WO2022073422A1 - 一种离型膜基材及其制备方法 - Google Patents

一种离型膜基材及其制备方法 Download PDF

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WO2022073422A1
WO2022073422A1 PCT/CN2021/120039 CN2021120039W WO2022073422A1 WO 2022073422 A1 WO2022073422 A1 WO 2022073422A1 CN 2021120039 W CN2021120039 W CN 2021120039W WO 2022073422 A1 WO2022073422 A1 WO 2022073422A1
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layer
parts
weight
release film
release
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PCT/CN2021/120039
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English (en)
French (fr)
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吴培服
王琪
池卫
钱向飞
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江苏双星彩塑新材料股份有限公司
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Publication of WO2022073422A1 publication Critical patent/WO2022073422A1/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
    • 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
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • 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
    • C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/26—Polymeric coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/304—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/54—Yield strength; Tensile strength
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/554—Wear resistance
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/728—Hydrophilic
    • 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
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • 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
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters

Definitions

  • the invention relates to the field of polyester films, in particular to a substrate specially used for release films and a preparation method thereof.
  • Release film also known as peeling film, isolation film, separation film, resist film, etc., refers to a film with separation on the surface.
  • the release film is not tacky, or slightly tacky, after contact with certain materials under limited conditions. Release films are widely used in packaging, printing, silk screen printing, pad printing, nameplates, membrane switches, flexible circuits, insulating products, circuit boards, laser anti-counterfeiting, lamination, electronics, film for sealing materials, reflective materials, waterproof materials , medicine (plaster paper), toilet paper, adhesive products, die-cutting and punching processing and other industries.
  • CN 111393699 A discloses a flame-retardant release film and a preparation method thereof.
  • the release film includes a base film, a release agent, and the release agent includes the following raw materials: organosilicon main polymer, cross-linking agent, catalyst, frame Bridge agent, flame retardant, reflective powder, organic solvent, the flame retardant is a phosphorus-based flame retardant containing alcohol hydroxyl group.
  • the alcoholic hydroxyl group-containing flame retardant is added to the release agent, and the alcoholic hydroxyl group reacts with the isocyanate group in the bridging agent under heating, so that the flame retardant is successfully grafted to a certain bond with the base film.
  • the release agent of the prior art has a flame retardant effect and does not improve the base material of the release film.
  • CN 111394010 A discloses a release film for polarizer.
  • the prior art release agent is calculated in parts by weight, and its preparation raw materials include: 100-125 parts of main agent, 550-900 parts of solvent, 2 parts of coupling agent -5 parts, 10-20 parts of metal catalyst, 4-6 parts of light stabilizer, 10-20 parts of mold release agent, 10-20 parts of polyurethane hot melt adhesive, 5-15 parts of leveling agent, among which the main agent is selected from iso At least one of propoxy trimethyl silane, methyl ethoxy silicone oil, methyl trifluoropropyl silicone oil, and methyl vinyl silicone oil, the coupling agent is selected from silane coupling agents, and the polarizer uses a release type
  • the film has good release effect and good resistance to silicon transfer, which makes the release film for polarizer easier to peel off and prevents the phenomenon of PSA glue being pulled up.
  • the improvement of the prior art also only lies in the release agent, and does not involve the substrate of the release film.
  • CN 111423609 A discloses an essential anti-static release film base film and its application.
  • the material of the anti-static release film base film is modified HDPE, and the modified HDPE includes the following raw materials: alkenyl compounds and double bond-containing Quaternary ammonium salts.
  • an intrinsic antistatic release film base film is prepared by doping a polymerizable quaternary ammonium salt into a high-density polyethylene polymer monomer.
  • the quaternary ammonium salt is an excellent cationic antistatic agent, which is uniformly dispersed in In the resin, a channel is formed to leak electrostatic charge, and the groups with anti-static function will not migrate or stick away, and play an essential anti-static effect.
  • CN 111518472 A discloses an antistatic agent, an antistatic release film and a preparation method thereof.
  • the antistatic release film includes a base film layer and a functional layer, and the functional layer is made of an antistatic agent.
  • the antistatic agent comprises the following components in parts by weight: 0.05-0.5 parts of conductive monomer, 20-40 parts of photocurable organosiloxane resin, 60-80 parts of photo-curable silicone release agent, and 0.05-0.5 part of photoinitiator share.
  • the prior art conductive monomer is preferably vinylmethyloxazolidone.
  • the release film of the prior art has the problem that the release agent and the substrate are not firmly combined and easily detached, which will cause the release agent to remain on the surface of the product when the release film is removed, resulting in a change in the working performance of the product surface. .
  • the technical problem to be solved by the present application is to provide a release film substrate and a preparation method thereof, so as to reduce or avoid the aforementioned problems.
