WO2016056319A1 - Couche de protection contre le rayonnement infrarouge et film de protection contre le rayonnement infrarouge - Google Patents

Couche de protection contre le rayonnement infrarouge et film de protection contre le rayonnement infrarouge Download PDF

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Publication number
WO2016056319A1
WO2016056319A1 PCT/JP2015/074446 JP2015074446W WO2016056319A1 WO 2016056319 A1 WO2016056319 A1 WO 2016056319A1 JP 2015074446 W JP2015074446 W JP 2015074446W WO 2016056319 A1 WO2016056319 A1 WO 2016056319A1
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shielding film
infrared shielding
infrared
resin
metal
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PCT/JP2015/074446
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English (en)
Japanese (ja)
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明土 川浪
聡史 久光
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コニカミノルタ株式会社
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/22—Absorbing filters
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/26—Reflecting filters
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters

Definitions

  • the present invention relates to an infrared shielding film and an infrared shielding film.
  • infrared shielding films that are attached to windows of buildings and vehicles to block the transmission of solar heat rays (infrared rays).
  • the infrared shielding film is required to have high infrared shielding characteristics and high optical characteristics such as high visible light transmittance.
  • infrared absorbing particles such as tungsten oxide and composite tungsten oxide for the purpose of imparting infrared shielding properties.
  • tungsten oxide and composite tungsten oxide have a problem of weather resistance such that the infrared shielding properties deteriorate with time.
  • Patent Document 1 pays attention to the fact that radicals are generated by irradiating tungsten oxide or composite tungsten oxide with ultraviolet rays or the like, and ultraviolet curing resin, thermoplastic resin, thermosetting resin, room temperature Cs, Sr, Ba, Ti, an infrared shielding film containing one or more media selected from a cured resin, a metal alkoxide, a hydrolysis polymer of metal alkoxide, and tungsten oxide particles or composite tungsten oxide particles.
  • Patent Document 2 states that the heat ray shielding performance of heat ray shielding fine particles such as tungsten oxide and composite tungsten oxide is lowered due to the influence of heat generated in receiving sunlight, water in the air, and oxygen. Paying attention, add a salt of one or more metal elements selected from Mg, Ni, Zn, In and Sn to an infrared shielding film containing polycarbonate resin and tungsten oxide particles or composite tungsten oxide particles Thus, a method for improving the weather resistance is proposed. Furthermore, in Patent Document 2, as a heat-resistant dispersant that can be used for melt-kneading at a high temperature of 200 ° C. or higher in order to obtain good optical characteristics by uniformly dispersing heat ray shielding fine particles in a polycarbonate resin, A method of adding a dispersant having a hydroxyl group or an epoxy group as a functional group in the main chain is proposed.
  • the present invention has been made paying attention to the above-mentioned problems, and the problem is that the generation of haze is suppressed, and the infrared ray has excellent weather resistance and high infrared shielding performance with little change in optical characteristics over time. It is to provide a shielding film. Furthermore, it is providing the infrared shielding film provided with the said infrared shielding film.
  • an alkylene oxide or styrene sulfonic acid group having 2 to 4 carbon atoms is contained in the plastic resin that is the main component of the infrared shielding film. It has been found that the above-mentioned problems can be solved by containing an additive resin having an SP value difference ( ⁇ SP value) of 3 or less.
  • ⁇ SP value SP value difference
  • the infrared shielding film includes a plastic resin composition, at least one infrared absorbing particle of tungsten oxide or composite tungsten oxide, a metal salt, and an alkylene oxide or styrene sulfonic acid group having 2 to 4 carbon atoms. And the absolute value of the difference in SP value ( ⁇ SP value) between the plastic resin contained in the plastic resin composition and the additive resin is 3 or less, and the metal salt and the An infrared shielding film, wherein an absolute value of a difference ( ⁇ SP value) in SP value from an additive resin is 3 or less. 2. 2. The infrared shielding film according to item 1, wherein the metal in the metal salt and the additive resin have a mass ratio of the metal to the additive resin amount of 0.02 or more.
  • the infrared shielding film according to item 1 or 2 wherein the additive resin has a molecular weight in the range of 550 to 55000. 4).
  • the metal salt is a metal organic salt or a metal inorganic salt containing a metal element selected from alkali metal, alkaline earth metal, nickel, manganese, cerium, zinc, copper, cobalt, zirconium, iron and aluminum. 5.
  • the infrared shielding film according to any one of items 1 to 4. 6 An infrared shielding film comprising the infrared shielding film according to any one of items 1 to 5 and a base material. 7).
  • the above means of the present invention it is possible to provide an infrared shielding film having excellent weather resistance and high infrared shielding performance in which the occurrence of haze is suppressed and the change in optical characteristics over time is small. Furthermore, the infrared shielding film provided with the said infrared shielding film can be provided.
  • the infrared shielding film of the present invention includes an infrared shielding film comprising a plastic resin composition, at least one infrared absorbing particle of tungsten oxide or tungsten oxide, a metal salt, and an alkylene having 2 to 4 carbon atoms.
  • An additive resin having an oxide or styrene sulfonic acid group, and a ⁇ SP value between the plastic resin and the additive resin contained in the plastic resin composition is 3 or less, and the metal salt and the additive resin
  • the absolute value of the difference between the SP values ( ⁇ SP value) is 3 or less.
  • the present invention relates to a difference between a metal salt or a metal dissolution parameter in the metal salt (hereinafter referred to as SP value) and a dissolution parameter of a plastic resin which is a main component of the infrared shielding film, that is, SP value (hereinafter referred to as “ ⁇ SP value”). ").") was made by paying attention to the point of dissociation.
  • SP value is one of the parameters representing affinity, and the smaller the ⁇ SP value, the higher the affinity.
  • the absolute value of the ⁇ SP value of the additive resin and the plastic resin as the main component of the infrared shielding film is 3 or less, preferably 2 or less, more preferably 1 or less. Since the absolute value of the ⁇ SP value is 3 or less and the additive resin has an affinity for the plastic resin, the additive resin can be dispersed in the infrared shielding film.
