CN111944405A - Coating liquid for optical polyester film prime coat and preparation method thereof - Google Patents

Coating liquid for optical polyester film prime coat and preparation method thereof Download PDF

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Publication number
CN111944405A
CN111944405A CN202010824047.5A CN202010824047A CN111944405A CN 111944405 A CN111944405 A CN 111944405A CN 202010824047 A CN202010824047 A CN 202010824047A CN 111944405 A CN111944405 A CN 111944405A
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solution
polyester film
deionized water
coating liquid
stirring
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CN111944405B (en
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潘世新
张志宏
吕军锋
卞伟冬
卞小通
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Jiangsu Sanfangxiang Film Co ltd
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Jiangsu San Fang Lane Film Co ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00—Producing flat articles, e.g. films or sheets
    • B29D7/01—Films or sheets
    • 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
    • B32B27/08—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 of synthetic resin
    • 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
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
    • C09D161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C09D161/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
    • C09D161/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
    • 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
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • 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
    • C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
    • C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy 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
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • 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
    • 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
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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

The invention discloses a coating liquid for priming coating of an optical polyester film and a preparation method thereof, wherein the coating liquid comprises the following components in parts by weight: 3-15% of waterborne polyurethane, 1-5% of waterborne polyester, 0.1-0.5% of melamine resin, 0.1-0.5% of epoxy resin, 0.3-1% of modified polyurethane, 0.5-1.5% of organic solvent, 0.05-0.3% of wetting agent, 0.1-1% of nano particles, 0.01-0.1% of pH value regulator and the balance of deionized water. The polyester film coated by the aqueous coating liquid has low haze, high light transmittance, good smoothness and strong adhesive force to an optical functional coating, is suitable for manufacturing brightening and diffusing optical films with strict requirements on the adhesive force, can enhance the surface adhesive force of the polyester film after the polyester film is subjected to on-line priming treatment, is suitable for production and processing of brightening films, diffusing films and composite films, and is suitable for wide popularization and use.

Description

Coating liquid for optical polyester film prime coat and preparation method thereof
Technical Field
The invention relates to the field of coating liquid for hardening film base coating, in particular to coating liquid for optical polyester film base coating and a preparation method thereof.
Background
The biaxially oriented polyester film has excellent physical properties, mechanical properties and optical properties, is widely applied to the fields of packaging, printing, aluminizing, compounding, electrical insulation, solar backing materials, optical fields of liquid crystal display, optical protection, heat insulation window films and the like, is commonly used for manufacturing optical films such as a brightness enhancement film, a diffusion film, a composite film and the like for a liquid crystal display backlight module, needs to process optical functional layers such as brightness enhancement, diffusion and the like on the surface of the optical functional layers, needs to carry out surface chemical priming on the polyester film to enhance the surface adhesive force under the high-temperature and high-humidity environmental conditions because the surface energy is low and the adhesive force of the functional layers cannot meet the required use standard, is produced and manufactured by a method of coating a chemical coating on line in the biaxially oriented manufacturing process of the polyester film, and is coated between a longitudinal stretching process and a transverse stretching process, the coating liquid for chemical priming treatment can affect optical properties of the polyester optical film, such as haze, light transmittance and the like, and the properties of the prepared optical polyester film can be affected due to insufficient adhesive force, UV resistance, high temperature and high humidity resistance. Therefore, we propose a coating liquid for priming an optical polyester film and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a coating liquid for priming an optical polyester film and a preparation method thereof, which are used for solving the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: the coating liquid for priming the optical polyester film comprises the following components in parts by weight: 3-15% of waterborne polyurethane, 1-5% of waterborne polyester, 0.1-0.5% of melamine resin, 0.1-0.5% of epoxy resin, 0.3-1% of modified polyurethane, 0.5-1.5% of organic solvent, 0.05-0.3% of wetting agent, 0.1-1% of nano particles, 0.01-0.1% of pH value regulator and the balance of deionized water.
In the technical scheme, the polyurethane resin has chemical resistance and aging resistance, the waterborne copolyester resin has higher toughness, the optical property and the chemical resistance are better, the compatibility is better, the melamine resin has high hardness, the scratch resistance and the hardness of the prepared coating can be improved, the epoxy resin is added into a coating liquid system, the adhesive force of the prepared coating can be improved, the heat resistance and the chemical resistance of the coating are improved, and the coating liquid system is formed by the respective performances of the resin, an organic solvent, a wetting agent, a pH value regulator and deionized water, so that the prepared coating has higher adhesive property, and the ultraviolet resistance, the high humidity and high temperature resistance of the coating are improved.
Further, the solid content of the waterborne polyurethane is 39-41%.
