WO2021213114A1 - 一种3d曲面屏防指纹tpu保护膜及其制备方法 - Google Patents

一种3d曲面屏防指纹tpu保护膜及其制备方法 Download PDF

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WO2021213114A1
WO2021213114A1 PCT/CN2021/082269 CN2021082269W WO2021213114A1 WO 2021213114 A1 WO2021213114 A1 WO 2021213114A1 CN 2021082269 W CN2021082269 W CN 2021082269W WO 2021213114 A1 WO2021213114 A1 WO 2021213114A1
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fingerprint
optical
tpu
protective film
curved screen
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PCT/CN2021/082269
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English (en)
French (fr)
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薛萌
丁敬德
庄永剑
朱丽萍
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广东邦固薄膜涂料创新研究院有限公司
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Publication of WO2021213114A1 publication Critical patent/WO2021213114A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
    • C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203—Polyhydroxy compounds
    • C08G18/3206—Polyhydroxy compounds aliphatic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
    • C08G18/4269—Lactones
    • C08G18/4277—Caprolactone and/or substituted caprolactone
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/44—Polycarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633—Compounds of group C08G18/42
    • C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/756—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a tertiary carbon atom of the cycloaliphatic ring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
    • 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
    • C09D175/14—Polyurethanes having 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • 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
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38—Pressure-sensitive adhesives [PSA]
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • C08J2375/06—Polyurethanes from 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
    • C09J2467/00—Presence of polyester
    • 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
    • C09J2475/006—Presence of polyurethane in the substrate

Definitions

  • This application relates to the technical field of screen protective films, and in particular to a 3D curved screen anti-fingerprint TPU protective film and a preparation method thereof.
  • the curvature of the 3D curved screen is getting larger and larger, and the traditional PET, PC, TAC, PMMA base film and the composite film with TPU cannot be attached to the 3D curved screen. Only pure TPU film can be bent arbitrarily on the curved screen without bursting. At present, most of the TPU films on the market are made by the casting method. The TPU films formed by this method are lacking in flatness and light transmittance, and the softness and hardness of the TPU films are difficult to match.
  • the screen protector mentioned in the patent CN110202901A uses a commercially available TPU base film
  • the mobile phone protection film mentioned in the patent CN110484156A uses a melt coating method made of TPU film and PET film combined by OCA glue , The process is complicated.
  • the existing mobile phone protective film puts forward higher requirements on the surface smoothness, scratch resistance, wear resistance, anti-fingerprint and other properties.
  • Flat screens generally use UV curing coatings to harden the surface of the protective film, but ordinary UV Cured coatings tend to burst when bent.
  • the surface of the 3D curved screen is generally treated with anti-fingerprints, and the water contact angle reaches 110-120°.
  • the surface energy of the 3D curved screen after anti-fingerprint treatment is lower.
  • the traditional protective film uses silicone pressure sensitive adhesive or acrylic Pressure-sensitive adhesives have relatively low adhesion, and it is difficult to stick firmly to the screen, and the curved surface is prone to rebound and warp after being attached to the mobile phone screen.
  • the main purpose of this application is to provide an anti-fingerprint TPU protective film for a 3D curved screen and a preparation method thereof, which has the advantages of anti-fingerprint, scratch-resistant, non-explosive and good fit of the curved screen.
  • the present application provides a 3D curved screen anti-fingerprint TPU protective film, which includes a top-down laminated low-viscosity protective film, and an anti-fingerprint UV hardened coating coated with an anti-fingerprint UV hardening coating.
  • the anti-fingerprint UV hardening coating components include: 100 parts by weight of UV prepolymer resin, 5-40 parts by weight of acrylate reactive diluent, 1-5 parts by weight of photoinitiator, 1-10 parts by weight of cool Slip aid, 100-180 parts by weight of the first solvent;
  • the optical grade hard TPU glue is formed by polymerizing polyisocyanate, polyester polyol and chain extender in a second solvent through the action of a first catalyst;
  • the optical-grade high-viscosity silica gel pressure-sensitive adhesive consists of 100 parts by weight of silica gel resin, 0.1-2 parts by weight of cross-linking agent, 0.1-1 parts by weight of anchoring agent, and 0.1-3 parts by weight of second catalyst.