  • the SP value of a metal salt is in the range of 10 to 15, and the metal in the metal salt is in the range of 10 to 80. Therefore, the additive resin according to the present invention has an absolute value of ⁇ SP value of 3 or less, preferably a functional group having high affinity with the metal salt or the metal in the metal salt, or the metal in the metal salt or the metal salt, It is presumed that the metal salt or the metal in the metal salt is fixed by the functional group and aggregation of the metal salts is suppressed by being 2 or less, more preferably 1 or less.
  • an alkylene oxide or styrene sulfonic acid group having 2 to 4 carbon atoms is preferable as a functional group having high affinity with the metal salt.
  • SP value in this specification is a method by Fedors [Polym. Eng. Sci. 14 (2) 152, (1974)].
  • the present invention is not limited to the embodiments described below, and the embodiments are arbitrarily modified within the scope not departing from the gist of the present invention. It is possible.
  • the additive resin according to the present invention has an alkylene oxide or styrene sulfonic acid group having 2 to 4 carbon atoms, and an absolute value of ⁇ SP value with the plastic resin is 3 or less.
  • the additive resin in the present invention has a functional group having an affinity for a metal salt or a metal in the metal salt, while having an affinity for a plastic resin.
  • the additive resin itself is prevented from precipitating and bleeding out from the infrared shielding film.
  • the metal group in which the said functional group has affinity or the metal in a metal salt is attracted and fixed, aggregation of metal salts is suppressed and it is estimated that generation
  • the alkylene oxide according to the present invention is presumed that the hydroxyl group in the structure attracts and fixes the metal salt or the metal in the metal salt.
  • the alkylene oxide having 2 to 4 carbon atoms include polyethylene glycol, polypropylene glycol, polybutylene glycol, etc. Among these, polypropylene glycol is preferable. These may be used alone or in combination of two or more.
  • the styrene sulfonic acid group according to the present invention is presumed that the SO 3 group contained in the structure attracts and fixes the metal salt or the metal in the metal salt.
  • the mass ratio of the metal to the amount of the added resin is preferably 0.02 or more, and particularly preferably the mass ratio is 0.04 or more.
  • a metal salt in the additive resin or a functional group showing affinity for the metal in the metal salt that is, an alkylene oxide or styrene sulfonic acid group having 2 to 4 carbon atoms
  • the mass ratio is less than 0.02
  • the metal salt or the metal in the metal salt cannot be sufficiently immobilized, and it becomes difficult to effectively suppress aggregation of the metal salts.
  • the amount of metal was measured using ICP-AES (SPS3520UV: SII Nano Technology). More specifically, the hard coat component was heated at 800 ° C., and the residue was dissolved with a strong acid or strong base, and quantitatively measured by ICP-AES. The amount of added resin was measured using LC / MS (HP1100 / LCQ Advantage: Agilent / Thermo Fisher). More specifically, after the hard coat component was immersed in ethanol for 24 hours, the ethanol solution from which the solid hard coat component was removed was quantitatively measured by LC / MS. Using each measured value, the mass ratio of the metal to the amount of added resin was calculated.
  • ICP-AES SPS3520UV: SII Nano Technology
  • the additive resin preferably has an equivalent ratio of alkylene oxide or styrene sulfonic acid group within the range of 2 to 4 carbon atoms in the additive resin of 0.5 or more, more preferably 0.8 or more, Especially preferably, it is 0.9 or more.
  • the equivalent ratio is 0.5 or more, the ratio of the additive resin in the plastic composition can be suppressed. By suppressing the ratio, it becomes easy to control physical properties such as electrical properties, mechanical properties, optical properties, and chemical properties of the plastic composition.
  • the said equivalent ratio is less than 0.5, it means that there are few functional groups which suppress aggregation of a metal salt in addition resin. In this case, it is necessary to increase the ratio of the additive resin in the plastic composition in order to sufficiently fix the metal salt or the metal in the metal salt and suppress aggregation between the metal salts.
  • the equivalent ratio of alkylene oxide or styrene sulfonic acid group having 2 to 4 carbon atoms in the additive resin was measured using LC / MS (HP1100 / LCQ Advantage: Agilent / Thermo Fisher).
  • the molecular weight of the additive resin according to the present invention is preferably in the range of 550 to 55000, particularly preferably in the range of 1000 to 50000. If it is 550 or more, the metal salt in the added resin or the functional group having an affinity for the metal in the metal salt does not flow in the plastic resin composition after attracting and fixing the metal, which is effective. It is presumed that aggregation of metal salts can be suppressed. Further, if it is 55000 or less, it is presumed that since the compatibility between the plastic resin and the additive resin is excellent and the dispersibility of the additive resin in the plastic resin composition is excellent, aggregation of metal salts can be effectively suppressed.
  • the main component of the plastic resin composition according to the present invention is a plastic resin, and the plastic resin is not particularly limited as long as the ⁇ SP value with the additive resin is within 3, but is not limited to silicone, acrylic, melamine, Epoxy, acrylate and polyfunctional (meth) acrylic compounds are preferred.
  • the plastic resin composition can contain an additive or the like as necessary within a range not impairing the effects of the present invention.
  • an additive or the like for example, dispersants, plasticizers, UV stabilizers, surfactants, antioxidants, flame retardants, preservatives, antioxidants, thermal stabilizers, lubricants, fillers, photoinitiators, photosensitizers, thermal polymerization Initiators, thickeners, coupling agents, antistatic agents, UV absorbers, leveling agents, adhesion modifiers, modifiers, or additives such as dyes and pigments to give any color tone may be included. . These may be used alone or in combination of two or more.
  • Infrared absorbing particles are compound particles that have absorption characteristics in the infrared wavelength region and have optical absorption characteristics.
  • the tungsten oxide or composite tungsten oxide that absorbs light in the infrared region particularly, having a wavelength of 1000 nm or more. Use at least one of the objects.
