JP2007211091A - 粘着剤組成物、粘着剤層、および粘着剤付光学部材 - Google Patents
粘着剤組成物、粘着剤層、および粘着剤付光学部材 Download PDFInfo
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- JP2007211091A JP2007211091A JP2006031137A JP2006031137A JP2007211091A JP 2007211091 A JP2007211091 A JP 2007211091A JP 2006031137 A JP2006031137 A JP 2006031137A JP 2006031137 A JP2006031137 A JP 2006031137A JP 2007211091 A JP2007211091 A JP 2007211091A
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Abstract
【解決手段】(メタ)アクリル系モノマー30〜98重量%およびその他の重合性モノマー0.1〜30重量%含有する(メタ)アクリル系ポリマー100重量部に対し、架橋剤0.02〜5重量部、および下記式で表されるイミダゾールシラン化合物0.001〜5重量部含有する粘着剤組成物。
(R1およびR2は水素原子またはアルキル基、R3およびR4はアルキル基、ならびにnは1〜20の整数である。また、aは1〜3の整数、bは1〜3の整数、ならびにcは0または1であり、かつa+b+c=4である。)
【選択図】なし
Description
モノマー単位として、一般式CH2=C(Ra)COORb(ただし、Raは水素またはメチル基、Rbは炭素数2〜14のアルキル基である)で表される(メタ)アクリル系モノマー30〜98重量%およびその他の重合性モノマー0.1〜30重量%含有する(メタ)アクリル系ポリマー100重量部に対し、
架橋剤0.02〜5重量部、および下記式(1)で表されるイミダゾールシラン化合物0.001〜5重量部含有することを特徴とする。
モノマー単位として、一般式CH2=C(Ra)COORb(ただし、Raは水素またはメチル基、Rbは炭素数2〜14のアルキル基である)で表される(メタ)アクリル系モノマー30〜98重量%およびその他の重合性モノマー0.1〜30重量%含有する(メタ)アクリル系ポリマー100重量部に対し、
架橋剤0.02〜5重量部、および下記式(1)で表されるイミダゾールシラン化合物0.001〜5重量部含有することを特徴とする。
得られた(メタ)アクリル系ポリマーの重量平均分子量は、GPC(ゲル・パーミエーション・クロマトグラフィー)により測定した。
・分析装置:東ソー社製、HLC−8120GPC
・データ処理装置:東ソー社製、GPC−8020
・カラム:東ソー社製、G7000HXL−H+GMHXL+GMHXL
・カラムサイズ;各7.8mmφ×30cm(計90cm)
・流量:0.8ml/min
・注入試料濃度:約0.1重量%
・注入量:100μl
・カラム温度:40℃
・溶離液:テトラヒドロフラン
・検出器:示差屈折計(RI)
なお、分子量はポリスチレン換算により算出した。
各実施例・比較例で作製した粘着剤層をW1g(約0.1g)取り出し、酢酸エチルに室温(約25℃)下で1週間浸漬した。その後、浸漬処理した粘着剤層(不溶分)を酢酸エチル中から取り出し、130℃で2時間乾燥後の重量W2gを測定し、(W2/W1)×100として計算される値をゲル分率(重量%)とした。
(初期接着力)
実施例、比較例で得られた粘着剤付光学フィルム(25mm×100mm)を、無アルカリガラス(コーニング社製、1737、厚み:0.7mm)に2kgローラーでロール1往復して貼着し、評価用サンプルを得た。その後、25℃/65%RH雰囲気下において、剥離角度90°、剥離速度300mm/minで剥離接着力(初期対ガラス接着力)(N/25mm)を測定した。
上記初期接着力の評価用サンプルと同様のサンプルを、70℃の水浴中に1時間放置した後、水浴から取り出しサンプル表面の水滴を拭き取り、25℃/65%RH雰囲気下において、剥離角度90°、剥離速度300mm/minで剥離接着力(N/25mm)を測定した。
