WO2014181620A1 - 光学フィルムの製造方法 - Google Patents
光学フィルムの製造方法 Download PDFInfo
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- WO2014181620A1 WO2014181620A1 PCT/JP2014/059951 JP2014059951W WO2014181620A1 WO 2014181620 A1 WO2014181620 A1 WO 2014181620A1 JP 2014059951 W JP2014059951 W JP 2014059951W WO 2014181620 A1 WO2014181620 A1 WO 2014181620A1
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Images
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/208—Filters for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation
Definitions
- the present invention relates to a method for producing an optical film. More specifically, the present invention relates to a method for manufacturing an optical film that includes a simultaneous multi-layer coating method and is unlikely to cause a coating failure.
- the optical film is a film that can transmit or reflect and absorb light, and can exhibit optical functions such as refraction, birefringence, antireflection, wide viewing angle, light diffusion, and brightness improvement.
- Optical films include liquid crystal displays (LCDs) and plasma displays as infrared shielding films, antireflection films, alignment films, polarizing films, polarizing plate protective films, retardation films, viewing angle widening films, brightness enhancement films, and electromagnetic wave shielding films. It is used for flat panel displays (FPD) such as (PDP), window glass of buildings and vehicles, and the like.
- LCDs liquid crystal displays
- plasma displays as infrared shielding films, antireflection films, alignment films, polarizing films, polarizing plate protective films, retardation films, viewing angle widening films, brightness enhancement films, and electromagnetic wave shielding films.
- FPD flat panel displays
- PDP flat panel displays
- an infrared shielding film that blocks transmission of heat rays (infrared rays) of sunlight is known (see, for example, Patent Documents 1 and 2).
- the infrared shielding film is a film in which a laminated film having a configuration in which a high refractive index layer and a low refractive index layer are alternately laminated is formed on a substrate, and the reflectance in a specific wavelength region of the infrared shielding film is It is determined by the refractive index difference between two adjacent layers, the number of layers, and the layer thickness.
- each of the coating liquids is applied and dried when the laminated film is formed on the substrate.
- a sequential multilayer coating method (sequential multilayer coating method) that repeats the above, a simultaneous multilayer coating method in which a plurality of coating liquids are stacked and then applied are used.
- the simultaneous multi-layer coating method is preferable in terms of high production efficiency.
- a coating liquid is applied using a slide type coater composed of a plurality of dies (bars) (see, for example, Patent Document 3).
- a slit is formed between the dies, and the tip surface of each die is the slide surface of the coater. And the coating liquid extruded from each slit is laminated
- a laminated film of the optical functional layer obtained due to various factors such as adhesion of foreign matters to the slide surface, etc., and the coating liquid not being stretched to a uniform thickness when the multilayer body of the coating liquid contacts the substrate In some cases, coating failure such as uneven film thickness or streaks may occur and the appearance of the optical film may be deteriorated.
- JP 2012-155052 A International Publication No. 2012/014644 JP 2013-667 A
- the present invention has been made in view of the above problems and situations, and the solution to the problem includes a coating process of a simultaneous multilayer coating method, and coating failure such as film thickness unevenness and streaks occurs in the laminated film of the optical functional layer. It is providing the manufacturing method of an optical film which is hard to carry out.
- the viscosity of the lowermost layer coating solution for forming the optical functional layer in contact with the substrate is 0.1 to 20 mPa ⁇ s
- the average thread length of the concentrated solution obtained by concentrating the lowermost layer coating solution to 50% by mass is 5 cm or less
- the lowermost layer coating solution has a uniform thickness when the multilayer body of the coating solution contacts the substrate.
- coating failure such as uneven film thickness and streaks is less likely to occur in the resulting laminated film of the optical functional layer. That is, the said subject which concerns on this invention is solved by the following means.
- An optical film manufacturing method for forming a laminated film comprising a plurality of optical functional layers on a substrate,
- the lowermost layer coating solution for forming the optical functional layer in contact with the substrate and the other coating solution for forming the optical functional layer are simultaneously coated on the substrate at a predetermined temperature and a predetermined speed.
- the lowermost layer coating solution has a viscosity at the predetermined temperature in the range of 0.1 to 20 mPa ⁇ s
- the concentrated solution obtained by concentrating the coating solution for the lowermost layer to 50% by mass immerses a glass rod having an outer diameter of 6 mm in the concentrated solution in the vertical direction for 3 cm, and vertically moves the glass rod at the predetermined temperature and the predetermined speed.
- An average film length is 5 cm or less when the length of the kite string when the kite string pulled out from the concentrated liquid is cut five times is measured.
- the said optical function layer contains polyvinyl alcohol
- the expression mechanism or action mechanism of the effect of the present invention is not clear, but is presumed as follows.
- the apparent molecular size of the polymer in the coating solution increases when bonds between polymer molecules in the coating solution and by end groups in the molecule, bonding in the cross-linking agent, and entanglement of molecules occur.
- the coating solution is in an inhomogeneous state in which a polymer having an apparent molecular size is mixed with a polymer having no apparent molecular size.
- the lowermost layer coating liquid in contact with the base material is A coating film is formed without being stretched to a uniform thickness, and as a result, coating failure such as uneven film thickness and streaks occurs in the obtained laminated film of the optical functional layer. Therefore, when the lowermost layer coating solution is kneaded to increase the homogeneity of the lowermost layer coating solution, the lowermost layer coating solution in contact with the base material is uniform when the multilayer solution is applied onto the substrate.
- the homogeneity of the lowermost layer coating solution is evaluated using the viscosity of the lowermost layer coating solution and the average yarn length of the concentrated solution obtained by concentrating the lowermost layer coating solution.
- the method for producing an optical film of the present invention is a method for producing an optical film in which a laminated film composed of a plurality of optical functional layers is formed on a substrate, and for the lowermost layer for forming the optical functional layer in contact with the substrate.
- a coating step in which a coating solution and another coating solution for forming the optical function layer are simultaneously coated on the substrate at a predetermined temperature and a predetermined speed, and the lowermost layer coating solution is the predetermined layer
- the concentrated solution in which the viscosity at a temperature of 0.1 to 20 mPa ⁇ s is in the range of 50% by mass with the lowermost layer coating solution is 3 cm in the vertical direction from a glass rod having an outer diameter of 6 mm to the concentrated solution.
- the average yarn length in the case where the length of the kite string is measured five times when the kite string is pulled up at the predetermined temperature and at the predetermined speed in the vertical direction and the kite string coming out of the concentrate is broken.
- the length is 5 cm or less.
- the “predetermined temperature” means a temperature at which the coating liquid is applied on the substrate in the coating process.
- the “predetermined speed” means a speed at which the coating liquid is applied onto the base material in the coating process.
- the laminated film has wavelength selectivity with respect to reflection or transmission of light from the viewpoint of manifesting the effects of the present invention.
- transmits a specific wavelength range can be manufactured.
- the said laminated film has infrared reflectivity.
- an infrared shielding film can be manufactured as an optical film.
- the said optical function layer contains polyvinyl alcohol. This makes it easy to control the refractive index of the optical functional layer. Moreover, in this invention, it is preferable that the difference of the saponification degree of the polyvinyl alcohol contained in the said optical function layer adjacent to each other is 3 mol% or more. Thereby, interlayer mixing between adjacent optical functional layers is suppressed.
- the predetermined speed is preferably in the range of 30 to 200 m / min. Thereby, generation
- the said concentrate has the said average thread length of 3 cm or less. Thereby, generation
- ⁇ is used to mean that the numerical values described before and after it are included as a lower limit value and an upper limit value.
- the optical film manufactured by the manufacturing method according to the present embodiment is a film in which a laminated film composed of a plurality of optical functional layers is formed on a substrate.
- the manufacturing method of the optical film is a simultaneous multi-layer coating method coating process, specifically, a lowermost layer coating solution for forming an optical functional layer in contact with a substrate, and a coating solution for forming another optical functional layer, A coating step of simultaneously applying multiple layers on the substrate at a predetermined temperature and a predetermined speed.
- the optical film has different functions depending on the composition and configuration of the optical functional layer. Therefore, the technical idea according to the present invention is various optical films, for example, an infrared shielding film, an antireflection film, an alignment film, a polarizing film, a polarizing plate protective film, a retardation film, by appropriately taking into account known matters. , A viewing angle widening film, a brightness enhancement film, and an electromagnetic wave shielding film.
- an infrared shielding film in which refractive index layers having different refractive indexes are laminated will be described, but the present invention is not limited thereto.
- a laminated film composed of a plurality of optical functional layers an optical film in which a laminated film having infrared reflectivity, specifically, a wavelength selective film that reflects infrared rays but transmits visible light is formed on a substrate is described.
- the present invention is not limited, and for example, a laminated film composed of a plurality of optical functional layers may have wavelength selectivity with respect to reflection or transmission of other light rays.
- the infrared shielding film corresponds to an optical film
- the refractive index layer corresponds to an optical functional layer.
- the refractive index differences between adjacent refractive index layers is preferably 0.1 or more, more preferably 0.3 or more, and particularly preferably 0.4 or more.
- it is preferable that all the refractive index differences between the laminated refractive index layers are within the preferable range.
- the outermost layer and the lowermost layer among the refractive index layers constituting the reflective layer may have a configuration outside the above preferred range.
- the reflectivity in a specific wavelength region is determined by the difference in refractive index between two adjacent layers, the number of layers and the thickness of the layer.
- the refractive index difference and the required number of layers can be calculated using commercially available optical design software. For example, in order to obtain an infrared reflectance of 90% or more, if the refractive index difference is smaller than 0.1, it is necessary to stack 100 layers or more. In such cases, productivity loss, increased scattering at the laminate interface, reduced transparency, and manufacturing failures can occur.
- the transmittance in the visible light region shown in JIS R3106: 1998 is preferably 50% or more, preferably 75% or more, more preferably 85% or more.
- the infrared shielding film has a configuration in which a refractive index layer is laminated, so that at least part of the infrared light is irradiated when infrared light is irradiated from the base material side or the laminated refractive index layer side. Can be shielded (reflected) to exhibit an infrared shielding effect.
- the stacked refractive index layers are formed by alternately stacking high refractive index layers and low refractive index layers.
- the laminated high refractive index layer and low refractive index layer may be the same or different.
- Whether the refractive index layer is a high refractive index layer or a low refractive index layer is determined by comparing the refractive index with the adjacent refractive index layer. Specifically, when a refractive index layer is used as a reference layer, if the refractive index layer adjacent to the reference layer has a lower refractive index than the reference layer, the reference layer is a high refractive index layer (the adjacent layer is a low refractive index layer).
- the refractive index of the adjacent layer is higher than that of the reference layer, it is determined that the reference layer is a low refractive index layer (the adjacent layer is a high refractive index layer).
- the refractive index (nH) of the high refractive index layer is: It is preferably 1.60 to 2.50, more preferably 1.70 to 2.50, further preferably 1.80 to 2.20, and 1.90 to 2.20. It is particularly preferred.
- the refractive index (nL) of the low refractive index layer is preferably 1.10 to 1.60, more preferably 1.30 to 1.55, and more preferably 1.30 to 1.50. More preferably.
- a sample is prepared by cutting a coating film obtained by applying a refractive index layer to be measured as a single layer on a support to a size of 10 cm ⁇ 10 cm.
- a surface (back surface) opposite to the measurement surface is roughened, and light absorption processing is performed with a black spray.
- the sample thus prepared was measured for 25 reflectances in the visible region (400 to 700 nm) under the condition of regular reflection at 5 degrees. An average value is obtained, and an average refractive index is obtained from the measurement result.
- the range of the total number of refractive index layers is preferably 200 layers or less, more preferably 100 layers or less, and even more preferably 50 layers or less from the viewpoint of productivity.
- the thickness of the refractive index layer per layer is preferably 1 to 1000 nm, more preferably 20 to 800 nm, and still more preferably 50 to 350 nm.
- the preparation step is a step of preparing a coating solution containing a polymer.
- a coating liquid for a high refractive index layer and a coating liquid for a low refractive index layer are prepared as coating liquids.