  • tungsten trioxide since there are no effective free electrons in tungsten trioxide, tungsten trioxide has little absorption and reflection characteristics in the near infrared region and is not effective as an infrared absorbing particle.
  • an infrared absorbing particle which is transparent in the visible light region and tungsten oxide particles and composite tungsten having absorption in the near infrared region.
  • Oxide particles are found and the tungsten oxide particles or / and composite tungsten oxide particles can be used as infrared absorbing particles.
  • the tungsten oxide is represented by the general formula WyOz (W is tungsten, O is oxygen, 2.2 ⁇ z / y ⁇ 2.999), and the composite tungsten oxide is represented by the general formula MxWyOz (where M H, He, alkali metal, alkaline earth metal, rare earth element, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Be, Hf, Os
  • M H He, alkali metal, alkaline earth metal, rare earth element, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd Al, Ga, In, Tl, Si, Ge, S
  • the composite tungsten oxide is represented by the general formula MxWyOz and has excellent durability when it has a hexagonal, tetragonal, or cubic crystal structure.
  • the above crystal structure is preferably included.
  • hexagonal crystals are particularly preferred because they have the least absorption in the visible light region.
  • a composite tungsten oxide having a hexagonal crystal structure one type selected from each element of Cs, Rb, K, Tl, In, Ba, Li, Ca, Sr, Fe, and Sn as preferable M elements.
  • a composite tungsten oxide containing the above elements can be given.
  • a cesium-containing composite tungsten oxide is preferable from the viewpoints of infrared shielding properties and weather resistance.
  • x / y indicating the amount of element M added. If the value of x / y is larger than 0.001, a sufficient amount of free electrons is generated and the intended infrared shielding effect can be obtained. As the amount of the element M added increases, the supply amount of free electrons increases and the infrared shielding efficiency also increases. However, when the value of x / y is about 1, the effect is saturated. Moreover, if the value of x / y is smaller than 1, it is preferable because an impurity phase can be prevented from being generated in the infrared absorbing particles.
  • the particle diameter of the infrared absorbing particles can be selected depending on the purpose of use.
  • the particle diameter is 200 nm or less, preferably 100 nm or less.
  • the reason for this is that if the particle size of the particles is small, the scattering of light in the visible light region having a wavelength of 400 to 780 nm due to geometric scattering or Mie scattering is reduced, and as a result, the infrared shielding film becomes like frosted glass, This is because it is possible to avoid the loss of clear transparency. That is, when the particle diameter is 200 nm or less, the geometric scattering or Mie scattering is reduced and a Rayleigh scattering region is obtained. This is because in the Rayleigh scattering region, the scattered light is reduced in inverse proportion to the sixth power of the particle diameter, so that the scattering is reduced and the transparency is improved as the particle diameter is reduced. Furthermore, when the particle diameter is 100 nm or less, the scattered light is preferably extremely small. From the viewpoint of avoiding light scattering, a smaller particle diameter is preferable. If the particle diameter is 1 nm or more, industrial production is easy.
  • the haze value of the infrared shielding film in which the infrared absorbing particles are dispersed in a medium such as resin can be set to 30% or less when the visible light transmittance is 85% or less.
  • the haze is a value larger than 30%, it becomes like frosted glass, and clear transparency cannot be obtained.
  • the composite tungsten oxide or the tungsten oxide may be used singly or in combination of two or more.
  • it may be used in combination with compound particles having optical absorption characteristics such as titanium oxide, cerium oxide, indium oxide, zinc sulfide, zinc oxide, anti-doped tin oxide (ATO) and tin-doped indium oxide (ITO).
  • the entire surface or a part of the infrared absorbing particles is coated with an oxide containing one or more kinds of metals of Si, Ti, Zr, and Al.
  • the coating method is not particularly limited, the surface of the infrared absorbing particles can be coated by adding the metal alkoxide to the solution in which the infrared absorbing particles are dispersed.
  • the metal salt according to the present invention is added for the purpose of suppressing deterioration over time of the infrared shielding properties of the infrared shielding film and improving the weather resistance.
  • the metal salt applied to the present invention is a metal organic salt or metal inorganic composed of a metal selected from alkali metals, alkaline earth metals, nickel, manganese, cerium, zinc, copper, cobalt, zirconium, iron, aluminum and tin. It is a salt, and these may be used alone or in combination of two or more.
  • the content of the metal salt contained in the infrared shielding film is preferably within the range of 5 to 60 parts by mass with respect to 100 parts by mass of the infrared absorbing particles, from the viewpoint of compatibility, dispersibility, and haze. Preferably, it is within the range of 10 to 40 parts by mass.
  • the amount is less than 5 parts by mass, it is not possible to sufficiently suppress the temporal deterioration of the infrared shielding property.
  • the amount exceeds 60 parts by mass the compatibility with the plastic resin or the solvent is inferior, the dispersibility is reduced, and the haze is reduced. An increase occurs.
  • the solvent is not particularly limited, and a known organic solvent can be used.
  • alcohol solvents such as methanol (MA), ethanol (EA), 1-propanol (NPA), isopropanol (IPA), butanol, pentanol, benzyl alcohol, diacetone alcohol, acetone, methyl ethyl ketone (MEK) , Ketone solvents such as methyl propyl ketone, methyl isobutyl ketone (MIBK), cyclohexanone, isophorone, ester solvents such as 3-methyl-methoxy-propionate (MMP), ethylene glycol monomethyl ether (MCS), ethylene glycol monoethyl ether (ECS), ethylene glycol isopropyl ether (IPC), propylene glycol methyl ether (PGM), propylene glycol ethyl ether (PE), propylene glycol methyl ether (PGM), propylene glycol ethyl ether
  • organic solvents having a low polarity are preferable, and particularly highly hydrophobic ones such as ketones such as MIBK and MEK, aromatic hydrocarbons such as toluene and xylene, glycol ether acetates such as PGMEA and PE-AC, and the like. More preferred. These solvents can be used alone or in combination of two or more.
