JP5357064B2 - Optical film - Google Patents

Optical film Download PDF

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JP5357064B2
JP5357064B2 JP2010000063A JP2010000063A JP5357064B2 JP 5357064 B2 JP5357064 B2 JP 5357064B2 JP 2010000063 A JP2010000063 A JP 2010000063A JP 2010000063 A JP2010000063 A JP 2010000063A JP 5357064 B2 JP5357064 B2 JP 5357064B2
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surfactant
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weight
film
polymer binder
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JP2011136539A (en
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弘晃 辻
久雄 奥村
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Teijin DuPont Films Japan Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an optical film in which foreign matters generated during coating for forming an easily adhesive layer are reduced. <P>SOLUTION: The optical film comprising a polyethylene terephthalate biaxially stretched film and the easily adhesive layer with thickness of 10 to 300 nm arranged in one face of the same is characterized in that the easily adhesive layer contains a polymer binder and a surfactant, the ratio of contents of the polymer binder and the surfactant in the easily adhesive layer is such that the surfactant is 0.5 to 10 pts.wt. relative to the 100 pts.wt. of the polymer binder, the content ratio of the surfactant in the easily adhesive layer is 0.5 to 6 wt.% based on the weight of the easily adhesive layer, the surfactant includes a hydrophobic group and a hydrophilic group, the hydrophobic group is a 13-15C straight-chain hydrocarbon, the hydrophilic group includes a copolymer of oxyethylene and oxypropylene, the ratio of the oxyethylene in the hydrophilic group is 30 to 50 mol%, and the weight-average molecular weight of the surfactant is 1,200 to 1,600. <P>COPYRIGHT: (C)2011,JPO&amp;INPIT

Description

本発明は、光学用フィルムに関する。詳しくは、表示装置のタッチパネル基材や保護フィルム等、光を透過する態様で用いる部材として使用される光学用フィルムに関する。   The present invention relates to an optical film. In detail, it is related with the film for optics used as a member used in the aspect which permeate | transmits light, such as the touchscreen base material of a display apparatus, and a protective film.

光学用フィルムとして二軸延伸ポリエステルフィルムが一般的に用いられており、フィルムを製膜した後、ハードコート層や粘着剤層といった加工層が設けられる。
このため、二軸延伸ポリエステルフィルムと加工層との密着性をよくするために、フィルム表面には易接着層が設けられる。易接着層はポリエステルのエマルジョンをコーティングすることにより塗設されるが、コーティングの際に、ロールによるせん断応力でエマルションが凝集し、しばしば異物が発生する。そうなると、凝集異物を含む易接着層の上にハードコート層や粘着剤層を設けても異物が残ってしまい、その光学フィルムを用いた表示装置の表示品質を低下させることになる。
A biaxially stretched polyester film is generally used as an optical film, and after the film is formed, processed layers such as a hard coat layer and an adhesive layer are provided.
For this reason, in order to improve the adhesiveness of a biaxially stretched polyester film and a process layer, an easily bonding layer is provided in the film surface. The easy-adhesion layer is applied by coating an emulsion of polyester. During coating, the emulsion aggregates due to the shear stress of the roll, and foreign matter is often generated. Then, even if a hard coat layer or a pressure-sensitive adhesive layer is provided on the easy-adhesion layer containing aggregated foreign substances, the foreign substances remain, and the display quality of the display device using the optical film is deteriorated.

特開2000−238221号公報JP 2000-238221 A 特開2002−155157号公報JP 2002-155157 A

本発明は、易接着層を設けるコーティングの際に発生する異物を低減した光学用フィルムを提供することを課題とする。   This invention makes it a subject to provide the film for optics which reduced the foreign material which generate | occur | produces in the coating which provides an easily bonding layer.

すなわち本発明は、ポリエチレンテレフタレート二軸延伸フィルムおよびその少なくとも片面に設けられた厚み10〜300nmの易接着層からなる光学用フィルムであって、易接着層は高分子バインダーおよび界面活性剤を含有し、易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー100重量部に対して界面活性剤0.5〜10重量部であり、易接着層における界面活性剤の含有率は易接着層の重量を基準に0.5〜6重量%であり、界面活性剤は疎水基と親水基とからなり、疎水基は炭素数13〜15の直鎖炭化水素であり、親水基はオキシエチレンとオキシプロピレンの共重合体からなり、オキシエチレンの親水基における割合が30〜50モル%であり、界面活性剤の重量平均分子量が1200〜1600であることを特徴とする光学用フィルムである。   That is, the present invention is an optical film comprising a polyethylene terephthalate biaxially stretched film and an easy-adhesion layer having a thickness of 10 to 300 nm provided on at least one surface thereof, and the easy-adhesion layer contains a polymer binder and a surfactant. The ratio of the content of the polymer binder and the surfactant in the easy adhesion layer is 0.5 to 10 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder, and the content of the surfactant in the easy adhesion layer The ratio is 0.5 to 6% by weight based on the weight of the easy-adhesion layer, the surfactant is composed of a hydrophobic group and a hydrophilic group, and the hydrophobic group is a linear hydrocarbon having 13 to 15 carbon atoms, and is hydrophilic. The group consists of a copolymer of oxyethylene and oxypropylene, the proportion of oxyethylene in the hydrophilic group is 30 to 50 mol%, and the weight average molecular weight of the surfactant is 1200 to An optical film, which is a 600.

本発明によれば、易接着層を設けるコーティングの際に発生する異物を低減した光学用フィルムを提供することができる。   ADVANTAGE OF THE INVENTION According to this invention, the film for optics which reduced the foreign material which generate | occur | produces in the case of the coating which provides an easily bonding layer can be provided.

以下、本発明を詳細に説明する。   Hereinafter, the present invention will be described in detail.