- composition of coating solution contains a polymer. Furthermore, a solvent, a crosslinking agent, metal oxide particles, an emulsion resin, and other additives may be included as necessary.
- the polymer that can be used is not particularly limited, and examples thereof include water-soluble polymers.
- the water-soluble polymer is not particularly limited, and examples thereof include a polymer having a reactive functional group, modified polyvinyl alcohol, gelatin, and thickening polysaccharide.
- water-soluble polymer means a G2 glass filter (maximum) when dissolved in water so that the concentration of 0.5% by mass is obtained at the temperature at which the water-soluble polymer is most dissolved. It means that the mass of the insoluble matter that is filtered off when filtering through pores of 40 to 50 ⁇ m is within 50 mass% of the added water-soluble polymer.
- polymer having reactive functional group examples include unmodified polyvinyl alcohols, polyvinylpyrrolidones, polyacrylic acid, acrylic acid-acrylonitrile copolymer, potassium acrylate-acrylonitrile copolymer, and vinyl acetate.
- -Acrylic resin such as acrylic acid ester copolymer or acrylic acid-acrylic acid ester copolymer, styrene-acrylic acid copolymer, styrene-methacrylic acid copolymer, styrene-methacrylic acid-acrylic acid ester copolymer Styrene-acrylic resin such as styrene- ⁇ -methylstyrene-acrylic acid copolymer or styrene- ⁇ -methylstyrene-acrylic acid-acrylic acid ester copolymer, styrene-sodium styrenesulfonate copolymer, styrene- 2-hydroxye Tyl acrylate copolymer, styrene-2-hydroxyethyl acrylate-potassium styrene sulfonate copolymer, styrene-maleic acid copolymer, styrene-male
- the form of the copolymer when the polymer having the reactive functional group is a copolymer may be any of a block copolymer, a random copolymer, a graft copolymer, and an alternating copolymer. Good.
- the modified polyvinyl alcohol used in the present invention is one obtained by subjecting unmodified polyvinyl alcohol to one or more arbitrary modification treatments.
- examples thereof include amine-modified polyvinyl alcohol, ethylene-modified polyvinyl alcohol, carboxylic acid-modified polyvinyl alcohol, diacetone-modified polyvinyl alcohol, thiol-modified polyvinyl alcohol, and acetal-modified polyvinyl alcohol.
- these modified polyvinyl alcohols commercially available products may be used, or those produced by methods known in the art may be used.
- modified polyvinyl alcohols such as polyvinyl alcohol having a cation-modified terminal, anion-modified polyvinyl alcohol having an anionic group, and nonion-modified polyvinyl alcohol may also be used.
- Examples of the cation-modified polyvinyl alcohol include primary to tertiary amino groups and quaternary ammonium groups as described in JP-A-61-10383 in the main chain or side chain of the polyvinyl alcohol. It can be obtained by saponifying a copolymer of an ethylenically unsaturated monomer having a cationic group and vinyl acetate.
- Examples of the ethylenically unsaturated monomer having a cationic group include trimethyl- (2-acrylamido-2,2-dimethylethyl) ammonium chloride and trimethyl- (3-acrylamido-3,3-dimethylpropyl) ammonium chloride.
- the ratio of the ethylenically unsaturated monomer having a cationic group in the cation-modified polyvinyl alcohol is 0.1 to 10 mol%, preferably 0.2 to 5 mol%, relative to vinyl acetate.
- anion-modified polyvinyl alcohol examples include polyvinyl alcohol having an anionic group as described in JP-A-1-206088, JP-A-61-237681 and JP-A-63-307979. And a copolymer of a vinyl compound having a water-soluble group and a modified polyvinyl alcohol having a water-soluble group as described in JP-A-7-285265.
- Nonionic modified polyvinyl alcohol includes, for example, a polyvinyl alcohol derivative in which a polyalkylene oxide group as described in JP-A-7-9758 is added to a part of vinyl alcohol, and JP-A-8-25795.
- the block copolymer of the vinyl compound and vinyl alcohol which have the described hydrophobic group is mentioned.
- modified polyvinyl alcohols (1) one or more selected from the group consisting of unmodified polyvinyl alcohol having an average degree of polymerization of 200 or more and 2400 or less, and (2) unsaturated carboxylic acid, its salt and ester It is preferable to use a copolymer (graft copolymer) obtained by copolymerizing with a polymerizable vinyl monomer.
- the modified polyvinyl alcohol is the above graft copolymer
- the above-mentioned various modified polyvinyl alcohols are used as the unmodified polyvinyl alcohol having an average degree of polymerization of 200 or more and 2400 or less constituting the graft copolymer (1). May be.
- the unmodified polyvinyl alcohol used as the raw material for the modified polyvinyl alcohol has an average degree of polymerization of about 200 to 2400, preferably an average degree of polymerization of about 900 to 2400, and more preferably an average degree of polymerization of about 1300 to 1700.
- the degree of saponification of unmodified polyvinyl alcohol is preferably about 60 to 100 mol%, more preferably 78 to 96 mol%.
- Such a saponified polyvinyl alcohol can be produced by radical polymerization of vinyl acetate and appropriately saponifying the obtained polyvinyl acetate.
- the polymerization degree and saponification degree are controlled by a method known per se.
- polyvinyl alcohol As such partially saponified polyvinyl alcohol, commercially available products can also be used.
- Preferred examples of commercially available unmodified polyvinyl alcohol include Gohsenol EG05, EG25 (manufactured by Nippon Synthetic Chemical Industry Co., Ltd.), PVA- 203 (manufactured by Kuraray Co., Ltd.), PVA-204 (manufactured by Kuraray Co., Ltd.), PVA-205 (manufactured by Kuraray Co., Ltd.), JP-04 (manufactured by Nihon Museum & Poval Co., Ltd.), JP-05 (Japan Poval Co., Ltd.).
- unmodified polyvinyl alcohol not only one kind of unmodified polyvinyl alcohol is used alone as a raw material for the modified polyvinyl alcohol, but also two or more kinds of unmodified polyvinyl alcohols having different degrees of polymerization and saponification may be appropriately used in accordance with the purpose. Can do.
- unmodified polyvinyl alcohol having an average polymerization degree of 300 and unmodified polyvinyl alcohol having an average polymerization degree of 1500 can be mixed and used.
- Examples of the polymerizable vinyl monomer that is polymerized with the raw unmodified (modified) polyvinyl alcohol include unsaturated carboxylic acids such as acrylic acid, methacrylic acid, crotonic acid, fumaric acid, maleic acid, itaconic acid, or salts thereof (for example, Alkali metal salts, ammonium salts, alkylamine salts), esters thereof (eg, substituted or unsubstituted alkyl esters, cyclic alkyl esters, polyalkylene glycol esters), unsaturated nitriles, unsaturated amides, aromatic vinyls , Aliphatic vinyls, unsaturated bond-containing heterocycles, and the like.
- unsaturated carboxylic acids such as acrylic acid, methacrylic acid, crotonic acid, fumaric acid, maleic acid, itaconic acid, or salts thereof (for example, Alkali metal salts, ammonium salts, alkylamine salts), esters thereof (eg
- acrylic acid esters include, for example, methyl acrylate, ethyl acrylate, butyl acrylate, isobutyl acrylate, cyclohexyl acrylate, 2-ethylhexyl acrylate, hydroxyethyl acrylate, polyethylene glycol acrylate (polyethylene glycol and acrylic acid Ester) and polypropylene glycol acrylate (ester of polypropylene glycol and acrylic acid).
- methacrylic acid esters examples include methyl methacrylate, ethyl methacrylate, butyl methacrylate, isobutyl methacrylate, cyclohexyl methacrylate, and 2-ethylhexyl.
- Unsaturated nitriles such as acrylonitrile, methacrylonitrile, etc.
- Unsaturated amides such as acrylamide, dimethylacrylamide, methacrylamide
- aromatic vinyls such as styrene and ⁇ -methylstyrene
- aliphatic vinyls such as vinyl acetate
- unsaturated bond-containing heterocycles such as N -Vinylpyrrolidone, acryloylmorpholine and the like
- the above-mentioned modified polyvinyl alcohol can be produced by modifying unmodified polyvinyl alcohol or a derivative thereof by a method known per se.
- examples of the method for producing the graft copolymer as the modified polyvinyl alcohol include methods known per se such as radical polymerization, for example, solution polymerization, suspension polymerization, emulsion polymerization, and bulk polymerization. It can be carried out under normal polymerization conditions.
- This polymerization reaction is usually performed in the presence of a polymerization initiator, if necessary, as a reducing agent (for example, sodium erythorbate, sodium metabisulfite, ascorbic acid), a chain transfer agent (for example, 2-mercaptoethanol, ⁇ -methylstyrene).
- a polymerization initiator for example, sodium erythorbate, sodium metabisulfite, ascorbic acid
- a chain transfer agent for example, 2-mercaptoethanol, ⁇ -methylstyrene
- pulverization method, etc. may be a well-known method, and there is no restriction
- gelatin examples of gelatin used in the present invention include various types of gelatin that have been widely used in the field of silver halide photographic materials.
- enzyme-treated gelatin and gelatin derivatives that undergo enzyme treatment in the production process of gelatin that is, amino, imino, hydroxy, or carboxy groups as functional groups in the molecule It may be modified by treating with a reagent having a group obtained by reacting with it.
- the general method for producing gelatin is well known and is described, for example, in T.W. H. James: The Theory of Photographic Process 4th. ed. Reference can be made to descriptions such as 1977 (Macmillan), p. 55, Science Photo Handbook (above), p.
- the thickening polysaccharide used in the present invention is not particularly limited, and examples thereof include generally known natural simple polysaccharides, natural complex polysaccharides, synthetic simple polysaccharides, and synthetic complex polysaccharides.
- synthetic simple polysaccharides include generally known natural simple polysaccharides, natural complex polysaccharides, synthetic simple polysaccharides, and synthetic complex polysaccharides.
- synthetic simple polysaccharides for details of these thickening polysaccharides, reference can be made to “Biochemical Dictionary (2nd edition)” (Tokyo Kagaku Dojin), “Food Industry”, Vol. 31 (1988), p.
- the thickening polysaccharide is a polymer of saccharides and has a large number of hydrogen bonding groups in the molecule. Due to the difference in hydrogen bonding strength between molecules depending on the temperature, the viscosity at low temperature and the viscosity at high temperature are different. It is a polysaccharide with the characteristic that the difference is large, and when metal oxide particles or polyvalent metal compounds are further added, the metal oxide particles or polyvalent metals react with the metal oxide particles or polyvalent metal compounds at low temperatures. It forms a hydrogen bond or an ionic bond with a compound to cause an increase in viscosity or gelation.
- the increase in viscosity is preferably at least 1.0 mPa ⁇ s at 15 ° C.
- the viscosity increase width is more preferably 5.0 mPa ⁇ s or more, and further preferably 10.0 mPa ⁇ s or more.
- the viscosity is a value measured with a Brookfield viscometer or a B-type viscometer.
- thickening polysaccharides applicable to the present invention include, for example, pectin, galactan (eg, agarose, agaropectin, etc.), galactomannoglycan (eg, locust bean gum, guaran, etc.), xyloglucan, etc.
- glucomannoglycan eg, konjac mannan, wood-derived glucomannan, xanthan gum, etc.
- galactoglucomannoglycan eg, softwood-derived glycan
- arabinogalactoglycan For example, soybean-derived glycan, microbial-derived glycan, etc.
- glucoraminoglycan eg, gellan gum
- glycosaminoglycan eg, hyaluronic acid, keratan sulfate, etc.
- alginic acid and alginate agar, ⁇ -carrageenan, ⁇ -Carragina
- Natural macromolecular polysaccharides derived from red algae such as chloromethane, ⁇ -carrageenan, and far cerulean
- celluloses such as carboxymethyl cellulose (cellulose carboxymethyl ether), carboxyethyl cellulose, methyl
- polysaccharides include pentoses such as L-arabitose, D-ribose, 2-deoxyribose and D-xylose, and hexoses such as D-glucose, D-fructose, D-mannose and D-galactose only. It is preferable that it is a polysaccharide.