  • a dispersion in which infrared absorbing particles are dispersed in a solvent, a plastic resin, a metal salt, an additive resin, etc. are added to prepare a plastic resin composition.
  • a method of forming a coating film by applying a plastic resin composition to the surface of a substrate and evaporating a solvent from the coating film.
  • the method for applying the plastic resin composition is not particularly limited as long as a coating film can be uniformly formed on the surface of the substrate, and a bar coating method, a gravure coating method, a spray coating method, a dip coating method, or the like can be used.
  • a film or a board may be used if desired, and a shape is not limited.
  • An infrared shielding film or an infrared shielding laminated body is obtained by laminating an infrared shielding film on a resin base material or transparent molded body transparent to visible light.
  • the transparent molded body PET, acrylic, urethane, polycarbonate, polyethylene, ethylene vinyl acetate copolymer, polyvinyl chloride, fluororesin, inorganic glass, resin glass, and the like can be used for various purposes.
  • the ⁇ SP value of the solvent and the plastic resin is more preferably within 5 or less.
  • the infrared shielding film of the present invention has a laminated structure including at least an infrared shielding film.
  • an infrared shielding film which concerns on this invention is demonstrated, this invention is not restrict
  • the infrared shielding film of the present invention can be used as a functional layer by appropriately selecting components such as a plastic resin and an additive.
  • the functional layer is a hard coat layer, or a conductive layer, an antistatic layer, a gas barrier layer, an antifouling layer, a deodorizing layer, a droplet layer, a slippery layer, an abrasion resistant layer, a protective layer, Separation layer, antireflection layer, electromagnetic wave shielding layer, ultraviolet absorption layer, infrared absorption layer, printing layer, fluorescent light emitting layer, hologram layer, release layer, adhesive layer, adhesive layer, high refractive index layer and low refractive index of the present invention It is a layer selected from an infrared cut layer (metal layer, liquid crystal layer) other than the layer, a colored layer (visible light absorbing layer), and an interlayer film used for laminated glass.
  • the infrared shielding film of the present invention is preferably used as a hard coat layer or an adhesive layer and disposed on the outermost surface of the infrared shielding film.
  • the order of lamination of the layers is not particularly limited, and the present invention is not limited to these.
  • E Infrared shielding film (hard coat layer) / Base material / Infrared reflective layer / Adhesive layer
  • the infrared shielding film By disposing an adhesive layer having adhesiveness on the outermost layer of the infrared shielding film, the infrared shielding film can be affixed to the indoor (inside or inside) or outdoor side of a substrate such as a glass window of a vehicle or a building. Moreover, by providing a hard coat layer as the outermost layer of the infrared shielding film, it is possible to impart scratch resistance to the surface of the infrared shielding film.
  • FIG. 1 is an example of an embodiment of an infrared shielding film in the present invention.
  • the infrared shielding film 5 is bonded to the base 1 via the adhesive layer 2.
  • a specific infrared wavelength region is reflected by the infrared reflecting layer 3 with respect to infrared rays incident from the substrate 1 in the direction of the infrared shielding film 4, and the infrared shielding film 4 absorbs infrared wavelengths that could not be reflected by the infrared reflecting layer 3. can do.
  • the infrared reflective layer 3 the infrared wavelength that can be shielded is wide, and the infrared shielding film 5 having high infrared shielding performance is obtained.
  • the infrared shielding film In the specification of attaching the infrared shielding film to the indoor side of the window glass (internal bonding), it is preferable to laminate the infrared reflection layer and the infrared shielding film in this order from the sunlight incident side, and the infrared shielding film of the present invention is provided on the outdoor side of the window glass. In the specifications for pasting (outside pasting), it is preferable to laminate the hard coat layer, the infrared reflecting layer, the infrared shielding film, and the adhesive layer in this order from the sunlight incident side.
  • the infrared shielding film and the infrared reflecting layer since the amount of infrared rays irradiated to the infrared shielding film is suppressed by arranging the infrared reflecting layer on the incident direction side with respect to the incident direction of infrared rays, the infrared shielding film Heat generation generated when the infrared absorbing particles contained in the resin absorb infrared rays is prevented, and high weather resistance is obtained.
  • the hard coat layer of the present invention refers to a film having a pencil hardness of H to 8H. Particularly preferably, it is in the range of 2H to 6H.
  • the pencil hardness is evaluated by pencil hardness evaluation specified by JIS K 5400 using a test pencil specified by JIS S 6006 after the prepared hard coat layer is conditioned for 2 hours at a temperature of 25 ° C. and a relative humidity of 60%. It is the value measured according to the method.
  • plastic resin used for the hard coat layer examples include organic hard coat materials such as silicone, melamine, epoxy, acrylate, and polyfunctional (meth) acrylic compounds; inorganic hard coat materials such as silicon dioxide; etc. Is mentioned.
  • organic hard coat materials such as silicone, melamine, epoxy, acrylate, and polyfunctional (meth) acrylic compounds
  • inorganic hard coat materials such as silicon dioxide; etc. Is mentioned.
  • a hard coat forming material of a (meth) acrylate-based or polyfunctional (meth) acrylic-based compound examples of the plastic resin used for the hard coat layer.
  • (meth) acryl refers to acrylic and methacrylic.
  • the hard coat layer is preferably a layer mainly composed of a resin that is cured through a crosslinking reaction, and more preferably an actinic radiation curable resin.
  • an ultraviolet curable resin is preferably used as the actinic radiation curable resin.
  • the ultraviolet curable resin is not particularly limited.
  • ADEKA OPTMER KR, BY series KR-400, KR-410, KR-550, KR-566, KR-567, BY-320B (above, Asahi Denka Kogyo Co., Ltd.) Manufactured by Koeihard Co., Ltd.), A-101-KK, A-101-WS, C-302, C-401-N, C-501, M-101, M-102, T-102, D-102 NS-101, FT-102Q8, MAG-1-P20, AG-106, M-101-C (manufactured by Guangei Chemical Industry Co., Ltd.), Seika Beam PHC2210 (S), PHCX-9 (K-3) ), PHC2213, DP-10, DP-20, DP-30, P1000, P1100, P1200, P1300, P1400, P
  • the coating composition for the UV curable resin layer preferably has a solid content in the range of 10 to 95% by mass, and an appropriate concentration is selected depending on the coating method.