[ポリエチレンテレフタレート二軸延伸フィルム]
本発明におけるポリエチレンテレフタレート二軸延伸フィルムは、ポリエチレンテレフタレートからなる二軸延伸フィルムである。
本発明におけるポリエチレンテレフタレートは、エチレンテレフタレート単位を、全繰返し単位を基準に95%以上、好ましくは98%以上の繰り返し単位としてなるポリエステルである。これは、ホモポリマーであってもよく、共重合ポリマーであってもよい。共重合ポリマーである場合、共重合成分として、例えば、イソフタル酸、ナフタレンジカルボン酸、ジエチレングリコールを用いることができる。ポリエチレンテレフタレートとして最も好ましいものは、ポリエチレンテレフタレートホモポリマーである。
光学用フィルムとしての機械的特性を得るために二軸延伸フィルムの厚みは、好ましくは30〜250μm、さらに好ましくは70〜225μmである。
[Polyethylene terephthalate biaxially stretched film]
The polyethylene terephthalate biaxially stretched film in the present invention is a biaxially stretched film made of polyethylene terephthalate.
The polyethylene terephthalate in the present invention is a polyester having ethylene terephthalate units as 95% or more, preferably 98% or more repeating units based on all repeating units. This may be a homopolymer or a copolymer. In the case of a copolymer, for example, isophthalic acid, naphthalene dicarboxylic acid, or diethylene glycol can be used as the copolymer component. Most preferred as polyethylene terephthalate is a polyethylene terephthalate homopolymer.
In order to obtain mechanical properties as an optical film, the thickness of the biaxially stretched film is preferably 30 to 250 μm, more preferably 70 to 225 μm.

[易接着層]
本発明の光学用フィルムは、ポリエチレンテレフタレート二軸延伸フィルムの片面または両面に易接着層を備える。易接着層の厚みは10〜300nm、好ましくは50〜120nmである。塗布層の厚みがこの範囲にないと、本発明の光学用フィルムのうえにハードコート層を設けたときに密着性が不足したり、干渉斑が生じたりするので、光学用フィルムとして不適である。
[Easily adhesive layer]
The optical film of the present invention includes an easy-adhesion layer on one side or both sides of a polyethylene terephthalate biaxially stretched film. The thickness of the easy adhesion layer is 10 to 300 nm, preferably 50 to 120 nm. If the thickness of the coating layer is not within this range, adhesion is insufficient or interference spots occur when a hard coat layer is provided on the optical film of the present invention, which is not suitable as an optical film. .

[高分子バインダー]
易接着層の高分子バインダーは、易接着層の表面にハードコート層を設ける場合にハードコート層との良好な接着性を得る観点から、ポリエステル樹脂およびオキサゾリン基とポリアルキレンオキシド鎖とを有するアクリル樹脂の混合物であることが好ましい。この高分子バインダーは、水に可溶性または分散性のものが好ましいが、多少の有機溶剤を含有する水に可溶なものも好ましく用いることができる。高分子バインダーのポリエステル樹脂のガラス転移点は、好ましくは40〜100℃、さらに好ましくは60〜80℃である。この範囲であれば、優れた接着性、耐傷性、耐ブロッキング性および塗布外観を得ることができる。
[Polymer binder]
The polymer binder of the easy adhesion layer is an acrylic resin having a polyester resin and an oxazoline group and a polyalkylene oxide chain from the viewpoint of obtaining good adhesion to the hard coat layer when a hard coat layer is provided on the surface of the easy adhesion layer. A mixture of resins is preferred. This polymer binder is preferably soluble or dispersible in water, but water-soluble one containing some organic solvent can also be preferably used. The glass transition point of the polyester resin of the polymer binder is preferably 40 to 100 ° C, more preferably 60 to 80 ° C. If it is this range, the outstanding adhesiveness, scratch resistance, blocking resistance, and application | coating external appearance can be obtained.

この場合、高分子バインダーを構成するポリエステル樹脂の塗布層中での含有割合は、好ましくは5〜95重量%、さらに好ましくは50〜90重量%である。高分子バインダーを構成するオキサゾリン基とポリアルキレンオキシド鎖とを有するアクリル樹脂の、塗布層中での含有割合は、好ましくは5〜95重量%、さらに好ましくは10〜50重量%である。高分子バインダーがこの範囲の組成であることで、ハードコート層との良好な接着性を得るとともに、フィルムへの特に良好な密着性を得ることができる。   In this case, the content ratio of the polyester resin constituting the polymer binder in the coating layer is preferably 5 to 95% by weight, more preferably 50 to 90% by weight. The content ratio in the coating layer of the acrylic resin having an oxazoline group and a polyalkylene oxide chain constituting the polymer binder is preferably 5 to 95% by weight, more preferably 10 to 50% by weight. When the polymer binder has a composition within this range, good adhesion to the hard coat layer can be obtained, and particularly good adhesion to the film can be obtained.

[界面活性剤]
本発明における界面活性剤は親水基と疎水基からなり、疎水基は炭素数が13〜15の直鎖炭化水素であり、かつ親水基はオキシエチレンとオキシプロピレンの共重合体からなり、オキシエチレンの親水基における割合が30〜50モル%である界面活性剤である。
易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー100重量部に対して界面活性剤0.5〜10重量部、好ましくは1〜3重量部である。界面活性剤の量が0.5重量部未満であるとポリエステルバインダーの水分散性が悪化する。他方、10重量部を越えると余剰の界面活性剤自身が凝集を促進する作用を持つ。
易接着層における界面活性剤の含有率は易接着層の重量を基準に0.5〜6重量%である。0.5重量%未満であると、ポリエステルバインダーの水分散性が悪化する。他方、6重量%を超えるとロールコーターで塗布する時のロールとフィルムとのせん断応力によってポリエステルバインダーを凝集させてしまう。
[Surfactant]
The surfactant in the present invention is composed of a hydrophilic group and a hydrophobic group, the hydrophobic group is a linear hydrocarbon having 13 to 15 carbon atoms, and the hydrophilic group is composed of a copolymer of oxyethylene and oxypropylene. Is a surfactant having a ratio of 30 to 50 mol% in the hydrophilic group.
The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer is 0.5 to 10 parts by weight, preferably 1 to 3 parts by weight, based on 100 parts by weight of the polymer binder. When the amount of the surfactant is less than 0.5 parts by weight, the water dispersibility of the polyester binder is deteriorated. On the other hand, when it exceeds 10 parts by weight, the surplus surfactant itself has an action of promoting aggregation.
The content of the surfactant in the easy adhesion layer is 0.5 to 6% by weight based on the weight of the easy adhesion layer. If it is less than 0.5% by weight, the water dispersibility of the polyester binder deteriorates. On the other hand, if it exceeds 6% by weight, the polyester binder will be agglomerated by the shear stress between the roll and the film when applied by a roll coater.