- tamarind seed gum known as xyloglucan whose main chain is glucose and side chain is glucose
- guar gum known as galactomannan whose main chain is mannose and side chain is glucose
- cationized guar gum Hydroxypropyl guar gum
- locust bean gum locust bean gum
- tara gum arabinogalactan whose main chain is galactose and whose side chain is arabinose
- arabinogalactan whose main chain is galactose and whose side chain is arabinose
- the above-mentioned polymers may be used alone or in combination of two or more, but at least polyvinyl alcohol (either unmodified polyvinyl alcohol or modified polyvinyl alcohol) is preferably used.
- polyvinyl alcohol used as the polymer, the refractive index of the refractive index layer can be easily controlled, and a desired refractive index can be easily obtained.
- the viscosity and spinnability of the coating liquid are likely to be high.
- the viscosity and the average thread length of the concentrated liquid are used for the lowermost layer coating liquid.
- the difference in the saponification degree of polyvinyl alcohol contained in the adjacent refractive index layers is preferably 3 mol% or more.
- the saponification degree of polyvinyl alcohol contained in the reference layer that is, polyvinyl alcohol contained in the coating solution for the reference layer
- the saponification degree of polyvinyl alcohol contained in the adjacent refractive index layer preferably has a difference of 3 mol% or more.
- the saponification degree is the ratio (percentage) of units actually saponified to vinyl alcohol units among units that can be converted to vinyl alcohol units by saponification.
- the weight average molecular weight of the polymer is preferably 1000 or more, more preferably from 5000 to 1000000, and further preferably from 10,000 to 100,000.
- the weight average molecular weight is a gel permeation chromatography (GPC) analyzer using a TSKgel GMHxL, TSKgel G4000HxL or TSKgel G2000HxL (Tosoh Corporation) column (solvent: tetrahydrofuran (THF)).
- GPC gel permeation chromatography
- the concentration of the polymer in the coating solution is preferably 0.01 to 20% by mass, and more preferably 0.1 to 10% by mass. It is preferable for the concentration of the polymer to be in the above range since the coating solution has a certain viscosity and can be advantageous for film formation.
- solvent Although the solvent which can be used by this invention is not restrict
- the organic solvent examples include alcohols such as methanol, ethanol, 2-propanol, and 1-butanol; esters such as ethyl acetate, butyl acetate, propylene glycol monomethyl ether acetate, and propylene glycol monoethyl ether acetate; diethyl ether; Examples include ethers such as propylene glycol monomethyl ether and ethylene glycol monoethyl ether; amides such as dimethylformamide and N-methylpyrrolidone; ketones such as acetone, methyl ethyl ketone, acetylacetone and cyclohexanone. These organic solvents may be used alone or in admixture of two or more. From the viewpoint of environment and simplicity of operation, the solvent of the coating solution is preferably water or a mixed solvent of water and methanol, ethanol, or ethyl acetate, and more preferably water.
- the crosslinking agent has a function of curing the polymer. By curing, water resistance can be imparted to the refractive index layer.
- the crosslinking agent that can be used is not particularly limited as long as it causes a curing reaction with a polymer.
- boric acid and its salt oxygen acid and its salt having a boron atom as a central atom
- orthoboric acid and diboric acid specifically, orthoboric acid and diboric acid , Metaboric acid, tetraboric acid, pentaboric acid, and octaboric acid or salts thereof are preferably used.
- Boric acid and its salt may be used alone or in combination of two or more, and it is particularly preferable to use a mixed aqueous solution of boric acid and borax.
- crosslinking agent examples include, for example, diglycidyl ethyl ether, ethylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether, 1,6-diglycidyl cyclohexane, N, N-diglycidyl-4-glycidyl.
- Epoxy crosslinking agents such as oxyaniline, sorbitol polyglycidyl ether, and glycerol polyglycidyl ether; aldehyde crosslinking agents such as formaldehyde and glioxal; 2,4-dichloro-4-hydroxy-1,3,5-S -Active halogen-based crosslinking agents such as triazine; active vinyl-based compounds such as 1,3,5-tris-acryloyl-hexahydro-S-triazine, bisvinylsulfonylmethyl ether; aluminum alum and the like.
- the crosslinking agent for example, organic compounds such as vinylsulfone compounds, urea-formalin condensates, melanin-formalin condensates, epoxy compounds, aziridine compounds, active olefins, isocyanate compounds, etc.
- Hardeners, inorganic polyvalent metal salts such as chromium, aluminum and zirconium may be used.
- the concentration of the crosslinking agent in the coating solution is preferably 0.001 to 20% by mass, and more preferably 0.01 to 10% by mass.
- the coating solution has a certain spinnability and viscosity, which is advantageous for film formation, and the formed refractive index layer can have suitable water resistance.
- the metal oxide particles which can be used is not particularly limited, titanium oxide (TiO 2), zinc oxide (ZnO), zirconium oxide (ZrO 2), niobium oxide (Nb 2 O 5), aluminum oxide (Al 2 O 3 ), silicon oxide (SiO 2 ), calcium fluoride (CaF 2 ), magnesium fluoride (MgF 2 ), indium tin oxide (ITO), antimony tin oxide (ATO), and the like.
- titanium oxide (TiO 2 ) is preferably used for the high refractive index layer coating solution
- silicon oxide (SiO 2 ) is preferably used for the low refractive index layer coating solution.
- titanium oxide TiO 2
- rutile type titanium oxide having a high refractive index and low catalytic activity. If the catalytic activity is low, side reactions (photocatalytic reactions) that occur in the refractive index layer and adjacent layers can be suppressed, and the weather resistance can be increased.
- a water-based titanium oxide sol having a pH of 1.0 to 3.0 and having a positive zeta potential of titanium particles is hydrophobized so that it can be dispersed in an organic solvent.
- examples of the method for preparing the aqueous titanium oxide sol include JP-A-63-17221, JP-A-7-819, JP-A-9-165218, JP-A-11-43327, JP-A-63. Reference can be made to the matters described in JP-A-17221, JP-A-7-819, JP-A-9-165218, JP-A-11-43327, and the like.
- the production method according to the step (2) is a step of treating titanium dioxide hydrate with at least one basic compound selected from the group consisting of alkali metal hydroxides and alkaline earth metal hydroxides.
- the titanium dioxide dispersion obtained in (1) is treated with a carboxylic acid group-containing compound and an inorganic acid.
- an aqueous sol of titanium oxide having a pH adjusted to 1.0 to 3.0 with an inorganic acid in the step (2) can be used.
- Examples of the silicon oxide (SiO 2 ) include synthetic amorphous silica and colloidal silica. Of these, an acidic colloidal silica sol is more preferably used, and a colloidal silica sol dispersed in water and / or an organic solvent is more preferably used.
- the colloidal silica can be obtained by heating and aging a silica sol obtained by metathesis with an acid of sodium silicate or the like and passing through an ion exchange resin layer.
- Such colloidal silica is disclosed in, for example, JP-A-57-14091, JP-A-60-219083, JP-A-60-218904, JP-A-61-20792, JP-A-61- No. 188183, No. 63-17807, No.
- Colloidal silica may be a synthetic product or a commercially available product.
- the metal oxide particles may be used alone or in combination of two or more.
- the average particle size of the metal oxide particles is preferably 2 to 100 nm, more preferably 3 to 50 nm, and further preferably 4 to 30 nm.
- the average particle size of the metal oxide particles is determined by observing the particles themselves or the particles appearing on the cross section or surface of the refractive index layer with an electron microscope, measuring the particle size of 1000 arbitrary particles, and calculating the simple average value ( (Number average).
- the particle diameter of each particle is represented by a diameter assuming a circle equal to the projected area.
- the concentration of the metal oxide particles in the coating solution is preferably 20 to 70% by mass and more preferably 30 to 70% by mass with respect to 100% by mass of the solid content of the refractive index layer. It is preferable that the content of the metal oxide particles is 20% by mass or more because a desired refractive index can be obtained. Further, it is preferable that the content of the metal oxide particles is 70% by mass or less because flexibility of the film can be obtained and film formation becomes easy.
- both refractive index layers having different refractive indexes include metal oxide particles
- anionization treatment or cationization treatment is performed, It is preferable to have the same ionicity (charge).
- anionization treatment or cationization treatment By performing anionization treatment or cationization treatment, a repulsive force is generated between the two types of metal oxide particles.
- a refractive index layer is formed by applying multiple layers, aggregation at a layer interface, etc. Can be difficult to occur.
- anionization treatment of metal oxide particles for example, anion treatment of titanium oxide is exemplified.
- the titanium oxide particles can be anionized by coating with a silicon-containing hydrated oxide.
- the coating amount of the silicon-containing hydrated compound is usually 3 to 30% by mass, preferably 3 to 10% by mass, and more preferably 3 to 8% by mass. When the coating amount is 30% by mass or less, a desired refractive index of the high refractive index layer can be obtained, and when the coating amount is 3% or more, particles can be stably formed.
- the cationization treatment of the metal oxide particles can be performed by using, for example, a cationic compound.
- the cationic compound include a cationic polymer and a polyvalent metal salt, and a polyvalent metal salt is preferred from the viewpoint of adsorption power and transparency.
- polyvalent metal salts include aluminum, calcium, magnesium, zinc, iron, strontium, barium, nickel, copper, scandium, gallium, indium, titanium, zirconium, tin, lead, and other metal hydrochlorides, sulfates, nitrates, Examples include acetate, formate, succinate, malonate, chloroacetate and the like.
- water-soluble aluminum compounds water-soluble calcium compounds, water-soluble magnesium compounds, water-soluble zinc compounds, and water-soluble zirconium compounds are preferably used, and water-soluble aluminum compounds and water-soluble zirconium compounds are more preferably used.
- the water-soluble aluminum compound include polyaluminum chloride (basic aluminum chloride), aluminum sulfate, basic aluminum sulfate, aluminum potassium sulfate (alum), ammonium aluminum sulfate (ammonium alum), sodium aluminum sulfate, aluminum nitrate, Examples thereof include aluminum phosphate, aluminum carbonate, polysulfuric acid aluminum silicate, aluminum acetate, and basic aluminum lactate.
- the coating amount of the cationic compound varies depending on the shape and particle size of the metal oxide particles, but is preferably 1 to 15% by mass with respect to the metal oxide particles.
- the emulsion resin is usually a polymer dispersed in a coating solution.
- the emulsion resins can be fused to each other at the time of application in an application process described later.
- the emulsion resin is obtained by emulsion polymerization of an oil-soluble monomer using a polymer dispersant or the like.
- the oil-soluble monomer that can be used is not particularly limited, but ethylene, propylene, butadiene, vinyl acetate and its partial hydrolyzate, vinyl ether, acrylic acid and its esters, methacrylic acid and its esters, acrylamide and its derivatives, Examples include methacrylamide and derivatives thereof, styrene, divinylbenzene, vinyl chloride, vinylidene chloride, maleic acid, vinyl pyrrolidone, and the like. Of these, acrylic acid, its esters, and vinyl acetate are preferably used from the viewpoint of transparency and particle size. As acrylic acid and / or its esters and vinyl acetate emulsion, commercially available ones may be used.
- the dispersant that can be used is not particularly limited, but in addition to a low-molecular dispersant such as alkyl sulfonate, alkylbenzene sulfonate, diethylamine, ethylenediamine, and quaternary ammonium salt, polyoxyethylene nonylphenyl is used.
- a low-molecular dispersant such as alkyl sulfonate, alkylbenzene sulfonate, diethylamine, ethylenediamine, and quaternary ammonium salt
- polyoxyethylene nonylphenyl examples thereof include polymer dispersants such as ether, polyethylene ethylene laurate, hydroxyethyl cellulose, and polyvinyl pyrrolidone.
- the above-mentioned emulsion preferably has a glass transition temperature (Tg) of 20 ° C. or lower, more preferably ⁇ 30 to 10 ° C. from the viewpoint of enhancing flexibility.
