WO2014061279A1 - 熱線遮蔽シート - Google Patents
熱線遮蔽シート Download PDFInfo
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- WO2014061279A1 WO2014061279A1 PCT/JP2013/006185 JP2013006185W WO2014061279A1 WO 2014061279 A1 WO2014061279 A1 WO 2014061279A1 JP 2013006185 W JP2013006185 W JP 2013006185W WO 2014061279 A1 WO2014061279 A1 WO 2014061279A1
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- heat ray
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- C—CHEMISTRY; METALLURGY
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- C09D7/67—Particle size smaller than 100 nm
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- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Definitions
- the present invention relates to a heat ray shielding sheet that efficiently absorbs and reflects heat rays and has excellent transparency and low haze.
- Patent Document 1 discloses a transparent heat ray shielding performance having a resin pressure sensitive adhesive layer in which heat ray shielding fine particles, for example, ATO (Antimony TinxOxide) fine particles are dispersed in an adhesive so as to be bonded to a window glass or the like.
- a sheet having the following is disclosed.
- Patent Document 2 has at least two heat ray reflecting units composed of two or more layers having different refractive indexes on one surface on a substrate, and the opposite surface on the substrate. And a heat ray blocking film having a heat ray absorbing layer containing an ultraviolet curable resin and tin-doped indium oxide (ITO) or antimony-doped tin oxide (ATO), wherein the heat ray absorbing layer contains a heat conductive filler.
- ITO ultraviolet curable resin
- ATO antimony-doped tin oxide
- a featured heat ray blocking film is disclosed.
- Patent Document 3 a coating liquid containing heat shielding fine particles and a silicon compound or a zirconium compound such as zirconium oxide or a titanium compound such as titanium oxide is applied on glass, and then baked at 500 to 600 ° C. There is disclosed a heat ray reflective film containing particles and silicon oxide, or zirconium oxide or titanium oxide and having radio wave transmissivity having a surface resistance of 10 K ⁇ / ⁇ .
- Patent Document 4 discloses a heat ray reflective film having radio wave permeability or radio wave shielding properties using noble metal fine particles such as Ag, Au, and Pt.
- Patent Document 5 discloses a heat insulating member in which cholesteric liquid crystal that reflects light in the near infrared region and heat shielding fine particles that absorb heat rays having a wavelength longer than the wavelength reflected by the cholesteric liquid crystal are stacked.
- JP-A-10-008010 JP 2012-126037 A Japanese Patent Laid-Open No. 5-70178 Japanese Patent Laid-Open No. 2002-131553 International Publication No. 2000/111548 Pamphlet
- Patent Document 1 is a technology that uses only the near-infrared absorption of ATO fine particles, does not make use of the near-infrared reflectivity of ATO fine particles, and has insufficient heat ray shielding properties. Moreover, since it is only near-infrared absorption, heat
- Patent Document 2 The technology of Patent Document 2 is to shield the heat rays by both the heat ray reflecting unit and the heat ray absorbing layer, and in order to prevent thermal cracking due to heat storage in the heat ray absorbing layer, a heat conductive filler is put in the heat ray absorbing layer, and preferably In order to promote heat dissipation and prevent thermal cracking by keeping the surface roughness and maximum cross-section height within a certain range, an excellent heat-shielding effect is achieved, but a heat conductive filler must be blended. .
- Patent Document 3 there is a problem that the film cannot be applied to a resin substrate such as a PET film because the film is formed by baking at 600 ° C. after coating on the substrate.
- Patent Document 4 since noble metals are used as the heat-shielding fine particles, there is a problem that they are expensive, and the noble metal fine particles are connected to each other at the time of film production, so that sufficient radio wave transmission performance cannot be imparted. Further, in Patent Document 5, heat shielding fine particles that absorb heat rays having a wavelength longer than the wavelength reflected by the cholesteric liquid crystal are laminated. However, the concentration of the heat shielding fine particles with respect to the resin binder is low, and the infrared rays are blocked on the long wavelength side. There is a problem that the thermal effect is insufficient.
- the present invention solves the various problems described above, and can be used for building windows, vehicle windows, refrigeration, frozen showcase window glass, etc., and has excellent transparency in the visible light region and has radio wave transparency. And it aims at development of the heat ray shielding sheet which is excellent also in heat ray shielding property.
- the present inventors have intensively studied to obtain a heat ray shielding sheet that is excellent in transparency, has radio wave permeability, has a greatly improved heat ray shielding property, and does not cause thermal cracking in a glass substrate or the like. .
- metal oxide fine particles such as tin-doped indium oxide are contained in the heat ray shielding layer at a high concentration, and the long-wavelength side of the near infrared (wavelength 2000 nm) due to plasma vibrations in the fine particles
- the surface resistance of the heat ray shielding layer is 10 6 ⁇ / ⁇ so as to reflect 15% or more of the above light, suppress the temperature rise of the heat ray shielding layer, and not impart conductivity when formed into a sheet.
- the present invention has been completed by finding out that thermal cracking of a glass substrate or the like can be prevented without any problems. That is, although it is known that the fine particles are contained in the heat ray shielding layer at a high concentration, in the study by the present inventors, the fine particles are contained in the binder component at a high concentration, and normal stirring (for example, Even when dispersed by stirring with a homogenizer or the like, a heat ray shielding sheet having both sufficient reflection performance and surface resistance could not be obtained.
- the cause is that the fine particles are not sufficiently dispersed, the above-mentioned surface resistance value is not obtained due to the aggregation of fine particles or the connection of fine particles, and the smoothness of the surface is lost. This is probably because the reflection due to plasma oscillation was not fully utilized.
- the present inventors appropriately disperse the fine particles in the binder component by, for example, a bead mill or the like so that the fine particles are in a non-aggregated and non-continuous state and do not hinder the reflective performance of the fine particles. If the dispersion is coated on a support to form a smooth surface, it has both sufficient reflection performance and surface resistance with sufficient radio wave transmission and sufficient visible light. It has been found that a heat ray shielding layer having a low permeability and a low haze can be obtained.
- the present invention relates to the following (1) to (21).
- a heat ray shielding layer containing fine particles having an average particle diameter of 100 nm or less and a resin binder that fills voids is formed on the support, and the heat ray shielding layer has a reflectance at a wavelength of at least 2000 nm.
- the heat ray shielding sheet which is 15% and whose surface resistance of the heat ray shielding layer is 10 6 ⁇ / ⁇ or more.
- the heat ray shielding sheet according to (1) wherein the maximum height difference on the surface of the heat ray shielding layer is 60 nm or less.
- the heat ray shielding layer further contains a near infrared absorbing dye, and the near infrared absorbing dye is dispersed in the resin binder.
- a dye layer containing a near infrared absorbing dye in addition to the heat ray shielding layer.
- M represents a metal atom, a metal oxide, a metal hydroxide, or a metal halide, or a hydrogen atom
- the broken line portions of rings A, B, C, and D are each independently the following:
- Formulas (2) to (8) Any one of the following structures, bonded to the skeleton structure at the opening to form an aromatic ring
- X is a lower alkyl group, a lower alkoxy group, an amino group, a nitro group, a halogen group, a hydroxy group, a carboxy group , Sulfonic acid group, or sulfonamido group
- Y is a divalent bridging group
- Z is a sulfonic acid group, a carboxy group, a residue obtained by removing at least one of hydrogen on the nitrogen atom of the primary or secondary amine.
- a group, an acid amide group, or a residue excluding at least one of hydrogen on a nitrogen atom of a heterocyclic ring containing a nitrogen atom, a and b represent the number of the respective groups, both of which are average values Each is independently 0 or more and 12 or less, and the sum of a and b is 0 or more and 12 or less]
- the porphyrazine dye of the formula (1) is represented by the following formula (9) [In the formula, the rings A, B, C and D are each independently represented by the following formula (4) or (8): Or an aromatic ring bonded to the skeleton structure at the opening.]
- the semiconductor device according to any one of (9) to (17), further including a reflective layer that has radio wave transparency and reflects light having at least one wavelength in a wavelength range of 780 to 2000 nm.
- Heat ray shielding sheet (19) The heat ray shielding sheet according to (18), wherein the reflective layer is at least one selected from the group consisting of at least one cholesteric liquid crystal layer, a dielectric multilayer film, and a birefringent multilayer film. (20) The heat ray shielding sheet according to (19), wherein the reflective layer is at least one cholesteric liquid crystal layer.
- the resin binder is a cured product of a heat or photocurable resin or a thermoplastic resin.
- the heat ray-shielding sheet of the present invention reflects the long-wavelength side of the near-infrared region (780 nm to 2500 nm), for example, light of 2000 nm or more at a certain ratio in addition to the good infrared absorption characteristics of the heat-shielding fine particles. It can prevent heat storage of the shielding layer, prevent thermal cracking of glass substrates, etc., has high surface resistance, good radio wave transmission, excellent visible light transmittance, low haze, and high transparency Have Therefore, the heat ray shielding sheet of the present invention can effectively greatly improve the heat ray shielding performance while preventing thermal cracking of the glass substrate or the like.
- 1 and 2 are model diagrams of the heat ray shielding sheet of the present invention.
- the heat ray shielding sheet of the present invention is a heat ray shielding sheet having a heat ray shielding layer on a support, and the heat ray shielding layer comprises fine particles having an average particle size of 100 nm or less (heat shielding fine particles) and void portions between the fine particles.
- the heat ray shielding layer has a light reflectance of at least 15%, and the surface resistance of the heat ray shielding layer is 10 6. It is characterized by being ⁇ / ⁇ or more.
- the above-mentioned fine particles, preferably transparent metal oxide fine particles (conductive fine particles) are high in concentration in a discontinuous and non-aggregated state in the binder component and the near-infrared reflection performance is not impaired.
- the surface of the heat ray shielding layer is 10 6 ⁇ / ⁇ or more, and the length of near infrared rays in the heat ray shielding layer is increased by dispersing the solution in a state and coating the dispersion liquid smoothly on the support.
- the reflectance of light on the wavelength side (2000 nm or more) can be made 15% or more.
- the surface resistance of the heat ray shielding layer is 10 6 ⁇ / ⁇ or more, radio waves can be transmitted, but it is preferably 10 7 ⁇ / ⁇ or more, more preferably 10 8 ⁇ / ⁇ or more, Preferably, it is 10 9 ⁇ / ⁇ or more, and most preferably 10 9.5 ⁇ / ⁇ or more.
- the upper limit of the surface resistance of the heat ray shielding layer is about 10 13 ⁇ / ⁇ , preferably about 10 12.5 ⁇ / ⁇ .
- the reflectance of the near-infrared long wavelength light (light having a wavelength of at least 2000 nm) in the heat ray shielding layer may be 15% or more, but the reflectance is preferably higher.
- the reflectance is preferably 20% or more, more preferably 25% or more, and further preferably 28% or more. In the most preferred embodiment of the present invention, 30% or more can be achieved.
- the range that can be actually achieved is up to about 37%, and the upper limit is usually up to about 35%.
- the value of the surface resistance is any one selected from the group consisting of the above preferable value, more preferable value, further preferable value, and most preferable value.
- the reflectance value is any one selected from the group consisting of the above preferable value, the more preferable value, and the most preferable value.
- the surface resistance value is 10 8 ⁇ / ⁇ or more, and the reflectance value is selected from the group consisting of 20% or more, 25% or more, and 28% or more.
- the surface resistance value is 10 9 ⁇ / ⁇ or more, and the reflectance value is 20% or more, 25% or more. And any one selected from the group consisting of 28% or more.
- the dispersion method of the fine particles is not particularly limited, but as one of the dispersion methods for achieving the above combination value, dispersion in a bead mill is possible. I can list.
- the dispersion in order to achieve the combination of the above surface resistance value and the above reflectance value, the dispersion is usually performed at a peripheral speed of 3 m / s or more.
- a preferable peripheral speed is 5 m / s or more, and more preferably 8 m / s or more. Even if the peripheral speed is too fast, the above combination cannot be achieved. Therefore, the speed is usually preferably about 12 m / s or less, and more preferably 11 m / s or less.
- the haze value in the heat ray shielding layer is usually 8% or less, preferably 5% or less, more preferably 2% or less, still more preferably 1% or less. And most preferably 0.8% or less.
- the heat ray shielding layer is more preferably a combination of the above surface resistance and the above reflectance, and more preferably a combination that achieves the above haze value, and a combination of the above surface resistance and the above reflectance.
- the aspect which combined the preferable haze value and the more preferable haze value is very preferable.
- the surface resistance of the heat ray shielding layer is 10 6 ⁇ / ⁇ or more, and the reflectance of light on the long-wavelength side (2000 nm or more) of the near infrared ray in the heat ray shielding layer is 15% or more. It is a combination whose haze value is any one selected from the group consisting of 8% or less, 5% or less, 3% or less, 2% or less, and 1% or less. Examples of other preferable combinations include a surface resistance of the heat ray shielding layer of 10 8 ⁇ / ⁇ or more, a reflectance of 15% or more, and a haze value of 3% or less, more preferably 1 % Or less.
- the surface resistance is 10 9 ⁇ / ⁇ or more, the reflectance is 15% or more, and the haze value is 1% or less, more preferably 0.8. % Or less.
- examples of other more preferable combinations include the above-mentioned surface resistance of 10 9 ⁇ / ⁇ or more, the reflectance of 15% or more, and the haze value of 1% or less, more preferably 0.8% or less. is there.
- the surface resistance is 10 9 ⁇ / ⁇ or more, the reflectance is 20% or more, more preferably 25% or more, and the haze value is 1% or less. More preferably, the combination is 0.8% or less.
- the visible light transmittance of the heat ray shielding layer is preferably 70% or more, more preferably 74% or more, and further preferably 80% or more.
- the surface resistance, the reflectance, the haze value, and the visible light transmittance of the heat ray shielding layer described above are all the same as that of the polyethylene terephthalate (PET) support ⁇ thickness, 100 ⁇ m, visible light transmittance 92. %, Haze value 0.3% ⁇ , and a thickness measured after drying or curing to be 500 nm. Therefore, this value includes the PET support. In the present invention, this value is referred to as the haze value and visible light transmittance value of the heat ray shielding layer for convenience. Therefore, when the heat ray shielding sheet of the present invention is composed of the heat ray shielding layer and the PET, the value of the heat ray shielding layer and the value of the heat ray shielding sheet are the same value.
- heat shielding fine particles having good absorption and / or scattering characteristics from the near infrared part to the far infrared part are suitable. Further, the heat shielding fine particles have good visible light permeability and no or little visible light absorption (for example, visible light absorption is 10% or less, preferably 5% or less, more preferably 1% or less. ) Is preferred.
- electrically conductive fine particles having a plasma wavelength in the near infrared region for example, conductive fine particles that shield the near infrared region (conductive heat shielding fine particles) are preferable, and as the conductive fine particles, Examples thereof include metal oxide fine particles.
- tin oxide indium oxide, zinc oxide, tungsten oxide, chromium oxide, molybdenum oxide, and the like.
- fine particles of metal oxide such as tin oxide, indium oxide, zinc oxide or tungsten oxide which do not absorb light in the visible light region are preferable, and indium oxide fine particles are particularly preferable.
- the third component in order to improve the electrical conductivity of these oxides.
- Sb, V, Nb, Ta, etc. are selected for tin oxide, Zn, Al, Sn, Sb, Ga, Ge, etc. are selected for indium oxide, and zinc oxide is used.
- Al, Ga, In, Sn, Sb, Nb, etc. are selected.
- Cs, Rb, K, Tl, In, Ca, Sr, Fe, Sn, Al, etc. are selected. .
- tin-containing indium oxide also referred to as ITO
- antimony-containing tin oxide ATO
- ITO tin-containing indium oxide
- the content of the dopant is not particularly limited, but is about 1 to 20% by weight, preferably about 5 to 15% by weight, based on the total amount of the metal doped.
- the tin content in ITO is the same.
- the fine particles used in the present invention are fine particles having an average particle size of 200 nm or less, usually 1 to 100 nm.
- the average particle diameter of the fine particles is preferably 10 to 50 nm, more preferably 10 to 40 nm, and most preferably about 10 to 30 nm.
- the average particle diameter is calculated from the specific surface area determined by the BET (Brunauer, Emmet and Teller's equation) method. If the average particle size becomes too large, the haze value becomes high and the visibility becomes poor when the heat ray shielding sheet is used.
- the fine particles usually have a powder resistance (measured by a powder resistance measurement system MCP-PD51, manufactured by Mitsubishi Chemical Analytech Co., Ltd.) of 100 ⁇ ⁇ cm or less, preferably 10 ⁇ ⁇ cm or less when compressed at 60 MPa. More preferably, it is 2 ⁇ ⁇ cm or less, and most preferably, 1 ⁇ ⁇ cm or less is used. Although there is no particular lower limit, it is usually 0.1 ⁇ ⁇ cm or more, and is preferably 0.4 ⁇ ⁇ cm or more from the viewpoint of ease of production.
- a powder resistance measured by a powder resistance measurement system MCP-PD51, manufactured by Mitsubishi Chemical Analytech Co., Ltd.
- the method for producing the fine particles is not particularly limited as long as the above can be obtained, and can be obtained by a known method such as a gas phase synthesis method or a liquid layer synthesis method.
- a gas phase synthesis method or a liquid layer synthesis method for indium oxide fine particles, the method disclosed in JP-A-6-227815 may be used. That is, it is a method of obtaining fine particles by neutralizing an aqueous solution of a salt containing a specific fine particle element with an alkali, filtering and washing the obtained precipitate, and heat-treating at a high temperature.
- methods for producing tin oxide fine particles and zinc oxide fine particles are disclosed in JP-A-2-105875 and JP-A-6-234522, respectively.
- the content of the fine particles in the heat ray shielding layer is usually 40% by weight or more, preferably 60% by weight or more, more preferably 70% by weight, still more preferably 75% by weight or more based on the total amount of the heat ray shielding layer. And most preferably 80% or more. In some cases, 82% by weight or more is more preferable. In particular, when it exceeds 80% by weight, light on the long-wavelength side of near-infrared light can be reflected at a higher rate, which is preferable.
- the upper limit of the fine particle content may be up to the upper limit at which a film can be formed with a binder, preferably about 95% by weight, more preferably about 92% by weight, and further preferably about 90% by weight.
- the total amount of the heat ray shielding layer is usually 40 to 95% by weight, preferably 60 to 95% by weight, more preferably 70 to 95% by weight, still more preferably, 75 to 92% by weight, most preferably more than 80% by weight and 92% by weight or less.
- the balance is a component (binder component) other than the fine particles. If the amount of the binder component is too small, it cannot be produced in a sheet shape, and the fine particles are connected to each other, so that radio wave transmission performance cannot be imparted. Further, when the binder component is increased, the concentration of the fine particles in the heat ray shielding layer is decreased, so that the surface resistance of the heat ray shielding layer can be increased.
- the binder component includes a resin binder, and may include various additives such as a dispersant, a near infrared absorbing dye, an ultraviolet absorber, an antioxidant, and a light stabilizer as necessary.
- the resin binder in the heat ray shielding layer is not particularly limited as long as it is a resin capable of dispersing and maintaining fine particles.
- a cured product of a thermoplastic resin or / and a curable resin that is cured by heat or light also referred to as a heat or photocurable resin
- a thermosetting resin or a photocurable resin specifically, a thermosetting resin or a photocurable resin
- the content of the resin binder in the heat ray shielding layer is 5 to 60% by weight, preferably 5 to 40% by weight, more preferably 5 to 30% by weight, still more preferably 5 to 25%, based on the total amount of the heat ray shielding layer. % By weight, most preferably 5% by weight or more and less than 20% by weight.