界面活性剤は疎水基と親水基とからなる。疎水基は炭素数13〜15の直鎖炭化水素である。疎水基の炭素数が13未満であると易接着層をコーティングするときに高分子バインダーが凝集する、15を超えると表面張力が下がりコーティングの斑になる。親水基はオキシエチレンとオキシプロピレンの共重合体からなる。オキシエチレンの親水基における割合が30〜50モル%である。30モル%未満であると水分散がうまくいかない、50モル%を超えるとコーティングするときに高分子バインダーが凝集する。
界面活性剤の分子量は1200〜1600である。界面活性剤の分子量がこの範囲から外れると、ポリエステルバインダーの水分散性が悪化する。また、ロールコーターで塗布する時のロールとフィルムとのせん断応力によってポリエステルバインダーを凝集させてしまう。
The surfactant consists of a hydrophobic group and a hydrophilic group. The hydrophobic group is a straight chain hydrocarbon having 13 to 15 carbon atoms. When the number of carbon atoms of the hydrophobic group is less than 13, the polymer binder aggregates when coating the easy-adhesion layer. When the number of the hydrophobic group exceeds 15, the surface tension decreases and the coating becomes uneven. The hydrophilic group consists of a copolymer of oxyethylene and oxypropylene. The ratio in the hydrophilic group of oxyethylene is 30-50 mol%. If it is less than 30 mol%, water dispersion will not be successful, and if it exceeds 50 mol%, the polymer binder will aggregate when coating.
The molecular weight of the surfactant is 1200-1600. When the molecular weight of the surfactant is out of this range, the water dispersibility of the polyester binder deteriorates. In addition, the polyester binder is agglomerated by the shear stress between the roll and the film when applied by a roll coater.

[帯電防止剤]
易接着層は、加工時の剥離帯電による異物の付着を防止するために、帯電防止剤を含有していることが好ましい。易接着層が耐電防止剤を含有する場合、易接着層の重量を基準として、好ましくは2〜5重量%である。この範囲で含有することにより、接着性および密着性を損なうことなく、異物の付着を防止する帯電防止性を付与することができる。
[Antistatic agent]
The easy-adhesion layer preferably contains an antistatic agent in order to prevent adhesion of foreign matters due to peeling charging during processing. When an easily bonding layer contains an antistatic agent, it is preferably 2 to 5% by weight based on the weight of the easily bonding layer. By containing in this range, the antistatic property which prevents adhesion of a foreign material can be provided, without impairing adhesiveness and adhesiveness.

[異物]
本発明の光学用フィルムにおいては、易接着層における、凸部の大きさの最大径が20μm以上かつ凸部の高さが1μm以上の異物が3個以下/100mであることが好ましい。異物が3個/100mを超えると、光学用基材を製造する際の歩留まりが低下して好ましくない。
[Foreign matter]
In the optical film of the present invention, it is preferable that in the easy-adhesive layer, there are 3 or less / 100 m 2 of foreign matter having a maximum diameter of the protrusions of 20 μm or more and a height of the protrusions of 1 μm or more. If the number of foreign matters exceeds 3/100 m 2 , the yield in producing an optical substrate is lowered, which is not preferable.

[製造方法]
本発明に用いる界面活性剤は、テトラデカノールもしくはペンタデカノールに触媒として水酸化ナトリウムを加え、攪拌しながら150〜180℃まで加熱し、これにエチレンオキサイドとプロピレンオキサイドを加えることで製造することができる。
本発明の光学用フィルムを製造するためには、コーティング速度を遅くすることができる同時二軸延伸法にて延伸することが肝要である。以下、ポリエステルの融点をTm、ガラス転移温度をTgと略記する。
[Production method]
The surfactant used in the present invention is manufactured by adding sodium hydroxide as a catalyst to tetradecanol or pentadecanol, heating to 150 to 180 ° C. with stirring, and adding ethylene oxide and propylene oxide thereto. Can do.
In order to produce the optical film of the present invention, it is important to stretch the film by a simultaneous biaxial stretching method that can reduce the coating speed. Hereinafter, the melting point of polyester is abbreviated as Tm, and the glass transition temperature is abbreviated as Tg.

本発明の光学用フィルムは、まず、ポリエステルを溶融し、シート状に押出し、冷却ドラムで冷却して未延伸フィルムとし、未延伸フィルムの少なくとも片面に易接着層の塗液を塗布したあと、二軸方向に同時に延伸し、熱固定し、熱弛緩処理することによって得ることができる。具体的には、ポリエステルを、(Tm+10℃)〜(Tm+30℃)の温度で溶融し、押出して未延伸フィルムとし、未延伸フィルムの少なくとも片面に易接着層をロールコーターで積層したあと、同時に二軸方向に、Tg〜(Tg+10℃)の温度で縦方向に3.0〜3.4倍、横方向に3.4〜4.0倍の倍率で延伸する。得られた延伸フィルムを、(Tg+60)〜Tmの温度で熱固定する。例えばポリエステルが、ポリエチレンテレフタレートホモポリマーである場合、230〜240℃の温度で、1〜60秒の時間熱固定処理するのが好ましい。   The optical film of the present invention is obtained by first melting a polyester, extruding it into a sheet, cooling it with a cooling drum to form an unstretched film, applying an easy-adhesion layer coating liquid on at least one side of the unstretched film, It can be obtained by simultaneously stretching in the axial direction, heat setting, and heat relaxation treatment. Specifically, the polyester is melted at a temperature of (Tm + 10 ° C.) to (Tm + 30 ° C.), extruded to be an unstretched film, and an easy-adhesion layer is laminated on at least one side of the unstretched film with a roll coater. In the axial direction, the film is stretched at a temperature of Tg to (Tg + 10 ° C.) at a magnification of 3.0 to 3.4 times in the longitudinal direction and 3.4 to 4.0 times in the transverse direction. The obtained stretched film is heat-set at a temperature of (Tg + 60) to Tm. For example, when polyester is a polyethylene terephthalate homopolymer, it is preferable to heat-set at a temperature of 230 to 240 ° C. for 1 to 60 seconds.

易接着層の塗布は、以下の方法で行うことができる。走行するフィルムの速度は10m/minとし、80線のグラビアロールを20m/minの回転速度で塗液を汲み上げ、ドクターブレードによってグラビアロール上の塗液を一定量となるように掻き落とし、フィルムに塗布する。もしくは、80線のグラビアロールを15m/minの回転速度で塗液を汲み上げ、ドクターブレードによってグラビアロール上の塗液を一定量となるように掻き落とし、25m/minで回転するゴムロールに転写させ、フィルムに塗布する。   Application | coating of an easily bonding layer can be performed with the following method. The speed of the traveling film is 10 m / min, the 80-line gravure roll is pumped up at a rotational speed of 20 m / min, and the coating liquid on the gravure roll is scraped off to a certain amount by a doctor blade. Apply. Alternatively, an 80-line gravure roll is pumped up at a rotation speed of 15 m / min, the doctor liquid is scraped off to a constant amount by a doctor blade, and transferred to a rubber roll rotating at 25 m / min, Apply to film.

