WO2015046245A1 - Optical laminate - Google Patents
Optical laminate Download PDFInfo
- Publication number
- WO2015046245A1 WO2015046245A1 PCT/JP2014/075276 JP2014075276W WO2015046245A1 WO 2015046245 A1 WO2015046245 A1 WO 2015046245A1 JP 2014075276 W JP2014075276 W JP 2014075276W WO 2015046245 A1 WO2015046245 A1 WO 2015046245A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- hard coat
- coat layer
- meth
- resin film
- thermoplastic resin
- Prior art date
Links
- 230000003287 optical effect Effects 0.000 title claims abstract description 84
- 239000010410 layer Substances 0.000 claims abstract description 172
- 229920005992 thermoplastic resin Polymers 0.000 claims abstract description 85
- 239000010419 fine particle Substances 0.000 claims abstract description 61
- 150000001875 compounds Chemical class 0.000 claims abstract description 50
- 239000011254 layer-forming composition Substances 0.000 claims abstract description 31
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 39
- 239000004925 Acrylic resin Substances 0.000 claims description 38
- 229920000178 Acrylic resin Polymers 0.000 claims description 38
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 35
- 239000000203 mixture Substances 0.000 claims description 27
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000005191 phase separation Methods 0.000 claims description 10
- 230000007423 decrease Effects 0.000 claims description 9
- 230000008595 infiltration Effects 0.000 claims description 4
- 238000001764 infiltration Methods 0.000 claims description 4
- 230000003247 decreasing effect Effects 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 description 30
- 239000011347 resin Substances 0.000 description 30
- KNCYXPMJDCCGSJ-UHFFFAOYSA-N piperidine-2,6-dione Chemical group O=C1CCCC(=O)N1 KNCYXPMJDCCGSJ-UHFFFAOYSA-N 0.000 description 29
- 238000000034 method Methods 0.000 description 21
- 238000010438 heat treatment Methods 0.000 description 19
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000047 product Substances 0.000 description 14
- 239000011247 coating layer Substances 0.000 description 13
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 13
- 239000000178 monomer Substances 0.000 description 13
- 239000002245 particle Substances 0.000 description 13
- -1 polyethylene Polymers 0.000 description 13
- 230000009477 glass transition Effects 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 12
- 230000035515 penetration Effects 0.000 description 12
- 239000002904 solvent Substances 0.000 description 12
- 238000001228 spectrum Methods 0.000 description 12
- 125000004432 carbon atom Chemical group C* 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 11
- 239000001257 hydrogen Substances 0.000 description 11
- 239000006096 absorbing agent Substances 0.000 description 10
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- 239000000654 additive Substances 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 9
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 8
- 238000001125 extrusion Methods 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
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- 238000002834 transmittance Methods 0.000 description 6
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 5
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 5
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 239000003999 initiator Substances 0.000 description 5
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 5
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- BGTOWKSIORTVQH-UHFFFAOYSA-N cyclopentanone Chemical compound O=C1CCCC1 BGTOWKSIORTVQH-UHFFFAOYSA-N 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000004973 liquid crystal related substance Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 125000005442 diisocyanate group Chemical group 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 150000002596 lactones Chemical group 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000000149 penetrating effect Effects 0.000 description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920000193 polymethacrylate Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 239000011342 resin composition Substances 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 2
- QQZOPKMRPOGIEB-UHFFFAOYSA-N 2-Oxohexane Chemical compound CCCCC(C)=O QQZOPKMRPOGIEB-UHFFFAOYSA-N 0.000 description 2
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 2
- ZPVFWPFBNIEHGJ-UHFFFAOYSA-N 2-octanone Chemical compound CCCCCCC(C)=O ZPVFWPFBNIEHGJ-UHFFFAOYSA-N 0.000 description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
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- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
- 150000008065 acid anhydrides Chemical class 0.000 description 2
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- 239000012298 atmosphere Substances 0.000 description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 2
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- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
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- 125000000753 cycloalkyl group Chemical group 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 2
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/10—Interconnection of layers at least one layer having inter-reactive properties
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/113—Anti-reflection coatings using inorganic layer materials only
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B27/00—Optical systems or apparatus not provided for by any of the groups G02B1/00 - G02B26/00, G02B30/00
- G02B27/02—Viewing or reading apparatus
- G02B27/08—Kaleidoscopes
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
- B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
- B32B2255/26—Polymeric coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
Definitions
- the present invention relates to an optical laminate.
- Image display devices such as liquid crystal display (LCD), cathode ray tube display device (CRT), plasma display (PDP), electroluminescence display (ELD), etc. are visible when the surface is damaged by external contact. May decrease. For this reason, the optical laminated body containing a base material layer and a hard-coat layer is used for the purpose of the surface protection of an image display apparatus.
- LCD liquid crystal display
- CRT cathode ray tube display device
- PDP plasma display
- ELD electroluminescence display
- the image display device is required to reduce the surface reflection due to the light irradiated from the outside and to improve the visibility.
- use of an optical laminate having a configuration of [base layer / hard coat layer / antireflection layer] has been proposed.
- a high refractive index is required for the hard coat layer and a low refractive index is required for the antireflection layer from the viewpoint of reflectivity. Therefore, high refractive index fine particles and low refractive index fine particles are added to the hard coat layer and the antireflection layer, respectively.
- an optical laminate including a high refractive index gradient hard coat layer in which the amount of high refractive index fine particles is continuously changed in the film thickness direction (for example, Patent Document 1).
- the antireflection film interference unevenness can be prevented. However, sufficient hardness may not be obtained.
- the present invention provides an optical laminate that includes a base material layer and a hard coat layer, prevents interference unevenness, and has sufficient hardness.
- the optical laminate of the present invention is a hard coat comprising a base material layer formed from a thermoplastic resin film, a curable compound having a molecular weight of 600 to 2500, and high refractive index fine particles having a refractive index of 1.50 or more.
- the said curable compound contains the oligomer of urethane (meth) acrylate and / or urethane (meth) acrylate.
- no phase separation occurs in the hard coat layer.
- the thermoplastic resin film is a (meth) acrylic resin film.
- the hard coat layer includes a thermoplastic resin that forms the thermoplastic resin film so that the concentration continuously decreases from the surface of the base material layer toward the thickness direction.
- a low refractive index layer is further provided on the side of the hard coat layer where the base material layer is not provided.
- a polarizing film is provided. This polarizing film contains the said optical laminated body.
- an image display device is provided. The image display device includes the optical laminate.
- a composition for forming a hard coat layer containing a curable compound having a predetermined molecular weight and high refractive index fine particles is applied onto a thermoplastic resin film, and a part of the composition is allowed to penetrate into the thermoplastic resin film. To form an infiltration region.
- the hard coat layer can be made to have a high refractive index with a small amount of high refractive index fine particles, interference unevenness can be prevented, and sufficient hardness can be obtained.
- the optical layered body of the present invention can be manufactured by a simple manufacturing method.
- FIG. 1 It is a schematic sectional drawing of the optical laminated body by one Embodiment of this invention. It is a schematic sectional drawing of the optical laminated body by another embodiment of this invention.
- (A) is the TEM photograph of the hard-coat layer cross section of the optical laminated body of Example 1
- (b) is the partial enlarged photograph. It is a graph showing the reflection spectrum of the optical laminated body obtained by the Example and the comparative example.
- (A) is a TEM photograph showing a cross section of the optical laminate T1
- (b) is a TEM photograph showing a cross section of the optical laminate T2.
- FIG. 1 is a schematic cross-sectional view of an optical laminate according to one embodiment of the present invention.
- the optical laminate 100 shown in FIG. 1 includes a base material layer 10 formed from a thermoplastic resin film and a hard coat layer 20 in this order.
- the hard coat layer 20 is formed by applying a composition for forming a hard coat layer to a thermoplastic resin film.
- the hard coat layer 20 includes a penetrating region 22 formed by penetrating a part of the applied hard coat layer forming composition into the thermoplastic resin film.
- the permeation region 22 is a portion where a hard coat layer forming composition component is present in the thermoplastic resin film.
- the base material layer 10 is a portion where the hard coat layer forming composition did not reach (penetrate) in the thermoplastic resin film when the hard coat layer forming composition penetrated into the thermoplastic resin film. It is.
- the boundary A in a figure is a boundary prescribed
- FIG. 2 is a schematic cross-sectional view of an optical laminate according to another embodiment of the present invention.
- the optical laminate 200 further includes a low refractive index layer 30 on the side of the hard coat layer 20 where the base material layer 10 is not provided.
- the optical laminate of the present invention is applied to, for example, a polarizing film (also referred to as a polarizing plate).
- a polarizing film also referred to as a polarizing plate.
- the optical laminate of the present invention is provided on one or both sides of a polarizer in a polarizing film, and can be suitably used as a protective material for the polarizer.
- the base material layer is formed from any appropriate thermoplastic resin film. More specifically, when the hard coat layer forming composition was applied to the thermoplastic resin film, the hard coat layer forming composition did not reach (penetrate) in the thermoplastic resin film. Part.
- thermoplastic resin film examples include (meth) acrylic resin film, cellulose resin film such as triacetyl cellulose, polyolefin resin film such as polyethylene and polypropylene; cycloolefin resin film such as polynorbornene, polyethylene terephthalate And polyester-based resin films such as polybutylene terephthalate.
- a (meth) acrylic resin film is preferable.
- the permeation region can be satisfactorily formed.
- “(meth) acryl” means acryl and / or methacryl.
- the light transmittance of the thermoplastic resin film at a wavelength of 380 nm is preferably 15% or less, more preferably 12% or less, and further preferably 9% or less. If the transmittance of light having a wavelength of 380 nm is in such a range, an excellent ultraviolet absorbing ability is exhibited, so that deterioration of ultraviolet rays due to external light or the like of the optical laminate can be prevented.
- the in-plane retardation Re of the thermoplastic resin film is preferably 10 nm or less, more preferably 7 nm or less, further preferably 5 nm or less, particularly preferably 3 nm or less, and most preferably 1 nm or less. is there.
- the thickness direction retardation Rth of the thermoplastic resin film is preferably 15 nm or less, more preferably 10 nm or less, further preferably 5 nm or less, particularly preferably 3 nm or less, and most preferably 1 nm or less. . If the in-plane retardation and the thickness direction retardation are within such ranges, the adverse effect on the display characteristics of the image display apparatus due to the phase difference can be remarkably suppressed.