  • any light source that generates ultraviolet rays can be used.
  • the aforementioned light source can be used.
  • Irradiation conditions vary depending on each lamp, but the amount of irradiation light may be about 20 to 1200 mJ / cm 2 , and preferably 50 to 1000 mJ / cm 2 . From the near ultraviolet region to the visible light region, it can be used by using a sensitizer having an absorption maximum in that region.
  • the dry film thickness of the hard coat layer is in the range of an average film thickness of 0.1 to 30 ⁇ m, preferably in the range of 1 to 20 ⁇ m, particularly preferably in the range of 3 to 15 ⁇ m. When it is 3 ⁇ m or more, sufficient durability and impact resistance can be obtained. Moreover, it is preferable that it is 15 micrometers or less from a flexible or economical viewpoint.
  • the hard coat layer can be formed, for example, by irradiating active rays during or after drying after applying a hard coat layer-forming coating solution obtained by dissolving an active ray curable resin in an organic solvent.
  • the coating method for the hard coat layer coating composition is not particularly limited, and for example, it can be coated by a known method such as a gravure coater, dip coater, reverse coater, wire bar coater, die coater, or ink jet method. It is preferable to apply a wet film thickness within a range of 0.1 to 100 ⁇ m on one surface of the plastic resin substrate using the above-described application method.
  • the hard coat layer may be a single layer or a multilayer structure of two or more layers.
  • inorganic or organic fine particles are added to the coating composition of the hard coat layer in order to give the hard coat layer an antiglare property, to prevent adhesion with other substances, and to improve scratch resistance and the like. You can also.
  • the average particle size of the fine particle powder is in the range of 0.01 to 10 ⁇ m, and the amount used is blended so as to be in the range of 0.1 to 20 parts by mass with respect to 100 parts by mass of the ultraviolet curable resin composition. It is desirable to do. In order to impart an antiglare effect, it is preferable to use 1 to 15 parts by mass of fine particles having an average particle size in the range of 0.1 to 1 ⁇ m with respect to 100 parts by mass of the ultraviolet curable resin composition.
  • an antioxidant that does not inhibit the photocuring reaction can be selected and used.
  • examples include hindered phenol derivatives, thiopropionic acid derivatives, phosphite derivatives, and the like.
  • 4,4′-thiobis (6-tert-3-methylphenol), 4,4′-butylidenebis (6-tert-butyl-3-methylphenol), 1,3,5-tris (3,5-di-tert-butyl-4-hydroxybenzyl) isocyanurate, 2,4,6-tris (3,5-di-tert-butyl-4-hydroxybenzyl) mesitylene, di-octadecyl-4-
  • examples include hydroxy-3,5-di-tert-butylbenzyl phosphate.
  • the hard coat layer coating solution may contain a solvent, or may be appropriately contained and diluted as necessary.
  • the organic solvent contained in the coating solution include hydrocarbons (toluene, xylene), alcohols (methanol, ethanol, isopropanol, butanol, cyclohexanol), ketones (acetone, methyl ethyl ketone, methyl isobutyl ketone), It can be appropriately selected from esters (methyl acetate, ethyl acetate, methyl lactate), glycol ethers, and other organic solvents, or a mixture thereof can be used.
  • Propylene glycol monoalkyl ether (1 to 4 carbon atoms in the alkyl group) or propylene glycol monoalkyl ether acetate ester (1 to 4 carbon atoms in the alkyl group) is 5% by mass or more, more preferably 5 to 80%. It is preferable to use the organic solvent contained in a mass% range.
  • the hard coat layer is a hard coat layer having a good smooth surface with a centerline average surface roughness Ra specified by JIS B 0601 of less than 0.05 ⁇ m, more preferably less than 0.002 to 0.04 ⁇ m. Can do.
  • the center line average roughness (Ra) is preferably measured by an optical interference type surface roughness measuring instrument, for example, using a non-contact surface fine shape measuring device (WYKO NT-2000) manufactured by WYKO. be able to.
  • ultrafine particles having a volume average particle size of 0.005 to 0.1 ⁇ m in the same components as described above are added in an amount of 0.1 to 100 parts by mass with respect to 100 parts by mass of the resin composition. 5 parts by mass can also be used.
  • a binder such as a known thermoplastic resin, thermosetting resin or hydrophilic resin such as gelatin can be mixed with the above active energy ray curable resin.
  • These resins preferably have polar groups in the molecule.
  • the polar group includes —COOM, —OH, —NR 2 , —NR 3 X, —SO 3 M, —OSO 3 M, —PO 3 M 2 , —OPO 3 M (where M is a hydrogen atom, alkali A metal or an ammonium group, X represents an acid that forms an amine salt, R represents a hydrogen atom or an alkyl group).
  • an antioxidant that does not inhibit the photocuring reaction can be selected and used.
  • examples include hindered phenol derivatives, thiopropionic acid derivatives, phosphite derivatives, and the like.
  • 4,4′-thiobis (6-t-3-methylphenol), 4,4′-butylidenebis (6-t-butyl-3-methylphenol), 1,3,5-tris (3,5-di-t-butyl-4-hydroxybenzyl) isocyanurate, 2,4,6-tris (3,5-di-t-butyl-4-hydroxybenzyl) mesitylene, di-octadecyl-4- Hydroxy-3,5-di-t-butylbenzyl phosphate and the like can be mentioned.
  • various additives can be further blended as necessary within the range where the effects of the present invention are not impaired.
  • an antioxidant an ultraviolet stabilizer, an ultraviolet absorber, a surfactant, a leveling agent, an antistatic agent and the like can be used.