- the optional additive such as a dispersant is 0 to 80% by weight, preferably 0 to 70% by weight, more preferably 10 to 70% by weight, based on the total amount of the binder component.
- Thermoplastic resins include high density polyethylene resin, low density polyethylene resin, linear low density polyethylene resin, ultra low density polyethylene resin, polypropylene resin, polybutadiene resin, cyclic olefin resin, polymethylpentene resin, polystyrene resin, ethylene acetate Vinyl copolymer, ionomer resin, ethylene vinyl alcohol copolymer resin, ethylene ethyl acrylate copolymer, acrylonitrile / styrene resin, acrylonitrile / chlorinated polystyrene / styrene copolymer resin, acrylonitrile / acrylic rubber / styrene copolymer resin, acrylonitrile / butadiene ⁇ Styrene copolymer resin, acrylonitrile, EPDM, styrene copolymer resin, silicone rubber, acrylonitrile, styrene copolymer resin, cellulose, acetate,
- thermoplastic resins are preferably a (meth) acrylic resin from the viewpoint of transparency and the like, and for example, a (meth) acrylate polymer, particularly a (meth) acrylic copolymer is preferable.
- fever or light as a resin binder of a heat ray shielding layer is preferable, and the aspect containing the hardened
- the thermosetting resin is not particularly limited as long as it has a functional group curable by heating, and examples thereof include a curable compound having a cyclic ether such as an epoxy group or an oxetanyl group.
- the photocurable resin is not particularly limited as long as it is a compound having a functional group curable by light irradiation.
- examples thereof include resins having a curable compound having a saturated double bond.
- the thermosetting resin having the cyclic ether is not particularly limited, and examples thereof include epoxy resins (aliphatic epoxy resins including alicyclic epoxy resins or aromatic epoxy resins), oxetane resins, and furan resins. Of these, epoxy resins (aliphatic rings such as aliphatic rings having 3 to 12 carbon atoms, for example) and oxetane resins are preferable from the viewpoint of reaction rate and versatility.
- the epoxy resin is not particularly limited.
- a novolak type such as a phenol novolak type, a cresol novolak type, a biphenyl novolak type, a trisphenol novolak type, a dicyclopentadiene novolak type; a bisphenol A type, a bisphenol F type, 2, 2 Examples thereof include bisphenol types such as' -diallyl bisphenol A type, hydrogenated bisphenol type, and polyoxypropylene bisphenol A type. Other examples include glycidylamine.
- Examples of commercially available epoxy resins include, for example, phenol novolac type epoxy resins such as Epicron (registered trademark) N-740, N-770, N-775 (all of which are manufactured by Dainippon Ink and Chemicals, Inc.) Epicoat (registered trademark) 152, Epicoat (registered trademark) 154 (all of which are manufactured by Japan Epoxy Resin Co., Ltd.) and the like.
- phenol novolac type epoxy resins such as Epicron (registered trademark) N-740, N-770, N-775 (all of which are manufactured by Dainippon Ink and Chemicals, Inc.)
- Epicoat (registered trademark) 152, Epicoat (registered trademark) 154 all of which are manufactured by Japan Epoxy Resin Co., Ltd.) and the like.
- cresol novolak type examples include Epicron (registered trademark) N-660, N-665, N-670, N-673, N-680, N-695, N-665 EXP, N-672-EXP (and above)
- a biphenyl novolak type for example, NC-3000P (manufactured by Nippon Kayaku Co., Ltd.);
- a trisphenol novolak type for example, EP1032S50, EP1032H60 (all of which are Japan)
- dicyclopentadiene novolak type examples include XD-1000-L (manufactured by Nippon Kayaku Co., Ltd.), HP-7200 (manufactured by Dainippon Ink & Chemicals, Inc.); bisphenol A type epoxy compound
- Epicoat (registered trademark) 828, Epicoat ( Registered trademark) 834, Epicoat 1001, Epicoat (registered trademark) 1004 all of which are manufactured by Japan Epoxy Resin Co., Ltd.), Epicoat (register
- Examples of commercially available products of the oxetane compound include Etanacol (registered trademark) EHO, Etanacol (registered trademark) OXBP, Etanacol (registered trademark) OXTP, Etanacol (registered trademark) OXMA (all of which are manufactured by Ube Industries, Ltd.). Can be mentioned.
- the alicyclic epoxy compound is not particularly limited.
- Celoxide (registered trademark) 2021, Celoxide (registered trademark) 2080, Celoxide (registered trademark) 3000 all are manufactured by Daicel UCB Co., Ltd.) Etc.
- These curable compounds having a cyclic ether group may be used alone or in combination of two or more.
- the photocurable resin having an unsaturated double bond is not particularly limited.
- a resin having a vinyl group, a vinyl ether group, an allyl group, a maleimide group, a (meth) acryl group, or the like can be given.
- a resin having a (meth) acryl group for example, a (meth) acrylate compound is preferable from the viewpoint of reactivity and versatility.
- a term such as “(meth) acryl” means “acryl” or “methacryl”, and for example, “(meth) acrylate” means “acrylate” or “methacrylate”.
- Examples of the resin having a (meth) acryl group include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 1,4-butanediol mono (meth) acrylate, carbitol (meth) acrylate, and acryloyl.
- the glycidyl compound used for the epoxy (meth) acrylate which is a reaction product of the mono- or polyglycidyl compound and (meth) acrylic acid, is not particularly limited.
- bisphenol A, bisphenol F, bisphenol S, 4,4′- Biphenylphenol tetramethylbisphenol A, dimethylbisphenol A, tetramethylbisphenol F, dimethylbisphenol F, tetramethylbisphenol S, dimethylbisphenol S, tetramethyl-4,4'-biphenol, dimethyl-4,4'-biphenylphenol, 1- (4-hydroxyphenyl) -2- [4- (1,1-bis- (4-hydroxyphenyl) ethyl) phenyl] propane, 2,2′-methylene-bis (4-methyl-6-tert- Butylpheno ), 4,4′-butylidene-bis (3-methyl-6-tert-butylphenol), trishydroxyphenylmethane, resorcinol, hydroquino
- the epoxy (meth) acrylate which is a reaction product of these mono- or polyglycidyl compounds and (meth) acrylic acid, can be obtained by esterifying an equivalent amount of (meth) acrylic acid to the epoxy group.
- This synthesis reaction can be performed by a generally known method.
- the (meth) acrylated resorcin diglycidyl ether thus obtained is a resin having a radically polymerizable (meth) acryloyl group.
- the heat ray shielding layer comprises fine particles having an average particle diameter of 100 nm or less (specifically, heat ray shielding fine particles or metal oxide fine particles) and a resin binder forming component (the thermoplastic resin or / and the curable resin), as required.
- a fine particle dispersion containing a solvent can be further applied on a support and dried or cured as necessary.
- the fine particle dispersion may contain various additives such as a solvent, a photoreaction initiator, a thermosetting agent, a dispersant, a near infrared absorbing dye, an ultraviolet absorber, an antioxidant, and a light stabilizer. Can be added.
- the photoinitiator is not particularly limited as long as it is for polymerizing an unsaturated double bond or an epoxy group in the curable resin by light irradiation.
- a cationic polymerization type photoinitiator or a radical is used.
- a polymerization type photoinitiator is mentioned.
- the thermosetting agent is not particularly limited as long as it is for reacting and crosslinking the unsaturated double bond or epoxy group in the curable resin by heating.
- the amount of photoinitiator used is usually 1 to 20% by weight based on the photocurable resin.
- the resin binder contains a curable resin, preferably a photocurable resin, more preferably a (meth) acrylate compound, and the additive contains a photoreaction initiator, more preferably a radical polymerization photoinitiator. Embodiments are preferred.
- the solvent used for dispersing the fine particles is not particularly limited, but water or an organic solvent is preferable in the present invention. In addition, two or more of these solvents may be appropriately mixed and used as a mixture.
- the organic solvent include hydrocarbon solvents (toluene, xylene, hexane, cyclohexane, n-heptane, etc.), alcohol solvents (methanol, ethanol, isopropyl alcohol, butanol, t-butanol, benzyl alcohol, etc.), ketone solvents.
- ketone solvents such as toluene or methyl ethyl ketone, methyl isobutyl ketone, and acetylacetone.
- a dispersing agent may be used to uniformly disperse the fine particles.
- an embodiment including a dispersant is preferable.
- the addition amount of the dispersing agent can be appropriately changed within the range of 0 to 50% by weight with respect to the fine particles, and is usually 1 to 30% by weight, preferably about 1 to 20% by weight.
- the dispersant include a low molecular weight dispersant (dispersant having a molecular weight of less than 2000, preferably 1000 or less) and a polymer dispersant (weight average molecular weight of about 2,000 to 500,000, preferably about 2,000 to 200). 2,000, more preferably about 2,000 to 100,000).
- Low molecular dispersants include fatty acid salts (soap), ⁇ -sulfo fatty acid ester salts (MES), alkylbenzene sulfonates (ABS), linear alkylbenzene sulfonates (LAS), alkyl sulfates (AS), alkyl ethers.
- Low molecular weight anionic (anionic) compounds such as sulfate ester salt (AES) and alkyl sulfate triethanol, fatty acid ethanolamide, polyoxyethylene alkyl ether (AE), polyoxyethylene alkyl phenyl ether (APE), sorbitol, sorbitan, etc.
- Low-molecular nonionic compounds alkyltrimethylammonium salts, dialkyldimethylammonium chloride, alkylpyridinium chloride, and other low-molecular cationic (cationic) compounds, alkylcarboxyl betaines, sulfo Tines, may be mentioned low molecular amphoteric compounds such as lecithin.
- Polymeric dispersants include naphthalenesulfonate formalin condensate, polystyrene sulfonate, polyacrylate, copolymer salt of vinyl compound and carboxylic acid monomer, carboxymethylcellulose, polyvinyl alcohol, etc.
- a polymer dispersant having a molecular weight of 000 or more and 100,000 or less is a typical one. As long as it is suitably applied to the fine particles of the present invention, it is not limited to those exemplified above.
- a polymer dispersant is preferable, and a (meth) acrylate copolymer dispersant is more preferable among the polymer dispersants.
- Dispersants include the following. Floren DOPA-15B, Floren DOPA-17 (manufactured by Kyoeisha Chemical Co., Ltd.), Solplus AX5, Solplus TX5, Solsperse (registered trademark) (hereinafter the same) 9000, Solsperse 12000, Solsperse 17000, Solsperse 20000, Solsperse 21000, Solsperse 24000, Solsperse 26000, Solsperse 27000, Solsperse 28000, Solsperse 32000, Solsperse 35100, Solsperse 54000, Sol Six 250 (manufactured by Nihon Lubrizol Corporation), EFKA4008, EFKA4009, EFKA4010, EFKA4015, EFKA4046, EFKA4040, EFKA4040E, EFKA4040E 50, EFKA4055, EFKA4400, EFKA4401, EFKA4402, EFKA4403, EFKA4300, EFKA43
- an embodiment in which the heat ray shielding layer contains a near-infrared absorbing dye is one of the preferred embodiments.
- the heat ray absorbing ability can be improved.
- the content of the near infrared absorbing dye is not particularly limited, but is in the range of about 1 to 30% by weight, preferably 3 to 15%, based on the total amount of the heat ray shielding layer. It is in the range of wt%.
- the dye layer may be a dye alone, but it is usually preferable to disperse the dye in a resin binder to form a dye layer.
- a pigment layer such as a support is formed as a dispersion by adding a solvent, if necessary, in the range of 0.01 to 20 parts by weight with respect to 1 part by weight of the resin binder.
- the dye layer may be coated on the layer to be formed, and dried or / and cured as necessary to form a dye layer.
- the dye layer is preferably formed so as to come after the heat ray shielding layer from the incident light direction.
- a method of forming the dye layer on a support (or a reflection layer described later) and forming the heat ray shielding layer on the dye layer is preferable.
- dye layer can also be formed in the surface opposite to the said heat ray shielding layer of a support body.
- an embodiment in which a near-infrared absorbing dye is included together with the fine particles in the heat ray shielding layer is preferable.
- Near-infrared absorbing dye is a general term for dyes that absorb near-infrared (wavelength of about 780 to 2000 nm) in the visible region. Any known near-infrared absorbing dye can be used. Examples of the near infrared absorbing dye include azo dyes, aminium dyes, anthraquinone dyes, cyanine dyes, diimonium dyes, dithiol metal complex dyes, squarylium dyes, porphyrazine dyes, and the like. In order to increase durability, porphyrazine dyes and diimonium dyes are preferable. In the present invention, porphyrazine dyes that efficiently block heat rays are more preferable, and any porphyrazine dye can be used.
- porphyrazine dyes represented by the following formula (1) are preferable.
- M represents a metal atom, a metal oxide, a metal hydroxide, a metal halide, or a hydrogen atom
- the broken line portions of the rings A, B, C, and D each independently represent the following formula (2) to (8)
- X represents a lower alkyl group, a lower alkoxy group, an amino group, a nitro group, a halogen group, a hydroxy group, a carboxy group, a sulfonic acid group, or a sulfonamide group
- Y represents a divalent bridge.
- Z is a sulfonic acid group, a carboxy group, a residue excluding at least one hydrogen on the nitrogen atom of a primary or secondary amine, an acid amide group, or a nitrogen atom of a heterocyclic ring containing a nitrogen atom.
- the following formulas (2) to (8) are openings and are bonded to the skeleton structure to form aromatic rings of rings A, B, C and D.
- the aromatic ring formed is a pyridine ring, and the broken line part is the above formula (5) to (7).
- the aromatic ring formed when any one of the above is a pyrazine ring, and when the broken line is the above formula (8), the aromatic ring formed is a naphthalene ring.
- the residue excluding at least one hydrogen on the nitrogen atom of the primary or secondary amine in Z include a mono-lower alkylamino group and a di-lower alkylamino group.
- the phthalamide group etc. which may have a substituent can be mentioned.
- the residue excluding at least one hydrogen on the nitrogen atom of the heterocyclic ring containing a nitrogen atom includes a pyridino group that may have a substituent, a piperazino group that may have a substituent, or a substituent. Examples thereof may include a piperidino group.
- examples of the aromatic ring in the rings A to D include a nitrogen-containing heteroaromatic containing one or two nitrogen atoms such as a benzene ring, a naphthalene ring, a pyridine ring, a pyrazine ring, and a pyridazine ring.
- a ring is mentioned.
- any one or a combination of two selected from the group consisting of a benzene ring, a pyridine ring and a naphthalene ring is preferable, and all may be the same aromatic ring.
- rings A to D it is preferable to contain, on average, 1 to 4, preferably 2 to 4, pyridine rings or naphthalene rings.
- the rest is a benzene ring.
- More preferred is a combination of 0 to 2 benzene rings, 0 to 3 pyridine rings and 1 to 4 naphthalene rings, and a total of 4.
- More preferable combinations include 0 to 2 benzene rings, 2 to 4 naphthalene rings, and a total of 4 or 1 to 3 pyridine rings and 1 to 3 naphthalene rings. In this combination, the sum of the two is 4.
- rings A to D are a combination of a pyridine ring and a naphthalene ring is one of the more preferred embodiments.
- the pyridine ring formed from the structure of said Formula (4) is preferable.
- M represents a hydrogen atom, a metal atom, a metal oxide, a metal hydroxide, or a metal halide.
- M is other than a hydrogen atom, the M means that the porphyrin ring in the formula (1) has a so-called central metal.
- M is a hydrogen atom, it means that the porphyrin ring has no central metal.
- metal atom in M include, for example, Li, Na, K, Mg, Ti, Zr, V, Nb, Ta, Cr, Mo, W, Mn, Fe, Co, Ni, Ru, Rh, Pd,
- Examples include Os, Ir, Pt, Cu, Ag, Au, Zn, Cd, Hg, Al, Ga, In, Si, Ge, Sn, Pb, Sb, or Bi.
- Examples of the metal oxide include VO and GeO.
- Examples of the metal hydroxide include Si (OH) 2 , Cr (OH) 2 , Sn (OH) 2, and AlOH.
- As the metal halide for example, SiCl 2, VCl, VCl 2 , VOCl, FeCl, GaCl, ZrCl or AlCl, and the like.
- metal atoms such as Fe, Co, Cu, Ni, Zn, Al or V
- metal oxides such as VO
- metal hydroxides such as AlOH, and the like are preferable. More preferred is Cu or VO, and VO is most preferred.
- X in the formula (1) represents a lower alkyl group, a lower alkoxy group, an amino group, a nitro group, a halogen group, a hydroxy group, a carboxy group, a sulfonic acid group or a sulfonamide group.
- “lower” means 1 to 4 carbon atoms.
- Y is preferably an alkylene group having 1 to 3 carbon atoms or —SO 2 NH—, and more preferably an alkylene group having 1 to 3 carbon atoms.
- Z include a carboxy group, a sulfonic acid group, a phthalimide group which may have a substituent, a piperazino group which may have a substituent, and a piperidino group which may have a substituent. it can.
- Z is a carboxy group, a sulfonic acid group, or a phthalimide group which may have a substituent, and a phthalimide group which may have a substituent is more preferable.
- Z when Z is a phthalimide group which may have a substituent, a piperazino group which may have a substituent, or a piperidino group which may have a substituent, the substituent may be a lower alkyl group or a lower alkoxy group.
- Z is a group which may have the above substituent, an unsubstituted or halogeno-substituted group is preferable. More preferred Z is an unsubstituted or halogeno-substituted phthalimide group, and unsubstituted phthalimide is most preferred.
- the substituted amino group is not particularly limited, and examples thereof include an amino group substituted with a lower alkyl group or a lower alkoxy group.
- “lower” means 1 to 4 carbon atoms, and the halogen atom is preferably Cl, Br or I.
- a and b in the formula (1) are each 0 or more and 12 or less, and the sum of a and b is 0 or more and 12 or less.
- a and b are each independently 0 or more and 4 or less, and the sum of a and b is 0 or more and 4 or less.
- a porphyrazine dye in which a and b are both 0 in the formula (1) is preferable.
- porphyrazine coloring matter represented by the formula (1) are shown in Table 2-1 below as Compound Nos. Shown with.
- the following examples show representative dyes for specifically explaining the dyes of the present invention, and the present invention is not limited to the following examples.
- the nitrogen-containing heteroaromatic rings of rings A to D are represented by the above formulas (3), (4) and (6), there are positional isomers of nitrogen atoms, and a mixture of isomers during dye synthesis. As obtained. Isolation of these isomers is difficult, and it is difficult to identify isomers by analysis. For this reason, it is usually used as a mixture.
- the coloring matter of the present invention includes such a mixture.
- the porphyrazine coloring matter represented by the formula (1) is generally a known compound, or can be easily synthesized according to a known compound.
- the porphyrazine coloring matter represented by the formula (1) can be synthesized according to known methods disclosed in, for example, International Publication No. 2010/143619 and International Publication No. 2010/013455.
- the compound represented by the formula (1) obtained by the above method is a positional isomer related to the substitution position of the nitrogen-containing heteroaromatic ring in rings A to D and the substitution position of the nitrogen atom of the nitrogen-containing heteroaromatic ring. It is also as described in the said well-known literature that it becomes a mixture. No. 1 in Table 1 above. 3 or No.