  • the present application proposes a release film base material, comprising a polyester film and an active coating, the active coating is formed on the surface of the polyester film, and the silicone oil release agent is coated on the surface of the active coating.
  • a release agent layer is formed; the active coating contains the following components: acrylic resin, dimethylsilylated silica surfactant, ethanolamine surface erosive agent, polyquaternium salt surface active bactericide, water-insoluble carbonic acid Salt, melamine hardener and propylene glycol solvent.
  • the wash coat comprises 80-100 parts by weight of acrylic resin, 1-2 parts by weight of dimethylsilylated silica, 10-15 parts by weight of ethanolamine, 0.5-0.8 parts by weight of polyquaternium Salt, 5-10 parts by weight of water-insoluble carbonate, 1-2 parts by weight of melamine, and 80-100 parts by weight of propylene glycol.
  • the washcoat has a thickness of 5-10 ⁇ m.
  • the water-insoluble carbonate is calcium carbonate or magnesium carbonate.
  • the particle size of the water-insoluble carbonate is 5-10 ⁇ m.
  • the polyester film is a polyester film with a three-layer co-extrusion composite structure, including a surface layer, a bottom layer and an intermediate layer sandwiched between them, and the active coating is formed on the surface layer of the polyester film and/or the outer surface of the bottom layer.
  • the surface layer and the bottom layer of the polyester film are made of the same polyester material, and the polyesters both contain silica, alkaline earth metal silicate and polydimethylsiloxane.
  • silica aerogel is used as the silica in the surface layer and the bottom layer of the polyester film.
  • the content of silicon dioxide is 0.3 wt % to 1.5 wt %
  • the content of alkaline earth metal silicate is 0.05 wt % to 0.5 wt %
  • the content of polydimethylsiloxane is 0.05 wt % to 0.5 wt %.
  • the content of alkane is 0.2wt% ⁇ 1.2 wt%.
  • the present invention also provides a preparation method of a release film base material, wherein the release film base material comprises a polyester film and an active coating, the active coating is formed on the surface of the polyester film, and the silicone oil is released.
  • the agent is coated on the surface of the active coating to form a release agent layer; the method includes the steps:
  • the precoat is subjected to plasma surface activation treatment
  • the surface activity and hydrophilicity of the release film base material are greatly improved, which is conducive to the close contact with the silicone oil type release agent. Combined, the release agent can be prevented from detaching.
  • FIG. 1 shows a schematic exploded view of the cross-sectional structure of the release film of the present application.
  • the present invention provides an improved release film, specifically an improved release film substrate, the surface of the release film substrate can be coated with a silicone oil release agent, thereby preparing a release film membrane.
  • the release film of the present invention can be applied to packaging, printing, screen printing, pad printing, nameplates, membrane switches, flexible circuits, insulating products, circuit boards, laser anti-counterfeiting, lamination, electronics, films for sealing materials, reflective materials, waterproofing Materials, medicine (plaster paper), toilet paper, adhesive products, die-cutting and punching processing and other industries.
  • the release film substrate 10 of the present invention includes a polyester film 1 and an active coating layer 2, and the polyester film 1 is preferably made of a biaxially oriented PET film, which can be a single layer
  • the structure can also be a multi-layer composite structure.
  • the polyester film 1 of the present invention can be a polyester film with a three-layer co-extrusion composite structure.
  • the polyester film with a three-layer co-extrusion composite structure can include a surface layer 11 , a bottom layer 12 and
  • the washcoat layer 2 is formed on the outer surface of the top layer 11 and/or the bottom layer 12 of the polyester film 1 with the intermediate layer 13 sandwiched therebetween.
  • the release agent is coated on the surface of the active coating 2 to form a release agent layer 3 (shown by the dotted line in the figure, for the sake of clarity, the release agent layer 3 is decomposed and shown).
  • the active coating 2 of the present invention comprises the following components: acrylic resin, dimethylsilylated silica surfactant, ethanolamine surface erosive agent, polyquaternary ammonium salt surface active bactericide, water-insoluble carbonate , melamine curing agent and propylene glycol solvent.
  • the ethanolamine surface etchant can form a certain degradation and erosion on the outer surface of the polyester film 1, reduce the flatness of the outer surface of the polyester film 1, and is conducive to the formation of the hydrophilic component in the active coating 2 and the polyester film 1 Strong bonding; and ethanolamine is easy to decompose gas during the curing process of the coating, which can make the active coating 2 form a fluffy and porous structure.
  • the acrylic resin is hydrophilic, and is further emulsified by the silica dimethylsilylate surfactant, and the silicon-containing surfactant and the polyester film 1 can obtain a strong bonding force.
  • Polyquaternium surface active fungicides can reduce the surface tension of the cured coating surface, improve the adsorption capacity of the coating to the silicone oil release agent, and avoid the release of the release agent.
  • the formulation layer remains in use for a long time.