  • the infrared shielding film of the present invention can be provided with an adhesive layer for the purpose of imparting adhesiveness for attaching the infrared shielding film to a substrate such as a window glass.
  • polymer materials such as elastomer and synthetic resin can be mentioned, and the material is appropriately selected depending on the material to be adhered and the use conditions of the member after adhesion.
  • resins, melamine resins, phenol resins, resorcinol resins, epoxy resins, polyimide resins, natural rubber, chloroprene rubber and the like examples include resins, melamine resins, phenol resins, resorcinol resins, epoxy resins, polyimide resins, natural rubber, chloroprene rubber and the like.
  • an acrylic resin (acrylic adhesive) or a silicone resin (silicone adhesive) is preferable.
  • an acrylic adhesive is preferable from the viewpoint of adhesive properties and cost.
  • solvent-based and emulsion-based acrylic adhesives are preferable, and solvent-based acrylic adhesives are more preferable because the peel strength can be easily controlled.
  • solvent-based acrylic adhesive known monomers can be used as the monomer.
  • This adhesive layer contains additives such as stabilizers, surfactants, UV absorbers, flame retardants, antistatic agents, antioxidants, thermal stabilizers, lubricants, fillers, coloring, adhesion modifiers, etc. It can also be made.
  • additives such as stabilizers, surfactants, UV absorbers, flame retardants, antistatic agents, antioxidants, thermal stabilizers, lubricants, fillers, coloring, adhesion modifiers, etc.
  • an ultraviolet absorber is effective for suppressing deterioration of the infrared shielding film due to ultraviolet rays.
  • the thickness of the adhesive layer is preferably in the range of 1 to 100 ⁇ m, more preferably in the range of 3 to 50 ⁇ m. If it is 1 micrometer or more, it exists in the tendency for adhesiveness to improve and sufficient adhesive force is obtained when an infrared shielding film is bonded to a base
  • any known method can be used.
  • a die coater method, a gravure roll coater method, a blade coater method, a spray coater method, an air knife coat method, a dip coat method, a transfer method, etc. are preferable.
  • These can be appropriately formed into a solution with a solvent capable of dissolving the adhesive, or can be applied using a dispersed coating solution, and known solvents can be used.
  • the adhesive layer may be formed directly on the infrared shielding film by the previous coating method, or once coated on the release film and dried, the infrared shielding film is bonded to the adhesive. May be transferred.
  • the drying temperature at this time is preferably such that the residual solvent is as small as possible.
  • the drying temperature and time are not specified, but preferably within the range of 50 to 150 ° C. and within the range of 10 seconds to 5 minutes. It is preferable to provide a drying time.
  • the infrared reflective layer in the present invention has a laminated structure in which at least three low refractive index layers or high refractive index layers are laminated.
  • a preferred form of the infrared reflecting layer has a form of an alternating laminate in which low refractive index layers and high refractive index layers are alternately laminated.
  • a refractive index layer having a higher refractive index than the other is referred to as a high refractive index layer
  • a refractive index layer having a lower refractive index than the other is referred to as a low refractive index layer.
  • the transmittance in the visible light region shown in JIS R3106-1998 is 50% or more, preferably 75% or more, more preferably 85% or more. It is preferable to have a region with a reflectance exceeding 50% in the region of 900 to 1400 nm.
  • the material for forming the infrared reflective layer conventionally known materials can be used, and examples thereof include metal oxide particles, polymers, and combinations thereof. It is preferable that at least one of the low refractive index layer and the high refractive index layer includes metal oxide particles, and it is more preferable that both include metal oxide particles.
  • the metal oxide particles may include titanium dioxide (TiO 2 ), zirconium dioxide (ZrO 2 ), tantalum pentoxide (Ta 2 O 5 ), and the like as examples of the high refractive index material.
  • examples thereof include silicon dioxide (SiO 2 ) and magnesium fluoride (MgF 2 ). These metal oxide particles can be dispersed in a polymer solution to form a coating.
  • the polymer contained in the infrared reflective layer is not particularly limited as long as it is a polymer that can form an infrared reflective layer.
  • the polymer described in JP-T-2002-509279 can be used as the polymer.
  • Specific examples include, for example, polyethylene naphthalate (PEN) and its isomers (eg, 2,6-, 1,4-, 1,5-, 2,7- and 2,3-PEN), polyalkylene terephthalate.
  • Copolymers such as copolymers of PEN [e.g. (a) terephthalic acid or ester thereof, (b) isophthalic acid or ester thereof, (c) phthalic acid or ester thereof, (d) alkane glycol, (e) cycloalkane glycol ( For example, cyclohexanedimethanoldiol), (f) alkanedicarboxylic acid, and / or (g) cycloalkanedicarboxylic acid (eg, cyclohexanedicarboxylic acid) and 2,6-, 1,4-, 1,5-, 2, 7- and / or copolymers with 2,3-naphthalenedicarboxylic acid or esters thereof], copolymers of polyalkylene terephthalates [eg (a) naphthalenedicarboxylic acid or esters thereof, (b) isophthalic acid or esters thereof, ( c) Phthalic acid or its s (D) alkan
  • each layer may each include a blend of two or more of the above polymers or copolymers (eg, a blend of syndiotactic polystyrene (SPS) and atactic polystyrene). These polymers may be used alone or in combination of two or more.
  • SPS syndiotactic polystyrene
  • an infrared reflecting layer can be formed from the polymer by melt extrusion and stretching of the polymer.
  • a water-soluble polymer as the polymer.
  • the high-refractive index layer or low-refractive index layer of the infrared shielding film of the present invention includes an ultraviolet absorber, an anti-fading agent, a curing agent, various anionic, cationic or nonionic surfactants, fluorescent whitening agents, sulfuric acid, Various known additives such as phosphoric acid, acetic acid, citric acid, sodium hydroxide, potassium hydroxide, potassium carbonate and other pH adjusters, antifoaming agents, diethylene glycol and other lubricants, preservatives, antistatic agents, matting agents, etc. May be contained.
