JP4906283B2 - Infrared absorption film - Google Patents
Infrared absorption film Download PDFInfo
- Publication number
- JP4906283B2 JP4906283B2 JP2005210337A JP2005210337A JP4906283B2 JP 4906283 B2 JP4906283 B2 JP 4906283B2 JP 2005210337 A JP2005210337 A JP 2005210337A JP 2005210337 A JP2005210337 A JP 2005210337A JP 4906283 B2 JP4906283 B2 JP 4906283B2
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- JP
- Japan
- Prior art keywords
- film
- particles
- layer
- infrared
- light transmittance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000010521 absorption reaction Methods 0.000 title claims description 41
- 239000010410 layer Substances 0.000 claims description 93
- 239000002245 particle Substances 0.000 claims description 70
- 238000002834 transmittance Methods 0.000 claims description 44
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 30
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- 229920005989 resin Polymers 0.000 claims description 26
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- 239000011342 resin composition Substances 0.000 claims description 22
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 239000006096 absorbing agent Substances 0.000 claims description 10
- 229910052792 caesium Inorganic materials 0.000 claims description 10
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 10
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 8
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- 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 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
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- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- LWRBVKNFOYUCNP-UHFFFAOYSA-N 2-methyl-1-(4-methylsulfanylphenyl)-2-morpholin-4-ylpropan-1-one Chemical compound C1=CC(SC)=CC=C1C(=O)C(C)(C)N1CCOCC1 LWRBVKNFOYUCNP-UHFFFAOYSA-N 0.000 description 2
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- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
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- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
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- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 2
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Images
Description
本発明は赤外線吸収フィルム、さらに詳しくは、８５０〜１３００ｎｍの近赤外領域の波長における光線の吸収能に優れると共に、良好な可視光線透過率を有し、かつ耐光性や耐候性に優れ、特にプラズマディスプレイ用の近赤外線吸収フィルムなどとして有用な赤外線吸収フィルムに関するものである。 The present invention is an infrared absorbing film, more specifically, has excellent light absorption ability in the near infrared wavelength range of 850 to 1300 nm, has good visible light transmittance, and excellent light resistance and weather resistance, The present invention relates to an infrared absorbing film useful as a near infrared absorbing film for a plasma display.
プラズマディスプレイ（ＰＤＰ）は、電極間のプラズマ放電により封入されているキセノンガスの分子を励起し、発生する紫外線で蛍光物質を励起し、可視光領域の光を発光させ映像を表示する装置である。
ＰＤＰにおいては、発光体より近赤外線を発することが知られている。この近赤外線は、コードレスホン、近赤外線リモートコントロール装置を使用するビデオデッキなど、周辺にある電子機器に作用し、正常な動作を阻害するおそれがあり、この近赤外線を極力遮断することが要求される。
さらに、ＰＤＰにおいては、表示面が平面であるため、外光が差し込んだ際に、広い範囲で反射した光が同時に目に入り、画面が見えにくくなる場合があり、外光の反射防止が必要である。また、ＰＤＰの発光を所定の透過率で透過させて、良好な画面表示をすることや、発光色の色調補正をすることも重要である。
ＰＤＰにおいては、これらの要求に対して、一般に表示画面に、（１）電磁波遮断フィルム、（２）近赤外線吸収フィルム及び（３）反射防止フィルムの少なくとも３枚の機能性フィルムを有する前面板を、該反射防止フィルムが、最表面（観察者側）になるように配置する処置が講ぜられている（例えば、特許文献１参照）。この場合、少なくとも３枚の機能性フィルムを別々に作製して、それらを貼合しなければならず、コストが高くつくのを免れない。
したがって、１枚のフィルムにおいて、近赤外線吸収層上に反射防止層を積層した複合機能性フィルムとすれば、コストリダクション効果は大きい。
近年、コストダウンの面から、最表面の反射防止フィルムにおいて、その基材の反射防止層とは反対側の面に近赤外線吸収層を設けることにより、１枚のフィルムで、反射防止性能と近赤外線吸収性能を兼ね備えた機能性フィルムが開発されている。このような機能性フィルムを製造する場合、（１）反射防止フィルムの裏面への近赤外線吸収層の形成、及び（２）近赤外線吸収フィルムの裏面への反射防止層の形成、の２つの方法があるが、いずれの場合も、フィルムのロスが発生するため、コストダウンの効果は小さい。
ＰＤＰに使用される近赤外線吸収フィルムは、現在、イモニウム系の有機系色素を主として利用したものであるが、この近赤外線吸収フィルムは耐光性や耐候性に劣り、経時により近赤外線吸収性能が劣化するという欠点を有している。
ＰＤＰ用の近赤外線吸収フィルムに対しては、近赤外線吸収性能に優れると共に、良好な耐光性や耐候性を有し、かつ可視光線透過率の高いものが要求されるが、これらを十分に満たす近赤外線吸収フィルムは、これまで見出されていないのが実状である。
他方、各種建築物や車両の窓などのいわゆる開口部は、太陽光線を取り入れるために透明なガラス板や樹脂板で構成されている。しかし、太陽光線には可視光線の他に紫外線や赤外線が含まれ、特に赤外線のうち８００〜２５００ｎｍの近赤外線は熱線と呼ばれ、開口部分から進入することにより室内の温度を上昇させる原因となる。
そこで近年では、各種建築物や車両の窓材などとして、可視光線を十分に取り入れながら熱線を遮蔽して、明るさを維持しつつ同時に室内の温度上昇を抑制する熱線遮蔽材が検討され、そのための各種手段が提案されている。
例えば、透明樹脂フィルムに金属を蒸着してなる熱線反射フィルムを、ガラス板、アクリル板、ポリカーボネート板などの透明基材に接着した熱線遮蔽板が提案されている（例えば、特許文献２参照）。しかしながら、このような金属を蒸着した熱線反射フィルムは、熱線遮蔽性能については優れているものの、透明性が悪く、可視光線を十分に取り入れることができない上、製造コストが高くつくなどの欠点を有している、
このような欠点を改良するために、近年、基材フィルム上に、赤外線遮蔽剤を含有する赤外線遮蔽層を設けてなる様々な赤外線遮蔽フィルムが提案されている（例えば、特許文献３、特許文献４参照）。
しかしながら、このような赤外線遮蔽フィルムに対しては、可視光線を良好に透過すると共に、近赤外領域の波長の光を効果的に遮蔽する機能を有し、かつ耐光性や耐候性が良好であって、経時により近赤外線吸収性能の劣化が抑制されたものが要求されるが、前記の赤外線遮蔽フィルムは、これらの要求性能を十分に満たしているとはいえない。
また、８００〜１１００ｎｍの近赤外領域における光線透過率が３０％以下で、可視光線透過率が高い赤外線吸収フィルタ（例えば、特許文献５参照）、８００〜１１００ｎｍの近赤外領域における光線透過率が２０％以下で、可視光線透過率が５０％以上である近赤外線遮蔽性減反射材（例えば、特許文献６参照）が開示されている。
しかしながら、８５０〜１３００ｎｍのより広い近赤外領域における光線透過率が１０％以下で、かつ可視光線透過率が６５％以上である赤外線吸収フィルムは、これまで開発されていない。
It is known that PDP emits near infrared rays from a light emitter. This near-infrared ray may affect peripheral electronic devices such as cordless phones and video decks that use a near-infrared remote control device, and may interfere with normal operation. It is required to block this near-infrared ray as much as possible. .
Furthermore, in the PDP, since the display surface is flat, when outside light is inserted, the light reflected in a wide range may enter the eyes at the same time, making the screen difficult to see, and it is necessary to prevent reflection of outside light. It is. It is also important to transmit the light emitted from the PDP with a predetermined transmittance to display a good screen and to correct the color tone of the emitted color.
In the PDP, in response to these requirements, a front plate having at least three functional films of (1) an electromagnetic wave shielding film, (2) a near infrared ray absorbing film, and (3) an antireflection film is generally provided on the display screen. Measures have been taken to arrange the antireflection film so as to be the outermost surface (observer side) (see, for example, Patent Document 1). In this case, at least three functional films must be prepared separately and bonded together, which is inevitable in cost.
Therefore, if a single functional film is a composite functional film in which an antireflection layer is laminated on a near infrared absorption layer, the cost reduction effect is large.
In recent years, from the viewpoint of cost reduction, by providing a near-infrared absorbing layer on the surface opposite to the antireflection layer of the base material in the outermost antireflection film, it is possible to achieve a near antireflection performance with a single film. Functional films that have infrared absorption performance have been developed. When manufacturing such a functional film, two methods of (1) formation of the near-infrared absorption layer on the back surface of the antireflection film and (2) formation of the antireflection layer on the back surface of the near-infrared absorption film However, in any case, film loss occurs, so the cost reduction effect is small.
Near-infrared absorbing films used for PDP are mainly made of immonium-based organic dyes, but these near-infrared absorbing films are inferior in light resistance and weather resistance, and near-infrared absorbing performance deteriorates with time. Has the disadvantage of
A near infrared absorbing film for PDP is required to have excellent near infrared absorbing performance, good light resistance and weather resistance, and high visible light transmittance. The reality is that no near-infrared absorbing film has been found so far.
On the other hand, so-called openings such as various buildings and vehicle windows are made of a transparent glass plate or resin plate for taking in sunlight. However, the sun rays include ultraviolet rays and infrared rays in addition to visible rays, and in particular, near infrared rays of 800 to 2500 nm out of infrared rays are called heat rays and cause the indoor temperature to rise by entering from the opening. .
Therefore, in recent years, as a window material for various buildings and vehicles, a heat ray shielding material that shields heat rays while sufficiently absorbing visible light and maintains the brightness while simultaneously suppressing the temperature rise in the room has been studied. Various means have been proposed.
For example, a heat ray shielding plate in which a heat ray reflective film obtained by vapor-depositing a metal on a transparent resin film is bonded to a transparent substrate such as a glass plate, an acrylic plate, or a polycarbonate plate has been proposed (see, for example, Patent Document 2). However, although the heat ray reflective film on which such a metal is deposited is excellent in heat ray shielding performance, it has disadvantages such as poor transparency, incapable of taking in sufficient visible light, and high production cost. is doing,
In order to improve such defects, in recent years, various infrared shielding films in which an infrared shielding layer containing an infrared shielding agent is provided on a substrate film have been proposed (for example, Patent Document 3 and Patent Document 3). 4).
However, for such an infrared shielding film, it has a function of transmitting visible light well, effectively shielding light of wavelengths in the near infrared region, and has good light resistance and weather resistance. Thus, a film in which deterioration of near-infrared absorption performance is suppressed over time is required, but the above-described infrared shielding film does not sufficiently satisfy these required performance.
In addition, an infrared absorption filter (see, for example, Patent Document 5) having a light transmittance of 30% or less in the near infrared region of 800 to 1100 nm and a high visible light transmittance, and a light transmittance in the near infrared region of 800 to 1100 nm. Is a near-infrared shielding and anti-reflective material having a visible light transmittance of 50% or more (for example, see Patent Document 6).
However, an infrared absorbing film having a light transmittance of 10% or less in a wider near infrared region of 850 to 1300 nm and a visible light transmittance of 65% or more has not been developed so far.
本発明は、このような事情のもとで、近赤外線吸収性能に優れると共に、可視光線透過率が高く、かつ耐光性や耐候性に優れ、経時により近赤外線吸収性能の劣化が抑制され、しかも製造コストが低く、ＰＤＰ用の近赤外線吸収フィルムとして、あるいは各種建築物や車両の窓材用などの熱線遮蔽フィルム等として好適な赤外線吸収フィルムを提供することを目的としてなされたものである。 Under such circumstances, the present invention has excellent near-infrared absorption performance, high visible light transmittance, excellent light resistance and weather resistance, and deterioration of near-infrared absorption performance over time is suppressed, The object of the present invention is to provide an infrared absorbing film which is low in production cost and suitable as a near infrared absorbing film for PDP or as a heat ray shielding film for window materials of various buildings and vehicles.