  • melamine is less sensitive to moisture and has better affinity with silicone oil-based release agents.
  • the water-insoluble carbonate can be selected from calcium carbonate or magnesium carbonate. It is necessary to avoid reaction with ethanolamine and avoid being dissolved in water and other water-soluble components.
  • the washcoat layer 2 of the present invention comprises 80-100 parts by weight of acrylic resin, 1-2 parts by weight of dimethylsilylated silica, 10-15 parts by weight of ethanolamine, 0.5-0.8 parts by weight of polyquaternary ammonium salt, 5-10 parts by weight of water-insoluble carbonate, 1-2 parts by weight of melamine, and 80-100 parts by weight of propylene glycol.
  • the preparation method of the above-mentioned release film substrate of the present invention can be obtained through the following steps.
  • the thickness of the precoat layer is 5-10 ⁇ m
  • the water-insoluble carbonate added is preferably calcium carbonate or magnesium carbonate, and the particle size is 5-10 ⁇ m.
  • Plasma surface activation treatment is a common treatment method in the field.
  • the activation treatment can be performed by oxygen.
  • the oxygen flow rate is 100sccm, and the vacuum degree is 0.1-0.2mbar and the time is 30s-60s.
  • the precoat layer after the activation treatment is pickled.
  • 6-8 mol/L hydrochloric acid is used to soak the precoat at 50-60 degrees Celsius for 10-20 minutes.
  • acid washing the exposed carbonate components on the precoat can be partially dissolved, and a porous structure can be further obtained, which further improves the surface activity of the coating and is conducive to the subsequent close combination with the release agent.
  • the surface activity and hydrophilicity of the release film base material are greatly improved, which is conducive to the close contact with the silicone oil type release agent. Combined, the release agent can be prevented from detaching.
  • the substrate with the active coating of the present invention can not only be used as a release film substrate, but also can be used in various substrates used as anti-fogging surfaces, such as anti-fogging substrates for anti-fog mirrors and the like.
  • the present invention also provides a specific polyester film, so that the release film substrate of the present invention can provide better adhesion to the release agent layer 3, and at the same time, the polyester film in the present invention has excellent Processability, good tensile strength and light transmittance, and flame retardant properties.
  • the surface layer 11 and the bottom layer 12 of the polyester film 1 of the present invention are made of the same polyester material, and the polyester preferably contains silicon dioxide and alkaline earth metal silicic acid. salt and polydimethylsiloxane.
  • the content of silicon dioxide is 0.3 wt % to 1.5 wt %
  • the content of alkaline earth metal silicate is 0.05 wt % to 0.5 wt %
  • the content of polydimethylsilicon The content of oxane is 0.2wt% ⁇ 1.2 wt%.
  • the intermediate layer 13 may contain only ordinary polyester to reduce cost.
  • the polyester components in the surface layer 11, the bottom layer 12 and the middle layer 13 are preferably the same.
  • the polyester in the middle layer 13 is If the polyester in the surface layer 11 and the bottom layer 12 is PETG, the polyester in the middle layer 13 is also PETG.
  • the polyester components in the surface layer 11 , the bottom layer 12 and the middle layer 13 may also be different, the compatibility between them will be slightly worse, and the preparation cost will be slightly higher.
  • the silica in the surface layer 11 and the bottom layer 12 can improve the light transmittance, processability and strength of the polyester film, and can adsorb the silicone oil component in the release agent layer 3 at the same time to improve the adhesion of the release agent layer.
  • the alkaline earth metal silicate can reduce the thermal shrinkage caused by the increased silica content in the polyester film, and the alkaline earth metal silicate is preferably magnesium silicate or calcium silicate, most preferably magnesium silicate.
  • Polydimethylsiloxane can improve the dispersion of silica in polyester, avoid agglomeration, reduce the amount of inorganic particles added, and improve the optical properties of polyester films. In addition, polydimethylsiloxane can also Produces stronger adhesion with Silica Dimethylsilylate in Washcoat 2.
  • the silicon atom of silica and alkaline earth metal silicate is combined with the silicon atom of polydimethylsiloxane, the polymer at the other end of polydimethylsiloxane can be combined with the alkane of polyester, which is conducive to the integration of dimethicone.
  • Silica and alkaline earth metal silicates are uniformly dispersed within the polyester.
  • the alkaline earth elements in alkaline earth metal silicates are easy to form interacting complexes with appropriate strength with phosphorus compound catalysts, stabilizers, flame retardants, etc. commonly used in polyesters, which can improve the dispersibility of silica.
  • the addition of alkaline earth metal silicates such as magnesium silicate or calcium silicate can reduce the shrinkage rate of polyester films, and is especially suitable for adding to polyester films in the optical field, which is beneficial to improve the base Optical properties of the film.
  • the shrinkage rate of the obtained polyester film will change significantly, which is quite favorable for the heat shrinkable film.