- nx is the refractive index in the slow axis direction of the thermoplastic resin film
- ny is the refractive index in the fast axis direction of the thermoplastic resin film
- nz is the refractive index in the thickness direction of the thermoplastic resin film.
- d (nm) is the thickness of the thermoplastic resin film.
- the slow axis refers to the direction in which the in-plane refractive index is maximized
- the fast axis refers to the direction perpendicular to the slow axis in the plane.
- Re and Rth are measured using light having a wavelength of 590 nm.
- the (meth) acrylic resin film includes a (meth) acrylic resin.
- the (meth) acrylic resin film is obtained, for example, by extruding a molding material containing a resin component containing a (meth) acrylic resin as a main component.
- a (meth) acrylic resin film having an in-plane retardation and a thickness direction retardation within the above ranges can be obtained using, for example, a (meth) acrylic resin having a glutarimide structure described later. .
- the moisture permeability of the (meth) acrylic resin film is preferably 200 g / m 2 ⁇ 24 hr or less, and more preferably 80 g / m 2 ⁇ 24 hr or less. According to the present invention, even when a (meth) acrylic resin film having such a high moisture permeability is used, the adhesion between the (meth) acrylic resin film and the hard coat layer is excellent, and interference unevenness is suppressed. An optical laminate can be obtained.
- the moisture permeability can be measured under the test conditions of 40 ° C. and a relative humidity of 92%, for example, by a method according to JIS Z 0208.
- any appropriate (meth) acrylic resin can be adopted as the (meth) acrylic resin.
- poly (meth) acrylate such as polymethyl methacrylate, methyl methacrylate- (meth) acrylic acid copolymer, methyl methacrylate- (meth) acrylic acid ester copolymer, methyl methacrylate-acrylic acid ester -(Meth) acrylic acid copolymer, (meth) acrylic acid methyl-styrene copolymer (MS resin, etc.), polymer having alicyclic hydrocarbon group (for example, methyl methacrylate-cyclohexyl methacrylate copolymer) And methyl methacrylate- (meth) acrylate norbornyl copolymer).
- poly (meth) acrylate such as polymethyl methacrylate, methyl methacrylate- (meth) acrylic acid copolymer, methyl methacrylate- (meth) acrylic acid ester copolymer, methyl methacrylate-acrylic acid
- poly (meth) acrylate C 1-6 alkyl such as poly (meth) acrylate methyl is used. More preferred is a methyl methacrylate resin containing methyl methacrylate as a main component (50 to 100% by weight, preferably 70 to 100% by weight).
- the weight average molecular weight of the (meth) acrylic resin is preferably 10,000 to 500,000, more preferably 30,000 to 300,000, and still more preferably 50,000 to 200,000. If the weight average molecular weight is within this range, the permeability and compatibility with the hard coat layer forming composition are appropriate. On the other hand, if the weight average molecular weight is too small, the mechanical strength of the film tends to be insufficient. When the weight average molecular weight is too large, the viscosity at the time of melt extrusion is high, the molding processability is lowered, and the productivity of the molded product tends to be lowered.
- the glass transition temperature of the (meth) acrylic resin is preferably 110 ° C. or higher, more preferably 120 ° C. or higher. When the glass transition temperature is in such a range, a (meth) acrylic resin film excellent in durability and heat resistance can be obtained.
- the upper limit of the glass transition temperature is not particularly limited, but is preferably 170 ° C. or less from the viewpoint of moldability and the like.
- the (meth) acrylic resin preferably has a structural unit that exhibits positive birefringence and a structural unit that exhibits negative birefringence. If these structural units are included, the abundance ratio can be adjusted to control the retardation of the (meth) acrylic resin film, and a (meth) acrylic resin film having a low retardation can be obtained. it can.
- the structural unit exhibiting positive birefringence include a structural unit constituting a lactone ring, polycarbonate, polyvinyl alcohol, cellulose acetate, polyester, polyarylate, polyimide, polyolefin, etc., and a general formula (1) described later. Examples include structural units.
- Examples of the structural unit exhibiting negative birefringence include a structural unit derived from a styrene monomer, a maleimide monomer, a structural unit of polymethyl methacrylate, a structural unit represented by the general formula (3) described later, and the like. Can be mentioned.
- a structural unit that exhibits positive birefringence is a case where a resin having only the structural unit exhibits positive birefringence characteristics (that is, a slow axis appears in the stretching direction of the resin). Means a structural unit.
- a structural unit that develops negative birefringence is when a resin having only the structural unit exhibits negative birefringence characteristics (that is, when a slow axis appears in a direction perpendicular to the stretching direction of the resin).
- a (meth) acrylic resin having a lactone ring structure or a glutarimide structure is preferably used as the (meth) acrylic resin.
- a (meth) acrylic resin having a lactone ring structure or a glutarimide structure is excellent in heat resistance. More preferred is a (meth) acrylic resin having a glutarimide structure. If a (meth) acrylic resin having a glutarimide structure is used, a (meth) acrylic resin film having low moisture permeability and a small retardation and ultraviolet transmittance can be obtained as described above.
- Examples of (meth) acrylic resins having a glutarimide structure include, for example, JP-A-2006-309033, JP-A-2006-317560, JP-A-2006-328329, and JP-A-2006-328329.
- the glutarimide resin includes a structural unit represented by the following general formula (1) (hereinafter also referred to as a glutarimide unit) and a structural unit represented by the following general formula (2) (hereinafter referred to as (meta)). Also referred to as an acrylate unit).
- R 1 and R 2 are each independently hydrogen or an alkyl group having 1 to 8 carbon atoms
- R 3 is hydrogen, an alkyl group having 1 to 18 carbon atoms, or 3 to 3 carbon atoms.
- 12 a cycloalkyl group or a substituent containing an aromatic ring having 5 to 15 carbon atoms.
- R 4 and R 5 are each independently hydrogen or an alkyl group having 1 to 8 carbon atoms
- R 6 is hydrogen, an alkyl group having 1 to 18 carbon atoms, or 3 to 3 carbon atoms.
- 12 a cycloalkyl group or a substituent containing an aromatic ring having 5 to 15 carbon atoms.
- the glutarimide resin may further contain a structural unit represented by the following general formula (3) (hereinafter also referred to as an aromatic vinyl unit) as necessary.
- R 7 is hydrogen or an alkyl group having 1 to 8 carbon atoms
- R 8 is an aryl group having 6 to 10 carbon atoms.
- R 1 and R 2 are each independently hydrogen or a methyl group
- R 3 is hydrogen, a methyl group, a butyl group, or a cyclohexyl group, and more preferably , R 1 is a methyl group, R 2 is hydrogen, and R 3 is a methyl group.
- the glutarimide resin may include only a single type as a glutarimide unit, or may include a plurality of types in which R 1 , R 2 , and R 3 in the general formula (1) are different. Good.
- the glutarimide unit can be formed by imidizing the (meth) acrylic acid ester unit represented by the general formula (2).
- the glutarimide unit may be an acid anhydride such as maleic anhydride, or a half ester of such an acid anhydride and a linear or branched alcohol having 1 to 20 carbon atoms; acrylic acid, methacrylic acid, maleic acid It can also be formed by imidizing an ⁇ , ⁇ -ethylenically unsaturated carboxylic acid such as maleic anhydride, itaconic acid, itaconic anhydride, crotonic acid, fumaric acid and citraconic acid.
- R 4 and R 5 are each independently hydrogen or a methyl group
- R 6 is hydrogen or a methyl group
- R 4 is hydrogen
- R 5 is a methyl group
- R 6 is a methyl group
- the glutarimide resin may contain only a single type as a (meth) acrylic acid ester unit, or a plurality of types in which R 4 , R 5 and R 6 in the general formula (2) are different. May be included.
- the glutarimide resin preferably contains styrene, ⁇ -methylstyrene, and more preferably styrene as the aromatic vinyl unit represented by the general formula (3).
- aromatic vinyl unit By having such an aromatic vinyl unit, the positive birefringence of the glutarimide structure can be reduced, and a (meth) acrylic resin film having a lower retardation can be obtained.
- the glutarimide resin may contain only a single type as an aromatic vinyl unit, or may contain a plurality of types in which R 7 and R 8 are different.
- the content of the glutarimide unit in the glutarimide resin is preferably changed depending on, for example, the structure of R 3 .
- the content of the glutarimide unit is preferably 1% by weight to 80% by weight, more preferably 1% by weight to 70% by weight, even more preferably 1% by weight, based on the total structural unit of the glutarimide resin. -60% by weight, particularly preferably 1-50% by weight.
- a (meth) acrylic resin film having a low retardation excellent in heat resistance can be obtained.
- the content of the aromatic vinyl unit in the glutarimide resin can be appropriately set according to the purpose and desired characteristics. Depending on the application, the content of the aromatic vinyl unit may be zero.
- the content thereof is preferably 10% by weight to 80% by weight, more preferably 20% by weight to 80% by weight, based on the glutarimide unit of the glutarimide resin. More preferably, it is 20% by weight to 60% by weight, and particularly preferably 20% by weight to 50% by weight.
- a (meth) acrylic resin film having a low retardation, excellent heat resistance and mechanical strength can be obtained.
- the glutarimide resin may be further copolymerized with other structural units other than the glutarimide unit, the (meth) acrylic acid ester unit, and the aromatic vinyl unit, if necessary.
- other structural units include structures composed of nitrile monomers such as acrylonitrile and methacrylonitrile, and maleimide monomers such as maleimide, N-methylmaleimide, N-phenylmaleimide, and N-cyclohexylmaleimide. Units are listed. These other structural units may be directly copolymerized or graft copolymerized in the glutarimide resin.
- the thermoplastic resin film contains an ultraviolet absorber.
- the ultraviolet absorber any appropriate ultraviolet absorber can be adopted as long as the desired characteristics are obtained.
- Representative examples of the above UV absorbers include triazine UV absorbers, benzotriazole UV absorbers, benzophenone UV absorbers, cyanoacrylate UV absorbers, benzoxazine UV absorbers, and oxadiazole UV absorbers. Agents. These ultraviolet absorbers may be used alone or in combination.
- the content of the ultraviolet absorber is preferably 0.1 to 5 parts by weight, more preferably 0.2 to 3 parts by weight with respect to 100 parts by weight of the thermoplastic resin.
- the content of the ultraviolet absorber is in such a range, ultraviolet rays can be absorbed effectively and the transparency of the film during film formation does not deteriorate.