- the compound represented by 18 can also be synthesized according to known methods disclosed in, for example, the pamphlet of Japanese Patent No. 2507786 and the pamphlet of Japanese Patent No. 3813750.
- the preferable aspect of the dispersion liquid for heat ray shielding layers of this invention is shown below.
- % in a content or a composition ratio etc. is weight% unless there is particular notice.
- ii The dispersion according to i above, wherein the powder resistance when the metal oxide fine particles are compressed at 60 MPa is 10 ⁇ ⁇ cm.
- viii The dispersion according to any one of the above i to vii, which contains a photocurable resin as a resin binder and a photoreaction initiator as an additive.
- ix The dispersion according to the above viii, wherein the addition amount of the photoinitiator is 1 to 20% with respect to the photocurable resin.
- x The dispersion liquid according to viii above, wherein the photocurable resin is a (meth) acrylate compound.
- xi The dispersion according to any one of viii to x above, wherein the photoreaction initiator is a radical polymerization type photoinitiator.
- xii The dispersion according to any one of the above i to xi containing a near-infrared absorbing dye as an additive.
- xiii The dispersion described in xii above, wherein the addition amount of the near-infrared absorbing dye is 1 to 30% with respect to the total solid content of the dispersion.
- xiv The dispersion according to xiii above, wherein the near-infrared absorbing dye is a porphyrazine dye or a dimonium dye.
- xv The dispersion according to xiv above, wherein the near-infrared absorbing dye is a porphyrazine dye represented by the formula (1).
- Rings A, B, C, and D in the porphyrazine dye represented by the formula (1) are at least one is a pyridine ring or a naphthalene ring, and the remaining rings are each independently a benzene ring, a pyridine ring, and a naphthalene ring.
- the combination of four rings A, B, C and D is a total of 0 to 2 benzene rings and 2 to 4 naphthalene rings.
- the dispersion according to xvi above which is a combination in which is 4 or a combination in which the number of pyridine rings is 1 to 3 and the number of naphthalene rings is 1 to 3 and the total of both is 4.
- xviii The dispersion according to the above xvii, wherein the rings A to D are a combination of a pyridine ring and a naphthalene ring.
- xix The dispersion according to any one of the above xv to xviii, wherein the near-infrared absorbing dye is a porphyrazine dye in which a and b in Formula (1) are 0. xx.
- the reflectance of the heat ray shielding layer with light having a wavelength of at least 2000 nm is at least 15%
- the surface resistance of the heat ray shielding layer is The dispersion liquid according to any one of i to xix, wherein the dispersion liquid is dispersed so as to be 10 6 ⁇ / ⁇ or more.
- xxi The dispersion according to any one of the above i to xx, which is dispersed at a peripheral speed of 6 m / s to 12 m / s by a bead mill.
- the heat ray shielding sheet of this invention which has the heat ray shielding layer of the preferable aspect of this invention on a support body can be obtained.
- the surface resistance of the heat ray shielding layer in the heat ray shielding sheet is 10 6 ⁇ / ⁇ or more, preferably 10 7 ⁇ / ⁇ or more, more preferably 10 8 ⁇ / ⁇ or more, and further preferably 10 9 ⁇ / ⁇ or more. If the surface resistance is too low, it is difficult to transmit radio waves. Further, the reflectance of the heat ray shielding layer with light having a wavelength of at least 2000 nm is at least 15%, preferably at least 20%. If the reflectance of light having a wavelength of 2000 nm or more is too small, not only will the contribution of heat ray shielding by reflection be small, but also absorption performance will be the main factor, leading to problems such as an increase in sheet surface temperature.
- the maximum height difference on the surface of the heat ray shielding layer is 70 nm or less, preferably 60 nm or less, more preferably 50 nm or less. In a more preferred embodiment, the maximum height difference is 40 nm or less, more preferably 30 nm or less, or 20 nm or less. Most preferably, it is 15 nm or less. If the maximum height difference is too large, scattering of incident near-infrared light occurs on the film surface, and good reflection performance cannot be imparted. Although there is no lower limit in particular, the lower limit that can be generally achieved is about 5 nm, and it is about 10 nm in terms of ease of achievement.
- the maximum difference in height of the surface of the heat ray shielding layer is determined by using a white light interference type surface observation device (Taylsurf CCI manufactured by Taylor Hobson) with a 50 magnification lens, and 0. The maximum height and the maximum height were measured in the range of 3 mm ⁇ 0.3 mm, and the difference between the maximum height and the maximum height was defined as the maximum height difference on the surface of the heat ray shielding layer.
- a white light interference type surface observation device Tiylsurf CCI manufactured by Taylor Hobson
- the fine particles are The dispersion is dispersed in a binder component so as to be contained at a high concentration, so that the fine particles at a high concentration are in a non-aggregated and non-continuous state and do not hinder the reflection performance of the fine particles. It was discovered that the film may be formed by, for example, coating the surface smoothly on the support.
- the reflectance of light having a wavelength of at least 2000 nm in the heat ray shielding layer can be at least 15%, preferably at least 20%, and the surface resistance of the heat ray shielding layer is at least 10. 6 ⁇ / ⁇ , preferably at least 10 7 ⁇ / ⁇ , more preferably at least 10 8 ⁇ / ⁇ , and even more preferably at least 10 9. ⁇ / ⁇ .
- the dispersion method is not particularly limited as long as it can be dispersed in a state where the above values can be achieved, but a preferable dispersion method includes a method of dispersing in a specific dispersion energy region with a bead mill.
- a preferable dispersion method includes a method of dispersing in a specific dispersion energy region with a bead mill.
- the specific energy region is 3 to 12 m / s, preferably 3 to 11 m / s, more preferably 3 to 10 m / s.
- Further preferred embodiments include a peripheral speed of 4 to 12 m / s or a peripheral speed of 4 to 11 m / s, and a most preferred embodiment is a peripheral speed of 5 to 12 m / s, or in some cases, 5 A peripheral speed of ⁇ 11 m / s or 5-10 m can be mentioned.
- the peripheral speed is too slow, the fine particles cannot be sufficiently dispersed, and if the peripheral speed is too fast, the reflection performance deteriorates and the heat shielding performance deteriorates.
- the appropriate range varies slightly depending on the apparatus used, the binder, the solid content at the time of dispersion, and the like, and it is preferable to adjust appropriately with reference to the above.
- the method for applying the heat ray shielding layer is not particularly limited as long as the surface can be applied smoothly.
- a comma coater, spray coater, roll coater, knife coater or the like can be used, but for sheet smoothness, a coating suitable for thin film production such as a bar coater, spin coater, die coater, and micro gravure coater is preferable.
- the use of a device is preferred.
- the thickness of the heat ray shielding layer containing the fine particles varies depending on the fine particle concentration, the binder component, and the like.
- the visible light transmittance of the heat ray shielding layer is preferably at least 70% or more, and more preferably adjusted to a thickness of 80% or more.
- the adjustment may be made between about 0.1 ⁇ m and 50 ⁇ m. More preferably, it is about 0.1 ⁇ m to 40 ⁇ m.
- a curable resin is used as the resin binder, it can be adjusted in the range of usually 0.1 ⁇ m to 30 ⁇ m, preferably about 0.1 ⁇ m to 20 ⁇ m, more preferably 0.1 ⁇ m to 10 ⁇ m.
- the visible light transmittance in the heat ray shielding layer obtained as described above is usually 50% or more, preferably 70% or more, more preferably 80% or more.
- the haze value in the heat ray shielding layer is usually 8% or less, preferably 5% or less, more preferably 3% or less, still more preferably 2% or less, and most preferably 1% or less.
- the haze value is preferably low. In a preferred embodiment of the present invention, the haze value is 0.8% or less, and in a more preferred embodiment, the haze value can be up to 0.5% or less. There is no particular lower limit to the haze value, but it seems to be about 0.1%.
- the support in the heat ray shielding sheet of the present invention is not a problem as long as it is a transparent thin plate that can form a heat ray shielding layer, and may be either an inorganic material or an organic material.
- seat which has the function etc. which reflect near infrared rays may be sufficient.
- a transparent thin plate-like body that does not impair light transmittance such as a resin sheet or an inorganic glass plate, is used.
- a thin plate having a visible light transmittance of at least 90% is preferred.
- the thickness is not particularly limited, but is usually about 50 ⁇ m to 3 mm.
- the heat ray shielding sheet of this invention may have another layer, for example, a near-infrared absorption layer and a near-infrared reflective layer, as needed.
- a near-infrared absorption layer and a near-infrared reflective layer may be another layer, for example, a near-infrared absorption layer and a near-infrared reflective layer, as needed.
- various additives such as a ultraviolet absorber, antioxidant, a light stabilizer, can be added to this another layer as needed.
- functional sheets such as an adhesive layer and a hard coat layer may be laminated on the heat ray shielding layer according to the purpose.
- the near-infrared absorbing dye may be included in the heat ray shielding layer for blocking near-infrared light on the short wavelength side (near infrared light close to visible light; mainly light having a wavelength of 780 nm to 2000 nm).
- the near-infrared absorbing dye is not included, or if the near-infrared absorbing dye is included and the light on the short wavelength side is to be shielded, the near-infrared ray is separated from the heat ray shielding layer.
- a reflective layer that mainly reflects light on the short wavelength side. Below, the heat ray shielding sheet of this invention which has this reflection layer is demonstrated.
- the reflection layer a known reflection layer can be used.
- the reflective layer include a cholesteric liquid crystal layer, a dielectric multilayer film having at least one combination of both a high refractive index layer and a low refractive index layer, and a birefringent multilayer film.
- the infrared selective reflection material to be used a known material can be used, and a material that transmits radio waves, that is, a material that is not conductive is preferable.
- cholesteric (chiral nematic) liquid crystal material cholesteric (chiral nematic) liquid crystal material
- dielectric multilayer film material hereinafter also referred to as dielectric multilayer structure material
- birefringence multilayer film material also referred to as birefringence multilayer structure material
- a dielectric multilayer structure material (also referred to as a dielectric multilayer film material) is formed by alternately stacking a high refractive index material layer (hereinafter also referred to as a high refractive index layer) and a low refractive index material layer (hereinafter also referred to as a low refractive index layer). Configured.
- the refractive index of the high refractive index layer is preferably about 1.60 to 2.40, more preferably about 1.80 to 2.10.
- the refractive index of the low refractive index layer is about 1.30 to 1.50, preferably about 1.34 to 1.50, both of which are at least 0.1, preferably at least 0.3, more preferably Preferably it has a refractive index difference of at least 0.4.
- Each optical thickness (the product nd of the refractive index n and the thickness d) is controlled so as When c the center wavelength of the wavelength range to be reflected lambda, the lambda c / 4. Titanium oxide, zirconium oxide, cerium oxide, lead oxide, zinc oxide, niobium oxide, tantalum oxide, hafnium oxide, etc. are used as high refractive index materials, and silicon oxide, magnesium fluoride, fluoride are used as low refractive index materials. Cerium or the like is used.
- the high refractive index material layer and the low refractive index material layer can be produced by a known method such as sputtering, vapor deposition, spraying, etc. (for example, Japanese Patent No. 3397824). Also, a method in which fine particles of each refractive index material layer are dispersed in a matrix and applied may be used. In that case, the particle diameter is preferably 200 nm or less in consideration of visible transmittance and haze value.
- the heat ray shielding sheet of the present invention having a dielectric multilayer film does not contain a near-infrared absorbing dye, and the visible light transmittance is 70% or more, preferably 75% or more.
- the dielectric multilayer film is formed by alternately laminating materials in which the refractive index difference between the high refractive index layer and the low refractive index layer is at least 0.3, more preferably at least 0.4.
- the high refractive index layer contains titanium oxide and the low refractive index layer contains silicon oxide, and 3 to 11 This is a case where the dielectric multilayer films are alternately laminated so as to achieve the above target value between the layers.
- the cholesteric liquid crystal material has molecular axes aligned in a certain direction on one plane, but the direction of the molecular axis is slightly shifted in the next plane, and the angle is shifted in the next plane. It is a structure in which the angle of the molecular axis shifts one after another in the normal direction of the plane. Such a structure in which the direction of the molecular axis is twisted is called a chiral structure.
- the normal line (chiral axis) of the plane is preferably substantially parallel to the thickness direction of the cholesteric liquid crystal layer.
- the center wavelength of the wavelength region to be reflected depends on the pitch length of the chiral structure in the cholesteric liquid crystal material.
- the central wavelength to be reflected can be changed by changing the pitch length of the chiral structure.
- the number of layers of the cholesteric liquid crystal material may be one or two or more. It is preferable that the number of layers is two or more because the wavelength band of near infrared rays that can be reflected can be widened.
- cholesteric liquid crystal layers having different molecular axis twist directions in order to more efficiently reflect the central wavelength region to be reflected. That is, both right circularly polarized light and left circularly polarized light can be reflected, and an effective reflectance can be realized.
- an appropriate combination can be used in view of manufacturing cost, visible light transmittance, and the like.
- a curable liquid crystal composition also referred to as a polymerizable liquid crystal composition
- An example of the liquid crystal composition contains at least a polymerizable liquid crystal compound (preferably a polymerizable rod-shaped liquid crystal compound), an optically active compound (chiral compound), and a polymerization initiator. Two or more of each component may be included.
- a polymerizable liquid crystal compound and a non-polymerizable liquid crystal compound can be used in combination. Also, a combination of a low-molecular liquid crystal compound and a high-molecular liquid crystal compound is possible.
- the liquid crystal composition contains at least one selected from various additives such as horizontal alignment, unevenness inhibitor, repellency inhibitor, and polymerizable monomer. Also good. Further, in the liquid crystal composition, a polymerization inhibitor, an antioxidant, an ultraviolet absorber, a light stabilizer, a colorant, metal oxide fine particles, and the like are further added as necessary so as not to deteriorate the optical performance. can do.
- Rod-like liquid crystal compound used in the present invention is a rod-like nematic liquid crystal compound.
- the rod-like nematic liquid crystal compound include azomethines, azoxys, cyanobiphenyls, cyanophenyl esters, benzoic acid esters, cyclohexanecarboxylic acid phenyl esters, cyanophenylcyclohexanes, cyano-substituted phenylpyrimidines, phenyldioxane.
- Low molecular liquid crystal compounds and high molecular liquid crystal compounds such as benzene, tolanes and alkenylcyclohexylbenzonitriles are preferably used.
- the rod-like liquid crystal compound used in the present invention may be polymerizable or non-polymerizable.
- a polymerizable rod-like liquid crystal compound is preferable.
- the rod-like liquid crystal compound having no polymerizable group is described in various documents (for example, Y. Goto et.al., Mol. Cryst. Liq. Cryst. 1995, Vol. 260, pp. 23-28). .
- the polymerizable rod-like liquid crystal compound can be obtained by introducing a polymerizable group into the rod-like liquid crystal compound.
- Examples of the polymerizable group include an unsaturated polymerizable group, an epoxy group, and an aziridinyl group, preferably an unsaturated polymerizable group, and particularly preferably an ethylenically unsaturated polymerizable group.
- the polymerizable group can be introduced into the molecule of the rod-like liquid crystal compound by various methods.
- the number of polymerizable groups possessed by the polymerizable rod-like liquid crystal compound is preferably 1 to 6, more preferably 1 to 3. Examples of the polymerizable rod-like liquid crystal compound are described in Makromol. Chem. 190, 2255 (1989), Advanced Materials 5, 107 (1993), US Pat. No. 4,683,327, US Pat. No. 5,622,648, US Pat. No.
- the liquid crystal composition exhibits a cholesteric liquid crystal phase, and for that purpose, it preferably contains an optically active compound.
- the rod-like liquid crystal compound is a molecule having an asymmetric carbon atom
- the cholesteric liquid crystal phase may be stably formed without adding an optically active compound.
- the optically active compound includes various known chiral agents (for example, Liquid Crystal Device Handbook, Chapter 3-4-3, TN, chiral agent for STN, 199 pages, edited by Japan Society for the Promotion of Science, 142nd Committee, 1989). ) Can be selected.
- the optically active compound generally contains an asymmetric carbon atom, but an axially asymmetric compound or a planar asymmetric compound that does not contain an asymmetric carbon atom can also be used as a chiral agent.
- the axial asymmetric compound or the planar asymmetric compound include binaphthyl, helicene, paracyclophane, and derivatives thereof.
- the optically active compound (chiral agent) may have a polymerizable group.
- the optically active compound has a polymerizable group and the rod-shaped liquid crystal compound used in combination also has a polymerizable group
- the repetition is induced from the rod-shaped liquid crystal compound by a polymerization reaction between the polymerizable optically active compound and the polymerizable rod-shaped liquid crystal compound.
- Polymers having units and repeating units derived from optically active compounds can be formed.
- the polymerizable group possessed by the polymerizable optically active compound is preferably the same group as the polymerizable group possessed by the polymerizable rod-like liquid crystal compound.
- the polymerizable group of the optically active compound is also preferably an unsaturated polymerizable group, an epoxy group or an aziridinyl group, more preferably an unsaturated polymerizable group, and an ethylenically unsaturated polymerizable group. Is particularly preferred.
- the optically active compound may be a liquid crystal compound.
- the optically active compound in the liquid crystal composition is preferably 0.1 to 30 mol% with respect to the liquid crystal compound used in combination. A smaller amount of the optically active compound is preferred because it often does not affect the liquid crystallinity. Therefore, the optically active compound used as the chiral agent is preferably a compound having a strong twisting power so that a twisted orientation with a desired helical pitch can be achieved even with a small amount. Examples of such a chiral agent exhibiting a strong twisting force include the chiral agents described in JP-A No. 2003-287623, which can be preferably used in the present invention.
- the liquid crystal composition used for forming the light reflecting layer is preferably a polymerizable liquid crystal composition, and for that purpose, it preferably contains a polymerization initiator.
- the polymerization initiator to be used is preferably a photopolymerization initiator capable of starting the polymerization reaction by irradiation with ultraviolet rays.
- the photopolymerization initiator is not particularly limited.
- Keracure RTX isopropylthioxanthone, 2,4-dichlorothioxanthone (Nippon Kayaku Co., Ltd. “Kayacure CTX”), 2,4-diethylthioxanthone (Nippon Kasei) And thioxanthone compounds such as “Kayacure DETX” manufactured by Yakuhin Co., Ltd.) and 2,4-diisopropylthioxanthone (“Kayacure DITX” manufactured by Nippon Kayaku Co., Ltd.). These photoinitiators may be used independently and 2 or more types may be used together.
- the content of the photopolymerization initiator in the composition is not particularly limited, but the preferred lower limit is preferably 0.5 parts by weight, preferably 100 parts by weight of the polymerizable liquid crystal compound or the (meth) acrylate monomer composition.
- the upper limit is 10 parts by weight or less, the more preferable lower limit is 2 parts by weight, and the more preferable upper limit is 8 parts by weight.
- reaction aid is not particularly limited, and for example, triethanolamine, methyldiethanolamine, triisopropanolamine, n-butylamine, N-methyldiethanolamine, diethylaminoethyl methacrylate, Michler's ketone, 4,4′-diethylaminophenone, 4- Examples include amine compounds such as ethyl dimethylaminobenzoate, ethyl 4-dimethylaminobenzoate (n-butoxy), and isoamyl 4-dimethylaminobenzoate.
- the content of the reaction aid in the polymerizable liquid crystal composition is not particularly limited, but is preferably used in a range that does not affect the liquid crystal properties of the polymerizable liquid crystal composition.
