cm 2 To give a 35 μm thick self-healing layer under UV energy.
(5) And tearing off the first release film on the first pressure-sensitive adhesive layer, attaching the self-repairing layer by using the first pressure-sensitive adhesive layer, and curing for 5 days in the environment of 40 ℃.
When the fluorine-containing self-repairing protective film is used, the fluorine-containing release film of the self-repairing protective film is torn off, the second pressure-sensitive adhesive layer is adhered to the curved surface screen of the curved surface mobile phone, and the upper protective layer is torn off.
Comparative example 1
This comparative example provides a protective film which differs from example 1 in that: the comparative example was not provided with a self-healing layer and the thermoplastic polyurethane elastomer layer had a thickness of 110 μm, and was prepared as follows:
(1) Coating a 50-mu m-thick PET film (base film layer) with glue corresponding to the first pressure-sensitive adhesive layer, baking at 120 ℃ for 2 minutes to obtain a 10-mu m-thick first pressure-sensitive adhesive layer, and coating the first pressure-sensitive adhesive layer with a 50-mu m silicon-based release film (first release film).
(2) Coating a corresponding coating of a thermoplastic polyurethane elastomer layer on a silicon release film (a second release film) with the thickness of 50 mu m, baking at 120 ℃ for 2 minutes to obtain a thermoplastic polyurethane elastomer layer with the thickness of 110 mu m, tearing off the first release film on the first pressure-sensitive adhesive layer, and bonding the thermoplastic polyurethane elastomer layer by using the first pressure-sensitive adhesive layer.
(3) And (3) tearing the second release film on the thermoplastic polyurethane elastomer layer, coating glue corresponding to the second pressure-sensitive layer on the thermoplastic polyurethane elastomer layer, baking at 150 ℃ for 2 minutes to obtain a second pressure-sensitive adhesive layer with the thickness of 15 mu m, and coating the second pressure-sensitive adhesive layer with a fluorine release film (release film layer).
When the protective film is used, the fluorine release film of the protective film is torn off, the second pressure-sensitive adhesive layer is adhered to the curved surface screen of the curved surface mobile phone, and the upper protective layer is torn off.
Comparative example 2
This comparative example provides a protective film which differs from example 1 in that: the comparative example was not provided with a thermoplastic polyurethane elastomer layer and the thickness of the self-healing layer was 110 μm, and the specific preparation method was as follows:
(1) Coating a 50-mu m-thick PET film (base film layer) with glue corresponding to the first pressure-sensitive adhesive layer, baking at 120 ℃ for 2 minutes to obtain a 10-mu m-thick first pressure-sensitive adhesive layer, and coating the first pressure-sensitive adhesive layer with a 50-mu m silicon-based release film (first release film).
(2) A self-repairing paint was applied to a 50 μm thick silicon-based release film (second release film), baked at 115℃for 2 minutes, and baked at 1000mJ/cm 2 To give a 110 μm thick self-healing layer under UV energy.
(3) And tearing off the first release film on the first pressure-sensitive adhesive layer, attaching the self-repairing layer by using the first pressure-sensitive adhesive layer, and curing for 5 days in the environment of 40 ℃.
(4) And (3) tearing off the second release film on the self-repairing coating, coating glue corresponding to the second pressure-sensitive layer on the self-repairing coating, baking at 150 ℃ for 2 minutes to obtain a second pressure-sensitive adhesive layer with the thickness of 15 mu m, and coating the second pressure-sensitive adhesive layer with a fluorine release film (release film layer).
When the protective film is used, the fluorine release film of the protective film is torn off, the second pressure-sensitive adhesive layer is adhered to the curved surface screen of the curved surface mobile phone, and the upper protective layer is torn off.
Comparative example 3
This comparative example provides a protective film which differs from example 1 in that: the self-healing layer of this comparative example was free of added acrylic ester to the material components of the self-healing coating, and the weight part of ketone-aldehyde resin was 110 weight parts.
Comparative example 4
This comparative example provides a protective film which differs from example 1 in that: the self-healing layer of this comparative example was free of hydroxyl polyester added to the material components of the corresponding self-healing coating.
Comparative example 5
This comparative example provides a protective film which differs from example 1 in that: the self-repairing layer of the comparative example was free of slip agent corresponding to the material components of the self-repairing coating.