- the content of the ultraviolet absorber is less than 0.1 parts by weight, the ultraviolet blocking effect tends to be insufficient.
- there is more content of a ultraviolet absorber than 5 weight part there exists a tendency for coloring to become intense or the haze of the film after shaping
- the thermoplastic resin film may contain any appropriate additive depending on the purpose.
- additives include hindered phenol-based, phosphorus-based and sulfur-based antioxidants; light-resistant stabilizers, weather-resistant stabilizers, heat stabilizers and other stabilizers; reinforcing materials such as glass fibers and carbon fibers; Infrared absorbers; flame retardants such as tris (dibromopropyl) phosphate, triallyl phosphate, antimony oxide; antistatic agents such as anionic, cationic and nonionic surfactants; coloring of inorganic pigments, organic pigments, dyes, etc. Agents; organic fillers and inorganic fillers; resin modifiers; plasticizers; lubricants; retardation reducing agents.
- the kind, combination, content, and the like of the additive to be contained can be appropriately set according to the purpose and desired characteristics.
- thermoplastic resin film is not particularly limited.
- the thermoplastic resin, the ultraviolet absorber, and other polymers and additives as necessary may be arbitrarily selected. It is possible to form a film from a thermoplastic resin composition that has been sufficiently mixed by an appropriate mixing method. Alternatively, a thermoplastic resin, an ultraviolet absorber, and if necessary, other polymers and additives are mixed in separate solutions to form a uniform mixed solution, and then formed into a film. Good.
- the film raw material is pre-blended with any suitable mixer such as an omni mixer, and then the obtained mixture is extruded and kneaded.
- the mixer used for extrusion kneading is not particularly limited, and for example, any suitable mixer such as an extruder such as a single screw extruder or a twin screw extruder or a pressure kneader may be used. Can do.
- the film forming method examples include any appropriate film forming methods such as a solution casting method (solution casting method), a melt extrusion method, a calendar method, and a compression molding method.
- a melt extrusion method is preferred. Since the melt extrusion method does not use a solvent, it is possible to reduce the manufacturing cost and the burden on the global environment and work environment due to the solvent.
- melt extrusion method examples include a T-die method and an inflation method.
- the molding temperature is preferably 150 to 350 ° C, more preferably 200 to 300 ° C.
- a T-die is attached to the tip of a known single-screw extruder or twin-screw extruder, and the film extruded into a film is wound to obtain a roll-shaped film Can do.
- simultaneous biaxial stretching, sequential biaxial stretching, and the like can be performed by stretching the film in a direction perpendicular to the extrusion direction.
- the thermoplastic resin film may be either an unstretched film or a stretched film as long as the desired retardation is obtained.
- a stretched film either a uniaxially stretched film or a biaxially stretched film may be used.
- a biaxially stretched film either a simultaneous biaxially stretched film or a sequential biaxially stretched film may be used.
- the stretching temperature is preferably in the vicinity of the glass transition temperature of the thermoplastic resin composition which is a film raw material, and more preferably, (glass transition temperature ⁇ 30 ° C.) to (glass transition temperature + 30 ° C.) Preferably, it is within the range of (glass transition temperature ⁇ 20 ° C.) to (glass transition temperature + 20 ° C.). If the stretching temperature is less than (glass transition temperature ⁇ 30 ° C.), the haze of the resulting film may increase, or the film may be torn or cracked, resulting in failure to obtain a predetermined stretching ratio.
- the stretching ratio is preferably 1.1 to 3 times, more preferably 1.3 to 2.5 times.
- the mechanical properties such as the film elongation, tear propagation strength, and fatigue resistance can be greatly improved.
- thermoplastic resin film can be subjected to a heat treatment (annealing) or the like after the stretching treatment in order to stabilize its optical isotropy and mechanical properties.
- Arbitrary appropriate conditions can be employ
- the thickness of the thermoplastic resin film is preferably 10 ⁇ m to 200 ⁇ m, more preferably 20 ⁇ m to 100 ⁇ m. There exists a possibility that intensity
- the surface tension of the thermoplastic resin film is preferably 40 mN / m or more, more preferably 50 mN / m or more, and further preferably 55 mN / m or more.
- the surface wetting tension is 40 mN / m or more, the adhesion between the thermoplastic resin film and the hard coat layer is further improved.
- Any suitable surface treatment can be applied to adjust the surface wetting tension. Examples of the surface treatment include corona discharge treatment, plasma treatment, ozone spraying, ultraviolet irradiation, flame treatment, and chemical treatment. Of these, corona discharge treatment and plasma treatment are preferable.
- the hard coat layer is formed by applying a composition for forming a hard coat layer containing a curable compound having a predetermined molecular weight and high refractive index fine particles to a thermoplastic resin film. More specifically, the hard coat layer is formed by applying a hard coat layer forming composition containing a curable compound having a predetermined molecular weight and high refractive index fine particles to a thermoplastic resin film, and a part of the hard coat layer is formed on the thermoplastic resin film. It is formed by infiltrating into. Preferably, elution of the thermoplastic resin that forms the thermoplastic resin film into the coating layer of the hard coat layer forming composition occurs simultaneously with the penetration of the hard coat layer forming composition into the thermoplastic resin film.
- the hard coat layer includes an infiltration region formed by infiltrating the thermoplastic resin film with the hard coat layer forming composition.
- the thermoplastic resin forming the thermoplastic resin film and the hard coat layer forming composition are compatible.
- the lower limit of the penetration depth into the thermoplastic resin film (thickness of the penetration region) of the composition for forming a hard coat layer is, for example, 1.2 ⁇ m, preferably 1.5 ⁇ m, more preferably 2.5 ⁇ m. More preferably, it is 3 ⁇ m.
- the upper limit of the penetration depth is preferably (thermoplastic resin film thickness ⁇ 70%) ⁇ m, more preferably (thermoplastic resin film thickness ⁇ 40%) ⁇ m, and even more preferably (thermoplastic resin film). Thickness ⁇ 30%) ⁇ m, particularly preferably (thermoplastic resin film ⁇ 20%) ⁇ m.
- the penetration depth is within such a range, an optical laminate having excellent adhesion between the thermoplastic resin film and the hard coat layer, suppressing interference unevenness, and excellent hardness can be obtained.
- the penetration depth can be measured by reflection with a hard coat layer or observation with an electron microscope such as SEM or TEM.
- the hard coat layer preferably contains a thermoplastic resin forming a thermoplastic resin film in the permeation region so that its concentration continuously decreases from the base material layer side surface toward the opposite surface.
- the hard coat layer may also include a thermoplastic resin beyond the permeation region (ie, beyond the boundary line A in FIG. 1). Even in this case, it is preferable that the thermoplastic resin is contained so that its concentration continuously decreases from the base material layer side surface toward the opposite surface. This is because, by continuously changing the concentration of the thermoplastic resin, interface reflection between the base material layer and the hard coat layer can be suppressed, and an optical laminated body with less interference unevenness can be obtained. Further, segregation of high refractive index fine particles and formation of a concentration gradient described later can be suitably performed.
- the hard coat layer is not phase-separated, in other words, has no upper and lower two-layer structure.
- phase separation occurs in the hard coat layer and an upper and lower two-layer structure is formed, segregation of high refractive index fine particles and formation of a concentration gradient, which will be described later, may be insufficient.
- thermoplastic resin concentration gradient in the upper layer (the base layer side layer is the lower layer) or the concentration gradient becomes gentle, resulting in high refraction. It is presumed that the fine particles can be dispersed with high uniformity.
- the present invention for example, in observation with an electron microscope such as SEM or TEM, it is confirmed that there is no phase separation interface in the hard coat layer, and the reflection spectrum of the hard coat layer is measured. It can be judged that there is no separation or upper and lower two-layer structure.
- the high refractive index fine particles are segregated on the surface on which the base material layer is not provided, and the concentration thereof continuously decreases from the surface in the thickness direction.
- the high refractive index fine particles are segregated on the surface on which the base material layer is not provided” means that 90% by weight or more of the high refractive index fine particles contained in the hard coat layer is the base material layer. It means that it exists in the area
- 90% by weight or more of the high refractive index fine particles contained in the hard coat layer is present in a region at a distance from the surface in the thickness direction (hard coat layer thickness ⁇ 60%) or less.
- the high refractive index fine particles any appropriate fine particles having a refractive index of 1.50 or more are used.
- the upper limit of the refractive index can be, for example, 2.80.
- the refractive index means a refractive index at a wavelength of 590 nm.
- Examples of the high refractive index fine particles include metal oxide fine particles.
- Specific examples of the metal oxide include titanium oxide (TiO 2 ), zirconium oxide (ZrO 2 ), cerium oxide (CeO 2 ), tin oxide (SnO 2 ), antimony tin oxide (ATO), indium tin oxide ( ITO), phosphorus tin compound (PTO), antimony oxide (Sb 2 O 5 ), aluminum zinc oxide (AZO), gallium zinc oxide (GZO), zinc antimonate (ZnSb 2 O 6 ), and the like.
- the average particle diameter of the high refractive index fine particles is preferably 1 nm to 100 nm, more preferably 1 nm to 50 nm. Such an average particle diameter is excellent in transparency and easy to handle.
- the average particle size is a value that is measured without distinguishing between primary particles and secondary particles, assuming that the secondary particles are also one particle.
- the average particle diameter can be obtained, for example, as an average value of the particle diameters of particles (for example, 50 particles) observed in a predetermined region of the cross section of the hard coat layer with a transmission electron microscope. .
- the content of the high refractive index fine particles in the hard coat layer forming composition is, for example, 10 to 80 parts by weight, preferably 15 to 50 parts by weight with respect to 100 parts by weight of the curable compound.
- the curable compound contained in the composition for forming a hard coat layer can be cured by heat, light (such as ultraviolet rays) or electron beam.
- the curable compound is preferably a photocurable curable compound.
- the curable compound may be any of a monomer, an oligomer and a prepolymer.
- the molecular weight of the curable compound is 2500 or less, preferably 2000 or less, more preferably 1800 or less, and further preferably 1500 or less.
- the molecular weight of the curable compound is 600 or more, more preferably 800 or more, and still more preferably 1000 or more.
- penetration of the composition for forming a hard coat layer into the thermoplastic resin film becomes excessive, and as a result, the desired hardness may not be achieved.
- the molecular weight of the said curable compound is a weight average molecular weight.