  • the method for producing the infrared reflective layer is not particularly limited, and a coextrusion method, a melt extrusion method, or the like can be used.
  • a melt extrusion method as in the method described in US Pat. No. 6,049,419, in addition to a method of forming an infrared reflective layer by melt extrusion and stretching of a polymer, an aqueous high refractive index layer is used. Examples include a method in which a coating solution and a coating solution for a low refractive index layer are alternately wet-coated and dried to form a laminate.
  • the following coating methods are preferably used.
  • rod bar coating method rod bar coating method, air knife coating method, spray coating method, curtain coating method, US Pat. Nos. 2,761,419 and 2,761,791
  • a slide hopper coating method, an extrusion coating method or the like is preferably used.
  • sequential multilayer coating or simultaneous multilayer coating may be used as a method of applying a plurality of layers in a multilayer manner.
  • the thicknesses of the coating solution for the high refractive index layer and the coating solution for the low refractive index layer in the infrared shielding film can be controlled by adjusting the coating amount so as to be the above-described preferable thickness at the time of drying.
  • the infrared shielding film of the present invention may use a substrate for the purpose of adding mechanical strength or protecting the constituent layers.
  • Various resin films can be used as the substrate. Specific examples include polyolefin films (polyethylene, polypropylene, etc.), polyester films (polyethylene terephthalate, polyethylene naphthalate, etc.), polyvinyl chloride, cellulose triacetate, etc., preferably polyester films. These may be used alone or in combination of two or more.
  • an antistatic agent an ultraviolet absorber, an antiseptic, a light stabilizer, a surfactant, a flame retardant, an antioxidant, a heat stabilizer, a lubricant, a filler, a modifier, or an arbitrary color tone is given as necessary.
  • Dyes or pigments may be added.
  • the thickness of the substrate used in the present invention is preferably in the range of 3 to 300 ⁇ m, particularly in the range of 20 to 150 ⁇ m.
  • the base material of the present invention may be a laminate of two sheets, and in this case, the type may be the same or different.
  • the infrared shielding film of this invention may have a some base material.
  • the infrared shielding film of the present invention has an infrared shielding performance of preferably at least 48% or more, more preferably 50% or more. Further, the ⁇ haze value after the 1000-hour weather test is 4 or less, more preferably 1.0 or less, and more preferably 0.5 or less.
  • the infrared shielding film provided by the present invention can be applied to a wide range of fields.
  • the infrared shielding film of the present invention is suitably used as a window pasting film for infrared shielding films such as outdoor windows of buildings and windows of vehicles, and films for agricultural greenhouses.
  • the infrared shielding film according to the present invention is suitable as an infrared shielding film used by being bonded to a substrate such as glass or a glass substitute resin directly or via an adhesive layer.
  • an optical shielding body in which the infrared shielding film according to the present invention is provided on at least one surface of a substrate.
  • this include architectural windows and vehicle windows as described above.
  • additive resins used in the present invention are shown in Table 1.
  • the equivalent ratio of alkylene oxide or styrene sulfonic acid group having 2 to 4 carbon atoms in the additive resin shown in Table 1 was measured using LC / MS (HP1100 / LCQ Advantage: Agilent / Thermo Fisher). Except for polyacryl, it was in the range of 0.8 to 1.
  • Metal salt The metal salts used in the present invention are listed in Table 2.
  • Example preparation ⁇ ⁇ Preparation of infrared shielding film forming liquid> (Preparation of infrared shielding film forming liquid 1) 18% Cs 0.33 WO 3 dispersion (product name: YMF-02A, Sumitomo Metal Mining Co., Ltd., 10 parts by weight of dispersant) as 100 parts by weight, UV curable resin (product name: Aronix UV3701, Toa Gosei Co., Ltd.) Company, SP value: 9.5) 23 parts by mass, nickel octylate 5 parts by mass as a metal salt, polyoxyethylene monomethyl ether having a molecular weight of 550 as an additive resin, surfactant (product name: Mega Infrared shielding film-forming liquid 1 was prepared by mixing 0.03 parts by mass of FAC F-552, DIC Corporation) and 83 parts by mass of a solvent (methyl isobutyl ketone, SP value: 9.5).
  • Infrared shielding film forming liquids 2 to 23 were configured as shown in Table 3, and were prepared in the same manner as the infrared shielding film forming liquid 1.
  • the metal salt and the additive resin of the infrared shielding film forming liquid 5 were added as sodium polystyrene sulfonate (product name: PS-1, sodium content 11%, Tosoh Organic Chemical Co., Ltd.).
  • PVA235 polyvinyl alcohol
  • a surfactant 5% by mass aqueous solution SOFTAZOLINE LSB-R, manufactured by Kawaken Fine Chemical Co., Ltd.
  • a coating solution L1 for forming a low refractive index layer was prepared.
  • 10 parts by mass of 15.0% by mass titanium oxide sol SRD-W, volume average particle size: 5 nm, rutile titanium dioxide particles, Sakai Chemical Industry Co., Ltd.
  • 40 parts by mass of pure water 90 ° C. Heated to.
  • silicic acid aqueous solution sodium silicate 4 (manufactured by Nippon Chemical Industry Co., Ltd.) diluted with pure water so that the SiO 2 concentration becomes 4% by mass
  • an autoclave was added. 18 hours of heat treatment performed after cooling at 175 ° C. during and concentrated using an ultrafiltration membrane, at a solids concentration of 20 mass% of titanium dioxide sol was deposited SiO 2 on the surface (hereafter " Also referred to as “silica modified titanium oxide sol”.
  • the low refractive index layer forming coating liquid L1 and the high refractive index layer forming coating liquid H1 prepared above are kept at 40 ° C. while maintaining a thickness of 50 ⁇ m of polyethylene.
  • the terephthalate film (A4300, with a double-sided easy-adhesion layer, manufactured by Toyobo Co., Ltd.)
  • 15 layers of simultaneous multilayer coating were performed.