Furthermore, the solid content of the water-based polyester is 33-35%, the molecular weight is 15000, and the hydroxyl value is 6 mgKOH/g.
Further, the solid content of the modified polyurethane is 22-23%.
Further, the organic solvent is absolute ethyl alcohol, the wetting agent is one or more of polyether modified polysiloxane and organic fluorocarbon wetting agents, the nanoparticles are silicon dioxide, and the particle size of the nanoparticles is 65 nm.
In the technical scheme, the characteristics of the raw material components are limited, the functions and effects of the raw material components under the limited conditions are exerted, the functions of the prepared coating liquid and the prepared coating are promoted, the prepared coating liquid and the prepared coating can achieve the optimized performance expression, and the method is more suitable for the preparation process of the coating liquid and the prepared coating.
A preparation method of a coating liquid for priming an optical polyester film comprises the following steps:
1) adding a wetting agent into an organic solvent for dilution, taking 50-80% of the total amount of deionized water in the components, adjusting the pH value to 8.0-9.0 by using an ammonia salt, slowly adding a wetting agent diluted solution into the deionized water, mixing and uniformly stirring to obtain a solution A;
2) adding deionized water with the weight 4 times that of the waterborne polyester into the waterborne polyester for dilution to prepare a diluted solution, stirring the solution A, slowly adding the UV-resistant modified polyurethane, stirring uniformly, then slowly adding the waterborne polyurethane, stirring uniformly, then slowly adding the diluted solution, and continuously stirring to obtain a solution B;
3) stirring the solution B, adding 1-2 times of deionized water by weight into melamine resin for dilution, taking an organic solvent and deionized water for diluting epoxy resin, wherein the weight ratio of epoxy resin to deionized water to ethanol is 1:1:1, slowly adding the prepared melamine resin diluted solution and epoxy resin diluted solution into the solution B respectively, continuously stirring for 5-25 min, and adjusting the pH value to 8.0-9.0 by using ammonia salt to obtain a solution C;
4) stirring the solution C, taking nanoparticles to prepare an aqueous dispersion liquid with the silicon dioxide content of 40%, diluting with deionized water of which the weight is 1-2 times that of the aqueous dispersion liquid, slowly adding the diluted solution into the solution C after uniformly stirring, adding the rest deionized water in the components after uniformly stirring, continuously stirring for 5-25 min, adding a pH value regulator to regulate the pH value of the system to be 8.0-9.0, and continuously stirring for 1-3 h to obtain an aqueous coating liquid with the solid content of 3-4%.
Further, the preparation method of the waterborne polyurethane comprises the following steps:
taking hydroxyl silicone oil and methyl acrylate for grafting, mixing with an emulsifier and deionized water for emulsification, and finally adding aminosilane for reaction to prepare modified silicone oil;
taking polytetrahydrofuran diol, dicyclohexylmethane diisocyanate, 1, 3-propylene glycol and modified silicone oil as monomers, drying in a nitrogen atmosphere, heating, adding a catalyst to synthesize a polyurethane prepolymer, adding 2, 2' -dicarboxymethylpropionic acid as a chain extender, uniformly stirring, continuing to react, adding 1, 4-butanediol and trimethylolpropane, cooling to react, adding a silane coupling agent, and cooling again to react to obtain the waterborne polyurethane.
In the technical scheme, the hydroxyl silicone oil and the methyl acrylate are grafted by a hydrosilation method, so that the thermal stability of the silicone oil can be improved, the intermolecular friction force is reduced, the uniform dispersion of materials in subsequent reactions is facilitated, the hydrophilicity and the polarity of amino groups can prevent the agglomeration among particles of the modified silicone oil, the stability of the modified silicone oil is improved, the adsorption capacity of the modified silicone oil is improved, the modified silicone oil can be orderly arranged in the polyurethane prepolymer, the flexibility and the transparency of the prepared polyurethane resin are improved, and the crease resistance, the smoothness and the bonding performance of the prepared coating are improved; the polyurethane resin prepared by using the materials as raw materials has good water resistance, ethanol resistance and mechanical property while maintaining the water property, has good compatibility with other resins, has good ultraviolet resistance, and can obtain the water-based UV-resistant polyurethane resin easy to attach.
Further, the preparation steps of the water-based polyester are as follows:
1, 4-cyclohexane dimethanol, biphenyl dicarboxylic acid and dimethyl isophthalate-5-sodium sulfonate are used as monomers for reaction and copolymerization, and prepolymer of phenoxy phosphoryl chloride and resorcinol is added, and the water-based polyester is prepared by heating and pressure increasing reaction.