- “the molecular weight of the curable compounds is 2500 or less” means that the weighted average value of the molecular weights of the two or more curable compounds is 2500 or less. To do.
- a curable compound having two or more (meth) acryloyl groups is preferably used.
- the upper limit of the number of (meth) acryloyl groups contained in the curable compound having two or more (meth) acryloyl groups is preferably 30. Since the curable compound having two or more (meth) acryloyl groups is excellent in compatibility with the (meth) acrylic resin, when a (meth) acrylic resin film is used as the thermoplastic resin film, It easily penetrates and diffuses into the (meth) acrylic resin film.
- “(meth) acryloyl” means methacryloyl and / or acryloyl.
- curable compound having two or more (meth) acryloyl groups include tricyclodecane dimethanol diacrylate, pentaerythritol di (meth) acrylate, pentaerythritol tri (meth) acrylate, and trimethylolpropane triacrylate.
- Pentaerythritol tetra (meth) acrylate dimethylolpropanthate tetraacrylate, dipentaerythritol hexa (meth) acrylate, 1,6-hexanediol (meth) acrylate, 1,9-nonanediol diacrylate, 1,10-decane Diol (meth) acrylate, polyethylene glycol di (meth) acrylate, polypropylene glycol di (meth) acrylate, dipropylene glycol diacrylate, isocyanuric acid Examples include li (meth) acrylate, ethoxylated glycerin triacrylate, ethoxylated pentaerythritol tetraacrylate, and oligomers or prepolymers thereof.
- the curable compound having two or more (meth) acryloyl groups may be used alone or in combination. In the present specification, “(meth) acrylate
- the curable compound having two or more (meth) acryloyl groups preferably has a hydroxyl group. If the composition for forming a hard coat layer contains such a curable compound, the heating temperature at the time of forming the hard coat layer can be set lower, the heating time can be set shorter, and deformation due to heating can be suppressed.
- the produced optical laminate can be produced efficiently. Moreover, the optical laminated body excellent in the adhesiveness of a thermoplastic resin film (for example, (meth) acrylic-type resin film) and a hard-coat layer can be obtained.
- the curable compound having a hydroxyl group and two or more (meth) acryloyl groups include pentaerythritol tri (meth) acrylate and dipentaerythritol pentaacrylate.
- urethane (meth) acrylate and / or urethane (meth) acrylate oligomers are preferably used as the curable compound having two or more (meth) acryloyl groups.
- the number of (meth) acryloyl groups contained in the urethane (meth) acrylate and / or urethane (meth) acrylate oligomer is preferably 3 or more, more preferably 4 to 15, and still more preferably 6 to 12.
- the molecular weight of the urethane (meth) acrylate and / or urethane (meth) acrylate is, for example, 3000 or less, preferably 500 to 2500, and more preferably 800 to 2000.
- Urethane (meth) acrylate and / or urethane (meth) acrylate oligomers having a molecular weight in the above range and having two or more (meth) acryloyl groups are thermoplastic resin films (especially (meth) acrylic). Resin film) and compatibility with thermoplastic resins (especially (meth) acrylic resins) are appropriate. As a result, a hard coat layer that does not have phase separation while maintaining hardness can be obtained.
- the urethane (meth) acrylate can be obtained, for example, by reacting hydroxy (meth) acrylate obtained from (meth) acrylic acid or (meth) acrylic acid ester and polyol with diisocyanate. Moreover, you may use arbitrary appropriate commercial items. Urethane (meth) acrylates and urethane (meth) acrylate oligomers may be used alone or in combination.
- Examples of the (meth) acrylic acid ester include methyl (meth) acrylate, ethyl (meth) acrylate, isopropyl (meth) acrylate, butyl (meth) acrylate, cyclohexyl (meth) acrylate, and the like.
- polyol examples include ethylene glycol, 1,3-propylene glycol, 1,2-propylene glycol, diethylene glycol, dipropylene glycol, neopentyl glycol, 1,3-butanediol, 1,4-butanediol, 1, 6-hexanediol, 1,9-nonanediol, 1,10-decanediol, 2,2,4-trimethyl-1,3-pentanediol, 3-methyl-1,5-pentanediol, neopentyl hydroxypivalate Glycol ester, tricyclodecane dimethylol, 1,4-cyclohexanediol, spiroglycol, hydrogenated bisphenol A, ethylene oxide added bisphenol A, propylene oxide added bisphenol A, trimethylol ethane, trimethylol Propane, glycerin, 3-methylpentane-1,3,5-triol, pentaeryth
- diisocyanate for example, various aromatic, aliphatic or alicyclic diisocyanates can be used. Specific examples of the diisocyanate include tetramethylene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, 2,4-tolylene diisocyanate, 4,4-diphenyl diisocyanate, 1,5-naphthalene diisocyanate, 3,3-dimethyl-4,4. -Diphenyl diisocyanate, xylene diisocyanate, trimethylhexamethylene diisocyanate, 4,4-diphenylmethane diisocyanate, and hydrogenated products thereof.
- the content ratio of the curable compound having two or more (meth) acryloyl groups is preferably based on the total curable compound (total amount of monomer, oligomer and prepolymer) in the hard coat layer forming composition. It is 60% by weight to 100% by weight, more preferably 70% by weight to 100% by weight, and still more preferably 80% by weight to 100% by weight. If it is such a range, the optical laminated body which was excellent in the adhesiveness of a thermoplastic resin film (for example, (meth) acrylic-type resin film) and a hard-coat layer, and the interference nonuniformity was suppressed can be obtained. . In addition, curing shrinkage of the hard coat layer can be effectively prevented.
- the total content of the urethane (meth) acrylate and the urethane (meth) acrylate oligomer is preferably 40% by weight to 100% by weight with respect to the total curable compound in the hard coat layer forming composition.
- the amount is preferably 50% to 95% by weight, particularly preferably 60% to 90% by weight. If it is such a range, the hard-coat layer excellent in hardness and adhesiveness with a base material layer can be formed.
- the hard coat layer forming composition may contain a monofunctional monomer as a curable compound.
- a monofunctional monomer easily penetrates into a thermoplastic resin film (for example, a (meth) acrylic resin film). Therefore, if the monofunctional monomer is contained, the adhesion between the thermoplastic resin film and the hard coat layer is excellent. And the optical laminated body by which interference nonuniformity was suppressed can be obtained.
- the content ratio of the monofunctional monomer is preferably 40% by weight or less, more preferably 30% by weight or less, and particularly preferably 20% by weight with respect to the total curable compound in the hard coat layer forming composition. It is as follows. When the content ratio of the monofunctional monomer is more than 40% by weight, desired hardness and scratch resistance may not be obtained.
- the hard coat layer forming composition preferably contains any appropriate photopolymerization initiator.
- the photopolymerization initiator include 2,2-dimethoxy-2-phenylacetophenone, acetophenone, benzophenone, xanthone, 3-methylacetophenone, 4-chlorobenzophenone, 4,4′-dimethoxybenzophenone, benzoinpropyl ether, benzyldimethyl Ketals, N, N, N ′, N′-tetramethyl-4,4′-diaminobenzophenone, 1- (4-isopropylphenyl) -2-hydroxy-2-methylpropan-1-one, thioxanthone compounds, etc. Can be mentioned.
- the hard coat layer forming composition may further contain any appropriate additive.
- additives include leveling agents, anti-blocking agents, dispersion stabilizers, thixotropic agents, antioxidants, UV absorbers, antifoaming agents, thickeners, dispersants, surfactants, catalysts, fillers, and lubricants. And antistatic agents.
- the leveling agent examples include a fluorine-based or silicone-based leveling agent, and a silicone-based leveling agent is preferable.
- the silicone leveling agent examples include reactive silicone, polydimethylsiloxane, polyether-modified polydimethylsiloxane, and polymethylalkylsiloxane. Of these, reactive silicone is preferable. If reactive silicone is added, the surface of the hard coat layer is provided with slipperiness and the scratch resistance is maintained for a long period of time.
- the content of the leveling agent is preferably 5% by weight or less, more preferably 0.01% by weight to 5% by weight, based on the total curable compound in the hard coat layer forming composition.
- the hard coat layer forming composition may or may not contain a solvent.
- the solvent include dibutyl ether, dimethoxymethane, dimethoxyethane, diethoxyethane, propylene oxide, 1,4-dioxane, 1,3-dioxolane, 1,3,5-trioxane, tetrahydrofuran, acetone, methyl ethyl ketone (MEK).
- the composition for forming a hard coat layer containing no solvent or the composition for forming a hard coat layer containing only the poor solvent for the thermoplastic resin film forming material as the solvent can be used.
- An object can permeate the thermoplastic resin film to form a permeation region having a desired thickness.
- the refractive index of the hard coat layer (refractive index on the surface on which the base material layer is not provided) is preferably 1.48 to 1.78.
- the pencil hardness of the hard coat layer is preferably 2H or more.
- the thickness of the hard coat layer is preferably 3 ⁇ m to 30 ⁇ m, more preferably 5 ⁇ m to 20 ⁇ m.
- the low refractive index layer has a lower refractive index than the hard coat layer. By laminating the low refractive index layer on the hard coat layer, the antireflection property of the obtained optical laminate is improved.
- the refractive index of the low refractive index layer is preferably 1.20 to 1.45, more preferably 1.23 to 1.42.
- the low refractive index layer is typically formed by applying a low refractive index layer-forming composition containing a binder component and low refractive index fine particles to the hard coat layer.
- the binder component may be a curable binder component that can be cured by heat, light (ultraviolet rays, etc.) or an electron beam, and does not react with heat, light (ultraviolet rays, etc.) or electron beams, and is dried or dried. It may be a non-curable binder component that is solidified by cooling. A curable binder component is preferably used.
- curable binder component Any appropriate curable compound may be selected as the curable binder component.
- the curable compound may be any of a monomer, an oligomer and a prepolymer. Specific examples include curable fluororesins and the curable compounds described in Section D.
- the refractive index of the low refractive index fine particles is, for example, 1.44 or less, preferably 1.20 to 1.44, more preferably 1.23 to 1.40.
- Examples of the low refractive index fine particles include fine particles having voids or fine particles formed of a low refractive index material.
- Examples of the fine particles having voids include hollow fine particles and porous fine particles.
- Examples of the material for forming fine particles having voids include metals, metal oxides, and resins.
- hollow silica fine particles can be preferably used.