本発明者らは、前記の好ましい性質を有する赤外線吸収フィルムを開発すべく鋭意研究を重ねた結果、基材フィルムの一方の面に、無機系色素を含むエネルギー硬化型樹脂組成物からなる硬化物層を設けてなり、少なくとも波長８５０〜１３００ｎｍの全領域における光線透過率がある値以下で、かつ可視光線透過率がある値以上の赤外線吸収フィルムがその目的に適合し得ることを見出し、この知見に基づいて、本発明を完成するに至った。
すなわち、本発明は、
（１）ポリエステルからなる基材フィルムと、その一方の面に近赤外線吸収硬化物層を有するフィルムであって、該硬化物層は、多官能アクリレートからなる紫外線硬化型樹脂組成物中に、近赤外線吸収剤として、０.５μｍ以下の粒径のセシウム含有酸化タングステンを２０〜４０質量％を含有し、さらに防眩性付与剤として、メラミン系樹脂粒子、アクリル系樹脂粒子、アクリル−スチレン系共重合体粒子、ポリカーボネート系粒子、ポリエチレン系粒子、ポリスチレン系粒子若しくはベンゾグアナミン系樹脂粒子である平均粒径２〜１０μｍの有機樹脂粒子又は平均粒径が０.５〜１０μｍのシリカ粒子若しくはコロイド状シリカ粒子のアミン化合物による凝集物からなり平均粒径が０.５〜１０μｍの無機フィラー３〜８質量％を含有するものであって、前記フィルムは、少なくとも波長８５０〜１３００ｎｍの全領域における光線透過率が１０％以下であり、かつ可視光線透過率が６５％以上であることを特徴とする赤外線吸収フィルム、
（２）ポリエステルからなる基材フィルムと、その一方の面に近赤外線吸収硬化物層及び単層反射防止層を有するフィルムであって、前記近赤外線吸収硬化物層は、多官能アクリレートからなる紫外線硬化型樹脂組成物中に、０.５μｍ以下の粒径のセシウム含有酸化タングステンを２０〜４０質量％を含有し、さらに、防眩性付与剤として、メラミン系樹脂粒子、アクリル系樹脂粒子、アクリル−スチレン系共重合体粒子、ポリカーボネート系粒子、ポリエチレン系粒子、ポリスチレン系粒子若しくはベンゾグアナミン系樹脂粒子である平均粒径２〜１０μｍの有機樹脂粒子又は平均粒径が０.５〜１０μｍ程度のシリカ粒子若しくはコロイド状シリカ粒子のアミン化合物による凝集物からなり平均粒径が０.５〜１０μｍの無機フィラー３〜８質量％を含有するものであり、前記単層反射防止層は、多官能アクリレートからなる紫外線硬化型樹脂組成物中に、平均粒径２０〜１００μｍ、比重１.７〜１.９、屈折率１.２５〜１.３６の多孔性シリカを５０〜８０質量％含有するものであり、前記フィルムは、少なくとも波長８５０〜１３００ｎｍの全領域における光線透過率が１０％以下であり、かつ可視光線透過率が６５％以上であることを特徴とする赤外線吸収フィルム、
（３）ｘｙ色度座標において、ｘが０.２７〜０.３３を示し、かつｙが０.２８〜０.３４を示す上記(１)又は(２)項に記載の赤外線吸収フィルム、
（４）近赤外線吸収硬化物層又は単層反射防止層が、有機系及び／又は無機系帯電防止剤を含む上記(１)〜(３)項のいずれかに記載の赤外線吸収フィルム、
（５）基材フィルムの他方の面に粘着剤層を有する上記(１)〜(４)項のいずれかに記載の赤外線吸収フィルム、及び
（６）プラズマディスプレイ用である上記(１)〜(５)項のいずれかに記載の赤外線吸収フィルム、
を提供するものである。
As a result of intensive studies to develop an infrared absorbing film having the above-mentioned preferable properties, the present inventors have found that a cured product comprising an energy curable resin composition containing an inorganic dye on one surface of a base film. It is found that an infrared absorption film having a layer and having a light transmittance in a whole range of at least wavelengths of 850 to 1300 nm is not more than a certain value and having a visible light transmittance not less than a certain value can meet the purpose. Based on the above, the present invention has been completed.
That is, the present invention
(1) A base film made of polyester and a film having a near-infrared-absorbing cured product layer on one surface thereof, the cured product layer being in the vicinity of an ultraviolet curable resin composition made of a polyfunctional acrylate. As an infrared absorber, cesium-containing tungsten oxide having a particle size of 0.5 μm or less is contained in an amount of 20 to 40% by mass. Further, as an antiglare imparting agent, melamine resin particles, acrylic resin particles, acrylic-styrene copolymers are used. Polymer particles, polycarbonate-based particles, polyethylene-based particles, polystyrene-based particles or benzoguanamine-based resin particles, organic resin particles having an average particle diameter of 2 to 10 μm, silica particles or colloidal silica particles having an average particle diameter of 0.5 to 10 μm Containing 3 to 8% by mass of an inorganic filler having an average particle diameter of 0.5 to 10 μm. A than the film, infrared-absorbing film, wherein at least the light transmittance in the entire wavelength region of 850~1300nm is 10% or less, and is visible light transmittance of 65% or more,
(2) A base film made of polyester, and a film having a near-infrared absorption cured product layer and a single-layer antireflection layer on one surface thereof, wherein the near-infrared absorption cured product layer is an ultraviolet ray made of a polyfunctional acrylate. The curable resin composition contains 20 to 40% by mass of cesium-containing tungsten oxide having a particle size of 0.5 μm or less. Further, as an antiglare imparting agent, melamine resin particles, acrylic resin particles, acrylic -Styrenic copolymer particles, polycarbonate particles, polyethylene particles, polystyrene particles, or benzoguanamine resin particles having an average particle diameter of 2 to 10 μm or silica particles having an average particle diameter of about 0.5 to 10 μm Or the inorganic filler 3-8 which consists of the aggregate by the amine compound of a colloidal silica particle, and whose average particle diameter is 0.5-10 micrometers All SANYO containing amount%, the single-layer antireflection layer, the ultraviolet curable resin composition comprising a polyfunctional acrylate, the mean particle diameter of 20 to 100 [mu] m, a specific gravity of 1.7 to 1.9, the refractive index 1. The film contains 50 to 80% by mass of 1.25 to 1.36 porous silica, and the film has a light transmittance of 10% or less in a total region of at least a wavelength of 850 to 1300 nm and a visible light transmission. Infrared absorbing film characterized in that the rate is 65% or more ,
( 3 ) The infrared absorbing film according to (1) or (2) above, wherein x represents 0.27 to 0.33 and y represents 0.28 to 0.34 in the xy chromaticity coordinates,
( 4 ) The infrared absorption film according to any one of (1) to ( 3 ), wherein the near infrared absorption cured product layer or the single-layer antireflection layer contains an organic and / or inorganic antistatic agent,
( 5 ) The infrared ray absorbing film according to any one of (1) to ( 4 ) above having an adhesive layer on the other surface of the base film, and ( 6 ) the above (1) to (1) for plasma display 5 ) The infrared absorbing film according to any one of
Is to provide.
本発明によれば、８５０〜１３００ｎｍの近赤外領域の波長における光線吸収性能に優れると共に、可視光線透過率が高く、かつ耐光性や耐候性に優れ、経時により近赤外線吸収性能の劣化が抑制され、しかも製造コストが低い赤外線吸収フィルムを提供することができる。
この赤外線吸収フィルムは、ＰＤＰ用の近赤外線吸収フィルムとして、あるいは各種建築物や車両の窓材用などの熱線遮蔽フィルム等として用いることができるが、特にＰＤＰ用の近赤外線吸収フィルムとして好適である。
According to the present invention, the light absorption performance at a wavelength in the near infrared region of 850 to 1300 nm is excellent, the visible light transmittance is high, the light resistance and the weather resistance are excellent, and the deterioration of the near infrared absorption performance is suppressed over time. In addition, it is possible to provide an infrared absorption film with low manufacturing cost.
This infrared absorbing film can be used as a near infrared absorbing film for PDP or as a heat ray shielding film for windows of various buildings and vehicles, etc., but is particularly suitable as a near infrared absorbing film for PDP. .
本発明の赤外線吸収フィルムは、基材フィルムと、その一方の面に設けられた無機系色素を含むエネルギー硬化型樹脂組成物からなる硬化物層を有している。
前記基材フィルムについては特に制限はなく、従来赤外線吸収フィルムの基材として公知のプラスチックフィルムの中から適宜選択して用いることができる。このようなプラスチックフィルムとしては、例えば、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリエチレンナフタレートなどのポリエステルフィルム、ポリエチレンフィルム、ポリプロピレンフィルム、セロファン、ジアセチルセルロースフィルム、トリアセチルセルロースフィルム、アセチルセルロースブチレートフィルム、ポリ塩化ビニルフィルム、ポリ塩化ビニリデンフィルム、ポリビニルアルコールフィルム、エチレン−酢酸ビニル共重合体フィルム、ポリスチレンフィルム、ポリカーボネートフィルム、ポリメチルペンテンフィルム、ポリスルホンフィルム、ポリエーテルエーテルケトンフィルム、ポリエーテルスルホンフィルム、ポリエーテルイミドフィルム、ポリイミドフィルム、フッ素樹脂フィルム、ポリアミドフィルム、アクリル樹脂フィルム、ノルボルネン系樹脂フィルム、シクロオレフィン樹脂フィルム等を挙げることができる。
これらの基材フィルムは、透明、半透明のいずれであってもよく、また、着色されていてもよいし、無着色のものでもよく、用途に応じて適宜選択すればよい。
これらの基材フィルムの厚さは特に制限はなく、適宜選定されるが、通常１５〜２５０μｍ、好ましくは３０〜２００μｍの範囲である。また、この基材フィルムは、その表面に設けられる層との密着性を向上させる目的で、所望により片面又は両面に、酸化法や凹凸化法などにより表面処理を施すことができる。上記酸化法としては、例えばコロナ放電処理、プラズマ処理、クロム酸処理（湿式）、火炎処理、熱風処理、オゾン・紫外線照射処理などが挙げられ、また、凹凸化法としては、例えばサンドブラスト法、溶剤処理法などが挙げられる。これらの表面処理法は基材フィルムの種類に応じて適宜選ばれるが、一般にはコロナ放電処理法が効果及び操作性などの面から、好ましく用いられる。また、片面又は両面にプライマー処理を施したものも用いることができる。
The infrared absorption film of the present invention has a cured product layer made of an energy curable resin composition containing a base film and an inorganic pigment provided on one surface thereof.
There is no restriction | limiting in particular about the said base film, It can select suitably from well-known plastic films as a base material of a conventional infrared rays absorption film, and can use it. Examples of such plastic films include polyester films such as polyethylene terephthalate, polybutylene terephthalate, and polyethylene naphthalate, polyethylene films, polypropylene films, cellophane, diacetyl cellulose films, triacetyl cellulose films, acetyl cellulose butyrate films, and polychlorinated. Vinyl film, polyvinylidene chloride film, polyvinyl alcohol film, ethylene-vinyl acetate copolymer film, polystyrene film, polycarbonate film, polymethylpentene film, polysulfone film, polyether ether ketone film, polyether sulfone film, polyetherimide film , Polyimide film, fluororesin film, Li amide film, acrylic resin film, norbornene resin film, a cycloolefin resin film.
These base films may be either transparent or translucent, may be colored, or may be uncolored, and may be appropriately selected depending on the application.
The thickness of these substrate films is not particularly limited and is appropriately selected, but is usually 15 to 250 μm, preferably 30 to 200 μm. Moreover, this base film can be surface-treated by an oxidation method, a concavo-convex method, or the like on one side or both sides as desired for the purpose of improving adhesion to a layer provided on the surface. Examples of the oxidation method include corona discharge treatment, plasma treatment, chromic acid treatment (wet), flame treatment, hot air treatment, ozone / ultraviolet irradiation treatment, and examples of the unevenness method include a sand blast method, a solvent, and the like. Treatment methods and the like. These surface treatment methods are appropriately selected according to the type of the base film, but generally, the corona discharge treatment method is preferably used from the viewpoints of effects and operability. Moreover, what gave the primer process to the single side | surface or both surfaces can also be used.
本発明の赤外線吸収フィルムにおいては、前記基材フィルムの少なくとも一方の面に、無機系色素を含むエネルギー硬化型樹脂組成物からなる硬化物層（以下、無機系色素含有硬化物層と称することがある。）が設けられている。
ここで、エネルギー硬化型樹脂組成物としては、熱硬化型樹脂組成物又は活性エネルギー線硬化型樹脂組成物を挙げることができる。
熱硬化型樹脂組成物としては、特に制限はなく、従来公知のものの中から、適宜選択して用いることができる。この熱硬化型樹脂組成物は、一般に熱硬化性樹脂を基本成分とし、さらに所望により他の樹脂及び硬化剤などを含有するものである。
上記熱硬化性樹脂としては、例えば炭素−炭素二重結合やグリシジル基を有するアクリレート系重合体、不飽和ポリエステル、イソプレン重合体、ブタジエン重合体、エポキシ樹脂、フェノール樹脂、尿素樹脂、メラミン樹脂などが挙げられる。これらは単独で用いてもよいし、２種以上を組み合わせて用いてもよい。
また、他の樹脂としては、ビニル樹脂、ウレタン樹脂、ポリエステル、ポリアミド、ポリカーボネート、ポリイミド、ニトリル樹脂、シリコーン樹脂などが挙げられる。これらの樹脂は、塗工液の粘度を調節したり、硬化物層に所望の物性を付与するために用いられるものであり、単独で用いても、２種以上を組み合わせて用いてもよい。
In the infrared absorption film of the present invention, a cured product layer (hereinafter referred to as an inorganic pigment-containing cured product layer) made of an energy curable resin composition containing an inorganic pigment is formed on at least one surface of the substrate film. Is provided).
Here, examples of the energy curable resin composition include a thermosetting resin composition and an active energy ray curable resin composition.
There is no restriction | limiting in particular as a thermosetting resin composition, From the conventionally well-known thing, it can select suitably and can be used. This thermosetting resin composition generally comprises a thermosetting resin as a basic component, and further contains other resins and a curing agent as required.
Examples of the thermosetting resin include an acrylate polymer having a carbon-carbon double bond and a glycidyl group, an unsaturated polyester, an isoprene polymer, a butadiene polymer, an epoxy resin, a phenol resin, a urea resin, and a melamine resin. Can be mentioned. These may be used alone or in combination of two or more.