In the technical scheme, the polyester resin prepared from the monomers has good hydrolysis resistance and stability, and the added prepolymer improves the heat-resistant flame-retardant property, so that the prepared polyester resin has the characteristics of high strength, aging resistance and excellent chemical resistance, and the water-based heat-resistant copolymerized polyester resin is obtained.
Further, the preparation method of the modified polyurethane comprises the following steps:
polycaprolactone diol, isophorone diisocyanate and dimethyl terephthalate are used as monomers to react and copolymerize, triethylene glycol bis-3-butyl-4-hydroxy-5-methylphenyl propionate is added, and the reacted products are blended with nano titanium dioxide modified polypropylene glycol to prepare the modified polyurethane.
In the technical scheme, the ultraviolet-resistant polyurethane resin is obtained by the monomers and is blended with the modified polypropylene glycol, so that the ultraviolet resistance and the yellowing resistance of the polyurethane resin are improved, and the plastic surface flatness of the prepared coating is improved, thereby obtaining the UV-resistant modified polyurethane resin.
A preparation method of an optical polyester film comprises the following steps:
1) film forming:
taking a polyester base film with the water content of 0-50 ppm, melting and extruding at the temperature of 270-290 ℃, filtering, then carrying out three-layer co-extrusion, and carrying out tape casting to obtain a membrane D;
2) primary stretching:
preheating the membrane D at the temperature of 70-85 ℃, then heating by using 70-85% of infrared rays, and then longitudinally stretching with the longitudinal stretching magnification of 3-4 times to obtain a membrane E;
3) coating:
coating the water-soluble coating liquid on the surface of the membrane E, wherein the wet coating amount of the single-side coating is 5-15 g/m2Obtaining a membrane F;
4) secondary stretching
Preheating the membrane F at the temperature of 100-130 ℃, then transversely stretching at the temperature of 110-150 ℃, wherein the transverse stretching magnification is 3-4 times, carrying out heat setting treatment and drying solidification after stretching is finished, wherein the treatment temperature is 220-250 ℃, the treatment time is 5-30 s, cooling at the temperature of 50-120 ℃, then carrying out traction and rolling, and the coating thickness is 80-120 nm at the moment, thus obtaining the finished product polyester film for optics.
In the technical scheme, the polyester base film comprises but is not limited to PET, PBT and PAR, and also comprises composite resin taking polyester as main resin, the coating liquid with uniform dispersion is prepared by setting the preparation process of the coating liquid and the optical polyester film coated with the coating liquid, the performances of the prepared coating liquid and the prepared coating layer are optimized, the coating liquid is adaptive to the production process of the polyester film, and the improvement of the adhesion of the coating layer, the UV resistance and the high temperature and high humidity resistance of the coating layer is promoted under the condition of improving the optical performances such as haze, light transmittance and the like of the optical polyester film.
Compared with the prior art, the invention has the following beneficial effects:
the coating liquid for the optical polyester film base coat and the preparation method thereof are used for preparing the coating liquid through setting the components, the proportion, the preparation process and the parameters thereof, the polyester film coated by the aqueous coating liquid is low in haze, high in light transmittance, good in smoothness and strong in binding power to an optical functional coating, is suitable for manufacturing brightening and diffusing optical films with strict requirements on binding power, and can be used for enhancing the surface adhesion of the polyester film after the polyester film is subjected to on-line base coat treatment, so that the coating liquid is suitable for producing and processing brightening films, diffusing films and composite films.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The component ratios of the coating solutions in examples 1 to 6 are shown in table 1, wherein the preparation steps of the aqueous polyurethane, the aqueous polyester and the modified polyurethane are as follows:
taking hydroxyl silicone oil and methyl acrylate for grafting, mixing with an emulsifier and deionized water for emulsification, and finally adding aminosilane for reaction to prepare modified silicone oil; taking polytetrahydrofuran diol, dicyclohexylmethane diisocyanate, 1, 3-propylene glycol and modified silicone oil as monomers, drying in a nitrogen atmosphere, heating, adding a catalyst to synthesize a polyurethane prepolymer, adding 2, 2' -dicarboxymethylpropionic acid as a chain extender, uniformly stirring, continuing to react, adding 1, 4-butanediol and trimethylolpropane, cooling to react, adding a silane coupling agent, and cooling again to react to obtain the waterborne polyurethane;
1, 4-cyclohexanedimethanol, biphenyldicarboxylic acid and dimethyl isophthalate-5-sodium sulfonate are used as monomers for reaction and copolymerization, and prepolymer of phenoxy phosphoryl chloride and resorcinol is added, and the temperature and pressure rise reaction is carried out to prepare water-based polyester;
polycaprolactone diol, isophorone diisocyanate and dimethyl terephthalate are used as monomers to react and copolymerize, triethylene glycol bis-3-butyl-4-hydroxy-5-methylphenyl propionate is added, and the reacted products are blended with nano titanium dioxide modified polypropylene glycol to prepare the modified polyurethane.
