CN102514275B - A kind of optical polyester film and preparation method thereof - Google Patents

A kind of optical polyester film and preparation method thereof Download PDF

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Publication number
CN102514275B
CN102514275B CN201110354876.2A CN201110354876A CN102514275B CN 102514275 B CN102514275 B CN 102514275B CN 201110354876 A CN201110354876 A CN 201110354876A CN 102514275 B CN102514275 B CN 102514275B
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priming coat
polyester
film
base film
filler
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CN102514275A (en
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李超
熊跃斌
霍新莉
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Lucky Healthcare Co ltd
Tianjin Lekai Film Technology Co ltd
Hefei Lucky Science and Technology Industry Co Ltd
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BAODING LUCKY FILM Co Ltd
Tianjin Lucky Bopet Co Ltd
Hefei Lucky Science and Technology Industry Co Ltd
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Abstract

A kind of optical polyester film and preparation method thereof, described film comprises the polyester base film of biaxial tension and is coated in the priming coat at least one surface of polyester base film, containing refractive index in described priming coat is the filler of 1.55 ~ 2.50, and the content forming solid content in the masking liquid of priming coat is 5% ~ 10% by weight.The present invention had both had high transparent, good adhesion and easily rolling, effectively can solve again produced problem after carrying out hard conating processing and interfere rainbow line, be applicable to various LCD optical functional film and high-grade type IMD film interior trim processes contour terminal membrane Material Field.

