JP2011018035A - Casting mold film and method of producing anti-dazzling resin plate - Google Patents
Casting mold film and method of producing anti-dazzling resin plate Download PDFInfo
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- JP2011018035A JP2011018035A JP2010131640A JP2010131640A JP2011018035A JP 2011018035 A JP2011018035 A JP 2011018035A JP 2010131640 A JP2010131640 A JP 2010131640A JP 2010131640 A JP2010131640 A JP 2010131640A JP 2011018035 A JP2011018035 A JP 2011018035A
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- film
- active energy
- energy ray
- polymerizable composition
- mold
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- 238000005266 casting Methods 0.000 title claims description 17
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- 208000028659 discharge Diseases 0.000 claims abstract description 22
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Abstract
【課題】基材に凹凸形状を付与するため、活性エネルギー線重合性組成物をコーティングして作製した凹凸層を有するフィルムを鋳型用フィルムとして用いた場合、鋳型用フィルムと基材間の活性エネルギー線重合性組成物を硬化して後、鋳型用フィルムの剥離を容易とする。
【解決手段】透明基材フィルム(Ａ)の表面に活性エネルギー線重合性組成物(Ｂ)が塗布、硬化された凹凸層を有し、凹凸層の表面に放電処理が施された鋳型用フィルム、並びにフィルム(Ａ)の表面に組成物(Ｂ)を塗布、硬化して凹凸層を設けた鋳型用フィルムを作製する第一の工程、鋳型用フィルムの凹凸層の表面に放電処理を施す第二の工程、組成物(Ｃ)を介して、鋳型用フィルムの凹凸層の表面と透明樹脂板を貼り合わせる第三の工程、照射により重合性組成物(Ｃ)を硬化させる第四の工程、鋳型用フィルムを剥離、除去する第五の工程からなる防眩性樹脂板の製造方法。
【選択図】なしWhen a film having a concavo-convex layer produced by coating an active energy ray-polymerizable composition is used as a mold film in order to impart a concavo-convex shape to the base material, the active energy between the mold film and the base material After the linear polymerizable composition is cured, the mold film is easily peeled off.
A mold film having a concavo-convex layer coated and cured with an active energy ray-polymerizable composition (B) on the surface of a transparent substrate film (A), and having a discharge treatment applied to the surface of the concavo-convex layer. And a first step of producing a mold film provided with a concavo-convex layer by applying and curing the composition (B) on the surface of the film (A), and applying a discharge treatment to the surface of the concavo-convex layer of the mold film. A second step, a third step of bonding the surface of the concavo-convex layer of the mold film and the transparent resin plate through the composition (C), a fourth step of curing the polymerizable composition (C) by irradiation, A method for producing an antiglare resin plate comprising a fifth step of peeling off and removing a mold film.
[Selection figure] None
Description
本発明はこの発明は、コンピュータ、ワードプロセッサ、テレビジョン等の画像表示に用いるＣＲＴ、液晶パネル等の高精細画像用ディスプレイの前面に設ける防眩性樹脂板の製造方法に関する。 The present invention relates to a method for producing an antiglare resin plate provided on the front surface of a high-definition image display such as a CRT or a liquid crystal panel used for image display of a computer, a word processor, a television or the like.
電子情報に基づいて、静止画像や動画を表示する表示装置（＝ディスプレイ）としては様々なものが知られて、現在、市場に出回っているものとしてはＣＲＴ、プラズマディスプレイ、液晶ディスプレイ、もしくはエレクトロルミネッセンスディスプレイ等がある。 Various display devices (= displays) that display still images and moving images based on electronic information are known, and currently on the market are CRTs, plasma displays, liquid crystal displays, or electroluminescence. There is a display.
ところで、液晶表示装置を駆動して画像を眺める際に、画面に、観察者の背後にあるものが写って見えることがあり、特に、室内の照明装置や、屋外光がある場合には、光源が写って見え、画像の視認性を著しく損なうものである。 By the way, when viewing an image by driving a liquid crystal display device, the screen may appear to show what is behind the viewer, especially when there is an indoor lighting device or outdoor light. Appears, and the visibility of the image is significantly impaired.
また、コンピュータの入力の手段の一つに、タッチパネルがあるが、中でも、表示装置の画面上で操作するタッチパネルは、選択してタッチすべき箇所を、自由に作成して、表示装置の画面に表示できるので、便利である。しかし、タッチ入力する頻度が多いと、指紋の付着や傷付きの原因となる上、種々の耐久性が必要になる。 In addition, there is a touch panel as one of the input means of the computer. Among them, the touch panel operated on the screen of the display device is free to create a place to be selected and touched on the screen of the display device. It is convenient because it can be displayed. However, if the frequency of touch input is high, it may cause fingerprints and scratches, and various durability is required.
また、太陽電池モジュールの表面保護部材の外表面に凹凸を形成し、反射光を散乱させることで、反射光が近隣の家屋内やビル内を照らしたりするなどの光公害の問題を解決する旨が記載されている（特許文献１）。しかしながら、この発明では表面保護部材にガラス板を使用するため、太陽電池モジュールが重くなり、屋根に設置する際には家屋の構造を補強する工事が必要になる等の課題があった。 In addition, by forming irregularities on the outer surface of the surface protection member of the solar cell module and scattering the reflected light, it solves the problem of light pollution, such as the reflected light illuminating a nearby house or building Is described (Patent Document 1). However, in this invention, since a glass plate is used for the surface protection member, the solar cell module becomes heavy, and there is a problem that a construction for reinforcing the structure of the house is required when installing on the roof.
従来から、画面に室内の照明装置や、太陽が写って見えるのを防止する目的では、透明プラスチックフィルム上に、有機質もしくは無機質の微小なビーズを配合した塗料組成物を塗布し、塗布後、乾燥、もしくは固化させて防眩層を形成した防眩性フィルムが用いられている（特許文献２）。しかしながら、この製造方法により製造される防眩性フィルムに使用されている、有機質もしくは無機質の微小なビーズは、使用中に脱落し、防眩性フィルムを擦ることによる傷の発生が避けられない上、製造時、ビーズを配合した塗料組成物を塗布する際に、スジが生じたり、塗布ムラが生ずる等、均一な防眩性を得ることが難しい。また、このようにして得られた防眩性フィルムをタッチパネルの表面材として使用する際に、指やタッチ用ペンで表面を触れると、脱落したビーズが防眩性フィルムを擦るため、傷の発生を助長するものである。さらには塗膜が空気にさらされるため、塵を含む欠陥が発生しやすいといった問題点があった。 Conventionally, for the purpose of preventing indoor lighting devices and the sun from appearing on the screen, a coating composition containing fine organic or inorganic beads is applied onto a transparent plastic film, and then dried after application. Or the anti-glare film which solidified and formed the anti-glare layer is used (patent document 2). However, the organic or inorganic fine beads used in the antiglare film produced by this production method are inevitably dropped during use and scratches due to rubbing the antiglare film are unavoidable. It is difficult to obtain uniform antiglare properties such as streaks or uneven coating when applying a coating composition containing beads during production. In addition, when the antiglare film obtained in this way is used as a surface material for a touch panel, if the surface is touched with a finger or a touch pen, the fallen beads rub against the antiglare film, resulting in scratches. It is to promote. Further, since the coating film is exposed to air, there is a problem that defects including dust are likely to occur.
そこで、硬度を備えた防眩層を持つ光学積層体の作製方法として所望の凹凸を有するフィルムを鋳型としてフィルムと基材間に活性エネルギー線重合性組成物を注入し、硬化させ、該フィルムを剥離することで目的の凹凸を有する防眩性樹脂板の製造方法が開示されている（特許文献１）。しかし、賦型用フィルムとして微粒子を練り込んだマットフィルムを使用した場合、表面が白みがかる「白ちゃけ」と呼ばれる欠陥が出てしまう。一方、表面に光硬化性樹脂をコーティングして作製したフィルムを鋳型用フィルムとして用いた場合、白ちゃけの少ない凹凸表面を持つ防眩性樹脂板の製造が可能だが、該フィルムと基材間に注入した活性エネルギー線重合性組成物を硬化した後、鋳型用フィルムの剥離が困難になるという問題点があった。 Therefore, as a method for producing an optical laminate having an antiglare layer with hardness, an active energy ray polymerizable composition is injected between a film and a substrate using a film having desired irregularities as a mold and cured, and the film is then cured. A method for producing an antiglare resin plate having desired unevenness by peeling is disclosed (Patent Document 1). However, when a mat film in which fine particles are kneaded is used as the shaping film, a defect called “whitening” occurs, which causes the surface to become white. On the other hand, when a film prepared by coating the surface with a photocurable resin is used as a mold film, it is possible to produce an antiglare resin plate having an uneven surface with little whiteness. After curing the active energy ray polymerizable composition injected into the mold, there was a problem that it was difficult to peel off the mold film.
基材に凹凸形状を付与するため、活性エネルギー線重合性組成物をコーティングして作製した凹凸層を有するフィルムを鋳型用フィルムとして用いた場合、鋳型用フィルムと基材間の活性エネルギー線重合性組成物を硬化して後、鋳型用フィルムの剥離を容易とすることを課題とする。 When a film having a concavo-convex layer prepared by coating an active energy ray-polymerizable composition is used as a mold film in order to impart a concavo-convex shape to the base material, the active energy ray polymerizability between the mold film and the base material is used. It is an object of the present invention to facilitate the peeling of the mold film after curing the composition.
従来技術の欠点を解決するため、鋭意検討した結果、通常、基材−硬化液間の密着性向上を目的としてコロナ処理やプラズマ処理を行うところ、活性エネルギー線重合性組成物の塗布、硬化により形成した凹凸層を有する鋳型用フィルムの該凹凸層側に対して前記処理を行うと、驚くべきことに活性エネルギー線重合性組成物の硬化物との剥離性が向上することを見出し本発明となった。剥離性が向上するメカニズムとしては、コロナ処理やプラズマ処理を行うことにより、押し込み弾性率の値が上昇していることから表面の硬化性が向上し、重合性組成物の浸透による密着を阻害しているものと考えられる。 As a result of intensive studies to solve the drawbacks of the prior art, usually corona treatment and plasma treatment are performed for the purpose of improving the adhesion between the substrate and the curable liquid. By applying and curing the active energy ray polymerizable composition, When the above-mentioned treatment is performed on the uneven layer side of the mold film having the formed uneven layer, it is surprisingly found that the releasability from the cured product of the active energy ray polymerizable composition is improved. became. As a mechanism for improving the peelability, by performing corona treatment or plasma treatment, the value of the indentation elastic modulus is increased, so that the curability of the surface is improved and the adhesion due to penetration of the polymerizable composition is inhibited. It is thought that.
即ち、本発明は、透明基材フィルム（Ａ）の少なくとも一方の表面に活性エネルギー線重合性組成物（Ｂ）が塗布及び硬化された凹凸層を有し、凹凸層の表面に対して放電処理が施された鋳型用フィルムである。 That is, the present invention has a concavo-convex layer in which the active energy ray-polymerizable composition (B) is applied and cured on at least one surface of the transparent substrate film (A), and discharge treatment is performed on the surface of the concavo-convex layer. It is a film for molds to which is applied.