  • the release film it is ideal to keep the shrinkage of the film at a low level.
  • the combination of the silicate component and the silica improves the dispersibility on the one hand, and reduces the shrinkage rate of the silica-added film by using the alkaline earth metal, thereby improving the optical properties of the film.
  • the silica in the surface layer 11 and the bottom layer 12 is preferably silica aerogel.
  • Silica aerogel is a porous, disordered, low-density silica aerogel with a nanoscale continuous network structure, and its specific surface area is much larger than that of ordinary silica.
  • Coupling agents, silane coupling agents (such as vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris( ⁇ -methoxyethoxy)silane, etc.) are more difficult to disperse than ordinary silica. Due to its very low density, it floats easily and cannot be dispersed inside the polyester.
  • the porous structure of the aerogel can generate strong binding force through the polydimethylsiloxane, which increases the density of the aerogel and allows the aerogel to sink into the polyester.
  • the specific surface area of alkaline earth metal silicates is also large, and the loose and porous properties are similar to aerogels, but the dispersibility is better.
  • the adsorption of the silicon element of alkaline earth metal silicates and aerogels can improve aerogels. Adhesive dispersibility to avoid agglomeration.
  • the surface layer 11 and the bottom layer 12 added with silica or silica aerogel, alkaline earth metal silicate and polydimethylsiloxane have little change in viscosity relative to the bulk polyester, which is beneficial to maintain polyester film parameters It can also reduce the amount of anti-blocking particles; improve the processing performance, tensile strength, light transmittance and flame retardant performance of polyester film. In addition, it can also improve the gloss, wear resistance, high temperature resistance and heat insulation properties of polyester film.