以下、実施例により本発明を具体的に説明する。
フィルムの評価および実施例で用いた界面活性剤の合成は、以下の方法で行った。
Hereinafter, the present invention will be described specifically by way of examples.
Evaluation of the film and synthesis of the surfactant used in the examples were performed by the following methods.

(1)異物の個数
以下に説明する光学欠点検出装置により、巾1m、長さ100mのフィルムロールについて、光学的に最大径が20μm以上の大きさと認識される光学欠点を異物として検出した。巻取り機の繰出し側と巻取り側の間に、パナソニック社製三波長形蛍光灯ラピッドスタータ形40Wの蛍光灯を巾10mmのスリットでマスキングした光源をフィルムの上方5cmの位置に設置し、フィルムロールをシワが入らないように、この巻取り機で巻き返し、この際に、繰出したフィルムへ光源と受光器とを結ぶ直線と測定対象のフィルム面の垂直方向とのなす角度が12度になるようにフィルムに光線を入射し、フィルムに光線があたる位置に光学欠点が存在すると受光器のCCDイメージセンサカメラで電気信号に変換し、光学欠点のある位置と無い位置での電機信号のシグナル強度変化により異物を認識し、異物のフィルム上での長手方向および横手方向の位置情報を記録した。この方法による異物の検出を、フィルムの繰出し速度5m毎分でフィルムの長手方向100mについて実施して、フィルムの100mあたりに存在する異物の個数と位置情報を検出した。
異物の高さ測定は、位置情報を基に異物を含む領域を適切な大きさにサンプリングし、オリンパス社製レーザー顕微鏡LEXT OLS4000で異物の高さを測定した。
最終的に、凸部の大きさの最大径が20μm以上かつ凸部の高さが1μm以上の異物の数を算出した。
(1) Number of Foreign Objects Optical defects that are optically recognized as having a maximum diameter of 20 μm or more were detected as foreign objects on a film roll having a width of 1 m and a length of 100 m using an optical defect detection apparatus described below. Between the unwinding side and the winding side of the winder, a light source obtained by masking a three-wavelength fluorescent lamp rapid starter type 40W made by Panasonic with a slit with a width of 10 mm is placed at a position 5 cm above the film. The roll is rewound by this winder so as not to be wrinkled. At this time, the angle formed by the straight line connecting the light source and the light receiver to the fed film and the vertical direction of the film surface to be measured is 12 degrees. When a light beam is incident on the film and there is an optical defect at the position where the light beam hits the film, it is converted into an electrical signal by the CCD image sensor camera of the receiver, and the signal strength of the electrical signal at the position where there is no optical defect The foreign matter was recognized by the change, and the positional information of the foreign matter on the film in the longitudinal direction and the lateral direction was recorded. The detection of foreign matters by this method was carried out in the longitudinal direction of the film at 100 m at a film feeding speed of 5 m per minute, and the number and position information of foreign matters existing per 100 m 2 of the film were detected.
The height of the foreign material was measured by sampling an area including the foreign material to an appropriate size based on the position information, and measuring the height of the foreign material using a laser microscope LEXT OLS4000 manufactured by Olympus.
Finally, the number of foreign matters having a maximum diameter of the convex portion of 20 μm or more and a height of the convex portion of 1 μm or more was calculated.

(2)界面活性剤の重量平均分子量
界面活性剤の重量平均分子量は、大塚電子社製DLS−8000で測定して求めた。
(2) Weight average molecular weight of surfactant The weight average molecular weight of the surfactant was determined by measuring with DLS-8000 manufactured by Otsuka Electronics Co., Ltd.

(3)界面活性剤の疎水基の炭素数
疎水基の炭素数は、BRUKER社製核磁気共鳴装置AVANCEでH−NMRの測定チャートから読み取った。
(3) Carbon number of hydrophobic group of surfactant The carbon number of the hydrophobic group was read from a measurement chart of 1 H-NMR with a nuclear magnetic resonance apparatus AVANCE manufactured by BRUKER.

(4)易接着層の厚み
易接着層の膜厚は、フィルムサンプルの断面を日立社製電界放出形透過電子顕微鏡 HF−3300で観察し、実際の膜厚を測定した。
(4) Thickness of easy-adhesion layer The film thickness of the easy-adhesion layer was measured by observing the cross section of the film sample with a field emission transmission electron microscope HF-3300 manufactured by Hitachi, Ltd.

(5)界面活性剤の合成
界面活性剤A〜Fを特許3187846号公報(特願平10−521226号)に記載の方法に準拠して、以下の方法にて作成した。「部」は重量部を意味する。
(5) Synthesis of Surfactant Surfactants A to F were prepared by the following method based on the method described in Japanese Patent No. 318784 (Japanese Patent Application No. 10-521226). “Parts” means parts by weight.

界面活性剤A
エチレンオキサイド用とプロピレンオキサイド用の2つ計量槽の付いた5リットルの回転攪拌式オートクレーブ中に、テトラデカノールを143部、水酸化カリウムを3.0部仕込み、窒素置換を行った後110℃に昇温して、40TORRで1時間脱水を行った。次に150℃に昇温し、エチレンオキサイドを3.5kg/cmの圧力で288部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、120℃に冷却してプロピレンオキサイド569部をオートクレーブ中に3.5kg/cmの圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約1000部の目的の界面活性剤Aを得た。
Surfactant A
143 parts of tetradecanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, and after nitrogen substitution, the temperature was changed to 110 ° C. The temperature was raised to 40 torr and dehydration was performed for 1 hour. Next, the temperature is raised to 150 ° C., 288 parts of ethylene oxide is introduced into the autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreases and becomes constant, and then cooled to 120 ° C. to propylene. 569 parts of oxide was introduced into the autoclave at a pressure of 3.5 kg / cm 2 , and the reaction was continued until the pressure decreased and became constant as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted by lowering the temperature to obtain about 1000 parts of the desired surfactant A.