  • the thickness of the low-viscosity protective film is 20-60 ⁇ m; the thickness of the anti-fingerprint UV hardening coating is 3-10 ⁇ m; the thickness of the optical-grade hard TPU resin film layer is 50-200 ⁇ m; The thickness of the optical-grade high-viscosity silicone pressure-sensitive adhesive layer is 25-50 ⁇ m.
  • the low-viscosity protective film is a low-peel force protective film of PE, PP or PET substrate.
  • the UV prepolymer resin is urethane acrylate, especially one or more of aliphatic urethane acrylate;
  • the acrylate reactive diluent is isooctyl acrylate, lauryl acrylate, iso-methacrylate One or more of borneol ester, 1,6-hexanediol diacrylate, and tripropylene glycol diacrylate;
  • the photoinitiator is 1-hydroxy-cyclohexyl benzophenone, 2,4,6-tri One or more of methylbenzoyl-diphenylphosphine oxide and 2-hydroxy-2-methyl-phenylacetone-1;
  • the slip aid is fluorine-containing acrylate and silicon-containing acrylate One or more of fluorosilicone acrylate;
  • the first solvent is one or more of ethyl acetate, n-butyl acetate, toluene, propylene glycol methyl ether acetate, and
  • the polyisocyanate is one or more of hexamethylene diisocyanate or its polymer, isophorone diisocyanate or its polymer;
  • the polyester polyol is a conventional polyester polyol One or more of alcohol, polycaprolactone polyol and polycarbonate diol;
  • the chain extender is ethylene glycol, 1,4-butanediol, 1,6-hexanediol, glycerin, tri One or more of methylolpropane;
  • the first catalyst is dibutyltin dilaurate;
  • the second solvent is ethyl acetate, toluene, butanone, N,N-dimethylformamide One or more.
  • the silicone resin is vinyl-terminated polydimethylsiloxane and MQ methyl silicone resin;
  • the crosslinking agent is hydrogen-based silicone oil;
  • the anchoring agent is a silane coupling agent;
  • the second The catalyst is a platinum catalyst with a concentration of 5000 ppm.
  • a method for preparing the above-mentioned 3D curved screen anti-fingerprint TPU protective film which is characterized in that the steps of the preparation method are as follows:
  • the coating is performed by knife coating or slit coating.
  • the prepared 3D curved screen anti-fingerprint TPU protective film has a light transmittance of greater than 91%, a haze of less than 1%, a water contact angle of 108° or more, and a dynamic friction coefficient of ⁇ 0.15.
  • TPU material As the base film, it has good optical performance, no rainbow pattern, interference pattern, and will not affect the fingerprint unlocking function under the light-sensitive screen.
  • the commercially available cast TPU base film is not used in this application.
  • This base film is relatively soft, and it is difficult to increase the smoothness of the surface coating in the later stage.
  • optical-grade hard TPU glue is synthesized first, and then the TPU base film is coated with a coater.
  • the single-layer base film has a relatively simple structure, does not require a hot bending process, and has low preparation cost; and the thickness is adjustable, the hardness of the film material is adjustable, the surface flatness is high, the film material thickness is uniform, and flexibility and curved surface are taken into account. Screen fit.
  • One side of the protective film attached to the 3D curved screen is coated with optical-grade high-viscosity silicone pressure-sensitive glue, which can make the protective film and the 3D curved screen with anti-fingerprint treatment stronger, and solve the problem that the conventional glue is easy to be in the arc after the 3D curved screen is attached.
  • the problem of surface rebound and warping; and the self-draining performance of using silicone pressure-sensitive adhesive on the surface of the screen is better.
  • the surface of the protective film is coated with anti-fingerprint UV hardening coating, which solves the problem that the TPU base film is not scratch resistant when used alone.
  • the UV prepolymer resin and acrylate reactive diluent with better flexibility are specially selected to keep the cured UV hardening coating to a certain extent. Its flexibility and tensile strength will not burst when the edge of the screen is curved.