また本発明は、透明基材フィルム（Ａ）の少なくとも一方の表面に活性エネルギー線重合性組成物（Ｂ）を塗布及び硬化して凹凸層を設けた鋳型用フィルムを作製する第一の工程、鋳型用フィルムの凹凸層の表面に対し、放電処理を施す第二の工程、活性エネルギー線重合性組成物（Ｃ）を介して、鋳型用フィルムの凹凸層の表面と透明樹脂板を貼り合わせる第三の工程、活性エネルギー線の照射により活性エネルギー線重合性組成物（Ｃ）を硬化させる第四の工程、鋳型用フィルムを剥離、除去する第五の工程からなる防眩性樹脂板の製造方法である。 The present invention also includes a first step of producing a film for a mold in which an active energy ray-polymerizable composition (B) is applied and cured on at least one surface of a transparent substrate film (A) to provide an uneven layer, The surface of the concavo-convex layer of the mold film is bonded to the surface of the concavo-convex layer of the mold film and the transparent resin plate via the second step of applying a discharge treatment, the active energy ray polymerizable composition (C). A method for producing an antiglare resin plate comprising three steps, a fourth step for curing the active energy ray polymerizable composition (C) by irradiation with an active energy ray, and a fifth step for peeling and removing the mold film. It is.
本発明によれば、鋳型用フィルムの、活性エネルギー線重合性組成物の硬化物からの剥離性を向上させることができる。また本発明の製造方法よれば、防眩性樹脂板の防眩層の耐擦傷性、基材との密着性を良好とすることができる。本発明の製造方法で得られた防眩性樹脂板は画像表示装置の前面板として好適に使用できる。更に、太陽光の反射を散乱させることから、太陽電池モジュールの表面保護部材としても好適に使用できる。 ADVANTAGE OF THE INVENTION According to this invention, the peelability from the hardened | cured material of the active energy ray polymeric composition of the film for casting_mold | template can be improved. Moreover, according to the manufacturing method of this invention, the abrasion resistance of the anti-glare layer of an anti-glare resin board and adhesiveness with a base material can be made favorable. The antiglare resin plate obtained by the production method of the present invention can be suitably used as a front plate of an image display device. Furthermore, since the reflection of sunlight is scattered, it can be suitably used as a surface protection member of a solar cell module.
以下、本発明の実施の形態について詳細に説明する。 Hereinafter, embodiments of the present invention will be described in detail.
鋳型用フィルムは、透明基材フィルム（Ａ）の少なくとも一方の表面に活性エネルギー線重合性組成物（Ｂ）が塗布及び硬化された凹凸層を有し、凹凸層の表面（以下、「凹凸面」という。）に対して放電処理が施されたものである。 The mold film has a concavo-convex layer on which at least one surface of the transparent substrate film (A) is coated and cured with the active energy ray polymerizable composition (B). ”) Is subjected to a discharge treatment.
以下の記載において量比を表す「部」および「％」は、特に断らない限り質量基準とする。 In the following description, “parts” and “%” representing the quantity ratio are based on mass unless otherwise specified.
本発明の鋳型用フィルムに使用するの透明基材フィルム（Ａ）は、透明性、耐溶剤性に優れ、酸素透過性の低いものが好ましい。例えば、ＰＥＴフィルム、ナイロンフィルム、ポリカーボネートフィルム、アクリル系フィルム、ポリプロピレン、ポリエチレン等のポリオレフィン系フィルム、ジアセチルセルロース、トリアセチルセルロース等のセルロース系フィルム、ポリ塩化ビニリデン系フィルム等が挙げられる。特に好ましいものとしては、ＰＥＴフィルムが挙げられる。フィルムの厚みは、フィルム強度を維持する目的で1μｍ以上が好ましく、取り扱い性、コスト等の点で２００μｍ以下が好ましい。また、凹凸層の密着性を確保する観点から表面に各種の易接着加工を施したものが好ましい。 The transparent substrate film (A) used for the mold film of the present invention is preferably one having excellent transparency and solvent resistance and low oxygen permeability. Examples thereof include PET films, nylon films, polycarbonate films, acrylic films, polyolefin films such as polypropylene and polyethylene, cellulose films such as diacetyl cellulose and triacetyl cellulose, and polyvinylidene chloride films. Particularly preferred is a PET film. The thickness of the film is preferably 1 μm or more for the purpose of maintaining the film strength, and is preferably 200 μm or less from the viewpoints of handleability and cost. Moreover, from the viewpoint of ensuring the adhesion of the concavo-convex layer, it is preferable that the surface is subjected to various easy adhesion processes.
鋳型用フィルムの凹凸層を形成するための、活性エネルギー線重合性組成物（Ｂ）としては、紫外線等の活性エネルギー線の照射により、硬化するものであれば、特に限定されるものではなく、例えば２つ以上の(メタ)アクリロイル基を有する重合性化合物を含んだ組成物（コーティング剤）とすることができる。；該組成物はシリコーン系やメラミン系化合物を含んでもよい。 The active energy ray polymerizable composition (B) for forming the concavo-convex layer of the mold film is not particularly limited as long as it is cured by irradiation with active energy rays such as ultraviolet rays. For example, it may be a composition (coating agent) containing a polymerizable compound having two or more (meth) acryloyl groups. The composition may comprise a silicone-based or melamine-based compound.
中でも、分子中に少なくとも２個の（メタ）アクリロイルオキシ基を有する重合性化合物と、光重合開始剤を含有する活性エネルギー線硬化型の組成物が硬化速度が速く生産性に優れるため好ましい。 Among these, an active energy ray-curable composition containing a polymerizable compound having at least two (meth) acryloyloxy groups in the molecule and a photopolymerization initiator is preferable because of its high curing rate and excellent productivity.
活性エネルギー線重合性組成物（Ｂ）を構成する、重合性化合物の好適なものとしては、１モルの多価アルコールと、２モル以上の（メタ）アクリル酸またはそれらの誘導体とから得られるエステル化物；多価アルコールと多価カルボン酸またはその無水物と（メタ）アクリル酸またはそれらの誘導体とから得られる、１分子中に２個以上の（メタ）アクリロイルオキシ基を有する線状のエステル化物；３量化により得られるポリイソシアネート１モル当たりに、活性水素を有するアクリルモノマー３モル以上を反応させて得られる化合物等を挙げることができる。具体的には、ジエチレングリコールジ（メタ）アクリレート、トリエチレングリコールジ（メタ）アクリレート、テトラエチレングリコールジ（メタ）アクリレート等のポリエチレングリコールのジ（メタ）アクリレート；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、１，９−ノナンジオールジ（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、トリメチロールエタントリ（メタ）アクリレート、ペンタグリセロールトリ（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、ペンタエリスリトールテトラ（メタ）アクリレート、グリセリントリ（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、ジペンタエリスリトールテトラ（メタ）アクリレート、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、トリペンタエリスリトールテトラ（メタ）アクリレート、トリペンタエリスリトールペンタ（メタ）アクリレート、トリペンタエリスリトールヘキサ（メタ）アクリレート、トリペンタエリスリトールヘプタ（メタ）アクリレート等の１モルの多価アルコールと、２モル以上の（メタ）アクリル酸とから得られるエステル化物を挙げることができる。 As a suitable polymerizable compound constituting the active energy ray polymerizable composition (B), an ester obtained from 1 mol of polyhydric alcohol and 2 mol or more of (meth) acrylic acid or a derivative thereof. A linear esterified product having two or more (meth) acryloyloxy groups in one molecule, obtained from a polyhydric alcohol, a polyvalent carboxylic acid or its anhydride, and (meth) acrylic acid or a derivative thereof. A compound obtained by reacting 3 moles or more of an acrylic monomer having active hydrogen with respect to 1 mole of polyisocyanate obtained by trimerization. Specifically, di (meth) acrylate of polyethylene glycol such as diethylene glycol di (meth) acrylate, triethylene glycol di (meth) acrylate, tetraethylene glycol di (meth) acrylate; 1,4-butanediol di (meth) Acrylate, 1,6-hexanediol di (meth) acrylate, 1,9-nonanediol di (meth) acrylate, trimethylolpropane tri (meth) acrylate, trimethylolethane tri (meth) acrylate, pentaglycerol tri (meth) Acrylate, pentaerythritol tri (meth) acrylate, pentaerythritol tetra (meth) acrylate, glycerin tri (meth) acrylate, dipentaerythritol tri (meth) acrylate, dipenta Thritol tetra (meth) acrylate, dipentaerythritol penta (meth) acrylate, dipentaerythritol hexa (meth) acrylate, tripentaerythritol tetra (meth) acrylate, tripentaerythritol penta (meth) acrylate, tripentaerythritol hexa (meth) And esterified products obtained from 1 mol of polyhydric alcohol such as acrylate and tripentaerythritol hepta (meth) acrylate and 2 mol or more of (meth) acrylic acid.
また、マロン酸／トリメチロールエタン／（メタ）アクリル酸、マロン酸／トリメチロールプロパン／（メタ）アクリル酸、マロン酸／グリセリン／（メタ）アクリル酸、マロン酸／ペンタエリスリトール／（メタ）アクリル酸、コハク酸／トリメチロールエタン／（メタ）アクリル酸、コハク酸／トリメチロールプロパン／（メタ）アクリル酸、コハク酸／グリセリン／（メタ）アクリル酸、コハク酸／ペンタエリスリトール／（メタ）アクリル酸、アジピン酸／トリメチロールエタン／（メタ）アクリル酸、アジピン酸／トリメチロールプロパン／（メタ）アクリル酸、アジピン酸／グリセリン／（メタ）アクリル酸、アジピン酸／ペンタエリスリトール／（メタ）アクリル酸、グルタル酸／トリメチロールエタン／（メタ）アクリル酸、グルタル酸／トリメチロールプロパン／（メタ）アクリル酸、グルタル酸／グリセリン／（メタ）アクリル酸、グルタル酸／ペンタエリスリトール／（メタ）アクリル酸、セバシン酸／トリメチロールエタン／（メタ）アクリル酸、セバシン酸／トリメチロールプロパン／（メタ）アクリル酸、セバシン酸／グリセリン／（メタ）アクリル酸、セバシン酸／ペンタエリスリトール／（メタ）アクリル酸、フマル酸／トリメチロールエタン／（メタ）アクリル酸、フマル酸／トリメチロールプロパン／（メタ）アクリル酸、フマル酸／グリセリン／（メタ）アクリル酸、フマル酸／ペンタエリスリトール／（メタ）アクリル酸、イタコン酸／トリメチロールエタン／（メタ）アクリル酸、イタコン酸／トリメチロールプロパン／（メタ）アクリル酸、イタコン酸／グリセリン／（メタ）アクリル酸、イタコン酸／ペンタエリスリトール／（メタ）アクリル酸、無水マレイン酸／トリメチロールエタン／（メタ）アクリル酸、無水マレイン酸／トリメチロールプロパン／（メタ）アクリル酸、無水マレイン酸／グリセリン／（メタ）アクリル酸、無水マレイン酸／ペンタエリスリトール／（メタ）アクリル酸等の多価アルコールと多価カルボン酸またはその無水物と（メタ）アクリル酸とから得られる、１分子中に２個以上の（メタ）アクリロイルオキシ基を有する直鎖状のエステル化物を挙げることができる。 Also, malonic acid / trimethylolethane / (meth) acrylic acid, malonic acid / trimethylolpropane / (meth) acrylic acid, malonic acid / glycerin / (meth) acrylic acid, malonic acid / pentaerythritol / (meth) acrylic acid Succinic acid / trimethylolethane / (meth) acrylic acid, succinic acid / trimethylolpropane / (meth) acrylic acid, succinic acid / glycerin / (meth) acrylic acid, succinic acid / pentaerythritol / (meth) acrylic acid, Adipic acid / trimethylolethane / (meth) acrylic acid, adipic acid / trimethylolpropane / (meth) acrylic acid, adipic acid / glycerin / (meth) acrylic acid, adipic acid / pentaerythritol / (meth) acrylic acid, glutar Acid / trimethylolethane / (meth) acrylic acid Glutaric acid / trimethylolpropane / (meth) acrylic acid, glutaric acid / glycerin / (meth) acrylic acid, glutaric acid / pentaerythritol / (meth) acrylic acid, sebacic acid / trimethylolethane / (meth) acrylic acid, sebacine Acid / trimethylolpropane / (meth) acrylic acid, sebacic acid / glycerin / (meth) acrylic acid, sebacic acid / pentaerythritol / (meth) acrylic acid, fumaric acid / trimethylolethane / (meth) acrylic acid, fumaric acid / Trimethylolpropane / (meth) acrylic acid, fumaric acid / glycerin / (meth) acrylic acid, fumaric acid / pentaerythritol / (meth) acrylic acid, itaconic acid / trimethylolethane / (meth) acrylic acid, itaconic acid / Trimethylolpropane / (meth) ac Acid, itaconic acid / glycerin / (meth) acrylic acid, itaconic acid / pentaerythritol / (meth) acrylic acid, maleic anhydride / trimethylolethane / (meth) acrylic acid, maleic anhydride / trimethylolpropane / (meta ) From polyhydric alcohols such as acrylic acid, maleic anhydride / glycerin / (meth) acrylic acid, maleic anhydride / pentaerythritol / (meth) acrylic acid and polyhydric carboxylic acids or their anhydrides and (meth) acrylic acid The resulting linear esterified product having two or more (meth) acryloyloxy groups in one molecule can be exemplified.