界面活性剤B
エチレンオキサイド用とプロピレンオキサイド用の2つ計量槽の付いた5リットルの回転攪拌式オートクレーブ中に、トリデカノールを154部、水酸化カリウムを3.0部仕込み、窒素置換を行った後110℃に昇温して、40TORRで1時間脱水を行った。次に150℃に昇温し、エチレンオキサイドを3.5kg/cmの圧力で208部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、120℃に冷却してプロピレンオキサイド639部をオートクレーブ中に3.5kg/cmの圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約1000部の目的の界面活性剤Bを得た。
Surfactant B
154 parts of tridecanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide. Warmed and dehydrated at 40 TORR for 1 hour. Next, the temperature was raised to 150 ° C., 208 parts of autoclave was introduced into the autoclave at a pressure of 3.5 kg / cm 2 , and the reaction was continued until the pressure decreased and became constant. 639 parts of oxide was introduced into the autoclave at a pressure of 3.5 kg / cm 2 and reacted until the pressure decreased and became constant in the same manner as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted at a reduced temperature to obtain about 1000 parts of the desired surfactant B.

界面活性剤C
エチレンオキサイド用とプロピレンオキサイド用の2つ計量槽の付いた5リットルの回転攪拌式オートクレーブ中に、テトラデカノールを306部、水酸化カリウムを3.0部仕込み、窒素置換を行った後110℃に昇温して、40TORRで1時間脱水を行った。次に150℃に昇温し、エチレンオキサイドを3.5kg/cmの圧力で233部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、120℃に冷却してプロピレンオキサイド461部をオートクレーブ中に3.5kg/cmの圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約1000部の目的の界面活性剤Cを得た。
Surfactant C
Into a 5 liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, 306 parts of tetradecanol and 3.0 parts of potassium hydroxide were charged, and after nitrogen substitution, 110 ° C. The temperature was raised to 40 torr and dehydration was performed for 1 hour. Next, the temperature was raised to 150 ° C., ethylene oxide was introduced into the 233 parts autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreased and became constant, and then cooled to 120 ° C. to propylene. 461 parts of oxide were introduced into the autoclave at a pressure of 3.5 kg / cm 2 and reacted until the pressure decreased and became constant in the same manner as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted at a reduced temperature, and about 1000 parts of the desired surfactant C was obtained.

界面活性剤D
エチレンオキサイド用とプロピレンオキサイド用の2つ計量槽の付いた5リットルの回転攪拌式オートクレーブ中に、ヘプタノールを77部、水酸化カリウムを3.0部仕込み、窒素置換を行った後110℃に昇温して、40TORRで1時間脱水を行った。次に150℃に昇温し、エチレンオキサイドを3.5kg/cmの圧力で310部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、120℃に冷却してプロピレンオキサイド613部をオートクレーブ中に3.5kg/cmの圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約1000部の目的の界面活性剤Dを得た。
Surfactant D
77 parts of heptanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, and the temperature was raised to 110 ° C. after nitrogen substitution. Warmed and dehydrated at 40 TORR for 1 hour. Next, the temperature was raised to 150 ° C., ethylene oxide was introduced into 310 parts autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreased and became constant, and then cooled to 120 ° C. to propylene. 613 parts of oxide was introduced into the autoclave at a pressure of 3.5 kg / cm 2 and reacted until the pressure decreased and became constant in the same manner as in the case of ethylene oxide. After completion of the reaction, a sample synthesized at a reduced temperature was extracted to obtain about 1000 parts of the desired surfactant D.

界面活性剤E
エチレンオキサイド用とプロピレンオキサイド用の2つ計量槽の付いた5リットルの回転攪拌式オートクレーブ中に、テトラデカノールを143部、水酸化カリウムを3.0部仕込み、窒素置換を行った後110℃に昇温して、40TORRで1時間脱水を行った。次に150℃に昇温し、エチレンオキサイドを3.5kg/cmの圧力で67部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、120℃に冷却してプロピレンオキサイド791部をオートクレーブ中に3.5kg/cmの圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約1000部の目的の界面活性剤Eを得た。
Surfactant E
143 parts of tetradecanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, and after nitrogen substitution, the temperature was changed to 110 ° C. The temperature was raised to 40 torr and dehydration was performed for 1 hour. Next, the temperature is raised to 150 ° C., ethylene oxide is introduced into 67 parts of an autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreases and becomes constant, and then cooled to 120 ° C. to propylene. 791 parts of oxide were introduced into the autoclave at a pressure of 3.5 kg / cm 2 and reacted until the pressure decreased and became constant in the same manner as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted by lowering the temperature, and about 1000 parts of the desired surfactant E was obtained.

界面活性剤F
エチレンオキサイド用とプロピレンオキサイド用の2つ計量槽の付いた5リットルの回転攪拌式オートクレーブ中に、テトラデカノールを143部、水酸化カリウムを3.0部仕込み、窒素置換を行った後110℃に昇温して、40TORRで1時間脱水を行った。次に150℃に昇温し、エチレンオキサイドを3.5kg/cmの圧力で645部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、120℃に冷却してプロピレンオキサイド213部をオートクレーブ中に3.5kg/cmの圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約1000部の目的の界面活性剤Fを得た。
得られた界面活性剤AからFの詳細を表1に示す。
Surfactant F
143 parts of tetradecanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, and after nitrogen substitution, the temperature was changed to 110 ° C. The temperature was raised to 40 torr and dehydration was performed for 1 hour. Next, the temperature was raised to 150 ° C., ethylene oxide was introduced into the 645 parts autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreased and became constant, and then cooled to 120 ° C. to propylene. 213 parts of oxide was introduced into the autoclave at a pressure of 3.5 kg / cm 2 , and the reaction was continued until the pressure decreased and became constant as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted by lowering the temperature, and about 1000 parts of the desired surfactant F was obtained.
Details of the obtained surfactants A to F are shown in Table 1.