Performance detection and detection method
1. Offset test:
the specific method comprises the following steps: the protective film is attached to TP glass (AF screen, water drop angle is more than 110+/-5 degrees), the upper protective layer is removed, the Mitsubishi HB pencil lead is cut into a cylinder with the length of 5mm and is ground to be flat on 400-mesh sand paper, the cylindrical Mitsubishi HB pencil lead is mounted on a pencil hardness tester, a load of 200g is applied on the pencil hardness tester, the included angle between the pencil and the surface of the protective film is 45 degrees, the pencil is pushed to slide forwards at a constant speed for about 5mm at a position to be tested, and 5 pens are marked at different positions. And if the surface of the protective film has no scratch or the scratch can be recovered within 60 seconds, the protective film is judged to be qualified (OK), and otherwise, the protective film is judged to be unqualified (NG).
2. AF peel force test:
the specific method comprises the following steps: cutting the protective film into test pieces with the width of 25mm plus or minus 1mm and the length of about 200mm, longitudinally adhering the test pieces to the middle position of TP glass (AF screen, water drop angle of more than 110 plus or minus 5 degrees) in parallel, rolling the test pieces on the TP glass back and forth three times at the speed of about 300mm/min by using a rolling device (the test pieces are adhered to the TP glass without bubbles and wrinkles), removing the upper protective layer, then standing the test pieces in a test environment for 20min, testing the test pieces by using a tensile and pressure tester at the speed of 300mm/min, recording stripping force data, continuously repeating the test for 5 times, and taking the average value.
3. Upper layer self-separation test:
the specific method comprises the following steps: and (3) attaching a protective film on TP glass (AF screen, water drop angle is more than 110+/-5 ℃), observing and recording the bouncing time of the upper protective layer at the cambered surface of the TP glass, and judging to be qualified (OK) if the bouncing time is less than 3 seconds, otherwise, judging to be unqualified (NG).
4. Copper brush test (self-healing ability):
the specific method comprises the following steps: a special copper brush (OSAKA JAPAN OK copper brush in Japan, brush head is 4*6 groups of brush hairs) is arranged on a wear-resisting instrument, a force of 500gf is applied in the vertical direction, the surface of the protective film is rubbed for 20 times (test frequency: 35-50 times per minute, 30-50mm is formed), the edge of the protective film is avoided during friction, the number of scratches in 60s is less than or equal to 5, and the number of scratches is qualified (OK), otherwise, the surface is judged to be unqualified (NG).
5. High temperature and high humidity test:
the specific method comprises the following steps: the protective film is stuck on TP glass (AF screen, water drop angle > 110+ -5 DEG), the upper protective layer is removed, then the protective film is placed in a constant temperature and humidity test box with the temperature of 60+ -2 ℃ and the humidity of 90+ -2%RH for 72 hours, and after being taken out, the protective film is kept stand for 12 hours at normal temperature (25+ -5 ℃ and 65+ -10%RH), and then the appearance of the protective film is observed. The surface of the protective film is judged to be qualified (OK) without any phenomena such as discoloration, cracking, layering, degumming, bubbles or cambered surface tilting, otherwise, the surface is judged to be unqualified (NG) without any phenomena such as discoloration, cracking, layering, degumming, bubbles or cambered surface tilting.
6. Cosmetic adsorption test:
the protective film is stuck on TP glass (AF screen, drop angle > 110+ -5 DEG), the upper protective layer is removed, cosmetic (LIDAAL brand blush) is dipped by cosmetic cotton and is uniformly smeared on the protective film, the protective film is kept stand for 1 hour and is wiped by dust-free cloth for 5 times, the qualified (OK) is judged after the clean cloth is visually and obviously remained, and otherwise, the unqualified (NG) is judged.
7. Dust adsorption test:
and (3) carrying out friction test on the surface of a sample for 50 times by using a new felt (EMPA 701 white) with 15mm in size, loading 500gf, taking a photograph and recording at a distance of 10-15cm from a test position after the test, pressurizing and blowing the test area for 2 times by using VSG010302 integrated air blowing at a position of 15cm above the test position, checking the state of residual wool on the surface, and judging whether the sample is qualified (OK) or not by visual observation without obvious residues from a distance of 10-15cm from the test sample, otherwise, judging whether the sample is unqualified (NG).