- a lipophilic group or a reactive group may be introduced on the surface using a silane coupling agent.
- the material for forming the fine particles formed of the low refractive index material is not limited as long as the refractive index is satisfied, and examples thereof include metal fluorides such as magnesium fluoride, aluminum fluoride, calcium fluoride, and lithium fluoride. It is done.
- the average particle size (average primary particle size) of the low refractive index fine particles is, for example, 1 nm to 100 nm. If the average particle size is within the range, both transparency and dispersibility can be achieved.
- the blending amount of the low refractive index fine particles is preferably 30% by weight to 250% by weight, more preferably 45% by weight to 200% by weight, and further preferably 60% by weight to 150% by weight with respect to the binder component. It is.
- the low refractive index layer forming composition preferably contains any appropriate photopolymerization initiator. Further, it may further contain a solvent and any appropriate additive as required. Specific examples of the photopolymerization initiator, the solvent and the additive include the same ones that can be used for the composition for forming a hard coat layer.
- the thickness of the low refractive index layer is, for example, 10 nm to 200 nm, preferably 20 nm to 120 nm.
- the manufacturing method of the optical laminated body of this invention includes apply
- the method further includes subjecting the composition for forming a hard coat layer to a curing treatment after the heating.
- the composition for forming a low refractive index layer is applied on the coating layer after heating or the hard coat layer after curing, and optionally subjected to curing treatment.
- the composition for forming a low refractive index layer is applied on the hard coat layer after the curing treatment, and the curing treatment is performed.
- any appropriate method can be adopted as a method for applying the hard coat layer forming composition and the low refractive index layer forming composition.
- Examples thereof include a bar coating method, a roll coating method, a gravure coating method, a rod coating method, a slot orifice coating method, a curtain coating method, a fountain coating method, and a comma coating method.
- the heating temperature of the coating layer can be set to an appropriate temperature according to the composition of the hard coat layer forming composition, and is preferably set to be equal to or lower than the glass transition temperature of the resin contained in the thermoplastic resin film.
- the heating temperature of the coating layer is, for example, 80 ° C. to 140 ° C. When heated at a temperature in such a range, the curable compound in the hard coat layer-forming composition penetrates and diffuses well into the thermoplastic resin film.
- the composition for hard-coat layer formation contains a solvent
- coated composition for hard-coat layer formation can be dried by the said heating. Further, the penetration depth can be increased, for example, by setting the heating temperature high within the above range.
- the heating temperature may be set according to the content ratio of the curable compound having two or more (meth) acryloyl groups and the monofunctional monomer.
- the heating temperature for example, 80 ° C. to 100 ° C.
- the curing process is performed by ultraviolet irradiation.
- the integrated light quantity of ultraviolet irradiation is preferably 200 mJ to 400 mJ.
- the reflection spectrum of the hard coat layer was measured under the following conditions using an instantaneous multi-photometry system (trade name: MCPD3700, manufactured by Otsuka Electronics Co., Ltd.), and the thickness of the hard coat layer was evaluated from the peak position of the FFT spectrum. .
- the value measured by said (1) was used for the refractive index.
- Reflection spectrum measurement conditions Reference: Mirror Algorithm: FFT method Calculation wavelength: 450 nm to 850 nm ⁇ Detection conditions Exposure time: 20 ms Lamp gain: Normal Integration count: 10 times / FFT method Film thickness range: 2 to 15 ⁇ m Film thickness resolution: 24nm
- -Laminate (R1) Implemented except that a PET base material (trade name: U48-3, refractive index: 1.60) manufactured by Toray Industries, Inc. was used as the base film, and the heating temperature of the coating layer was 60 ° C. Obtained in the same manner as in Example 1. Since the composition for forming a hard coat layer does not penetrate into the PET substrate used for the laminate (R1), the thickness of the hard coat layer measured from the peak position of the FFT spectrum obtained from the laminate (R1) is: It becomes smaller by the penetration depth than the thickness of the hard coat layer of the optical laminate obtained in the examples and comparative examples.
- the penetration depth is determined by subtracting (thickness of hard coat layer of laminate (R1)) from (thickness of hard coat layer of optical laminate obtained in Examples and Comparative Examples).
- the film is stretched in an atmosphere of 150 ° C. in the transport direction (thickness 80 ⁇ m), and then stretched in an atmosphere of 150 ° C. in a direction orthogonal to the film transport direction to form a base film A (( (Meth) acrylic resin film).
- the base film A thus obtained had a light transmittance of 8.5% at a wavelength of 380 nm, an in-plane retardation Re of 0.4 nm, and a thickness direction retardation Rth of 0.78 nm.
- the moisture permeability of the obtained base film A was 61 g / m 2 ⁇ 24 hr.
- the light transmittance was measured by measuring a transmittance spectrum in a wavelength range of 200 nm to 800 nm using a spectrophotometer (device name: U-4100) manufactured by Hitachi High-Tech Co., Ltd., and reading the transmittance at a wavelength of 380 nm. .
- the phase difference value was measured at a wavelength of 590 nm and 23 ° C. using a trade name “KOBRA21-ADH” manufactured by Oji Scientific Instruments.
- the moisture permeability was measured by a method according to JIS K 0208 under conditions of a temperature of 40 ° C. and a relative humidity of 92%.
- the obtained composition for forming a hard coat layer was applied to form a coating layer, and the coating layer was heated at 100 ° C. for 1 minute.
- the heated coating layer was irradiated with ultraviolet rays having an integrated light amount of 300 mJ / cm 2 with a high-pressure mercury lamp to cure the coating layer, thereby obtaining an optical laminate having a structure of [base material layer / hard coat layer].
- Example 2 An optical laminate was obtained in the same manner as in Example 1 except that the amount of the ZrO 2 fine particle-containing sol was 67 parts.
- Example 3 An optical laminate was obtained in the same manner as in Example 1 except that the blending amount of the ZrO 2 fine particle-containing sol was 133 parts.
- Example 4 Sb 2 O 5 fine particle-containing sol in place of ZrO 2 fine particle-containing sol 100 parts (JGC Catalysts and Chemicals Ltd., trade name "ELCOM V-4562", solid content: 30%, average particle diameter: 15 nm, refractive index: 1. (7, solvent: methyl isobutyl ketone) An optical laminate was obtained in the same manner as in Example 1 except that 133 parts were used.
- an optical laminate was obtained in the same manner as in Example 1 except that the heating temperature of the coating layer was set to 110 ° C.
- An optical laminate was obtained in the same manner as in Example 1 except that the heating temperature of the coating layer was 110 ° C.
- the optical laminate of the present invention has suppressed interference unevenness and sufficient hardness. Moreover, since it can manufacture with 1 coat, manufacture is easy.
- the cross section of the optical laminated body obtained in each Example was observed with a TEM, the hard coat layer was not phase-separated, and the high refractive index fine particles were on the surface on which the base material layer was not provided. The segregation was such that the concentration continuously decreased in the thickness direction.
- FIGS A TEM photograph of a cross section of the hard coat layer of the optical layered body of Example 1 is shown in FIGS. As shown in FIG.
- the hard coat layer of the optical laminate of Example 1 is not phase-separated, and the high refractive index fine particles are segregated on the side where the base material layer is not provided.
- FIG. 3B which is a partially enlarged photograph of FIG. 3A, the high refractive index fine particles are concentrated from the surface on the side where the base material layer is not provided toward the base material layer side. Are distributed so as to be continuously lower.
- the reflection spectra of the optical laminate of Example 1 and the optical laminate of Comparative Example 3 were measured under the same conditions as the measurement of the thickness of the hard coat layer except that the calculation wavelength was 380 nm to 780 nm.
- the results are shown in FIG.
- the optical layered body of Example 1 has a smooth reflection spectrum and no interference unevenness.
- the reflection spectrum is wavy, and it can be seen that there is interference unevenness.
- the reflection spectrum of the optical laminated body of Comparative Example 3 has such a shape is that the optical laminated body has two interfaces having different refractive indexes (that is, a phase separation interface in the hard coat layer, a hard coat layer and a base). This is probably because there is an interface with the material layer. That is, the shape of the reflection spectrum of the optical laminate of Comparative Example 3 is a result of light recognizing the phase separation interface in the hard coat layer, and the high refractive index particles are uniformly dispersed in the upper layer. Recognize.
- FIGS. 5 (a) and 5 (b) TEM photographs of cross sections of the optical laminates T1 and T2 are shown in FIGS. 5 (a) and 5 (b), respectively.
- no phase separation occurs in the hard coat layer of the optical laminate T1.
- phase separation occurs in the hard coat layer of the optical laminate T2.
- the optical layered body of the present invention can be suitably used for an image display device.
- the optical layered body of the present invention can be suitably used as a front plate of an image display device or a protective material for a polarizer, and particularly suitably used as a front plate of a liquid crystal display device (in particular, a three-dimensional liquid crystal display device). obtain.
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Abstract
Description
1つの実施形態においては、上記硬化性化合物が、ウレタン(メタ)アクリレートおよび/またはウレタン(メタ)アクリレートのオリゴマーを含む。
1つの実施形態においては、上記ハードコート層において、相分離が生じていない。
1つの実施形態においては、上記熱可塑性樹脂フィルムが、(メタ)アクリル系樹脂フィルムである。
1つの実施形態においては、上記ハードコート層が、上記基材層側表面から厚み方向に向かって濃度が連続的に低くなるように上記熱可塑性樹脂フィルムを形成する熱可塑性樹脂を含む。
1つの実施形態においては、上記ハードコート層の上記基材層が設けられていない側に、低屈折率層をさらに備える。
本発明の別の局面によれば、偏光フィルムが提供される。該偏光フィルムは、上記光学積層体を含む。
本発明のさらに別の局面によれば、画像表示装置が提供される。該画像表示装置は、上記光学積層体を含む。 The optical laminate of the present invention is a hard coat comprising a base material layer formed from a thermoplastic resin film, a curable compound having a molecular weight of 600 to 2500, and high refractive index fine particles having a refractive index of 1.50 or more. A hard coat layer formed by applying the layer forming composition to the thermoplastic resin film, and the hard coat layer penetrates the thermoplastic resin film. Including the formed penetrating region, the high refractive index fine particles segregate in the hard coat layer so that the concentration decreases continuously in the thickness direction from the surface on the side where the base material layer is not provided. ing.
In one embodiment, the said curable compound contains the oligomer of urethane (meth) acrylate and / or urethane (meth) acrylate.