- a preferred lower limit is 0.5 parts by weight
- a preferred upper limit is 10 parts by weight or less
- a more preferred lower limit is 2 parts by weight
- a more preferred upper limit is 8 parts by weight with respect to a total of 100 parts by weight of the curable polymerizable compound. is there.
- the content of the reaction aid is preferably 0.5 to 2 times the content of the photopolymerization initiator.
- the method for applying the cholesteric liquid crystal layer is not particularly limited, and examples include a comma coater, a spray coater, a roll coater, a knife coater, and the like. It is preferable to use a coating apparatus suitable for thin film production such as a die coater or a micro gravure coater. Further, in order to more precisely define the alignment direction of the liquid crystal compound in the cholesteric liquid crystal layer, the surface of the layer (fine particle layer, substrate, etc.) to which the cholesteric liquid crystal layer is applied may be aligned. In order to align, it is preferable to form an alignment surface by rubbing the surface of the substrate.
- the cholesteric liquid crystal layer may have at least one layer, but it is usually preferable to have a plurality of cholesteric liquid crystal layers, usually at least two layers, preferably about 2 to 8 layers.
- the combination of the plurality of cholesteric liquid crystal layers may be any combination of at least two kinds of cholesteric liquid crystal layers having different molecular axis twist directions, and / or a combination of cholesteric liquid crystal layers having different pitch lengths.
- a preferred embodiment of the heat ray shielding sheet of the present invention having a cholesteric liquid crystal layer has at least one cholesteric liquid crystal layer on the support, preferably at least two layers, more preferably 2 to 8 layers. And the heat ray shielding layer.
- the cholesteric liquid crystal layer contains a polymerizable liquid crystal composition (preferably a photopolymerizable liquid crystal composition, more preferably a photopolymerizable liquid crystal composition containing a photopolymerizable rod-like liquid crystal compound, or further a chiral agent.
- the photopolymerizable liquid crystal composition is a polymer layer.
- the heat ray shielding layer may be either an embodiment that does not contain a near-infrared absorbing dye or an embodiment that contains it.
- the visible light transmittance is 70% or more, preferably 75% or more, and the haze value is 2% or less, preferably 1.5% or less, and more.
- the total solar energy transmittance described later is preferably 1% or less, and 65% or less, more preferably 60% or less.
- the visible light transmittance is the above preferable or more preferable value, and the total solar energy transmittance is 60%. In the following, it is preferably 55% or less, and in the most preferred embodiment, it can be 50% or less.
- the near-infrared absorbing dye the preferred porphyrazine dyes listed above are preferable, and the preferred or more preferable porphyrazine dyes listed above are more preferable.
- a birefringent multilayer structure material includes alternating layers having birefringence (preferably positive birefringence) (hereinafter referred to as birefringent layers) and layers having isotropic refraction or negative birefringence (hereinafter referred to as isotropic refractive layers). And is based on the coherent interference caused by the refractive index difference between the birefringent layer and the isotropic refractive layer and the respective film thicknesses. When the in-plane refractive index is different between the birefringent layer and the isotropic refractive layer, the interface between the two layers forms a reflective surface.
- birefringence preferably positive birefringence
- isotropic refractive layers layers having isotropic refraction or negative birefringence
- Birefringence means that the refractive indices in the orthogonal x, y and z directions are not all the same.
- the x-axis and y-axis are in the plane of the layer, the z-axis is perpendicular to the plane of the layer, and for oriented polymers, the x-axis is chosen to be the in-plane direction with the highest refractive index, The direction corresponds to one of the directions in which the optical body is oriented (eg, stretched).
- the in-plane refractive indexes of both the birefringent layer and the isotropic refractive layer are different between the layers (ie, n 1x ⁇ n 2x , n 1y ⁇ n 2y , where n 1x and n 1y are the in-plane refractive indices of the birefringent layer And n 2x and n 2y are the in-plane refractive indices of the isotropic refractive layer).
- the z-axis refractive indexes of the birefringent layer and the isotropic refractive layer are equal, since the reflection of p-polarized light does not depend on the incident angle of light, and the reflectance becomes uniform over the range of viewing angles.
- a birefringent polymer (preferably a polymer having positive birefringence) that is uniaxially or preferably biaxially oriented is used, and isotropically refraction with the birefringent layer. Increase the refractive index difference of the layer.
- the optical film thickness of each layer is controlled to be ⁇ c / 4 where ⁇ c is the center wavelength of the wavelength region to be reflected.
- a material that is oriented by stretching positive birefringence
- PEN polyethylene naphthalate
- PET PET
- isotropic refractive material a material that is not oriented by stretching (or a material that is negatively birefringent by stretching) is used.
- PMMA polymethyl methacrylate
- the birefringent multilayer structure material can be produced by forming a multilayer film and stretching it by, for example, a co-extrusion method described in JP-T-2008-528313. Since the refractive index difference between the birefringent layer and the isotropic refractive layer is small, a large number of layers need to be laminated.
- the number of stacked layers is preferably 3 or more and 1000 or less in view of the reflection region to be reflected, the manufacturing cost, and the like.
- the order of stacking the reflective layer and the heat ray shielding layer is not particularly limited.
- the heat ray shielding layer may be laminated between the support and the reflective layer.
- the reflective layer may be used as the support.
- the reflective layer a dielectric multilayer film or a cholesteric liquid crystal layer is more preferable.
- the visible light transmittance of the heat ray shielding sheet of the present invention having both the heat ray shielding layer and the reflective layer is 50% or more, preferably 70% or more. Further, the haze value of the heat ray shielding sheet needs to be such that transparency is not impaired, and should be 8% or less, preferably 3% or less, more preferably 1% or less.
- the total solar energy transmittance (Tts) in the heat ray shielding sheet of the present invention having both the heat ray shielding layer and the reflective layer is preferably about 70% or less, more preferably 60% or less, Preferably, it is 55% or less, and in the most preferred embodiment, it is 50% or less.
- various additives such as an ultraviolet absorber, an antioxidant, and a light stabilizer can be added to the heat ray shielding layer or the reflective layer as necessary.
- other layers such as an ultraviolet absorbing layer containing an ultraviolet absorber and a dye layer containing a near infrared pigment may be included as necessary.
- an embodiment composed of both the heat ray shielding layer and the reflective layer is preferable.
- functional sheets such as an adhesive layer and a hard coat layer may be laminated on the heat ray shielding sheet to form a heat ray shielding laminated sheet.
- the heat ray shielding sheet of the present invention may be a heat ray shielding laminated sheet obtained by further laminating a dye layer containing a near infrared absorbing dye, if necessary, in addition to the heat ray shielding layer.
- a dye layer containing a near infrared absorbing dye the aforementioned porphyrazine-based compounds and diimonium-based compounds are preferable.
- a fine particle layer, a layer combining infrared selective reflection materials, and a near infrared absorbing dye may be appropriately combined.
- Infrared selective reflection materials are commercially available as long as they meet the above performance (heat shielding, radio wave transmission, haze, visible transmittance, etc.). You may use what you have.
- part means “part by weight”
- % means “% by weight”.
- Example 1 Tin-containing indium oxide having an average particle size of 25.6 nm and powder resistance of 0.8 ⁇ ⁇ cm (trade name: ITO-R, manufactured by CIK Nanotech Co., Ltd.) (hereinafter referred to as ITO), 1.4 parts, KAYARAD DPHA (Trade name, dipentaerythritol hexaacrylate, manufactured by Nippon Kayaku Co., Ltd.) 0.1 part, Irgacure 184 (radical photopolymerization initiator, manufactured by BASF Japan Ltd.) 0.01 part, aminoalkyl methacrylate copolymer dispersion 0.1 parts of an agent (trade name, Disper BYK140, manufactured by Big Chemie Japan Co., Ltd.) was added to 7 parts of toluene, and dispersed at a peripheral speed of 10 m / s using a bead mill to prepare a dispersion.
- ITO Tin-containing indium oxide having an average particle size of 25.6 nm and powder
- the prepared dispersion was applied to a polyethylene terephthalate (PET) sheet (base material) (thickness 100 ⁇ m) with a wire bar so that the thickness after drying would be 500 nm, and dried at 100 ° C. for 2 minutes to evaporate toluene. Then, a heat ray shielding sheet was prepared by UV irradiation. A pressure-sensitive adhesive was applied on the produced heat ray shielding sheet to form a pressure sensitive adhesive sheet, and then bonded to 3 mm clear glass to produce heat ray shielding glass.
- PET polyethylene terephthalate
- Example 2 A heat ray shielding sheet was produced in the same manner as in Example 1 except that KAYARAD DPHA was changed to 0.3 part.
- Example 3 A heat ray shielding sheet was produced in the same manner as in Example 1 except that the peripheral speed of the bead mill was changed to 5 m / s.
- Example 4 28 parts of ITO and 12 parts of acrylic copolymer resin (Dainal Resin BR-116, manufactured by Mitsubishi Chemical) are added to 30 parts of xylene, 20 parts of toluene and 10 parts of ethanol, and dispersed at a peripheral speed of 10 m / s using a bead mill. A dispersion was prepared. The prepared dispersion was applied to a PET substrate with a wire bar so that the thickness after drying was 500 nm, and dried at 140 ° C. for 2 minutes to prepare a heat ray shielding sheet.
- acrylic copolymer resin (Dainal Resin BR-116, manufactured by Mitsubishi Chemical)
- Table 2 shows the results of measuring the visible light transmittance, near-infrared reflectance, haze value, surface resistance, maximum height difference of the layer surface, and heat shielding effect of Examples 1 to 4 and Comparative Examples 1 to 3.
- Table 3 shows. (Measurement of visible light transmittance) The visible light transmittance at a wavelength of 380 nm to 780 nm of the obtained heat ray shielding sheet was measured using a spectrophotometer (UV-3100, manufactured by Shimadzu Corporation) in accordance with JIS R3106.
- Test environment Inner width 150 mm ⁇ length 235 mm ⁇ height 110 mm outside air-blocking and airtightness, the ceiling is outside the center of the ceiling of a transparent glass test box, and the height is 40 cm from the ceiling.
- Install an infrared lamp 100V, 250W: Toshiba Corporation
- the manufactured heat ray shielding glass inside the test box ceiling so that the glass surface is on the infrared lamp side.
- the four sides were fixed with tape.
- a thermometer was installed on the central part inside the test box and on the heat-shielding glass surface inside the box so that the light from the lamp was not directly applied.
- the lamp was turned on and the heat ray shielding glass was irradiated with infrared rays.
- the temperature was measured every 10 seconds, and the temperature in the test box after 60 minutes was measured.
- the test box was installed in a room at about 25 ° C. In this test, the temperature inside the box when using the heat ray shielding glass prepared in Comparative Example 2 and the heat ray shielding glass of Example 1 was compared, and the temperature inside the box and the sheet surface temperature using the heat ray shielding glass of the present invention were compared. If each is low, the heat ray shielding effect is improved.
- the calculation method of the temperature difference in a box is each of the temperature in a box and the surface temperature using the heat ray shielding glass of the comparative example 2 from each of the temperature and surface temperature in the box using the heat ray shielding glass produced in Example 1. Is derived by subtracting.
- Examples 1 to 4 satisfy all the requirements of the present invention, but in Comparative Example 1, since the dispersion is insufficient, the fine particles are connected to each other and the surface resistance is low. Further, since the film surface is not smooth, the near infrared reflectance is less than 15%.
- the heat ray shielding sheet of the present invention has the visible light transmittance equivalent to that of the comparative example, but suppresses the rise in the temperature in the box and the glass surface temperature, and the heat shielding effect is improved. I can see that
- Comparative Example 3 the requirements such as surface resistance are satisfied, but since the dispersion energy is too high, the surface of the heat shielding fine particles is damaged, and as a result, the near-infrared reflection performance is not exhibited.
- Synthesis Example 1 Synthesis of near-infrared absorbing dye
- Add 15.9 parts of naphthalic anhydride, 29 parts of urea, 0.40 part of ammonium molybdate and 3.5 parts of vanadyl chloride (V) to 120 parts of sulfolane, heat up to 200 ° C., and react at that temperature for 11 hours. It was. After completion of the reaction, the reaction mixture was cooled to 65 ° C., 100 parts of N, N-dimethylformamide (DMF) was added, and the precipitated solid was separated by filtration. The obtained solid was washed with 50 parts of DMF to obtain 20.3 parts of a wet cake.
- N, N-dimethylformamide DMF
- the obtained wet cake was added to 100 parts of DMF, heated to 80 ° C., and stirred at the same temperature for 2 hours.
- the precipitated solid was separated by filtration and washed with 200 parts of water to obtain 18.9 parts of a wet cake.
- the obtained wet cake was added to 150 parts of water, heated to 90 ° C., and stirred at the same temperature for 2 hours.
- the precipitated solid was separated by filtration and washed with 200 parts of water to obtain 16.1 parts of a wet cake.
- the obtained wet cake was dried at 80 ° C. 12.3 parts of 25 were obtained.
- Synthesis Example 2 (Synthesis of near-infrared absorbing dye) In the same manner as in Synthesis Example 1 except that 15.9 parts of naphthalic anhydride of Synthesis Example 1 was changed to 11.9 parts and 3.0 parts of phthalic anhydride was added, Table 1 No. 12.3 parts of 1 were obtained.
- Synthesis Example 3 (Synthesis of near-infrared absorbing dye) In the same manner as in Synthesis Example 2 except that 3.0 parts of phthalic anhydride of Synthesis Example 2 are changed to 5.9 parts and 11.9 parts of naphthalic anhydride are changed to 7.9 parts, the above Table 1 No. 1 is prepared. 12.1 parts of 2 were obtained.
- the obtained wet cake was added to 100 parts of DMF, heated to 80 ° C., and stirred at the same temperature for 2 hours.
- the precipitated solid was separated by filtration and washed with 200 parts of water to obtain 40.1 parts of a wet cake.
- the obtained wet cake was added to 150 parts of water, heated to 90 ° C., and stirred at the same temperature for 2 hours.
- the precipitated solid was separated by filtration and washed with 7.9 parts of water to obtain 35.2 parts of a wet cake.
- the obtained wet cake was dried at 80 ° C. 10.8 parts of 9 were obtained.
- Synthesis Example 5 Synthesis of near-infrared absorbing dye
- Synthesis Example 4 Synthesis of near-infrared absorbing dye
- 3.3 parts of 3,4-pyridinedicarboxylic acid of Synthesis Example 4 were changed to 6.7 parts and 11.9 parts of naphthalic anhydride were changed to 7.9 parts. . 11.4 parts of 8 were obtained.
- Synthesis Example 6 Synthesis of near-infrared absorbing dye
- Compound 40 obtained in Synthesis Example 2 was added to 40 parts of polyphosphoric acid (116%). 1 part 3.4 parts, phthalimide 4.9 parts and paraformaldehyde 1.0 part were added, it heated up at 140 degreeC, and was made to react at the same temperature for 6 hours. After completion of the reaction, the mixture was cooled to 60 ° C. and 100 parts of water was added. The precipitated solid was separated by filtration and washed with water to obtain 34.0 parts of a wet cake. The obtained wet cake was added to 100 parts of a 10% aqueous potassium hydroxide solution and reacted at 50 ° C. for 2 hours.
- the precipitated solid was separated by filtration and washed with water to obtain 29 parts of a wet cake.
- the obtained wet cake was added to 100 parts of DMF and reacted at 25 ° C.
- the precipitated solid was separated by filtration and washed with water to obtain 13.3 parts of a wet cake.
- the obtained wet cake was dried at 80 ° C. 6.5 parts of 3 were obtained.
- Example 5 1.4 parts of tin-containing indium oxide (hereinafter referred to as ITO) described in Example 1, 0.1 part of the compound (near-infrared absorbing dye) obtained in Synthesis Example 1, KAYARAD DPHA (trade name, dipentaerythritol hexaacrylate, Nippon Kayaku Co., Ltd.) 0.1 part, Irgacure 184 (photopolymerization initiator, BASF Japan Co., Ltd.) 0.01 part, aminoalkyl methacrylate copolymer dispersant 0.1 part is added in 7 parts of toluene, A dispersion was prepared by dispersing the particles at a peripheral speed of 10 m / s using a bead mill.
- ITO tin-containing indium oxide
- the prepared dispersion was applied to a PET substrate (Cosmo Shine A4100, manufactured by Toyobo Co., Ltd.) with a wire bar, dried at 100 ° C. for 2 minutes to evaporate toluene, and then a heat ray shielding sheet was prepared by UV irradiation.
- the total solar energy transmittance (Tts) described later on the heat ray shielding sheet was 53.5%.
- a pressure-sensitive adhesive (Cooponyl N-2147, manufactured by Nippon Synthetic Chemical Industry Co., Ltd.) is applied onto the heat ray shielding sheet thus prepared, and is then attached to a 3 mm clear glass to obtain the heat ray shielding glass of the present invention. Produced.
- Example 10 A heat ray shielding sheet of the present invention was produced in the same manner as in Example 5 except that KAYARAD DPHA was changed to 0.3 part.
- Example 11 A heat ray shielding sheet of the present invention was produced in the same manner as in Example 5 except that the peripheral speed of the bead mill was changed to 5 m / s.
- the postscript total solar energy transmittance (Tts) of the obtained heat ray shielding sheet was 55.1%.
- Example 12 (Production of cholesteric liquid crystal laminate) 10 parts of LC-242 (photopolymerizable liquid crystal compound, manufactured by BASF), 0.30 part of LC-756 (chiral agent, manufactured by BASF), 0.51 part of lucillin TPO (photopolymerization initiator, manufactured by BASF) A coating solution 1 was prepared by dissolving in 25 parts of cyclopentanone.
- LC-242 photopolymerizable liquid crystal compound, manufactured by BASF
- LC-756 chiral agent, manufactured by BASF
- Lucillin TPO photopolymerization initiator, manufactured by BASF
- the prepared coating solution 1 was applied to a PET substrate (Cosmo Shine A4100, manufactured by Toyobo Co., Ltd.) with a wire bar so as to have a film thickness of 7 ⁇ m, and dried at 150 ° C. for 5 minutes to evaporate cyclopentanone. Thereafter, it was cured by UV irradiation. Further, in the same manner as the coating solution 1, the coating solution 2 was applied, dried, and UV-irradiated to produce a cholesteric liquid crystal laminate.
- Comparative Example 4 In order to see the difference in reflectance and haze, etc. depending on the ITO dispersion method, the ITO concentration, etc. is exactly the same as in Example 5, and only the peripheral speed of the bead mill is changed to 2 m / s, as in Example 5. Thus, a comparative heat ray shielding sheet was produced.
- Comparative Example 5 In order to see the difference in performance at the ITO concentration, a comparative heat ray shielding sheet was produced in the same manner as in Example 5 except that KAYARAD DPHA of Example 1 was changed to 1.3 parts. Moreover, after apply
- Comparative Example 6 In order to investigate the influence of dispersion at high energy, a comparative heat ray shielding sheet was produced in the same manner as in Example 10 except that the bead mill peripheral speed was changed to 14 m / s.
- the lamp was turned on and the heat ray shielding glass was irradiated with infrared rays.
- the temperature was measured every 10 seconds, and the temperature in the test box after 60 minutes was measured.
- the test box was installed in a room at about 25 ° C. In this test, the temperature inside the box when using the heat ray shielding glass prepared in Comparative Example 5 and the heat ray shielding glass of Example 5 was compared, and the temperature inside the box and the sheet surface temperature using the heat ray shielding glass of the present invention were compared. If it is low, the heat ray shielding effect is improved.