Table 1 test results
The test results of comparative example 1 and comparative example 1 show that the protective film of comparative example 1 has no self-repairing layer, and the thermoplastic polyurethane elastomer has good restorability, but has poor hardness, off-grade NG in offset and copper brush tests, low water contact angle of thermoplastic polyurethane, large upper protective stripping force data, inability of attaching curved-surface mobile phones to realize upper protective self-separating function, off-grade NG in cosmetic adsorption test and dust adsorption test.
The test results of comparative example 1 and comparative example 2, the protective film of comparative example 2 was free of a thermoplastic polyurethane elastomer layer, and in the offset test, the offset test was recovered slowly, and the offset test failed NG.
According to the test results of the comparative examples 1 and 3, the self-repairing component of the comparative example 3 is not added with acrylic ester, the content of ketone-aldehyde resin is increased, the ketone-aldehyde resin has carbonyl groups in a molecular structure, terminal groups are hydroxyl groups, and the ketone-aldehyde resin has good compatibility with the self-repairing resin, so that the initial drying property, the chemical resistance and the weather resistance of the self-repairing coating can be effectively improved, the ketone-aldehyde resin does not participate in the chemical crosslinking process of film formation in the self-repairing coating, but is only used as a physical film forming material, acrylic ester directly participates in the chemical crosslinking in the thermal-photo curing process of the self-repairing layer, the self-repairing layer is endowed with higher hardness, and the addition of excessive ketone-aldehyde resin and the non-addition of acrylic ester can influence the hardness of the self-repairing layer, so that offset test and copper brush test NG are caused.
The results of the tests of comparative example 1 and comparative example 4, the self-healing layer composition of comparative example 4 did not contain hydroxyl polyesters, which would increase the strength and toughness of the self-healing layer.
The test results of comparative examples 1 and 5, the self-healing layer of comparative example 5 contained no slipping agent, the water contact angle of the self-healing layer was reduced, and the increase in the upper holding tearing force resulted in unacceptable NG of the upper holding self-separation test, cosmetic adsorption test, and dust adsorption test.
In summary, the self-repairing coating, the electronic screen protective film and the preparation method of the self-repairing coating, provided by the embodiment of the application, have the advantages of good offset printing, excellent self-repairing capability, capability of ensuring the self-repairing effect for a long time and capability of being used under extreme conditions.
The foregoing is merely exemplary embodiments of the present application and is not intended to limit the scope of the present application, and various modifications and variations may be suggested to one skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (10)
1. The self-repairing coating is characterized by comprising the following components in parts by weight:
2. the self-healing coating according to claim 1, wherein the linear aliphatic polycarbonate polyol is a polymer containing repeating carbonate groups in the molecular main chain and hydroxyl groups at the chain ends, selected from Covestro Desmophen C, covestro Desmophen C1200, desmophen C2200, desmophen C2100, asahi chemical "Duozhen Lei" from Kogyo Polymer Co., ltd TM At least one of.
3. The self-healing coating according to claim 1, wherein the hydroxyl polyester is obtained by dehydration esterification of a dibasic acid with an excess of a polyol, and is selected from at least one of H101, H103, H104 of the HyPer H10 series of Desmophen 670BA, desmophen 651MPA/X, of kosmocase polymers limited.
4. The self-healing coating according to claim 1, wherein the dual-cure resin is a modified urethane acrylate, optionally at least one of 1831A, 1443 of guangdongdingmbh, D-039 of tri-chemical industry limited, everstate, HUV-201A of avionics material limited, and dual-stage cure coating DHC-92L of guangzhou tetrahedral new materials technology limited.
5. The self-repairing paint according to claim 1, wherein the acrylic acid ester is at least one of a-NOD-N, A-HD-N,1, 4-cyclohexanedimethanol diacrylate, polyethylene glycol diacrylate, ethoxylated trimethylolpropane triacrylate, caprolactone acrylate of new middle village chemical industry co;
and/or, the ketone-aldehyde resin is KR-1021 of An Feng technical Co., ltd;
and/or the aliphatic isocyanate is at least one of isophorone diisocyanate, hexamethylene diisocyanate, 4' -diisocyanate, methylcyclohexane diisocyanate, trimethylhexamethylene diisocyanate and xylylene diisocyanate;
and/or, the free radical photoinitiator is a benzophenone derivative;
and/or, the non-organotin catalyst is at least one of TMG 160, TMG 720, TMG 634, TMG 612 and TMG 330 of Shanghai Mannheim chemical industry Co., ltd;
and/or the slip agent is a silicone acrylate, optionally winning digao TEGO Rad2250;
and/or the solvent is at least one of methyl isobutyl ketone, ethyl acetate, methyl acetate, propyl acetate, methyl isobutyl ketone, toluene, xylene, cyclohexane, 120# solvent, cyclohexanone and isopropanol.