Description

A kind of optical polyester film and preparation method thereof
Technical field
The present invention relates to a kind of optical polyester film and preparation method thereof, in particular to the optical polyester film with anti-interference rainbow line, this optical polyester film is applicable to various LCD optical functional film and high-grade type IMD film interior trim processes contour terminal membrane Material Field.
Background technology
Polyester film mainly adopts stretch processes to make, when producing biaxially oriented polyester film, for avoiding producing cut at film surface, prevent rolling adhesion, known method adds particulate filler in polyester slice, but the interpolation of particulate filler, will affect the transparency of polyester film.
Optical polyester film is as the upstream materials of FPD, and its market potential is huge, in the middle of household electrical appliances proportion and range of application more and more extensive; Optical polyester film for high-grade type IMD film interior trim manufacture field requires to have good optical property, heat endurance, printing, shock-resistant, scratch-resistantly injure good chemical stability.For the purposes such as display and Dicoration base material, the large area of present market demands product, but the thing followed particularly requires more and more higher to the interference rainbow line that film carries out hard conating processing generation, due to fluorescent lamp be realize daylight repeatability and using three wavelength as main flow, more easily occur interfering rainbow line so carry out the optical polyester film after hard conating processing, the existence of rainbow line is interfered seriously to constrain the application of product, in the process using product, easily make people produce visual fatigue, therefore, how effectively to solve and interfere rainbow line, it is the problem that those skilled in the art are concerned about always.
Carrying out the generation of the optical polyester film after hard conating processing interferes rainbow line to produce due to polyester film refractive index and hard conating specific refractivity, in order to reduce this specific refractivity to prevent from interfering the generation of line.Japan Patent JP Laid-Open 7-151902 discloses a kind of method improving hard conating refractive index by adding metal oxide microparticle in hard coat resin, but its there are the following problems: the transparency, scratch resistance, soil resistance etc. of polyester film reduce because adding metal oxide microparticle in hard conating; The reflectivity by suppressing the back side is disclosed in Japan Patent TOHKEMY 2002-210906, the method of the hard conating of stacked particular stiffness, when the reverse side setting of the hard conating of film has the coating of specific refractive index and specific thicknesses, backside reflection rate must be controlled below 0.1%, but it is very difficult to control backside reflection rate in this way.
Summary of the invention
For solving the problem, the object of this invention is to provide a kind of optical polyester film, by to its modifying surface, make it both have high transparent, good adhesion and easily rolling, effectively can solve again produced problem after carrying out hard conating processing and interfere rainbow line.
Another object of the present invention is to provide the preparation method of above-mentioned optical polyester film.
For achieving the above object, the present invention takes following technical scheme:
A kind of optical polyester film, it comprises the polyester base film of biaxial tension and is coated in the priming coat at least one surface of polyester base film, after improvement, containing refractive index in described priming coat is the filler of 1.55 ~ 2.50, and the content forming solid content in the masking liquid of priming coat is 5% ~ 10% by weight.
Containing refractive index in described priming coat is the filler of 1.60 ~ 2.35.
The average diameter of described filler is 0.02 μm ~ 0.50 μm.
The average diameter of described filler is 0.05 μm ~ 0.20 μm.
The thickness of described priming coat is 0.05 ~ 0.2 μm.
Described filler is one or more in silica, zinc oxide, zinc sulphide, boron oxide, aluminium oxide, bismuth oxide, indium oxide, titanium dioxide, neodymium fluoride and zirconium dioxide.
A preparation method for optical polyester film, it carries out according to the following steps:
(1) melt extruded by dry polyester slice, melt is cooled to polyester base film sheet on slab roller;
(2) contain at least one surface coating of polyester base film sheet the priming coat masking liquid that refractive index is the filler of 1.55 ~ 2.50, the content of solid content is 5% ~ 10% by weight;
(3) by the polyester base film sheet longitudinal stretching 3.0 ~ 3.8 times of coating base coat masking liquid;
(4) by cross directional stretch 3.0 ~ 4.0 times again after the polyester base film preheating after longitudinal stretching, rolling, obtains optical polyester film.
Compared with prior art, the present invention has the following advantages:
1. do not contain filler in polyester base film of the present invention, ensure that optical polyester film high transparent;
2. by adding filler in priming coat, controlling the content of solid content in the masking liquid of the refractive index of filler in priming coat and formation priming coat, film is made to have good adhesiveness and easy rolling on the one hand, the interference rainbow line occurred after can preventing carrying out hard conating processing on the other hand;
3. by controlling the thickness of priming coat further, improve the fastness of optical polyester film and other functional resin interlayers on the one hand, ensure that priming coat can play the inhibition to interfering rainbow line on the other hand;
4. optical polyester film provided by the invention is applicable to various LCD optical functional film and high-grade type IMD film interior trim processes contour terminal membrane Material Field.
Detailed description of the invention
Polyester base film of the present invention is made primarily of polyester slice melting biaxial tension, polyester slice for biaxial tension mainly refers to the condensation product of binary acid and dihydroxylic alcohols, wherein, binary acid can be straight chain fatty acid, but mainly aromatic diacid, as terephthalic acid (TPA), to phenylenediacetic Acid, to naphthalenedicarboxylic acid etc.; Dihydroxylic alcohols mainly carbon number is the aliphatic diol of 2 ~ 4, as ethylene glycol, propane diols, butanediol etc.Except mentioned component, polyester slice can also be the polyester of the modification adding the materials such as a small amount of M-phthalic acid, phthalic acid.The condensation polymer of the preferred terephthalic acid (TPA) of the polyester slice in invention and ethylene glycol.