Example 1
Taking an organic solvent, adding a wetting agent, blending to prepare a wetting agent solution, taking 80% of the total amount of deionized water in the components, slowly adding the wetting agent solution into the deionized water, mixing and uniformly stirring to obtain a solution A; adding deionized water into the water-based polyester for dilution to prepare a diluted solution, stirring the solution A, slowly adding the UV-resistant modified polyurethane, stirring uniformly, then slowly adding the water-based polyurethane, stirring uniformly, then slowly adding the diluted solution, and continuously stirring to obtain a solution B; stirring the solution B, taking deionized water to dilute melamine resin, taking an organic solvent and deionized water to dilute epoxy resin, respectively and slowly adding the organic solvent and the deionized water to the solution B, and continuously stirring to obtain a solution C; stirring the solution C, taking the nano particles to prepare an aqueous dispersion liquid with the silicon dioxide content of 40%, diluting the aqueous dispersion liquid by using deionized water, slowly adding the aqueous dispersion liquid into the solution C after uniformly stirring, adding the rest deionized water in the components after uniformly stirring, continuously stirring for 25min, adding a pH value regulator to regulate the pH value of the system to be 9.0, and continuously stirring for 3h to obtain the aqueous coating liquid.
Taking a polyester base film with the water content of 50ppm, melting and extruding at 290 ℃, filtering, then carrying out three-layer co-extrusion, and carrying out tape casting to obtain a membrane D; preheating the membrane D at 85 ℃, heating by 85% of infrared rays, and longitudinally stretching at a longitudinal stretching ratio of 4 times to obtain a membrane E; coating the water-based coating liquid on one surface or two surfaces of the membrane E, wherein the wet coating amount of the single-surface coating is 5g/m2, so as to obtain a membrane F; preheating the membrane F at 130 ℃, then transversely stretching at 150 ℃, wherein the transverse stretching magnification is 4 times, carrying out heat setting treatment and drying solidification after stretching is finished, the treatment temperature is 250 ℃, the treatment time is 15s, cooling at 120 ℃, and then drawing and rolling, wherein the coating thickness is 80nm, and the thickness of the polyester film is 125 mu m, so that the finished product of the polyester film for optics is obtained.
Example 2
Taking an organic solvent, adding a wetting agent, blending to prepare a wetting agent solution, taking 80% of the total amount of deionized water in the components, slowly adding the wetting agent solution into the deionized water, mixing and uniformly stirring to obtain a solution A; adding deionized water into the water-based polyester for dilution to prepare a diluted solution, stirring the solution A, slowly adding the UV-resistant modified polyurethane, stirring uniformly, then slowly adding the water-based polyurethane, stirring uniformly, then slowly adding the diluted solution, and continuously stirring to obtain a solution B; stirring the solution B, taking deionized water to dilute melamine resin, taking an organic solvent and deionized water to dilute epoxy resin, respectively and slowly adding the organic solvent and the deionized water to the solution B, and continuously stirring to obtain a solution C; stirring the solution C, taking the nano particles to prepare an aqueous dispersion liquid with the silicon dioxide content of 40%, diluting the aqueous dispersion liquid by using deionized water, slowly adding the aqueous dispersion liquid into the solution C after uniformly stirring, adding the rest deionized water in the components after uniformly stirring, continuously stirring for 25min, adding a pH value regulator to regulate the pH value of the system to be 9.0, and continuously stirring for 3h to obtain the aqueous coating liquid.
Taking a polyester base film with the water content of 50ppm, melting and extruding at 290 ℃, filtering, then carrying out three-layer co-extrusion, and carrying out tape casting to obtain a membrane D; preheating the membrane D at 85 ℃, heating by 85% of infrared rays, and longitudinally stretching at a longitudinal stretching ratio of 4 times to obtain a membrane E; coating the water-based coating liquid on one surface or two surfaces of the membrane E, wherein the wet coating amount of the single-surface coating is 7g/m2, and obtaining a membrane F; preheating the membrane F at 130 ℃, then transversely stretching at 150 ℃, wherein the transverse stretching magnification is 4 times, carrying out heat setting treatment and drying solidification after stretching is finished, the treatment temperature is 250 ℃, the treatment time is 15s, cooling at 120 ℃, and then carrying out traction rolling, wherein the coating thickness is 95nm, and the thickness of the polyester film is 125 mu m, so that the finished product of the polyester film for optics is obtained.