Examples of other resins include vinyl resin, urethane resin, polyester, polyamide, polycarbonate, polyimide, nitrile resin, and silicone resin. These resins are used for adjusting the viscosity of the coating liquid or imparting desired physical properties to the cured product layer, and may be used alone or in combination of two or more.
さらに、硬化剤としては、例えばジベンゾイルペルオキシド、ジラウロイルペルオキシド、ｔ−ブチルぺルオキシベンゾエート、ジ−２−エチルヘキシルペルオキシジカーボネートなどの有機過酸化物、２,２'−アゾビスイソブチロニトリル、２,２'−アゾビス−２−メチルブチロニトリル、２,２'−アゾビスジメチルバレロニトリルなどのアゾ化合物、トリレンジイソシアネート、ジフェニルメタンジイソシアネート、イソホロンジイソシアネート、ヘキサメチレンジイソシアネートなどのポリイソシアネート化合物、フェニレンジアミン、ヘキサメチレンテトラミン、イソホロンジアミン、ジアミノジフェニルメタンなどのポリアミン類、ドデセニル無水コハク酸、無水フタル酸、テトラヒドロ無水フタル酸などの酸無水物、２−メチルイミダゾール、２−エチルイミダゾール、２−フェニルイミダゾールなどのイミダゾール類やジシアンジアミド、ｐ−トルエンスルホン酸、トリフルオロメタンスルホン酸などのルイス酸、ホルムアルデヒドなどが挙げられる。これらの硬化剤は、使用する熱硬化性樹脂の種類に応じて適宜選択される。
一方、活性エネルギー線硬化型樹脂組成物は、活性エネルギー線硬化性化合物を基本成分とし、所望により光重合開始剤などを含有するものである。
ここで、活性エネルギー線硬化性化合物とは、電磁波又は荷電粒子線の中でエネルギー量子を有するもの、すなわち、紫外線又は電子線などを照射することにより、架橋、硬化する化合物を指す。
このような活性エネルギー線硬化性化合物としては、例えば活性エネルギー線重合性プレポリマー及び／又は活性エネルギー線重合性モノマーを挙げることができる。上記活性エネルギー線重合性プレポリマーには、ラジカル重合型とカチオン重合型があり、ラジカル重合型の活性エネルギー線重合性プレポリマーとしては、例えばポリエステルアクリレート系、エポキシアクリレート系、ウレタンアクリレート系、ポリオールアクリレート系などが挙げられる。ここで、ポリエステルアクリレート系プレポリマーとしては、例えば多価カルボン酸と多価アルコールの縮合によって得られる両末端に水酸基を有するポリエステルオリゴマーの水酸基を(メタ)アクリル酸でエステル化することにより、あるいは、多価カルボン酸にアルキレンオキシドを付加して得られるオリゴマーの末端の水酸基を(メタ)アクリル酸でエステル化することにより得ることができる。
Further, examples of the curing agent include organic peroxides such as dibenzoyl peroxide, dilauroyl peroxide, t-butyl peroxybenzoate, and di-2-ethylhexyl peroxydicarbonate, and 2,2′-azobisisobutyronitrile. 2,2′-azobis-2-methylbutyronitrile, azo compounds such as 2,2′-azobisdimethylvaleronitrile, polyisocyanate compounds such as tolylene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate, phenylene Polyamines such as diamine, hexamethylenetetramine, isophoronediamine, diaminodiphenylmethane, acid anhydrides such as dodecenyl succinic anhydride, phthalic anhydride, tetrahydrophthalic anhydride, Imidazole, 2-ethylimidazole, 2-imidazoles and dicyandiamide, such as phenylimidazole, p- toluenesulfonic acid, Lewis acids such as trifluoromethanesulfonic acid, formaldehyde. These curing agents are appropriately selected according to the type of thermosetting resin to be used.
On the other hand, the active energy ray-curable resin composition contains an active energy ray-curable compound as a basic component and optionally contains a photopolymerization initiator.
Here, the active energy ray-curable compound refers to a compound having energy quanta in an electromagnetic wave or a charged particle beam, that is, a compound that is crosslinked and cured by irradiation with ultraviolet rays or electron beams.
Examples of such an active energy ray-curable compound include an active energy ray-polymerizable prepolymer and / or an active energy ray-polymerizable monomer. The active energy ray polymerizable prepolymer includes a radical polymerization type and a cationic polymerization type. Examples of the radical polymerization type active energy ray polymerizable prepolymer include polyester acrylate, epoxy acrylate, urethane acrylate, and polyol acrylate. The system etc. are mentioned. Here, as the polyester acrylate-based prepolymer, for example, by esterifying the hydroxyl group of a polyester oligomer having a hydroxyl group at both ends obtained by condensation of a polyvalent carboxylic acid and a polyhydric alcohol with (meth) acrylic acid, or It can be obtained by esterifying the terminal hydroxyl group of an oligomer obtained by adding an alkylene oxide to a polyvalent carboxylic acid with (meth) acrylic acid.
エポキシアクリレート系プレポリマーは、例えば、比較的低分子量のビスフェノール型エポキシ樹脂やノボラック型エポキシ樹脂のオキシラン環に、(メタ)アクリル酸を反応しエステル化することにより得ることができる。ウレタンアクリレート系プレポリマーは、例えば、ポリエーテルポリオールやポリエステルポリオールとポリイソシアネートの反応によって得られるポリウレタンオリゴマーを、(メタ)アクリル酸でエステル化することにより得ることができる。さらに、ポリオールアクリレート系プレポリマーは、ポリエーテルポリオールの水酸基を(メタ)アクリル酸でエステル化することにより得ることができる。これらの活性エネルギー線重合性プレポリマーは１種用いてもよいし、２種以上を組み合わせて用いてもよい。
一方、カチオン重合型の活性エネルギー線重合性プレポリマーとしては、エポキシ系樹脂が通常使用される。このエポキシ系樹脂としては、例えばビスフェノール樹脂やノボラック樹脂などの多価フェノール類にエピクロルヒドリンなどでエポキシ化した化合物、直鎖状オレフィン化合物や環状オレフィン化合物を過酸化物などで酸化して得られた化合物などが挙げられる。
活性エネルギー線重合性モノマーとしては、例えば１,４−ブタンジオールジ(メタ)アクリレート、１,６−ヘキサンジオールジ(メタ)アクリレート、ネオペンチルグリコールジ(メタ)アクリレート、ポリエチレングリコールジ(メタ)アクリレート、ネオペンチルグリコールアジペートジ(メタ)アクリレート、ヒドロキシピバリン酸ネオペンチルグリコールジ(メタ)アクリレート、ジシクロペンタニルジ(メタ)アクリレート、カプロラクトン変性ジシクロペンテニルジ(メタ)アクリレート、エチレンオキシド変性リン酸ジ(メタ)アクリレート、アリル化シクロヘキシルジ(メタ)アクリレート、イソシアヌレートジ(メタ)アクリレート、トリメチロールプロパントリ(メタ)アクリレート、ジペンタエリスリトールトリ(メタ)アクリレート、プロピオン酸変性ジペンタエリスリトールトリ(メタ)アクリレート、ペンタエリスリトールトリ(メタ)アクリレート、プロピレンオキシド変性トリメチロールプロパントリ(メタ)アクリレート、トリス(アクリロキシエチル)イソシアヌレート、プロピオン酸変性ジペンタエリスリトールペンタ(メタ)アクリレート、ジペンタエリスリトールヘキサ(メタ)アクリレート、カプロラクトン変性ジペンタエリスリトールヘキサ(メタ)アクリレートなどの多官能アクリレートが挙げられる。これらの活性エネルギー線重合性モノマーは１種用いてもよいし、２種以上を組み合わせて用いてもよく、また、前記活性エネルギー線重合性プレポリマーと併用してもよい。
The epoxy acrylate prepolymer can be obtained, for example, by reacting (meth) acrylic acid with an oxirane ring of a relatively low molecular weight bisphenol type epoxy resin or novolak type epoxy resin and esterifying it. The urethane acrylate-based prepolymer can be obtained, for example, by esterifying a polyurethane oligomer obtained by reaction of polyether polyol or polyester polyol and polyisocyanate with (meth) acrylic acid. Furthermore, the polyol acrylate-based prepolymer can be obtained by esterifying the hydroxyl group of the polyether polyol with (meth) acrylic acid. These active energy ray polymerizable prepolymers may be used alone or in combination of two or more.
On the other hand, as a cationic polymerization type active energy ray polymerizable prepolymer, an epoxy resin is usually used. Examples of the epoxy resins include compounds obtained by epoxidizing polyphenols such as bisphenol resins and novolac resins with epichlorohydrin, etc., and compounds obtained by oxidizing a linear olefin compound or a cyclic olefin compound with a peroxide or the like. Etc.
Examples of active energy ray polymerizable monomers include 1,4-butanediol di (meth) acrylate, 1,6-hexanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, and polyethylene glycol di (meth) acrylate. , Neopentyl glycol adipate di (meth) acrylate, hydroxypivalate neopentyl glycol di (meth) acrylate, dicyclopentanyl di (meth) acrylate, caprolactone-modified dicyclopentenyl di (meth) acrylate, ethylene oxide-modified diphosphate ( (Meth) acrylate, allylated cyclohexyl di (meth) acrylate, isocyanurate di (meth) acrylate, trimethylolpropane tri (meth) acrylate, dipentaerythritol tri (meth) acrylate, propionic acid modified Dipentaerythritol tri (meth) acrylate, pentaerythritol tri (meth) acrylate, propylene oxide modified trimethylolpropane tri (meth) acrylate, tris (acryloxyethyl) isocyanurate, propionic acid modified dipentaerythritol penta (meth) acrylate, Examples thereof include polyfunctional acrylates such as dipentaerythritol hexa (meth) acrylate and caprolactone-modified dipentaerythritol hexa (meth) acrylate. These active energy ray polymerizable monomers may be used alone or in combination of two or more thereof, or may be used in combination with the active energy ray polymerizable prepolymer.
所望により用いられる光重合開始剤としては、ラジカル重合型の活性エネルギー線重合性プレポリマーや活性エネルギー線重合性モノマーに対しては、例えばベンゾイン、ベンゾインメチルエーテル、ベンゾインエチルエーテル、ベンゾインイソプロピルエーテル、ベンゾイン−ｎ−ブチルエーテル、ベンゾインイソブチルエーテル、アセトフェノン、ジメチルアミノアセトフェノン、２,２−ジメトキシ−２−フェニルアセトフェノン、２,２−ジエトキシ−２−フェニルアセトフェノン、２−ヒドロキシ−２−メチル−１−フェニルプロパン−１−オン、１−ヒドロキシシクロヘキシルフェニルケトン、２−メチル−１−[４−(メチルチオ)フェニル]−２−モルフォリノ−プロパン−１−オン、４−(２−ヒドロキシエトキシ)フェニル−２(ヒドロキシ−２−プロプル)ケトン、ベンゾフェノン、ｐ−フェニルベンゾフェノン、４,４'−ジエチルアミノベンゾフェノン、ジクロロベンゾフェノン、２−メチルアントラキノン、２−エチルアントラキノン、２−ターシャリ−ブチルアントラキノン、２−アミノアントラキノン、２−メチルチオキサントン、２−エチルチオキサントン、２−クロロチオキサントン、２,４−ジメチルチオキサントン、２,４−ジエチルチオキサントン、ベンジルジメチルケタール、アセトフェノンジメチルケタール、ｐ−ジメチルアミン安息香酸エステルなどが挙げられる。また、カチオン重合型の活性エネルギー線重合性プレポリマーに対する光重合開始剤としては、例えば芳香族スルホニウムイオン、芳香族オキソスルホニウムイオン、芳香族ヨードニウムイオンなどのオニウムと、テトラフルオロボレート、ヘキサフルオロホスフェート、ヘキサフルオロアンチモネート、ヘキサフルオロアルセネートなどの陰イオンとからなる化合物が挙げられる。これらは１種用いてもよいし、２種以上を組み合わせて用いてもよく、また、その配合量は、前記活性エネルギー線重合性プレポリマー及び／又は活性エネルギー線重合性モノマー１００質量部に対して、通常０.２〜１０質量部の範囲で選ばれる。 As photopolymerization initiators used as desired, for radical polymerization type active energy ray polymerizable prepolymers and active energy ray polymerizable monomers, for example, benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin -N-butyl ether, benzoin isobutyl ether, acetophenone, dimethylaminoacetophenone, 2,2-dimethoxy-2-phenylacetophenone, 2,2-diethoxy-2-phenylacetophenone, 2-hydroxy-2-methyl-1-phenylpropane- 1-one, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- [4- (methylthio) phenyl] -2-morpholino-propan-1-one, 4- (2-hydroxyethoxy) phenyl-2 Roxy-2-propyl) ketone, benzophenone, p-phenylbenzophenone, 4,4′-diethylaminobenzophenone, dichlorobenzophenone, 2-methylanthraquinone, 2-ethylanthraquinone, 2-tert-butylanthraquinone, 2-aminoanthraquinone, 2- Examples include methylthioxanthone, 2-ethylthioxanthone, 2-chlorothioxanthone, 2,4-dimethylthioxanthone, 2,4-diethylthioxanthone, benzyldimethyl ketal, acetophenone dimethyl ketal, p-dimethylamine benzoate, and the like. Examples of the photopolymerization initiator for the cationic polymerization type active energy ray polymerizable prepolymer include oniums such as aromatic sulfonium ions, aromatic oxosulfonium ions and aromatic iodonium ions, tetrafluoroborate, hexafluorophosphate, Examples thereof include compounds composed of anions such as hexafluoroantimonate and hexafluoroarsenate. These may be used alone or in combination of two or more thereof, and the blending amount thereof is based on 100 parts by mass of the active energy ray polymerizable prepolymer and / or the active energy ray polymerizable monomer. In general, it is selected in the range of 0.2 to 10 parts by mass.