  • the slip additives added to the UV hardening coating can make the outer surface of the protective film have good anti-fouling ability and anti-fingerprint performance.
  • the water contact angle can reach 108° or more, and the dynamic friction coefficient is less than 0.15 to achieve better sliding operation. Touch.
  • the preparation method is simple and easy to implement, and can quickly produce 3D curved screen self-repairing TPU protective film products with good protection effect and good comprehensive performance, and high production efficiency.
  • Fingerprint UV hardening coating It is composed of 100 parts by weight of urethane acrylate, 5 parts by weight of isooctyl acrylate, 1 part by weight of 1-hydroxy-cyclohexyl benzophenone, 1 part by weight of fluorine-containing acrylate, and 100 parts by weight of ethyl acetate. Fingerprint UV hardening coating;
  • the anti-fingerprint UV hardened coating is covered with a low-viscosity protective film of a PET substrate with a thickness of 25 ⁇ m, and cured at room temperature for 24 hours to obtain a 3D curved screen anti-fingerprint TPU protective film.
  • 100 parts by weight of polydimethylsiloxane, 2 parts by weight of hydrogen-based silicone oil, 1 part by weight of silane coupling agent, and 3 parts by weight of platinum catalyst with a concentration of 5000ppm are composed of optical-grade high-viscosity silica gel pressure-sensitive glue;
  • the anti-fingerprint UV hardened coating is covered with a low-viscosity protective film of a PET substrate with a thickness of 50 ⁇ m, and cured at room temperature for 24 hours to obtain a 3D curved screen anti-fingerprint TPU protective film.