また、３量化により得られるポリイソシアネート（たとえば、トリメチロールプロパントルイレンジイソシアネート、ヘキサメチレンジイソシアネート、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、キシレンジイソシアネート、４，４’−メチレンビス（シクロヘキシルイソシアネート）、イソホロンジイソシアネート、トリメチルヘキサメチレンジイソシアネート等）と、活性水素を有するアクリルモノマー（たとえば、２−ヒドロキシエチル（メタ）アクリレート、２−ヒドロキシプロピル（メタ）アクリレート、２−ヒドロキシ−３−メトキシプロピル（メタ）アクリレート、Ｎ−メチロール（メタ）アクリルアミド、Ｎ−ヒドロキシ（メタ）アクリルアミド、１，２，３−プロパントリオール−１，３−ジ（メタ）アクリレート、３−アクリロイルオキシ−２−ヒドロキシプロピル（メタ）アクリレート等）とを、ポリイソシアネート１モル当たりにアクリルモノマー３モル以上を反応させて得られるウレタン（メタ）アクリレート；トリス（２−ヒドロキシエチル）イソシアヌル酸のジ（メタ）アクリレート、トリ（メタ）アクリレート等のポリ［（メタ）アクリロイルオキシエチレン］イソシアヌレート；公知のエポキシポリアクリレート；公知のウレタンポリアクリレート等を挙げることができる。上述した重合性化合物は、１種を単独で用いてもよく、２種以上を併用してもよい。 Polyisocyanates obtained by trimerization (for example, trimethylolpropane toluylene diisocyanate, hexamethylene diisocyanate, tolylene diisocyanate, diphenylmethane diisocyanate, xylene diisocyanate, 4,4'-methylenebis (cyclohexyl isocyanate), isophorone diisocyanate, trimethylhexamethylene Diisocyanate and the like) and an acrylic monomer having active hydrogen (for example, 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 2-hydroxy-3-methoxypropyl (meth) acrylate), N-methylol (meta ) Acrylamide, N-hydroxy (meth) acrylamide, 1,2,3-propanetriol-1,3-di (me ) Acrylate, 3-acryloyloxy-2-hydroxypropyl (meth) acrylate, etc.) and a urethane (meth) acrylate obtained by reacting 3 moles or more of an acrylic monomer per mole of polyisocyanate; tris (2-hydroxyethyl) ) Poly [(meth) acryloyloxyethylene] isocyanurate such as di (meth) acrylate and tri (meth) acrylate of isocyanuric acid; known epoxy polyacrylate; known urethane polyacrylate. The above-mentioned polymerizable compounds may be used alone or in combination of two or more.
光重合開始剤は、特に限定されるものではなく、たとえばベンゾイン、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、ベンゾインイソブチルエーテル、アセトイン、ブチロイン、トルオイン、ベンゾフェノン、ｐ−メトキシベンゾフェノン、２，２−ジエトキシアセトフェノン、α，α−ジメトキシ−α−フェニルアセトフェノン、メチルフェニルグリオキシレート、エチルフェニルグリオキシレート、４，４’−ビス（ジメチルアミノ）ベンゾフェノン、２−ヒドロキシ−２−メチル−１−フェニルプロパン−１−オン等のカルボニル化合物；テトラメチルチウラムモノスルフィド、テトラメチルチウラムジスルフィド等の硫黄化合物；２，４，６−トリメチルベンゾイルジフェニルフォスフィンオキサイド、ベンゾイルジエトキシフォスフィンオキサイド等を挙げることができる。上述した光重合開始剤は、１種を単独で用いてもよく、２種以上を併用してもよい。 The photopolymerization initiator is not particularly limited. For example, benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin isobutyl ether, acetoin, butyroin, toluoin, benzophenone, p-methoxybenzophenone, 2,2- Diethoxyacetophenone, α, α-dimethoxy-α-phenylacetophenone, methylphenylglyoxylate, ethylphenylglyoxylate, 4,4′-bis (dimethylamino) benzophenone, 2-hydroxy-2-methyl-1-phenyl Carbonyl compounds such as propan-1-one; sulfur compounds such as tetramethylthiuram monosulfide and tetramethylthiuram disulfide; 2,4,6-trimethylbenzoyldiphenyl phosphite Oxide, can be exemplified benzo dichloride ethoxy phosphine oxide and the like. The photoinitiator mentioned above may be used individually by 1 type, and may use 2 or more types together.
光重合開始剤の添加量は、重合性化合物１００質量部に対し、０．１〜１０質量部であることが好ましい。０．１質量部以上であると、活性エネルギー線重合性組成物の硬化性が向上する傾向がある。また、１０質量部以下であると、硬化後の着色が発生しない傾向がある。 It is preferable that the addition amount of a photoinitiator is 0.1-10 mass parts with respect to 100 mass parts of polymeric compounds. There exists a tendency for the sclerosis | hardenability of an active energy ray polymeric composition to improve that it is 0.1 mass part or more. Moreover, there exists a tendency for coloring after hardening to not generate | occur | produce that it is 10 mass parts or less.
鋳型用フィルムの凹凸層を形成するための、活性エネルギー線重合性組成物（Ｂ）は必要に応じて溶剤を含んでもよい。溶剤は活性エネルギー線重合性組成物（Ｂ）を構成する重合性化合物を溶解すると共に、透明基材フィルム（Ａ）を白化させないものが好ましく、例えば、アセトン、ジエチルケトン、ジプロピルケトン、メチルエチルケトン、メチルブチルケトン、メチルイソブチルケトン、シクロヘキサノン、ギ酸メチル、ギ酸エチル、ギ酸プロピル、ギ酸イソプロピル、ギ酸ブチル、酢酸メチル、酢酸エチル、酢酸プロピル、酢酸イソプロピル、酢酸ブチル、酢酸イソブチル、酢酸第二ブチル、酢酸アミル、酢酸イソアミル、酢酸第二アミル、プロピオン酸メチル、プロピオン酸エチル、酪酸メチル、酪酸エチル、乳酸メチルなどのケトン類またはカルボン酸エステル類、メタノール、エタノール、イソプロパノール、ｎ−ブタノール、sec-ブタノール、tert-ブタノールなどのアルコール類を挙げることができる。これらの溶剤は単一でも２成分以上の混合物でもよい。 The active energy ray-polymerizable composition (B) for forming the concavo-convex layer of the mold film may contain a solvent as necessary. The solvent preferably dissolves the polymerizable compound constituting the active energy ray polymerizable composition (B) and does not whiten the transparent substrate film (A). For example, acetone, diethyl ketone, dipropyl ketone, methyl ethyl ketone, Methyl butyl ketone, methyl isobutyl ketone, cyclohexanone, methyl formate, ethyl formate, propyl formate, isopropyl formate, butyl formate, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate, sec-butyl acetate, amyl acetate , Ketones or carboxylic esters such as isoamyl acetate, secondary amyl acetate, methyl propionate, ethyl propionate, methyl butyrate, ethyl butyrate, methyl lactate, methanol, ethanol, isopropanol, n-butanol, sec-butanol, Mention may be made of alcohols such as tert-butanol. These solvents may be single or a mixture of two or more components.
さらに、活性エネルギー線重合性組成物（Ｂ）は必要に応じて従来から使用されている種々の添加剤を添加してもよい。添加剤としては、界面活性剤、レベリング剤、染料、顔料、酸化防止剤、紫外線吸収剤、安定剤、難燃剤、可塑剤等を挙げることができる。 Furthermore, the active energy ray-polymerizable composition (B) may be added with various additives conventionally used as necessary. Examples of the additive include a surfactant, a leveling agent, a dye, a pigment, an antioxidant, an ultraviolet absorber, a stabilizer, a flame retardant, and a plasticizer.
鋳型用フィルムの製造方法の一つとしては、透明基材フィルム（Ａ）上に溶剤を含む活性エネルギー線重合性組成物（Ｂ）と凹凸形成のための微粒子との混合物を塗工し、乾燥させて溶剤を揮発させた上で、活性エネルギー線を照射して活性エネルギー線重合性組成物と微粒子の混合物を硬化させることで、表面に凹凸の皮膜を形成する方法がある。 As one method for producing a mold film, a mixture of an active energy ray-polymerizable composition (B) containing a solvent and fine particles for forming irregularities is coated on a transparent substrate film (A) and dried. Then, after volatilizing the solvent, there is a method of forming an uneven film on the surface by irradiating the active energy ray to cure the mixture of the active energy ray polymerizable composition and the fine particles.
微粒子は有機微粒子または無機微粒子を使用することができる。有機微粒子としては、例えば、アクリル樹脂（ＰＭＭＡ）、ポリスチレン（ＰＳ）、アクリル−スチレン共重合体、メラミン樹脂、ポリカーボート（ＰＣ）などを用いることができる。有機微粒子は、架橋や未架橋などの特性には特に限定されるものではなく、任意に選択できる。また、無機微粒子としては、例えば、酸化珪素、酸化チタン、酸化アルミニウム、酸化亜鉛、酸化錫、炭酸カルシウム、硫酸バリウム、タルク、カオリン、硫酸カルシウムなどからなるものを用いることができる。これらの無機微粒子に対して例えばシランカップリング処理等の有機物処理を施すことにより、該微粒子が有機物に分散し易くすることが好ましい。 As the fine particles, organic fine particles or inorganic fine particles can be used. As the organic fine particles, for example, acrylic resin (PMMA), polystyrene (PS), acrylic-styrene copolymer, melamine resin, polycarbonate (PC) and the like can be used. The organic fine particles are not particularly limited in properties such as crosslinking and non-crosslinking, and can be arbitrarily selected. Moreover, as inorganic fine particles, what consists of silicon oxide, titanium oxide, aluminum oxide, zinc oxide, tin oxide, calcium carbonate, barium sulfate, talc, kaolin, calcium sulfate etc. can be used, for example. These inorganic fine particles are preferably subjected to an organic treatment such as a silane coupling treatment so that the fine particles are easily dispersed in the organic matter.