前記の熱硬化型樹脂組成物又は活性エネルギー線硬化型樹脂組成物に含有させる無機系色素（無機系近赤外線吸収剤）については、少なくとも波長８５０〜１３００ｎｍの全領域における光線透過率が１０％以下で、かつ可視光線透過率が６５％以上である赤外線吸収フィルムを与えることのできるものであればよく、特に制限されず、様々な種類のものを適宜選択して用いることができる。
当該無機系色素としては、例えば、酸化タングステン系化合物、酸化チタン、酸化ジルコニウム、酸化タンタル、酸化ニオブ、酸化亜鉛、酸化インジウム、錫ドープ酸化インジウム(ＩＴＯ)、酸化錫、アンチモンドープ酸化錫(ＡＴＯ)、酸化セシウム、硫化亜鉛、さらにはＬａＢ6、ＣｅＢ6、ＰｒＢ6、ＮｄＢ6、ＧｄＢ6、ＴｂＢ6、ＤｙＢ6、ＨｏＢ6、ＹＢ6、ＳｍＢ6、ＥｕＢ6、ＥｒＢ6、ＴｍＢ6、ＹｂＢ6、ＬｕＢ6、ＳｒＢ6、ＣａＢ6、(Ｌａ，Ｃｅ)Ｂ6などの六ホウ化物等が挙げられる。これらの中では、近赤外線の吸収率が高く、かつ可視光線の透過率が高いことから、酸化タングステン系化合物が好ましく、特にセシウム含有酸化タングステンが好適である。
一般に、有機系色素（有機系近赤外線吸収剤）と無機系色素を比較した場合、近赤外線の吸収能力は有機系の方が優れているが、耐光性や耐候性については、無機系の方が格段に優れている。また、有機系のものは着色しやすいという欠点も有している上、１１００〜１３００ｎｍの領域における光線透過率を１０％以下にすることは困難である。
したがって、本発明においては無機系色素が用いられ、特にセシウム含有酸化タングステンの使用が好ましい。この無機系色素は、可視光領域において吸収が少なく、かつ透明なコート層を形成するには、好ましくは０.５μｍ以下、より好ましくは０.１μｍ以下の粒径を有するものが有利である。
About the inorganic pigment | dye (inorganic near-infrared absorber) contained in the said thermosetting resin composition or active energy ray curable resin composition, the light transmittance in the whole area | region of wavelength 850-1300nm is 10% or less at least. And what is necessary is just a thing which can provide the infrared rays absorption film whose visible light transmittance | permeability is 65% or more, and it does not restrict | limit, Various types can be selected and used suitably.
Examples of the inorganic dye include tungsten oxide compounds, titanium oxide, zirconium oxide, tantalum oxide, niobium oxide, zinc oxide, indium oxide, tin-doped indium oxide (ITO), tin oxide, and antimony-doped tin oxide (ATO). , Cesium oxide, zinc sulfide, and LaB 6 , CeB 6 , PrB 6 , NdB 6 , GdB 6 , TbB 6 , DyB 6 , HoB 6 , YB 6 , SmB 6 , EuB 6 , ErB 6 , TmB 6 , YbB 6 And hexaboride such as LuB 6 , SrB 6 , CaB 6 and (La, Ce) B 6 . Among these, tungsten oxide compounds are preferred, and cesium-containing tungsten oxide is particularly preferred because of its high near-infrared absorptivity and high visible light transmittance.
In general, when comparing organic dyes (organic near-infrared absorbers) and inorganic dyes, near-infrared absorption capacity is superior to organic ones, but light resistance and weather resistance are better for inorganic ones. Is much better. In addition, organic materials have a drawback that they are easily colored, and it is difficult to reduce the light transmittance in the region of 1100 to 1300 nm to 10% or less.
Accordingly, inorganic dyes are used in the present invention, and the use of cesium-containing tungsten oxide is particularly preferable. In order to form a transparent coat layer with little absorption in the visible light region, the inorganic dye preferably has a particle size of preferably 0.5 μm or less, more preferably 0.1 μm or less.
本発明においては、前記無機系色素は１種用いてもよいし、２種以上を組み合わせて用いてもよく、また、本発明の目的が損なわれない範囲で、所望により有機系色素と併用することができる。ここで、有機系色素としては、例えばシアニン系化合物、スクワリリウム系化合物、チオールニッケル錯塩系化合物、ナフタロシアニン系化合物、フタロシアニン系化合物、トリアリルメタン系化合物、ナフトキノン系化合物、アントラキノン系化合物、さらにはＮ,Ｎ,Ｎ',Ｎ'−テトラキス(ｐ−ジ−ｎ−ブチルアミノフェニル)−ｐ−フェニレンジアミニウムの過塩素酸塩、フェニレンジアミニウムの塩素塩、フェニレンジアミニウムのヘキサフルオロアンチモン酸塩、フェニレンジアミニウムのフッ化ホウ素酸塩、フェニレンジアミニウムのフッ素塩、フェニレンジアミニウムの過塩素酸塩などのアミノ化合物やイモニウム化合物、銅化合物とビスチオウレア化合物、リン化合物と銅化合物、リン酸エステル化合物と銅化合物との反応により得られるリン酸エステル銅化合物などが挙げられる。
これらの中では、チオールニッケル錯塩系化合物（特開平９−２３０１３４号公報など）及びフタロシアニン系化合物が好ましく、特に、特開２０００−２６７４８号公報などに開示されているフッ素含有フタロシアニン化合物が、有機系色素の中で、可視光線透過率が高く、かつ良好な耐熱性、耐光性、耐候性などを有することから、好適である。
なお、無機系色素を単独使用した場合、たとえ波長が８５０〜１３００ｎｍの領域で光線透過率が１０％を超える部分があったり、あるいは可視光線透過率が６５％未満であったとしても、２種以上を併用（少なくとも１つは無機系色素）することにより、波長８５０〜１３００ｎｍの全領域における光線透過率が、１０％以下で、かつ可視光線透過率が６５％以上であればよい。
本発明における前記無機系色素の使用量は、硬化物層中の無機系色素の含有量が、通常１０〜６０質量％、好ましくは２０〜４０質量％になるように選定される。
In the present invention, one kind of inorganic dye may be used, or two or more kinds may be used in combination, and it is used in combination with an organic dye as desired so long as the object of the present invention is not impaired. be able to. Here, examples of the organic dye include cyanine compounds, squarylium compounds, thiol nickel complex compounds, naphthalocyanine compounds, phthalocyanine compounds, triallylmethane compounds, naphthoquinone compounds, anthraquinone compounds, and N , N, N ′, N′-tetrakis (p-di-n-butylaminophenyl) -p-phenylenediaminium perchlorate, phenylenediaminium chloride, phenylenediaminium hexafluoroantimonate, Amino and imonium compounds such as phenylenediaminium fluorinated boronate, phenylenediaminium fluoride, phenylenediaminium perchlorate, copper compounds and bisthiourea compounds, phosphorus compounds and copper compounds, phosphate ester compounds Reaction of copper with copper compounds The obtained phosphoric acid ester copper compound etc. are mentioned.
Among these, a thiol nickel complex salt compound (JP-A-9-230134, etc.) and a phthalocyanine compound are preferable. In particular, a fluorine-containing phthalocyanine compound disclosed in JP-A-2000-26748 is an organic compound. Among dyes, it is preferable because it has high visible light transmittance and good heat resistance, light resistance, weather resistance and the like.
When an inorganic dye is used alone, there are two types even if the light transmittance exceeds 10% in the wavelength range of 850 to 1300 nm or the visible light transmittance is less than 65%. By using the above in combination (at least one is an inorganic pigment), the light transmittance in the entire region with a wavelength of 850 to 1300 nm may be 10% or less and the visible light transmittance may be 65% or more.
The amount of the inorganic dye used in the present invention is selected so that the content of the inorganic dye in the cured product layer is usually 10 to 60% by mass, preferably 20 to 40% by mass.
本発明においては、無機系色素含有硬化物層には、防眩性付与剤として、有機及び／又は無機フィラーを含有させることができる。有機フィラーとしては、例えばメラミン系樹脂粒子、アクリル系樹脂粒子、アクリル−スチレン系共重合体粒子、ポリカーボネート系粒子、ポリエチレン系粒子、ポリスチレン系粒子、ベンゾグアナミン系樹脂粒子などが挙げられる。これらの有機フィラーの平均粒径は、通常２〜１０μｍ程度である。
また、無機フィラーとしては、例えば平均粒径が０.５〜１０μｍ程度のシリカ粒子や、コロイド状シリカ粒子のアミン化合物による凝集物であって、平均粒径が０.５〜１０μｍ程度のものなどを挙げることができる。
これらの防眩性付与剤は１種を単独で用いてもよいし、２種以上を組み合わせて用いてもよく、当該硬化物層中のその含有量は、通常２〜１５質量％、好ましくは３〜８質量％である。当該硬化物層に防眩性付与剤を含有させることにより、本発明の赤外線吸収フィルムの６０°グロス値は、通常３０〜１２０となる。
本発明において、基材フィルムの一方の面に無機系色素含有硬化物層を形成させるには、例えば以下に示す方法を用いることができる。
まず、（１）無機系色素を含む熱硬化型樹脂組成物、又は（２）無機系色素を含む活性エネルギー線硬化型樹脂組成物を調製する。
前記（１）の無機系色素を含む熱硬化型樹脂組成物は、前述の熱硬化性樹脂と、無機系色素を含む近赤外線吸収剤と、所望により用いられる前述の他の樹脂、硬化剤、防眩性付与剤、さらには各種添加剤、例えば酸化防止剤、紫外線吸収剤、レベリング剤、消泡剤などを、それぞれ所定の割合で加えることにより、調製することができる。
一方、前記（２）の無機系色素を含む活性エネルギー線硬化型樹脂組成物は、前述の活性エネルギー線硬化性化合物と、無機系色素を含む近赤外線吸収剤と、所望により用いられる前述の光重合開始剤、防眩性付与剤、さらには各種添加剤、例えば酸化防止剤、紫外線吸収剤、光安定剤、レベリング剤、消泡剤などを、それぞれ所定の割合で加えることにより、調製することができる。
In the present invention, the inorganic pigment-containing cured product layer can contain an organic and / or inorganic filler as an antiglare property-imparting agent. Examples of the organic filler include melamine resin particles, acrylic resin particles, acrylic-styrene copolymer particles, polycarbonate particles, polyethylene particles, polystyrene particles, and benzoguanamine resin particles. These organic fillers usually have an average particle size of about 2 to 10 μm.
Examples of the inorganic filler include silica particles having an average particle diameter of about 0.5 to 10 μm, and aggregates of colloidal silica particles with an amine compound having an average particle diameter of about 0.5 to 10 μm. Can be mentioned.
One of these antiglare imparting agents may be used alone, or two or more thereof may be used in combination, and the content thereof in the cured product layer is usually 2 to 15% by mass, preferably 3 to 8% by mass. By including the antiglare property-imparting agent in the cured product layer, the 60 ° gloss value of the infrared absorption film of the present invention is usually 30 to 120.
In the present invention, for example, the following method can be used to form the inorganic pigment-containing cured product layer on one surface of the base film.
First, (1) a thermosetting resin composition containing an inorganic dye, or (2) an active energy ray curable resin composition containing an inorganic dye is prepared.
The thermosetting resin composition containing the inorganic dye of the above (1) includes the above-mentioned thermosetting resin, a near-infrared absorber containing an inorganic dye, and the other resins and curing agents used as desired. It can be prepared by adding an antiglare property-imparting agent and various additives such as an antioxidant, an ultraviolet absorber, a leveling agent, an antifoaming agent and the like at a predetermined ratio.
On the other hand, the active energy ray-curable resin composition containing the inorganic dye (2) includes the above-mentioned active energy ray-curable compound, a near-infrared absorber containing an inorganic dye, and the above-described light used as desired. Preparation by adding a polymerization initiator, an antiglare agent, and various additives such as an antioxidant, an ultraviolet absorber, a light stabilizer, a leveling agent, an antifoaming agent, etc. in a predetermined ratio. Can do.