  • Fingerprint UV hardening coating It is composed of 100 parts by weight of urethane acrylate, 5 parts by weight of isooctyl acrylate, 1 part by weight of 1-hydroxy-cyclohexyl benzophenone, 1 part by weight of fluorine-containing acrylate, and 100 parts by weight of ethyl acetate. Fingerprint UV hardening coating;
  • the anti-fingerprint UV hardened coating is covered with a low-viscosity protective film of a PET substrate with a thickness of 50 ⁇ m, and cured at room temperature for 24 hours to obtain a 3D curved screen anti-fingerprint TPU protective film.
  • 100 parts by weight of polydimethylsiloxane, 2 parts by weight of hydrogen-based silicone oil, 1 part by weight of silane coupling agent, and 3 parts by weight of platinum catalyst with a concentration of 5000ppm are composed of optical-grade high-viscosity silicone pressure-sensitive adhesive;
  • the anti-fingerprint UV hardened coating is covered with a low-viscosity protective film of a PET substrate with a thickness of 38 ⁇ m, and cured at room temperature for 24 hours to obtain a 3D curved screen anti-fingerprint TPU protective film.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Laminated Bodies (AREA)
  • Adhesive Tapes (AREA)

Abstract

一种3D曲面屏防指纹TPU保护膜，包括自上而下贴合的低粘保护膜、由防指纹UV硬化涂料涂布而成的防指纹UV硬化涂层、由光学级硬质TPU胶水涂布而成的光学级硬质TPU树脂膜层、由光学级高粘性硅胶压敏胶水涂布而成的光学级高粘性硅胶压敏胶层及氟素离型膜；防指纹UV硬化涂料组分包括：UV预聚体树脂、丙烯酸酯活性稀释剂、光引发剂、爽滑助剂、第一溶剂；光学级硬质TPU胶水由多异氰酸酯、聚酯多元醇和扩链剂通过第一催化剂的作用在第二溶剂中聚合而成；光学级高粘性硅胶压敏胶水由硅胶树脂、交联剂、锚固剂、第二催化剂组成。该3D曲面屏防指纹TPU保护膜具有防指纹、耐刮花、不易爆裂及曲面屏贴合性好的性能。

Description

一种3D曲面屏防指纹TPU保护膜及其制备方法 技术领域
本申请涉及屏幕保护膜的技术领域，特别涉及一种3D曲面屏防指纹TPU保护膜及其制备方法。
背景技术
现有智能手机已由直板触屏进入曲面屏、折叠屏时代，触摸屏对屏幕防摔碎和刮花等指标需求较为严格，而当屏幕变为曲面屏或折叠屏后，对于屏幕保护膜的性能也提出了更高的要求。