微粒子の大きさは、適宜選択することができる。例えば、本鋳型用フィルムを用いて後述の防眩性樹脂板を製造する場合、該樹脂板の表面凹凸形状としては、表面中心線平均粗さが０．０５〜０．３μｍ、表面凹凸ピッチが３０〜２００μｍであることが好ましく、このようになる粒子径の微粒子を用いることになる。 The size of the fine particles can be appropriately selected. For example, when manufacturing the below-mentioned anti-glare resin plate using this mold film, the surface roughness of the resin plate is 0.05 to 0.3 μm on the surface center line average roughness, and the surface roughness pitch is It is preferable that it is 30-200 micrometers, and the microparticles | fine-particles of such a particle diameter will be used.
活性エネルギー線重合性組成物（Ｂ）の塗工方法は、特に限定されるものではなく、公知の塗工方法を用いることができる。塗工方法としては、例えば、マイクログラビアコート法、ワイヤーバーコート法、ダイレクトグラビアコート法、ダイコート法、ディップ法、スプレーコート法、リバースロールコート法、カーテンコート法、コンマコート法、ナイフコート法、スピンコート法などが挙げられる。 The coating method of the active energy ray polymerizable composition (B) is not particularly limited, and a known coating method can be used. As the coating method, for example, micro gravure coating method, wire bar coating method, direct gravure coating method, die coating method, dipping method, spray coating method, reverse roll coating method, curtain coating method, comma coating method, knife coating method, Examples include spin coating.
活性エネルギー線重合性組成物（Ｂ）の乾燥後の平均膜厚は、好ましくは３μｍ以上であることが好ましく、４μｍ以上であることがより好ましい。また３０μｍ以下であることが好ましく、１５μｍ以下であることがより好ましい。膜厚が薄すぎると、所望の凹凸を得ることが困難となり、膜厚が厚すぎると、大きくカールすることがある。 The average film thickness after drying of the active energy ray polymerizable composition (B) is preferably 3 μm or more, and more preferably 4 μm or more. Moreover, it is preferable that it is 30 micrometers or less, and it is more preferable that it is 15 micrometers or less. If the film thickness is too thin, it becomes difficult to obtain desired irregularities, and if the film thickness is too thick, the film may be largely curled.
乾燥条件は特に限定されるものではなく、自然乾燥であっても、乾燥温度や乾燥時間などの調整による人工的乾燥であってもよい。但し、乾燥時に塗料表面に風を当てる場合、塗膜表面に風紋が生じないようすることが好ましい。風紋が生じると防眩層表面に所望のなだらかなうねりの微細凹凸形状が形成されにくくなる傾向があり、防眩性とコントラストとを両立することが困難になるからである。また、乾燥温度および乾燥時間は塗料中に含まれる溶剤の沸点によって適宜決定することが可能である。その場合、乾燥温度および乾燥時間は、透明基材フィルムの耐熱性を配慮し、熱収縮により透明基材フィルム（Ａ）の変形が起きない範囲で選定することが好ましい。 The drying conditions are not particularly limited, and may be natural drying or artificial drying by adjusting drying temperature, drying time, and the like. However, when wind is applied to the surface of the paint at the time of drying, it is preferable not to generate a wind pattern on the surface of the coating film. This is because when the wind ripples are generated, it is difficult to form a desired undulating fine uneven shape on the surface of the antiglare layer, and it is difficult to achieve both antiglare property and contrast. Further, the drying temperature and drying time can be appropriately determined depending on the boiling point of the solvent contained in the paint. In that case, considering the heat resistance of the transparent substrate film, the drying temperature and drying time are preferably selected within a range in which the deformation of the transparent substrate film (A) does not occur due to heat shrinkage.
乾燥後の活性エネルギー線重合性組成物（Ｂ）は活性エネルギー線を照射することによって硬化する。 The active energy ray polymerizable composition (B) after drying is cured by irradiation with active energy rays.
活性エネルギー線としては紫外線が好ましく、活性エネルギー線の光源としては、超高圧水銀ランプ、高圧水銀ランプ、中圧水銀ランプ、低圧水銀ランプ、メタルハライドランプ、キセノンランプ、高周波誘導水銀ランプ、ケミカルランプ等が適している。 As the active energy ray, ultraviolet rays are preferable, and as the light source of the active energy ray, an ultrahigh pressure mercury lamp, a high pressure mercury lamp, a medium pressure mercury lamp, a low pressure mercury lamp, a metal halide lamp, a xenon lamp, a high frequency induction mercury lamp, a chemical lamp, etc. Is suitable.
積算照射量は、重合性組成物の硬化特性などを考慮して適宜選択することが好ましい。また、照射の雰囲気としては、樹脂硬化の程度に応じて適宜選択することができ、例えば、窒素、アルゴンなどの不活性ガス、または空気の雰囲気が挙げられる。 It is preferable that the integrated dose is appropriately selected in consideration of the curing characteristics of the polymerizable composition. Further, the irradiation atmosphere can be appropriately selected according to the degree of resin curing, and examples thereof include an atmosphere of an inert gas such as nitrogen and argon, or air.
また、鋳型用フィルムの他の製造方法としては、表面に凹凸形状を有する原版の該凹凸形状を、活性エネルギー線重合性組成物（Ｂ）に転写することで凹凸層の凹凸形状を形成する方法が挙げられる。即ち、透明基材フィルム（Ａ）の任意の面に活性エネルギー線重合性組成物（Ｂ）を塗工し、表面に凹凸形状を有するエンボスローラーまたは平板状のエンボス板等の凹凸鋳型を活性エネルギー線重合性組成物（Ｂ）を介して透明基材フィルム（Ａ）に圧着させ、透明基材フィルム（Ａ）を介して活性エネルギー線を照射して、活性エネルギー線重合性組成物（Ｂ）を硬化させ、該凹凸鋳型から透明基材フィルム（Ａ）を活性エネルギー線重合性組成物（Ｂ）の硬化膜とともに剥離することで、表面に凹凸形状を転写した鋳型用フィルムを製造することができる。 In addition, as another method for producing a mold film, a method for forming a concavo-convex shape of a concavo-convex layer by transferring the concavo-convex shape of an original having a concavo-convex shape on the surface to the active energy ray polymerizable composition (B). Is mentioned. That is, the active energy ray polymerizable composition (B) is applied to an arbitrary surface of the transparent substrate film (A), and an embossed mold such as an embossing roller having a concavo-convex shape on the surface or a flat embossed plate is used as the active energy. The active energy ray polymerizable composition (B) is bonded to the transparent substrate film (A) through the linear polymerizable composition (B) and irradiated with active energy rays through the transparent substrate film (A). Is cured, and the transparent substrate film (A) is peeled from the concavo-convex mold together with the cured film of the active energy ray polymerizable composition (B) to produce a mold film having the concavo-convex shape transferred to the surface. it can.
エンボスローラーまたは平板状のエンボス板等に形成されている凹凸型面は、良好な光学特性を発現する凹凸形状を形成できる方法であれば、特に限定されないが、例えばメッキ処理をした金属ロールもしくは平板にサンドブラスト法またはビーズショット法によって表面を荒らすことにより得ることができる。 The concavo-convex surface formed on the embossing roller or the flat embossing plate is not particularly limited as long as it is a method capable of forming the concavo-convex shape exhibiting good optical characteristics. For example, a plated metal roll or flat plate It can be obtained by roughening the surface by sandblasting or bead shot.
透明基材フィルム（Ａ）の少なくとも一方の表面に対する活性エネルギー線重合性組成物（Ｂ）を塗布し、硬化させる方法は前記の方法が使用できる。 As the method for applying and curing the active energy ray polymerizable composition (B) on at least one surface of the transparent substrate film (A), the above-described method can be used.
本発明の鋳型用フィルムは、凹凸面に対して放電処理を施す。この放電処理により鋳型用フィルムの、活性エネルギー線重合性組成物の硬化皮膜からの良好な剥離性を得ることができる。本発明の鋳型用フィルムに対する放電処理としてはコロナ処理もしくはプラズマ処理を用いることができる。 The casting film of the present invention is subjected to a discharge treatment on the uneven surface. By this electric discharge treatment, it is possible to obtain good peelability of the casting film from the cured film of the active energy ray polymerizable composition. Corona treatment or plasma treatment can be used as the discharge treatment for the mold film of the present invention.
コロナ処理は、通常のコロナ処理装置を使用して処理することができる。コロナ処理の一例を以下に示す。即ち、電気絶縁されたベルトとベルト上方に近接させて配置した電極からなるコロナ処理装置を用いて、該電極に高エネルギーを作用させてコロナ放電させ、ベルト上に凹凸面を上面として配置した鋳型用フィルムを電極下を通すことにより鋳型用フィルムの凹凸面にコロナ処理を施す。 Corona treatment can be carried out using a normal corona treatment apparatus. An example of corona treatment is shown below. That is, using a corona treatment device comprising an electrically insulated belt and an electrode disposed close to the belt, a high energy is applied to the electrode to cause corona discharge, and a mold having an uneven surface on the belt as an upper surface. The corrugated surface of the casting film is subjected to corona treatment by passing the working film under the electrode.
この時の鋳型用フィルムに対する照射エネルギーは１０Ｗ・分／ｍ以上２００Ｗ・分／ｍ以下が好ましい。照射エネルギーが低すぎると性能が十分に発揮されず、照射エネルギーが高すぎるとフィルム外観に影響が出ることがある。また、鋳型用フィルムと電極のクリアランスはコロナ放電を安定に発生させるために５ｍｍ以下が好ましい。 The irradiation energy for the mold film at this time is preferably 10 W · min / m or more and 200 W · min / m or less. If the irradiation energy is too low, the performance is not sufficiently exhibited, and if the irradiation energy is too high, the film appearance may be affected. Further, the clearance between the mold film and the electrode is preferably 5 mm or less in order to stably generate corona discharge.
プラズマ処理は、通常のプラズマ処理装置を使用して処理することができるが、大気圧プラズマ処理装置が操作上、簡便であることから好ましい。中でもリモート法、ダイレクト法いずれでもよいが、均一な処理が得られる点でダイレクト法が好ましい。 The plasma processing can be performed using a normal plasma processing apparatus, but the atmospheric pressure plasma processing apparatus is preferable because it is simple in operation. Of these, either the remote method or the direct method may be used, but the direct method is preferable in that uniform treatment can be obtained.
大気圧プラズマ処理装置の構成の一例を以下に示す。即ち処理用のチャンバー内に上部電極と下部電極からなる一対の対向電極を備え、少なくとも一方の電極の対向面が誘電体で被覆されたものである。プラズマが発生する部位は、対向電極のいずれか一方のみに誘電体が被覆された場合には誘電体と電極の間であり、いずれにも誘電体が被覆された場合には誘電体間である。このようなプラズマ処理装置の対向電極間に鋳型用フィルムを配置し、電源部に高周波電力を印加して対向電極間にプラズマを発生させ、表面をプラズマ処理する。 An example of the configuration of the atmospheric pressure plasma processing apparatus is shown below. That is, a pair of counter electrodes made up of an upper electrode and a lower electrode are provided in a processing chamber, and the opposing surface of at least one of the electrodes is covered with a dielectric. The part where the plasma is generated is between the dielectric and the electrode when only one of the counter electrodes is covered with the dielectric, and between the dielectric when any of the counter electrodes is covered with the dielectric. . A casting film is disposed between the counter electrodes of such a plasma processing apparatus, high-frequency power is applied to the power supply unit to generate plasma between the counter electrodes, and the surface is subjected to plasma processing.