6. The utility model provides an electronic screen protection film which characterized in that, it includes that top-down stacks in proper order sets up: the self-repairing coating comprises a base film layer, a first pressure-sensitive adhesive layer, a self-repairing layer, a thermoplastic polyurethane elastomer layer, a second pressure-sensitive adhesive layer and a release film layer, wherein the self-repairing layer is obtained by coating, thermally curing and ultraviolet curing the self-repairing coating according to any one of claims 1 to 5.
7. The electronic screen protective film according to claim 6, wherein the components of the first pressure-sensitive adhesive layer corresponding to the glue include, in parts by weight:
and/or the second pressure-sensitive adhesive layer comprises the following components in parts by weight:
8. a method for producing the protective film for electronic screen according to claim 6 or 7, comprising the steps of:
a first pressure-sensitive adhesive layer is arranged on the base film layer;
and the two sides of the thermoplastic polyurethane elastomer layer are respectively provided with a self-repairing layer, a second pressure-sensitive adhesive layer and a release film layer, so that the first pressure-sensitive adhesive layer and the self-repairing layer are laminated and compounded together.
9. The method for manufacturing an electronic screen protective film according to claim 8, comprising the steps of:
coating glue corresponding to the first pressure-sensitive adhesive layer on the base film layer, thermally curing to obtain the first pressure-sensitive adhesive layer, and coating the first pressure-sensitive adhesive layer with a first release film;
coating a coating corresponding to the thermoplastic polyurethane elastomer layer on the second release film, thermally curing to obtain the thermoplastic polyurethane elastomer layer, and coating the thermoplastic polyurethane elastomer layer with a third release film;
tearing off the second release film on the thermoplastic polyurethane elastomer layer, coating a layer of self-repairing coating on the thermoplastic polyurethane elastomer layer, and obtaining a self-repairing layer through heat curing and ultraviolet curing;
tearing off the first release film on the first pressure-sensitive adhesive layer, and coating and curing the self-repairing layer by using the first pressure-sensitive adhesive layer;
tearing off the third release film on the thermoplastic polyurethane elastomer layer, coating a layer of glue corresponding to the second pressure-sensitive layer on the thermoplastic polyurethane elastomer layer, thermally curing to obtain a second pressure-sensitive adhesive layer, and coating the second pressure-sensitive adhesive layer with the release film layer;
or alternatively, the process may be performed,
coating glue corresponding to the first pressure-sensitive adhesive layer on the base film layer, thermally curing to obtain the first pressure-sensitive adhesive layer, and coating the first pressure-sensitive adhesive layer with a first release film;
coating a coating corresponding to the thermoplastic polyurethane elastomer layer on the second release film, thermally curing to obtain the thermoplastic polyurethane elastomer layer, and coating the thermoplastic polyurethane elastomer layer with a third release film;
and tearing off the third release film on the thermoplastic polyurethane elastomer layer, coating a layer of glue corresponding to the second pressure-sensitive layer on the thermoplastic polyurethane elastomer layer, thermally curing to obtain a second pressure-sensitive adhesive layer, and coating the second pressure-sensitive adhesive layer with the release film layer.
Tearing off the second release film on the thermoplastic polyurethane elastomer layer, coating a layer of self-repairing coating on the thermoplastic polyurethane elastomer layer, and obtaining a self-repairing layer through heat curing and ultraviolet curing;
and tearing off the first release film on the first pressure-sensitive adhesive layer, and coating and curing the self-repairing layer by using the first pressure-sensitive adhesive layer.
10. The method for producing an electronic screen protective film according to claim 9, wherein the heat curing temperature is 110-155 ℃, and the energy of the ultraviolet light curing is 1000-2000mJ/cm 2 ；
And/or coating in a doctor blade coating or slot coating mode in all steps.
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