3D曲面屏的弯曲弧度越来越大，传统的PET、PC、TAC、PMMA基膜及与TPU的复合膜都无法与3D曲面屏很好的附贴。只有纯粹的TPU膜才有可能在曲面屏上做到任意弯曲而不爆裂。而目前市面上的TPU膜大多是通过流延法做出的，该方法成型的TPU膜在平整度和透光率方面有所欠缺，且TPU膜的软硬度很难匹配。如专利CN110202901A中提到的屏幕保护贴采用的是市售的TPU基膜，而专利CN110484156A中提到的手机保护膜采用的是熔融涂布法制成的TPU膜和PET膜通过OCA胶水复合而成，工艺复杂。
并且，现有手机保护膜对表面的爽滑、耐刮、耐磨、防指纹等性能提出了更高的要求，平面屏一般采用UV固化涂料对保护膜的表面进行硬化处理，但普通的UV固化涂料容易在弯曲时爆裂。
再者，3D曲面屏的表面一般都做了防指纹处理，水接触角达到110～120°，防指纹处理后的3D曲面屏的表面能较低，传统保护膜用的硅胶压敏胶或者丙烯酸压敏胶粘着力都比较低，很难与屏幕 贴得牢，贴合手机屏后容易出现弧面反弹起翘的现象。
为此，我们提出了一种3D曲面屏防指纹TPU保护膜及其制备方法。
申请内容
本申请的主要目的在于提供一种3D曲面屏防指纹TPU保护膜及其制备方法，具有防指纹、耐刮花、不易爆裂及曲面屏贴合性好的优点。
为实现上述目的，本申请提供了一种3D曲面屏防指纹TPU保护膜，包括自上而下贴合的低粘保护膜、由防指纹UV硬化涂料涂布而成的防指纹UV硬化涂层、由光学级硬质TPU胶水涂布而成的光学级硬质TPU树脂膜层、由光学级高粘性硅胶压敏胶水涂布而成的光学级高粘性硅胶压敏胶层及氟素离型膜；
所述防指纹UV硬化涂料组分包括：100重量份的UV预聚体树脂、5～40重量份的丙烯酸酯活性稀释剂、1～5重量份的光引发剂、1～10重量份的爽滑助剂、100～180重量份的第一溶剂；
所述光学级硬质TPU胶水由多异氰酸酯、聚酯多元醇和扩链剂通过第一催化剂的作用在第二溶剂中聚合而成；
所述光学级高粘性硅胶压敏胶水由100重量份硅胶树脂、0.1～2重量份交联剂、0.1～1重量份锚固剂、0.1～3重量份第二催化剂组成。
优选的，所述低粘保护膜的厚度为20～60μm；所述防指纹UV硬化涂层的厚度为3～10μm；所述光学级硬质TPU树脂膜层的厚度为50～200μm；所述光学级高粘性硅胶压敏胶层的厚度为25～50 μm。
优选的，所述低粘保护膜为PE、PP或PET基材的低剥离力保护膜。
优选的，所述UV预聚体树脂为聚氨酯丙烯酸酯，特指脂肪族聚氨酯丙烯酯的一种或几种；所述丙烯酸酯活性稀释剂为丙烯酸异辛酯、丙烯酸月桂酯、甲基丙烯酸异冰片酯、1,6-己二醇二丙烯酸酯、三丙二醇二丙烯酸酯中的一种或几种；所述光引发剂为1-羟基-环己基苯甲酮、2,4,6-三甲基苯甲酰基-二苯基氧化膦、2-羟基-2-甲基-苯基丙酮-1中的一种或几种；所述爽滑助剂为含氟丙烯酸酯、含硅丙烯酸酯、氟硅丙烯酸酯中的一种或几种；所述第一溶剂为乙酸乙酯、乙酸正丁酯、甲苯、丙二醇甲醚醋酸酯、丁酮中的一种或几种。
优选的，所述多异氰酸酯为六亚甲基二异氰酸酯或其多聚体、异佛尔酮二异氰酸酯或其多聚体中的一种或几种；所述聚酯多元醇为常规聚酯多元醇、聚己内酯多元醇和聚碳酸酯二醇中的一种或几种；所述扩链剂为乙二醇、1,4-丁二醇、1,6-己二醇、甘油、三羟甲基丙烷中的一种或几种；所述第一催化剂为二月桂酸二丁基锡；所述第二溶剂为乙酸乙酯、甲苯、丁酮、N,N-二甲基甲酰胺中的一种或几种。
优选的，所述硅胶树脂为乙烯基封端的聚二甲基硅氧烷和MQ甲基硅树脂；所述交联剂为氢基硅油；所述锚固剂为硅烷偶联剂；所述第二催化剂为5000ppm浓度的铂金催化剂。
一种如上述的3D曲面屏防指纹TPU保护膜的制备方法，其特 征在于，制备方法步骤如下：
(1)将光学级硬质TPU胶水涂布在PET离型膜上，在90-120℃温度下烘干后固化后形成光学级硬质TPU树脂膜层；
(2)将光学级高粘性硅胶压敏胶水涂布于所述光学级硬质TPU树脂膜层上，在120-150℃温度下烘干后固化后形成光学级高粘性硅胶压敏胶层，再在胶层表面覆盖氟素离型膜；
(3)撕掉PET离型膜，将防指纹UV硬化涂料涂布于光学级硬质TPU树脂膜层的另一面，在90-120℃温度下烘干并经过200～500mj/cm 2能量的UV光固化后形成防指纹UV硬化涂层；
