JP2011245809A - 積層ポリエステルフィルム - Google Patents
積層ポリエステルフィルム Download PDFInfo
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- JP2011245809A JP2011245809A JP2010123621A JP2010123621A JP2011245809A JP 2011245809 A JP2011245809 A JP 2011245809A JP 2010123621 A JP2010123621 A JP 2010123621A JP 2010123621 A JP2010123621 A JP 2010123621A JP 2011245809 A JP2011245809 A JP 2011245809A
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- acid
- polyester film
- film
- coating layer
- polyester
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
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- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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Abstract
【解決手段】 ナフタレン骨格を含有するポリエステル樹脂、金属酸化物、および2種類以上の架橋剤を含有する塗布層をポリエステルフィルムの少なくとも片面に有することを特徴とする積層ポリエステルフィルム。
【選択図】 なし
Description
特に塗布層中に使用する樹脂の屈折率が低いために、高い屈折率を有する金属酸化物を使用することが好ましく、屈折率として1.7以上のものを使用することが好ましい。金属酸化物の具体例としては、例えば、酸化ジルコニウム、酸化チタン、酸化スズ、酸化イットリウム、酸化アンチモン、酸化インジウム、酸化亜鉛、アンチモンチンオキサイド、インジウムチンオキサイド等が挙げられ、これらを単独で使用してもよいし、2種類以上使用してもよい。これらの中でも酸化ジルコニウムや酸化チタンがより好適に用いられ、特に、耐候性の観点から酸化ジルコニウムがより好適に用いられる。
ただし、後述するように、易滑性等の取り扱い性も付与する目的で使用する場合は、透明性を損なわない範囲で、平均粒径が0.1〜1.0μmの範囲の粒子を少量使用することも可能である。
ポリエステルに非相溶な他のポリマー成分および顔料を除去したポリエステル1gを精秤し、フェノール/テトラクロロエタン=50/50(重量比)の混合溶媒100mlを加えて溶解させ、30℃で測定した。
TEM(Hitachi製 H−7650、加速電圧100V)を使用して塗布層を観察し、粒子10個の粒径の平均値を平均粒径とした。
塗布層の表面をRuO4で染色し、エポキシ樹脂中に包埋した。その後、超薄切片法により作成した切片をRuO4で染色し、塗布層断面をTEM(Hitachi製 H−7650、加速電圧100V)を用いて測定した。
あらかじめ、ポリエステルフィルムの測定裏面に黒テープ(ニチバン株式会社製ビニールテープVT―50)を貼り、分光光度計(日本分光株式会社製 紫外可視分光光度計 V−570 および自動絶対反射率測定装置 AM−500N)を使用して同期モード、入射角5°、N偏光、レスポンス Fast、データ取区間隔1.0nm、バンド幅10nm、走査速度1000m/minで塗布層面を波長範囲300〜800nmの絶対反射率を測定し、その極小値における波長(ボトム波長)と反射率を評価した。
ポリエステルフィルムの塗布層側に、ジペンタエリスリトールヘキサアクリレート72重量部、1,6−ヘキサンジオールジアクリレート18重量部、五酸化アンチモン10重量部、光重合開始剤(商品名:イルガキュア184、チバスペシャルティケミカル製)1重量部、メチルエチルケトン200重量部の混合塗液を乾燥膜厚が5μmになるように塗布し、紫外線を照射して硬化させハードコート層を形成した。得られたフィルムを3波長光域型蛍光灯下で目視にて、干渉ムラを観察し、干渉ムラが確認できないものを◎、薄くまばらな干渉ムラが確認されるものを○、薄いが線状の干渉ムラが確認できるものを△、明瞭な干渉ムラが確認されるものを×とした。