In one embodiment, no phase separation occurs in the hard coat layer.
In one embodiment, the thermoplastic resin film is a (meth) acrylic resin film.
In one embodiment, the hard coat layer includes a thermoplastic resin that forms the thermoplastic resin film so that the concentration continuously decreases from the surface of the base material layer toward the thickness direction.
In one embodiment, a low refractive index layer is further provided on the side of the hard coat layer where the base material layer is not provided.
According to another aspect of the present invention, a polarizing film is provided. This polarizing film contains the said optical laminated body.
According to still another aspect of the present invention, an image display device is provided. The image display device includes the optical laminate.
A.光学積層体の全体構成
図1は、本発明の1つの実施形態による光学積層体の概略断面図である。図1に示す光学積層体100は、熱可塑性樹脂フィルムから形成される基材層10と、ハードコート層20とをこの順に備える。ハードコート層20は、熱可塑性樹脂フィルムにハードコート層形成用組成物を塗布して形成される。ハードコート層20は、塗布されたハードコート層形成用組成物の一部が熱可塑性樹脂フィルムに浸透して形成された浸透領域22を含む。すなわち、浸透領域22は、熱可塑性樹脂フィルムにおいて、ハードコート層形成用組成物成分が存在している部分である。一方、基材層10は、このようにハードコート層形成用組成物が熱可塑性樹脂フィルムに浸透した際に、熱可塑性樹脂フィルムにおいてハードコート層形成用組成物が到達(浸透)しなかった部分である。なお、図中の境界Aは、熱可塑性樹脂フィルムのハードコート層形成用組成物塗布面により規定される境界である。 Hereinafter, although preferable embodiment of this invention is described, this invention is not limited to these embodiment.
A. FIG. 1 is a schematic cross-sectional view of an optical laminate according to one embodiment of the present invention. The
基材層は、任意の適切な熱可塑性樹脂フィルムから形成される。より詳細には、基材層は、熱可塑性樹脂フィルムにハードコート層形成用組成物を塗布した際に、熱可塑性樹脂フィルムにおいて、当該ハードコート層形成用組成物が到達(浸透)しなかった部分である。 B. Base material layer The base material layer is formed from any appropriate thermoplastic resin film. More specifically, when the hard coat layer forming composition was applied to the thermoplastic resin film, the hard coat layer forming composition did not reach (penetrate) in the thermoplastic resin film. Part.
Re=(nx-ny)×d
Rth=(nx-nz)×d
ここで、nxは熱可塑性樹脂フィルムの遅相軸方向の屈折率であり、nyは熱可塑性樹脂フィルムの進相軸方向の屈折率であり、nzは熱可塑性樹脂フィルムの厚み方向の屈折率であり、d(nm)は熱可塑性樹脂フィルムの厚みである。遅相軸は、フィルム面内の屈折率が最大になる方向をいい、進相軸は、面内で遅相軸に垂直な方向をいう。代表的には、ReおよびRthは、波長590nmの光を用いて測定される。 The in-plane retardation Re of the thermoplastic resin film is preferably 10 nm or less, more preferably 7 nm or less, further preferably 5 nm or less, particularly preferably 3 nm or less, and most preferably 1 nm or less. is there. The thickness direction retardation Rth of the thermoplastic resin film is preferably 15 nm or less, more preferably 10 nm or less, further preferably 5 nm or less, particularly preferably 3 nm or less, and most preferably 1 nm or less. . If the in-plane retardation and the thickness direction retardation are within such ranges, the adverse effect on the display characteristics of the image display apparatus due to the phase difference can be remarkably suppressed. More specifically, interference unevenness and 3D image distortion when used in a liquid crystal display device for 3D display can be significantly suppressed. The in-plane retardation Re and the thickness direction retardation Rth can be obtained by the following equations, respectively:
Re = (nx−ny) × d
Rth = (nx−nz) × d
Here, nx is the refractive index in the slow axis direction of the thermoplastic resin film, ny is the refractive index in the fast axis direction of the thermoplastic resin film, and nz is the refractive index in the thickness direction of the thermoplastic resin film. Yes, d (nm) is the thickness of the thermoplastic resin film. The slow axis refers to the direction in which the in-plane refractive index is maximized, and the fast axis refers to the direction perpendicular to the slow axis in the plane. Typically, Re and Rth are measured using light having a wavelength of 590 nm.
式(1)において、R1およびR2は、それぞれ独立して、水素または炭素数1~8のアルキル基であり、R3は、水素、炭素数1~18のアルキル基、炭素数3~12のシクロアルキル基、または炭素数5~15の芳香環を含む置換基である。式(2)において、R4およびR5は、それぞれ独立して、水素または炭素数1~8のアルキル基であり、R6は、水素、炭素数1~18のアルキル基、炭素数3~12のシクロアルキル基、または炭素数5~15の芳香環を含む置換基である。 Preferably, the glutarimide resin includes a structural unit represented by the following general formula (1) (hereinafter also referred to as a glutarimide unit) and a structural unit represented by the following general formula (2) (hereinafter referred to as (meta)). Also referred to as an acrylate unit).
In the formula (1), R 1 and R 2 are each independently hydrogen or an alkyl group having 1 to 8 carbon atoms, and R 3 is hydrogen, an alkyl group having 1 to 18 carbon atoms, or 3 to 3 carbon atoms. 12 a cycloalkyl group or a substituent containing an aromatic ring having 5 to 15 carbon atoms. In the formula (2), R 4 and R 5 are each independently hydrogen or an alkyl group having 1 to 8 carbon atoms, and R 6 is hydrogen, an alkyl group having 1 to 18 carbon atoms, or 3 to 3 carbon atoms. 12 a cycloalkyl group or a substituent containing an aromatic ring having 5 to 15 carbon atoms.
ハードコート層は、所定の分子量の硬化性化合物と高屈折率微粒子とを含むハードコート層形成用組成物を熱可塑性樹脂フィルムに塗布して形成される。より具体的には、ハードコート層は、所定の分子量の硬化性化合物と高屈折率微粒子とを含むハードコート層形成用組成物を熱可塑性樹脂フィルムに塗布し、その一部を熱可塑性樹脂フィルムに浸透させて形成される。好ましくは、ハードコート層形成用組成物の熱可塑性樹脂フィルムへの浸透と同時に熱可塑性樹脂フィルムを形成する熱可塑性樹脂のハードコート層形成用組成物の塗布層への溶出が生じる。 B. Hard coat layer The hard coat layer is formed by applying a composition for forming a hard coat layer containing a curable compound having a predetermined molecular weight and high refractive index fine particles to a thermoplastic resin film. More specifically, the hard coat layer is formed by applying a hard coat layer forming composition containing a curable compound having a predetermined molecular weight and high refractive index fine particles to a thermoplastic resin film, and a part of the hard coat layer is formed on the thermoplastic resin film. It is formed by infiltrating into. Preferably, elution of the thermoplastic resin that forms the thermoplastic resin film into the coating layer of the hard coat layer forming composition occurs simultaneously with the penetration of the hard coat layer forming composition into the thermoplastic resin film.
低屈折率層は、上記ハードコート層よりも低い屈折率を有する。低屈折率層をハードコート層上に積層することにより、得られる光学積層体の反射防止性が向上される。低屈折率層の屈折率は、好ましくは1.20~1.45、より好ましくは1.23~1.42である。 E. Low Refractive Index Layer The low refractive index layer has a lower refractive index than the hard coat layer. By laminating the low refractive index layer on the hard coat layer, the antireflection property of the obtained optical laminate is improved. The refractive index of the low refractive index layer is preferably 1.20 to 1.45, more preferably 1.23 to 1.42.
本発明の光学積層体の製造方法は、熱可塑性樹脂フィルム上にハードコート層形成用組成物を塗布して塗布層を形成し、該塗布層を加熱することを含む。好ましくは、該加熱後にハードコート層形成用組成物に硬化処理を施すことをさらに含む。低屈折率層を備える光学積層体を製造する場合は、加熱後の塗布層または硬化処理後のハードコート層上に低屈折率層形成用組成物を塗布し、任意に硬化処理を施すことをさらに含む。好ましくは、硬化処理後のハードコート層上に低屈折率層形成用組成物を塗布し、硬化処理を施す。 F. 2. Manufacturing method of optical laminated body The manufacturing method of the optical laminated body of this invention includes apply | coating the composition for hard-coat layer formation on a thermoplastic resin film, forming an application layer, and heating this application layer. Preferably, the method further includes subjecting the composition for forming a hard coat layer to a curing treatment after the heating. When producing an optical laminate comprising a low refractive index layer, the composition for forming a low refractive index layer is applied on the coating layer after heating or the hard coat layer after curing, and optionally subjected to curing treatment. In addition. Preferably, the composition for forming a low refractive index layer is applied on the hard coat layer after the curing treatment, and the curing treatment is performed.
基材層およびハードコート層の屈折率をアタゴ社製のアッベ屈折率計(商品名:DR-M2/1550)を用い、中間液としてモノブロモナフタレンを選択して測定した。
(2)ハードコート層の厚みおよび浸透深さ
実施例および比較例で得られた光学積層体の基材層側に、黒色アクリル板(三菱レイヨン社製、厚み2mm)を、厚み20μmのアクリル系粘着剤を介して貼着した。次いで、ハードコート層の反射スペクトルを、瞬間マルチ測光システム(大塚電子社製、商品名:MCPD3700)を用いて以下の条件で測定し、FFTスペクトルのピーク位置から、ハードコート層の厚みを評価した。なお屈折率は、上記(1)で測定した値を用いた。
・反射スペクトル測定条件
リファレンス:ミラー
アルゴリズム:FFT法
計算波長:450nm~850nm
・検出条件
露光時間:20ms
ランプゲイン:ノーマル
積算回数:10回
・FFT法
膜厚値の範囲:2~15μm
膜厚分解能:24nm
一方、下記積層体(R1)についての上記反射スペクトル測定により評価した。
・積層体(R1):基材フィルムとしてPET基材(東レ社製、商品名:U48-3、屈折率:1.60)を用い、塗布層の加熱温度を60℃とした以外は、実施例1と同様にして得た。
積層体(R1)に用いられるPET基材には、ハードコート層形成用組成物が浸透しないので、積層体(R1)から得られるFFTスペクトルのピーク位置から測定されるハードコート層の厚みは、実施例および比較例で得られた光学積層体のハードコート層の厚みよりも浸透深さの分だけ小さくなる。よって、(実施例および比較例で得られた光学積層体のハードコート層の厚み)から(積層体(R1)のハードコート層の厚み)を引くことによって、浸透深さが求められる。
(3)干渉ムラ
実施例および比較例で得られた光学積層体の基材層側に、黒色アクリル板(三菱レイヨン社製、厚み2mm)をアクリル系粘着剤を介して貼着した後、3波長蛍光灯下で、干渉ムラを目視観察し、以下の基準で評価した。
○:干渉ムラの発生無し
△:少し干渉ムラの発生が認められるが、実用上の問題はない
×:多くの干渉ムラの発生が認められ、実用上の問題となる
(4)鉛筆硬度
実施例および比較例で得られた光学積層体のハードコート層表面の鉛筆硬度をJIS K 5400に準拠して測定し、以下の基準で評価した。
○:2H以上
×:H以下 (1) Refractive index The refractive index of the base material layer and the hard coat layer was measured using an Abbe refractometer (trade name: DR-M2 / 1550) manufactured by Atago Co., Ltd., selecting monobromonaphthalene as an intermediate solution.