(4)在防指纹UV硬化涂层上覆盖低粘保护膜，在常温下熟化24h，得到3D曲面屏防指纹TPU保护膜。
优选的，采用刮刀涂布或者狭缝涂布的方式进行涂布。
优选的，制得的所述3D曲面屏防指纹TPU保护膜，其透光率大于91％，雾度小于1％，水接触角达到108°以上，动摩擦系数＜0.15。
现有技术相比，本申请具有如下有益效果：
1.采用TPU材质作为基膜，具有较好的光学性能，没有彩虹纹、干涉纹，不会影响光感屏下指纹解锁功能。且本申请中并不采用市售的流延法TPU基膜，这种基膜偏软，后期表面涂层的爽滑度很难做高。而是先合成光学级硬质TPU胶水，再用涂布机涂出该种TPU基膜。该单层基膜的结构比较简单，不需经过热弯工艺，制备成本低；且厚度可调、膜材硬度可调、表面平整度高、膜材厚度均匀性好，兼顾了柔韧性和曲面屏贴合性。
2.保护膜贴3D曲面屏的一面涂覆光学级高粘性硅胶压敏胶水，可使得保护膜与做过防指纹处理的3D曲面屏更加牢固，解决常规胶水贴合3D曲面屏后容易在弧面反弹起翘的问题；且使用硅胶压敏胶水在屏幕表面的自排泡性能较好。
3.保护膜表面涂覆防指纹UV硬化涂料，解决了TPU基膜在单独使用时不耐刮花的问题。为了使保护膜在贴3D曲面屏时能够弯曲，在制备UV硬化涂料时，特意选择了柔韧性较好的UV预聚体树脂和丙烯酸酯活性稀释剂，使固化后的UV硬化涂料保持有一定的柔韧性和拉伸强度，在贴屏边缘弧度弯曲时不会爆裂。另外UV硬化涂料中添加的爽滑助剂可使保护膜的外表面具有很好的抗污能力、防指纹性能，水接触角达到108°以上，动摩擦系数＜0.15，来取得较佳的滑动操作触感。
4.该制备方法简洁、易实现，能快速生产出保护效果好、综合性能佳的3D曲面屏自修复TPU保护膜产品，生产效率高。
具体实施方式
为使本申请实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施方式，进一步阐述本申请。
实施例1
由100重量份的聚氨酯丙烯酸酯、5重量份的丙烯酸异辛酯、1重量份的1-羟基-环己基苯甲酮、1重量份的含氟丙烯酸酯、100重量份的乙酸乙酯组成防指纹UV硬化涂料；
由六亚甲基二异氰酸酯、聚己内酯多元醇、乙二醇按摩尔比1：0.8：0.2混合并通过二月桂酸二丁基锡的催化作用在乙酸乙酯溶剂 中聚合形成光学级硬质TPU胶水；
由100重量份MQ甲基硅树脂、0.1重量份氢基硅油、0.1重量份硅烷偶联剂、0.1重量份5000ppm浓度的铂金催化剂组成光学级高粘性硅胶压敏胶水；
将光学级硬质TPU胶水涂布在PET离型膜上，涂布厚度为50μm，在90-120℃温度下烘干后固化后形成光学级硬质TPU树脂膜层；
将光学级高粘性硅胶压敏胶水涂布于光学级硬质TPU树脂膜层上，涂布厚度为30μm，在120-150℃温度下烘干后固化后形成光学级高粘性硅胶压敏胶层，再在胶层表面覆盖氟素离型膜；
撕掉PET离型膜，将防指纹UV硬化涂料涂布于光学级硬质TPU树脂膜层的另一面，涂布厚度为3μm，在90-120℃温度下烘干并经过200mj/cm2能量的UV光固化后形成防指纹UV硬化涂层；
在防指纹UV硬化涂层上覆盖厚度为25μm的PET基材的低粘保护膜，在常温下熟化24h，得到3D曲面屏防指纹TPU保护膜。
实施例2
由100重量份的聚氨酯丙烯酸酯、40重量份的丙烯酸月桂酯、5重量份的2-羟基-2-甲基-苯基丙酮-1、10重量份的含硅丙烯酸酯、180重量份的丙二醇甲醚醋酸酯组成防指纹UV硬化涂料；
由异佛尔酮二异氰酸酯、聚碳酸酯二醇、1,4-丁二醇按摩尔比1：0.85：0.15混合并通过二月桂酸二丁基锡的催化作用在甲苯溶剂中聚合形成光学级硬质TPU胶水；
由100重量份聚二甲基硅氧烷、2重量份氢基硅油、1重量份 硅烷偶联剂、3重量份5000ppm浓度的铂金催化剂组成光学级高粘性硅胶压敏胶水；
将光学级硬质TPU胶水涂布在PET离型膜上，涂布厚度为50μm，在90-120℃温度下烘干后固化后形成光学级硬质TPU树脂膜层；