Figure 0005357064
Figure 0005357064

[実施例1]
溶融ポリエチレンテレフタレート([η]=0.63dl/g、Tg=78℃)をダイより押出し、常法により冷却ドラムで冷却して未延伸フィルムとし、次いでその両面に表1に示す塗剤組成1の濃度10重量%の水性塗液をロールコーターで均一に塗布して塗布フィルムを得た。この水性塗液における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー100重量部に対して界面活性剤5重量部であり、塗布フィルムを、引き続いて95℃で乾燥し、120℃で縦方向に3.3倍、横方向に3.7倍の延伸倍率で縦横方向を同時に延伸し、240℃で熱固定し、厚さ100μmの光学用フィルムを得た。この光学用フィルムの易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー100重量部に対して界面活性剤4重量部であり、易接着層における界面活性剤の含有率は易接着層の重量を基準に4重量%である。評価結果を表2に示す。
[Example 1]
Molten polyethylene terephthalate ([η] = 0.63 dl / g, Tg = 78 ° C.) is extruded from a die, cooled with a cooling drum by a conventional method to form an unstretched film, and then a coating composition 1 shown in Table 1 on both sides thereof An aqueous coating solution having a concentration of 10% by weight was uniformly applied by a roll coater to obtain a coated film. The ratio of the content of the polymer binder and the surfactant in this aqueous coating liquid is 5 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder, and the coated film is subsequently dried at 95 ° C. The film was stretched at the same time in the longitudinal and transverse directions at a stretching ratio of 3.3 times in the longitudinal direction and 3.7 times in the transverse direction, and heat-set at 240 ° C. to obtain an optical film having a thickness of 100 μm. The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer of the optical film is 4 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder. The rate is 4% by weight based on the weight of the easily adhesive layer. The evaluation results are shown in Table 2.

[実施例2]
水性塗液を表2に示す塗剤組成2の濃度10重量%の水性塗液に変更すること以外は実施例1と同様にして厚さ100μmの光学用フィルムを得た。この光学用フィルムの易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー100重量部に対して界面活性剤4重量部であり、易接着層における界面活性剤の含有率は易接着層の重量を基準に4重量%である。評価結果を表2に示す。
[Example 2]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 2 shown in Table 2. The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer of the optical film is 4 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder. The rate is 4% by weight based on the weight of the easily adhesive layer. The evaluation results are shown in Table 2.

[比較例1]
水性塗液を表2に示す塗剤組成3の濃度10重量%の水性塗液に変更すること以外は実施例1と同様にして厚さ100μmの光学用フィルムを得た。この光学用フィルムの易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー100重量部に対して界面活性剤0.4重量部である。評価結果を表2に示す。
[Comparative Example 1]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 3 shown in Table 2. The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer of this optical film is 0.4 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder. The evaluation results are shown in Table 2.

[比較例2]
水性塗液を表2に示す塗剤組成4の濃度10重量%の水性塗液に変更すること以外は実施例1と同様にして厚さ100μmの光学用フィルムを得た。この光学用フィルムの易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー100重量部に対して界面活性剤20重量部である。評価結果を表2に示す。
[Comparative Example 2]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 4 shown in Table 2. The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer of the optical film is 20 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder. The evaluation results are shown in Table 2.

[比較例3]
水性塗液を表2に示す塗剤組成5の濃度10重量%の水性塗液に変更すること以外は実施例1と同様にして厚さ100μmの光学用フィルムを得た。評価結果を表2に示す。
[Comparative Example 3]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 5 shown in Table 2. The evaluation results are shown in Table 2.

[比較例4]
水性塗液を表2に示す塗剤組成6の濃度10重量%の水性塗液に変更すること以外は実施例1と同様にして厚さ100μmの光学用フィルムを得た。評価結果を表2に示す。
[Comparative Example 4]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 6 shown in Table 2. The evaluation results are shown in Table 2.

[比較例5]
水性塗液を表2に示す塗剤組成7の濃度10重量%の水性塗液に変更すること以外は実施例1と同様にして厚さ100μmの光学用フィルムを得た。評価結果を表2に示す。
[Comparative Example 5]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 7 shown in Table 2. The evaluation results are shown in Table 2.

[比較例6]
水性塗液を表2に示す塗剤組成8の濃度10重量%の水性塗液に変更すること以外は実施例1と同様にして厚さ100μmの光学用フィルムを得た。評価結果を表2に示す。
[Comparative Example 6]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 8 shown in Table 2. The evaluation results are shown in Table 2.

Figure 0005357064
Figure 0005357064

なお、表2の塗液組成の成分は次のとおりである。「部」は重量部を意味する。   In addition, the component of the coating liquid composition of Table 2 is as follows. “Parts” means parts by weight.

水分散性ポリエステル組成物1
水分散性ポリエステル組成物1は、水分散性ポリエステル1と界面活性剤Aとの混合物である。
水分散性ポリエステル1は、ジカルボン酸成分が2,6−ナフタレンジカルボン酸75モル%/イソフタル酸20モル%/5−ナトリウムスルホイソフタル酸5モル%、グリコール成分がエチレングリコール90モル%/ジエチレングリコール10モル%で構成されている(Tg=80℃、平均分子量15000)。なお、この水分散性ポリエステル1は、下記の方法で製造した。すなわち、2,6−ナフタレンジカルボン酸ジメチル51部、イソフタル酸ジメチル11部、5−ナトリウムスルホイソフタル酸ジメチル4部、エチレングリコール31部、ジエチレングリコール2部を反応器に仕込み、これにテトラブトキシチタン0.05部を添加して窒素雰囲気下で温度を230℃にコントロールして加熱し、生成するメタノールを留去させてエステル交換反応を行った。次いで攪拌器のモータートルクの高い重合釜で反応系の温度を徐々に255℃まで上昇させ系内を1mmHgの減圧にして重縮合反応を行い、固有粘度が0.56の水分散性ポリエステル1を得た。この水分散性ポリエステル1の25部をテトラヒドロフラン75部に溶解させ、得られた溶液に界面活性剤Aを1部添加し、10000回転/分の高速攪拌下で水75部を滴下して乳白色の分散体を得、次いでこの分散体を20mmHgの減圧下で蒸留し、テトラヒドロフランを留去した。
Water dispersible polyester composition 1
The water dispersible polyester composition 1 is a mixture of the water dispersible polyester 1 and the surfactant A.
The water dispersible polyester 1 has a dicarboxylic acid component of 75 mol% of 2,6-naphthalenedicarboxylic acid / 20 mol% of isophthalic acid / 5 mol% of 5-sodium sulfoisophthalic acid, and a glycol component of 90 mol% of ethylene glycol / 10 mol of diethylene glycol. % (Tg = 80 ° C., average molecular weight 15000). The water dispersible polyester 1 was produced by the following method. That is, 51 parts of dimethyl 2,6-naphthalenedicarboxylate, 11 parts of dimethyl isophthalate, 4 parts of dimethyl 5-sodium sulfoisophthalate, 31 parts of ethylene glycol and 2 parts of diethylene glycol were charged into a reactor. 05 parts were added, the temperature was controlled at 230 ° C. in a nitrogen atmosphere, and the resulting methanol was distilled off to conduct a transesterification reaction. Next, the temperature of the reaction system is gradually raised to 255 ° C. in a polymerization kettle with high motor torque of a stirrer, and the inside of the system is reduced to 1 mmHg to carry out a polycondensation reaction, and water dispersible polyester 1 having an intrinsic viscosity of 0.56 is obtained. Obtained. 25 parts of this water-dispersible polyester 1 was dissolved in 75 parts of tetrahydrofuran, 1 part of surfactant A was added to the resulting solution, and 75 parts of water was added dropwise under high-speed stirring at 10,000 rpm to give a milky white color. A dispersion was obtained, and then the dispersion was distilled under a reduced pressure of 20 mmHg to distill off the tetrahydrofuran.