対向電極の対向面間の距離（最短距離）は、処理される鋳型用フィルムの厚さ、被覆された誘電体の厚さ、印加される電圧の大きさ等を考慮して決定されるが、対向電極の一方のみに誘電体が被覆された場合、両方に誘電体が被覆された場合のいずれにおいても、５０ｍｍ以下であることが好ましい。最短距離が５０ｍｍ以下であると、均一な放電プラズマを発生させることができる。 The distance between the opposing surfaces of the counter electrode (shortest distance) is determined in consideration of the thickness of the mold film to be processed, the thickness of the coated dielectric, the magnitude of the applied voltage, etc. In either case where only one of the counter electrodes is coated with a dielectric, and both are coated with a dielectric, it is preferably 50 mm or less. When the shortest distance is 50 mm or less, uniform discharge plasma can be generated.
対向電極間に印加する高周波電力の周波数は、１ｋＨｚ以上であることが好ましい。また１０ＭＨｚ以下であることが好ましく、５００ｋＨｚ以下であることがより好ましい。電力面密度は２．０Ｗ／ｃｍ２以上であることが好ましく、３０．０Ｗ／ｃｍ２以下であることが好ましい。周波数が１ｋＨｚ以上５００ｋＨｚ以下であると、鋳型用フィルムの処理時の変形や劣化が抑制される。また、電力面密度が３０．０Ｗ／ｃｍ２以下であると、プラズマ照射熱による鋳型用フィルムの変形を抑制することができる。なお、電力面密度とは、一対の対向電極間に投入する電力をプラズマと接している一方の電極の表面積で割った値である。 The frequency of the high frequency power applied between the counter electrodes is preferably 1 kHz or more. Moreover, it is preferable that it is 10 MHz or less, and it is more preferable that it is 500 kHz or less. The power surface density is preferably 2.0 W / cm 2 or more, and preferably 30.0 W / cm 2 or less. When the frequency is 1 kHz or more and 500 kHz or less, deformation and deterioration during processing of the mold film are suppressed. Further, when the power surface density is 30.0 W / cm 2 or less, deformation of the mold film due to plasma irradiation heat can be suppressed. The power surface density is a value obtained by dividing the power input between a pair of counter electrodes by the surface area of one electrode in contact with plasma.
コロナ処理、プラズマ処理を行うことにより得られた鋳型用フィルムはマイクロインデンター測定により得られる凹凸層側の押し込み弾性率が、処理前のそれより大きい値であることが好ましい。コロナ処理あるいはプラズマ処理の際、前記の処理条件を適宜選択することにより、押し込み弾性率の値を調整することができる。 The casting film obtained by performing the corona treatment or the plasma treatment preferably has a larger indentation elastic modulus on the uneven layer side obtained by microindenter measurement than that before the treatment. In the case of corona treatment or plasma treatment, the value of the indentation elastic modulus can be adjusted by appropriately selecting the treatment conditions.
次に防眩性樹脂板の製造方法について説明する。 Next, the manufacturing method of an anti-glare resin board is demonstrated.
即ち、透明基材フィルム（Ａ）の少なくとも一方の表面に活性エネルギー線重合性組成物（Ｂ）を塗布及び硬化して凹凸層を設けた鋳型用フィルムを作製する第一の工程、鋳型用フィルムの凹凸層の表面に対し、放電処理を施す第二の工程、活性エネルギー線重合性組成物（Ｃ）を介して、鋳型用フィルムの凹凸層の表面と透明樹脂板を貼り合わせる第三の工程、活性エネルギー線の照射により活性エネルギー線重合性組成物（Ｃ）を硬化させる第四の工程、鋳型用フィルムを剥離、除去する第五の工程からなる防眩性樹脂板の製造方法である。 That is, a first step for producing a mold film in which an uneven layer is provided by applying and curing the active energy ray polymerizable composition (B) on at least one surface of the transparent substrate film (A), the mold film The second step of applying a discharge treatment to the surface of the concavo-convex layer, the third step of bonding the surface of the concavo-convex layer of the mold film and the transparent resin plate via the active energy ray polymerizable composition (C) And a fourth step of curing the active energy ray-polymerizable composition (C) by irradiation of active energy rays, and a fifth method of peeling and removing the mold film, and a method for producing an antiglare resin plate.
防眩性樹脂板を製造する際に使用する透明樹脂板としては、トリアセテートセルロース（ＴＡＣ）、ポリエチレンテレフタレート（ＰＥＴ）、ジアセチルセルロース、アセテートブチレートセルロース、ポリエーテルサルホン、アクリル樹脂、ポリウレタン樹脂、ポリエステル、ポリカーボネート、ポリスルホン、ポリエーテル、ポリメチルペンテン、ポリエーテルケトン、（メタ）アクリルロニトリル等からなる樹脂板を用いることができる。 Transparent resin plates used for producing anti-glare resin plates include triacetate cellulose (TAC), polyethylene terephthalate (PET), diacetyl cellulose, acetate butyrate cellulose, polyethersulfone, acrylic resin, polyurethane resin, polyester A resin plate made of polycarbonate, polysulfone, polyether, polymethylpentene, polyetherketone, (meth) acrylonitrile, or the like can be used.
本発明の防眩性樹脂板の製造で使用する活性エネルギー線重合性組成物（Ｃ）は、紫外線等の活性エネルギー線の照射により、硬化するものであれば、特に限定されるものではなく、例えば２つ以上のアクリロイル基、メタクリロイル基を含んだ組成物が挙げられる。該組成物は、シリコーン系やメラミン系化合物を含んでもよい。 The active energy ray polymerizable composition (C) used in the production of the antiglare resin plate of the present invention is not particularly limited as long as it is cured by irradiation with active energy rays such as ultraviolet rays. For example, a composition containing two or more acryloyl groups and methacryloyl groups can be mentioned. The composition may contain a silicone-based or melamine-based compound.
中でも、光硬化性組成物が好ましく、分子中に少なくとも２個の（メタ）アクリロイルオキシ基を有する重合性化合物と、光重合開始剤との混合物がより好ましく、活性エネルギー線重合性組成物（Ｃ）を構成する、重合性化合物と光重合開始剤の具体例としては、活性エネルギー線重合性組成物（Ｂ）で例示したものが使用できる。 Among these, a photocurable composition is preferable, a mixture of a polymerizable compound having at least two (meth) acryloyloxy groups in the molecule and a photopolymerization initiator is more preferable, and an active energy ray polymerizable composition (C As the specific examples of the polymerizable compound and the photopolymerization initiator that constitute a), those exemplified for the active energy ray polymerizable composition (B) can be used.
本発明の防眩性樹脂板の製造において、鋳型用フィルムの凹凸面と透明樹脂板を活性エネルギー線重合性組成物（Ｃ）を介して貼り合せる工程において、活性エネルギー線重合性組成物（Ｃ）は鋳型用フィルムの凹凸面、もしくは透明樹脂板のいずれかに塗工すればよく、その塗工法としてはバーコーター法、アプリケーター法、カーテンフローコーター法、ロールコーター法等、公知の方法を適用可能である。その後、プレスロールで圧接し、透明樹脂板上に一定膜厚に圧延する。活性エネルギー線重合性組成物（Ｃ）の膜厚としては、硬度の観点より1μｍ以上であることが好ましく、得られる防眩性樹脂板の反りや作製される硬化膜のクラック等の欠陥を抑制する観点より５０μｍ以下であることが好ましい。 In the production of the antiglare resin plate of the present invention, in the step of bonding the uneven surface of the mold film and the transparent resin plate via the active energy ray polymerizable composition (C), the active energy ray polymerizable composition (C ) Can be applied to either the concavo-convex surface of the mold film or a transparent resin plate. As the coating method, a known method such as a bar coater method, an applicator method, a curtain flow coater method, or a roll coater method is applied. Is possible. Then, it press-contacts with a press roll and it rolls to a fixed film thickness on a transparent resin board. The film thickness of the active energy ray polymerizable composition (C) is preferably 1 μm or more from the viewpoint of hardness, and suppresses defects such as warpage of the resulting antiglare resin plate and cracks in the cured film produced. It is preferable that it is 50 micrometers or less from the viewpoint to do.
鋳型用フィルムと透明樹脂板を活性エネルギー線重合性組成物（Ｃ）を介して貼り合わせる前記第三の工程において、活性エネルギー線重合性組成物（Ｃ）の硬化膜と透明樹脂板の良好な密着性を得るという観点から、４０℃以上の温度で貼り合せることが好ましい。また、得られる防眩性樹脂板の耐擦傷性を維持する観点から、７０℃以下の温度で貼り合わせることが好ましい。また、活性エネルギー線重合性組成物（Ｃ）の硬化膜と透明樹脂板の良好な密着性を得るという観点から、貼り合せたその温度において３０秒以上保持することが好ましい。また、得られる防眩性樹脂板の耐擦傷性を維持する観点から、貼り合せたその温度において１２０秒以下保持することが好ましい。 In the third step of bonding the film for mold and the transparent resin plate via the active energy ray polymerizable composition (C), the cured film of the active energy ray polymerizable composition (C) and the transparent resin plate are excellent. From the viewpoint of obtaining adhesion, it is preferable to bond at a temperature of 40 ° C. or higher. Moreover, it is preferable to bond together at the temperature of 70 degrees C or less from a viewpoint of maintaining the abrasion resistance of the anti-glare resin board obtained. Further, from the viewpoint of obtaining good adhesion between the cured film of the active energy ray-polymerizable composition (C) and the transparent resin plate, it is preferably maintained for 30 seconds or more at the bonded temperature. Moreover, it is preferable to hold | maintain for 120 seconds or less at the temperature which bonded together from a viewpoint of maintaining the abrasion resistance of the anti-glare resin board obtained.
本発明では、鋳型用フィルムと透明樹脂板を貼り合せた後、鋳型用フィルムを介して、活性エネルギー線を照射し、活性エネルギー線重合性組成物（Ｃ）を硬化させ、凹凸を有する硬化膜を形成する。 In the present invention, after the mold film and the transparent resin plate are bonded together, the active energy ray is irradiated through the mold film to cure the active energy ray polymerizable composition (C), and a cured film having irregularities. Form.
活性エネルギー線及びその光源としては、前記活性エネルギー線重合性組成物（Ｂ）を硬化させる時に使用するものと同様のものが使用できる。活性エネルギー線の照射エネルギーとしては、硬化膜と透明樹脂板の密着性を確保する点から、３００ｍＪ／ｃｍ２以上とすることが好ましい。該照射エネルギーは、光源の種類、光源と樹脂フィルム面との距離、照射時間を適宜選択することにより調整できる。 As the active energy ray and the light source thereof, the same materials as those used when the active energy ray polymerizable composition (B) is cured can be used. The irradiation energy of the active energy ray is preferably 300 mJ / cm 2 or more from the viewpoint of securing the adhesion between the cured film and the transparent resin plate. The irradiation energy can be adjusted by appropriately selecting the type of light source, the distance between the light source and the resin film surface, and the irradiation time.
本発明の防眩性樹脂板の製造において、活性エネルギー線重合性組成物（Ｃ）を硬化した後に、鋳型用フィルムを剥離する。これにより透明樹脂板の表面に耐擦傷性を有する硬化被膜が形成された、防眩性樹脂板を得ることができる。 In the production of the antiglare resin plate of the present invention, the mold film is peeled after the active energy ray polymerizable composition (C) is cured. Thereby, the anti-glare resin board in which the cured film which has abrasion resistance was formed on the surface of the transparent resin board can be obtained.