(耐久性試験(a))
作製した粘着剤付光学フィルム(15インチサイズ)を、無アクリルガラス(コーニング社製、1737、厚み:0.7mm)に貼り付けた後、50℃、5atm(0.5MPa)のオートクレーブにて15分間、次いで110℃(ドライ)の雰囲気下で500時間保存してから、室温(約25℃)に戻し、評価用サンプルを得た。耐久性試験(a)(加熱処理試験)の評価は目視でおこない、評価基準は以下のとおりである。なお、視認性として、浮き、剥がれの有無と表示画像の見易さを評価した。
・粘着剤層の浮きや剥がれが生じなかった場合:○
・粘着剤層の浮きや剥がれが生じたが、視認性には影響を与えなかった場合:×
・粘着剤層の浮きや剥がれが生じ、視認性にも影響を与えた場合:××
(耐久性試験(b))
作製した粘着剤付光学フィルム(15インチサイズ)を、無アクリルガラス(コーニング社製、1737、厚み:0.7mm)に貼り付けた後、50℃、5atm(0.5Pa)のオートクレーブにて15分間、次いで70/95%RHの雰囲気下で500時間保存してから、室温(約25℃)に戻し、評価用サンプルを得た。耐久性試験(b)(加熱加湿処理試験)の評価は目視でおこない、評価基準は以下のとおりである。なお、視認性として、浮き、剥がれの有無と表示画像の見易さを評価した。
・粘着剤層の浮きや剥がれが生じなかった場合:○
・粘着剤層の浮きや剥がれが生じたが、視認性には影響を与えなかった場合:×
・粘着剤層の浮きや剥がれが生じ、視認性にも影響を与えた場合:××
〔アクリル系ポリマー(A)〕
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた4つ口フラスコに、ブチルアクリレート85重量部、アクリル酸15重量部、重合開始剤として過酸化ベンゾイル0.2重量部、酢酸エチル200重量部を仕込み、緩やかに攪拌しながら窒素ガスを導入して窒素置換した後、フラスコ内の液温を60℃付近に保って8時間重合反応を行い、アクリル系ポリマー(A)溶液を調製した。上記アクリル系ポリマー(A)の重量平均分子量は190万であった。
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた4つ口フラスコに、ブチルアクリレート85重量部、N−シクロヘキシルマレイミド15重量部、重合開始剤として過酸化ベンゾイル0.2重量部、酢酸エチル200重量部を仕込み、緩やかに攪拌しながら窒素ガスを導入して窒素置換した後、フラスコ内の液温を60℃付近に保って8時間重合反応を行い、アクリル系ポリマー(B)溶液を調製した。上記アクリル系ポリマー(B)の重量平均分子量は185万であった。
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた4つ口フラスコに、ブチルアクリレート85重量部、N,N−ジメチルアクリルアミド15重量部、重合開始剤として過酸化ベンゾイル0.2重量部、酢酸エチル200重量部を仕込み、緩やかに攪拌しながら窒素ガスを導入して窒素置換した後、フラスコ内の液温を60℃付近に保って8時間重合反応を行い、アクリル系ポリマー(C)溶液を調製した。上記アクリル系ポリマー(C)の重量平均分子量は170万であった。
ポリビニルアルコールフィルム(厚さ:80μm)をヨウ素水溶液中で5倍に延伸した後、乾燥させた。次いで、前記フィルムの両側にトリアセチルセルロースフィルム(厚さ:80μm)を接着剤(日本合成化学社製、ゴーセノール NH−18)を介して接着し、偏光板を作製した。
(粘着剤付光学フィルムの作製)
上記アクリル系ポリマー(A)溶液の固形分100重量部に対して、イソシアネート系架橋剤(日本ポリウレタン工業社製、コロネートL)0.5重量部、および下記式(2)で表されるイミダゾールシラン化合物0.1重量部を配合したアクリル系粘着剤溶液(1)を調整した。
(粘着剤付光学フィルムの作製)
実施例1において、上記イミダゾールシラン化合物に代えて、下記式(3)で表されるイミダゾールシラン化合物0.1重量部用いたこと以外は同様に行い、アクリル系粘着剤溶液(2)を調整した。
(粘着剤付光学フィルムの作製)