次に、適当な溶剤に、前記（１）の無機系色素を含む熱硬化型樹脂組成物、又は（２）の無機系色素を含む活性エネルギー線硬化型樹脂組成物を加え、それぞれ熱硬化型塗工液又は活性エネルギー線硬化型塗工液を調製する。
この際用いる溶剤としては、例えばヘキサン、ヘプタン、シクロヘキサンなどの脂肪族炭化水素、トルエン、キシレンなどの芳香族炭化水素、塩化メチレン、塩化エチレンなどのハロゲン化炭化水素、メタノール、エタノール、プロパノール、ブタノール、１−メトキシ−２−プロパノールなどのアルコール、アセトン、メチルエチルケトン、２−ペンタノン、メチルイソブチルケトン、イソホロンなどのケトン、酢酸エチル、酢酸ブチルなどのエステル、エチルセロソルブなどのセロソルブ系溶剤などが挙げられる。
このようにして調製された塗工液の濃度、粘度としては、コーティング可能な濃度、粘度であればよく、特に制限されず、状況に応じて適宜選定することができる。
次に、基材フィルムの一方の面に、上記塗工液を、従来公知の方法、例えばバーコート法、ナイフコート法、ロールコート法、ブレードコート法、ダイコート法、グラビアコート法などを用いて、コーティングして塗膜を形成させ、乾燥させる。
塗工液が熱硬化型の場合は、恒温槽や赤外加熱灯などを用いて加熱硬化させるのがよい。これにより無機系色素含有硬化物層が形成される。加熱条件としては、温度は１００〜１３０℃の範囲が好ましく、加熱時間は２分ないし５分間程度で十分である。
一方、塗工液が活性エネルギー線硬化型である場合には、前記乾燥塗膜に活性エネルギー線を照射して該塗膜を硬化させることにより、無機系色素含有硬化物層が形成される。
活性エネルギー線としては、例えば紫外線や電子線などが挙げられる。上記紫外線は、高圧水銀ランプ、フュージョンＨランプ、キセノンランプなどで得られる。一方電子線は、電子線加速器などによって得られる。この活性エネルギー線の中では、特に紫外線が好適である。なお、電子線を使用する場合は、重合開始剤を添加することなく、硬化物層を得ることができる。
Next, the thermosetting resin composition containing the inorganic dye of the above (1) or the active energy ray curable resin composition containing the inorganic dye of the above (2) is added to an appropriate solvent. A coating solution or an active energy ray-curable coating solution is prepared.
Examples of the solvent used in this case include aliphatic hydrocarbons such as hexane, heptane, and cyclohexane, aromatic hydrocarbons such as toluene and xylene, halogenated hydrocarbons such as methylene chloride and ethylene chloride, methanol, ethanol, propanol, butanol, Examples include alcohols such as 1-methoxy-2-propanol, ketones such as acetone, methyl ethyl ketone, 2-pentanone, methyl isobutyl ketone, and isophorone, esters such as ethyl acetate and butyl acetate, and cellosolv solvents such as ethyl cellosolve.
The concentration and viscosity of the coating solution thus prepared are not particularly limited as long as the concentration and viscosity can be coated, and can be appropriately selected depending on the situation.
Next, the coating liquid is applied to one surface of the base film using a conventionally known method such as a bar coating method, a knife coating method, a roll coating method, a blade coating method, a die coating method, or a gravure coating method. Coating to form a coating and drying.
When the coating liquid is a thermosetting type, it is preferable to heat and cure using a thermostatic bath or an infrared heating lamp. Thereby, an inorganic pigment-containing cured product layer is formed. As heating conditions, the temperature is preferably in the range of 100 to 130 ° C., and the heating time is about 2 to 5 minutes.
On the other hand, when the coating liquid is an active energy ray curable type, an inorganic dye-containing cured material layer is formed by irradiating the dry coating film with an active energy ray to cure the coating film.
Examples of the active energy rays include ultraviolet rays and electron beams. The ultraviolet rays can be obtained with a high-pressure mercury lamp, a fusion H lamp, a xenon lamp, or the like. On the other hand, the electron beam is obtained by an electron beam accelerator or the like. Among these active energy rays, ultraviolet rays are particularly preferable. In addition, when using an electron beam, a hardened | cured material layer can be obtained, without adding a polymerization initiator.
本発明においては、得られる赤外線吸収フィルムに、優れた耐擦傷性を付与し得る点から、熱硬化型塗工液よりも、活性エネルギー線硬化型塗工液の方が好ましい。
また、この無機系色素含有硬化物層の厚さは２〜１５μｍの範囲が好ましく、より好ましくは４〜１０μｍである。
本発明の赤外線吸収フィルムが、例えばＰＤＰ用として用いられる場合には、必要に応じ、無機系色素含有硬化物層上に、反射防止層を設けることができる。
この反射防止層の形成方法については特に制限はなく、従来公知の方法、例えばドライプロセス法及びウェットプロセス法のいずれも用いることができるが、本発明においては、ウェットプロセス法により、活性エネルギー線照射による硬化樹脂と多孔性シリカ粒子とを含む低屈折率層からなる反射防止層を設けることが好ましい。
この活性エネルギー線照射による硬化樹脂と多孔性シリカ粒子とを含む低屈折率層は、例えば活性エネルギー線硬化性化合物と、多孔性シリカ粒子と、所望により光重合開始剤などを含む低屈折率層形成用塗工液を、無機系色素含有硬化物層上にコーティングして塗膜を形成させ、活性エネルギー線を照射して、該塗膜を硬化させることにより、形成することができる。
前記の活性エネルギー線硬化性化合物及び所望により用いられる光重合開始剤については、前述の無機系色素含有硬化物層の説明において示したとおりである。
この低屈折率層に含まれる多孔性シリカ粒子としては、比重が１.７〜１.９、屈折率が１.２５〜１.３６及び平均粒径が２０〜１００ｎｍの範囲にあるものが好ましく用いられる。このような性状を有する多孔性シリカ粒子を用いることにより、反射防止性能に優れる反射防止層が１層タイプの赤外線吸収フィルムを得ることができる。
本発明においては、この低屈折率層中の多孔性シリカ粒子の含有量は、好ましくは３０〜８０質量％の範囲で選定される。該多孔性シリカ粒子の含有量が上記範囲にあれば、当該低屈折率層は所望の低屈折率を有する層となり、得られる赤外線吸収フィルムは、反射防止性に優れたものとなる。該多孔性シリカ粒子の好ましい含有量は、５０〜８０質量％であり、特に６０〜７５質量％の範囲が好ましい。
In the present invention, the active energy ray curable coating liquid is more preferable than the thermosetting coating liquid from the viewpoint that the obtained infrared absorbing film can be provided with excellent scratch resistance.
Moreover, the thickness of this inorganic pigment containing cured | curing material layer has the preferable range of 2-15 micrometers, More preferably, it is 4-10 micrometers.
When the infrared ray absorbing film of the present invention is used, for example, for PDP, an antireflection layer can be provided on the inorganic pigment-containing cured product layer as necessary.
There is no particular limitation on the method for forming the antireflection layer, and any conventionally known method, for example, a dry process method or a wet process method can be used. In the present invention, active energy ray irradiation is performed by a wet process method. It is preferable to provide an antireflection layer composed of a low refractive index layer containing a cured resin and porous silica particles.
The low refractive index layer containing a cured resin and porous silica particles by this active energy ray irradiation is, for example, a low refractive index layer containing an active energy ray curable compound, porous silica particles, and a photopolymerization initiator as required. It can be formed by coating the forming coating liquid on the inorganic pigment-containing cured product layer to form a coating film, irradiating active energy rays and curing the coating film.
About the said active energy ray hardening compound and the photoinitiator used depending on necessity, it is as having shown in description of the above-mentioned inorganic pigment containing hardened material layer.
As the porous silica particles contained in the low refractive index layer, those having a specific gravity of 1.7 to 1.9, a refractive index of 1.25 to 1.36 and an average particle size of 20 to 100 nm are preferable. Used. By using porous silica particles having such properties, it is possible to obtain an infrared absorption film having a single-layer type antireflection layer excellent in antireflection performance.
In the present invention, the content of the porous silica particles in the low refractive index layer is preferably selected in the range of 30 to 80% by mass. When the content of the porous silica particles is in the above range, the low refractive index layer becomes a layer having a desired low refractive index, and the obtained infrared absorbing film has excellent antireflection properties. The preferable content of the porous silica particles is 50 to 80% by mass, and particularly preferably 60 to 75% by mass.
当該低屈折率層は、厚さが５０〜２００ｎｍ、好ましくは７０〜１３０ｎｍであって、屈折率が、１.４３以下、好ましくは１.３０〜１.４２、さらに好ましくは１.３５〜１.４０の範囲にあるものが好適である。当該低屈折率層の厚さや屈折率が上記範囲にあれば、反射防止性能、及び耐擦傷性に優れる赤外線吸収フィルムを得ることができる。
なお、この低屈折率層の下層の無機系色素含有硬化物層の屈折率は、通常１.４７〜１.６０、好ましくは１.４９〜１.５５の範囲である。
本発明において用いられるこの低屈折率層形成用塗工液は、必要に応じ、適当な溶剤中に、前記の活性エネルギー線硬化性化合物と、多孔性シリカ粒子と、所望により用いられる前記の光重合開始剤、さらには各種添加剤、例えば酸化防止剤、紫外線吸収剤、光安定剤、レベリング剤、消泡剤などを、それぞれ所定の割合で加え、溶解又は分散させることにより、調製することができる。
この際用いる溶剤については、前述の無機系色素含有硬化物層形成用塗工液の説明において示したとおりである。
このようにして調製された塗工液の濃度、粘度としては、コーティング可能な濃度、粘度であればよく、特に制限されず、状況に応じて適宜選定することができる。
無機系色素含有硬化物層上に、この塗工液を、従来公知の方法、例えばバーコート法、ナイフコート法、ロールコート法、ブレードコート法、ダイコート法、グラビアコート法などを用いて、コーティングして塗膜を形成させ、乾燥後、これに活性エネルギー線を照射して該塗膜を硬化させることにより、所望の低屈折率層が形成される。
活性エネルギー線については、前述の無機系色素含有硬化物層の説明において示したとおりである。
The low refractive index layer has a thickness of 50 to 200 nm, preferably 70 to 130 nm, and a refractive index of 1.43 or less, preferably 1.30 to 1.42, more preferably 1.35 to 1. Those in the range of .40 are preferred. If the thickness and refractive index of the low refractive index layer are in the above ranges, an infrared absorbing film excellent in antireflection performance and scratch resistance can be obtained.
In addition, the refractive index of the inorganic dye containing cured | curing material layer of the lower layer of this low-refractive-index layer is normally 1.47-1.60, Preferably it is the range of 1.49-1.55.
The coating solution for forming a low refractive index layer used in the present invention comprises the above-mentioned active energy ray-curable compound, porous silica particles, and the above-mentioned light used as required, in an appropriate solvent, if necessary. It can be prepared by adding a polymerization initiator and further various additives such as an antioxidant, an ultraviolet absorber, a light stabilizer, a leveling agent, an antifoaming agent, etc. in a predetermined ratio and dissolving or dispersing them. it can.
About the solvent used in this case, it is as having shown in description of the coating liquid for inorganic pigment containing cured | curing material layer formation mentioned above.
The concentration and viscosity of the coating solution thus prepared are not particularly limited as long as the concentration and viscosity can be coated, and can be appropriately selected depending on the situation.
The coating liquid is coated on the inorganic dye-containing cured product layer using a conventionally known method such as a bar coating method, a knife coating method, a roll coating method, a blade coating method, a die coating method, or a gravure coating method. Then, a coating film is formed, and after drying, an active energy ray is irradiated to cure the coating film, whereby a desired low refractive index layer is formed.
About an active energy ray, it is as having shown in description of the above-mentioned inorganic pigment | dye containing hardened | cured material layer.
本発明において、無機系色素含有硬化物層の形成を、活性エネルギー線硬化型の塗工液を用いて形成する場合、無機系色素含有硬化物層及び低屈折率層の形成は、以下に示す方法で行うのが有利である。
まず、基材フィルムの一方の面に無機系色素含有硬化物形成用の活性エネルギー線硬化型塗工液をコーティングして塗膜を形成させ、活性エネルギー線を照射してハーフキュア状態に硬化させる。この際、紫外線を照射する場合には、光量は、通常５０〜１５０ｍＪ／ｃｍ2程度である。次いで、このようにして形成されたハーフキュア状態の硬化層上に、低屈折率層形成用塗工液をコーティングして塗膜を形成させ、活性エネルギー線を十分に照射し、前記ハーフキュア状態の硬化層と共に完全に硬化させる。この際、紫外線を照射する場合、光量は、通常４００〜１０００ｍＪ／ｃｍ2程度である。なお、無機系色素含有硬化物層及び／又は低屈折率層を完全に硬化させる際は、酸素による硬化阻害を防ぐために、窒素ガスなどの雰囲気下で、活性エネルギー線を照射することができる。この場合、酸素濃度は低い方がよく、２容量％以下が好ましい。
このようにして、基材フィルムの一方の面に、無機系色素含有硬化物層及び低屈折率層を、順にかつ層間密着性よく、形成することができる。
本発明の赤外線吸収フィルムにおいては、無機系色素含有硬化物層又は反射防止層に、有機系及び／又は無機系帯電防止剤を含有させることができる。この帯電防止剤を含有させることにより、得られる赤外線吸収フィルムには、埃や塵などが付着しにくくなる。
有機系帯電防止剤としては特に制限はなく、従来公知の非イオン系、アニオン系、カチオン系、両性系帯電防止剤の中から選ばれる少なくとも１種が用いられる。これらの中で、効果及び均質分散性などの点から、分子内に１個以上の四級アンモニウム塩基を有するカチオン系帯電防止剤が好適である。
In the present invention, when forming the inorganic dye-containing cured material layer using an active energy ray-curable coating liquid, the formation of the inorganic dye-containing cured material layer and the low refractive index layer is shown below. It is advantageous to do so.