より厳しい密着性の評価を行うために、上記(5)の評価で使用したハードコート液から五酸化アンチモンを除いた材料で検討した。すなわち、ジペンタエリスリトールヘキサアクリレート80重量部、1,6−ヘキサンジオールジアクリレート20重量部、光重合開始剤(商品名:イルガキュア184、チバスペシャルティケミカル製)5重量部、メチルエチルケトン200重量部の混合塗液を乾燥膜厚が5μmになるように塗布し、紫外線を照射して硬化させハードコート層を形成した。得られたフィルムに対して、60℃、90%RHの環境下で100時間後、10×10のクロスカットをして、その上に18mm幅のテープ(ニチバン株式会社製セロテープ(登録商標)CT−18)を貼り付け、180度の剥離角度で急激にはがした後の剥離面を観察し、剥離面積が3%未満ならば◎、3%以上10%未満なら○、10%以上50%未満なら△、50%以上ならば×とした。
<ポリエステル(A)の製造方法>
テレフタル酸ジメチル100重量部とエチレングリコール60重量部とを出発原料とし、触媒として酢酸マグネシウム・四水塩0.09重量部を反応器にとり、反応開始温度を150℃とし、メタノールの留去とともに徐々に反応温度を上昇させ、3時間後に230℃とした。4時間後、実質的にエステル交換反応を終了させた。この反応混合物にエチルアシッドフォスフェート0.04重量部を添加した後、三酸化アンチモン0.04重量部を加えて、4時間重縮合反応を行った。すなわち、温度を230℃から徐々に昇温し280℃とした。一方、圧力は常圧より徐々に減じ、最終的には0.3mmHgとした。反応開始後、反応槽の攪拌動力の変化により、極限粘度0.63に相当する時点で反応を停止し、窒素加圧下ポリマーを吐出させた。得られたポリエステル(A)の極限粘度は0.63であった。
ポリエステル(A)の製造方法において、エチルアシッドフォスフェート0.04重量部を添加後、平均粒径1.6μmのエチレングリコールに分散させたシリカ粒子を0.2重量部、三酸化アンチモン0.04重量部を加えて、極限粘度0.65に相当する時点で重縮合反応を停止した以外は、ポリエステル(A)の製造方法と同様の方法を用いてポリエステル(B)を得た。得られたポリエステル(B)は、極限粘度0.65であった。
(化合物例)
・ナフタレン骨格を含有するポリエステル樹脂:(IA)
下記組成で共重合したポリエステル樹脂の水分散体
モノマー組成:(酸成分)2,6−ナフタレンジカルボン酸/5−ナトリウムスルホイソフタル酸//(ジオール成分)エチレングリコール/ジエチレングリコール=92/8//80/20(mol%)
・ナフタレン骨格を含有するポリエステル樹脂:(IB)
下記組成で共重合したポリエステル樹脂の水分散体
モノマー組成:(酸成分)2,6−ナフタレンジカルボン酸/テレフタル酸/5−ナトリウムスルホイソフタル酸//(ジオール成分)エチレングリコール/ジエチレングリコール=78/15/7//90/10(mol%)
・金属酸化物:(IIB)平均粒径15nmの酸化ジルコニウム粒子
・金属酸化物:(IIC)平均粒径15nmの酸化チタン粒子
メチルエチルケトン溶媒中で、アジピン酸/イソフタル酸//1,6−ヘキサンジオール=50/50//100(mol%)のポリエステルポリオール(平均分子量1700)100重量部、1,4−ブタンジオール9重量部、トリメチロールプロパン8重量部に、トリレンジイソシアネート80重量部を添加して、反応を行った後、ジメチロールプロピオン酸12重量部、ポリエチレングリコール(平均分子量600)16重量部、アミン触媒を添加し、75℃で反応を行った。次に55℃にてメチルエチルケトンオキシム16重量部を添加し、ブロック化イソシアネート基含有ウレタンプレポリマーとした。さらに、トリエチルアミン7.2重量部、水450重量部を混合し、トリエチレンテトラミン2.9重量部を添加し、反応させ、メチルエチルケトン溶媒を除去し得られたブロック化イソシアネート化合物。
・イソシアネート化合物:(IIIB)
ビスフェノールAのエチレンオキサイド2モル付加物とマレイン酸とのポリエステル(分子量2000)200重量部に、ヘキサメチレンジイソシアネート33.6重量部を添加し、100℃で2時間反応を行った。次いで系の温度を一旦50℃まで下げ、30%重亜硫酸ナトリウム水溶液73重量部を添加し、45℃で60分間攪拌を行った後、水718重量部で希釈したブロック化イソシアネート系化合物。
・オキサゾリン化合物:(IIIC)
オキサゾリン基及びポリアルキレンオキシド鎖を有するアクリルポリマー エポクロスWS−500(日本触媒製)
・ヘキサメトキシメチルメラミン(IIID)
・エポキシ化合物:(IIIE)ポリグリセロールポリグリシジルエーテルである、デナコールEX−521(ナガセケムテックス製)。
下記組成で共重合したポリエステル樹脂の水分散体
モノマー組成:(酸成分)テレフタル酸/イソフタル酸/5−ナトリウムスルホイソフタル酸//(ジオール成分)エチレングリコール/1,4−ブタンジオール/ジエチレングリコール=56/40/4//70/20/10(mol%)
・粒子:(VB)平均粒径0.30μmのシリカ粒子
・粒子:(VC)平均粒径0.16μmのシリカ粒子