Example 3
Taking an organic solvent, adding a wetting agent, blending to prepare a wetting agent solution, taking 65% of the total amount of deionized water in the components, slowly adding the wetting agent solution into the deionized water, mixing and uniformly stirring to obtain a solution A; adding deionized water into the water-based polyester for dilution to prepare a diluted solution, stirring the solution A, slowly adding the UV-resistant modified polyurethane, stirring uniformly, then slowly adding the water-based polyurethane, stirring uniformly, then slowly adding the diluted solution, and continuously stirring to obtain a solution B; stirring the solution B, taking deionized water to dilute melamine resin, taking an organic solvent and deionized water to dilute epoxy resin, respectively and slowly adding the organic solvent and the deionized water to the solution B, and continuously stirring to obtain a solution C; stirring the solution C, taking nanoparticles to prepare an aqueous dispersion liquid with the silicon dioxide content of 40%, diluting the aqueous dispersion liquid by using deionized water, slowly adding the aqueous dispersion liquid into the solution C after uniformly stirring, adding the rest deionized water in the components after uniformly stirring, continuously stirring for 15min, adding a pH value regulator to regulate the pH value of the system to be 8.5, and continuously stirring for 2h to obtain an aqueous coating liquid with the solid content of 5-15%.
Taking a polyester base film with the water content of 25ppm, melting and extruding at the temperature of 280 ℃, filtering, then carrying out three-layer co-extrusion, and carrying out tape casting to obtain a membrane D; preheating the membrane D at 77 ℃, heating by 77% of infrared rays, and longitudinally stretching at a longitudinal stretching ratio of 3.5 times to obtain a membrane E; coating the water-based coating liquid on one surface or two surfaces of the membrane E, wherein the wet coating amount of the single-surface coating is 9g/m2, and obtaining a membrane F; preheating the membrane F at the temperature of 115 ℃, then transversely stretching the membrane F at the temperature of 130 ℃, wherein the transverse stretching magnification is 3.5 times, carrying out heat setting treatment and drying solidification after stretching is finished, the treatment temperature is 235 ℃, the treatment time is 10s, cooling the membrane F at the temperature of 85 ℃, and then carrying out traction and rolling, wherein the coating thickness is 100nm, and the thickness of the polyester film is 188 microns, so that the finished product of the polyester film for optics is obtained.
Example 4
Taking an organic solvent, adding a wetting agent, blending to prepare a wetting agent solution, taking 65% of the total amount of deionized water in the components, slowly adding the wetting agent solution into the deionized water, mixing and uniformly stirring to obtain a solution A; adding deionized water into the water-based polyester for dilution to prepare a diluted solution, stirring the solution A, slowly adding the UV-resistant modified polyurethane, stirring uniformly, then slowly adding the water-based polyurethane, stirring uniformly, then slowly adding the diluted solution, and continuously stirring to obtain a solution B; stirring the solution B, taking deionized water to dilute melamine resin, taking an organic solvent and deionized water to dilute epoxy resin, respectively and slowly adding the organic solvent and the deionized water to the solution B, and continuously stirring to obtain a solution C; stirring the solution C, taking nanoparticles to prepare an aqueous dispersion liquid with the silicon dioxide content of 40%, diluting the aqueous dispersion liquid by using deionized water, slowly adding the aqueous dispersion liquid into the solution C after uniformly stirring, adding the rest deionized water in the components after uniformly stirring, continuously stirring for 15min, adding a pH value regulator to regulate the pH value of the system to be 8.5, and continuously stirring for 2h to obtain an aqueous coating liquid with the solid content of 5-15%.
Taking a polyester base film with the water content of 25ppm, melting and extruding at the temperature of 280 ℃, filtering, then carrying out three-layer co-extrusion, and carrying out tape casting to obtain a membrane D; preheating the membrane D at 77 ℃, heating by 77% of infrared rays, and longitudinally stretching at a longitudinal stretching ratio of 3.5 times to obtain a membrane E; coating the water-based coating liquid on one surface or two surfaces of the membrane E, wherein the wet coating amount of the single-surface coating is 11g/m2, and obtaining a membrane F; preheating the membrane F at the temperature of 115 ℃, then transversely stretching the membrane F at the temperature of 130 ℃, wherein the transverse stretching magnification is 3.5 times, carrying out heat setting treatment and drying solidification after stretching is finished, the treatment temperature is 235 ℃, the treatment time is 10s, cooling the membrane F at the temperature of 85 ℃, and then carrying out traction and rolling, wherein the thickness of the coating is 105nm, and the thickness of the polyester film is 188 microns, so that the finished product of the polyester film for optics is obtained.