First, an active energy ray-curable coating liquid for forming an inorganic pigment-containing cured product is coated on one surface of a base film to form a coating film, and then irradiated with active energy rays to be cured to a half-cure state. . In this case, when irradiating with ultraviolet rays, the amount of light is usually about 50 to 150 mJ / cm 2 . Next, a coating film is formed by coating a coating liquid for forming a low refractive index layer on the cured layer in the half-cured state thus formed, and the half-cured state is sufficiently irradiated with active energy rays. And completely cured together with the cured layer. Under the present circumstances, when irradiating an ultraviolet-ray, a light quantity is about 400-1000mJ / cm < 2 > normally. When the inorganic dye-containing cured product layer and / or the low refractive index layer is completely cured, active energy rays can be irradiated in an atmosphere of nitrogen gas or the like in order to prevent curing inhibition by oxygen. In this case, the oxygen concentration is preferably low and is preferably 2% by volume or less.
In this way, an inorganic pigment-containing cured product layer and a low refractive index layer can be formed in order and with good interlayer adhesion on one surface of the substrate film.
In the infrared absorption film of the present invention, an organic and / or inorganic antistatic agent can be contained in the inorganic pigment-containing cured product layer or antireflection layer. By including this antistatic agent, it becomes difficult for dust, dust, and the like to adhere to the obtained infrared absorbing film.
The organic antistatic agent is not particularly limited, and at least one selected from conventionally known nonionic, anionic, cationic, and amphoteric antistatic agents is used. Of these, cationic antistatic agents having one or more quaternary ammonium bases in the molecule are preferred from the standpoint of effects and homogeneous dispersibility.
四級アンモニウム塩基を有するカチオン系帯電防止剤は、低分子型及び高分子型のいずれも使用することができるが、効果の持続性及びブリードアウトやガス発生の防止性などの点から、高分子型カチオン系帯電防止剤が好ましい。
上記高分子型カチオン系帯電防止剤としては、従来公知のものの中から、任意のものを適宜選択して用いることができる。具体的には、分子内に、一般式（Ｉ）
で表される四級アンモニウム塩基を有する高分子重合体を好ましく挙げることができる。
上記一般式（Ｉ）において、Ｒ1及びＲ2で示されるアルキル基並びにＲ3のうちのアルキル基としては、炭素数１〜６のアルキル基、特に炭素数１〜４のアルキル基が好ましく、また、Ｒ3のうちのアラルキル基としては、ベンジル基が好ましい。炭素数１〜４のアルキル基としては、メチル基、エチル基、ｎ−プロピル基、イソプロピル基、ｎ−ブチル基、イソブチル基、ｓｅｃ−ブチル基、ｔｅｒｔ−ブチル基が挙げられる。
一方、Ｘn-は無機陰イオン、有機陰イオンのいずれであってもよく、その例としてはＦ-、Ｃｌ-、Ｂｒ-、Ｉ-のハロゲンイオン、ＮＯ3 -、ＣｌＯ4 -、ＢＦ4 -、ＣＯ3 2-、ＳＯ4 2-などの無機陰イオン、ＣＨ3ＯＳＯ3 -、Ｃ2Ｈ5ＯＳＯ3 -、さらには酢酸、マロン酸、コハク酸、マレイン酸、フマル酸、ｐ−トルエンスルホン酸、トリフルオロ酢酸などの有機酸の残基からなる有機陰イオンが挙げられる。
As the cationic antistatic agent having a quaternary ammonium base, either a low molecular type or a high molecular type can be used. However, in terms of durability of the effect and prevention of bleeding out and gas generation, the polymer Type cationic antistatic agents are preferred.
As the polymer-type cationic antistatic agent, an arbitrary one can be appropriately selected from conventionally known ones. Specifically, in the molecule, the general formula (I)
Preferred examples include a polymer having a quaternary ammonium base represented by the formula:
In the general formula (I), the alkyl group represented by R 1 and R 2 and the alkyl group in R 3 are preferably an alkyl group having 1 to 6 carbon atoms, particularly an alkyl group having 1 to 4 carbon atoms, The aralkyl group in R 3 is preferably a benzyl group. Examples of the alkyl group having 1 to 4 carbon atoms include methyl group, ethyl group, n-propyl group, isopropyl group, n-butyl group, isobutyl group, sec-butyl group, and tert-butyl group.
On the other hand, X n− may be either an inorganic anion or an organic anion. Examples thereof include halogen ions of F − , Cl − , Br − and I − , NO 3 − , ClO 4 − and BF 4. -, CO 3 2-, SO 4 2- , etc. of the inorganic anion, CH 3 OSO 3 -, C 2 H 5 OSO 3 -, more acetic acid, malonic acid, succinic acid, maleic acid, fumaric acid, p- toluene Examples include organic anions composed of residues of organic acids such as sulfonic acid and trifluoroacetic acid.
このような高分子型四級アンモニウム塩系帯電防止剤としては、例えば以下に示す化合物、すなわち、ポリビニルベンジル型［（ａ）］、ポリ(メタ)アクリレート型［（ｂ）］、スチレン−(メタ)アクリレート共重合体型［（ｃ）］、スチレン−マレイミド共重合体型［（ｄ）］、メタクリレート−メタクリルイミド共重合体型［（ｅ）］などを挙げることができる。なお、（ｃ）、（ｄ）及び（ｅ）の共重合体型においては、ランダム共重合体型及びブロック共重合体型のいずれであってもよい。
一方、低分子型カチオン系帯電防止剤としては、例えば、一般式（II）
で表される四級アンモニウム塩基を有する化合物を好ましく挙げることができる。
上記一般式（II）におけるＡの例としては、ラウリル基などのドデシル基、ミリスチル基などのテトラデシル基、パルミチル基などのヘキサデシル基、ステアリル基などのオクタデシル基、エイコシル基、ベヘニル基などが挙げられる。
また、Ｒ4、Ｒ5、Ｒ6、Ｙm-及びｍは、それぞれ一般式（Ｉ）におけるＲ1、Ｒ2、Ｒ3、Ｘn-及びｎと同じである。
本発明においては、この低分子型カチオン系帯電防止剤は１種用いてもよいし、２種以上を組み合わせて用いてもよい。
さらに、本発明においては、帯電防止剤として、分子内に１個以上の四級アンモニウム塩基及び１個以上の重合性不飽和基を有する反応性カチオン系帯電防止剤を用いてもよい。
このような反応性カチオン系帯電防止剤を用いることにより、熱エネルギーを印加又は活性エネルギー線を照射した際に、前述の熱硬化性又は活性エネルギー線硬化性化合物と共重合して、形成される高分子鎖内に取り込まれるため、得られる赤外線吸収フィルムは、帯電防止性能の持続性が向上する。
この反応性カチオン系帯電防止剤としては、例えば一般式（III）
で表される反応性四級アンモニウム塩系化合物などを挙げることができる。
Examples of such a polymer type quaternary ammonium salt antistatic agent include the following compounds, that is, polyvinylbenzyl type [(a)], poly (meth) acrylate type [(b)], styrene- (meta ) Acrylate copolymer type [(c)], styrene-maleimide copolymer type [(d)], and methacrylate-methacrylimide copolymer type [(e)]. The copolymer types (c), (d) and (e) may be either a random copolymer type or a block copolymer type.
On the other hand, as a low molecular type cationic antistatic agent, for example, the general formula (II)
The compound which has the quaternary ammonium base represented by these can be mentioned preferably.
Examples of A in the general formula (II) include dodecyl groups such as lauryl groups, tetradecyl groups such as myristyl groups, hexadecyl groups such as palmityl groups, octadecyl groups such as stearyl groups, eicosyl groups, and behenyl groups. .
R 4 , R 5 , R 6 , Y m− and m are the same as R 1 , R 2 , R 3 , X n− and n in the general formula (I), respectively.
In the present invention, the low molecular weight cationic antistatic agent may be used singly or in combination of two or more.
Furthermore, in the present invention, a reactive cationic antistatic agent having one or more quaternary ammonium bases and one or more polymerizable unsaturated groups in the molecule may be used as the antistatic agent.
By using such a reactive cationic antistatic agent, it is formed by copolymerization with the aforementioned thermosetting or active energy ray-curable compound when heat energy is applied or active energy rays are irradiated. Since it is taken into the polymer chain, the resulting infrared absorbing film has improved antistatic performance sustainability.
Examples of the reactive cationic antistatic agent include, for example, the general formula (III)
The reactive quaternary ammonium salt type compound etc. which are represented by these can be mentioned.
本発明においては、この反応性カチオン系帯電防止剤は１種用いてもよいし、２種以上を組み合わせて用いてもよい。また、前記高分子型カチオン系帯電防止剤、低分子型カチオン系帯電防止剤及び反応性カチオン系帯電防止剤を適当に組み合わせて用いることができる。
一方、無機系帯電防止剤としては特に制限はなく、従来公知の透明導電フィラー、あるいはテトラアルコキシシランの加水分解、縮合反応により得られるシラノール基を有するシリカゾル、シラノール基やその他親水性基を有するシロキサン系ポリマーなどを用いることができる。これらの無機系帯電防止剤は１種用いてもよいし、２種以上を組み合わせて用いてもよく、また、前記有機系帯電防止剤と併用してもよい。
本発明においては、無機系色素含有硬化物層又は反射防止層中の前記帯電防止剤の含有量は、その種類に応じて適宜選定されるが、例えば有機系帯電防止剤の場合、通常２〜２５質量％の範囲で選定される。該帯電防止剤の含有量が上記範囲にあれば、赤外線吸収フィルムは、良好な帯電防止性能を発揮すると共に、他の性能に悪影響を及ぼすことがない。この含有量は、好ましくは３〜２５質量％、より好ましくは５〜２０質量％の範囲である。ここで、帯電防止性能としては、例えば表面抵抗率が、通常温湿度条件下（２３℃、５０％ＲＨ）で、３×１０13（Ω／□）以下、好ましくは３×１０12（Ω／□）以下である。
このようにして作製された本発明の赤外線吸収フィルムは、少なくとも波長８５０〜１３００ｎｍの全領域における光線透過率が１０％以下であり、かつ可視光線透過率が６５％以上である。前記波長における光線透過率が１０％以下であれば、本発明の赤外線吸収フィルムをＰＤＰの前面板に用いた場合に、該ＰＤＰから発生する近赤外線による周辺電子機器（例えば、コードレスホン、近赤外線リモートコントロール装置を使用するビデオデッキなど）の誤作動を効果的に抑制することができる。また、建築物や車両の窓材用などの熱線遮蔽フィルムとして用いる場合、太陽光中の熱線を効果的に遮蔽することができる。
In the present invention, this reactive cationic antistatic agent may be used alone or in combination of two or more. Further, the polymer cationic antistatic agent, the low molecular cationic antistatic agent and the reactive cationic antistatic agent can be used in appropriate combination.
On the other hand, the inorganic antistatic agent is not particularly limited, and conventionally known transparent conductive fillers, silica sols having silanol groups obtained by hydrolysis and condensation reactions of tetraalkoxysilane, siloxanes having silanol groups and other hydrophilic groups. A polymer or the like can be used. These inorganic antistatic agents may be used alone or in combination of two or more thereof, or may be used in combination with the organic antistatic agent.
In the present invention, the content of the antistatic agent in the inorganic dye-containing cured product layer or the antireflection layer is appropriately selected according to the type thereof. For example, in the case of an organic antistatic agent, usually 2 to It is selected in the range of 25% by mass. When the content of the antistatic agent is within the above range, the infrared absorbing film exhibits good antistatic performance and does not adversely affect other performance. This content is preferably in the range of 3 to 25% by mass, more preferably 5 to 20% by mass. Here, as the antistatic performance, for example, the surface resistivity is 3 × 10 13 (Ω / □) or less, preferably 3 × 10 12 (Ω / □) under normal temperature and humidity conditions (23 ° C., 50% RH). □) The following.
The infrared ray absorbing film of the present invention thus produced has a light transmittance of 10% or less and a visible light transmittance of 65% or more in at least the entire region having a wavelength of 850 to 1300 nm. If the light transmittance at the wavelength is 10% or less, when the infrared absorption film of the present invention is used for the front plate of the PDP, peripheral electronic devices (for example, cordless phones, near infrared remotes) generated by the near infrared rays generated from the PDP. Malfunction of a video deck using a control device) can be effectively suppressed. Moreover, when using as a heat ray shielding film for buildings or vehicle window materials, heat rays in sunlight can be effectively shielded.