本発明において、硬化被膜の耐擦傷性をさらに向上させる目的で、鋳型用フィルム剥離の後に、硬化被膜を形成した防眩性樹脂板に活性エネルギー線をさらに照射することが可能である。 In the present invention, for the purpose of further improving the scratch resistance of the cured coating, it is possible to further irradiate the anti-glare resin plate on which the cured coating is formed with an active energy ray after the mold film is peeled off.
本発明の製造方法で得られた防眩性樹脂板はＣＲＴ、プラズマディスプレイ、液晶ディスプレイ、エレクトロルミネッセンスディスプレイ、もしくは電子ペーパー等の画像表示装置の前面板として好適に使用できる。さらに、太陽電池モジュールの表面保護樹脂板としても使用できる。この場合における太陽電池モジュールの構造は特に限定されないが、例えば、光入射面から、防眩層を表面とした防眩性表面保護樹脂板、充填材、光起電力素子、充填材、裏面保護シートの順に積層された公知の構成とすることが出来る。 The anti-glare resin plate obtained by the production method of the present invention can be suitably used as a front plate of an image display device such as a CRT, plasma display, liquid crystal display, electroluminescence display, or electronic paper. Furthermore, it can also be used as a surface protective resin plate for solar cell modules. The structure of the solar cell module in this case is not particularly limited. For example, the antiglare surface protective resin plate, the filler, the photovoltaic element, the filler, and the back surface protective sheet having the antiglare layer as the surface from the light incident surface. It can be set as the well-known structure laminated | stacked in order.
以下、実施例により本発明を詳しく説明するが、本発明はこれらに限定されるものではない。ここで、実施例、比較例で使用した化合物の略称は以下の通りである。
Ｍ４００：ジペンタエリスリトールヘキサアクリレート Ｍ−４００（東亞合成（株）製）
ＴＡＳ：トリメチロールエタン・アクリル酸・無水コハク酸縮合エステル（大阪有機（株）製）
Ｍ−３０５：ペンタエリスルトールトリ／テトラアクリレート（東亞合成（株）製）
Ｃ６ＤＡ：１,６−ヘキサンジオールジアクリレート（大阪有機化学工業(株)社製）
ルシリンＴＰＯ：ジフェニル−（２，４，６−トリメチルベンゾイル）フォスフィンオキサイド（ＢＡＳＦジャパン（株）社製）
ＩＲＧＡＣＵＲＥ９０７：２−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（チバジャパン（株）製）
ダロキュア１１７３：２−ヒドロキシ−２−メチル−１−フェニル−プロパン−１−オン（チバジャパン（株）製）
トスパール１２０：シリカ粒子 粒子系１．９μｍ（ＧＥ東芝シリコーン社製）
ＫＢＭ５０３：３−メタクリロキシプロピルトリメトキシシラン（信越シリコーン（株）製）
ＳＳＸ‐１０５：架橋ＰＭＭＡ微粒子 平均粒子径５μｍ（積水化成品工業（株）製テクポリマー）
ＸＸ‐１１０Ｂ：架橋スチレン微粒子 平均粒子径３．５μｍ（積水化成品工業（株）製テクポリマー）
トスパール１４５：シリコーン粒子 粒子系４．５μｍ（ＧＥ東芝シリコーン社製）
ＭＢＸ−５：架橋ＰＭＭＡ微粒子 平均粒子径５μｍ（積水化成品工業（株）製テクポリマー）
ＭＳＸ−６：架橋スチレン微粒子 平均粒子径６μｍ（積水化成品工業（株）製テクポリマー）
ビスコート＃１９２：フェノキシエチルアクリレート（大阪有機化学工業(株)社製）
エポキシエステル３０００Ａ：ビスフェノールＡ−ジエポキシ−アクリレート（共栄社油脂化学工業社製）
コスモシャインＡ４１００：ＰＥＴフィルム（東洋紡績（株）社製）
アクリライトＬ：アクリル樹脂板（三菱レイヨン（株）製）
また、実施例、比較例で行った評価方法は下記の通りである。
（剥離性試験）
活性エネルギー線重合性組成物（Ｃ）を硬化した後に、鋳型用フィルムを剥離しようとした際に剥離すれば○、フィルムが破れる等、剥離できなかった場合は×として評価した。
（密着性試験）
防眩性樹脂板の凹凸面に目通しカッター（商品名、コーテック（株）製）を用いて、カッターで１００マスをカットし、セロハンテープ（商品名：ＣＴ−２４、ニチバン（株））を用いて、剥離試験を実施して、凹凸層の未剥離マスの数で密着性を以下の基準で評価した。
EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited to these. Here, the abbreviations of the compounds used in Examples and Comparative Examples are as follows.
M400: Dipentaerythritol hexaacrylate M-400 (manufactured by Toagosei Co., Ltd.)
TAS: Trimethylolethane / acrylic acid / succinic anhydride condensation ester (Osaka Organic Co., Ltd.)
M-305: Pentaerythritol tri / tetraacrylate (manufactured by Toagosei Co., Ltd.)
C6DA: 1,6-hexanediol diacrylate (manufactured by Osaka Organic Chemical Industry Co., Ltd.)
Lucillin TPO: Diphenyl- (2,4,6-trimethylbenzoyl) phosphine oxide (manufactured by BASF Japan Ltd.)
IRGACURE907: 2-methyl-1- [4- (methylthio) phenyl] -2-morpholinopropan-1-one (manufactured by Ciba Japan Co., Ltd.)
Darocur 1173: 2-hydroxy-2-methyl-1-phenyl-propan-1-one (manufactured by Ciba Japan)
Tospearl 120: Silica particle particle system 1.9 μm (GE Toshiba Silicone)
KBM503: 3-methacryloxypropyltrimethoxysilane (manufactured by Shin-Etsu Silicone Co., Ltd.)
SSX-105: Cross-linked PMMA fine particles Average particle size 5 μm (Techpolymer manufactured by Sekisui Plastics Co., Ltd.)
XX-110B: Cross-linked styrene fine particles Average particle size 3.5 μm (Techpolymer manufactured by Sekisui Plastics Co., Ltd.)
Tospearl 145: Silicone particle particle system 4.5 μm (GE Toshiba Silicone)
MBX-5: Cross-linked PMMA fine particles Average particle size 5 μm (Techpolymer manufactured by Sekisui Plastics Co., Ltd.)
MSX-6: Cross-linked styrene fine particles Average particle diameter 6 μm (Techpolymer manufactured by Sekisui Plastics Co., Ltd.)
Biscote # 192: Phenoxyethyl acrylate (manufactured by Osaka Organic Chemical Industry Co., Ltd.)
Epoxy ester 3000A: Bisphenol A-diepoxy-acrylate (manufactured by Kyoeisha Yushi Chemical Co., Ltd.)
Cosmo Shine A4100: PET film (manufactured by Toyobo Co., Ltd.)
Acrylite L: Acrylic resin board (Mitsubishi Rayon Co., Ltd.)
Moreover, the evaluation method performed by the Example and the comparative example is as follows.
(Peelability test)
After the active energy ray polymerizable composition (C) was cured, it was evaluated as x when it was not peeled off when it was peeled off when the film for mold was peeled off, and when the film was broken.
(Adhesion test)
Using a cutter (trade name, manufactured by Co-Tech Co., Ltd.) on the uneven surface of the antiglare resin plate, 100 squares are cut with the cutter, and cellophane tape (trade name: CT-24, Nichiban Co., Ltd.) is used. Then, a peel test was performed, and the adhesion was evaluated according to the following criteria by the number of unpeeled masses of the uneven layer.
剥離しない ○
一部剥離する ×
（耐擦傷性）
防眩性樹脂板の凹凸面の擦傷試験の前後におけるヘーズの変化（Δヘーズ）をもって評価した。即ち、＃０００のスチールウール（商品名：「ボンスター Ｎｏ．０００」、日本スチールウール（株）製）を装着した直径２４ｍｍの円形パッドをサンプルの防眩性樹脂板の凹凸面上に置き、２０００ｇの荷重下で、２０ｍｍの距離を１００回往復擦傷する。擦傷前と擦傷後のヘーズ値の差を下記式（１）より求めた。
[Δヘーズ（％）]＝[擦傷後ヘーズ値（％）]−[擦傷前ヘーズ値（％）] ・・・（１）
（防眩性）
防眩性樹脂板の凹凸面に対して４５°の方向の３ｍ離れた位置に６０Ｗの蛍光灯を配置し、該蛍光灯の光の正反射像を観察し、像の鮮明性を目視により評価した。蛍光灯の像が見えないと、防眩性良好とした。
（押し込み弾性率）
鋳型用フィルム表面における凹凸層側の押し込み弾性率について以下の条件のマイクロインデンター測定により得た。
Does not peel ○
Partially peel off ×
(Abrasion resistance)
The haze change (Δhaze) before and after the scratch test on the uneven surface of the antiglare resin plate was evaluated. That is, a circular pad with a diameter of 24 mm, on which # 000 steel wool (trade name: “Bonster No. 000”, manufactured by Nippon Steel Wool Co., Ltd.) was placed on the uneven surface of the sample antiglare resin plate, 2000 g Under a load of 100 mm, a reciprocal abrasion is performed 100 times over a distance of 20 mm. The difference in haze value before and after scratching was determined from the following formula (1).
[Δhaze (%)] = [haze value after abrasion (%)] − [haze value before abrasion (%)] (1)
(Anti-glare)
A 60 W fluorescent lamp is placed at a position 3 m away from the concavo-convex surface of the antiglare resin plate in a direction of 45 °, the specular reflection image of the light from the fluorescent lamp is observed, and the image clarity is visually evaluated. did. If no fluorescent lamp image was seen, the antiglare property was good.
(Indentation modulus)
The indentation elastic modulus on the uneven layer side on the surface of the mold film was obtained by microindenter measurement under the following conditions.
試験片に対し、圧子にかける力Ｆを０ｍＮより０．７ｍＮまで１０秒間かけて連続的に変化させて負荷を行い、その直後０．７ｍＮより０ｍＮまで１０秒間かけて除荷を行った。 The test piece was loaded by continuously changing the force F applied to the indenter from 0 mN to 0.7 mN over 10 seconds, and immediately after that, unloading was performed from 0.7 mN to 0 mN over 10 seconds.
その間の力Ｆと押込み深さｈの負荷−除荷曲線よりＩＳＯ１４５７７に準拠して押し込み弾性率の算出を行った。 The indentation elastic modulus was calculated according to ISO14577 from the load-unloading curve of the force F and the indentation depth h during that time.
（２ｃｍの四角形の各頂点と対角線の交点の計）５点を計測して、その平均値を値として用いた。
装置名：（株）フィッシャー・インストルメンツ製 フィッシャースコープHM2000
圧子：ビッカース角錐 ダイヤモンド圧子
試験時温度：２３℃
試験時湿度：６０％
（実施例１）
Ｍ４００ １００質量部
ＭＢＸ−５ １０質量部
イルガキュア９０７ ５質量部
メチルエチルケトン １５０質量部
上記原料からなる活性エネルギー線重合性組成物（Ｂ）をバーコーターにて、厚さ１００μｍのＰＥＴフィルム（コスモシャインＡ４１００）の易接着面上に、乾燥膜厚が１５μｍとなるように塗布し、８０℃で５分間乾燥した。その後、出力１２０Ｗ／ｃｍの高圧水銀灯を用いて、活性エネルギー線８００ｍＪ／ｃｍ２を照射することによって硬化させ凹凸形状を有する防眩層が形成された鋳型用フィルムを得た。
5 points were measured (total of intersections of 2 cm square vertices and diagonal lines), and the average value was used as a value.