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

Abstract

本发明提供了一种离型膜基材及其制备方法，所述离型膜基材包括聚酯薄膜（1）和活化涂层（2），活化涂层（2）形成在聚酯薄膜（1）的表面，硅油离型剂涂覆在活化涂层（2）的表面形成离型剂层（3），所述活化涂层（2）包含如下组分：丙烯酸树脂、二甲基甲硅烷基化硅石表面活性剂、乙醇胺表面侵蚀剂、聚季铵盐表面活性杀菌剂、非水溶性碳酸盐、三聚氰胺固化剂以及丙二醇溶剂。通过在本发明的离型膜基材的聚酯薄膜表面形成的多孔的亲水性活化涂层，离型膜基材的表面活性和亲水性大大提高，有利于与硅油类离型剂紧密结合，可以避免离型剂脱离。

Description

一种离型膜基材及其制备方法 技术领域
本发明涉及聚酯薄膜领域，尤其涉及一种专用于离型膜的基材及其制备方法。
 背景技术
离型膜，又称剥离膜、隔离膜、分离膜、阻胶膜等，是指表面具有分离性的薄膜。离型膜与特定的材料在有限的条件下接触后不具有粘性，或轻微的粘性。离型膜被广泛的应用于包装、印刷、丝印、移印、铭板、薄膜开关、柔性线路、绝缘制品、线路板、激光防伪、贴合、电子、密封材料用膜、反光材料、防水材料、医药（膏药用纸）、卫生用纸、胶粘制品、模切冲型加工等行业领域。
CN 111393699 A公开了一种阻燃离型膜及其制备方法，所述离型膜包括基膜，离型剂，离型剂包括以下原料：有机硅主体聚合物，交联剂，催化剂，架桥剂，阻燃剂，反光粉，有机溶剂，所述阻燃剂为含醇羟基的磷系阻燃剂。该现有技术通过在离型剂中加入含醇羟基阻燃剂，通过醇羟基与架桥剂中的异氰酸根在加热情况下反应，使阻燃剂成功接枝到与基膜有一定结合力的有机硅聚合物上，使用时可大大降低阻燃剂的迁移、析出，进而达到持久阻燃的效果。该现有技术的离型剂具有阻燃效果，对离型膜的基材没有改进。
CN 111394010 A公开了一种偏光片用离型膜，该现有技术的离型剂按重量份数计，其制备原料包括：主剂100-125份、溶剂550-900份、偶联剂2-5份、金属催化剂10-20份、光稳定剂4-6份、脱模剂10-20份、聚氨酯热熔胶10-20份、流平剂5-15份，其中主剂选自异丙氧基三甲基硅烷、甲基乙氧基硅油、甲基三氟丙基硅油、甲基乙烯基硅油中的至少一种，偶联剂选自硅烷偶联剂，该偏光片用离型膜具有较好的离型效果和较好的抵抗硅转移能力，使得偏光片用离型膜较易剥离以及防止出现PSA胶被拉起来的现象。该现有技术的改进也仅在于离型剂，没有涉及离型膜的基材。
CN 111423609 A公开了一种本质型防静电离型膜基膜及其应用，防静电离型膜基膜材质为改性HDPE，所述改性HDPE包括以下原料：烯基化合物和含双键的季铵盐。该现有技术通过在高密度聚乙烯聚合单体中掺杂可聚合的季铵盐制备出可本质型防静电离型膜基膜，季铵盐是优良的阳离子防静电剂，其均匀分散在树脂中，形成通路泄露静电荷，具有防静电功能的基团不会迁移，不会被粘走，发挥本质型防静电的作用。该现有技术中，在改性HDPE的共聚单体中加入了少量的含有两个及以上碳碳双键的季铵盐，其不仅具有提高改性HDPE防静电性能的作用，还预想不到的发现其具有提高离型膜高温高湿环境下的防静电的作用。
CN 111518472 A公开了一种抗静电剂和一种抗静电离型膜及其制备方法。所述抗静电离型膜包括基膜层和功能层，功能层由抗静电剂制得。其中抗静电剂包含如下重量份的组分：导电单体0.05～0.5份，光固化有机硅氧烷树脂20～40份，光固化有机硅离型剂60～80份，光引发剂0.05～0.5份。该现有技术的导电单体优选为乙烯基甲基恶唑烷酮。
现有技术的离型膜，存在离型剂与基材结合不牢固容易脱离的问题，从而会导致移除离型膜的时候，离型剂残留在产品表面，造成产品表面的工作性能发生改变。
 技术问题
本申请要解决的技术问题是提供一种离型膜基材及其制备方法，以减少或避免前面所提到的问题。
 技术解决方案
为解决上述技术问题，本申请提出了一种离型膜基材，包括聚酯薄膜和活化涂层，活化涂层形成在聚酯薄膜的表面，硅油离型剂涂覆在活化涂层的表面形成离型剂层；所述活化涂层包含如下组分：丙烯酸树脂、二甲基甲硅烷基化硅石表面活性剂、乙醇胺表面侵蚀剂、聚季铵盐表面活性杀菌剂、非水溶性碳酸盐、三聚氰胺固化剂以及丙二醇溶剂。
优选地，所述活化涂层包含80-100重量份的丙烯酸树脂、1-2重量份的二甲基甲硅烷基化硅石、10-15重量份的乙醇胺、0.5-0.8重量份的聚季铵盐、5-10重量份的非水溶性碳酸盐、1-2重量份的三聚氰胺以及80-100重量份的丙二醇。