Priming coat of the present invention is coated at least one surface of polyester base film by priming coat masking liquid and is formed, and priming coat makes to have between polyester base film and other functional tree lipid layer excellent adhesiveness, and significantly improves its processing characteristics.Formed containing adhesive and high-refractive index particulate filler in the masking liquid of priming coat,
It can be solvent type for being applicable to adhesive of the present invention, also can be water-based, the adhesive dispersion emulsion of preferred water-based.Be applicable to adhesive of the present invention can be selected from polyesters, polyurethane type resin, modified polyurethane resin class, esters of acrylic acid, polyamide-based in one or more, in adhesive, add crosslinking agent as required, crosslinking agent preferentially uses one or more in hexamethylene diisocyanate (HDI), toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate (MDI), IPDI (IPDI), tetramethylxylylene diisocyanate (TMXDI).
High-refractive index particulate filler of the present invention refers to that refractive index is the filler of 1.55 ~ 2.50, preferred index is the filler of 1.6 ~ 2.35, when the refractive index of filler in priming coat be less than 1.55 or be greater than 2.50 time all effectively cannot prevent from carrying out hard conating processing after the interference rainbow line that occurs; The average diameter of high-refractive index particulate filler material is 0.02 μm ~ 0.50 μm, if average diameter is less than 0.02 μm, then because the addition of filler is more and reduce the partial optical performance of film, if average diameter is greater than 0.50 μm, then affect the adhesiveness of film and easy rolling, the average diameter of high-refractive index particulate filler material more preferably 0.05 μm ~ 0.20 μm.
High-refractive index particulate filler of the present invention can be selected from one or more in silica, zinc oxide, zinc sulphide, boron oxide, aluminium oxide, bismuth oxide, indium oxide, titanium dioxide, neodymium fluoride and zirconium dioxide.High-refractive index particulate uniform filling is dispersed in emulsion, uses, the aqueous dispersion emulsion of preferential oxidation silicon, zinc oxide, boron oxide, aluminium oxide, bismuth oxide, indium oxide, titanium dioxide, zirconium dioxide after forming dispersion emulsion.More preferably the aqueous dispersion emulsion of silica, boron oxide, aluminium oxide, bismuth oxide, indium oxide, zirconium dioxide.
Form the percentage by weight of the solid content of the masking liquid of priming coat 5% ~ 10%, preferred water paint, in order to improve the wetability of bottom masking liquid, the silicon or acrylic compounds etc. that can add appropriate amount in masking liquid improve the wetting agent of basement membrane, make underlying liquid energy even spread, also can add the additives such as antistatic additive, ultraviolet absorber, coupling agent and make priming coat have other functional characteristic such as antistatic, UV resistance.
Primer thickness in the present invention controls at 0.05 ~ 0.2 μm, to improve the fastness of optical polyester film and other functional resin interlayers, and ensures that priming coat plays the inhibition of interfering rainbow line.When the thickness of priming coat is lower than 0.05 μm or higher than 0.2 μm, poor for film surface adhesivity, and insufficient to what interfere rainbow line inhibition also to become.
In the present invention, on the surface of polyester base film, the process of coating base coat step before film biaxial tension completes, and coating method can adopt intaglio plate roller coat, bar to stitch the known manner such as painting, pneumatic blade coating, dip-coating.
The manufacture method of optical polyester film is as follows,
1. crystallization and drying
Poliester chip is the high polymer with moisture absorption tendency, pre-crystallized and dry process first must be carried out before carrying out biaxial tension, improve the softening point of polymer, avoid it in drying and melt extrude the mutual adhesion of resin particle in process, caking; Remove moisture in resin, prevent the polymer containing ester group from hydrolytic degradation and generation bubble occurring melt extruding in process.Pre-crystallized and baking temperature at about 160 ~ 180 DEG C, crystallization time 10 ~ 20min, 4 ~ 6 hours drying times.
2. melt extrude
Polyester slice after crystallizing and drying melt extrudes through extruder, and extruder temperature is 210 DEG C ~ 280 DEG C.
3. polyester base film slab
The melt melt extruded cools and forms polyester base film sheet on slab roller.
4. be coated with (In-line coating) online
The online one be coated with in modes such as using intaglio plate roller coat, bar seam painting, pneumatic blade coating, dip-coating, in the coating of the surface of polyester base film sheet containing adhesive and high-refractive index particulate filler priming coat masking liquid, the solids by weight percentage of masking liquid is 5% ~ 10%.
5. longitudinal stretching (MDO)
Longitudinal stretching is the longitudinal stretching polyester base film sheet from slab machine being carried out in a heated state 3.0 ~ 3.8 multiples by the speed difference between pull-down roller and fast withdrawing roll.
6. cross directional stretch (TDO)
Draw ratio: the cross directional stretch of 3.0 ~ 4.0 multiples, heat setting temperature 190 DEG C-210 DEG C.
7. draw rolling
Film, by controlled pressure roller, crimp roll, guide roller, finally completes rolling work.
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
The preparation of priming coat masking liquid:
Aqueous polyurethanes bottom adhesive emulsion NeoRoz R-620(DSM provides) 15 parts, wetting agent BYK-346(Bi Ke chemistry) 0.1 part, crosslinking agent V-02 (Nisshinbo system) 1 part, deionized water 80 parts, add and contain the dispersion emulsion 0.8 part that refractive index is 1.55, average diameter is the silica of 0.079 μm, be uniformly dispersed through high-shear emulsion machine, obtain the priming coat masking liquid that solid content is 5 quality %.
The preparation of polyester film:
Melt extruded by dry polyester slice, melt is cooled to polyester base film sheet on slab roller; By two of polyester base film sheet above-mentioned priming coat masking liquids prepared of surface coating; By the polyester base film sheet longitudinal stretching 3.8 times of surperficial coating base coat masking liquid; After the diaphragm preheating after longitudinal stretching, cross directional stretch 4.0 times, rolling after 190 DEG C of thermal finalizations, obtains the optical polyester film that thickness is 125um, and the thickness of priming coat is 0.05 μm, surveys its performance (see table 1).
Optical polyester film carries out coating UV hardening resin RC29-120(DIC), observation Surface Interference rainbow line (see table 1).
Embodiment 2
The preparation of priming coat masking liquid:
Aqueous polyesters bottom adhesive latex A LFA 15GE(ALFA) 18 parts; Wetting agent BYK-346 (Bi Ke chemistry) 0.1 part; Crosslinking agent V-02 (Nisshinbo system) 1 part; Deionized water 80 parts; Adding containing refractive index is 2.18, and average diameter is the dispersion emulsion 1 part of the zirconium dioxide of 0.02 μm, is uniformly dispersed through high-shear emulsion machine, obtains the priming coat masking liquid that solid content is 6 quality %.
The preparation of polyester film:
Melt extruded by dry polyester slice, melt is cooled to polyester base film sheet on slab roller; By two of polyester base film sheet above-mentioned priming coat masking liquids prepared of surface coating; By the polyester base film sheet longitudinal stretching 3.5 times of surperficial coating base coat masking liquid; After the diaphragm preheating after longitudinal stretching, cross directional stretch 3.5 times, rolling after 200 DEG C of thermal finalizations, obtains the optical polyester film that thickness is 175um, and the thickness of priming coat is 0.1 μm, surveys its performance (see table 1).
Optical polyester film carries out coating UV hardening resin RC28-608(DIC), observation Surface Interference rainbow line (see table 1).
Embodiment 3
The preparation of priming coat masking liquid:
Aqueous polyesters and polyurethanes mixing bottom adhesive latex A LFA 15GE(ALFA) 10 parts and NeoRoz R-620(DSM) 10 parts; Wetting agent BYK-346(Bi Ke chemistry) 0.1 part; Crosslinking agent V-02 (Nisshinbo system) 1 part; Deionized water 80 parts; Adding containing refractive index is 1.62, and average diameter is the dispersion emulsion 1.5 parts of the alundum (Al2O3) of 0.05 μm, is uniformly dispersed through high-shear emulsion machine, obtains the priming coat masking liquid that solid content is 8 quality %.
The preparation of polyester film:
Melt extruded by dry polyester slice, melt is cooled to polyester base film sheet on slab roller; By two of polyester base film sheet above-mentioned priming coat masking liquids prepared of surface coating; By the polyester base film sheet longitudinal stretching 3.0 times of surperficial coating base coat masking liquid; After the diaphragm preheating after longitudinal stretching, cross directional stretch 3.5 times, rolling after 210 DEG C of thermal finalizations, obtains the optical polyester film that thickness is 188um, and the thickness of priming coat is 0.15 μm, surveys its performance (see table 1).
Optical polyester film carries out coating UV hardening resin EKS-675(DIC), observation Surface Interference rainbow line (see table 1).
Embodiment 4
The preparation of priming coat masking liquid:
Aqueous polyesters and polyurethanes mixing bottom adhesive latex A LFA 15GE(ALFA) 10 parts and NeoRoz R-620(DSM) 10 parts; Wetting agent BYK-346(Bi Ke chemistry) 0.1 part; Crosslinking agent V-02 (Nisshinbo system) 1 part; Deionized water 80 parts; Add containing refractive index be 2.0, average diameter is the dispersion emulsion 1.0 parts that the indium oxide dispersion emulsion 0.5 part of 0.2 μm and refractive index are 2.3, average diameter is the boron oxide of 0.1 μm, be uniformly dispersed through high-shear emulsion machine, obtain the priming coat masking liquid that solid content is 10 quality %.
The preparation of polyester film:
Melt extruded by dry polyester slice, melt is cooled to polyester base film sheet on slab roller; By two of polyester base film sheet above-mentioned priming coat masking liquids prepared of surface coating; By the polyester base film sheet longitudinal stretching 3.0 times of surperficial coating base coat masking liquid; After the diaphragm preheating after longitudinal stretching, cross directional stretch 3.0 times, rolling after 210 DEG C of thermal finalizations, obtains the optical polyester film that thickness is 188um, and the thickness of priming coat is 0.2 μm, surveys its performance (see table 1).
Optical polyester film carries out coating UV hardening resin V-4025(DIC), observation Surface Interference rainbow line (see table 1).
Embodiment 5
The preparation of priming coat masking liquid:
Aqueous polyesters and polyurethanes mixing bottom adhesive latex A LFA 15GE(ALFA) 10 parts and NeoRoz R-620(DSM) 10 parts; Wetting agent BYK-346(Bi Ke chemistry) 0.1 part; Crosslinking agent V-02 (Nisshinbo system) 1 part; Deionized water 80 parts; Add containing refractive index be 2.45, average diameter be 0.5um bismuth oxide dispersion emulsion 0.5 part and containing refractive index be 1.62, average diameter is the alundum (Al2O3) dispersion emulsion 1.0 parts of 0.3 μm, be uniformly dispersed through high-shear emulsion machine, obtain the priming coat masking liquid that solid content is 10 quality %.
The preparation of polyester film:
Melt extruded by dry polyester slice, melt is cooled to polyester base film sheet on slab roller; By two of polyester base film sheet above-mentioned priming coat masking liquids prepared of surface coating; By the polyester base film sheet longitudinal stretching 3.0 times of surperficial coating base coat masking liquid; After the diaphragm preheating after longitudinal stretching, cross directional stretch 3.0 times, rolling after 200 DEG C of thermal finalizations, obtains the optical polyester film that thickness is 188um, and the thickness of priming coat is 0.2 μm, surveys its performance (see table 1).
Optical polyester film carries out coating UV hardening resin V-6841(DIC), observation Surface Interference rainbow line (see table 1).
Comparative example 1
By solvent identical with embodiment 1, dispersion emulsion is replaced with containing refractive index be 1.23, average diameter is the calcirm-fluoride dispersion emulsion 1.5 parts of 80nm, by manufacture method of the present invention, finally obtain the optical polyester film that thickness is 125um, survey its performance (see table 1).
Optical polyester film carries out coating UV hardening resin V-6841(DIC), observation Surface Interference rainbow line (see table 1).
Comparative example 2
By solvent identical with embodiment 1, do not add the particulate filler of high index of refraction.By manufacture method of the present invention, finally obtain the optical polyester film that thickness is 188um, survey its performance (see table 1).
Optical polyester film carries out coating UV hardening resin V-6841(DIC), observation Surface Interference rainbow line (see table 1).
Table 1: each embodiment performance data table
In table, the method for testing of properties is as follows:
1. light transmittance, mist degree:
Denshoku NDH-4000 tests by ASTM D1003 prescriptive procedure.
2. tack:
In film surface coating UV cured resin coating, hundred lattice method of testing resin bed tacks, judge that grade: 5B represents and do not come off; 4B comes off within representing 5% area; 3B represents that 5-15% area comes off; 2B represents that 15-35% area comes off; 1B represents that 35-65% area comes off; 0B represents that more than 65% area comes off.
3. interfere rainbow line:
Observation Surface Interference rainbow line, FNA-35 inspecting lamp, wavelength is 550 ~ 600nm, reflects visual, point A, B, C Three Estate.A indicate represent slight rainbow line without rainbow line, B, C represents serious rainbow line.