(2) Hard Coat Layer Thickness and Penetration Depth On the base layer side of the optical laminate obtained in the examples and comparative examples, a black acrylic plate (manufactured by Mitsubishi Rayon Co., Ltd., thickness 2 mm) and an acrylic system having a thickness of 20 μm It stuck through the adhesive. Next, the reflection spectrum of the hard coat layer was measured under the following conditions using an instantaneous multi-photometry system (trade name: MCPD3700, manufactured by Otsuka Electronics Co., Ltd.), and the thickness of the hard coat layer was evaluated from the peak position of the FFT spectrum. . In addition, the value measured by said (1) was used for the refractive index.
Reflection spectrum measurement conditions Reference: Mirror Algorithm: FFT method Calculation wavelength: 450 nm to 850 nm
・ Detection conditions Exposure time: 20 ms
Lamp gain: Normal Integration count: 10 times / FFT method Film thickness range: 2 to 15 μm
Film thickness resolution: 24nm
On the other hand, it evaluated by the said reflection spectrum measurement about the following laminated body (R1).
-Laminate (R1): Implemented except that a PET base material (trade name: U48-3, refractive index: 1.60) manufactured by Toray Industries, Inc. was used as the base film, and the heating temperature of the coating layer was 60 ° C. Obtained in the same manner as in Example 1.
Since the composition for forming a hard coat layer does not penetrate into the PET substrate used for the laminate (R1), the thickness of the hard coat layer measured from the peak position of the FFT spectrum obtained from the laminate (R1) is: It becomes smaller by the penetration depth than the thickness of the hard coat layer of the optical laminate obtained in the examples and comparative examples. Therefore, the penetration depth is determined by subtracting (thickness of hard coat layer of laminate (R1)) from (thickness of hard coat layer of optical laminate obtained in Examples and Comparative Examples).
(3) Interference unevenness After a black acrylic plate (Mitsubishi Rayon Co., Ltd., thickness 2 mm) was attached to the base layer side of the optical laminate obtained in Examples and Comparative Examples via an acrylic adhesive, 3 Interference unevenness was visually observed under a wavelength fluorescent lamp and evaluated according to the following criteria.
○: No interference unevenness Δ: Some interference unevenness is observed, but there is no practical problem ×: Many interference unevenness is recognized and becomes a practical problem (4) Pencil hardness Example And the pencil hardness of the hard coat layer surface of the optical laminated body obtained by the comparative example was measured based on JISK5400, and the following references | standards evaluated.
○: 2H or more ×: H or less
特開2010-284840号公報の製造例1に記載のイミド化MS樹脂(重量平均分子量:105,000)100重量部およびトリアジン系紫外線吸収剤(アデカ社製、商品名:T-712)0.62重量部を、2軸混練機にて220℃にて混合し、樹脂ペレットを作製した。得られた樹脂ペレットを、100.5kPa、100℃で12時間乾燥させ、単軸の押出機にてダイス温度270℃でTダイから押出してフィルム状に成形した(厚み160μm)。さらに当該フィルムを、その搬送方向に150℃の雰囲気下に延伸し(厚み80μm)、次いでフィルム搬送方向と直交する方向に150℃の雰囲気下に延伸して、厚み40μmの基材フィルムA((メタ)アクリル系樹脂フィルム)を得た。得られた基材フィルムAの波長380nmの光の透過率は8.5%、面内位相差Reは0.4nm、厚み方向位相差Rthは0.78nmであった。また得られた基材フィルムAの透湿度は、61g/m2・24hrであった。なお、光透過率は、日立ハイテク(株)社製の分光光度計(装置名称;U-4100)を用いて波長範囲200nm~800nmで透過率スペクトルを測定し、波長380nmにおける透過率を読み取った。また、位相差値は、王子計測機器(株)製 商品名「KOBRA21-ADH」を用いて、波長590nm、23℃で測定した。透湿度は、JIS K 0208に準じた方法により、温度40℃、相対湿度92%の条件で測定した。 <Production Example 1> Production of
硬化性化合物としてのウレタンアクリレートのオリゴマー(ダイセル・オルネクス社製、製品名「KRM8452」、Mw=1200、官能基数:10)80部およびペンタエリスリトールトリアクリレート(大阪有機化学工業社製、製品名「ビスコート#300」、Mw=298)20部と、ZrO2微粒子含有ゾル(日産化学社製、製品名「ナノユースOZ-S30K」、固形分:30%、平均粒子径:10nm、屈折率:2.2、溶媒:メチルイソブチルケトン)100部と、レベリング剤(DIC社製、商品名:PC4100)0.5部と、光重合開始剤(チバ・ジャパン社製、商品名:イルガキュア907)3部とを混合し、固形分濃度が50%となるように、メチルイソブチルケトンで希釈して、ハードコート層形成用組成物を調製した。 <Example 1>
Urethane acrylate oligomer as curable compound (Daicel Ornex, product name “KRM8452”, Mw = 1200, functional group number: 10) 80 parts and pentaerythritol triacrylate (Osaka Organic Chemical Co., product name “Biscoat” # 300 ", Mw = 298) 20 parts and, ZrO 2 fine particle-containing sol (manufactured by Nissan chemical Industries, Ltd., product name" Nanoyusu OZ-S30K ", solid content: 30%, average particle diameter: 10 nm, refractive index: 2.2 , Solvent: methyl isobutyl ketone), 0.5 part of a leveling agent (manufactured by DIC, trade name: PC4100), and 3 parts of a photopolymerization initiator (manufactured by Ciba Japan, trade name: Irgacure 907). Mix and dilute with methyl isobutyl ketone so that the solids concentration is 50%. Prepared.
ZrO2微粒子含有ゾルの配合量を67部としたこと以外は、実施例1と同様にして光学積層体を得た。 <Example 2>
An optical laminate was obtained in the same manner as in Example 1 except that the amount of the ZrO 2 fine particle-containing sol was 67 parts.
ZrO2微粒子含有ゾルの配合量を133部としたこと以外は、実施例1と同様にして光学積層体を得た。 <Example 3>
An optical laminate was obtained in the same manner as in Example 1 except that the blending amount of the ZrO 2 fine particle-containing sol was 133 parts.
ZrO2微粒子含有ゾル100部の代わりにSb2O5微粒子含有ゾル(日揮触媒化成社製、製品名「ELCOM V-4562」、固形分:30%、平均粒子径:15nm、屈折率:1.7、溶媒:メチルイソブチルケトン)133部を用いたこと以外は、実施例1と同様にして光学積層体を得た。 <Example 4>
Sb 2 O 5 fine particle-containing sol in place of ZrO 2 fine particle-containing
硬化性化合物としてウレタンアクリレートのオリゴマー(日本合成化学社製、製品名「UV1700B」、Mw=2000、官能基数:10)70部およびペンタエリスリトールトリアクリレート(大阪有機化学工業社製、製品名「ビスコート#300」、Mw=298)30部を用いたこと、および、ZrO2微粒子含有ゾルの配合量を133部にしたこと以外は、実施例1と同様にして光学積層体を得た。 <Example 5>
Urethane acrylate oligomer (product name “UV1700B”, product name “UV1700B”, Mw = 2000, functional group number: 10) 70 parts as a curable compound and pentaerythritol triacrylate (manufactured by Osaka Organic Chemical Industry Co., Ltd., product name “Biscoat #” 300 ”, Mw = 298) 30 parts were used, and an optical laminate was obtained in the same manner as in Example 1 except that the amount of the ZrO 2 fine particle-containing sol was 133 parts.
硬化性化合物としてウレタンアクリレートのオリゴマー(日本合成化学社製、製品名「UV1700B」、Mw=2000、官能基数:10)100部を用いたこと、ZrO2微粒子含有ゾルの配合量を133部にしたこと、および、塗布層の加熱温度を110℃とした以外は、実施例1と同様にして光学積層体を得た。 <Example 6>
100 parts of urethane acrylate oligomer (manufactured by Nippon Synthetic Chemical Co., Ltd., product name “UV1700B”, Mw = 2000, number of functional groups: 10) was used as the curable compound, and the amount of ZrO 2 fine particle-containing sol was 133 parts. In addition, an optical laminate was obtained in the same manner as in Example 1 except that the heating temperature of the coating layer was set to 110 ° C.
硬化性化合物としてペンタエリスリトールトリアクリレート(大阪有機化学工業社製、製品名「ビスコート#300」、Mw=298)100部を用いたこと、および、ZrO2微粒子含有ゾルの配合量を133部にしたこと以外は、実施例1と同様にして光学積層体を得た。 <Comparative Example 1>
100 parts of pentaerythritol triacrylate (manufactured by Osaka Organic Chemical Industry Co., Ltd., product name “Biscoat # 300”, Mw = 298) was used as the curable compound, and the blending amount of the ZrO 2 fine particle-containing sol was 133 parts. Except for this, an optical layered body was obtained in the same manner as in Example 1.