- Tg glass transition temperature
- additives include ultraviolet absorbers described in JP-A-57-74193, JP-A-57-87988, and JP-A-62-261476, various surfactants of anion, cation, or nonion, sulfuric acid, PH adjusters such as phosphoric acid, acetic acid, citric acid, sodium hydroxide, potassium hydroxide, potassium carbonate, antifoaming agents, lubricants such as diethylene glycol, antiseptics, antifungal agents, antistatic agents, matting agents, antioxidants And various known additives such as additives, flame retardants, infrared absorbers, dyes and pigments.
- PH adjusters such as phosphoric acid, acetic acid, citric acid, sodium hydroxide, potassium hydroxide, potassium carbonate, antifoaming agents, lubricants such as diethylene glycol, antiseptics, antifungal agents, antistatic agents, matting agents, antioxidants
- additives flame retardants, infrared absorbers, dyes and pigments.
- the method for preparing the coating solution is not particularly limited, and examples thereof include a method in which a polymer and, if necessary, additives such as a crosslinking agent and metal oxide particles are added to a solvent and mixed with stirring.
- the order of addition of the respective components is not particularly limited, and the respective components may be sequentially added and mixed while stirring, or may be added and mixed at one time while stirring.
- the “lowermost layer” means a refractive index layer in contact with the base material among the plurality of refractive index layers formed on the base material.
- the “predetermined temperature” means a temperature at which the coating liquid is applied onto a substrate that is applied in an application process described later. The viscosity is measured with a Brookfield viscometer or a B-type viscometer as described above.
- the present invention is characterized in that the average thread length of the concentrated solution of the lowermost layer coating solution is 5 cm or less.
- the “concentrated liquid of the lowermost layer coating liquid” means a liquid concentrated by evaporating the solvent from the prepared lowermost layer coating liquid to 50% by mass.
- the “average string length” means that a glass rod having an outer diameter of 6 mm is immersed in a concentrated solution in a vertical direction by 3 cm, and the glass rod is pulled up in a vertical direction at a predetermined temperature and a predetermined speed. It means the average value when the length of the kite string when the exit kite is broken is measured five times.
- the “predetermined temperature” and the “predetermined speed” mean the temperature and speed at which the coating liquid is applied onto the substrate in the coating process described later.
- the length of the kite string when the kite string coming out of the concentrate is broken means the liquid level of the concentrate at the time when the kite string is broken—the length of the tip of the glass rod.
- the measurement of the string length performed five times may be performed continuously, or may be performed at regular intervals (for example, 3 seconds to 10 minutes). Further, the measurement of the length of the kite is performed by visual observation and photographing with a video camera.
- Factors that affect the viscosity and spinnability of the coating solution include bonding between end groups of the polymer in the coating solution and within the molecule, bonding in the cross-linking agent, and entanglement between molecules. Due to the occurrence of such bonds and entanglements, some of the polymers in the coating solution have an increased apparent molecular size, which increases the viscosity and spinnability of the coating solution. In other words, when such bonds, entanglements, and the like occur, the coating liquid is in a heterogeneous state in which a polymer having an apparent molecular size is mixed with a polymer having no apparent molecular size.
- the lower the homogeneity of the coating solution the higher the viscosity and spinnability of the coating solution.
- using the viscosity of the lowermost layer coating solution and the average string length of the concentrated solution The homogeneity of the coating solution for the lowermost layer is evaluated.
- the lowermost layer coating solution having a viscosity in the range of 0.1 to 20 mPa ⁇ s is used as it is for the measurement of the kite length, problems such as no formation of the kite occur, and the homogeneity of the lowermost layer coating solution. Therefore, in the present invention, a concentrated solution is produced in order to improve the spinnability, and the length of the kite is measured using the concentrated solution.
- the lowermost layer coating solution has a high degree of homogeneity, if the lowermost layer coating solution does not have a certain viscosity, it contacts the substrate when a multilayer body of the coating solution is applied onto the substrate. A tear or a hole is formed in the layer of the lowermost layer coating solution, and a coating film is formed without the lowermost layer coating solution being stretched to a uniform thickness. As a result, coating failure such as film thickness unevenness and streaks occurs in the obtained laminated film of refractive index layers. When a coating failure such as uneven film thickness or streaks occurs in the obtained refractive index layer, the transmitted light is refracted and the appearance (appearance) of the infrared shielding film is deteriorated.
- the film thickness of the laminated film of the refractive index layer obtained by using the lowermost layer coating solution having a viscosity of 0.1 to 20 mPa ⁇ s and an average string length of the concentrated solution of 5 cm or less Occurrence of coating failures such as unevenness and streaks can be suppressed. And the said effect is acquired irrespective of the component of a lowermost-layer coating liquid, coating conditions, etc. The reason for this is that the viscosity and the average string length are physically measured regardless of the components of the lowermost layer coating liquid, and when the coating liquid is applied onto the substrate in the coating process described later. This is because it is measured in consideration of the temperature and speed.
- the lowermost layer coating solution can be stretched to a uniform thickness by using the lowermost layer coating solution having a viscosity of 0.1 to 20 mPa ⁇ s and an average thread length of the concentrated solution of 5 cm or less. It is possible to suppress the occurrence of coating failures such as uneven film thickness and streaks.
- the average string length of the concentrated liquid is more preferably 3 cm or less, and particularly preferably 0. When it is 3 cm or less, it becomes possible to further suppress the occurrence of coating failures such as film thickness unevenness and streaks.
- the method for reducing the viscosity and the average thread length is not particularly limited.
- Shear treatment / dispersion treatment By applying a shearing treatment to the coating solution for the bottom layer, cutting of bonds (van der Waals bonds, etc.) between polymer molecules and intra-molecular end groups, elimination of entanglement between molecules, etc. occur. The viscosity of the liquid and the average string length of the concentrated liquid can be reduced.
- Fig. 1 shows a milder as an example of a device that performs shearing using shear stress.
- the milder in FIG. 1 has a stator tooth 1 that is a fixed tooth and a rotor tooth 2 that is a rotating tooth.
- a velocity gradient (shear velocity) is generated in the radial direction of the rotor teeth 2. Due to the velocity gradient, an internal frictional force (shearing force) is generated between the stator teeth 1 and the rotor teeth 2.
- the polymer in the coating solution 4 passes through the shear gap 3 while receiving a shearing force, the molecular structure of the polymer is broken and the molecules are oriented in the flow direction, resulting in a decrease in viscosity and average thread length. Yes.
- the introduction of the coating liquid 5 into the shear gap 3 is performed in the radial direction from the slit gap of the rotor teeth 2, the coating liquid 4 flowing into the shear gap 3 and the introduced coating liquid 5 are continuously provided. The collision is repeated. That is, according to the milder shown in FIG. 1, shearing and mixing are continuously performed on the coating solution.
- the shortest distance between the stator teeth 1 and the rotor teeth 2 in the shear gap 3 is preferably 0.05 to 0.5 mm, and more preferably 0.1 to 0.3 mm.
- the rotation speed of the rotor teeth 2 is preferably 1 to 500 m / s, and more preferably 3 to 300 m / s.
- the above-mentioned shearing conditions are appropriately determined by those skilled in the art so that the viscosity and the average string length are predetermined values. Can be set.
- Ebara Milder manufactured by Ebara Manufacturing Co., Ltd.
- Milder manufactured by Taihei Kiko Co., Ltd.
- the shearing process may be performed by stirring, mixing, or the like.
- the apparatus for performing the shearing process by stirring / mixing are not particularly limited, and examples thereof include a high-speed stirring type dispersing apparatus, an emulsifying apparatus, and a pressure homogenizer.
- Specific examples of the apparatus include TK Robomix (manufactured by PRIMIX Co., Ltd.), CLEARMIX CLM-0.8S (manufactured by M Technique Co., Ltd.), and homogenizer (manufactured by Microtech Nichion Co., Ltd.).
- Dispersion treatment can be expected to have the same effect as shear treatment.
- the dispersion processing can be performed using an apparatus generally marketed as a dispersion processing apparatus.
- the output of the ultrasonic treatment is preferably 30 to 1200 W, and more preferably 150 to 1200 W.
- the frequency of the ultrasonic treatment is preferably 10 to 50 kHz, more preferably 20 to 40 kHz.
- the ultrasonic treatment conditions can be appropriately set by those skilled in the art so that the viscosity and the average yarn length become predetermined values.
- the ultrasonic processing apparatus that can be used in this embodiment is not particularly limited, and a known apparatus can be used. For example, an ultrasonic disperser (manufactured by SMT Co., Ltd.), an ultrasonic homogenizer (manufactured by Sonic Technology Co., Ltd.) and the like can be mentioned.
- the high-pressure spraying process is a process of spraying the lowermost layer coating liquid at a high pressure to collide with the wall.
- the injection speed of the high-pressure injection treatment is preferably 1000 to 100,000 m / s, more preferably 5000 to 20000 m / s.
- the pressure of the high pressure injection treatment is preferably 100 to 2000 atm, and more preferably 500 to 1500 atm.
- Conditions for the above-described high-pressure injection treatment can be appropriately set by those skilled in the art so that the viscosity and the average string length become predetermined values.
- the high-pressure injection processing apparatus that can be used in this embodiment is not particularly limited, and a known apparatus can be used. For example, a pressure type homogenizer (manufactured by SMT Co., Ltd.), a pressure type homogenizer (manufactured by Bertoli Co., Ltd.) and the like can be mentioned.
- the dilution ratio and concentration ratio vary depending on the type and molecular weight of the polymer used, but are diluted so that the amount of polymer in the lowermost layer coating solution is in the above-described range, that is, 0.01 to 20% by mass. -It is preferable to concentrate, and it is more preferable to dilute and concentrate to 0.1 to 10% by mass.
- the coating solution may contain a crosslinking agent.
- a crosslinking agent By reducing the content of the cross-linking agent in the coating solution for the lowermost layer, the binding between the intermolecular molecules and the end groups in the molecule and the binding in the cross-linking agent are suppressed, and the viscosity and the concentrated solution of the lowermost layer coating solution The average thread length of can be reduced.
- the viscosity of the lowermost layer coating liquid is less than 0.1 mPa ⁇ s, the viscosity of the lowermost layer coating liquid can be increased by increasing the content of the crosslinking agent in the lowermost layer coating liquid.
- the amount of the crosslinking agent in the lowermost layer coating solution varies depending on the type of polymer used, the functional group contained, the type of crosslinking agent, etc., but the range of the amount of the crosslinking agent in the lowermost layer coating solution described above, That is, it is preferably set to 0.01 to 10% by mass, and more preferably set to 0.001 to 20% by mass.
- the coating step is a step of forming a coating film by simultaneously applying the coating solution obtained in the preparation step on a substrate at a predetermined temperature and a predetermined speed.
- the substrate applied to the optical film of the present invention is not particularly limited as long as it is transparent, and a known resin film can be used.
- a known resin film can be used.
- PE polyethylene
- PP polypropylene
- PS polystyrene
- PC polyethylene terephthalate
- PET polybutylene terephthalate
- PBT polyethylene naphthalate
- PEN phthalate
- polysulfone polyethersulfone
- polyetheretherketone polyimide
- aromatic polyamide and polyetherimide.
- polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polycarbonate (PC), and the like are preferably used from the viewpoints of cost and availability.
- the substrate using the resin film may be an unstretched film or a stretched film, but in the case of a resin film having crystallinity such as PET or PEN, the strength is improved. From the viewpoint of suppressing thermal expansion, a film that is heat-set after stretching is preferred.
- the base material using the resin film can be manufactured by a conventionally known general method.
- an unstretched film that is substantially amorphous and not oriented can be produced by melting a resin as a material with an extruder, extruding it with an annular die or a T-die, and quenching.
- the unstretched film is uniaxially stretched, tenter-type sequential biaxial stretching, tenter-type simultaneous biaxial stretching, tubular-type simultaneous biaxial stretching, and other known methods such as resin film flow (vertical axis) direction, and / or
- a stretched film can be produced by stretching in the direction perpendicular to the flow direction of the resin film (horizontal axis).
- the draw ratio in this case can be appropriately selected according to the resin as the raw material of the substrate, but is preferably 2 to 10 times in the vertical axis direction and the horizontal axis direction.