ポリエステル(A)を押出機に各々供給し、285℃で溶融した後、40℃に設定した冷却ロール上に、押出し冷却固化させて未延伸シートを得た。次いで、ロール周速差を利用してフィルム温度85℃で縦方向に3.4倍延伸した後、この縦延伸フィルムの両面に、下記表1に示す塗布液1を塗布し、テンターに導き、横方向に120℃で4.0倍延伸し、225℃で熱処理を行った後、横方向に2%弛緩し、膜厚(乾燥後)が0.09μmの塗布層を有する厚さ125μmのポリエステルフィルムを得た。得られたポリエステルフィルムの絶対反射率を測定したところ、極小値は580nmで、その反射率は4.8%であった。ハードコート層を積層後のフィルムには明瞭な干渉ムラはなく、また密着性も良好であった。このフィルムの特性を下記表3に示す。
実施例1において、塗布剤組成を下記表1または表2に示す塗布剤組成に変更する以外は実施例1と同様にして製造し、ポリエステルフィルムを得た。でき上がったポリエステルフィルムは表3に示すとおり、高い反射率を有し、干渉ムラレベルも良好で、密着性も良好なものであった。
ポリエステル(A)、(B)をそれぞれ90%、10%の割合で混合した混合原料を最外層(表層)の原料とし、ポリエステル(A)を中間層の原料として、2台の押出機に各々を供給し、各々285℃で溶融した後、40℃に設定した冷却ロール上に、2種3層(表層/中間層/表層=1:18:1の吐出量)の層構成で共押出し冷却固化させて未延伸シートを得た。次いで、ロール周速差を利用してフィルム温度85℃で縦方向に3.4倍延伸した後、この縦延伸フィルムの両面に、下記表1に示す塗布液1を塗布し、テンターに導き、横方向に120℃で4.0倍延伸し、225℃で熱処理を行った後、横方向に2%弛緩し、膜厚(乾燥後)が0.09μmの塗布層を有する厚さ125μmのポリエステルフィルムを得た。得られたポリエステルフィルムの絶対反射率を測定したところ、極小値は580nmで、その反射率は4.8%であった。ハードコート層を積層後のフィルムには明瞭な干渉ムラはなく、また密着性も良好であった。このフィルムの特性を表3に示す。
実施例27において、塗布剤組成を表2に示す塗布剤組成に変更する以外は実施例27と同様にして製造し、ポリエステルフィルムを得た。でき上がったポリエステルフィルムは表3に示すとおり、高い反射率を有し、干渉ムラレベルも良好で、密着性も良好なものであった。
実施例1において、塗布剤組成を表2に示す塗布剤組成に変更する以外は実施例1と同様にして製造し、ポリエステルフィルムを得た。でき上がった積層ポリエステルフィルムを評価したところ、表3に示すとおり、明瞭な干渉ムラが観察できる場合、密着性が劣る場合が見られた。
Claims (3)
- ナフタレン骨格を含有するポリエステル樹脂、金属酸化物、および2種類以上の架橋剤を含有する塗布層をポリエステルフィルムの少なくとも片面に有することを特徴とする積層ポリエステルフィルム。
- 金属酸化物が酸化ジルコニウムである請求項1記載の積層ポリエステルフィルム。
- 塗布層表面の絶対反射率が波長400〜800nmの範囲で極小値を1つ有し、当該極小値における絶対反射率が4.0%以上である請求項1または2記載の積層ポリエステルフィルム。
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JP2014000775A (ja) * | 2012-06-21 | 2014-01-09 | Mitsubishi Plastics Inc | 積層ポリエステルフィルム |
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JP2015071309A (ja) * | 2014-11-28 | 2015-04-16 | 三菱樹脂株式会社 | 積層ポリエステルフィルム |
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Also Published As
Publication number | Publication date |
---|---|
CN102905899A (zh) | 2013-01-30 |
EP2578400B1 (en) | 2020-05-06 |
US20130108864A1 (en) | 2013-05-02 |
WO2011152173A1 (ja) | 2011-12-08 |
EP2578400A1 (en) | 2013-04-10 |
US9507056B2 (en) | 2016-11-29 |
KR20130097072A (ko) | 2013-09-02 |
EP2578400A4 (en) | 2014-10-08 |
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