优选地，所述活化涂层的厚度为5-10μm。
优选地，所述非水溶性碳酸盐为碳酸钙或者碳酸镁。
优选地，所述非水溶性碳酸盐的粒径为5-10μm。
优选地，所述聚酯薄膜为三层共挤复合结构的聚酯薄膜，包括表层、底层以及夹持在二者之间的中间层，所述活化涂层形成在所述聚酯薄膜的表层和/或底层的外表面上。
另外还可以优选，所述聚酯薄膜的表层和底层采用相同的聚酯材料制成，其聚酯中均含有二氧化硅和碱土金属硅酸盐以及聚二甲基硅氧烷。
优选地，所述聚酯薄膜的表层和底层中的二氧化硅采用二氧化硅气凝胶。
优选地，所述聚酯薄膜的表层和底层中，二氧化硅的含量为0.3 wt%~1.5 wt%，碱土金属硅酸盐的含量为0.05 wt%~0.5 wt%，聚二甲基硅氧烷的含量为0.2wt%~1.2 wt%。
另外，本发明还提出了一种离型膜基材的制备方法，其中，所述离型膜基材包括聚酯薄膜和活化涂层，活化涂层形成在聚酯薄膜的表面，硅油离型剂涂覆在活化涂层的表面形成离型剂层；所述方法包括如下步骤：
首先，将80-100重量份的丙烯酸树脂、1-2重量份的二甲基甲硅烷基化硅石、10-15重量份的乙醇胺、0.5-0.8重量份的聚季铵盐、5-10重量份的非水溶性碳酸盐、1-2重量份的三聚氰胺以及80-100重量份的丙二醇均匀混合之后，通过旋涂或者喷涂方式涂覆在聚酯薄膜的外表面，在70-120℃下固化1-2小时，从而在聚酯薄膜的外表面获得预涂层；
之后，对预涂层进行等离子表面活化处理；
然后，对活化处理之后的预涂层进行酸洗；
最后用水冲洗、烘干，获得活化涂层。
优选，酸洗步骤中采用6-8mol/L的盐酸50-60摄氏度浸泡预涂层10-20分钟。
优选，最后用水冲洗10-20分钟，50-60度烘干30分钟。
 有益效果
通过在本发明的离型膜基材的聚酯薄膜表面形成的多孔的亲水性活化涂层，离型膜基材的表面活性和亲水性大大提高，有利于与硅油类离型剂紧密结合，可以避免离型剂脱离。
 附图说明
以下附图仅旨在于对本申请做示意性说明和解释，并不限定本申请的范围。
其中，图1显示的是本申请的离型膜的剖面结构分解示意图。
 本发明的实施方式
为了对本申请的技术特征、目的和效果有更加清楚的理解，现详细说明本申请的具体实施方式。
本发明提出了一种改进的离型膜，具体来说是提供了一种改进的离型膜基材，所述离型膜基材的表面可以涂布硅油离型剂，从而制备获得离型膜。本发明的离型膜可应用于包装、印刷、丝印、移印、铭板、薄膜开关、柔性线路、绝缘制品、线路板、激光防伪、贴合、电子、密封材料用膜、反光材料、防水材料、医药（膏药用纸）、卫生用纸、胶粘制品、模切冲型加工等行业领域。
具体的，如图1所示，本发明的离型膜基材10包括聚酯薄膜1和活化涂层2，所述聚酯薄膜1优选由双向拉伸PET薄膜制成，其可以是单层结构，也可以是多层复合结构。在一个具体实施例中，本发明的聚酯薄膜1可以为三层共挤复合结构的聚酯薄膜，例如如图，该三层共挤复合结构的聚酯薄膜可以包括表层11、底层12以及夹持在二者之间的中间层13，所述活化涂层2形成在聚酯薄膜1的表层11和/或底层12的外表面上。离型剂涂覆在活化涂层2的表面形成离型剂层3（图中虚线所示，为了表示清楚，离型剂层3进行了分解表示）。
进一步的，本发明的活化涂层2包含如下组分：丙烯酸树脂、二甲基甲硅烷基化硅石表面活性剂、乙醇胺表面侵蚀剂、聚季铵盐表面活性杀菌剂、非水溶性碳酸盐、三聚氰胺固化剂以及丙二醇溶剂。
其中，乙醇胺表面侵蚀剂可以对聚酯薄膜1的外表面形成一定的降解侵蚀，降低聚酯薄膜1的外表面的平整度，有利于活化涂层2中的亲水成分与聚酯薄膜1形成牢固的结合；而且乙醇胺在涂层固化过程中易于分解出气体，可使得活化涂层2形成蓬松多孔的结构。丙烯酸树脂具有亲水性，通过二甲基甲硅烷基化硅石表面活性剂进一步乳化，且该含硅表面活性剂与聚酯薄膜1可以获得很强的结合力。聚季铵盐表面活性杀菌剂可以降低固化后的涂层表面的表面张力，提高涂层对硅油离型剂的吸附能力，避免离型剂脱离，且聚季铵盐具备杀菌功能，可以使离型剂层长时间保持使用状态。三聚氰胺相对其它固化剂对水分不敏感，且与硅油类离型剂的亲和性更好。非水溶性碳酸盐可以选择碳酸钙或者碳酸镁，需要避免与乙醇胺反应，也要避免溶解在水及其它水溶性成分中。
在一个具体实施例中，本发明的活化涂层2包含80-100重量份的丙烯酸树脂、1-2重量份的二甲基甲硅烷基化硅石、10-15重量份的乙醇胺、0.5-0.8重量份的聚季铵盐、5-10重量份的非水溶性碳酸盐、1-2重量份的三聚氰胺以及80-100重量份的丙二醇。
本发明的上述离型膜基材的制备方法，可以通过如下步骤获得。