  • the lowermost layer and the outermost layer were set as low refractive index layers, and other layers were set to be alternately laminated.
  • the coating amount was adjusted so that the film thickness during drying was 150 nm for each low refractive index layer and 130 nm for each high refractive index layer.
  • 5 ° C. cold air was blown and set. After the setting was completed, warm air of 80 ° C. was blown and dried to prepare an infrared reflective layer.
  • Example 1 On the polyethylene terephthalate film (A4300, with double-sided easy-adhesion layer, manufactured by Toyobo Co., Ltd.) having a thickness of 50 ⁇ m, the infrared shielding film forming liquid 1 is applied, and the constant rate drying zone temperature is 50 ° C., the decreasing rate drying zone temperature is 90 ° C. After drying, an ultraviolet lamp was used to cure the irradiated portion with an illuminance of 100 mW / cm 2 and an irradiation amount of 0.2 J / cm 2 to prepare Sample 1. The thickness of the infrared shielding film was adjusted so that the visible light transmittance of Sample 1 was 70%.
  • Samples 2 to 23 were constructed in the same manner as Sample 1 with the configuration shown in Table 2.
  • Sample 1 was prepared in the same manner except that the base material was an infrared reflective layer and the infrared shielding film forming liquid 12 was applied.
  • ⁇ haze before and after the weather resistance test Samples 1 to 24 were irradiated for 500 hours or 1000 hours using a sunshine weatherometer (Suga Test Machine) in accordance with JIS K 6783b. Next, the haze of the sample after irradiation for 500 hours or 1000 hours was measured, and the difference was determined by the haze before the test to obtain ⁇ haze.
  • the haze is an average value obtained from five points measured using “turbidimeter NDH-300A” manufactured by Nippon Denshoku Industries Co., Ltd. in accordance with JIS K7361-1997.
  • Samples 1 to 21 satisfying the requirements of the present invention have excellent heat resistance, haze generation, and excellent weather resistance with little change in optical characteristics over time.
  • the infrared shielding film and infrared shielding film satisfying the requirements of the present invention have high heat shielding performance and excellent weather resistance.
  • the present invention can be suitably used to realize excellent weather resistance and high infrared shielding performance such that generation of haze is suppressed and change in optical characteristics with time is small.

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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

L'invention concerne : une couche de protection contre le rayonnement infrarouge (4), dans laquelle l'apparition de trouble est supprimée, qui présente une excellente résistance aux intempéries et des propriétés de protection contre les infrarouges élevées, ce qui entraîne peu de changement dans les caractéristiques optiques au cours du temps ; un film de protection contre le rayonnement infrarouge (5) pourvu de la couche de protection contre le rayonnement infrarouge. La couche de protection contre le rayonnement infrarouge (4) contient : une composition de résine plastique ; des particules absorbant le rayonnement infrarouge comprenant de l'oxyde de tungstène et/ou un oxyde de tungstène composite ; un sel métallique ; une résine d'additif ayant soit un oxyde d'alkylène ayant 2 à 4 atomes de carbone ou un groupe d'acide styrène sulfonique. La différence de valeur SP (ΔSP) entre la résine plastique et la résine d'additif contenue dans la composition de résine plastique présente une valeur absolue de 3 ou moins, et la différence de valeur SP (ΔSP) entre le sel métallique et la résine d'additif présente une valeur absolue de 3 ou moins.
PCT/JP2015/074446 2014-10-09 2015-08-28 Couche de protection contre le rayonnement infrarouge et film de protection contre le rayonnement infrarouge WO2016056319A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007034789A1 (fr) * 2005-09-20 2007-03-29 Toyo Styrene Co., Ltd. Composition contenant une résine de copolymère composé vinylique aromatique/acide (méth)acrylique et procédé servant à produire celle-ci
JP2009197146A (ja) * 2008-02-22 2009-09-03 Sumitomo Metal Mining Co Ltd 赤外線遮蔽材料微粒子分散液、赤外線遮蔽膜と赤外線遮蔽光学部材およびプラズマディスプレイパネル用近赤外線吸収フィルター
JP2012144418A (ja) * 2010-12-22 2012-08-02 Bridgestone Corp 熱線遮蔽ガラス、及びこれを用いた複層ガラス
WO2013094641A1 (fr) * 2011-12-20 2013-06-27 東洋スチレン株式会社 Composition de résine optique à base de styrène
JP2013170239A (ja) * 2012-02-22 2013-09-02 Sumitomo Metal Mining Co Ltd 複合タングステン酸化物微粒子分散ポリカーボネート樹脂組成物およびそれを用いた熱線遮蔽成形体並びに熱線遮蔽積層体
WO2014045853A1 (fr) * 2012-09-24 2014-03-27 旭硝子株式会社 Composition liquide et objet en verre

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007034789A1 (fr) * 2005-09-20 2007-03-29 Toyo Styrene Co., Ltd. Composition contenant une résine de copolymère composé vinylique aromatique/acide (méth)acrylique et procédé servant à produire celle-ci
JP2009197146A (ja) * 2008-02-22 2009-09-03 Sumitomo Metal Mining Co Ltd 赤外線遮蔽材料微粒子分散液、赤外線遮蔽膜と赤外線遮蔽光学部材およびプラズマディスプレイパネル用近赤外線吸収フィルター
JP2012144418A (ja) * 2010-12-22 2012-08-02 Bridgestone Corp 熱線遮蔽ガラス、及びこれを用いた複層ガラス
WO2013094641A1 (fr) * 2011-12-20 2013-06-27 東洋スチレン株式会社 Composition de résine optique à base de styrène
JP2013170239A (ja) * 2012-02-22 2013-09-02 Sumitomo Metal Mining Co Ltd 複合タングステン酸化物微粒子分散ポリカーボネート樹脂組成物およびそれを用いた熱線遮蔽成形体並びに熱線遮蔽積層体
WO2014045853A1 (fr) * 2012-09-24 2014-03-27 旭硝子株式会社 Composition liquide et objet en verre

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