将光学级高粘性硅胶压敏胶水涂布于光学级硬质TPU树脂膜层上，涂布厚度为35μm，在120-150℃温度下烘干后固化后形成光学级高粘性硅胶压敏胶层，再在胶层表面覆盖氟素离型膜；
撕掉PET离型膜，将防指纹UV硬化涂料涂布于光学级硬质TPU树脂膜层的另一面，涂布厚度为3μm，在90-120℃温度下烘干并经过200mj/cm2能量的UV光固化后形成防指纹UV硬化涂层；
在防指纹UV硬化涂层上覆盖厚度为50μm的PET基材的低粘保护膜，在常温下熟化24h，得到3D曲面屏防指纹TPU保护膜。
实施例3
由100重量份的聚氨酯丙烯酸酯、5重量份的丙烯酸异辛酯、1重量份的1-羟基-环己基苯甲酮、1重量份的含氟丙烯酸酯、100重量份的乙酸乙酯组成防指纹UV硬化涂料；
由六亚甲基二异氰酸酯、聚己内酯多元醇、乙二醇按摩尔比1：0.9：0.1混合并通过二月桂酸二丁基锡的催化作用在乙酸乙酯溶剂中聚合形成光学级硬质TPU胶水；
由100重量份MQ甲基硅树脂、0.1重量份氢基硅油、0.1重量份硅烷偶联剂、0.1重量份5000ppm浓度的铂金催化剂组成光学级高粘性硅胶压敏胶水；
将光学级硬质TPU胶水涂布在PET离型膜上，涂布厚度为200μm，在90-120℃温度下烘干后固化后形成光学级硬质TPU树脂膜层；
将光学级高粘性硅胶压敏胶水涂布于光学级硬质TPU树脂膜层上，涂布厚度为50μm，在120-150℃温度下烘干后固化后形成光学级高粘性硅胶压敏胶层，再在胶层表面覆盖氟素离型膜；
撕掉PET离型膜，将防指纹UV硬化涂料涂布于光学级硬质TPU树脂膜层的另一面，涂布厚度为10μm，在90-120℃温度下烘干并经过300mj/cm2能量的UV光固化后形成防指纹UV硬化涂层；
在防指纹UV硬化涂层上覆盖厚度为50μm的PET基材的低粘保护膜，在常温下熟化24h，得到3D曲面屏防指纹TPU保护膜。
实施例4
由100重量份的聚氨酯丙烯酸酯、40重量份的丙烯酸月桂酯、5重量份的2-羟基-2-甲基-苯基丙酮-1、10重量份的含硅丙烯酸酯、180重量份的丙二醇甲醚醋酸酯组成防指纹UV硬化涂料；
由异佛尔酮二异氰酸酯、聚碳酸酯二醇、1,4-丁二醇按摩尔比1：0.92：0.08混合并通过二月桂酸二丁基锡的催化作用在甲苯溶剂中聚合形成光学级硬质TPU胶水；
由100重量份聚二甲基硅氧烷、2重量份氢基硅油、1重量份硅烷偶联剂、3重量份5000ppm浓度的铂金催化剂组成光学级高粘性硅胶压敏胶水；
将光学级硬质TPU胶水涂布在PET离型膜上，涂布厚度为200μm，在90-120℃温度下烘干后固化后形成光学级硬质TPU树脂膜 层；
将光学级高粘性硅胶压敏胶水涂布于光学级硬质TPU树脂膜层上，涂布厚度为50μm，在120-150℃温度下烘干后固化后形成光学级高粘性硅胶压敏胶层，再在胶层表面覆盖氟素离型膜；
撕掉PET离型膜，将防指纹UV硬化涂料涂布于光学级硬质TPU树脂膜层的另一面，涂布厚度为10μm，在90-120℃温度下烘干并经过200mj/cm2能量的UV光固化后形成防指纹UV硬化涂层；
在防指纹UV硬化涂层上覆盖厚度为38μm的PET基材的低粘保护膜，在常温下熟化24h，得到3D曲面屏防指纹TPU保护膜。
下面对实施例1～4制得的3D曲面屏防指纹TPU保护膜进行性能测试，实施例1～4的光学性能测试结果如表1所示：
表1
Figure PCTCN2021082269-appb-000001
结合实施例1～4中的光学性能测试结果，由表1可知，实施例1～4所得3D曲面屏防指纹TPU保护膜透光率大于91％，雾度小 于1％，水接触角达到108°以上，动摩擦系数≤0.15，增加滑动操作触感。
以上显示和描述了本申请的基本原理和主要特征和本申请的优点。本行业的技术人员应该了解，本申请不受上述实施例的限制，上述实施例和说明书中描述的只是说明本申请的原理，在不脱离本申请精神和范围的前提下，本申请还会有各种变化和改进，这些变化和改进都落入要求保护的本申请范围内。本申请要求保护范围由所附的权利要求书及其等效物界定。

Claims (9)