さらに、可視光線透過率が６５％以上であれば、本発明の赤外線吸収フィルムをＰＤＰの前面板に用いても、該ＰＤＰの視認性（表示画面）が良好である。また、建築物や車両の窓材用などの熱線遮蔽フィルムとして用いる場合、室内に可視光線を十分に取り入れ、明るさを維持することができる。
本発明の赤外線吸収フィルムは、無機系色素含有硬化物層上に反射防止層を設けた場合、波長５００〜７００ｎｍにおける反射率は、通常６％以下である。また、ヘイズ値は、通常３％未満であるが、無機系色素含有硬化物層に防眩性付与剤を含有させた場合は、３〜３０％程度である。
本発明の赤外線吸収フィルムは、通常ｘｙ色度座標において、ｘが０.２７〜０.３３を示し、かつｙが０.２８〜０.３４を示す。
三刺激値ＸＹＺによる色の表示方法は、ＣＩＥ（国際照明委員会）の１９３１年の会議で定められた表色系で、ＣＩＥ表色系ともいわれ、色を定量的に取扱うのには、最も適した科学的表色方法である。なお、三刺激値ＸＹＺとは、表色上の三原色光の等エネルギーにおける色刺激値を指す。
スペクトルの三刺激値ＸＹＺから、スペクトル色の色度座標ｘ、ｙを求め、該ｘ、ｙを直交軸とする座標空間で色を表したものがｘｙ色度図（ＣＩＥ色度図）であり、図１に示すようにＲＧＢ曲線となる。図１はＣＩＥ色度図である。
全ての色の色度は、ＲＧＢ曲線とＲＢ直線で囲まれた図形の中にはいる。
本発明の赤外線吸収フィルムにおいては、このＣＩＥ色度図において、通常ｘが０.２７〜０.３３の範囲にあり、かつｙが０.２８〜０.３４の範囲にある。
Furthermore, if the visible light transmittance is 65% or more, the visibility (display screen) of the PDP is good even when the infrared absorbing film of the present invention is used for the front plate of the PDP. Further, when used as a heat ray shielding film for a window of a building or vehicle, visible light can be sufficiently taken into the room to maintain brightness.
In the infrared absorbing film of the present invention, when an antireflection layer is provided on the inorganic pigment-containing cured product layer, the reflectance at a wavelength of 500 to 700 nm is usually 6% or less. Moreover, although a haze value is usually less than 3%, when an anti-glare imparting agent is contained in the inorganic pigment-containing cured product layer, it is about 3 to 30%.
The infrared ray absorbing film of the present invention usually has x of 0.27 to 0.33 and y of 0.28 to 0.34 in the xy chromaticity coordinates.
The color display method using tristimulus values XYZ is the color system defined at the 1931 meeting of the CIE (International Lighting Commission), also called the CIE color system. It is a suitable scientific color method. The tristimulus values XYZ indicate color stimulus values at the same energy of the three primary color lights on the color.
An xy chromaticity diagram (CIE chromaticity diagram) is obtained by obtaining chromaticity coordinates x and y of spectral colors from the tristimulus values XYZ of the spectrum and expressing the colors in a coordinate space with x and y being orthogonal axes. As shown in FIG. 1, an RGB curve is obtained. FIG. 1 is a CIE chromaticity diagram.
The chromaticity of all colors is in the figure surrounded by the RGB curve and the RB straight line.
In the infrared absorbing film of the present invention, in this CIE chromaticity diagram, x is usually in the range of 0.27 to 0.33 and y is in the range of 0.28 to 0.34.
本発明の赤外線吸収フィルムにおいては、無機系色素含有硬化物層上又は反射防止層上に、必要に応じさらに防汚コート層を設けることができる。この防汚コート層は、一般にフッ素系樹脂を含む塗工液を、従来公知の方法、例えばバーコート法、ナイフコート法、ロールコート法、ブレードコート法、ダイコート法、グラビアコート法などを用いて、前記各層上にコーティングし、塗膜を形成させ、乾燥処理することにより、形成することができる。
この防汚コート層の厚さは、通常１〜１０ｎｍ、好ましくは３〜８ｎｍの範囲である。該防汚コート層を設けることにより、得られる赤外線吸収フィルムは、表面の滑り性が良くなると共に、汚れにくくなる。
本発明の赤外線吸収フィルムにおいては、基材フィルムの無機系色素含有硬化物層とは反対側の面に、被着体に貼着させるための粘着剤層を形成させることができる。この粘着剤層を構成する粘着剤としては、例えばアクリル系粘着剤、ウレタン系粘着剤、シリコーン系粘着剤が好ましく用いられる。この粘着剤層の厚さは、通常５〜５０μｍの範囲である。
なお、本発明の赤外線吸収フィルムをＰＤＰ用の近赤外線吸収フィルムとして用いる場合には、前記粘着剤層には、表示装置の発光色を色調補正するために、染料や顔料を含有させることができる。
さらに、この粘着剤層の上に、剥離フィルムを設けることができる。この剥離フィルムとしては、例えばグラシン紙、コート紙、ラミネート紙などの紙及び各種プラスチックフィルムに、シリコーン樹脂などの剥離剤を塗付したものなどが挙げられる。この剥離フィルムの厚さについては特に制限はないが、通常２０〜１５０μｍ程度である。
本発明の非反射防止型赤外線吸収フィルムは、ＰＤＰ用の近赤外線吸収フィルムとして、あるいは各種建築物や車両の窓材用などの熱線遮蔽フィルム等として用いることができ、特にＰＤＰ用の近赤外線吸収フィルムとして好適である。
また、本発明の反射防止型赤外線吸収フィルムは、特にＰＤＰ用の近赤外線吸収兼反射防止機能を有するフィルムとして、ＰＤＰ前面板の層構成を簡略化することができ、好適である。
In the infrared ray absorbing film of the present invention, an antifouling coating layer can be further provided on the inorganic pigment-containing cured product layer or the antireflection layer as necessary. This antifouling coating layer is generally obtained by applying a coating solution containing a fluororesin using a conventionally known method such as a bar coating method, a knife coating method, a roll coating method, a blade coating method, a die coating method, or a gravure coating method. It can form by coating on each said layer, forming a coating film, and drying-processing.
The thickness of the antifouling coating layer is usually in the range of 1 to 10 nm, preferably 3 to 8 nm. By providing the antifouling coating layer, the resulting infrared absorbing film has improved surface slipperiness and is less likely to become dirty.
In the infrared absorption film of this invention, the adhesive layer for making it adhere to a to-be-adhered body can be formed in the surface on the opposite side to the inorganic pigment | dye containing cured | curing material layer of a base film. As the pressure-sensitive adhesive constituting the pressure-sensitive adhesive layer, for example, an acrylic pressure-sensitive adhesive, a urethane pressure-sensitive adhesive, and a silicone pressure-sensitive adhesive are preferably used. The thickness of this pressure-sensitive adhesive layer is usually in the range of 5 to 50 μm.
When the infrared absorbing film of the present invention is used as a near infrared absorbing film for PDP, the pressure-sensitive adhesive layer can contain a dye or a pigment in order to correct the color tone of the display device. .
Furthermore, a release film can be provided on this pressure-sensitive adhesive layer. Examples of the release film include paper such as glassine paper, coated paper, and laminate paper, and various plastic films coated with a release agent such as silicone resin. Although there is no restriction | limiting in particular about the thickness of this peeling film, Usually, it is about 20-150 micrometers.
The non-reflection preventing infrared absorbing film of the present invention can be used as a near infrared absorbing film for PDP or as a heat ray shielding film for various building or vehicle window materials, and in particular, a near infrared absorbing film for PDP. Suitable as a film.
In addition, the antireflection infrared absorbing film of the present invention is suitable because it can simplify the layer structure of the PDP front plate, particularly as a film having near infrared absorption and antireflection functions for PDP.
次に、本発明を実施例により、さらに詳細に説明するが、本発明は、これらの例によってなんら限定されるものではない。
なお、各例で得られた赤外線吸収フィルムの物性は、以下に示す方法に従って測定した。
（１）波長８５０〜１３００ｎｍにおける光線透過率
(株)島津製作所製「ＵＶ−３１０１ＰＣ」により、各波長による透過率を測定した。
（２）ｘｙ色度座標
分光光度計［(株)島津製作所製「ＵＶ−３１０１ＰＣ」］を用い、ＪＩＳ Ｚ ８７０１−１９９９に準拠して測定した。
（３）可視光線透過率及びヘイズ値
日本電色工業社製ヘイズメーター「ＮＤＨ ２０００」を使用し、ＪＩＳ Ｋ ７１０５に準拠して可視光線透過率（全光線透過率）及びヘイズ値を測定した。
（４）波長５００ｎｍ、６００ｎｍ及び７００ｎｍにおける反射率
分光光度計［(株)島津製作所製「ＵＶ−３１０１ＰＣ」］により、波長５００ｎｍ、６００ｎｍ及び７００ｎｍにおける反射率を測定した。
（５）６０°グロス値
日本電色工業社製グロスメーター「ＶＧ ２０００」を使用し、ＪＩＳ Ｋ ７１０５に準拠して測定した。
（６）耐擦傷性
スチールウール＃００００を使用し、荷重９.８×１０-3Ｎ／ｍｍ2で５往復擦った後に目視観察を行い、下記の判定基準で評価した。
○：傷が付かない。
×：傷が付く。
（７）耐光性
ガラス板に透明粘着剤を介して貼付した試料を、フェードメータ（カーボンアーク、ブラックパネル温度６３℃）に投入し、試料側から２００時間紫外線を照射した後に各種光学特性を評価した。
（８）表面抵抗率
試料を２３℃、湿度５０％の条件下２４時間調湿後、表面層の表面抵抗率を、ＪＩＳ Ｋ ６９１１に準拠し、(株)アドバンテスト社製デジタルエレクトロメーターに連結した平行電極を使用して測定した。
EXAMPLES Next, although an Example demonstrates this invention further in detail, this invention is not limited at all by these examples.
In addition, the physical property of the infrared rays absorption film obtained in each case was measured in accordance with the method shown below.
(1) Light transmittance at a wavelength of 850 to 1300 nm
The transmittance at each wavelength was measured by “UV-3101PC” manufactured by Shimadzu Corporation.
(2) xy chromaticity coordinates Using a spectrophotometer [“UV-3101PC” manufactured by Shimadzu Corporation], the measurement was performed according to JIS Z 8701-1999.
(3) Visible light transmittance and haze value A visible light transmittance (total light transmittance) and a haze value were measured according to JIS K 7105 using a Nippon Denshoku Industries Co., Ltd. haze meter "NDH 2000".
(4) Reflectance at wavelengths of 500 nm, 600 nm, and 700 nm The reflectance at wavelengths of 500 nm, 600 nm, and 700 nm was measured with a spectrophotometer [manufactured by Shimadzu Corporation “UV-3101PC”].
(5) 60 ° gloss value A gloss meter “VG 2000” manufactured by Nippon Denshoku Industries Co., Ltd. was used and measured according to JIS K 7105.
(6) Scratch resistance Steel wool # 0000 was used, and after 5 rubbing with a load of 9.8 × 10 −3 N / mm 2 , visual observation was performed, and evaluation was performed according to the following criteria.
○: Not scratched.
×: Scratched.
(7) Light resistance A sample affixed to a glass plate via a transparent adhesive is put into a fade meter (carbon arc, black panel temperature 63 ° C.) and irradiated with ultraviolet rays from the sample side for 200 hours, and then various optical properties are evaluated. did.
(8) Surface resistivity After the sample was conditioned for 24 hours under conditions of 23 ° C. and 50% humidity, the surface resistivity of the surface layer was connected to a digital electrometer manufactured by Advantest Corporation in accordance with JIS K 6911. Measurements were made using parallel electrodes.