Example 5
Taking an organic solvent, adding a wetting agent, blending to prepare a wetting agent solution, taking 50% of the total amount of deionized water in the components, slowly adding the wetting agent solution into the deionized water, mixing and uniformly stirring to obtain a solution A; adding deionized water into the water-based polyester for dilution to prepare a diluted solution, stirring the solution A, slowly adding the UV-resistant modified polyurethane, stirring uniformly, then slowly adding the water-based polyurethane, stirring uniformly, then slowly adding the diluted solution, and continuously stirring to obtain a solution B; stirring the solution B, taking deionized water to dilute melamine resin, taking an organic solvent and deionized water to dilute epoxy resin, respectively and slowly adding the organic solvent and the deionized water to the solution B, and continuously stirring to obtain a solution C; stirring the solution C, taking the nano particles to prepare an aqueous dispersion liquid with the silicon dioxide content of 40%, diluting the aqueous dispersion liquid by using deionized water, slowly adding the aqueous dispersion liquid into the solution C after uniformly stirring, adding the rest deionized water in the components after uniformly stirring, continuously stirring for 5min, adding a pH value regulator to adjust the pH value of the system to be 8.0, and continuously stirring for 1h to obtain an aqueous coating liquid with the solid content of 5%.
Taking a polyester base film with the water content of 10ppm, melting and extruding at the temperature of 270 ℃, filtering, then carrying out three-layer co-extrusion, and carrying out tape casting to obtain a membrane D; preheating the membrane D at the temperature of 70 ℃, heating by 70% of infrared rays, and longitudinally stretching at the longitudinal stretching ratio of 3 times to obtain a membrane E; coating the water-based coating liquid on one surface or two surfaces of the membrane E, wherein the wet coating amount of the single-surface coating is 13g/m2, and obtaining a membrane F; preheating the membrane F at the temperature of 100 ℃, then transversely stretching the membrane F at the temperature of 110 ℃, wherein the transverse stretching magnification is 3 times, carrying out heat setting treatment and drying solidification after stretching is finished, the treatment temperature is 220 ℃, the treatment time is 5s, cooling the membrane F at the temperature of 50 ℃, and then carrying out traction and rolling, wherein the thickness of the coating is 110nm, and the thickness of the polyester film is 250 mu m, so that the finished product of the polyester film for optics is obtained.
Example 6
Taking an organic solvent, adding a wetting agent, blending to prepare a wetting agent solution, taking 50% of the total amount of deionized water in the components, slowly adding the wetting agent solution into the deionized water, mixing and uniformly stirring to obtain a solution A; adding deionized water into the water-based polyester for dilution to prepare a diluted solution, stirring the solution A, slowly adding the UV-resistant modified polyurethane, stirring uniformly, then slowly adding the water-based polyurethane, stirring uniformly, then slowly adding the diluted solution, and continuously stirring to obtain a solution B; stirring the solution B, taking deionized water to dilute melamine resin, taking an organic solvent and deionized water to dilute epoxy resin, respectively and slowly adding the organic solvent and the deionized water to the solution B, and continuously stirring to obtain a solution C; stirring the solution C, taking the nano particles to prepare an aqueous dispersion liquid with the silicon dioxide content of 40%, diluting the aqueous dispersion liquid by using deionized water, slowly adding the aqueous dispersion liquid into the solution C after uniformly stirring, adding the rest deionized water in the components after uniformly stirring, continuously stirring for 5min, adding a pH value regulator to adjust the pH value of the system to be 8.0, and continuously stirring for 1h to obtain an aqueous coating liquid with the solid content of 5%.
Taking a polyester base film with the water content of 10ppm, melting and extruding at the temperature of 270 ℃, filtering, then carrying out three-layer co-extrusion, and carrying out tape casting to obtain a membrane D; preheating the membrane D at the temperature of 70 ℃, heating by 70% of infrared rays, and longitudinally stretching at the longitudinal stretching ratio of 3 times to obtain a membrane E; coating the water-based coating liquid on one surface or two surfaces of the membrane E, wherein the wet coating amount of the single-surface coating is 15g/m2, so as to obtain a membrane F; preheating the membrane F at the temperature of 100 ℃, then transversely stretching the membrane F at the temperature of 110 ℃, wherein the transverse stretching magnification is 3 times, carrying out heat setting treatment and drying solidification after stretching is finished, the treatment temperature is 220 ℃, the treatment time is 5s, cooling the membrane F at the temperature of 50 ℃, and then carrying out traction and rolling, wherein the coating thickness is 120nm, and the thickness of the polyester film is 250 mu m, so that the finished product of the polyester film for optics is obtained.