硬化性化合物としてジペンタエリスリトールヘキサアクリレート(DPHA)(新中村化学社製、製品名「A-DPH」、Mw=578)100部を用いたこと、ZrO2微粒子含有ゾルの配合量を133部にしたこと、および、塗布層の加熱温度を110℃としたこと以外は、実施例1と同様にして光学積層体を得た。 <Comparative example 2>
100 parts of dipentaerythritol hexaacrylate (DPHA) (manufactured by Shin-Nakamura Chemical Co., Ltd., product name “A-DPH”, Mw = 578) was used as the curable compound, and the blending amount of the ZrO 2 fine particle-containing sol was 133 parts. An optical laminate was obtained in the same manner as in Example 1 except that the heating temperature of the coating layer was 110 ° C.
硬化性化合物としてウレタンアクリレートのオリゴマー(ダイセル・オルネクス社製、製品名「KRM7804」、Mw=3000、官能基数:9)100部を用いたこと、ZrO2微粒子含有ゾルの配合量を133部にしたこと、および、塗布層の加熱温度を110℃としたこと以外は、実施例1と同様にして光学積層体を得た。 <Comparative Example 3>
Urethane acrylate oligomer (product name “KRM7804”, Mw = 3000, functional group number: 9) 100 parts was used as the curable compound, and the amount of ZrO 2 fine particle-containing sol was 133 parts. In addition, an optical layered body was obtained in the same manner as in Example 1 except that the heating temperature of the coating layer was 110 ° C.
硬化性化合物としてウレタンアクリレートのオリゴマー(日本合成化学社製、製品名「UV7620EA」、固形分:65%、Mw=4100、官能基数:9)154部を用いたこと、ZrO2微粒子含有ゾルの配合量を133部にしたこと、および、塗布層の加熱温度を110℃としたこと以外は、実施例1と同様にして光学積層体を得た。 <Comparative example 4>
Use of 154 parts of urethane acrylate oligomer (product name “UV7620EA”, solid content: 65%, Mw = 4100, number of functional groups: 9) as a curable compound, blend of ZrO 2 fine particle-containing sol An optical layered body was obtained in the same manner as in Example 1 except that the amount was 133 parts and the heating temperature of the coating layer was 110 ° C.
高屈折率微粒子含有ゾルを添加しなかったこと以外は、実施例1と同様にして光学積層体T1を得た。 [Reference Example 1]
An optical laminate T1 was obtained in the same manner as in Example 1 except that the high refractive index fine particle-containing sol was not added.
高屈折率微粒子含有ゾルを添加しなかったこと以外は、比較例3と同様にして光学積層体T2を得た。 [Reference Example 2]
An optical laminate T2 was obtained in the same manner as in Comparative Example 3 except that the high refractive index fine particle-containing sol was not added.
20 ハードコート層
22 浸透領域
30 低屈折率層
100、200 光学積層体 DESCRIPTION OF
Claims (8)
- 熱可塑性樹脂フィルムから形成される基材層と、
分子量が600~2500である硬化性化合物と屈折率が1.50以上である高屈折率微粒子とを含むハードコート層形成用組成物を該熱可塑性樹脂フィルムに塗布して形成されたハードコート層と、を備え、
該ハードコート層が、該ハードコート層形成用組成物が該熱可塑性樹脂フィルムに浸透して形成された浸透領域を含み、
該高屈折率微粒子が、該ハードコート層において、該基材層が設けられていない側の表面から厚み方向に向かって濃度が連続的に低くなるように偏析している、光学積層体。 A base material layer formed from a thermoplastic resin film;
A hard coat layer formed by coating a composition for forming a hard coat layer containing a curable compound having a molecular weight of 600 to 2500 and high refractive index fine particles having a refractive index of 1.50 or more on the thermoplastic resin film. And comprising
The hard coat layer includes an infiltration region formed by infiltrating the thermoplastic resin film with the hard coat layer forming composition;
The optical laminated body in which the high refractive index fine particles are segregated in the hard coat layer so that the concentration continuously decreases in the thickness direction from the surface on which the base material layer is not provided. - 前記硬化性化合物が、ウレタン(メタ)アクリレートおよび/またはウレタン(メタ)アクリレートのオリゴマーを含む、請求項1に記載の光学積層体。 The optical laminate according to claim 1, wherein the curable compound contains an oligomer of urethane (meth) acrylate and / or urethane (meth) acrylate.
- 前記ハードコート層において、相分離が生じていない、請求項1または2に記載の光学積層体。 The optical laminate according to claim 1 or 2, wherein no phase separation occurs in the hard coat layer.
- 前記熱可塑性樹脂フィルムが、(メタ)アクリル系樹脂フィルムである、請求項1から3のいずれかに記載の光学積層体。 The optical laminate according to any one of claims 1 to 3, wherein the thermoplastic resin film is a (meth) acrylic resin film.
- 前記ハードコート層が、前記基材層側表面から厚み方向に向かって濃度が連続的に低くなるように前記熱可塑性樹脂フィルムを形成する熱可塑性樹脂を含む、請求項1から4のいずれかに記載の光学積層体。 The hard coat layer includes a thermoplastic resin that forms the thermoplastic resin film so that the concentration continuously decreases in the thickness direction from the base layer side surface. The optical laminated body as described.
- 前記ハードコート層の前記基材層が設けられていない側に、低屈折率層をさらに備える、請求項1から5のいずれかに記載の光学積層体。 The optical laminate according to any one of claims 1 to 5, further comprising a low refractive index layer on a side of the hard coat layer on which the base material layer is not provided.
- 請求項1から6のいずれかに記載の光学積層体を含む、偏光フィルム。 A polarizing film comprising the optical laminate according to any one of claims 1 to 6.
- 請求項1から6のいずれかに記載の光学積層体を含む、画像表示装置。
The image display apparatus containing the optical laminated body in any one of Claim 1 to 6.
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020247003382A KR20240015752A (en) | 2013-09-30 | 2014-09-24 | Optical laminate |
KR1020167008273A KR20160065104A (en) | 2013-09-30 | 2014-09-24 | Optical laminate |
KR1020217008569A KR102632656B1 (en) | 2013-09-30 | 2014-09-24 | Optical laminate |
CN201480053650.0A CN105579871B (en) | 2013-09-30 | 2014-09-24 | Optical laminate |
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JP2013-203461 | 2013-09-30 | ||
JP2013203461A JP6235288B2 (en) | 2013-09-30 | 2013-09-30 | Optical laminate |
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WO2015046245A1 true WO2015046245A1 (en) | 2015-04-02 |
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PCT/JP2014/075276 WO2015046245A1 (en) | 2013-09-30 | 2014-09-24 | Optical laminate |
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KR (3) | KR20240015752A (en) |
CN (1) | CN105579871B (en) |
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WO (1) | WO2015046245A1 (en) |
Cited By (1)
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CN113574420A (en) * | 2019-03-18 | 2021-10-29 | 三菱瓦斯化学株式会社 | Laminate for antireflection film, and method for producing laminate for antireflection film |
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US10377913B2 (en) * | 2016-09-16 | 2019-08-13 | Corning Incorporated | High refractive index nanocomposites |
JP6937115B2 (en) * | 2016-12-13 | 2021-09-22 | 日東電工株式会社 | Optical laminate |
CN110476091B (en) * | 2017-03-28 | 2022-05-06 | 富士胶片株式会社 | High refractive index film and optical interference film |
KR102604388B1 (en) * | 2017-04-10 | 2023-11-22 | 닛토덴코 가부시키가이샤 | Optical laminates, polarizers, and image display devices |
KR102510766B1 (en) * | 2017-04-10 | 2023-03-17 | 닛토덴코 가부시키가이샤 | Optical laminate, polarizer, and image display device |
KR102032316B1 (en) * | 2018-07-09 | 2019-10-15 | 에스케이씨 주식회사 | Optical multilayer film, optical component and display device comprising same |
JP7343321B2 (en) * | 2019-07-23 | 2023-09-12 | 株式会社アドマテックス | Hard coat layer, method for manufacturing the same, transparent member, and method for manufacturing the same |
CN115989137A (en) * | 2020-08-27 | 2023-04-18 | 日东电工株式会社 | Hard-coated polarizing plate and image display device comprising same |
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JP2009066884A (en) * | 2007-09-12 | 2009-04-02 | Dainippon Printing Co Ltd | Manufacturing method of optical laminate, ooptical laminate, polarizing plate, and image display device |
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JP2004287392A (en) * | 2003-03-03 | 2004-10-14 | Toppan Printing Co Ltd | Optical film |
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CN102112309B (en) * | 2008-05-28 | 2015-01-28 | 东丽株式会社 | Laminated polyester film and antireflection film |
JP5764903B2 (en) * | 2009-12-18 | 2015-08-19 | 大日本印刷株式会社 | Manufacturing method of optical film |
CN102782527B (en) * | 2010-03-05 | 2015-02-18 | 株式会社大赛璐 | Optical film and method for producing the same |
JP6128629B2 (en) * | 2011-04-22 | 2017-05-17 | 日東電工株式会社 | Optical laminate |
JP2013142793A (en) * | 2012-01-11 | 2013-07-22 | Dainippon Printing Co Ltd | Hard coat film and production method of the same, and antireflection film |
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2013
- 2013-09-30 JP JP2013203461A patent/JP6235288B2/en active Active
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- 2014-09-24 KR KR1020247003382A patent/KR20240015752A/en active Search and Examination
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- 2014-09-24 KR KR1020167008273A patent/KR20160065104A/en active Application Filing
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Patent Citations (3)
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JP2002338702A (en) * | 2001-05-11 | 2002-11-27 | Kanegafuchi Chem Ind Co Ltd | Transparent film |
JP2006328329A (en) * | 2005-05-30 | 2006-12-07 | Kaneka Corp | Base material for surface-protective film and surface-protective film |
JP2009066884A (en) * | 2007-09-12 | 2009-04-02 | Dainippon Printing Co Ltd | Manufacturing method of optical laminate, ooptical laminate, polarizing plate, and image display device |
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CN113574420A (en) * | 2019-03-18 | 2021-10-29 | 三菱瓦斯化学株式会社 | Laminate for antireflection film, and method for producing laminate for antireflection film |
Also Published As
Publication number | Publication date |
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JP6235288B2 (en) | 2017-11-22 |
KR102632656B1 (en) | 2024-02-01 |
KR20240015752A (en) | 2024-02-05 |
TW201515840A (en) | 2015-05-01 |
KR20160065104A (en) | 2016-06-08 |
KR20210035331A (en) | 2021-03-31 |
TWI564153B (en) | 2017-01-01 |
CN105579871A (en) | 2016-05-11 |
CN105579871B (en) | 2018-01-19 |
JP2015069015A (en) | 2015-04-13 |
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