Device name: Fisherscope HM2000 manufactured by Fisher Instruments Co., Ltd.
Indenter: Vickers pyramid Diamond indenter test temperature: 23 ° C
Test humidity: 60%
Example 1
M400 100 parts by mass MBX-5 10 parts by mass Irgacure 907 5 parts by mass Methyl ethyl ketone 150 parts by mass The active energy ray-polymerizable composition (B) made of the above raw materials was used with a bar coater to form a PET film having a thickness of 100 μm (Cosmo Shine A4100). On the easy-adhesive surface, it was applied so that the dry film thickness was 15 μm, and dried at 80 ° C. for 5 minutes. Thereafter, using a high-pressure mercury lamp with an output of 120 W / cm, the film for a mold on which an antiglare layer having an uneven shape was formed by curing by irradiating active energy rays of 800 mJ / cm 2 was obtained.
搬送ベルト上に配置した、厚さ１ｍｍ、長さ２６０ｍｍのＳＵＳ製電極に対してＮａｖｉｔａｓ製 コロナ処理装置ＰＯＬＹＤＹＮＥを用いて印加電圧 １１．６ｋＶをかけ、コロナ放電を起こし、凹凸面を上面にして搬送ベルト上に配置した鋳型用フィルムを、鋳型用フィルム−電極間ギャップ ３ｍｍ、搬送速度２.０ｍ／ｍｉｎで電極下部を通すことでコロナ処理を実施した。かかる条件における鋳型用フィルムに対する照射エネルギーは１００Ｗ・分／ｍであった。
Ｍ４００ ２５質量部
ＴＡＳ ３０質量部
Ｍ−３０５ ３５質量部
Ｃ６ＤＡ １０質量部
ルシリンＴＰＯ ２質量部
上記原料からなる活性エネルギー線重合性組成物（Ｃ）を、予め約７０℃に加熱した樹脂板（アクリライトＬ）上に塗工し、上記鋳型用フィルムを凹凸面を内面として被せ、プレスロールで圧接し活性エネルギー線重合性組成物（Ｃ）の厚みを１２μｍとなるように展延した。前記樹脂板に被せた鋳型用フィルムの表面温度を非接触式赤外線温度計で測定すると６０℃であり、その温度において６０秒保持した後、出力８４Ｗ／ｃｍのメタルハライドランプを用いて、積算光量で８００ｍＪ／ｃｍ２の紫外線を前記フィルム側から照射することによって活性エネルギー線重合性組成物（Ｃ）を硬化させた。硬化後鋳型用フィルムを剥離することで防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であり、得られた防眩性樹脂板の凹凸層（防眩層）は、良好な耐擦傷性を有し、樹脂板との密着性も良好であった。結果を表１に示す。
（実施例２）
実施例１の鋳型用フィルムに対するコロナ放電処理を、Ｎａｖｉｔａｓ製 コロナ処理装置ＰＯＬＹＤＹＮＥを用いて印加電圧を ９．３ｋＶに変更し、コロナ放電を起こし、凹凸面を上面にして搬送ベルト上に配置した鋳型用フィルムを、鋳型用フィルム−電極間ギャップ ３ｍｍ、搬送速度２.０ｍ／ｍｉｎで電極下部を通すことでコロナ処理を実施した以外は実施例１と同様の方法で鋳型用フィルムを作成した。かかる条件におけるコロナ処理の鋳型用フィルムに対する照射エネルギーは５０Ｗ・分／ｍであった。それを用いて実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であり、得られた防眩性樹脂板の防眩層は、良好な耐擦傷性を有し、樹脂板との密着性も良好であった。結果を表１に示す。
（実施例３）
実施例１の鋳型用フィルムに対する放電処理を、２０×２０×２００ｍｍのＳＵＳ製電極表面に、厚さ１ｍｍの酸化アルミニウムを溶射したものを用いた上部電極と、２００×２００×２０ｍｍのＳＵＳ製電極表面に、厚さ１ｍｍの酸化アルミニウムを溶射したものを用いた移動可能な下部電極を備える大気圧プラズマ処理装置を用いた。下部電極上に凹凸面を上面にして鋳型用フィルムを乗せ、電極間に処理ガス：Ｈｅ／Ｏ２＝３．０／０．０４L／minの供給速度にてガスを導入し、出力１００ｋＨｚ、２．５Ｗ／ｃｍ２にてプラズマを発生させ、搬送速度２．０ｍ／ｍｉｎ、処理時間０．６秒、電極間隔２．０ｍｍとなるよう、前記下部電極を移動させて、実施した以外は実施例１と同様の方法で鋳型用フィルムを作製、それを用いて実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であり、得られた防眩性樹脂板の防眩層は、良好な耐擦傷性を有し、樹脂板との密着性も良好であった。結果を表１に示す。
（実施例４）
実施例１の微粒子ＭＢＸ−５をＭＳＸ−６に変更した以外は、実施例１と同様の方法で鋳型用フィルムを作成、それを用いて実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であり、得られた防眩性樹脂板の防眩層は、良好な耐擦傷性を有し、樹脂板との密着性も良好であった。結果を表１に示す。
（実施例５）
実施例１の微粒子ＭＢＸ−５をトスパール１２０に変更した以外は実施例１と同様の方法で鋳型用フィルムを作成、それを用いて実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であり、得られた防眩性樹脂板の防眩層は、良好な耐擦傷性を有し、樹脂板との密着性も良好であった。結果を表１に示す。
（実施例６）
実施例１の鋳型用フィルムの作製方法で、ロール状の鉄部材の外周面に厚さ３００μｍの銅めっきを施し、さらに銅の酸化防止のために銅めっき上にニッケルめっきを施したロ−ル状部材に中心粒径１５〜２０μｍ、上限粒径２１μｍのガラス微粒子を吐出させてブラスト処理を施し、外周面に微細凹凸構造を有するロール状金型を得た。
ビスコート＃１９２ ５０重量部
エポキシエステル３０００Ａ ５０重量部
ダロキュア１１７３ １．５重量部
上記原料の活性エネルギー線重合性組成物（Ｂ）を該ロール状金型と厚さ１００μｍのＰＥＴフィルム（コスモシャインＡ４１００）の易接着面との間に注入し、出力１２０Ｗ／ｃｍの高圧水銀灯を用いて、活性エネルギー線８００ｍＪ／ｃｍ２を前記フィルム側より照射することによって硬化させた後、前記フィルムを金型より剥離することで凹凸形状を有する防眩層（凹凸層）が形成された鋳型用フィルムを得た。次いで実施例１と同様の方法で鋳型用フィルムの凹凸面にコロナ処理を実施、それを用いて実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であり、得られた防眩性樹脂板の防眩層は、良好な耐擦傷性を有し、樹脂板との密着性も良好であった。結果を表１に示す。
（実施例７）
実施例１におけるアクリライトＬに塗工した活性エネルギー線重合性組成物（Ｂ）と鋳型用フィルムの圧接時の保持温度を２０℃にした以外は、実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であったが、アクリル板と硬化膜が密着しておらず、密着性試験を実施したところ防眩層が剥離してしまった。結果を表１に示す。
（実施例８）
実施例１におけるアクリライトＬに塗工したエネルギー線重合性組成物（Ｂ）と鋳型用フィルムの圧接時の保持温度を１００℃にした以外は、実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であったが、活性エネルギー線で硬化する際に樹脂板が熱で変形し、得られた硬化膜に対する耐擦傷性試験の結果も値が低下した。結果を表１に示す。
（実施例９）
実施例１におけるアクリライトＬに塗工したエネルギー線重合性組成物（Ｂ）と鋳型用フィルムの圧接時の保持時間を１５秒にした以外は、実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であったが、アクリル板と硬化膜が密着しておらず、密着性試験を実施したところ防眩層が剥離してしまった。結果を表１に示す。
（実施例１０）
実施例１におけるアクリライトＬに塗工したエネルギー線重合性組成物（Ｂ）と鋳型用フィルムの圧接時の保持時間を１０分にした以外は、実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であったが、得られた硬化膜に対する耐擦傷性試験の結果の値が低下した。結果を表１に示す。
（実施例１１）
実施例１の微粒子ＭＢＸ−５をＳＳＸ−１０５に変更した以外は、実施例１と同様の方法で鋳型用フィルムを作成した。鋳型用フィルムのコロナ処理前の押し込み弾性率は１８０３Ｎ／ｍｍ２であり、コロナ処理後の押し込み弾性率は１９３２Ｎ／ｍｍ２であった。それを用いて実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であり、得られた防眩性樹脂板の防眩層は、良好な耐擦傷性を有し、樹脂板との密着性も良好であった。結果を表２に示す。
（実施例１２）
実施例１の微粒子ＭＢＸ−５をＸＸ−１１０Ｂに変更した以外は、実施例１と同様の方法で鋳型用フィルムを作成した。鋳型用フィルムのコロナ処理前の押し込み弾性率は１７１１Ｎ／ｍｍ２であり、コロナ処理後の押し込み弾性率は１７７３Ｎ／ｍｍ２であった。それを用いて実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であり、得られた防眩性樹脂板の防眩層は、良好な耐擦傷性を有し、樹脂板との密着性も良好であった。結果を表２に示す。
（実施例１３）
実施例１の微粒子ＭＢＸ−５をトスパール１４５に変更した以外は、実施例１と同様の方法で鋳型用フィルムを作成した。鋳型用フィルムのコロナ処理前の押し込み弾性率は１５１８Ｎ／ｍｍ２であり、コロナ処理後の押し込み弾性率は１９４４Ｎ／ｍｍ２であった。それを用いて実施例１と同様の方法で防眩性樹脂板を得た。鋳型用フィルムの剥離性は良好であり、得られた防眩性樹脂板の防眩層は、良好な耐擦傷性を有し、樹脂板との密着性も良好であった。結果を表２に示す。
（比較例１）
実施例１におけるコロナ処理を省いた以外は実施例１と同様の方法で防眩性樹脂板を得ようとしたが、活性エネルギー線重合性組成物（Ｃ）の層を硬化させた後、鋳型用フィルムを、活性エネルギー線重合性組成物（Ｃ）を硬化した層から剥離することができなかった。結果を表１に示す。
（比較例２）
実施例４におけるコロナ処理を省いた以外は実施例４と同様の方法で防眩性樹脂板を得ようとしたが、活性エネルギー線重合性組成物（Ｃ）の層を硬化させた後、鋳型用フィルムを、活性エネルギー線重合性組成物（Ｃ）を硬化した層から剥離することができなかった。結果を表１に示す。
（比較例３）
実施例１１におけるコロナ処理を省いた以外は実施例１１と同様の方法で防眩性樹脂板を得ようとしたが、活性エネルギー線重合性組成物（Ｃ）の層を硬化させた後、鋳型用フィルムを、活性エネルギー線重合性組成物（Ｃ）を硬化した層から剥離することができなかった。結果を表２に示す。なお、鋳型用フィルムの押し込み弾性率は１８０３Ｎ／ｍｍ２であった。
An applied voltage of 11.6 kV is applied to a SUS electrode with a thickness of 1 mm and a length of 260 mm placed on the conveyor belt using a Navitas corona treatment device POLYDYNE, causing corona discharge, and conveying with the uneven surface as the upper surface. Corona treatment was carried out by passing the mold film placed on the belt through the lower part of the electrode at a gap between the mold film and the electrode of 3 mm and a conveying speed of 2.0 m / min. The irradiation energy for the mold film under such conditions was 100 W · min / m.