水分散性ポリエステル組成物2
水分散性ポリエステル組成物2は、水分散性ポリエステル2と界面活性剤Bとの混合物である。
水分散性ポリエステル2は、ジカルボン酸成分がテレフタルジカルボン酸97モル%/イソフタル酸1モル%/5−ナトリウムスルホイソフタル酸2モル%、グリコール成分がエチレングリコール90モル%/ジエチレングリコール10モル%で構成されている(Tg=80℃、平均分子量15000)。なお、この水分散性ポリエステル2は、下記の方法で製造した。すなわち、テレフタル酸ジメチル62部、イソフタル酸ジメチル1部、5−ナトリウムスルホイソフタル酸ジメチル4部、エチレングリコール31部、ジエチレングリコール2部を反応器に仕込み、これにテトラブトキシチタン0.05部を添加して窒素雰囲気下で温度を230℃にコントロールして加熱し、生成するメタノールを留去させてエステル交換反応を行った。次いで攪拌器のモータートルクの高い重合釜で反応系の温度を徐々に255℃まで上昇させ系内を1mmHgの減圧にして重縮合反応を行い、固有粘度が0.56の水分散性ポリエステル2を得た。この水分散性ポリエステル2の25部をテトラヒドロフラン75部に溶解させ、得られた溶液に界面活性剤Bを1部添加し、10000回転/分の高速攪拌下で水75部を滴下して乳白色の分散体を得、次いでこの分散体を20mmHgの減圧下で蒸留し、テトラヒドロフランを留去した。
Water dispersible polyester composition 2
The water dispersible polyester composition 2 is a mixture of the water dispersible polyester 2 and the surfactant B.
In the water dispersible polyester 2, the dicarboxylic acid component is composed of 97 mol% terephthaldicarboxylic acid / 1 mol% isophthalic acid / 5 mol% 5-sodium sulfoisophthalic acid, and the glycol component is composed of 90 mol% ethylene glycol / 10 mol% diethylene glycol. (Tg = 80 ° C., average molecular weight 15000). This water-dispersible polyester 2 was produced by the following method. That is, 62 parts of dimethyl terephthalate, 1 part of dimethyl isophthalate, 4 parts of dimethyl 5-sodium sulfoisophthalate, 31 parts of ethylene glycol and 2 parts of diethylene glycol were charged into the reactor, and 0.05 part of tetrabutoxy titanium was added thereto. Then, the temperature was controlled at 230 ° C. in a nitrogen atmosphere, and the produced methanol was distilled off to conduct a transesterification reaction. Next, the temperature of the reaction system is gradually raised to 255 ° C. in a polymerization kettle with high motor torque of the stirrer, and the inside of the system is depressurized to 1 mmHg to carry out a polycondensation reaction. Obtained. 25 parts of this water-dispersible polyester 2 was dissolved in 75 parts of tetrahydrofuran, 1 part of surfactant B was added to the resulting solution, and 75 parts of water was added dropwise under high-speed stirring at 10,000 rpm to give a milky white color. A dispersion was obtained, and then the dispersion was distilled under a reduced pressure of 20 mmHg to distill off the tetrahydrofuran.

水分散性ポリエステル組成物3
水分散性ポリエステル組成物3は、水分散性ポリエステル1と界面活性剤Aとの混合物である。界面活性剤Aの添加量を0.1部に変更する以外は水分散性ポリエステル組成物1と同様にして、水分散性ポリエステル組成物3を得た。
Water dispersible polyester composition 3
The water dispersible polyester composition 3 is a mixture of the water dispersible polyester 1 and the surfactant A. A water-dispersible polyester composition 3 was obtained in the same manner as the water-dispersible polyester composition 1 except that the addition amount of the surfactant A was changed to 0.1 part.

水分散性ポリエステル組成物4
水分散性ポリエステル組成物4は、水分散性ポリエステル1と界面活性剤Aとの混合物である。界面活性剤Aの添加量を5部に変更する以外は水分散性ポリエステル組成物1と同様にして、水分散性ポリエステル組成物4を得た。
Water dispersible polyester composition 4
The water dispersible polyester composition 4 is a mixture of the water dispersible polyester 1 and the surfactant A. A water-dispersible polyester composition 4 was obtained in the same manner as the water-dispersible polyester composition 1 except that the addition amount of the surfactant A was changed to 5 parts.

水分散性ポリエステル組成物5
水分散性ポリエステル組成物5は、水分散性ポリエステル1と界面活性剤Cとの混合物である。界面活性剤Aの代わりに界面活性剤Cを用いた以外は水分散性ポリエステル組成物1と同様にして、水分散性ポリエステル組成物5を得た。
Water dispersible polyester composition 5
The water dispersible polyester composition 5 is a mixture of the water dispersible polyester 1 and the surfactant C. A water-dispersible polyester composition 5 was obtained in the same manner as the water-dispersible polyester composition 1 except that the surfactant C was used instead of the surfactant A.

水分散性ポリエステル組成物6
水分散性ポリエステル組成物5は、水分散性ポリエステル1と界面活性剤Dとの混合物である。界面活性剤Aの代わりに界面活性剤Dを用いた以外は水分散性ポリエステル組成物1と同様にして、水分散性ポリエステル組成物6を得た。
Water dispersible polyester composition 6
The water dispersible polyester composition 5 is a mixture of the water dispersible polyester 1 and the surfactant D. A water-dispersible polyester composition 6 was obtained in the same manner as the water-dispersible polyester composition 1 except that the surfactant D was used instead of the surfactant A.