- the calculation method of the temperature difference in a box is the temperature in the box and the surface temperature using the heat ray shielding glass of Comparative Example 5 from the temperature in the box and the surface temperature using the heat ray shielding glass produced in Example 5, respectively. Guided by subtracting each.
- Comparative Example 4 since the dispersion is insufficient, the conductive fine particles are connected to each other, the surface resistance is low, and the film surface is not smooth. Therefore, the near infrared reflectance is less than 15%. In Comparative Example 6, the requirements such as surface resistance are satisfied, but since the dispersion energy is high, the surface of the conductive fine particles is damaged, and as a result, the near-infrared reflection performance is not exhibited.
- the heat ray shielding sheet of the present invention has the visible light transmittance equivalent to that of the comparative example, but suppresses the rise in the temperature inside the box and the glass surface temperature, and provides near infrared reflection performance. It can be seen that the heat shielding effect is improved.
- Example 13 (Dielectric multilayer film) Preparation of high refractive index layer dispersion Titanium oxide (trade name: TTO-V3, manufactured by Ishihara Sangyo Co., Ltd.) 1.4 parts, KAYARAD DPHA (trade name, dipentaerythritol hexaacrylate, manufactured by Nippon Kayaku Co., Ltd.) 0 .1 part, Irgacure 184 (radical photopolymerization initiator, manufactured by BASF Japan Ltd.) 0.01 part, aminoalkyl methacrylate copolymer dispersant (trade name, Disper BYK145, manufactured by Big Chemie Japan Co., Ltd.) 0.1 Part was added to 7 parts of toluene and dispersed at a peripheral speed of 10 m / s using a bead mill to prepare a high refractive index layer dispersion.
- TiO-V3 manufactured by Ishihara Sangyo Co., Ltd.
- KAYARAD DPHA trade name
- the prepared high refractive index dispersion was applied to a polyethylene terephthalate (PET) sheet (base material) (thickness 100 ⁇ m) with a wire bar so that the optical film thickness after drying was 250 nm. After drying at 100 ° C. for 2 minutes, a high refractive index layer was produced by UV irradiation. Similarly, a low refractive index layer dispersion was formed on the high refractive index layer by coating, drying and UV irradiation so that the optical film thickness after drying was 250 nm.
- PET polyethylene terephthalate
- the prepared dispersion was applied to the prepared dielectric multilayer film with a wire bar, dried at 100 ° C. for 2 minutes to evaporate toluene, and then the heat ray shielding sheet of the present invention was prepared by UV irradiation.
- Example 14 (Production of cholesteric liquid crystal laminate) 10 parts of LC-242 (liquid crystal compound, manufactured by BASF), 0.38 parts of LC-756 (chiral agent, manufactured by BASF), 0.52 parts of lucillin TPO (photopolymerization initiator, manufactured by BASF), cyclopentanone Dissolved in 25 parts to prepare coating solution 1.
- 10 parts of LC-242 (liquid crystal compound, manufactured by BASF), 0.30 part of LC-756 (manufactured by BASF), 0.51 part of lucillin TPO (photopolymerization initiator, manufactured by BASF) were added to cyclohexane. Dissolved in 25 parts of pentanone to prepare coating solution 2.
- LC-242 liquid crystal compound, manufactured by BASF
- 0.26 part of LC-756 manufactured by BASF
- 0.51 part of lucillin TPO photopolymerization initiator, manufactured by BASF
- coating solution 3 Dissolved in 25 parts of pentanone to prepare coating solution 3.
- the prepared coating solution 1 was applied to a PET substrate (Cosmo Shine A4100, manufactured by Toyobo Co., Ltd.) with a wire bar, dried at 150 ° C. for 5 minutes to evaporate cyclopentanone, and then cured by UV irradiation.
- Example 15 A heat ray shielding sheet of the present invention was produced in the same manner as in Example 13 except that the dielectric multilayer film was changed to Nano 90S (manufactured by Sumitomo 3M Limited, birefringence multilayer film).
- Example 16 A heat ray shielding sheet of the present invention was produced in the same manner as in Example 13 except that KAYARAD DPHA was changed to 0.3 part.
- Example 17 A heat ray shielding sheet of the present invention was produced in the same manner as in Example 13 except that the peripheral speed of the bead mill was changed to 5 m / s.
- Comparative Example 7 A comparative heat ray shielding sheet was prepared in the same manner as in Example 14 except that KAYARAD DPHA was changed to 1.3 parts. Moreover, after apply
- Tables 6 and 7 show the results of measuring the visible light transmittance, total solar energy, haze value, surface resistance, maximum height difference of the layer surface, and heat shielding effect of the heat ray shielding sheets of Examples 13 to 17 and Comparative Example 7. .
- the visible light transmittance at a wavelength of 380 nm to 780 nm of the obtained heat ray shielding sheet was measured using a spectrophotometer (UV-3100, manufactured by Shimadzu Corporation) in accordance with JIS R3106.
- the total solar energy transmission (Tts) is a measure of how much of the thermal energy from the sun is transmitted through the material of interest, and is a spectrophotometer (UV-3100 manufactured by Shimadzu Corporation). Based on JIS R3106, based on the data obtained by measuring the transmittance and reflectance at 300 nm to 2500 nm of the obtained heat ray shielding sheet, it was calculated by a calculation formula defined in ISO13837. It shows that the transmitted solar radiation energy is so small that the calculated numerical value is small, and heat ray shielding property is high.
- the temperature inside the box when using the heat ray shielding glass prepared in Comparative Example 7 and the heat ray shielding glass of Example 14 was compared, and the temperature inside the box and the sheet surface temperature using the heat ray shielding glass of the present invention were compared. If each is low, the heat ray shielding effect is improved.
- the calculation method of the temperature difference in a box calculates each of the temperature in a box and the surface temperature using the heat ray shielding glass of Comparative Example 7 from each of the temperature in the box and the surface temperature using the heat ray shielding glass produced in Example 14. Guided by subtracting.
- the heat ray shielding sheet of the present invention has the visible light transmittance equivalent to that of the comparative example, but suppresses the temperature rise in the box and the glass surface temperature, as shown in Table 2 above.
- the heat shielding effect is improved by imparting near-infrared reflection performance to the heat ray shielding layer (expressed as a fine particle layer in Table 6 below).
- the metal oxide fine particles are sufficiently dispersed in the heat ray shielding layer, and the near-infrared absorptivity of the metal oxide fine particles is also utilized, and the near-infrared reflectivity is also utilized.
- the heat ray shielding layer contains a near infrared absorbing dye, or a heat ray shielding sheet containing a near infrared absorbing dye layer together with the heat ray shielding layer, or a reflective layer.
- 10 shows a model diagram of the heat ray shielding sheet of the present invention.
- 11 is a heat ray shielding layer of the present invention, 12 is a support, and 13 is a reflective layer.
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Abstract
Description
また、特許文献5では、近赤外線領域の光線を反射するコレステリック液晶と、コレステリック液晶が反射する波長より長波長の熱線を吸収する遮熱微粒子を積層した断熱部材が開示されている。
本発明は、上記の種々の問題を解決し、建物の窓、乗り物の窓、冷蔵、冷凍ショーケースの窓ガラス等に用いることが出来る、可視光領域における透明性に優れ、電波透過性を有し、且つ、熱線遮蔽性にも優れる熱線遮蔽シートの開発を目的とするものである。
即ち、該微粒子を高濃度で該熱線遮蔽層に含ませることは知られているが、本発明者らの検討では、該微粒子を、バインダー成分中に高濃度で含ませ、通常の攪拌(例えば、ホモジナイザー等にによる攪拌)で分散させても、十分な反射性能と、表面抵抗を併せ有する熱線遮蔽シートを得ることが出来無かった。その原因は、該微粒子が、十分に分散されず、微粒子の凝集や微粒子の連結等により、上記の表面抵抗値が出ず、かつ、表面の平滑性が失われたりするため、該微粒子でのプラズマ振動での反射が十分に活用できなかったためと思われる。しかしながら、本発明者らは、例えば、ビーズミル等により、該微粒子を、非凝集で非連続の状態になるように、かつ、該微粒子の反射性能を阻害しないように、適切にバインダー成分中に分散させ、該分散液を支持体上に塗布するなどして、表面を平滑に成膜するならば、十分な反射性能と、十分な電波透過性を有する表面抵抗を併せ有すると共に、十分な可視光の透過性を有し、かつ、低ヘイズである熱線遮蔽層を得ることが出来ることを見いだしたものである。
(1) 支持体の上に、平均粒径100nm以下の微粒子と空隙部分を埋める樹脂バインダーとを含有する熱線遮蔽層を有し、該熱線遮蔽層における、少なくとも2000nmの波長での反射率が少なくとも15%であり、且つ該熱線遮蔽層の表面抵抗が106Ω/□以上である熱線遮蔽シート。
(2) 熱線遮蔽層表面の最大高低差が60nm以下である上記(1)に記載の熱線遮蔽シート。
(3) 熱線遮蔽層のヘイズが3%以下である上記(1)または(2)に記載の熱線遮蔽シート。
(4) 用いる微粒子の粉体抵抗が10Ω・cm以下である上記(1)乃至(3)の何れか一項に記載の熱線遮蔽シート。
(5) 微粒子が酸化錫、酸化インジウム、酸化亜鉛、及び酸化タングステンからなる群から選ばれる少なくとも一種の微粒子である上記(1)乃至(4)の何れか一項に記載の熱線遮蔽シート。
(6) 微粒子が錫ドープ酸化インジウムである上記(1)及至(5)の何れか一項に記載の熱線遮蔽シート。
(8) 熱線遮蔽層の可視光線透過率が70%以上である上記(1)乃至(7)の何れか一項に記載の熱線遮蔽シート。
(9) 微粒子が導電性微粒子であり、熱線遮蔽層が、更に、近赤外線吸収色素を含み、該近赤外線吸収色素が樹脂バインダー中に分散している上記(1)~(7)の何れか一項に記載の熱線遮蔽シート。
(10) 熱線遮蔽層とは別に、更に、近赤外線吸収色素を含む色素層を含む上記(1)~(7)の何れか一項に記載の熱線遮蔽シート。
(11) 可視光透過率が50%以上、ヘイズが3%以下であることを特徴とする上記(9)又は(10)に記載の熱線遮蔽シート。
(12) 近赤外線吸収色素としてポルフィラジン色素、またはジイモニウム色素を含む上記(9)~(11)の何れか一項に記載の熱線遮蔽シート。
(13) ポルフィラジン色素として、下記式(1)
[式(1)中、Mは金属原子、金属酸化物、金属水酸化物、若しくは金属ハロゲン化物、又は水素原子を表し、環A、B、C及びDの破線部は、それぞれ独立に、下記式(2)~(8)
の何れか一つの構造であり、開口部で、骨格構造へ結合して、芳香環を形成し、Xは低級アルキル基、低級アルコキシ基、アミノ基、ニトロ基、ハロゲン基、ヒドロキシ基、カルボキシ基、スルホン酸基、又はスルホンアミド基を表し、Yは二価の架橋基を、Zはスルホン酸基、カルボキシ基、第1または2級アミンの窒素原子上の水素の少なくとも1つを除いた残基、酸アミド基、または、窒素原子を含む複素環の窒素原子上の水素の少なくとも1つを除いた残基を表し、a及びbは、それぞれの基の数を表し、いずれも平均値であり、それぞれ独立に0以上12以下であり、かつ、aとbとの和は0以上12以下である]