  1. 一种3D曲面屏防指纹TPU保护膜，其特征在于，包括自上而下贴合的低粘保护膜、由防指纹UV硬化涂料涂布而成的防指纹UV硬化涂层、由光学级硬质TPU胶水涂布而成的光学级硬质TPU树脂膜层、由光学级高粘性硅胶压敏胶水涂布而成的光学级高粘性硅胶压敏胶层及氟素离型膜；
    所述防指纹UV硬化涂料组分包括：100重量份的UV预聚体树脂、5～40重量份的丙烯酸酯活性稀释剂、1～5重量份的光引发剂、1～10重量份的爽滑助剂、100～180重量份的第一溶剂；
    所述光学级硬质TPU胶水由多异氰酸酯、聚酯多元醇和扩链剂通过第一催化剂的作用在第二溶剂中聚合而成；
    所述光学级高粘性硅胶压敏胶水由100重量份硅胶树脂、0.1～2重量份交联剂、0.1～1重量份锚固剂、0.1～3重量份第二催化剂组成。
  2. 根据权利要求1所述的3D曲面屏防指纹TPU保护膜，其特征在于，所述低粘保护膜的厚度为20～60μm；所述防指纹UV硬化涂层的厚度为3～10μm；所述光学级硬质TPU树脂膜层的厚度为50～200μm；所述光学级高粘性硅胶压敏胶层的厚度为25～50μm。
  3. 根据权利要求1所述的3D曲面屏防指纹TPU保护膜，其特征在于，所述低粘保护膜为PE、PP或PET基材的低剥离力保护膜。
  4. 根据权利要求1所述的3D曲面屏防指纹TPU保护膜，其特征在于，所述UV预聚体树脂为聚氨酯丙烯酸酯，特指脂肪族聚氨 酯丙烯酯的一种或几种；所述丙烯酸酯活性稀释剂为丙烯酸异辛酯、丙烯酸月桂酯、甲基丙烯酸异冰片酯、1,6-己二醇二丙烯酸酯、三丙二醇二丙烯酸酯中的一种或几种；所述光引发剂为1-羟基-环己基苯甲酮、2,4,6-三甲基苯甲酰基-二苯基氧化膦、2-羟基-2-甲基-苯基丙酮-1中的一种或几种；所述爽滑助剂为含氟丙烯酸酯、含硅丙烯酸酯、氟硅丙烯酸酯中的一种或几种；所述第一溶剂为乙酸乙酯、乙酸正丁酯、甲苯、丙二醇甲醚醋酸酯、丁酮中的一种或几种。
  5. 根据权利要求1所述的3D曲面屏防指纹TPU保护膜，其特征在于，所述多异氰酸酯为六亚甲基二异氰酸酯或其多聚体、异佛尔酮二异氰酸酯或其多聚体中的一种或几种；所述聚酯多元醇为常规聚酯多元醇、聚己内酯多元醇和聚碳酸酯二醇中的一种或几种；所述扩链剂为乙二醇、1,4-丁二醇、1,6-己二醇、甘油、三羟甲基丙烷中的一种或几种；所述第一催化剂为二月桂酸二丁基锡；所述第二溶剂为乙酸乙酯、甲苯、丁酮、N,N-二甲基甲酰胺中的一种或几种。
  6. 根据权利要求1所述的3D曲面屏防指纹TPU保护膜，其特征在于，所述硅胶树脂为乙烯基封端的聚二甲基硅氧烷和MQ甲基硅树脂；所述交联剂为氢基硅油；所述锚固剂为硅烷偶联剂；所述第二催化剂为5000ppm浓度的铂金催化剂。
  7. 一种如权利要求1-6任一项所述3D曲面屏防指纹TPU保护膜的制备方法，其特征在于，制备方法步骤如下：
    (1)将光学级硬质TPU胶水涂布在PET离型膜上，在90-120℃温度下烘干后固化后形成光学级硬质TPU树脂膜层；
    (2)将光学级高粘性硅胶压敏胶水涂布于所述光学级硬质TPU树脂膜层上，在120-150℃温度下烘干后固化后形成光学级高粘性硅胶压敏胶层，再在胶层表面覆盖氟素离型膜；
    (3)撕掉PET离型膜，将防指纹UV硬化涂料涂布于光学级硬质TPU树脂膜层的另一面，在90-120℃温度下烘干并经过200～500mj/cm 2能量的UV光固化后形成防指纹UV硬化涂层；
    (4)在防指纹UV硬化涂层上覆盖低粘保护膜，在常温下熟化24h，得到3D曲面屏防指纹TPU保护膜。
  8. 根据权利要求7所述3D曲面屏防指纹TPU保护膜的制备方法，其特征在于，采用刮刀涂布或者狭缝涂布的方式进行涂布。
  9. 根据权利要求7所述3D曲面屏防指纹TPU保护膜的制备方法，其特征在于，制得的所述3D曲面屏防指纹TPU保护膜，其透光率大于91％，雾度小于1％，水接触角达到108°以上，动摩擦系数＜0.15。
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