首先，将80-100重量份的丙烯酸树脂、1-2重量份的二甲基甲硅烷基化硅石、10-15重量份的乙醇胺、0.5-0.8重量份的聚季铵盐、5-10重量份的非水溶性碳酸盐、1-2重量份的三聚氰胺以及80-100重量份的丙二醇均匀混合之后，通过旋涂或者喷涂方式涂覆在聚酯薄膜1的外表面，在70-120℃下固化1-2小时，从而在聚酯薄膜1的外表面获得预涂层。
在一个具体实施例中，所述预涂层的厚度为5-10μm，优选添加的非水溶性碳酸盐为碳酸钙或者碳酸镁，粒径为5-10μm。
之后，对预涂层进行等离子表面活化处理。经表面活化处理，预涂层表面会形成均匀的凸凹粗糙表面，可以将其中的非水溶性碳酸盐部分裸露出来。等离子表面活化处理为本领域常用处理方式，例如可以通过氧气进行活化处理，氧气流量为100sccm，真空度0.1-0.2mbar时间为30s-60s。
然后，对活化处理之后的预涂层进行酸洗。优选采用6-8mol/L的盐酸50-60摄氏度浸泡预涂层10-20分钟。通过酸洗，预涂层上裸露的碳酸盐成分可以部分溶解，可以进一步获得多孔的结构，进一步提高了涂层的表面活性，有利于后续与离型剂的紧密结合。
最后用水冲洗、烘干，获得本发明的活化涂层2。用水冲洗时间10-20分钟，50-60度烘干30分钟。
通过在本发明的离型膜基材的聚酯薄膜表面形成的多孔的亲水性活化涂层，离型膜基材的表面活性和亲水性大大提高，有利于与硅油类离型剂紧密结合，可以避免离型剂脱离。
具有本发明的活化涂层的基材，不但可以用作离型膜基材，而且还可用于各种用作防雾表面的基材，例如防雾镜的防雾基材等。
另外，本发明还提供了一种特定的聚酯薄膜，使得本发明的离型膜基材可以对离型剂层3提供更好的附着力，同时使得本发明中的聚酯薄膜具备优异的加工性能、良好的拉伸强度和透光率以及阻燃性能。
如图，在本发明的一个具体实施例中，本发明的聚酯薄膜1的表层11和底层12采用相同的聚酯材料制成，其聚酯中优选均含有二氧化硅和碱土金属硅酸盐以及聚二甲基硅氧烷。在另一个具体实施例中，表层11和底层12中，二氧化硅的含量为0.3 wt%~1.5 wt%，碱土金属硅酸盐的含量为0.05 wt%~0.5 wt%，聚二甲基硅氧烷的含量为0.2wt%~1.2 wt%。
中间层13可以只包含普通聚酯以降低成本。在一个具体实施例中，表层11、底层12和中间层13中的聚酯成分优选相同，例如，如果表层11和底层12中的聚酯采用的是PET，则中间层13中的聚酯采用的也是PET；如果表层11和底层12中的聚酯采用的是PETG，则中间层13中的聚酯采用的也是PETG。当然，这也意味着，表层11、底层12和中间层13中的聚酯成分也可以是不同的，二者相容性会略差一些，制备成本也会略高。
表层11和底层12中的二氧化硅可以提高聚酯薄膜的透光性、加工性能以及强度，同时可以与离型剂层3中的硅油成分产生吸附作用，提高离型剂层的附着力。碱土金属硅酸盐可以降低由于聚酯薄膜中二氧化硅含量增高导致的热收缩性，所述碱土金属硅酸盐优选为硅酸镁或者硅酸钙，最优选为硅酸镁。聚二甲基硅氧烷可以提高聚酯中二氧化硅的分散性，避免团聚，有利于减少无机粒子的添加量，提高聚酯薄膜的光学性能，另外，聚二甲基硅氧烷还可以与活化涂层2中的二甲基甲硅烷基化硅石产生更强的附着力。
二氧化硅以及碱土金属硅酸盐的硅原子由于结合了聚二甲基硅氧烷的硅原子，聚二甲基硅氧烷另一端的高分子可以与聚酯的烷烃结合，有利于将二氧化硅和碱土金属硅酸盐均匀分散保持在聚酯内部。碱土金属硅酸盐中的碱土元素易于与聚酯中常用磷类化合物催化剂、稳定剂、阻燃剂等形成具有适当强度的相互作用的络合物，除了可以提高二氧化硅的分散性之外，还可以提高二氧化硅以及碱土金属硅酸盐在聚酯中的结合力，有利于提高聚酯薄膜的光线透过率。另外如前所述，硅酸镁或硅酸钙之类的碱土金属硅酸盐的加入，可以降低聚酯薄膜的收缩率，尤其适用于添加到光学领域聚酯薄膜之中，有利于提高基膜的光学性能。
需要提及的是，由于二氧化硅的添加，制得的聚酯薄膜的收缩率会发生较为明显的变化，对于热收缩薄膜是相当有利的。然而对于离型膜来说，要求薄膜的收缩率保持较低的水平较为理想。本发明中，通过硅酸盐成分与二氧化硅的结合，一方面提高分散性，另一方面利用碱土金属降低添加了二氧化硅的薄膜的收缩率，进而提高薄膜的光学性能。