で表されるポルフィラジン色素を含む上記(9)~(12)の何れか一項に記載の熱線遮蔽シート。
(14) 式(1)中の環A、B、C及びDがそれぞれ独立に式(2)、式(4)または式(8)の何れかである上記(13)に記載の熱線遮蔽シート。
(15) 式(1)中のMはVOまたはCuである上記(13)又は(14)に記載の熱線遮蔽シート。
(16) 式(1)中、Yは炭素数1~3のアルキレン基であり、Zは置換基を有してもよいフタルイミド基又は置換基を有してもよいピペラジノ基である上記(13)~(15)の何れか一項に記載の熱線遮蔽シート。
(17) 式(1)のポルフィラジン色素が下記式(9)
[式中の環A、B、C及びDはそれぞれ独立に下記式(4)または式(8)
の何れかの構造であり、開口部で、骨格構造へ結合して芳香環を示す]
で表されるポルフィラジン色素である上記(14)又は(15)に記載の熱線遮蔽シート。
(19) 反射層が少なくとも1つのコレステリック液晶層、誘電体多層膜及び複屈折多層膜からなる群から選ばれる少なくとも一つである上記(18)に記載の熱線遮蔽シート。
(20) 反射層が少なくとも1つのコレステリック液晶層である上記(19)に記載の熱線遮蔽シート。
(21) 樹脂バインダーが熱または光硬化性樹脂の硬化物または熱可塑性樹脂である上記(1)~(20)の何れか一項に記載の熱線遮蔽シート。
本発明においては、上記の微粒子、好ましくは、透明金属酸化物微粒子(導電性微粒子)を、バインダー成分中に、非連続、非凝集の状態で高濃度で、かつ、近赤外線反射性能を損なわない状態で、分散させ、該分散液を支持体上に、平滑に塗布成膜することにより、該熱線遮蔽層の表面抵抗を106Ω/□以上で、該熱線遮蔽層での近赤外線の長波長側(2000nm以上)の光の反射率を15%以上とすることができる。
該熱線遮蔽層の表面抵抗は、106Ω/□以上であれば、電波を透過させることが出来るが、好ましくは107Ω/□以上であり、より好ましくは108Ω/□以上、更に好ましくは、109Ω/□以上、最も好ましくは109.5Ω/□以上である。該表面抵抗の値に、上限は無いが、該熱線遮蔽層の表面抵抗の上限は1013Ω/□程度、好ましくは1012.5Ω/□程度である。
上記の表面抵抗と上記の反射率の好ましい組み合わせとしては、上記の表面抵抗の値が上記の、好ましい値、より好ましい値、更に好ましい値及び最も好ましい値からなる群から選ばれる何れか一つであり、上記の反射率の値が、上記の好ましい値、より好ましい値及び最も好ましい値からなる群から選ばれる何れか一つである場合である。好ましい組み合わせの例を示すと、上記の表面抵抗の値が、108Ω/□以上であり、上記の反射率の値が、20%以上、25%以上及び28%以上からなる群から選ばれる何れか一つである場合であり、より好ましい組み合わせの例としては、上記の表面抵抗の値が、109Ω/□以上であり、上記の反射率の値が、20%以上、25%以上及び28%以上からなる群から選ばれる何れか一つである場合である。
本発明においては、上記の表面抵抗と上記の反射率の組み合わせを達成できれば、該微粒子の分散方法は特に問わないが、上記組み合わせの値を達成する分散方法の一つとして、ビーズミルでの分散を挙げることが出来る。該ビーズミルでの分散の場合、上記の表面抵抗の値と上記の反射率の値の組み合わせを達成するには、通常周速3m/s以上で分散させる。好ましい周速は5m/s以上であり、より好ましくは8m/s以上である。該周速が早すぎても、上記の組み合わせを達成することが出来なくなるので、通常は12m/s以下程度が好ましく、11m/s以下がより好ましい。
該熱線遮蔽層は、上記の表面抵抗と上記の反射率の組み合わせに、更に、上記のヘイズ値を達成する組み合わせはより好ましく、上記の表面抵抗と上記の反射率の組み合わせに、更に、上記の好ましいヘイズ値、より好ましいヘイズ値を組み合わせた態様は、非常に好ましい。例えば、該熱線遮蔽層の表面抵抗を106Ω/□以上で、該熱線遮蔽層での近赤外線の長波長側(2000nm以上)の光の反射率が15%以上で、該熱線遮蔽層におけるヘイズ値が、8%以下、5%以下、3%以下、2%以下及び1%以下からなる群から選ばれる何れか一つである組合せである。また、他の好ましい組合せの例としては、該熱線遮蔽層の表面抵抗が108Ω/□以上、上記の反射率が15%以上で、そして上記のヘイズ値が3%以下、より好ましくは1%以下の組合せである。また、他のより好ましい組み合わせの1例としては、上記の表面抵抗が109Ω/□以上、上記の反射率が15%以上で、上記のヘイズ値が1%以下、より好ましくは0.8%以下である。より好ましい他の組み合わせの例としては、上記の表面抵抗が109Ω/□以上、上記の反射率が15%以上で、上記のヘイズ値が1%以下、より好ましくは0.8%以下である。更に好ましい組合せの例としては、上記の表面抵抗が109Ω/□以上であり、上記の反射率が20%以上、より好ましくは25%以上であり、そして、上記のヘイズ値が1%以下、より好ましくは0.8%以下である組合せである。
また、該熱線遮蔽層の可視光透過率は、70%以上が好ましく、より好ましくは74%以上、更に好ましくは80%以上である。
なお、上記の該熱線遮蔽層の表面抵抗、反射率、ヘイズ値、可視光透過率は何れも、上記熱線遮蔽層を、ポリエチレンテレフタレート(PET)支持体{厚さ、100μm、可視光透過率92%、ヘイズ値0.3%}に、乾燥後又は硬化後の厚さ500nmになるように形成して、測定した値である。従って、この値は、上記PET支持体を含めた値である。本発明においては、この値を、便宜的に該熱線遮蔽層のヘイズ値及び可視光透過率の値とする。従って、本発明の熱線遮蔽シートが該熱線遮蔽層と上記のPETの2者で構成されるときは、上記の該熱線遮蔽層の値と熱線遮蔽シートの値は、同じ値となる。
ドーパントの含量は特に限定されないが、ドーパントされた金属の総量に対して、1~20重量%程度、好ましくは、5~15重量%程度である。ITOにおける錫含量も同じである。
平均粒子径が大きくなり過ぎると熱線遮蔽シートにした際、ヘイズ値が高くなり視認性が劣ってしまう。
市販品としては、ITOまたは超微粒ITO等として、CIKナノテック株式会社、住友金属工業株式会社、三菱マテリアル株式会社等から販売されており、上記の平均粒子経と粉体抵抗値を満たすものは何れも使用可能である。その中でも、ITO-R(CIKナノテック株式会社製)はより好ましい。
熱線遮蔽層における樹脂バインダーとしては微粒子を分散維持できる樹脂であれば、特に制限はない。通常、熱可塑性樹脂、又は/及び、熱又は光で硬化する硬化性樹脂(熱または光硬化性樹脂とも言う)(具体的には熱硬化性樹脂又は光硬化性樹脂)の硬化物等が挙げられる。熱線遮蔽層中の樹脂バインダーの含有率は、熱線遮蔽層の総量に対して、5~60重量%、好ましくは5~40重量%、より好ましくは5~30重量%、更に好ましくは5~25重量%、最も好ましくは、5重量%以上で、20重量%未満である。分散剤等の任意の添加剤は、バインダー成分の総量に対して、0~80重量%、好ましくは0~70重量%、より好ましくは10~70重量%である。
これらの熱可塑性樹脂の重量平均分子量は1000~1,000,000程度であり、好ましくは2000乃至500,000程度、より好ましくは2000~200,000程度である。
熱可塑性樹脂として好ましい樹脂は、透明性等の観点から(メタ)アクリル樹脂が好ましく、例えば(メタ)アクリレートポリマー、特に(メタ)アクリル共重合体等が好ましい。
熱硬化性樹脂としては、加熱により硬化可能な官能基を有する化合物であれば特に限定されず、例えば、エポキシ基、オキセタニル基等の環状エーテルを有する硬化性化合物が挙げられる。また、光硬化性樹脂としては、光照射により硬化可能な官能基を有する化合物であれば特に限定されず、例えば、ビニル基、ビニルエーテル基、アリル基、マレイミド基、(メタ)アクリル基等の不飽和二重結合を有する硬化性化合物を有する樹脂が挙げられる。
該微粒子分散液には、必要に応じて、溶媒の他、光反応開始剤、熱硬化剤、分散剤、近赤外線吸収色素、紫外線吸収剤、酸化防止剤、光安定剤等の各種添加剤を添加することができる。
光反応開始剤としては、光照射により、硬化性樹脂中の不飽和二重結合やエポキシ基等を重合反応させるためのものであれば特に制限は無く、例えば、カチオン重合型光開始剤やラジカル重合型光開始剤が挙げられる。
また、熱硬化剤としては、加熱により硬化性樹脂中の不飽和二重結合やエポキシ基等を反応させ、架橋させるためのものであれば特に制限は無く、例えば酸無水物、アミン類、フェノール類、イミダゾール類、ジヒドラジン類、ルイス酸、ブレンステッド酸塩類、ポリメルカプトン類、イソシアネート類、ブロックイソシアネート類等が挙げられる。光反応開始剤の使用量は通常、光硬化性樹脂に対して、1~20重量%の割合で使用される。
本発明においては、樹脂バインダーとして、硬化性樹脂、好ましくは光硬化性樹脂、より好ましくは(メタ)アクリレート化合物を含み、添加剤として光反応開始剤、より好ましくはラジカル重合型光開始剤を含む態様は好ましい。
分散剤としては、低分子分散剤(分子量2000未満、好ましくは1000以下の分散剤)や、高分子分散剤(重量平均分子量2,000以上、500、000以下程度、好ましくは2,000~200,000、より好ましくは2,000~100,000程度)などを挙げることができる。
低分子分散剤としては、脂肪酸塩(石けん)、α-スルホ脂肪酸エステル塩(MES)、アルキルベンゼンスルホン酸塩(ABS)、直鎖アルキルベンゼンスルホン酸塩(LAS)、アルキル硫酸塩(AS)、アルキルエーテル硫酸エステル塩(AES)、アルキル硫酸トリエタノールといった低分子陰イオン性(アニオン性)化合物、脂肪酸エタノールアミド、ポリオキシエチレンアルキルエーテル(AE)、ポリオキシエチレンアルキルフェニルエーテル(APE)、ソルビトール、ソルビタンといった低分子非イオン系化合物、アルキルトリメチルアンモニウム塩、ジアルキルジメチルアンモニウムクロリド、アルキルピリジニウムクロリド、といった低分子陽イオン性(カチオン性)化合物、アルキルカルボキシルベタイン、スルホベタイン、レシチンといった低分子両性系化合物を挙げることができる。
また、高分子分散剤としては、ナフタレンスルホン酸塩のホルマリン縮合物、ポリスチレンスルホン酸塩、ポリアクリル酸塩、ビニル化合物とカルボン酸系単量体の共重合体塩、カルボキシメチルセルロース、ポリビニルアルコールなどに代表される高分子水系分散剤、ポリアクリル酸部分アルキルエステル、ポリアルキレンポリアミンといった高分子非水系分散剤、ポリエチレンイミン又はアミノアルキルメタクリレート共重合体といった高分子カチオン系分散剤等の重量平均分子量2,000以上、100,000以下の高分子分散剤が代表的なものである。本発明の微粒子に好適に適用されるものであれば、上記に例示したものに限定されない。
本発明においては、高分子分散剤が好ましく、高分子分散剤の中では、(メタ)アクリレート共重合体分散剤がより好ましい。
フローレンDOPA-15B、フローレンDOPA-17(共栄社化学株式会社製)、ソルプラスAX5、ソルプラスTX5、ソルスパース(登録商標) (以下同じ)9000、ソルスパース12000、ソルスパース17000、ソルスパース20000、ソルスパース21000、ソルスパース24000、ソルスパース26000、ソルスパース27000、ソルスパース28000、ソルスパース32000、ソルスパース35100、ソルスパース54000、ソルシックス250(日本ルーブリゾール株式会社製)、EFKA4008、EFKA4009、EFKA4010、EFKA4015、EFKA4046、EFKA4047、EFKA4060、EFKA4080、EFKA7462、EFKA4020、EFKA4050、EFKA4055、EFKA4400、EFKA4401、EFKA4402、EFKA4403、EFKA4300、EFKA4320、EFKA4330、EFKA4340、EFKA6220、EFKA6225、EFKA6700、EFKA6780、EFKA6782、EFKA8503(エフカアディディブズ株式会社製)、アジスパーPA111、アジスパー(登録商標) (以下同じ)PB711、アジスパーPB821、アジスパーPB822、アジスパーPN411、フェイメックスL-12(味の素ファインテクノ株式会社製)、TEXAPHOR-UV21、TEXAPHOR-UV61(コグニスジャパン株式会社製)、DisperBYK101、DisperBYK102、DisperBYK106、DisperBYK108、DisperBYK111、DisperBYK116、DisperBYK130、DisperBYK140、DisperBYK142、DisperBYK145、DisperBYK161、DisperBYK162、DisperBYK163、DisperBYK164、DisperBYK166、DisperBYK167、DisperBYK168、DisperBYK170、DisperBYK171、DisperBYK174、DisperBYK180、DisperBYK182、DisperBYK192、DisperBYK193、DisperBYK2000、DisperBYK2001、DisperBYK2020、DisperBYK2025、DisperBYK2050、DisperBYK2070、DisperBYK2155、DisperBYK2164、BYK220S、BYK300、BYK306、BYK320、BYK322、BYK325、BYK330、BYK340、BYK350、BYK377、BYK378、BYK380N、BYK410、BYK425、BYK430(ビックケミー・ジャパン株式会社製)、ディスパロン(登録商標) (以下同じ)1751N、ディスパロン1831、ディスパロン1850、ディスパロン1860、ディスパロン1934、ディスパロンDA-400N、ディスパロンDA-703-50、ディスパロンDA-725、ディスパロンDA-705、ディスパロンDA-7301、ディスパロンDN-900、ディスパロンNS-5210、ディスパロンNVI-8514L、ヒップラードED-152、ヒップラードED-216、ヒップラードED-251、ヒップラードED-360(楠本化成株式会社製)、FTX-207S、FTX-212P、FTX-220P、FTX-220S、FTX-228P、FTX-710LL、FTX-750LL、フタージェント(登録商標) (以下同じ)212P、フタージェント220P、フタージェント222F、フタージェント228P、フタージェント245F、フタージェント245P、フタージェント250、フタージェント251、フタージェント710FM、フタージェント730FM、フタージェント730LL、フタージェント730LS、フタージェント750DM、フタージェント750FM(株式会社ネオス製)、AS-1100、AS-1800、AS-2000(東亞合成株式会社製)、カオーセラ(登録商標) (以下同じ)2000、カオーセラ2100、KDH-154、MX-2045L、ホモゲノール(登録商標) (以下同じ)L-18、ホモゲノールL-95、レオドール(登録商標) (以下同じ)SP-010V、レオドールSP-030V、レオドールSP-L10、レオドールSP-P10(花王株式会社製)、エバンU103、シアノールDC902B、ノイゲン(登録商標)EA-167、ブライサーフA219B、ブライサーフAL(第一工業製薬株式会社製)、メガファック(登録商標) (以下同じ)F-477、メガファック480SF、メガファックF-482、(DIC株式会社製)、シルフェイス(登録商標)SAG503A、ダイノール604(日信化学工業株式会社製)、SNスパーズ2180、SNスパーズ2190、SNレベラーS-906(サンノプコ株式会社製)、S-386、S-420(AGCセイミケミカル株式会社製)といったものが例示できる。
また、本発明においては、上記熱線遮蔽層に近赤外線吸収色素を含める代わりに、該熱線吸収層とは別に、更に、該近赤外線吸収色素を含む色素層を含む熱線遮蔽シートとしてもよい。この場合、色素層は、色素単独でもよいが、通常、樹脂バインダー中に、該色素を分散させ、色素層とするのが好ましい。樹脂バインダー中に分散させる場合、樹脂バインダー1重量部に対して、0.01~20重量部の範囲で、必要に応じて、溶媒を添加して分散液として、支持体等の色素層を形成させる層の上に塗布して、必要に応じて、乾燥又は/及び硬化を行い色素層を形成すればよい。通常、該色素層は、入射光方向から、上記熱線遮蔽層の後に来るように形成するのが好ましい。例えば、支持体(若しくは後記する反射層)上に、該色素層を形成し、該色素層の上に、上記熱線遮蔽層を形成する等の方法が好ましい。また、場合により、該色素層を、支持体の上記熱線遮蔽層とは反対の面に形成することもできる。
本発明においては、上記熱線遮蔽層中に、前記微粒子と共に近赤外線吸収色素を含ませる態様が好ましい。
近赤外線吸収色素は、赤外線の中でも可視領域に近い近赤外線(波長約780~2000nm)を吸収する色素の総称である。近赤外線吸収色素としては公知のものは何れも使用しうる。近赤外線吸収色素の種類としてはアゾ色素、アミニウム色素、アンスラキノン色素、シアニン色素、ジイモニウム色素、ジチオール金属錯体色素、スクアリリウム色素、ポルフィラジン色素等が挙げられる。耐久性を高くするには、ポルフィラジン色素、ジイモニウム色素が好ましい。本発明においては、熱線を効率良く遮断するポルフィラジン色素がより好ましく、何れのポルフィラジン色素も使用できる。
式(1)中、Mは金属原子、金属酸化物、金属水酸化物、若しくは金属ハロゲン化物、又は水素原子を表し、環A、B、C及びDの破線部は、それぞれ独立に、下記式(2)~(8)
の何れか一つの構造であり、Xは低級アルキル基、低級アルコキシ基、アミノ基、ニトロ基、ハロゲン基、ヒドロキシ基、カルボキシ基、スルホン酸基、スルホンアミド基を表し、Yは二価の架橋基を、Zはスルホン酸基、カルボキシ基、第1または2級アミンの窒素原子上の水素の少なくとも1つを除いた残基、酸アミド基、又は窒素原子を含む複素環の窒素原子上の水素の少なくとも1つを除いた残基を表し、a及びbはそれぞれの基の数を表し、いずれも平均値であり、a及びbはそれぞれ独立に0以上12以下であり、かつ、aとbとの和は0以上12以下である。下記式(2)~(8)は開口部で、骨格構造へ結合して、環A、B、C及びDの芳香環を形成する。
Zにおける第1又は第2級アミンの窒素原子上の水素の少なくとも1つを除いた残基としてはモノ低級アルキルアミノ基、ジ低級アルキルアミノ基等を挙げることが出来る。また、酸アミド基としては、置換基を有してもよいフタル酸アミド基等を挙げることが出来る。窒素原子を含む複素環の窒素原子上の水素の少なくとも1つを除いた残基としては、置換基を有してもよいピリジノ基、置換基を有してもよいピペラジノ基、又は置換基を有してもよいピペリジノ基等を挙げることができる。
好ましいZとしては例えば、カルボキシ基、スルホン酸基、置換基を有してもよいフタルイミド基、置換基を有してもよいピペラジノ基、置換基を有してもよいピペリジノ基等を挙げることができる。より好ましいZはカルボキシ基、スルホン酸基、又は、置換基を有してもよいフタルイミド基であり、置換基を有してもよいフタルイミド基が更に好ましい。なお、Zが置換基を有してもよいフタルイミド基、置換基を有してもよいピペラジノ基又は置換基を有してもよいピペリジノ基であるときの置換基としては低級アルキル基、低級アルコキシ基、置換アミノ基、ニトロ基、ハロゲン原子又はスルホン酸基等を挙げることができる。Zが、上記の置換基を有してもよい基であるとき、無置換又はハロゲノ置換された基が好ましい。より好ましいZは、無置換又はハロゲノ置換フタルイミド基であり、無置換フタルイミドが最も好ましい。
本発明において「低級」とは炭素数1~4を示し、ハロゲン原子としてはCl、Br又はIが好ましい。
下記の例は、本発明の色素を具体的に説明するために代表的な色素を示すものであり、本発明は下記の例に限定されるものではない。また、環A乃至Dの含窒素複素芳香環が前記式(3)、(4)及び(6)である場合、窒素原子の位置異性体が存在し、色素合成の際には異性体の混合物として得られる。これら異性体の単離は困難であり、また分析による異性体の特定も困難である。このため、通常は混合物のまま使用する。本発明の色素は、このような混合物も含むものである。本明細書においては、これらの異性体等を区別することなく、構造式で表示される場合は、便宜的に代表的な1つの構造式を記載する。
表1において、A乃至Dの欄の数字は、前記式(2)~(8)の式番号を示し、a及びbの欄には、それぞれ、a及びbの値を示し、X、Y及びZの欄には基名を示した。X、Y及びZの欄における横線-は置換基が無いことを示す。
前記式(1)で表されるポルフィラジン色素は、例えば、国際公開第2010/143619号パンフレット及び国際公開第2010/013455号パンフレットに開示された公知の方法に準じて合成することができる。なお、上記方法によって得られる前記式(1)で表される化合物は、環A乃至Dにおける含窒素複素芳香環の置換位置、及び含窒素複素芳香環の窒素原子の置換位置に関する位置異性体の混合物となることも、上記公知文献に記載の通りである。
また、前記表1におけるNo.3やNo.18で示される化合物は、上記国際公開パンフレットの他、例えば、特許第2507786号パンフレット及び特許第3813750号パンフレットに開示された公知の方法に準じても合成することが出来る。