Comparative example 1
The film was coated with a common coating solution, and the remaining steps of the preparation of the polyester film for optical use were the same as in example 3, to obtain a finished polyester film for optical use having the same thickness and coating thickness as in example 3.
Comparative example 2
The waterborne polyurethane, the waterborne polyester and the modified polyurethane are replaced by the common waterborne polyurethane resin, the waterborne polyester resin and the polyurethane resin, and the rest processes and parameters are the same as those in the embodiment 3, so that the finished product of the polyester film for the optics, which has the same thickness and coating thickness as those in the embodiment 3, is obtained.
Comparative example 3
The waterborne polyurethane is replaced by the common polyurethane resin, and the rest processes and parameters are the same as those in the embodiment 3, so that the finished product of the polyester film for optics, which has the same thickness and coating thickness as those in the embodiment 3, is obtained.
Comparative example 4
The waterborne polyester is replaced by the common waterborne polyester resin, and the rest processes and parameters are the same as those in the example 3, so that the finished product of the polyester film for optical use, the thickness and the coating thickness of which are the same as those in the example 3, is obtained.
Comparative example 5
The modified polyurethane is replaced by the common polyurethane resin, and the rest processes and parameters are the same as those in the embodiment 3, so that the finished product of the polyester film for optics, the thickness of which is the same as that in the embodiment 3, is obtained.
Experiment of
Samples were prepared from the optical polyester films obtained in examples 1 to 6 and comparative examples 1 to 4, and the light transmittance, haze, friction coefficient and adhesion were measured and recorded:
wherein, the light transmittance and the haze are tested by adopting an AT-4725 transmission haze imaging instrument of Germany BYK company and using ASTM D1003 as a test standard;
testing the friction coefficient by adopting an FP-2260 friction coefficient tester of THWING-ALBERT company in the United states and taking ASTM D1894 as a test standard;
testing the adhesiveness by adopting a Baige method and taking ASTM D3359 as a test standard;
an aging test box with an ultraviolet lamp is adopted, and HG/T5659-2019 is used as a test standard to test the ultraviolet resistance;
and (3) testing the high temperature and high humidity resistance by taking the constant humidity and heat in GB/T26331-2010 as a test standard.
Figure BDA0002635502510000131
Figure BDA0002635502510000132
Figure BDA0002635502510000141
From the data in the table above, it is clear that the following conclusions can be drawn:
the comparison between the polyester optical films obtained in examples 1 to 6 and the optical polyester films obtained in comparative examples 1 to 5 shows that the transmittance and the adhesion of the polyester optical films in examples 1 to 6 are significantly improved compared with those of comparative examples 1 to 5, and the haze and the friction coefficient of the polyester optical films in examples 1 to 6 are significantly reduced compared with those of comparative examples 1 to 5, which fully illustrates that the transmittance and the haze adhesion of the optical polyester films are improved, the friction coefficient of the optical polyester films is reduced, and the experimental data and experimental phenomena show that the yellowing index of the optical polyester films is significantly reduced, the films and the bonding surfaces have no defects after constant moist heat, and the modification of the resin can improve the ultraviolet resistance and the high temperature and high humidity resistance of the optical polyester films, has stable effect and higher practicability.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Figure BDA0002635502510000161
TABLE 1

Claims (10)

1. The coating liquid for priming the optical polyester film is characterized by comprising the following components in parts by weight: 3-15% of waterborne polyurethane, 1-5% of waterborne polyester, 0.1-0.5% of melamine resin, 0.1-0.5% of epoxy resin, 0.3-1% of modified polyurethane, 0.5-1.5% of organic solvent, 0.05-0.3% of wetting agent, 0.1-1% of nano particles, 0.01-0.1% of pH value regulator and the balance of deionized water.
2. The coating liquid for undercoating an optical polyester film as claimed in claim 1, wherein: the solid content of the waterborne polyurethane is 39-41%.
3. The coating liquid for undercoating an optical polyester film as claimed in claim 1, wherein: the solid content of the water-based polyester is 33-35%, the molecular weight is 15000, and the hydroxyl value is 6 mgKOH/g.
4. The coating liquid for undercoating an optical polyester film as claimed in claim 1, wherein: the solid content of the modified polyurethane is 22-23%.
5. The coating liquid for undercoating an optical polyester film as claimed in claim 1, wherein: the organic solvent is absolute ethyl alcohol, the wetting agent is one or more of polyether modified polysiloxane and organic fluorocarbon wetting agents, the nano particles are silicon dioxide, and the particle size of the nano particles is 65 nm.