在一个优选实施例中，表层11和底层12中的二氧化硅优选采用二氧化硅气凝胶。二氧化硅气凝胶是一种具有多孔、无序、具有纳米量级连续网络结构的低密度二氧化硅气凝胶，比表面积比普通二氧化硅大很多，用现有技术的磷酸酯偶联剂、硅烷偶联剂（例如乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三（β-甲氧乙氧基）硅烷等）比普通二氧化硅更加难以分散。由于密度非常低，很容易漂浮，无法分散到聚酯内部。气凝胶的多孔结构可以通过聚二甲基硅氧烷产生强大的结合力，增大了气凝胶的密度，可以使气凝胶沉入聚酯内部。碱土金属硅酸盐的比表面积也很大，疏松多孔特性与气凝胶类似，但是分散性却较好，利用碱土金属硅酸盐的硅元素成分与气凝胶产生的吸附，可以提高气凝胶的分散性，避免团聚。
添加有二氧化硅或二氧化硅气凝胶、碱土金属硅酸盐以及聚二甲基硅氧烷的表层11和底层12，其粘度相对本体聚酯变化很小，有利于保持聚酯薄膜参数的稳定性；还可降低抗粘连粒子的用量；提高了聚酯薄膜的加工性能、拉伸强度、透光率和阻燃性能。另外也可以改善聚酯薄膜的光泽度、耐磨、耐高温、隔热性能。
本领域技术人员应当理解，虽然本申请是按照多个实施例的方式进行描述的，但是并非每个实施例仅包含一个独立的技术方案。说明书中如此叙述仅仅是为了清楚起见，本领域技术人员应当将说明书作为一个整体加以理解，并将各实施例中所涉及的技术方案看作是可以相互组合成不同实施例的方式来理解本申请的保护范围。
以上所述仅为本申请示意性的具体实施方式，并非用以限定本申请的范围。任何本领域的技术人员，在不脱离本申请的构思和原则的前提下所作的等同变化、修改与结合，均应属于本申请保护的范围。

Claims (12)

  1. 一种离型膜基材，包括聚酯薄膜（1）和活化涂层（2），其特征在于，活化涂层（2）形成在聚酯薄膜（1）的表面，硅油离型剂涂覆在活化涂层（2）的表面形成离型剂层（3）；所述活化涂层包含如下组分：丙烯酸树脂、二甲基甲硅烷基化硅石表面活性剂、乙醇胺表面侵蚀剂、聚季铵盐表面活性杀菌剂、非水溶性碳酸盐、三聚氰胺固化剂以及丙二醇溶剂。
  2. 如权利要求1所述的离型膜基材，其特征在于，所述活化涂层（2）包含80-100重量份的丙烯酸树脂、1-2重量份的二甲基甲硅烷基化硅石、10-15重量份的乙醇胺、0.5-0.8重量份的聚季铵盐、5-10重量份的非水溶性碳酸盐、1-2重量份的三聚氰胺以及80-100重量份的丙二醇。
  3. 如权利要求1所述的离型膜基材，其特征在于，所述活化涂层（2）的厚度为5-10μm。
  4. 如权利要求3所述的离型膜基材，其特征在于，所述非水溶性碳酸盐为碳酸钙或者碳酸镁。
  5. 如权利要求4所述的离型膜基材，其特征在于，所述非水溶性碳酸盐的粒径为5-10μm。
  6. 如权利要求1所述的离型膜基材，其特征在于，所述聚酯薄膜（1）为三层共挤复合结构的聚酯薄膜，包括表层（11）、底层（12）以及夹持在二者之间的中间层（13），所述活化涂层（2）形成在所述聚酯薄膜（1）的表层（11）和/或底层（12）的外表面上。
  7. 如权利要求6所述的离型膜基材，其特征在于，所述聚酯薄膜（1）的表层（11）和底层（12）采用相同的聚酯材料制成，其聚酯中均含有二氧化硅和碱土金属硅酸盐以及聚二甲基硅氧烷。
  8. 如权利要求7所述的离型膜基材，其特征在于，所述聚酯薄膜（1）的表层（11）和底层（12）中的二氧化硅采用二氧化硅气凝胶。
  9. 如权利要求7或8所述的离型膜基材，其特征在于，所述聚酯薄膜（1）的表层（11）和底层（12）中，二氧化硅的含量为0.3 wt%~1.5 wt%，碱土金属硅酸盐的含量为0.05 wt%~0.5 wt%，聚二甲基硅氧烷的含量为0.2wt%~1.2 wt%。
  10. 一种离型膜基材的制备方法，所述离型膜基材包括聚酯薄膜（1）和活化涂层（2），活化涂层（2）形成在聚酯薄膜（1）的表面，硅油离型剂涂覆在活化涂层（2）的表面形成离型剂层（3），所述方法包括如下步骤：首先，将80-100重量份的丙烯酸树脂、1-2重量份的二甲基甲硅烷基化硅石、10-15重量份的乙醇胺、0.5-0.8重量份的聚季铵盐、5-10重量份的非水溶性碳酸盐、1-2重量份的三聚氰胺以及80-100重量份的丙二醇均匀混合之后，通过旋涂或者喷涂方式涂覆在聚酯薄膜（1）的外表面，在70-120℃下固化1-2小时，从而在聚酯薄膜（1）的外表面获得预涂层；之后，对预涂层进行等离子表面活化处理；然后，对活化处理之后的预涂层进行酸洗；最后用水冲洗、烘干，获得活化涂层（2）。
  11. 如权利要求10所述的方法，其特征在于，酸洗步骤中采用6-8mol/L的盐酸50-60摄氏度浸泡预涂层10-20分钟。
  12. 如权利要求10所述的方法，其特征在于，最后用水冲洗10-20分钟，50-60度烘干30分钟。
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