Claims (2)

1. the preparation method of an optical polyester film, described optical polyester film comprises the polyester base film of biaxial tension and is coated in the priming coat at least one surface of polyester base film, it is characterized in that, filler refractive index in described priming coat is 1.55 ~ 2.50, and the content forming solid content in the masking liquid of priming coat is 5% ~ 10% by weight;
The average diameter of described filler is 0.05 μm ~ 0.20 μm;
The thickness of described priming coat is 0.05 ~ 0.2 μm;
Described filler is one or more in silica, zinc oxide, zinc sulphide, boron oxide, aluminium oxide, bismuth oxide, indium oxide, titanium dioxide, neodymium fluoride and zirconium dioxide;
Preparation is carried out according to the following steps:
(1) melt extruded by dry polyester slice, melt is cooled to polyester base film sheet on slab roller;
(2) apply at least one surface of polyester base film sheet the priming coat masking liquid that refractive index is the filler of 1.55 ~ 2.50, the content of solid content is 5% ~ 10% by weight;
(3) by the polyester base film sheet longitudinal stretching 3.0 ~ 3.8 times of coating base coat masking liquid;
(4) by cross directional stretch 3.0 ~ 4.0 times again after the polyester base film preheating after longitudinal stretching, rolling, obtains optical polyester film.
2. method according to claim 1, is characterized in that, in described priming coat, the refractive index of filler is 1.60 ~ 2.35.
CN201110354876.2A 2011-11-10 2011-11-10 A kind of optical polyester film and preparation method thereof Active CN102514275B (en)

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Address after: 230041 Lekai Industrial Park, zone a, Xinzhan Industrial Park, Xinzhan District, Hefei City, Anhui Province

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