水分散性ポリエステル組成物7
水分散性ポリエステル組成物5は、水分散性ポリエステル1と界面活性剤Eとの混合物である。界面活性剤Aの代わりに界面活性剤Eを用いた以外は水分散性ポリエステル組成物1と同様にして、水分散性ポリエステル組成物7を得た。
Water dispersible polyester composition 7
The water dispersible polyester composition 5 is a mixture of the water dispersible polyester 1 and the surfactant E. A water-dispersible polyester composition 7 was obtained in the same manner as the water-dispersible polyester composition 1 except that the surfactant E was used instead of the surfactant A.

水分散性ポリエステル組成物8
水分散性ポリエステル組成物8は、水分散性ポリエステル1と界面活性剤Fとの混合物である。界面活性剤Aの代わりに界面活性剤Fを用いた以外は水分散性ポリエステル組成物1と同様にして、水分散性ポリエステル組成物8を得た。
Water dispersible polyester composition 8
The water dispersible polyester composition 8 is a mixture of the water dispersible polyester 1 and the surfactant F. A water-dispersible polyester composition 8 was obtained in the same manner as the water-dispersible polyester composition 1 except that the surfactant F was used instead of the surfactant A.

架橋剤
メチルメタクリレート10モル%/2−イソプロペニル−2−オキサゾリン70モル%/ポリエチレンオキシド(n=10)メタクリレート5モル%/アクリルアミド15モル%で構成されている(Tg=100℃)。なお、架橋剤は、特開昭63−37167号公報の製造例1〜3に記載の方法に準じて下記の通り製造した。すなわち、四つ口フラスコに、イオン交換水302部を仕込んで窒素気流中で60℃まで昇温させ、次いで重合開始剤として過硫酸アンモニウム0.5部、亜硫酸水素ナトリウム0.2部を添加し、メタクリル酸メチル7.8部、2−イソプロペニル−2−オキサゾリン52.8部、ポリエチレンオキシド(n=10)メタクリル酸20.4部、アクリルアミド6.6部の混合物を3時間にわたり、液温が60〜70℃になるよう調整しながら滴下した。滴下終了後も同温度範囲に2時間保持しつつ、撹拌下に反応を継続させ、次いで冷却して固形分が25%の架橋剤の水分散体を得た。
The crosslinking agent is composed of 10 mol% of methyl methacrylate / 2 mol of 2-isopropenyl-2-oxazoline / 5 mol% of polyethylene oxide (n = 10) methacrylate / 15 mol% of acrylamide (Tg = 100 ° C.). The crosslinking agent was produced as follows according to the method described in Production Examples 1 to 3 of JP-A No. 63-37167. That is, 302 parts of ion-exchanged water was charged into a four-necked flask and the temperature was raised to 60 ° C. in a nitrogen stream, then 0.5 parts of ammonium persulfate and 0.2 parts of sodium bisulfite were added as a polymerization initiator, A mixture of methyl methacrylate (7.8 parts), 2-isopropenyl-2-oxazoline (52.8 parts), polyethylene oxide (n = 10) methacrylic acid (20.4 parts) and acrylamide (6.6 parts) was stirred for 3 hours. The solution was added dropwise while adjusting to 60 to 70 ° C. After the completion of dropping, the reaction was continued under stirring while maintaining the same temperature range for 2 hours, and then cooled to obtain an aqueous dispersion of a crosslinking agent having a solid content of 25%.

添加剤
帯電防止剤(複合資材株式会社製 商品名エレカットL)
Additives Antistatic agent (trade name ELECUT L manufactured by Composite Materials Co., Ltd.)

本発明の光学用フィルムは、タッチパネルの基材フィルムとして好適に用いることができる。また、液晶表示面に貼付ける表面保護フィルムとして好適に用いることができる。
本発明の光学用フィルムは、少なくとも片面にハードコート層を設ける加工を施したあと、透明導電層や粘着層を設ける加工を施し製品サイズに裁断することで、タッチパネルの基材フィルムや表面保護フィルム等の光学部材に加工することができる。
The optical film of the present invention can be suitably used as a base film for a touch panel. Moreover, it can use suitably as a surface protection film stuck on a liquid crystal display surface.
The optical film of the present invention has a process of providing a hard coat layer on at least one side, and then a process of providing a transparent conductive layer or an adhesive layer and cutting it into a product size. It can process into optical members, such as.

Claims (2)

ポリエチレンテレフタレート二軸延伸フィルムおよびその少なくとも片面に設けられた厚み10〜300nmの易接着層からなる光学用フィルムであって、易接着層は高分子バインダーおよび界面活性剤を含有し、易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー100重量部に対して界面活性剤0.5〜10重量部であり、易接着層における界面活性剤の含有率は易接着層の重量を基準に0.5〜6重量%であり、界面活性剤は疎水基と親水基とからなり、疎水基は炭素数13〜15の直鎖炭化水素であり、親水基はオキシエチレンとオキシプロピレンの共重合体からなり、オキシエチレンの親水基における割合が30〜50モル%であり、界面活性剤の重量平均分子量が1200〜1600であることを特徴とする光学用フィルム。   An optical film comprising a polyethylene terephthalate biaxially stretched film and an easy-adhesion layer having a thickness of 10 to 300 nm provided on at least one surface thereof, the easy-adhesion layer containing a polymer binder and a surfactant, The ratio of the content of the polymer binder to the surfactant is 0.5 to 10 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder, and the content of the surfactant in the easy adhesion layer is the easy adhesion layer. The surfactant is composed of a hydrophobic group and a hydrophilic group, the hydrophobic group is a linear hydrocarbon having 13 to 15 carbon atoms, and the hydrophilic group is oxyethylene and It consists of a copolymer of oxypropylene, the proportion of oxyethylene in the hydrophilic group is 30 to 50 mol%, and the weight average molecular weight of the surfactant is 1200 to 1600. Optical film characterized. 易接着層における、凸部の大きさの最大径が20μm以上かつ凸部の高さが1μm以上の異物が3個以下/100mである、請求項1記載の光学用フィルム。 2. The optical film according to claim 1, wherein in the easy-adhesive layer, the number of foreign matters having a maximum diameter of 20 μm or more and a height of 1 μm or more is 3 or less / 100 m 2 .
JP2010000063A 2010-01-04 2010-01-04 Optical film Expired - Fee Related JP5357064B2 (en)

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