- the thickness of the substrate according to the present invention is preferably 5 to 300 ⁇ m, more preferably 15 to 150 ⁇ m.
- the base material may be a laminate of two or more, and in this case, the type of the base material may be the same or different.
- the base material may be subjected to relaxation treatment and off-line heat treatment from the viewpoint of dimensional stability.
- the relaxation treatment is performed in a process from the heat setting in the stretching process of the resin film to the winding in the transversely stretched tenter or after exiting the tenter.
- the relaxation treatment is preferably carried out at a treatment temperature of 80 to 200 ° C., more preferably 100 to 180 ° C.
- the relaxation rate is preferably processed to 0.1 to 10%, more preferably 2 to 6%.
- the relaxed base material is further subjected to off-line heat treatment to improve heat resistance and further improve dimensional stability.
- the base material is preferably provided with an undercoat layer on one side or both sides during the film forming process.
- the undercoat layer can be formed in-line or after film formation.
- Examples of the method for forming the undercoat layer include a method of applying an undercoat layer coating solution and drying the obtained coating film.
- the undercoat layer coating solution usually contains a resin.
- the resin include polyester resins, acrylic-modified polyester resins, polyurethane resins, acrylic resins, vinyl resins, vinylidene chloride resins, polyethyleneimine vinylidene resins, polystyrene butadiene resins, polyethyleneimine resins, polyvinyl alcohol, and gelatin. .
- a known additive may be further added to the undercoat layer coating solution.
- the coating amount of the undercoat layer coating solution is preferably applied so as to be about 0.01 to 2 g / m 2 in a dry state.
- the coating method of the undercoat layer coating solution is not particularly limited, and known methods such as a roll coating method, a gravure coating method, a knife coating method, a dip coating method, and a spray coating method can be used.
- the obtained coating film may be stretched, and usually an undercoat layer can be formed by drying at 80 to 120 ° C. while performing lateral stretching in a tenter after coating the coating solution.
- the undercoat layer may have a single layer structure or a laminated structure.
- the substrate according to the present invention further includes a conductive layer, an antistatic layer, a gas barrier layer, an easy adhesion layer (adhesion layer), an antifouling layer, a deodorant layer, a droplet layer, an easy slip layer, a hard coat layer, and wear resistance.
- a conductive layer such as an adhesive layer, an adhesive layer, and an interlayer film layer.
- the total film thickness of the substrate and the intermediate layer is preferably 5 to 500 ⁇ m, more preferably 25 to 250 ⁇ m. preferable.
- the intermediate layer is also referred to as a “substrate”. Therefore, when a laminate composed of a plurality of refractive index layers is formed on the intermediate layer of the substrate, the “lowermost layer” means a refractive index layer in contact with the intermediate layer.
- the coating solution prepared in the preparation step is applied to the substrate at a predetermined temperature and a predetermined speed to form a coating film.
- the coating method of the coating solution is not particularly limited as long as it is a simultaneous multilayer coating method.
- roll coating method, rod bar coating method, air knife coating method, spray coating method, curtain coating method, or slide bead coating method using a hopper described in US Pat. No. 2,761,419 and US Pat. No. 2,761791 A method of applying the multilayer coating simultaneously by applying an extrusion coating method or the like is preferably used.
- the viscosity of the coating solution other than the lowermost layer coating solution is preferably 1 to 2000 mPa ⁇ s, and preferably 1 to 1000 mPa ⁇ s. It is more preferable.
- the coating temperature is the same as that measured when the above-mentioned viscosity and average thread length are measured, and is preferably 20 to 60 ° C. When the coating temperature is 20 ° C. or higher, a facility for cooling the coating solution is not necessary, and the cost can be reduced. On the other hand, it is preferable that the coating temperature is 60 ° C. or lower because a facility for heating the coating liquid becomes unnecessary, costs can be reduced, and work safety can be improved.
- the coating speed is the same as that when measuring the above average thread length, and is preferably 1 m / min or more, more preferably 1 to 500 m / min, and 30 to 200 m / min. It is particularly preferred. A coating speed of 1 m / min or more is preferable because high productivity can be obtained. When the coating speed is 30 to 200 m / min, it is possible to further suppress the occurrence of coating failures such as film thickness unevenness and streaks.
- Coating for the lowermost layer having a viscosity measured in consideration of the coating temperature of 0.1 to 20 mPa ⁇ s and an average string length of the concentrated liquid measured in consideration of the coating temperature and coating speed of 5 cm or less
- the refractive index layer formed by the lowermost layer that is, the lowermost layer coating solution may be a high refractive index layer or a low refractive index layer.
- the refractive index layer can be formed by drying the coating film obtained in the coating step.
- the drying method is not particularly limited, and may be performed by a known method. Examples of the drying method include natural drying, heat drying, a method of applying hot air, a method of applying cold air, and the like. From the viewpoint of rapid drying, it is preferable to perform drying by heat drying. In this case, the heating temperature is preferably 15 to 120 ° C., more preferably 20 to 90 ° C., although it varies depending on the composition of the formed coating film.
- the manufacturing method according to the present invention may further include a step of cooling the coating film obtained in the coating step once before drying. By performing the cooling step, the surface and interface of the refractive index layer can be made more uniform.
- the coating film immediately after coating has a low viscosity
- the surface of the obtained refractive index layer may vary in thickness due to the hot air.
- interlayer mixing that is, movement of coating film components between coating films is likely to occur, and the resulting boundary between refractive index layers may become ambiguous.
- the viscosity and spinnability of the coating film are rapidly increased and the coating film can be stabilized.
- the performance of the infrared shielding film may vary depending on the movement of the coating component between the coating films, whether or not to perform the cooling step can be appropriately determined according to the desired performance of the infrared shielding film. .
- the cooling step it is preferable to use a polymer whose viscosity and spinnability are likely to be increased by cooling the coating film as a component of the coating solution.
- the viscosity and the spinnability can be caused by bonding between end groups of the polymer in the coating liquid and within the molecule, bonding in the cross-linking agent, entanglement between molecules, and the like. Therefore, in order to more effectively exhibit the effect of the cooling step, it is preferable to use a polymer having a large number of functional groups or a polymer having a large molecular weight as a component of the coating solution and including a crosslinking agent.
- the cooling temperature in the cooling step varies depending on the coating solution used, but is preferably ⁇ 20 to 20 ° C., more preferably ⁇ 5 to 10 ° C.
- the infrared shielding film obtained above can be applied to a wide range of fields. For example, pasting to facilities exposed to sunlight for a long time such as outdoor windows of buildings and automobile windows, as film for window pasting such as infrared shielding film to give infrared shielding effect, film for agricultural greenhouse, etc. It is mainly used for the purpose of improving weather resistance.
- the infrared shielding film can be suitably applied to a member in which the infrared shielding film according to the present invention is bonded to a substrate such as glass or a glass substitute resin directly or via an adhesive. That is, according to still another aspect of the present invention, there is also provided an infrared shielding body in which the infrared shielding film is provided on at least one surface of a base.
- the substrate include, for example, glass, polycarbonate resin, polysulfone resin, acrylic resin, polyolefin resin, polyether resin, polyester resin, polyamide resin, polysulfide resin, unsaturated polyester resin, epoxy resin, melamine resin, Examples thereof include phenol resin, diallyl phthalate resin, polyimide resin, urethane resin, polyvinyl acetate resin, polyvinyl alcohol resin, styrene resin, vinyl chloride resin, metal plate, ceramic and the like.
- the type of the resin may be any of a thermoplastic resin, a thermosetting resin, and an ionizing radiation curable resin, and two or more of these may be used in combination.
- the substrate that can be used in the present invention can be produced by a known method such as extrusion molding, calendar molding, injection molding, hollow molding, compression molding and the like.
- the thickness of the substrate is not particularly limited, but is usually 0.1 mm to 5 cm.
- the adhesive layer or adhesive layer that bonds the infrared shielding film and the substrate is preferably provided with the infrared shielding film on the sunlight (heat ray) incident surface side. Moreover, it is preferable to sandwich the infrared shielding film according to the present invention between a window glass and a substrate because it can be sealed from surrounding gas such as moisture and has excellent durability. Even if the infrared shielding film according to the present invention is installed outdoors or outside the car (for external application), it is preferable because of environmental durability.
- an adhesive mainly composed of a photocurable or thermosetting resin can be used.
- the adhesive preferably has durability against ultraviolet rays, and is preferably an acrylic adhesive or a silicone adhesive.
- an acrylic adhesive is preferable from the viewpoint of adhesive properties and cost.
- a solvent system is preferable in the acrylic pressure-sensitive adhesive because the peel strength can be easily controlled.
- known monomers can be used as the monomer.
- polyvinyl butyral resin or ethylene-vinyl acetate copolymer resin used as an intermediate layer of laminated glass may be used.
- plastic polyvinyl butyral manufactured by Sekisui Chemical Co., Ltd., Mitsubishi Monsanto, etc.
- ethylene-vinyl acetate copolymer manufactured by DuPont, Takeda Pharmaceutical Co., Ltd., duramin
- modified ethylene-vinyl acetate copolymer manufactured by Tosoh Corporation.
- blend an ultraviolet absorber, an antioxidant, an antistatic agent, a heat stabilizer, a lubricant, a filler, coloring, an adhesion adjusting agent etc. suitably in a contact bonding layer.
- the heat insulation performance and solar heat shielding performance of the infrared shielding film or the infrared shielding body are generally JIS R 3209 (multi-layer glass), JIS R 3106 (permeability, reflectance, emissivity, and solar heat acquisition rate of plate glass). Test method), JIS R 3107 (calculation method of thermal resistance of plate glass and thermal transmissivity in architecture).
- Measure solar transmittance, solar reflectance, emissivity, and visible light transmittance (1) Using a spectrophotometer with a wavelength (300 to 2500 nm), measure the spectral transmittance and spectral reflectance of various single glass plates. The emissivity is measured using a spectrophotometer having a wavelength of 5.5 to 50 ⁇ m. In addition, a predetermined value is used for the emissivity of float plate glass, polished plate glass, mold plate glass, and heat ray absorbing plate glass. (2) The solar transmittance, solar reflectance, solar absorption rate, and modified emissivity are calculated according to JIS R 3106 by calculating the solar transmittance, solar reflectance, solar absorption rate, and vertical emissivity.
- the corrected emissivity is obtained by multiplying the vertical emissivity by the coefficient shown in JIS R 3107.
- the heat insulation and solar heat shielding properties are calculated by (1) calculating the thermal resistance of the multilayer glass according to JIS R 3209 using the measured thickness value and the corrected emissivity. However, when the hollow layer exceeds 2 mm, the gas thermal conductance of the hollow layer is determined according to JIS R 3107. (2) The heat insulation is obtained by adding a heat transfer resistance to the heat resistance of the double-glazed glass and calculating the heat flow resistance. (3) The solar heat shielding property is calculated by obtaining the solar heat acquisition rate according to JIS R 3106 and subtracting it from 1.
- the infrared shielding film obtained above is thinned, it may be applied to the surface of the display panel.
- an infrared shielding film can be bonded to a highly transparent PET film and introduced into a display screen.
- infrared rays radiated from the plasma display panel can be shielded, contributing to protection of the human body, prevention of malfunction between electronic devices, prevention of malfunction of the remote control, and the like.
- an infrared shielding film was prepared by applying a coating solution on a substrate by a simultaneous multilayer coating method.
- Preparation of coating solution for the bottom layer (Preparation of coating solution precursor 1) To 1200 parts by mass of colloidal silica (Snowtex OXS, manufactured by Nissan Chemical Industries, Ltd., solid content 10% by mass), 5% by mass polyvinyl alcohol (PVA-103, polymerization degree 300, saponification degree 98.5 mol%, Kuraray Co., Ltd.) Manufactured) 200 parts by weight of an aqueous solution and 1000 parts by weight of a 3% by weight aqueous boric acid solution were added respectively, and then heated to 45 ° C. while stirring, 5% by weight polyvinyl alcohol (PVA-117, polymerization degree 1700, saponification degree 98).