参考例１
活性エネルギー線硬化性化合物として多官能アクリレート混合物［荒川化学(株)製、商品名「ビームセット５７５ＣＢ」、固形分濃度１００％、光重合開始剤含有］１００質量部に、近赤外線吸収剤［住友金属鉱山(株)製、商品名「ＹＭＦ−０１」、セシウム含有酸化タングステン（タングステンに対し、セシウム３３モル％含有、平均粒径３０ｎｍ）含有量１０質量％懸濁液、全固形分濃度１４質量％］３００質量部を混合したのち、全体の固形分濃度が３０質量％になるようにメチルイソブチルケトン（ＭＩＢＫ）で希釈して、塗工液を調製した。
次に、 基材フィルムとして厚さ１００μｍの両面易接着処理ポリエチレンテレフタレート（ＰＥＴ）フィルム［東洋紡績(株)製、商品名「Ａ４３００」］表面に、前記塗工液を硬化後の厚さが７μｍになるように、マイヤーバーＮｏ.１６で塗布した。次いで、８０℃で１分間乾燥したのち、紫外線を光量２５０ｍＪ／ｃｍ2で照射して、赤外線吸収フィルムを作製した。
このようにして作製された赤外線吸収フィルムの性能を第１表に示す。
実施例２
参考例１において、紫外線光量を７０ｍＪ／ｃｍ2として作製した近赤外線吸収剤含有硬化物層に、以下のようにして調製した反射防止層形成用塗工液を、硬化後の厚さが１００ｎｍになるようにマイヤーバーＮｏ.４で塗布した。次いで、８０℃で１分間乾燥したのち、紫外線を光量５００ｍＪ／ｃｍ2照射して、反射防止層を有する赤外線吸収フィルムを作製した。このときの反射防止層の屈折率は１.３８であった。
このようにして作製された赤外線吸収フィルムの性能を第１表に示す。
＜反射防止層形成用塗工液の調製＞
多官能アクリレート混合物［荒川化学(株)製、商品名「ビームセット５７５ＣＢ」、固形分濃度１００％］１００質量部に、多孔性シリカ粒子のメチルイソブチルケトン（ＭＩＢＫ）分散体［触媒化成工業(株)製、商品名「ＥＬＣＯＭ ＲＴ−１００２ＳＩＶ」、固形分濃度２１質量％、多孔性シリカ粒子：比重１.８、屈折率１.３０、平均粒径６０ｎｍ］１２００質量部を混合したのち、全体の固形分濃度が２質量％になるようにＭＩＢＫで希釈して、反射防止層形成用塗工液を調製した。
実施例３
活性エネルギー線硬化性化合物として多官能アクリレート混合物［荒川化学(株)製、商品名「ビームセット５７５ＣＢ」、固形分濃度１００％、光重合開始剤含有］１００質量部に、近赤外線吸収剤［住友金属鉱山(株)製、商品名「ＹＭＦ−０１」、セシウム含有酸化タングステン（タングステンに対し、セシウム３３モル％含有）含有量１０質量％懸濁液、全固形分濃度１４質量％］３００質量部を混合し、さらに防眩性付与剤としてシリカ粒子［東ソー・シリカ(株)製、商品名「ニップシールＥ−２００」、平均粒径３μｍ］５質量部を加えたのち、全体の固形分濃度が３０質量％になるようにＭＩＢＫで希釈して塗工液を調製した以外は、参考例１と同様にして防眩性を付与した赤外線吸収フィルムを作製した。
このようにして作製された赤外線吸収フィルムの性能を第１表に示す。
実施例４
参考例１の活性エネルギー線硬化性化合物を、帯電防止性ハードコート剤［ＪＳＲ(株)製、商品名「デソライトＫＺ６１６３」固形分濃度７５質量％］１３０質量部とし、光重合開始剤として［チバスペシャリティーケミカルズ(株)製、商品名「イルガキュア９０７」］４質量部を加えた以外は、参考例１と同様にして赤外線吸収フィルムを作製した。
このようにして作製された赤外線吸収フィルムの性能を第１表に示す。
比較例１
ポリエステル系樹脂として［東洋紡績(株)製、商品名「バイロン２０ＳＳ」、固形分濃度３０質量％、トルエンとＭＥＫの混合溶剤希釈］１００質量部と代表的な近赤外線吸収剤（イモニウム系色素）［日本化薬(株)製、商品名「ＫＡＹＡＳＯＲＢ ＩＲＧ−０２２」、固形分濃度１００％（粉体）］１質量部を混合し、さらに希釈溶剤としてシクロヘキサノンを加え全体の固形分濃度が１２質量％になるように希釈して塗工液を調製した。
次に基材フィルムとして厚さ１００μｍの両面易接着処理ＰＥＴフィルム［東洋紡績(株)製、商品名「Ａ４３００」］の表面に、前記塗工液を乾燥後の厚さが４μｍになるように、マイヤーバーＮｏ.１６で塗布した。１３０℃、２分間乾燥して赤外線吸収フィルムを作製した。
このようにして作製された赤外線吸収フィルムの性能を第１表に示す。
Reference example 1
As an active energy ray-curable compound, a polyfunctional acrylate mixture [made by Arakawa Chemical Co., Ltd., trade name “Beam Set 575CB”, solid content concentration 100%, containing photopolymerization initiator] 100 parts by mass, near infrared absorber [Sumitomo Product name “YMF-01”, manufactured by Metal Mining Co., Ltd., cesium-containing tungsten oxide (containing 33 mol% of cesium, average particle size of 30 nm with respect to tungsten) content of 10% by mass suspension, total solid content concentration of 14 mass %] After mixing 300 parts by mass, it was diluted with methyl isobutyl ketone (MIBK) so that the total solid concentration was 30% by mass to prepare a coating solution.
Next, a double-sided easy-adhesion-treated polyethylene terephthalate (PET) film [trade name “A4300”, manufactured by Toyobo Co., Ltd.] having a thickness of 100 μm as a base film has a thickness of 7 μm after curing the coating liquid. It applied with Mayer bar No. 16 so that it might become. Subsequently, after drying at 80 degreeC for 1 minute, the ultraviolet rays were irradiated with the light quantity of 250 mJ / cm < 2 >, and the infrared rays absorption film was produced.
The performance of the infrared absorbing film thus prepared is shown in Table 1.
Example 2
In Reference Example 1, an antireflection layer-forming coating solution prepared as follows was applied to a near-infrared absorber-containing cured product layer prepared with an ultraviolet light amount of 70 mJ / cm 2 so that the thickness after curing was 100 nm. It applied with Mayer bar No. 4 so that it might become. Subsequently, after drying at 80 degreeC for 1 minute, the ultraviolet-ray was irradiated with light quantity 500mJ / cm < 2 >, and the infrared rays absorption film which has an antireflection layer was produced. At this time, the refractive index of the antireflection layer was 1.38.
The performance of the infrared absorbing film thus prepared is shown in Table 1.
<Preparation of antireflection layer forming coating solution>
Polyfunctional acrylate mixture [trade name “Beamset 575CB”, manufactured by Arakawa Chemical Co., Ltd., solid content concentration: 100%] in 100 parts by mass, methyl isobutyl ketone (MIBK) dispersion of porous silica particles [Catalyst Chemical Industries, Ltd. ), Trade name “ELCOM RT-1002SIV”, solid content concentration 21% by mass, porous silica particles: specific gravity 1.8, refractive index 1.30, average particle size 60 nm] after mixing 1200 parts by mass, An antireflection layer-forming coating solution was prepared by diluting with MIBK so that the solid content concentration was 2% by mass.
Example 3
As an active energy ray-curable compound, a polyfunctional acrylate mixture [made by Arakawa Chemical Co., Ltd., trade name “Beam Set 575CB”, solid content concentration 100%, containing photopolymerization initiator] 100 parts by mass, near infrared absorber [Sumitomo Product name “YMF-01” manufactured by Metal Mining Co., Ltd., cesium-containing tungsten oxide (containing 33 mol% of cesium with respect to tungsten) content 10% by mass suspension, total solid content concentration 14% by mass] 300 parts by mass And further adding 5 parts by mass of silica particles [made by Tosoh Silica Co., Ltd., trade name “Nip Seal E-200”, average particle size 3 μm] as an anti-glare imparting agent. An infrared absorbing film imparted with antiglare property was produced in the same manner as in Reference Example 1 except that the coating liquid was prepared by diluting with MIBK so as to be 30% by mass.
The performance of the infrared absorbing film thus prepared is shown in Table 1.
Example 4
The active energy ray-curable compound of Reference Example 1 is 130 parts by mass of an antistatic hard coat agent [trade name “Desolite KZ6163” solid content concentration: 75% by mass, manufactured by JSR Corporation], and [Ciba An infrared absorption film was produced in the same manner as in Reference Example 1 except that 4 parts by mass of Specialty Chemicals Co., Ltd., trade name “Irgacure 907” was added.
The performance of the infrared absorbing film thus prepared is shown in Table 1.
Comparative Example 1
As a polyester resin [Toyobo Co., Ltd., trade name “Byron 20SS”, solid content concentration 30% by mass, diluted with a mixed solvent of toluene and MEK] 100 parts by mass and a typical near infrared absorber (imonium dye) [Nippon Kayaku Co., Ltd., trade name “KAYASORB IRG-022”, solid content concentration: 100% (powder)] 1 part by weight is mixed, and cyclohexanone is further added as a diluent solvent to a total solid content concentration of 12 masses. The coating solution was prepared by diluting to a concentration of%.
Next, on the surface of a 100 μm-thick double-sided easy-adhesion-treated PET film [trade name “A4300” manufactured by Toyobo Co., Ltd.] as the base film, the thickness after drying the coating solution is 4 μm. And Meyer bar No.16. An infrared absorption film was prepared by drying at 130 ° C. for 2 minutes.
The performance of the infrared absorbing film thus prepared is shown in Table 1.
第１表から明らかなように、本発明の赤外線吸収フィルム（参考例１及び実施例２〜４）は、初期値の光線透過率及び耐光性における光線透過率のいずれにおいても、波長８５０〜１３００ｎｍの全領域において、光線透過率が１０％未満の値を示しており、また、ｘｙ色度座標において、初期値及び耐光性共に、ｘが０.２７〜０.３３、ｙが０.２８〜０.３４の範囲にある。したがって、耐光性に極めて優れていることが分かる。
これに対し、比較例１の赤外線吸収フィルムは、初期値の光線透過率が、波長１２００ｎｍ、１３００ｎｍで１０％を超えており、また、耐光性における光線透過率が、８５０〜１３００ｎｍの全ての領域において、初期値に比べて著しく高くなっており（６９％＜）、耐光性が極めて悪いことが分かる。
As is apparent from Table 1, the infrared absorbing film of the present invention ( Reference Example 1 and Examples 2 to 4) has a wavelength of 850 to 1300 nm in both the initial light transmittance and the light transmittance in light resistance. In the entire region, the light transmittance is less than 10%, and in the xy chromaticity coordinates, both the initial value and the light resistance are x of 0.27 to 0.33, and y is 0.28 to 0.28. It is in the range of 0.34. Therefore, it turns out that it is excellent in light resistance.
On the other hand, the infrared ray absorbing film of Comparative Example 1 has an initial light transmittance of more than 10% at wavelengths of 1200 nm and 1300 nm, and has a light transmittance of 850 to 1300 nm in all regions. In FIG. 4, it is remarkably higher than the initial value (69% <), which indicates that the light resistance is extremely poor.
本発明の赤外線吸収フィルムは、８５０〜１３００ｎｍの近赤外線吸収性能に優れると共に、可視光線透過率が高く、かつ耐光性や耐候性に優れ、経時により近赤外線吸収性能の劣化が抑制され、しかも製造コストが低い。したがって、ＰＤＰ用の近赤外線吸収フィルムとして、あるいは各種建築物や車両の窓材用などの熱線遮蔽フィルム等に用いることができ、特にＰＤＰ用近赤外線吸収フィルムとして好適である。 The infrared absorbing film of the present invention has excellent near infrared absorption performance of 850 to 1300 nm, high visible light transmittance, excellent light resistance and weather resistance, and deterioration of near infrared absorption performance is suppressed over time, and is manufactured. Cost is low. Therefore, it can be used as a near-infrared absorbing film for PDP or a heat ray shielding film for various buildings and vehicle windows, and is particularly suitable as a near-infrared absorbing film for PDP.
Claims (6)
It is an object for plasma displays, The infrared absorption film in any one of Claims 1-5 .
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| JP5588588B2 (en) * | 2007-02-20 | 2014-09-10 | リンテック株式会社 | Near-infrared shielding film for automobile window glass and method for producing automobile window glass using the film |
| JP2008216568A (en) * | 2007-03-02 | 2008-09-18 | Sumitomo Osaka Cement Co Ltd | Antireflective/near ir light blocking laminate and its manufacturing method |
| JP5358976B2 (en) * | 2008-02-29 | 2013-12-04 | 大日本印刷株式会社 | Near infrared absorbing material |
| JP5264331B2 (en) * | 2008-07-08 | 2013-08-14 | 株式会社ブリヂストン | Functional film |
| JP2010164713A (en) * | 2009-01-14 | 2010-07-29 | Nof Corp | Near-infrared ray absorption hard coat film and antireflection film |
| JP5499837B2 (en) * | 2010-03-31 | 2014-05-21 | 住友大阪セメント株式会社 | Heat ray shielding film |
| WO2012026577A1 (en) | 2010-08-26 | 2012-03-01 | 住友大阪セメント株式会社 | Black film, substrate provided with black film, image display device, black resin composition, and black material dispersion liquid |
| TWI422552B (en) * | 2012-02-08 | 2014-01-11 | Nanya Plastics Corp | A kind of transparent and heat shielding material and manufacturing method thereof |
| JP5824386B2 (en) * | 2012-02-29 | 2015-11-25 | 富士フイルム株式会社 | Infrared absorbing composition and infrared cut filter |
| JP2014024537A (en) | 2012-06-19 | 2014-02-06 | 3M Innovative Properties Co | Sheet for license plate, laminated body for license plate, license plate and decorative member for license plate |
| JP2016014690A (en) * | 2012-11-14 | 2016-01-28 | 旭硝子株式会社 | Optical filter |
| KR101724562B1 (en) | 2013-02-14 | 2017-04-07 | 후지필름 가부시키가이샤 | Infrared absorption composition and infrared absorption composition kit infrared cut-off filter using same and manufacturing method thereof and camera module and manufacturing method thereof |
| JP6443329B2 (en) * | 2013-04-10 | 2018-12-26 | Ａｇｃ株式会社 | Infrared shielding filter and imaging device |
| CN104553215B (en) | 2013-10-16 | 2017-05-24 | 北京化工大学 | Transparent, flame-retardant, thermal-insulation and anti-ultraviolet polymer composite film as well as preparation method and application thereof |
| JP7283993B2 (en) * | 2019-06-20 | 2023-05-30 | アイカ工業株式会社 | Infrared cut hard coat resin and hard coat film using the same |
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| JP2005062506A (en) * | 2003-08-13 | 2005-03-10 | Asahi Glass Co Ltd | Near-infrared ray absorbing adhesive composition, and optical film |
| JP4626284B2 (en) * | 2003-12-05 | 2011-02-02 | 住友金属鉱山株式会社 | Method for producing tungsten oxide fine particles for forming solar shield, and tungsten oxide fine particles for forming solar shield |
| JP4586970B2 (en) * | 2004-11-30 | 2010-11-24 | 住友金属鉱山株式会社 | Near infrared absorption filter for plasma display panel and plasma display panel using the same |
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