6. A preparation method of a coating liquid for priming an optical polyester film is characterized by comprising the following steps:
1) adding a wetting agent into an organic solvent for dilution, taking 50-80% of the total amount of deionized water in the components, adjusting the pH value to 8.0-9.0 by using an ammonia salt, slowly adding a wetting agent diluted solution into the deionized water, mixing and uniformly stirring to obtain a solution A;
2) adding deionized water with the weight 4 times that of the waterborne polyester into the waterborne polyester for dilution to prepare a diluted solution, stirring the solution A, slowly adding the UV-resistant modified polyurethane, stirring uniformly, then slowly adding the waterborne polyurethane, stirring uniformly, then slowly adding the diluted solution, and continuously stirring to obtain a solution B;
3) stirring the solution B, adding 1-2 times of deionized water by weight into melamine resin for dilution, taking an organic solvent and deionized water for diluting epoxy resin, wherein the weight ratio of epoxy resin to deionized water to ethanol is 1:1:1, slowly adding the prepared melamine resin diluted solution and epoxy resin diluted solution into the solution B respectively, continuously stirring for 5-25 min, and adjusting the pH value to 8.0-9.0 by using ammonia salt to obtain a solution C;
4) stirring the solution C, taking nanoparticles to prepare an aqueous dispersion liquid with the silicon dioxide content of 40%, diluting with deionized water of which the weight is 1-2 times that of the aqueous dispersion liquid, slowly adding the diluted solution into the solution C after uniformly stirring, adding the rest deionized water in the components after uniformly stirring, continuously stirring for 5-25 min, adding a pH value regulator to regulate the pH value of the system to be 8.0-9.0, and continuously stirring for 1-3 h to obtain an aqueous coating liquid with the solid content of 3-4%.
7. The coating liquid for undercoating an optical polyester film as claimed in claim 6, wherein: the preparation steps of the waterborne polyurethane are as follows:
taking hydroxyl silicone oil and methyl acrylate for grafting, mixing with an emulsifier and deionized water for emulsification, and finally adding aminosilane for reaction to prepare modified silicone oil;
taking polytetrahydrofuran diol, dicyclohexylmethane diisocyanate, 1, 3-propylene glycol and modified silicone oil as monomers, drying in a nitrogen atmosphere, heating, adding a catalyst to synthesize a polyurethane prepolymer, adding 2, 2' -dicarboxymethylpropionic acid as a chain extender, uniformly stirring, continuing to react, adding 1, 4-butanediol and trimethylolpropane, cooling to react, adding a silane coupling agent, and cooling again to react to obtain the waterborne polyurethane.
8. The coating liquid for undercoating an optical polyester film as claimed in claim 6, wherein: the preparation steps of the water-based polyester are as follows:
1, 4-cyclohexane dimethanol, biphenyl dicarboxylic acid and dimethyl isophthalate-5-sodium sulfonate are used as monomers for reaction and copolymerization, and prepolymer of phenoxy phosphoryl chloride and resorcinol is added, and the water-based polyester is prepared by heating and pressure increasing reaction.
9. The coating liquid for undercoating an optical polyester film as claimed in claim 6, wherein: the preparation steps of the modified polyurethane are as follows:
polycaprolactone diol, isophorone diisocyanate and dimethyl terephthalate are used as monomers to react and copolymerize, triethylene glycol bis-3-butyl-4-hydroxy-5-methylphenyl propionate is added, and the reacted products are blended with nano titanium dioxide modified polypropylene glycol to prepare the modified polyurethane.
10. The preparation method of the optical polyester film is characterized by comprising the following steps:
1) film forming:
taking a polyester base film with the water content of 0-50 ppm, melting and extruding at the temperature of 270-290 ℃, filtering, then carrying out three-layer co-extrusion, and carrying out tape casting to obtain a membrane D;
2) primary stretching:
preheating the membrane D at the temperature of 70-85 ℃, then heating by using 70-85% of infrared rays, and then longitudinally stretching with the longitudinal stretching magnification of 3-4 times to obtain a membrane E;
3) coating:
coating the aqueous coating solution obtained in claims 1 to 9 on one side of the surface of a film EThe wet coating amount of the coating is 5 to 15g/m2Obtaining a membrane F;
4) secondary stretching
Preheating the membrane F at the temperature of 100-130 ℃, then transversely stretching at the temperature of 110-150 ℃, wherein the transverse stretching magnification is 3-4 times, carrying out heat setting treatment and drying solidification after stretching is finished, wherein the treatment temperature is 220-250 ℃, the treatment time is 5-30 s, cooling at the temperature of 50-120 ℃, then carrying out traction and rolling, and the coating thickness is 80-120 nm at the moment, thus obtaining the finished product polyester film for optics.
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