M400 25 parts by mass TAS 30 parts by mass M-305 35 parts by mass C6DA 10 parts by mass Lucillin TPO 2 parts by mass An active energy ray-polymerizable composition (C) composed of the above raw materials was previously heated to about 70 ° C. It was coated on the light L), and the mold film was covered with the concavo-convex surface as the inner surface, and pressed with a press roll to spread the active energy ray polymerizable composition (C) to a thickness of 12 μm. The surface temperature of the mold film placed on the resin plate is 60 ° C. when measured with a non-contact infrared thermometer. After holding at that temperature for 60 seconds, using a metal halide lamp with an output of 84 W / cm, The active energy ray polymerizable composition (C) was cured by irradiating ultraviolet rays of 800 mJ / cm 2 from the film side. After curing, the mold film was peeled off to obtain an antiglare resin plate. The mold film had good peelability, and the uneven layer (antiglare layer) of the resulting antiglare resin plate had good scratch resistance and good adhesion to the resin plate. The results are shown in Table 1.
(Example 2)
Corona discharge treatment for the mold film of Example 1 was performed by changing the applied voltage to 9.3 kV using a corona treatment apparatus POLYDYNE manufactured by Navitas, causing corona discharge, and placing the uneven surface on the upper surface of the casting belt. A casting film was prepared in the same manner as in Example 1 except that the casting film was subjected to corona treatment by passing the lower part of the electrode at a casting film-electrode gap of 3 mm and a conveying speed of 2.0 m / min. The irradiation energy for the corona-treated mold film under such conditions was 50 W · min / m. Using this, an antiglare resin plate was obtained in the same manner as in Example 1. The peelability of the mold film was good, and the antiglare layer of the obtained antiglare resin plate had good scratch resistance and good adhesion to the resin plate. The results are shown in Table 1.
(Example 3)
An upper electrode using a 20 mm x 20 mm x 200 mm SUS electrode surface sprayed with 1 mm thick aluminum oxide and a 200 x 200 x 20 mm SUS electrode. An atmospheric pressure plasma processing apparatus having a movable lower electrode using a sprayed aluminum oxide having a thickness of 1 mm on the surface was used. A casting film is placed on the lower electrode with the concavo-convex surface as the upper surface, a gas is introduced between the electrodes at a supply rate of processing gas: He / O 2 = 3.0 / 0.04 L / min, and an output of 100 kHz, 2 Except that the plasma was generated at 0.5 W / cm 2 and the lower electrode was moved so that the conveyance speed was 2.0 m / min, the processing time was 0.6 seconds, and the electrode interval was 2.0 mm. A film for a mold was produced in the same manner as in No. 1, and an antiglare resin plate was obtained in the same manner as in Example 1 using the same. The peelability of the mold film was good, and the antiglare layer of the obtained antiglare resin plate had good scratch resistance and good adhesion to the resin plate. The results are shown in Table 1.
Example 4
A mold film was prepared in the same manner as in Example 1 except that the microparticles MBX-5 in Example 1 was changed to MSX-6, and an antiglare resin plate was prepared in the same manner as in Example 1 using this film. Obtained. The peelability of the mold film was good, and the antiglare layer of the obtained antiglare resin plate had good scratch resistance and good adhesion to the resin plate. The results are shown in Table 1.
(Example 5)
A mold film was prepared in the same manner as in Example 1 except that the fine particle MBX-5 in Example 1 was changed to Tospearl 120, and an antiglare resin plate was obtained in the same manner as in Example 1 using this film. . The peelability of the mold film was good, and the antiglare layer of the obtained antiglare resin plate had good scratch resistance and good adhesion to the resin plate. The results are shown in Table 1.
(Example 6)
A roll in which the outer peripheral surface of a roll-shaped iron member was subjected to copper plating with a thickness of 300 μm and nickel plating was applied on the copper plating to prevent copper oxidation in the method for producing a mold film of Example 1. A glass fine particle having a center particle diameter of 15 to 20 μm and an upper limit particle diameter of 21 μm was discharged onto the shaped member and blasted to obtain a roll-shaped mold having a fine uneven structure on the outer peripheral surface.
Biscoat # 192 50 parts by weight Epoxy ester 3000A 50 parts by weight Darocur 1173 1.5 parts by weight The above active energy ray-polymerizable composition (B) as the raw material and a PET film having a thickness of 100 μm (Cosmo Shine A4100) After being cured by irradiating an active energy ray of 800 mJ / cm 2 from the film side using a high-pressure mercury lamp with an output of 120 W / cm, the film is peeled from the mold. By doing this, a film for a mold on which an antiglare layer (unevenness layer) having an uneven shape was formed was obtained. Next, a corona treatment was performed on the concavo-convex surface of the mold film in the same manner as in Example 1, and an antiglare resin plate was obtained in the same manner as in Example 1 using this. The peelability of the mold film was good, and the antiglare layer of the obtained antiglare resin plate had good scratch resistance and good adhesion to the resin plate. The results are shown in Table 1.
(Example 7)
Anti-glare properties in the same manner as in Example 1 except that the holding temperature at the time of pressure contact between the active energy ray-polymerizable composition (B) coated on the acrylite L in Example 1 and the mold film was 20 ° C. A resin plate was obtained. Although the peelability of the mold film was good, the acrylic plate and the cured film were not in close contact, and the antiglare layer was peeled off when the adhesion test was performed. The results are shown in Table 1.
(Example 8)
An anti-glare resin in the same manner as in Example 1 except that the holding temperature at the time of pressure contact between the energy ray polymerizable composition (B) coated on the acrylite L in Example 1 and the mold film is 100 ° C. I got a plate. Although the peelability of the mold film was good, the resin plate was deformed by heat when it was cured with active energy rays, and the value of the result of the scratch resistance test on the resulting cured film also decreased. The results are shown in Table 1.
Example 9
An anti-glare resin in the same manner as in Example 1 except that the holding time at the time of pressure contact between the energy ray polymerizable composition (B) coated on the acrylite L in Example 1 and the casting film is 15 seconds. I got a plate. Although the peelability of the mold film was good, the acrylic plate and the cured film were not in close contact, and the antiglare layer was peeled off when the adhesion test was performed. The results are shown in Table 1.
(Example 10)
An anti-glare resin in the same manner as in Example 1 except that the holding time during pressure welding of the energy ray polymerizable composition (B) coated on the acrylite L in Example 1 and the mold film was 10 minutes. I got a plate. Although the peelability of the mold film was good, the value of the result of the scratch resistance test for the obtained cured film was lowered. The results are shown in Table 1.
(Example 11)
A mold film was prepared in the same manner as in Example 1 except that the fine particle MBX-5 in Example 1 was changed to SSX-105. The indentation elastic modulus of the casting film before corona treatment was 1803 N / mm 2 , and the indentation elastic modulus after corona treatment was 1932 N / mm 2 . Using this, an antiglare resin plate was obtained in the same manner as in Example 1. The peelability of the mold film was good, and the antiglare layer of the obtained antiglare resin plate had good scratch resistance and good adhesion to the resin plate. The results are shown in Table 2.
(Example 12)
A casting film was prepared in the same manner as in Example 1 except that the fine particle MBX-5 in Example 1 was changed to XX-110B. The indentation elastic modulus of the casting film before corona treatment was 1711 N / mm 2 , and the indentation elastic modulus after corona treatment was 1773 N / mm 2 . Using this, an antiglare resin plate was obtained in the same manner as in Example 1. The peelability of the mold film was good, and the antiglare layer of the obtained antiglare resin plate had good scratch resistance and good adhesion to the resin plate. The results are shown in Table 2.
(Example 13)
A casting film was prepared in the same manner as in Example 1 except that the fine particle MBX-5 in Example 1 was changed to Tospearl 145. The indentation elastic modulus before corona treatment of the mold film was 1518 N / mm 2 , and the indentation elastic modulus after corona treatment was 1944 N / mm 2 . Using this, an antiglare resin plate was obtained in the same manner as in Example 1. The peelability of the mold film was good, and the antiglare layer of the obtained antiglare resin plate had good scratch resistance and good adhesion to the resin plate. The results are shown in Table 2.
(Comparative Example 1)
An attempt was made to obtain an antiglare resin plate in the same manner as in Example 1 except that the corona treatment in Example 1 was omitted, but after the layer of the active energy ray polymerizable composition (C) was cured, the mold was The film for use could not be peeled from the layer obtained by curing the active energy ray polymerizable composition (C). The results are shown in Table 1.
(Comparative Example 2)
An attempt was made to obtain an antiglare resin plate in the same manner as in Example 4 except that the corona treatment in Example 4 was omitted, but after the layer of the active energy ray polymerizable composition (C) was cured, the mold was The film for use could not be peeled from the layer obtained by curing the active energy ray polymerizable composition (C). The results are shown in Table 1.
(Comparative Example 3)
An attempt was made to obtain an antiglare resin plate by the same method as in Example 11 except that the corona treatment in Example 11 was omitted, but after the layer of the active energy ray polymerizable composition (C) was cured, the mold was The film for use could not be peeled from the layer obtained by curing the active energy ray polymerizable composition (C). The results are shown in Table 2. The indentation elastic modulus of the mold film was 1803 N / mm 2 .
なお、実施例１〜１３で得られた防眩性樹脂板の防眩性はいずれも良好であった。比較例１〜３では防眩性樹脂板が得られず、防眩性の評価はできなかった。結果を表１、２に示す。 In addition, all of the anti-glare properties of the anti-glare resin plates obtained in Examples 1 to 13 were good. In Comparative Examples 1 to 3, no antiglare resin plate was obtained, and the antiglare property could not be evaluated. The results are shown in Tables 1 and 2.
本発明によれば、凹凸形状を付与する鋳型用フィルムとして、広く適用できる。 According to this invention, it can apply widely as a film for casting_mold | template which provides uneven | corrugated shape.
Claims (12)
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| KR20150024394A (en) * | 2012-06-20 | 2015-03-06 | 미쯔비시 레이온 가부시끼가이샤 | Method for producing laminate, laminate, and article |
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| JP2005047283A (en) * | 1994-05-18 | 2005-02-24 | Dainippon Printing Co Ltd | Anti-glare film |
| JP2003090902A (en) * | 2001-09-19 | 2003-03-28 | Dainippon Printing Co Ltd | Anti-reflection shaped film and anti-reflection processing method using the same |
| JP2003340852A (en) * | 2002-05-24 | 2003-12-02 | Keiwa Inc | Mat coat film for forming mold and mat sheet using the same |
| JP2004207370A (en) * | 2002-12-24 | 2004-07-22 | Cmk Corp | Manufacturing method of printed wiring board |
| JP2007304366A (en) * | 2006-05-12 | 2007-11-22 | Konica Minolta Opto Inc | Polarizer |
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| KR20150024394A (en) * | 2012-06-20 | 2015-03-06 | 미쯔비시 레이온 가부시끼가이샤 | Method for producing laminate, laminate, and article |
| KR101716588B1 (en) | 2012-06-20 | 2017-03-14 | 미쯔비시 레이온 가부시끼가이샤 | Method for producing laminate, laminate, and article |
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