i.分散液の固形分総量(溶媒を除いたとき残る成分の総量:通常溶媒を除く全成分の総量)に対して、平均粒径100nm以下の金属酸化物微粒子を60~95%、樹脂バインダーを2~40%、添加剤を0~38%及び溶媒を含む分散液。
ii.金属酸化物微粒子の60MPaで圧縮した際の粉体抵抗が10Ω・cmである上記iに記載の分散液。
iii.金属酸化物微粒子が酸化錫、酸化インジウム、酸化亜鉛及び酸化タングステンからなる群から選ばれる少なくとも一つの微粒子である上記i又はiiに記載の分散液。
iv.金属酸化物微粒子が錫ドープ酸化インジウムの微粒子である上記i~iiiの何れか一項に記載の分散液。
v.金属酸化物微粒子の60MPaで圧縮した際の粉体抵抗が1Ω・cmである上記i~ivに記載の分散液。
vi.金属酸化物微粒子の平均粒径が30nm以下の金属酸化物微粒子である上記i~vの何れか一項に記載の分散液。
vii.樹脂バインダーが熱可塑性樹脂又は硬化性樹脂である上記i~viの何れか一項に記載の分散液。
viii.樹脂バインダーとして光硬化性樹脂を含み、添加剤として光反応開始剤を含む上記i~viiの何れか一項に記載の分散液。
ix.光反応開始剤の添加量が、光硬化性樹脂に対して1~20%である上記viiiに記載の分散液。
x.光硬化性樹脂が(メタ)アクリレート化合物である上記viiiに記載の分散液。
xi.光反応開始剤がラジカル重合型光開始剤である上記viii~xの何れか一項に記載の分散液。
xiii.近赤外線吸収色素の添加量が、分散液の固形分総量に対して、1~30%含む上記xiiに記載の分散液。
xiv.近赤外線吸収色素が、ポルフィラジン色素又はジイモニウム色素である上記xiiiに記載の分散液。
xv.近赤外線吸収色素が、前記式(1)で表されるポルフィラジン色素である上記xivに記載の分散液。
xvi.前記式(1)で表されるポルフィラジン色素における環A、B、C及びDが、少なくとも一つはピリジン環又はナフタレン環で、残りの環がそれぞれ独立にベンゼン環、ピリジン環及びナフタレン環からなる群から選択される一つである上記xvに記載の分散液。
xvii.前記式(1)で表されるポルフィラジン色素における環A、B、C及びDの4個の環の組み合わせが、ベンゼン環が0~2個で、ナフタレン環が2~4個の範囲で合計が4となる組合わせ又はピリジン環が1~3個及びナフタレン環が1~3個の範囲で、両者の合計が4となる組合わせである上記xviに記載の分散液。
xviii.環A乃至Dがピリジン環とナフタレン環の組合せからなる上記xviiに記載の分散液。
xix.近赤外線吸収色素が、前記式(1)におけるa及びbが0であるポルフィラジン色素である上記xv~xviiiの何れか一項に記載の分散液。
xx.分散液における金属酸化物微粒子が、熱線遮蔽層とされた時、該熱線遮蔽層における、少なくとも2000nmの波長の光での反射率が少なくとも15%であり、且つ、該熱線遮蔽層の表面抵抗が106Ω/□以上となるように分散された上記i~xixの何れか一項に記載の分散液。
xxi.ビーズミルで、周速6m/s~12m/sで分散された上記i~xxの何れか一項に記載の分散液。
下限は特にないが、一般的に達成し得る下限としては5nm程度であり、達成し易さでは10nm程度である。
なお、熱線遮蔽層表面の最大高低差は白色光干渉式表面観察装置(テーラーホブソン製 タリサーフCCI)を用いて、50倍率レンズで、該熱線遮蔽層の全面の任意の1個所を、それぞれ0.3mm×0.3mmの範囲で、最大高さと最大低さを測定して、その中の最大高さと最大低さの差を、熱線遮蔽層表面の最大高低差とした。
ビーズミルを用いた場合、上記の特定なエネルギー領域としては3~12m/sの周速、好ましくは3~11m/sの周速、より好ましくは3~10m/sの周速が適当であり、更に好ましい態様としては、4~12m/sの周速又は4~11m/sの周速を挙げることができ、最も好ましい態様としては、5~12m/sの周速、又は、場合により、5~11m/s又は5~10mの周速を挙げることができる。上記した様に、周速が遅すぎると、微粒子を十分分散できずに、周速があまり早すぎると反射性能の低下で、遮熱性能が低下する。
適正な範囲は用いる装置、バインダー、分散時固形分等によって若干異なるので、上記を参照に適宜調整するのが好ましい。
上記のようにして得られた熱線遮蔽層における可視光透過率は通常50%以上、好ましくは70%以上、より好ましくは80%以上である。また、該熱線遮蔽層におけるヘイズ値は通常8%以下であり、好ましくは5%以下であり、より好ましくは3%以下であり、更に好ましくは2%以下、最も好ましくは1%以下である。ヘイズ値は低い方が好ましく、本発明の好ましい態様では、0.8%以下であり、より好ましい態様では0.5%以下までにすることができる。ヘイズ値の下限は特にないが、0.1%程度までと思われる。
また、本発明の熱線遮蔽シートは、上記の熱線遮蔽層を有すれば、更に、必要に応じて、別の層、例えば近赤外線吸収層や近赤外線反射層を有してもよい。
また、該別の層に、必要に応じ、例えば、紫外線吸収剤、酸化防止剤、光安定剤等の各種添加剤を添加することができる。
さらに目的に応じて熱線遮蔽層の上に粘着層、ハードコート層等の機能性シートを積層させても構わない。
本発明においては、近赤外線の短波長側の光(可視光に近い近赤外線;主として波長780nm~2000nmの光)の遮断には、該熱線遮蔽層に前記の近赤外線吸収色素を含ませることが出来るが、該近赤外線吸収色素を含まない場合、または、該近赤外線吸収色素を含んでも、更に、該短波長側の光を遮蔽したい場合には、上記の熱線遮蔽層とは別に、近赤外線の短波長側の光を主に反射する反射層をもうけるのが好ましい。以下に、該反射層を有する本発明の熱線遮蔽シートについて説明する。
反射層としては、コレステリック液晶層、高屈折率層と低屈折率層の両者の組み合わせを少なくとも一つ有する誘電体多層膜または複屈折多層膜等を挙げることができる。
用いる赤外線選択反射材料は、公知の材料を使用することが出来、電波を透過する材料、つまり導電性がない材料が好ましい。そのような赤外線選択反射材料として、コレステリック(キラル・ネマチック)液晶材料、誘電体多層膜材料(以下誘電体多層構造材料ともいう)、または複屈折多層膜材料(複屈折多層構造材料とも言う)が挙げられ、このうち1種または2種以上を組み合わせて使用できる。
それぞれの光学膜厚(屈折率nと膜厚dとの積nd)は反射させる波長領域の中心波長をλcとすると、λc/4となるように制御されている。高屈折率材料としては酸化チタン、酸化ジルコニウム、酸化セリウム、酸化鉛、酸化亜鉛、酸化ニオブ、酸化タンタル、酸化ハフニウム等が用いられ、低屈折率材料としては、酸化ケイ素、フッ化マグネシウム、フッ化セリウム等が用いられる。
好ましい態様によれば、誘電体多層膜を有する本発明の熱線遮蔽シートにおいては、熱線遮蔽層に、近赤外線吸収色素を含むことなく、可視光透過率70%以上、好ましくは75%以上、更に好ましくは80%以上で、かつ、ヘイズが2%以下、好ましくは1.5%以下、更に好ましくは1%以下で、該熱線遮蔽シート通過後の全日射エネルギー透過率を70%以下、好ましくは、65%以下、より好ましくは55%以下を達成することが出来る。また、必要に応じて、熱線遮蔽層に、近赤外線吸収色素を含ませても良い。
好ましい態様によれば、誘電体多層膜が、高屈折率層と低屈折率層の屈折率差が少なくとも0.3、より好ましくは少なくとも0.4となる材料を交互に積層し、上記の目標値を達成するように積層した誘電多層膜の場合であり、より好ましい対応においては高屈折率層が酸化チタンを含有し、低屈折率層が酸化ケイ素を含有する層であり、3層~11層の間で上記の目標値を達成するように交互に積層された誘電体多層膜である場合である。
式(a)
式(b)
式(a)及び式(b)中、λcは反射させる波長領域の中心波長、noは液晶化合物の短軸方向の屈折率、neは液晶化合物の長軸方向の屈折率、nは(no+ne)/2、θは光の入射角(面法線からの角度)を表す。
本発明で使用する棒状液晶化合物としては、棒状ネマチック液晶化合物である。前記棒状ネマチック液晶化合物の例には、アゾメチン類、アゾキシ類、シアノビフェニル類、シアノフェニルエステル類、安息香酸エステル類、シクロヘキサンカルボン酸フェニルエステル類、シアノフェニルシクロヘキサン類、シアノ置換フェニルピリミジン類、フェニルジオキサン類、トラン類及びアルケニルシクロヘキシルベンゾニトリル類等の低分子液晶化合物および高分子液晶化合物が好ましく用いられる。
重合性基を有しない棒状液晶化合物については、様々な文献(例えば、Y.Goto et.al., Mol.Cryst. Liq. Cryst. 1995, Vol. 260, pp.23-28)に記載がある。
重合性棒状液晶化合物は、重合性基を棒状液晶化合物に導入することにより得られる。重合性基の例には、不飽和重合性基、エポキシ基、及びアジリジニル基が含まれ、不飽和重合性基が好ましく、エチレン性不飽和重合性基が特に好ましい。重合性基は種々の方法で、棒状液晶化合物の分子中に導入できる。重合性棒状液晶化合物が有する重合性基の個数は、好ましくは1~6個、より好ましくは1~3個である。重合性棒状液晶化合物の例は、Makromol.Chem.,190巻、2255頁(1989年)、Advanced Materials 5巻、107頁(1993年)、米国特許第4683327号明細書、同5622648号明細書、同5770107号明細書、国際公開WO95/22586号公報、同95/24455号公報、同97/00600号公報、同98/23580号公報、同98/52905号公報、特開平1-272551号公報、同6-16616号公報、同7-110469号公報、同11-80081号公報、及び特開2001-328973号公報などに記載の化合物が含まれる。2種類以上の重合性棒状液晶化合物を併用してもよい。2種類以上の重合性棒状液晶化合物を併用すると、配向温度を低下させることができる。
前記液晶組成物は、コレステリック液晶相を示すものであり、そのためには、光学活性化合物を含有しているのが好ましい。ただし、上記棒状液晶化合物が不斉炭素原子を有する分子である場合には、光学活性化合物を添加しなくても、コレステリック液晶相を安定的に形成可能である場合もある。前記光学活性化合物は、公知の種々のキラル剤(例えば、液晶デバイスハンドブック、第3章4-3項、TN、STN用カイラル剤、199頁、日本学術振興会第142委員会編、1989に記載)から選択することができる。光学活性化合物は、一般に不斉炭素原子を含むが、不斉炭素原子を含まない軸性不斉化合物あるいは面性不斉化合物もカイラル剤として用いることができる。軸性不斉化合物または面性不斉化合物の例には、ビナフチル、ヘリセン、パラシクロファン及びこれらの誘導体が含まれる。光学活性化合物(キラル剤)は、重合性基を有していてもよい。光学活性化合物が重合性基を有するとともに、併用する棒状液晶化合物も重合性基を有する場合は、重合性光学活性化合物と重合性棒状液晶化合物との重合反応により、棒状液晶化合物から誘導される繰り返し単位と、光学活性化合物から誘導される繰り返し単位とを有するポリマーを形成することができる。この態様では、重合性光学活性化合物が有する重合性基は、重合性棒状液晶化合物が有する重合性基と、同種の基であることが好ましい。したがって、光学活性化合物の重合性基も、不飽和重合性基、エポキシ基又はアジリジニル基であることが好ましく、不飽和重合性基であることがさらに好ましく、エチレン性不飽和重合性基であることが特に好ましい。
また、光学活性化合物は、液晶化合物であってもよい。
前記光反射層の形成に用いる液晶組成物は、重合性液晶組成物であるのが好ましく、そのためには、重合開始剤を含有しているのが好ましい。本発明では、紫外線照射により硬化反応を進行させるので、使用する重合開始剤は、紫外線照射によって重合反応を開始可能な光重合開始剤であるのが好ましい。上記光重合開始剤は特に限定されず、例えば、2-メチル-1-[4-(メチルチオ)フェニル]-2-モルホリノプロパン-1-オン(チバスペシャリティーケミカルズ社製「イルガキュアー(登録商標)(以下同じ)907」)、1-ヒドロキシシクロヘキシルフェニルケトン(チバスペシャリティーケミカルズ社製「イルガキュアー184」)、4-(2-ヒドロキシエトキシ)-フェニル(2-ヒドロキシ-2-プロピル)ケトン(チバスペシャリティーケミカルズ社製「イルガキュアー2959」)、1-(4-ドデシルフェニル)-2-ヒドロキシ-2-メチルプロパン-1-オン(メルク社製「ダロキュアー(登録商標)(以下同じ)953」)、1-(4-イソプロピルフェニル)-2-ヒドロキシ-2-メチルプロパン-1-オン(メルク社製「ダロキュアー1116」)、2-ヒドロキシ-2-メチル-1-フェニルプロパン-1-オン(チバスペシャリティーケミカルズ社製「イルガキュアー1173」)、ジエトキシアセトフェノン等のアセトフェノン化合物、ベンゾイン、ベンゾインメチルエーテル、ベンゾインエチルエーテル、ベンゾインイソプロピルエーテル、ベンゾインイソブチルエーテル、2,2-ジメトキシ-2-フェニルアセトフェノン(チバスペシャリティーケミカルズ社製「イルガキュアー651」)等のベンゾイン化合物、ベンゾイル安息香酸、ベンゾイル安息香酸メチル、4-フェニルベンゾフェノン、ヒドロキシベンゾフェノン、4-ベンゾイル-4 ’-メチルジフェニルサルファイド、3,3 ’-ジメチル-4-メトキシベンゾフェノン(日本化薬株式会社製「カヤキュアー(登録商標)(以下同じ)MBP」)等のベンゾフェノン化合物、チオキサントン、2-クロルチオキサントン(日本化薬株式会社製「カヤキュアーCTX」)、2-メチルチオキサントン、2,4-ジメチルチオキサントン(日本化薬株式会社製「カヤキュアーRTX」)、イソプロピルチオキサントン、2,4-ジクロロチオキサントン(日本化薬株式会社製「カヤキュアーCTX」)、2,4-ジエチルチオキサントン(日本化薬株式会社製「カヤキュアーDETX」)、2,4-ジイソプロピルチオキサントン(日本化薬株式会社製「カヤキュアーDITX」)等のチオキサントン化合物等が挙げられる。これらの光重合開始剤は、単独で用いられてもよいし、2種以上が併用されてもよい。
また、上記反応助剤の含有量は、上記光重合開始剤の含有量に対して、0.5~2倍量であることが好ましい。
コレステリック液晶層は少なくとも1層有すればよいが、通常複数のコレステリック液晶層を有する方が好ましく、通常少なくとも2層、好ましくは2~8層程度有するのが好ましい。複数のコレステリック液晶層の組み合わせは分子軸のねじれ方向が異なる少なくとも2種のコレステリック液晶層を組み合わせるかまたは/及びピッチ長の異なるコレステリック液晶層を組み合わせる等何れでもよい。
コレステリック液晶層を有する本発明の熱線遮蔽シートの好ましい態様としては、支持体上に少なくとも1層、好ましくは少なくとも2層、より好ましくは2~8層のコレステリック液晶層を有し、該液晶層上に前記熱線遮蔽層を有する態様である。より好ましくは、コレステリック液晶層が重合性液晶組成物(好ましくは光重合性液晶組成物、より好ましくは、光重合性棒状液晶化合物を含む光重合性液晶組成物、又は、更に、キラル剤を含む光重合性液晶組成物)の重合物層からなる態様である。
上記熱線遮蔽層は、近赤外線吸収色素を含まない態様、または、それを含む態様の何れでもよい。
上記のコレステリック液晶層を有する本発明の熱線遮蔽シートの好ましい態様においては、可視光透過率を70%以上、好ましくは75%以上、ヘイズ値が2%以下、好ましくは1.5%以下、より好ましくは1%以下、後記する全日射エネルギー透過率が、65%以下、より好ましくは60%以下とすることが出来る。特に、前記熱線遮蔽層として、近赤外線吸収色素を含む熱線遮蔽層を使用した場合には、可視光透過率が上記の好ましい又はより好ましい値であり、且つ、全日射エネルギー透過率を、60%以下、好ましくは55%以下、最も好ましい態様においては50%以下とすることが出来る。この場合、近赤外線吸収色素としては、先に挙げた好ましいポルフィラジン色素が好ましく、先に挙げた好ましい、またはより好ましいポルフィラジン色素がより好ましい。
反射層としては、誘電体多層膜またはコレステリック液晶層がより好ましい。
平均粒径25.6nm、粉体抵抗0.8Ω・cmであった錫含有酸化インジウム(商品名;ITO-R、CIKナノテック株式会社製)(以下、ITOという;)1.4部、KAYARAD DPHA(商品名、ジペンタエリスリトールヘキサアクリレート、日本化薬株式会社製)0.1部、イルガキュア184(ラジカル性光重合開始剤、BASFジャパン株式会社製)0.01部、アミノアルキルメタクリレート共重合体分散剤(商品名、Disper BYK140、ビックケミージャパン株式会社製)0.1部をトルエン7部中に加え、ビーズミルを用いて周速10m/sにて分散させ分散液を作製した。作製した分散液をポリエチレンテレフタレート(PET)シート(基材)(厚さ100μm)にワイヤーバーにて、乾燥後の厚さが500nmとなるように塗布し、100℃、2分間乾燥させトルエンを蒸発させた後、UV照射によって熱線遮蔽シートを作製した。
作製した熱線遮蔽シートの上に粘着剤を塗布し、粘着シートにした後、3mmクリアガラスに貼合し、熱線遮蔽ガラスを作製した。
KAYARAD DPHAを0.3部に変更した以外は実施例1と同様にして熱線遮蔽シートを作製した。
ビーズミルの周速を5m/sに変更した以外は実施例1と同様にして熱線遮蔽シートを作製した。
ITO28部、アクリル共重合体樹脂(ダイヤナールレジンBR-116 三菱化学製)12部をキシレン30部、トルエン20部、エタノール10部中に加え、ビーズミルを用いて周速10m/sにて分散させ分散液を作製した。作製した分散液をPET基材にワイヤーバーにて、乾燥後の厚さが500nmとなるように塗布し、140℃、2分間乾燥させて熱線遮蔽シートを作製した。
ITOの分散の仕方での反射率及びヘイズ等の相違を見るため、ITOの濃度等は、実施例1と全く同一とし、ビーズミルの周速のみを2m/sに変更し、実施例1と同様にして熱線遮蔽シートを作製した。
ITO濃度での性能の違いを見るため、KAYARAD DPHAを1.3部に変更した以外は実施例1と同様にして熱線遮蔽シートを作製した。
また、実施例1と同様に、作製した熱線遮蔽シートの上に粘着剤を塗布し、粘着シートにした後、3mmクリアガラスに貼合し、熱線遮蔽ガラスを作製した。
高エネルギーでの分散の影響を調べるため、ビーズミル周速を14m/sに変更した以外は実施例2と同様にして熱線遮蔽シートを作製した。
(可視光透過率の測定)
分光光度計(株式会社島津製作所製 UV-3100)を用いて、JIS R3106に準拠して、得られた熱線遮蔽シートの波長380nm~780nmにおける上記可視光透過率を測定した。
(近赤外反射率の測定)
分光光度計(株式会社島津製作所製 UV-3100)を用いて、JIS R3106に準拠して、得られた熱線遮蔽シートの300nm~2500nmにおける正反射率を測定した。
(ヘイズ値の測定)
ヘーズメーター(有限会社東京電色製 TC-HIIIDPK)を用いて、JIS K6714に準拠して、得られた熱線遮蔽シートのヘイズ値を測定した。
(表面抵抗の測定)
表面抵抗計(株式会社三菱化学アナリテック製 ハイレスターUP、ロレスターGP)を用いて測定した。
(層表面の最大高低差)
白色光干渉式表面観察装置(テーラーホブソン製 タリサーフCCI)を用いて、50倍率レンズで0.3mm×0.3mmの範囲での最大高さと最大低さの差を測定した。
試験環境:
試験環境:内径幅150mm×長さ235mm×高さ110mmの外気温遮断性と気密性とを有し、天井部が透明ガラスの試験箱の天井中央部の外側に、天井部から高さ40cmの位置になるように、赤外ランプ(100V、250W:東芝株式会社)を設置し、次に試験箱天井部内側に、作製した熱線遮蔽ガラスを、ガラス面が赤外線ランプ側になるように設置し、四方をテープで貼り付け固定した。また、ランプの光が直接当たらないようこの試験箱内部の中央部と、箱の内側にある熱線遮蔽ガラス面に温度計を設置した。その後、ランプを点灯し、熱線遮蔽ガラスに赤外線を照射した。温度を10秒ごとに測定し、60分後の試験箱内温度を測定した。なお、上記試験箱は25℃程度の部屋に設置した。
この試験において比較例2で作成した熱線遮蔽ガラスと実施例1の熱線遮蔽ガラスをそれぞれ用いた時の箱内温度を比較し、本発明の熱線遮蔽ガラスを用いた箱内温度及びシート表面温度のそれぞれが低ければ、熱線遮蔽効果が向上していることになる。
なお、箱内温度差の計算方法は実施例1で作製した熱線遮蔽ガラスを用いた箱内温度及び表面温度のそれぞれから、比較例2の熱線遮蔽ガラスを用いた箱内温度及び表面温度のそれぞれを差し引くことにより導かれる。
スルホラン120部にナフタル酸無水物15.9部、尿素29部、モリブデン酸アンモニウム0.40部及び塩化バナジル(V)3.5部加え、200℃まで昇温し、同温度で11時間反応させた。反応終了後65℃まで冷却し、N,N-ジメチルホルムアミド(DMF)100部加え、析出固体をろ過分離した。得られた固体をDMF50部で洗浄し、ウェットケーキ20.3部得た。得られたウェットケーキをDMF100部に加え、80℃に昇温し、同温度で2時間撹拌した。析出固体をろ過分離し、水200部で洗浄しウェットケーキを18.9部得た。得られたウェットケーキを水150部に加え、90℃に昇温し、同温度で2時間撹拌した。析出固体をろ過分離し、水200部で洗浄してウェットケーキ16.1部を得た。得られたウェットケーキを80℃で乾燥し、前記表1No.25を12.3部得た。