- aqueous solution 100 parts by mass, added with 10500 parts by mass of pure water, and a coating solution precursor 1 was prepared at 15000 parts by mass.
- a surfactant Liapisol A30, manufactured by NOF Corporation
- coating solution precursor 2 1800 parts by weight of colloidal silica, 300 parts by weight of 5% by weight polyvinyl alcohol (PVA-103) aqueous solution, 1250 parts by weight of 3% by weight boric acid aqueous solution, and 3000% by weight of 5% by weight polyvinyl alcohol (PVA-117) aqueous solution.
- a coating liquid precursor 2 was prepared in the same manner as the coating liquid precursor 1 except that the pure water was changed to 8550 parts by mass.
- coating solution precursor 3 2400 parts by weight of colloidal silica, 400 parts by weight of 5% by weight polyvinyl alcohol (PVA-103) aqueous solution, 1500 parts by weight of 3% by weight boric acid aqueous solution, and 4000% by weight of 5% by weight polyvinyl alcohol (PVA-117) aqueous solution.
- a coating solution precursor 3 was prepared in the same manner as the coating solution precursor 1 except that the pure water was changed to 6600 parts by mass.
- Shear treatment was performed using CLEARMIX CLM-0.8S (manufactured by M Technique Co., Ltd.), which is a high-speed stirring type dispersion apparatus.
- the coating solution precursor was supplied to a dispersion processing container (350 ml vessel) at a flow rate of 1 L / min using a rotary pump. Shearing was performed at 18000 rpm, R2 was used for the rotor, and S2.0-24 was used for the screen.
- Kneading process B A shearing process was performed in the same manner as the kneading process A, except that the rotation speed was changed to 12000 rpm.
- Kneading process C A shearing process was performed in the same manner as the kneading process A, except that the rotation speed was changed to 6000 rpm.
- Ultrasonic treatment was performed using UH-600S (manufactured by SMT Co., Ltd.) which is an ultrasonic treatment apparatus.
- the coating liquid precursor was supplied to the 350 ml vessel of the ultrasonic processing apparatus at a flow rate of 0.1 L / min using a rotary pump.
- the ultrasonic treatment was performed at a processing intensity of 600W.
- the average yarn length was measured as follows. First, the lowermost layer coating solution was sampled in a beaker and concentrated to 50% by mass by evaporation to obtain a concentrated solution, which was then kept at 45 ° C. Next, a glass rod having an outer diameter of 6 mm was immersed in the concentrated solution for 3 cm in the vertical direction, and the glass rod was pulled up in the vertical direction at a speed of 30 m / min. At this time, the liquid level of the concentrated liquid when the connection between the glass rod and the concentrated liquid (filament string) was broken—the length of the tip of the glass rod was measured visually and photographed with a video camera. This was repeated 5 times in succession, and the average value was calculated as the average thread length. The obtained results are shown in Table 2 below. The temperature of 45 ° C. and the speed of 30 m / min are in accordance with the conditions during the coating process described later.
- the viscosity of the lowermost coating solutions 1 to 20 obtained above was measured as follows. First, the lowermost layer coating solution was sampled in a beaker and kept at 45 ° C. Next, the viscosity of the lowermost layer coating solution was measured using a rotary viscometer calibrated with a reference solution in advance. This was repeated 5 times in succession, and the average value was calculated as the viscosity. The obtained results are shown in Table 2 below.
- An aqueous solution 200 of 5% by weight polyvinyl alcohol (PVA-103, polymerization degree 300, saponification degree 98.5 mol%, manufactured by Kuraray Co., Ltd.) is added to 3000 parts by mass of the anion-treated titanium dioxide sol (solid content 20.0% by weight).
- PVA-103 polyvinyl alcohol
- 1 part by weight, 1000 parts by weight of a 3% by weight boric acid aqueous solution, and 1000 parts by weight of a 2% by weight aqueous citric acid solution were added.
- a coating liquid precursor was prepared in the same manner as the coating liquid precursor 1 except that the pure water was changed to 3550 parts by mass.
- a solution obtained by subjecting the precursor to the kneading treatment B was used as a coating solution for a low refractive index layer.
- Example 1 a polyethylene terephthalate film (A4300 manufactured by Toyobo Co., Ltd .: double-sided easy-adhesion layer) having a thickness of 50 ⁇ m was prepared. Then, the lowermost layer coating solution 1, 5, 13, 2, 6, 14, 3, 7, or 15 is kept at 45 ° C. for the low refractive index layer coating solution and the high refractive index layer coating solution. However, nine layers were simultaneously applied at a speed of 30 m / min using a slide hopper coating apparatus so that nine layers of low refractive index layers and high refractive index layers were alternately laminated on the substrate.
- A4300 manufactured by Toyobo Co., Ltd .: double-sided easy-adhesion layer having a thickness of 50 ⁇ m was prepared. Then, the lowermost layer coating solution 1, 5, 13, 2, 6, 14, 3, 7, or 15 is kept at 45 ° C. for the low refractive index layer coating solution and the high refractive index layer coating solution. However, nine layers were simultaneously applied at a speed
- the obtained coating film was dried to produce an infrared shielding film.
- the refractive index layer in contact with the substrate that is, the lowermost layer is a low refractive index layer formed by the lowermost layer coating liquid, and the high refractive index formed by the high refractive index layer coating liquid thereon.
- Eight layers of the refractive index layer and the low refractive index layer formed by the coating solution for the low refractive index layer were alternately laminated.
- the average film thickness after drying was 150 nm for each layer of low refractive index layers (including the lowermost layer), and 150 nm for each high refractive index layer.
- the infrared shielding films of Examples 1 to 9 were highly visible when attached to the window glass, that is, the appearance was high.
- the infrared shielding films of Examples 1 to 6, that is, the infrared shielding films prepared using the coating solution for the lowermost layer in which the average string length of the concentrated liquid is 3 cm or less have no problem in visibility in all samples. A good result was obtained.