合成例1のナフタル酸無水物15.9部を11.9部にし、フタル酸無水物3.0部加えた以外は合成例1同様にして、前記表1No.1を12.3部得た。
合成例2のフタル酸無水物3.0部を5.9部に、ナフタル酸無水物11.9部を7.9部にする以外は合成例2と同様にして、前記表1No.2を12.1部得た。
スルホラン120部に3,4-ピリジンジカルボン酸3.3部、ナフタル酸無水物7.9部、尿素29部、モリブデン酸アンモニウム0.40部及び塩化バナジル(V)3.5部加え、200℃まで昇温し、同温度で11時間反応させた。反応終了後65℃まで冷却し、N,N-ジメチルホルムアミド(DMF)100部加え、析出固体をろ過分離した。得られた固体を80℃のDMF200部で洗浄し、ウェットケーキ20.3部得た。得られたウェットケーキをDMF100部に加え、80℃に昇温し、同温度で2時間撹拌した。析出固体をろ過分離し、水200部で洗浄しウェットケーキを40.1部得た。得られたウェットケーキを水150部に加え、90℃に昇温し、同温度で2時間撹拌した。析出固体をろ過分離し、水7.9部で洗浄してウェットケーキ35.2部を得た。得られたウェットケーキを80℃で乾燥し、前記表1No.9を10.8部得た。
合成例4の3,4-ピリジンジカルボン酸3.3部を6.7部に、ナフタル酸無水物11.9部を7.9部にする以外は合成例4と同様にして、前記表1No.8を11.4部得た。
ポリリン酸(116%)40部中に、合成例2で得られた化合物No.1を3.4部、フタルイミド4.9部、パラホルムアルデヒド1.0部加え、140℃に昇温し、同温度で6時間反応させた。反応終了後、60℃まで冷却し、水100部を加えた。析出固体をろ過分離、水洗してウェットケーキを34.0部得た。
得られたウェットケーキを10%水酸化カリウム水溶液100部に加え、50℃で2時間反応させた。析出固体をろ過分離し、水洗してウェットケーキ29部を得た。
得られたウェットケーキをDMF100部に加え、25℃で反応させた。析出固体をろ過分離し、水洗してウェットケーキを13.3部得た。得られたウェットケーキを80℃で乾燥し、前記表1No.3を6.5部得た。
実施例1に記載の錫含有酸化インジウム(以下、ITO)1.4部、合成例1で得た化合物(近赤外線吸収色素)0.1部、KAYARAD DPHA(商品名、ジペンタエリスリトールヘキサアクリレート、日本化薬株式会社製)0.1部、イルガキュア184(光重合開始剤、BASFジャパン社製)0.01部、アミノアルキルメタクリレート共重合体分散剤0.1部をトルエン7部中に加え、ビーズミルを用いて周速10m/sにて分散させ分散液を作製した。作製した分散液をPET基材(コスモシャインA4100、東洋紡株式会社製)にワイヤーバーにて塗布し、100℃、2分間乾燥させトルエンを蒸発させた後、UV照射によって熱線遮蔽シートを作製した。熱線遮蔽シートの後記全日射エネルギー透過率(Tts)は53.5%であった。
作製した熱線遮蔽シートの上に粘着剤(コーポニール N-2147、日本合成化学工業株式会社製)を塗布し、粘着シートにした後、3mmクリアガラスに貼合し、本発明の熱線遮蔽ガラスを作製した。
実施例5の色素をそれぞれ、合成例2~5で得られた化合物に変更した以外は実施例5と同様にして、合成例2~5で得られた化合物をそれぞれ含む本発明の熱線遮蔽シートを作製した(それぞれを順に実施例6~9とする)。
KAYARAD DPHAを0.3部に変更した以外は実施例5と同様にして本発明の熱線遮蔽シートを作製した。
ビーズミルの周速を5m/sに変更した以外は実施例5と同様にして本発明の熱線遮蔽シートを作製した。得られた熱線遮蔽シートの後記全日射エネルギー透過率(Tts)は55.1%であった。
(コレステリック液晶積層体の作製)
LC-242(光重合性液晶化合物、BASF社製)10部、LC-756(キラル剤、BASF社製)0.30部、ルシリンTPO(光重合開始剤、BASF社製)0.51部をシクロペンタノン25部中で溶解させ、塗布液1を調製した。また、LC-242(光重合性液晶化合物、BASF社製)10部、LC-756(キラル剤、BASF社製)0.26部、ルシリンTPO(光重合開始剤、BASF社製)0.51部をシクロペンタノン25部中で溶解させ、塗布液2を調製した。調製した塗布液1をPET基材(コスモシャインA4100、東洋紡株式会社製)にワイヤーバーにて乾燥後膜厚7μmになる様に塗布し、150℃、5分間乾燥させシクロペンタノンを蒸発させた後、UV照射によって硬化させた。さらに塗布液1と同様して塗布液2を塗布、乾燥、UV照射によってコレステリック液晶積層体を作製した。
(本発明のコレステリック液晶層を有する熱線遮蔽シートの作製)
作製したコレステリック液晶積層体上に実施例5と同様にして作製した分散液をワイヤーバーにて乾燥後膜厚500nmになる様に塗布し、100℃、2分間乾燥させトルエンを蒸発させた後、UV照射によって本発明のコレステリック液晶層を有する熱線遮蔽シートを作製した。得られた熱線遮蔽シートの後記全日射エネルギー透過率(Tts)は51.8%であった。
ITOの分散の仕方での反射率及びヘイズ等の相違を見るため、ITOの濃度等は、実施例5と全く同一とし、ビーズミルの周速のみを2m/sに変更し、実施例5と同様にして比較用の熱線遮蔽シートを作製した。
ITO濃度での性能の違いを見るため、実施例1のKAYARAD DPHAを1.3部に変更した以外は実施例5と同様にして比較用の熱線遮蔽シートを作製した。
また、作製した熱線遮蔽シートの上に粘着剤を塗布し、粘着シートにした後、3mmクリアガラスに貼合し、実施例5と同様に、熱線遮蔽ガラスを作製した。
高エネルギーでの分散の影響を調べるため、ビーズミル周速を14m/sに変更した以外は実施例10と同様にして比較用の熱線遮蔽シートを作製した。
(可視光透過率の測定)
分光光度計(株式会社島津製作所製 UV-3100)を用いて、JIS R3106に準拠して、得られた熱線遮蔽シートの波長380~780nmにおける上記可視光透過率を測定した。
(近赤外線反射率の測定)
分光光度計(株式会社島津製作所製 UV-3100)を用いて、JIS R3106に準拠して、得られた熱線遮蔽シートの300nm~2500nmにおける正反射率を測定した。
(ヘイズ値の測定)
ヘーズメーター(有限会社東京電色製 TC-HIIIDPK)を用いて、JIS K6714に準拠して、得られた熱線遮蔽シートのヘイズ値を測定した。
(表面抵抗の測定)
表面抵抗計(株式会社三菱化学アナリテック製 ハイレスターUP、ロレスターGP)を用いて測定した。
(層表面の最大高低差)
白色光干渉式表面観察装置(テーラーホブソン製 タリサーフCCI)を用いて、50倍率レンズで0.3mm×0.3mmの範囲での最大高さと最大低さとの差を測定した。
試験環境:内径幅150mm×長さ235mm×高さ110mmの外気温遮断性と気密性とを有し、天井部が透明ガラスの試験箱の天井中央部の外側に、天井部から高さ40cmの位置になるように、赤外ランプ(100V、250W:東芝株式会社)を設置し、次に試験箱天井部内側に作製した熱線遮蔽ガラスを、ガラス面が赤外線ランプ側になるように設置し、四方をテープで貼り付け固定した。また、ランプの光が直接当たらないようこの試験箱内部の中央部と、箱の内側にある熱線遮蔽ガラス面に温度計を設置した。その後、ランプを点灯し、熱線遮蔽ガラスに赤外線を照射した。温度を10秒ごとに測定し、60分後の試験箱内温度を測定した。なお、上記試験箱は25℃程度の部屋に設置した。
この試験において比較例5で作製した熱線遮蔽ガラスと実施例5の熱線遮蔽ガラスをそれぞれ用いた時の箱内温度を比較し、本発明の熱線遮蔽ガラスを用いた箱内温度、シート表面温度が低ければ、熱線遮蔽効果が向上していることになる。 なお、箱内温度差の計算方法は、実施例5で作製した熱線遮蔽ガラスを用いた箱内温度及び表面温度のそれぞれから、比較例5の熱線遮蔽ガラスを用いた箱内温度及び表面温度のそれぞれを差し引くことにより導かれる。
比較例6では表面抵抗等の要件は満たしているが、分散エネルギーが高い為、導電性微粒子表面が傷つけられた結果、近赤外線反射性能が発現していない。
(誘電体多層膜)
・高屈折率層分散液の調製
酸化チタン(商品名:TTO-V3、石原産業株式会社製)1.4部、KAYARAD DPHA(商品名、ジペンタエリスリトールヘキサアクリレート、日本化薬株式会社製)0.1部、イルガキュア184(ラジカル性光重合開始剤、BASFジャパン株式会社製)0.01部、アミノアルキルメタクリレート共重合体分散剤(商品名、Disper BYK145、ビックケミージャパン株式会社製)0.1部をトルエン7部中に加え、ビーズミルを用いて周速10m/sにて分散させ高屈折率層分散液を作製した。
・低屈折率層分散液の調製
酸化ケイ素微粒子分散液(固形分濃度:20wt%、商品名:MEK-ST、日産化学工業株式会社製)7部、KAYARAD DPHA(商品名、ジペンタエリスリトールヘキサアクリレート、日本化薬株式会社製)0.1部、イルガキュア184(ラジカル性光重合開始剤、BASFジャパン株式会社製)0.01部を加え、低屈率層分散液を作製した。
・誘電体多層膜の作製
作製した高屈折率分散液をポリエチレンテレフタレート(PET)シート(基材)(厚さ100μm)にワイヤーバーにて、乾燥後の光学膜厚が250nmとなるように塗布し、100℃、2分間乾燥させた後、UV照射によって高屈折率層を作製した。前記高屈折率層の上に低屈折率層分散液を同様に、乾燥後の光学膜厚が250nmとなるよう塗布、乾燥、UV照射によって低屈折率層を作製した。
高屈折率層と低屈折率層が交互に重なる様、上記操作を行い、9層積層させた誘電体多層膜を作製した。
(熱線遮蔽シートの作製)
実施例1に記載の錫含有酸化インジウム(以下、ITO)1.4部、KAYARAD DPHA(商品名、ジペンタエリスリトールヘキサアクリレート、日本化薬株式会社製)0.1部、イルガキュアー184(光重合開始剤、BASFジャパン株式会社製)0.01部、アミノアルキルメタクリレート共重合体分散剤0.1部をトルエン7部中に加え、ビーズミルを用いて周速10m/sにて分散させ分散液を作製した。
作製した分散液を前記作製した誘電体多層膜上にワイヤーバーにて塗布し、100℃、2分間乾燥させトルエンを蒸発させた後、UV照射によって本発明の熱線遮蔽シートを作製した。
(コレステリック液晶積層体の作製)
LC-242(液晶化合物、BASF社製)10部、LC-756(キラル剤、BASF社製)0.38部、ルシリンTPO(光重合開始剤、BASF社製)0.52部をシクロペンタノン25部中で溶解させ、塗布液1を調製した。また、LC-242(液晶化合物、BASF社製)10部、LC-756(キラル剤、BASF社製)0.30部、ルシリンTPO(光重合開始剤、BASF社製)0.51部をシクロペンタノン25部中で溶解させ、塗布液2を調製した。また、LC-242(液晶化合物、BASF社製)10部、LC-756(キラル剤、BASF社製)0.26部、ルシリンTPO(光重合開始剤、BASF社製)0.51部をシクロペンタノン25部中で溶解させ、塗布液3を調製した。
調製した塗布液1をPET基材(コスモシャインA4100、東洋紡株式会社製)にワイヤーバーにて塗布し、150℃、5分間乾燥させシクロペンタノンを蒸発させた後、UV照射によって硬化させた。さらに塗布液1と同様して塗布液2、3を順次塗布、乾燥、UV照射を繰り返すことによってコレステリック液晶積層体を作製した。
(熱線遮蔽シートの作製)
作製したコレステリック液晶積層体上に実施例13と同様にして作製した分散液をワイヤーバーにて塗布し、100℃、2分間乾燥させトルエンを蒸発させた後、UV照射によって本発明の熱線遮蔽シートを作製した。
また、作製した熱線遮蔽シートの上に粘着剤を塗布し、粘着シートにした後、3mmクリアガラスに貼合し、熱線遮蔽ガラスを作製した。
誘電体多層膜をナノ90S(住友スリーエム株式会社製、複屈折率多層膜)に変更した以外は実施例13と同様にして本発明の熱線遮蔽シートを作製した。
KAYARAD DPHAを0.3部に変更した以外は実施例13と同様にして本発明の熱線遮蔽シートを作製した。
ビーズミルの周速を5m/sに変更した以外は実施例13と同様にして本発明の熱線遮蔽シートを作製した。
KAYARAD DPHAを1.3部に変更した以外は実施例14と同様にして比較用の熱線遮蔽シートを作製した。また、作製した熱線遮蔽シートの上に粘着剤を塗布し、粘着シートにした後、3mmクリアガラスに貼合し、熱線遮蔽ガラスを作製した。
(可視光透過率の測定)
分光光度計(株式会社島津製作所製 UV-3100)を用いて、JIS R3106に準拠して、得られた熱線遮蔽シートの波長380nm~780nmにおける上記可視光透過率を測定した。
(全日射エネルギー透過率(Tts)の測定)
全日射エネルギー透過率(Tts;Total Solar Transmittance)は太陽からの熱的エネルギーのうち、対象となる材料をどの程度透過するかという尺度であり、分光光度計(株式会社島津製作所製 UV-3100)を用いて、JIS R3106に準拠して、上記得られた熱線遮蔽シートの300nm~2500nmにおける透過率、反射率を測定したデータに基づき、ISO13837に定義されている計算式にて算出した。
算出された数値が小さいほど透過された全日射エネルギーが小さいことを示し、熱線遮蔽性が高いことを示す。
(ヘイズ値の測定)
ヘーズメーター(有限会社東京電色製 TC-HIIIDPK)を用いて、JIS K6714に準拠して、得られた熱線遮蔽シートのヘイズ値を測定した。
(表面抵抗の測定)
表面抵抗計(株式会社三菱化学アナリテック製 ハイレスターUP、ロレスターGP)を用いて測定した。
白色光干渉式表面観察装置(テーラーホブソン製 タリサーフCCI)を用いて、50倍率レンズで0.3mm×0.3mmの範囲での最大高さと最大低さとの差を測定した。
(遮熱効果)
試験環境:内径幅150mm×長さ235mm×高さ110mmの外気温遮断性と気密性とを有し、天井部が透明ガラスの試験箱の天井中央部の外側に、天井部から高さ40cmの位置になるように、赤外ランプ(100V、250W:東芝株式会社)を設置し、次に試験箱天井部内側に作製した熱線遮蔽ガラスを、ガラス面が赤外線ランプ側になるように設置し、四方をテープで貼り付け固定した。また、ランプの光が直接当たらないようこの試験箱内部の中央部と、箱の内側にある熱線遮蔽ガラス面に温度計を設置した。その後、ランプを点灯し、熱線遮蔽ガラスに赤外線を照射した。温度を10秒ごとに測定し、60分後の試験箱内温度を測定した。なお、上記試験箱は25℃程度の部屋に設置した。
この試験において比較例7で作成した熱線遮蔽ガラスと実施例14の熱線遮蔽ガラスをそれぞれ用いた時の箱内温度を比較し、本発明の熱線遮蔽ガラスを用いた箱内温度及びシート表面温度のそれぞれが低ければ、熱線遮蔽効果が向上していることになる。
なお、箱内温度差の計算方法は実施例14で作製した熱線遮蔽ガラスを用いた箱内温度及び表面温度のそれぞれから比較例7の熱線遮蔽ガラスを用いた箱内温度及び表面温度のそれぞれを差し引くことにより導かれる。
11は本発明の熱線遮蔽層、12は支持体、13は反射層を示す。
Claims (21)
- 支持体の上に、平均粒径100nm以下の微粒子と空隙部分を埋める樹脂バインダーとを含有する熱線遮蔽層を有し、該熱線遮蔽層における、少なくとも2000nmの波長での反射率が少なくとも15%であり、且つ該熱線遮蔽層の表面抵抗が106Ω/□以上である熱線遮蔽シート。
- 熱線遮蔽層表面の最大高低差が60nm以下である請求項1に記載の熱線遮蔽シート。
- 熱線遮蔽層のヘイズが3%以下である請求項1または2に記載の熱線遮蔽シート。
- 用いる微粒子の粉体抵抗が10Ω・cm以下である請求項1乃至3の何れか一項に記載の熱線遮蔽シート。
- 微粒子が酸化錫、酸化インジウム、酸化亜鉛、及び酸化タングステンからなる群から選ばれる少なくとも一種の微粒子である請求項1乃至4の何れか一項に記載の熱線遮蔽シート。
- 微粒子が錫ドープ酸化インジウムである請求項1及至5の何れか一項に記載の熱線遮蔽シート。
- 熱線遮蔽シートにおいて、微粒子の含有率が60~95重量%である請求項1乃至6の何れか一項に記載の熱線遮蔽シート。
- 熱線遮蔽層の可視光線透過率が70%以上である請求項1乃至7の何れか一項に記載の熱線遮蔽シート。
- 微粒子が導電性微粒子であり、熱線遮蔽層が、更に、近赤外線吸収色素を含み、該近赤外線吸収色素が樹脂バインダー中に分散している請求項1~7の何れか一項に記載の熱線遮蔽シート。
- 熱線遮蔽層とは別に、更に、近赤外線吸収色素を含む色素層を含む請求項1~7の何れか一項に記載の熱線遮蔽シート。
- 可視光透過率が50%以上、ヘイズが3%以下であることを特徴とする請求項9又は10に記載の熱線遮蔽シート。
- 近赤外線吸収色素としてポルフィラジン色素、またはジイモニウム色素を含む請求項9~11の何れか一項に記載の熱線遮蔽シート。
- ポルフィラジン色素として、下記式(1)
[式(1)中、Mは金属原子、金属酸化物、金属水酸化物、若しくは金属ハロゲン化物、又は水素原子を表し、環A、B、C及びDの破線部は、それぞれ独立に、下記式(2)~(8)
の何れか一つの構造であり、開口部で、骨格構造へ結合して、芳香環を形成し、Xは低級アルキル基、低級アルコキシ基、アミノ基、ニトロ基、ハロゲン基、ヒドロキシ基、カルボキシ基、スルホン酸基、又はスルホンアミド基を表し、Yは二価の架橋基を、Zはスルホン酸基、カルボキシ基、第1又は2級アミンの窒素原子上の水素の少なくとも1つを除いた残基、酸アミド基、又は窒素原子を含む複素環の窒素原子上の水素の少なくとも1つを除いた残基を表し、a及びbは、それぞれの基の数を表し、いずれも平均値であり、それぞれ独立に0以上12以下であり、かつ、aとbとの和は0以上12以下である]
で表されるポルフィラジン色素を含む請求項9~12の何れか一項に記載の熱線遮蔽シート。 - 式(1)中の環A、B、C及びDがそれぞれ独立に式(2)、式(4)または式(8)の何れかである請求項13に記載の熱線遮蔽シート。
- 式(1)中のMはVOまたはCuである請求項13又は14に記載の熱線遮蔽シート。
- 式(1)中、Yは炭素数1~3のアルキレン基であり、Zは置換基を有してもよいフタルイミド基又は置換基を有してもよいピペラジノ基である請求項13~15の何れか一項に記載の熱線遮蔽シート。
- 更に、電波透過性を有し、且つ、780~2000nmの波長域の少なくともいずれかの波長の光を反射する反射層を含む請求項9~17の何れか一項に記載の熱線遮蔽シート。
- 反射層が少なくとも1つのコレステリック液晶層、誘電体多層膜及び複屈折多層膜からなる群から選ばれる少なくとも一つである請求項18に記載の熱線遮蔽シート。
- 反射層が少なくとも1つのコレステリック液晶層である請求項19に記載の熱線遮蔽シート。
- 樹脂バインダーが熱または光硬化性樹脂の硬化物または熱可塑性樹脂である請求項1~20の何れか一項に記載の熱線遮蔽シート。
Priority Applications (3)
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US14/436,188 US20150285972A1 (en) | 2012-10-19 | 2013-10-18 | Heat-Ray-Shielding Sheet |
EP13847359.0A EP2910985B1 (en) | 2012-10-19 | 2013-10-18 | Heat-ray-shielding sheet |
JP2014541956A JP6276695B2 (ja) | 2012-10-19 | 2013-10-18 | 熱線遮蔽シート |
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JP2012-231814 | 2012-10-19 | ||
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JP2012-269388 | 2012-12-10 | ||
JP2013-022952 | 2013-02-08 | ||
JP2013022952 | 2013-02-08 |
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US (1) | US20150285972A1 (ja) |
EP (1) | EP2910985B1 (ja) |
JP (1) | JP6276695B2 (ja) |
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Also Published As
Publication number | Publication date |
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EP2910985B1 (en) | 2019-05-08 |
JP6276695B2 (ja) | 2018-02-07 |
JPWO2014061279A1 (ja) | 2016-09-05 |
TW201429711A (zh) | 2014-08-01 |
EP2910985A4 (en) | 2016-06-01 |
US20150285972A1 (en) | 2015-10-08 |
EP2910985A1 (en) | 2015-08-26 |
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