- by controlling the viscosity and spinnability of the coating solution for the lowermost layer it is possible to stably apply and obtain an infrared shielding film in which the occurrence of coating failures such as film thickness unevenness and streaks is suppressed. Is understood.
- the present invention is used for production of optical films such as an infrared shielding film, an antireflection film, an orientation film, a polarizing film, a polarizing plate protective film, a retardation film, a viewing angle widening film, a brightness enhancement film, and an electromagnetic wave shielding film.
- optical films such as an infrared shielding film, an antireflection film, an orientation film, a polarizing film, a polarizing plate protective film, a retardation film, a viewing angle widening film, a brightness enhancement film, and an electromagnetic wave shielding film.
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Abstract
Description
同時重層塗布方式では、例えば、複数のダイス(バー)で構成されるスライド型コータを使用して塗布液を塗布する(例えば、特許文献3参照。)。具体的には、スライド型コータにおいては、例えば、ダイス同士の間にスリットが形成されており、各ダイスの先端面がコータのスライド面になっている。そして、各スリットから押し出された塗布液をスライド面上で順次積層させて塗布液の重層体を形成し、その重層体を基材上に塗布する。その際、スライド面等に異物が付着する、塗布液の重層体が基材に接する際に塗布液が均一な厚さに引き伸ばされない等の様々な要因で、得られる光学機能層の積層膜に膜厚ムラやスジ等の塗布故障が発生し、光学フィルムの外観が悪くなってしまう場合がある。
すなわち、本発明に係る上記課題は、以下の手段により解決される。
前記基材に接する前記光学機能層を形成する最下層用塗布液と、他の前記光学機能層を形成する塗布液とを、所定の温度及び所定の速度で前記基材上に同時重層塗布する塗布工程を含み、
前記最下層用塗布液は、前記所定の温度における粘度が0.1~20mPa・sの範囲内であり、
前記最下層用塗布液を50質量%に濃縮した濃縮液は、外径6mmのガラス棒を当該濃縮液に鉛直方向に3cm浸し、前記所定の温度及び前記所定の速度で前記ガラス棒を鉛直方向に引き上げて、当該濃縮液から出る曳糸が切れたときの曳糸の長さを5回測定した場合における平均曳糸長さが5cm以下であることを特徴とする光学フィルムの製造方法。
塗布液中の高分子の分子間及び分子内の末端基による結合、架橋剤における結合、分子どうしの絡み合い等が生じると、塗布液中の高分子の中に見かけの分子サイズが大きくなっているものが存在し、塗布液は、見かけの分子サイズが大きくなっている高分子と、そうでない高分子とが混在した不均質な状態となる。均質度の低い最下層用塗布液上に塗布液を積層させて塗布液の重層体を形成し、その塗布液の重層体を基材上に塗布すると、基材に接する最下層用塗布液が均一な厚さに引き伸ばされることなく塗膜が形成され、その結果、得られる光学機能層の積層膜に膜厚ムラやスジ等の塗布故障が発生する。よって、最下層用塗布液を混練等して最下層用塗布液の均質度を高めると、塗布液の重層体を基材上に塗布する際に、基材に接する最下層用塗布液が均一な厚さに引き伸ばされた状態で塗膜が形成され、その結果、得られる光学機能層の積層膜に膜厚ムラやスジ等の塗布故障が発生しにくくなると推察する。本発明では、最下層用塗布液の粘度と、最下層用塗布液を濃縮して得た濃縮液の平均曳糸長さとを用いて、最下層用塗布液の均質度を評価している。
かかる構成によって、光学機能層の積層膜に膜厚ムラやスジ等の塗布故障が発生しにくい光学フィルムの製造方法を提供するものである。この特徴は、請求項1から請求項7までの請求項に係る発明に共通する技術的特徴である。
また、本発明においては、前記積層膜が、赤外線反射性を有することが好ましい。これにより、光学フィルムとして、赤外線遮蔽フィルムを製造することができる。
また、本発明においては、互いに隣接する前記光学機能層に含まれるポリビニルアルコールのケン化度の差が、3モル%以上であることが好ましい。これにより、隣接する光学機能層同士の層間混合が抑制される。
また、本発明においては、前記濃縮液は、前記平均曳糸長さが3cm以下であることが好ましい。これにより、塗布故障の発生を効果的に抑制することができる。
本形態に係る製造方法で製造される光学フィルムは、複数の光学機能層からなる積層膜が基材上に形成されたフィルムである。当該光学フィルムの製造方法は、同時重層塗布方式の塗布工程、具体的には基材に接する光学機能層を形成する最下層用塗布液と、他の光学機能層を形成する塗布液とを、所定の温度及び所定の速度で基材上に同時重層塗布する塗布工程を含む。
屈折率層の1層あたりの厚さは、好ましくは1~1000nmであり、より好ましくは20~800nmであり、さらに好ましくは50~350nmである。
調製工程は、高分子を含む塗布液を調製する工程である。
赤外線遮蔽フィルムの製造においては、通常、塗布液として、高屈折率層用塗布液及び低屈折率層用塗布液の少なくとも2種の塗布液を調製する。
塗布液は、高分子を含む。さらに、必要に応じて溶媒、架橋剤、金属酸化物粒子、エマルジョン樹脂、その他の添加剤を含んでいてもよい。
用いられうる高分子としては、特に制限されないが、水溶性高分子が挙げられる。水溶性高分子としては、特に制限されないが、反応性官能基を有するポリマー、変性ポリビニルアルコール、ゼラチン、及び増粘多糖類等が挙げられる。なお、本明細書において、「水溶性高分子」とは、水溶性高分子が最も溶解する温度で0.5質量%の濃度となるように水に溶解させた場合において、G2ガラスフィルター(最大細孔40~50μm)でろ過した際にろ別される不溶物の質量が、加えた水溶性高分子の50質量%以内であるものを意味する。
本発明で用いられる反応性官能基を有するポリマーとしては、例えば、未変性ポリビニルアルコール類、ポリビニルピロリドン類、ポリアクリル酸、アクリル酸-アクリロニトリル共重合体、アクリル酸カリウム-アクリロニトリル共重合体、酢酸ビニル-アクリル酸エステル共重合体、若しくはアクリル酸-アクリル酸エステル共重合体などのアクリル樹脂、スチレン-アクリル酸共重合体、スチレン-メタクリル酸共重合体、スチレン-メタクリル酸-アクリル酸エステル共重合体、スチレン-α-メチルスチレン-アクリル酸共重合体、若しくはスチレン-α-メチルスチレン-アクリル酸-アクリル酸エステル共重合体などのスチレンアクリル酸樹脂、スチレン-スチレンスルホン酸ナトリウム共重合体、スチレン-2-ヒドロキシエチルアクリレート共重合体、スチレン-2-ヒドロキシエチルアクリレート-スチレンスルホン酸カリウム共重合体、スチレン-マレイン酸共重合体、スチレン-無水マレイン酸共重合体、ビニルナフタレン-アクリル酸共重合体、ビニルナフタレン-マレイン酸共重合体、酢酸ビニル-マレイン酸エステル共重合体、酢酸ビニル-クロトン酸共重合体、酢酸ビニル-アクリル酸共重合体などの酢酸ビニル系共重合体及びそれらの塩が挙げられる。これらの中でも、未変性ポリビニルアルコール類、ポリビニルピロリドン類、及びこれらの共重合体を用いることが好ましい。
本発明において用いられる変性ポリビニルアルコールは、未変性ポリビニルアルコールに任意の変性処理の1又は2以上を施したものである。例えば、アミン変性ポリビニルアルコール、エチレン変性ポリビニルアルコール、カルボン酸変性ポリビニルアルコール、ジアセトン変性ポリビニルアルコール、チオール変性ポリビニルアルコール、アセタール変性ポリビニルアルコール等が挙げられる。これらの変性ポリビニルアルコールは、市販品を使用してもよく、あるいは当該分野で公知の方法で製造したものを使用してもよい。
特に、変性ポリビニルアルコールとしての上記グラフト共重合体を製造する方法としては、ラジカル重合、例えば溶液重合、懸濁重合、乳化重合及び塊状重合などのそれ自体公知の方法を挙げることができ、各々の通常の重合条件下で実施することができる。この重合反応は、通常、重合開始剤の存在下、必要に応じて還元剤(例えば、エリソルビン酸ナトリウム、メタ重亜硫酸ナトリウム、アスコルビン酸)、連鎖移動剤(例えば2-メルカプトエタノール、α-メチルスチレンダイマー、2-エチルヘキシルチオグリコレート、ラウリルメルカプタン)あるいは分散剤(例えばソルビタンエステル、ラウリルアルコールなどの界面活性剤)等の存在下、水、有機溶媒(例えばメタノール、エタノール、セロソルブ、カルビトール)あるいはそれらの混合物中で実施される。また、未反応の単量体の除去方法、乾燥、粉砕方法等も公知の方法でよく、特に制限はない。
本発明で用いられるゼラチンとしては、従来、ハロゲン化銀写真感光材料分野で広く用いられてきた各種ゼラチンを挙げることができる。例えば、酸処理ゼラチン、アルカリ処理ゼラチンの他に、ゼラチンの製造過程で酵素処理をする酵素処理ゼラチン及びゼラチン誘導体、すなわち分子中に官能基としてのアミノ基、イミノ基、ヒドロキシ基、又はカルボキシ基を有し、それと反応して得る基を持った試薬で処理し改質したものでもよい。ゼラチンの一般的製造法に関しては良く知られており、例えば、T.H.James:The Theory of Photographic Process 4th.ed.1977(Macmillan)55頁、科学写真便覧(上)72~75頁(丸善株式会社)、写真工学の基礎-銀塩写真編 119~124頁(コロナ社)等の記載を参考にすることができる。また、リサーチ・ディスクロージャー誌第176巻、No.17643(1978年12月)のIXページに記載されているゼラチンを挙げることができる。
本発明で用いられる増粘多糖類としては、特に制限はなく、例えば、一般に知られている天然単純多糖類、天然複合多糖類、合成単純多糖類及び合成複合多糖類などを挙げることができる。これら増粘多糖類の詳細については、「生化学辞典(第2版)」(東京化学同人)、「食品工業」第31巻(1988)21頁等を参照することができる。
なお、ケン化度とは、ケン化によりビニルアルコール単位に変換されうる単位の中で、実際にビニルアルコール単位にケン化された単位の割合(百分率)のことである。
本発明で用いられうる溶媒は、特に制限されないが、水、有機溶媒、又はその混合溶媒等が挙げられる。
架橋剤は、高分子を硬化させる機能を有する。硬化によって、屈折率層に耐水性が付与されうる。
用いられうる金属酸化物粒子としては、特に制限されないが、酸化チタン(TiO2)、酸化亜鉛(ZnO)、酸化ジルコニウム(ZrO2)、酸化ニオブ(Nb2O5)、酸化アルミニウム(Al2O3)、酸化ケイ素(SiO2)、フッ化カルシウム(CaF2)、フッ化マグネシウム(MgF2)、酸化インジウムスズ(ITO)、酸化アンチモンスズ(ATO)等が挙げられる。これらのうち、高屈折率層用塗布液には酸化チタン(TiO2)を、低屈折率層用塗布液には酸化ケイ素(SiO2)を、それぞれ用いることが好ましい。
金属酸化物粒子の平均粒径は、2~100nmであることが好ましく、3~50nmであることがより好ましく、4~30nmであることがさらに好ましい。当該金属酸化物粒子の平均粒径は、粒子そのものあるいは屈折率層の断面や表面に現れた粒子を電子顕微鏡で観察し、1000個の任意の粒子の粒径を測定し、その単純平均値(個数平均)として求められる。ここで個々の粒子の粒径は、その投影面積に等しい円を仮定したときの直径で表したものである。
エマルジョン樹脂は、通常、塗布液に分散されたポリマーである。当該エマルジョン樹脂は、後述する塗布工程における塗布時に互いに融着しうる。エマルジョン樹脂は、油溶性のモノマーを、高分子分散剤等を用いてエマルジョン重合して得られる。
アクリル酸及び/又はそのエステル類、酢酸ビニル系エマルジョンとしては、市販されているものを用いてもよく、例えば、アクリットUW-309、UW-319SX、UW-520(大成ファインケミカル株式会社製)、及びモビニール(日本合成化学工業株式会社製)等が挙げられる。
本発明に係る屈折率層に適用可能なその他の添加剤を、以下に列挙する。例えば、特開昭57-74193号公報、特開昭57-87988号公報、及び特開昭62-261476号公報に記載の紫外線吸収剤、アニオン、カチオン、又はノニオンの各種界面活性剤、硫酸、リン酸、酢酸、クエン酸、水酸化ナトリウム、水酸化カリウム、炭酸カリウム等のpH調整剤、消泡剤、ジエチレングリコール等の潤滑剤、防腐剤、防カビ剤、帯電防止剤、マット剤、酸化防止剤、難燃剤、赤外線吸収剤、色素、顔料等の公知の各種添加剤などが挙げられる。
塗布液の調製方法は、特に制限されず、例えば、高分子、及び必要に応じて架橋剤、金属酸化物粒子等の添加剤を溶媒に添加し、撹拌混合する方法が挙げられる。この際、各成分の添加順も特に制限されず、撹拌しながら各成分を順次添加し混合してもよいし、撹拌しながら一度に添加し混合してもよい。
一方、最下層用塗布液の均質度が高くても、当該最下層用塗布液が一定の粘性を有さないと、塗布液の重層体を基材上に塗布した場合に、基材に接する最下層用塗布液の層に裂け目や孔が生じ、最下層用塗布液が均一な厚さに引き伸ばされることなく塗膜が形成される。その結果、得られる屈折率層の積層膜に膜厚ムラやスジ等の塗布故障が生じる。
得られる屈折率層の積層膜に膜厚ムラやスジ等の塗布故障が生じると、透過光が屈折し、赤外線遮蔽フィルムの外観(アピアランス)が悪くなってしまう。
最下層用塗布液にせん断処理を施すことによって、高分子の分子間及び分子内の末端基による結合(ファンデルワールス結合等)の切断、分子どうしの絡み合いの解消等が生じ、最下層用塗布液の粘度や濃縮液の平均曳糸長さを低下させうる。
また、ローター歯2の回転速度としては、1~500m/sであることが好ましく、3~300m/sであることがより好ましい。
上記せん断処理の条件(せん断間隙3におけるステーター歯1とローター歯2との最短距離、ローター歯2の回転速度等)は、粘度及び平均曳糸長さが所定の値となるように適宜当業者によって設定されうる。
上記のようなマイルダーとしては、例えば、エバラマイルダー(株式会社荏原製作所製)、マイルダー(大平洋機工株式会社製)等を用いることができる。
最下層用塗布液に超音波処理を施すことによって、高分子の分子間及び分子内の末端基による結合(ファンデルワールス結合等)の切断、分子どうしの絡み合いの解消等が生じ、最下層用塗布液の粘度や濃縮液の平均曳糸長さを低下させうる。
また、超音波処理の周波数としては、10~50kHzであることが好ましく、20~40kHzであることがより好ましい。
上記超音波処理の条件(出力、周波数、処理時間等)は、粘度及び平均曳糸長さが所定の値となるように適宜当業者によって設定されうる。
本形態に用いられうる超音波処理装置としては、特に制限されず公知のものを使用することができる。例えば、超音波分散機(株式会社エスエムテー製)、超音波ホモジナイザー(株式会社ソニックテクノロジー製)等が挙げられる。
最下層用塗布液に高圧噴射処理を施すことによって、高分子の分子間及び分子内の末端基による結合(ファンデルワールス結合等)の切断、分子どうしの絡み合いの解消等が生じ、最下層用塗布液の粘度や濃縮液の平均曳糸長さを低下させうる。なお、高圧噴射処理とは、最下層用塗布液を高圧で噴射して壁に衝突させる処理である。
また、高圧噴射処理の圧力としては、100~2000atmであることが好ましく、500~1500atmであることがより好ましい。
上記高圧噴射処理の条件(噴射速度、圧力、壁までの距離等)は、粘度及び平均曳糸長さが所定の値となるように適宜当業者によって設定されうる。
本形態に用いられうる高圧噴射処理装置としては、特に制限されず公知のものを使用することができる。例えば、圧力式ホモジナイザー(株式会社エスエムテー製)、圧力式ホモジナイザー(ベルトーリ社製)等が挙げられる。
最下層用塗布液を希釈し、最下層用塗布液中の高分子含有量を低下させることによって、高分子の分子間及び分子内の末端基による結合(ファンデルワールス結合等)の抑制、分子どうしの絡み合いの防止等により、最下層用塗布液の粘度や濃縮液の平均曳糸長さを低下させうる。
一方、最下層用塗布液の粘度が0.1mPa・sを下回る場合には、最下層用塗布液を濃縮し、最下層用塗布液中の高分子含有量を上昇させることによって、最下層用塗布液の粘度を上昇させうる。
上述のように塗布液中には、架橋剤を含みうる。最下層用塗布液中の架橋剤の含有量を低減することにより、高分子の分子間及び分子内の末端基による結合や架橋剤における結合を抑制し、最下層用塗布液の粘度や濃縮液の平均曳糸長さが低下しうる。
一方、最下層用塗布液の粘度が0.1mPa・sを下回る場合には、最下層用塗布液中の架橋剤の含有量を増やすことにより、最下層用塗布液の粘度が上昇しうる。
塗布工程は、調製工程で得られた塗布液を所定の温度及び所定の速度で基材上に同時重層塗布して塗膜を形成する工程である。
本発明の光学フィルムに適用する基材としては、透明であれば特に制限されることはなく、公知の樹脂フィルムを用いることができる。具体的には、ポリエチレン(PE)、ポリプロピレン(PP)、ポリスチレン(PS)、ポリアリレート、ポリメタクリル酸メチル、ポリアミド、ポリカーボネート(PC)、ポリエチレンテレフタレート(PET)、ポリブチレンテレフタレート(PBT)、ポリエチレンナフタレート(PEN)、ポリスルホン、ポリエーテルスルホン、ポリエーテルエーテルケトン、ポリイミド、芳香族ポリアミド、ポリエーテルイミド等が挙げられる。これらのうち、コストや入手の容易性の観点から、ポリエチレンテレフタレート(PET)、ポリエチレンナフタレート(PEN)、ポリカーボネート(PC)等を用いることが好ましい。
なお、本発明では、基材が、上述の下引層や機能層等の中間層を有する場合には、中間層も含めて「基材」と称する。したがって、基材の中間層上に、複数の屈折率層からなる積層体が形成される場合には、「最下層」とは、中間層に接する屈折率層を意味する。
塗布工程では、調製工程で調製した塗布液を、上記基材に所定の温度、所定の速度で塗布して塗膜を形成する。
なお、最下層、すなわち最下層用塗布液により形成される屈折率層は、高屈折率層であってもよいし、低屈折率層であってもよい。
塗布工程で得られた塗膜を乾燥させることにより、屈折率層が形成されうる。
乾燥の方法としては、特に制限されず、公知の方法で行われうる。乾燥方法の例としては、自然乾燥、加熱乾燥、熱風を当てる方法、冷風を当てる方法等が挙げられる。迅速に乾燥を行う観点から、加熱乾燥により乾燥を行うことが好ましい。この際、加熱温度としては、形成された塗膜の組成等によっても異なるが、15~120℃であることが好ましく、20~90℃であることがより好ましい。
本発明に係る製造方法には、前記塗布工程で得られた塗膜を、乾燥前に一度冷却する工程をさらに含んでいてもよい。冷却工程を行うことにより、屈折率層の表面や界面がより均一となりうる。
冷却工程における冷却温度は、用いる塗布液によっても異なるが、-20~20℃であることが好ましく、-5~10℃であることがより好ましい。
上記で得られた赤外線遮蔽フィルムは、幅広い分野に応用することができる。例えば、建物の屋外の窓や自動車窓等の長期間太陽光に晒らされる設備に貼り合せ、赤外線遮蔽効果を付与する赤外線遮蔽フィルム等の窓貼用フィルム、農業用ビニールハウス用フィルム等として、主として耐候性を高める目的で用いられる。
特に、本発明に係る赤外線遮蔽フィルムが直接又は接着剤を介してガラス又はガラス代替の樹脂などの基体に貼合されている部材には、赤外線遮蔽フィルムは好適に適用されうる。
すなわち、本発明のさらに他の形態によれば、上記赤外線遮蔽フィルムを、基体の少なくとも一方の面に設けた、赤外線遮蔽体をも提供する。
接着剤は紫外線に対して耐久性を有するものが好ましく、アクリル系粘着剤又はシリコーン系粘着剤が好ましい。更に粘着特性やコストの観点から、アクリル系粘着剤が好ましい。特に剥離強さの制御が容易なことから、アクリル系粘着剤において、溶剤系が好ましい。アクリル溶剤系粘着剤として溶液重合ポリマーを使用する場合、そのモノマーとしては公知のものを使用できる。
また、合わせガラスの中間層として用いられるポリビニルブチラール系樹脂、あるいはエチレン-酢酸ビニル共重合体系樹脂を用いてもよい。具体的には可塑性ポリビニルブチラール(積水化学工業社製、三菱モンサント社製等)、エチレン-酢酸ビニル共重合体(デュポン社製、武田薬品工業社製、デュラミン)、変性エチレン-酢酸ビニル共重合体(東ソー社製、メルセンG)等である。なお、接着層には紫外線吸収剤、抗酸化剤、帯電防止剤、熱安定剤、滑剤、充填剤、着色、接着調整剤等を適宜添加配合してもよい。
まず、同時重層塗布方式で塗布液を基板上に塗布して赤外線遮蔽フィルムを作製した。
(塗布液前駆体1の調製)
コロイダルシリカ(スノーテックスOXS、日産化学工業株式会社製、固形分10質量%)1200質量部に、5質量%ポリビニルアルコール(PVA-103、重合度300、ケン化度98.5mol%、株式会社クラレ製)水溶液200質量部、3質量%ホウ酸水溶液1000質量部をそれぞれ添加した後、45℃に加熱し、撹拌しながら、5質量%ポリビニルアルコール(PVA-117、重合度1700、ケン化度98.5mol%、株式会社クラレ製)水溶液2000質量部、1質量%界面活性剤(ラピゾールA30、日油株式会社製)水溶液100質量部を添加し、純水10500質量部を加えて塗布液前駆体1を15000質量部調製した。
コロイダルシリカを1800質量部に、5質量%ポリビニルアルコール(PVA-103)水溶液を300質量部に、3質量%ホウ酸水溶液を1250質量部に、5質量%ポリビニルアルコール(PVA-117)水溶液を3000質量部に、純水を8550質量部に変更したことを除いては、塗布液前駆体1と同様に塗布液前駆体2を調製した。
コロイダルシリカを2400質量部に、5質量%ポリビニルアルコール(PVA-103)水溶液を400質量部に、3質量%ホウ酸水溶液を1500質量部に、5質量%ポリビニルアルコール(PVA-117)水溶液を4000質量部に、純水を6600質量部に変更したことを除いては、塗布液前駆体1と同様に塗布液前駆体3を調製した。
前記調製した塗布液前駆体1~3について、混練処理A~Dを適宜組み合わせて行い、最下層用塗布液1~20を調製した。当該組み合わせについて下記表1に示す。なお、混練処理A~Dの詳細は以下のとおりである。
高速撹拌型分散装置であるクレアミックスCLM-0.8S(エム・テクニック株式会社製)を用いてせん断処理を行った。塗布液前駆体は、ロータリーポンプを用いて1L/minの流量で分散用処理容器(350mlベッセル)に供給した。せん断処理は、回転数18000rpmで行い、ローターにはR2を、スクリーンにはS2.0-24をそれぞれ用いた。
回転数を12000rpmに変更したことを除いては、混練処理Aと同様にせん断処理を行った。
回転数を6000rpmに変更したことを除いては、混練処理Aと同様にせん断処理を行った。
超音波処理装置であるUH-600S(株式会社エスエムテー製)を用いて超音波処理を行った。塗布液前駆体は、ロータリーポンプを用いて0.1L/minの流量で超音波処理装置の350mlベッセルに供給した。超音波処理は、600Wの処理強度で行った。
前記調製した混練処理済みの最下層用塗布液1~20を、製膜実施まで保管した。その保管時間について下記表1に示す。
上記で得られた最下層用塗布液1~20について、下記のように平均曳糸長さを測定した。
始めに最下層用塗布液をビーカーにサンプリングし、エバポレーションにて50質量%に濃縮して濃縮液を得た後、45℃に保温した。次に、外径6mmのガラス棒を濃縮液に鉛直方向に3cm浸し、速度30m/minでガラス棒を鉛直方向に引き上げた。この際、ガラス棒と濃縮液との液のつながり(曳糸)が切れたときの濃縮液の液面-ガラス棒の先端の長さを、目視及びビデオカメラで撮影して測定した。これを連続して5回繰り返し、その平均値を平均曳糸長さとして算出した。得られた結果を下記表2に示す。
なお、温度45℃及び速度30m/minは、後述する塗布工程時における条件に合わせたものである。
上記で得られた最下層用塗布液1~20について、下記のように粘度を測定した。
始めに最下層用塗布液をビーカーにサンプリングし、45℃に保温した。次に、あらかじめ基準液で校正した回転式粘度計を用いて、最下層用塗布液の粘度を測定した。これを連続して5回繰り返し、その平均値を粘度として算出した。得られた結果を下記表2に示す。
15.0質量%酸化チタンゾル(SRD-W、体積平均粒径5nm、ルチル型二酸化チタン粒子、堺化学工業株式会社製)5000質量部に純水20000質量部を加えた後、90℃に加熱した。次いで、ケイ酸水溶液(ケイ酸ソーダ4号(日本化学工業株式会社製)をSiO2濃度が2.0質量%となるように純水で希釈したもの)13000質量部を徐々に添加し、オートクレーブ中、175℃で18時間加熱処理を行った。冷却後、限外ろ過膜にて濃縮することにより、固形分濃度が20質量%であるSiO2が表面に付着した二酸化チタンゾル(以下、アニオン処理された二酸化チタンゾル)を得た。
コロイダルシリカを1800質量部に、5質量%ポリビニルアルコール(PVA-103)水溶液を300質量部に、3質量%ホウ酸水溶液を1250質量部に、5質量%ポリビニルアルコール(PVA-117)水溶液を3000質量部に、純水を3550質量部に変更したことを除いては、塗布液前駆体1と同様に塗布液前駆体を調製した。その前駆体に対し、前記混練処理Bを行ったものを低屈折率層用塗布液とした。
(実施例1~9)
基材として、厚さ50μmのポリエチレンテレフタレートフィルム(東洋紡績株式会社製A4300:両面易接着層)を用意した。
そして、最下層用塗布液1、5、13、2、6、14、3、7、又は15と、低屈折率層用塗布液と、高屈折率層用塗布液と、を45℃に保温しながら、基材上に、低屈折率層と高屈折率層とがそれぞれ交互に9層積層されるように、スライドホッパー塗布装置を用いて速度30m/minで9層同時塗布を行い、得られた塗膜を乾燥させて赤外線遮蔽フィルムを作製した。具体的には、基材に接する屈折率層、すなわち最下層を、最下層用塗布液により形成される低屈折率層とし、その上に、高屈折率層用塗布液により形成される高屈折率層と、低屈折率層用塗布液により形成される低屈折率層と、を交互に8層積層した。乾燥後の平均膜厚が低屈折率層(最下層を含む)は各層150nmであり、高屈折率層は各層150nmであった。
最下層用塗布液を、最下層用塗布液9、17、10、18、12、19、11、4、8、16又は20に変更したことを除いては、実施例と同様に赤外線遮蔽フィルムを作製した。
次いで、実施例1~9並びに比較例1~11で作製した赤外線遮蔽フィルムについて、下記の性能評価を行った。
赤外線遮蔽フィルムを窓ガラスに貼り付けて、目視で窓の外の視認性を確認した。サンプル数Nは、各赤外線遮蔽フィルムについて、それぞれN=20とした。
そして、下記基準に従い、窓ガラス視認性を評価した:
◎:20枚全てのフィルムで視認性問題なし
○:18枚以上20枚未満のフィルムで視認性問題なし
△:10枚以上18枚未満のフィルムで視認性問題なし
×:10枚未満のフィルムで視認性問題なし
得られた結果を下記表3に示す。
2 ローター歯
3 せん断間隙
4、5 塗布液
Claims (7)
- 複数の光学機能層からなる積層膜を基材上に形成する光学フィルムの製造方法であって、
前記基材に接する前記光学機能層を形成する最下層用塗布液と、他の前記光学機能層を形成する塗布液とを、所定の温度及び所定の速度で前記基材上に同時重層塗布する塗布工程を含み、
前記最下層用塗布液は、前記所定の温度における粘度が0.1~20mPa・sの範囲内であり、
前記最下層用塗布液を50質量%に濃縮した濃縮液は、外径6mmのガラス棒を当該濃縮液に鉛直方向に3cm浸し、前記所定の温度及び前記所定の速度で前記ガラス棒を鉛直方向に引き上げて、当該濃縮液から出る曳糸が切れたときの曳糸の長さを5回測定した場合における平均曳糸長さが5cm以下であることを特徴とする光学フィルムの製造方法。 - 前記積層膜が、光線の反射又は透過について波長選択性を有することを特徴とする請求項1に記載の光学フィルムの製造方法。
- 前記積層膜が、赤外線反射性を有することを特徴とする請求項2に記載の光学フィルムの製造方法。
- 前記光学機能層が、ポリビニルアルコールを含むことを特徴とする請求項1から請求項3までのいずれか一項に記載の光学フィルムの製造方法。
- 互いに隣接する前記光学機能層に含まれるポリビニルアルコールのケン化度の差が、3モル%以上であることを特徴とする請求項4に記載の光学フィルムの製造方法。
- 前記所定の速度が、30~200m/minの範囲内であることを特徴とする請求項1から請求項5までのいずれか一項に記載の光学フィルムの製造方法。
- 前記濃縮液は、前記平均曳糸長さが3cm以下であることを特徴とする請求項1から請求項6までのいずれか一項に記載の光学フィルムの製造方法。
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