実施例1において、上記イミダゾールシラン化合物を0.5重量部用いたこと以外は同様に行い、アクリル系粘着剤溶液(3)を調整した。
(粘着剤付光学フィルムの作製)
実施例1において、上記アクリル系ポリマー(A)に代えて、上記アクリル系ポリマー(B)を用いたこと以外は同様に行い、アクリル系粘着剤溶液(4)を調整した。
(粘着剤付光学フィルムの作製)
実施例1において、上記アクリル系ポリマー(A)に代えて、上記アクリル系ポリマー(C)を用いたこと以外は同様に行い、アクリル系粘着剤溶液(5)を調整した。
(粘着剤付光学フィルムの作製)
実施例1において、上記式(2)で表されるイミダゾールシラン化合物の使用量を0.1重量部に代えたこと以外は同様に行い、粘着剤付光学フィルムを作製した。
(粘着剤付光学フィルムの作製)
実施例1において、上記式(2)で表されるイミダゾールシラン化合物の使用量を4重量部に代えたこと以外は同様に行い、粘着剤付光学フィルムを作製した。
(粘着剤付光学フィルムの作製)
実施例1において、イソシアネート系架橋剤に代えてエポキシ系架橋剤(三菱瓦斯化学、TETRAD−C)を用いたこと以外は同様に行い、粘着剤付光学フィルムを作製した。
(粘着剤付光学フィルムの作製)
上記イミダゾールシラン化合物を用いなかったこと以外は、実施例1と同様の方法によりアクリル系粘着剤溶液(6)を調整した。
(粘着剤付光学フィルムの作製)
実施例1において、上記イミダゾールシラン化合物に代えて、下記式(4)で表されるエポキシシラン化合物0.1重量部用いたこと以外は同様に行い、アクリル系粘着剤溶液(7)を調整した。
(粘着剤付光学フィルムの作製)
実施例1において、上記イミダゾールシラン化合物に代えて、下記式(5)で表される(メタ)アクリル酸エステル0.1重量部用いたこと以外は同様に行い、アクリル系粘着剤溶液(8)を調整した。
(粘着剤付光学フィルムの作製)
実施例1において、上記イミダゾールシラン化合物に代えて、下記式(6)で表されるβケトエステル構造を有するシラン化合物0.1重量部用いたこと以外は同様に行い、アクリル系粘着剤溶液(9)を調整した。
(粘着剤付光学フィルムの作製)
実施例1において、上記アクリル系ポリマー(A)に代えて、上記アクリル系ポリマー(C)を用いたこと、ならびに、上記イミダゾールシラン化合物に代えて、上記式(6)で表されるβケトエステル構造を有するシラン化合物0.1重量部用いたこと以外は同様に行い、アクリル系粘着剤溶液(10)を調整した。
Claims (7)
- モノマー単位として、一般式CH2=C(Ra)COORb(ただし、Raは水素またはメチル基、Rbは炭素数2〜14のアルキル基である)で表される(メタ)アクリル系モノマー30〜98重量%およびその他の重合性モノマー0.1〜30重量%含有する(メタ)アクリル系ポリマー100重量部に対し、
架橋剤0.02〜5重量部、および下記式(1)で表されるイミダゾールシラン化合物0.001〜5重量部含有することを特徴とする粘着剤組成物。
- 前記架橋剤がイソシアネート系架橋剤、エポキシ系架橋剤、および過酸化物からなる群より選ばれる少なくとも1種を含む請求項1に記載の粘着剤組成物。
- 光学部材用として用いられる請求項1または2に記載の粘着剤組成物。
- 請求項1〜3のいずれかに記載の粘着剤組成物を架橋してなることを特徴とする粘着剤層。
- 光学部材用として用いられる請求項4に記載の粘着剤層。
- 請求項4または5のいずれかに記載の粘着剤層を光学部材の片面または両面に形成してなることを特徴とする粘着剤付光学部材。
- 請求項6に記載の粘着剤付光学部材を少なくとも1枚用いた画像表示装置。
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JP2001187836A (ja) * | 2001-02-16 | 2001-07-10 | Nikko Materials Co Ltd | エポキシ樹脂組成物用添加剤およびそのエポキシ樹脂組成物 |
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WO2020003857A1 (ja) * | 2018-06-26 | 2020-01-02 | 日東電工株式会社 | 粘着剤層付片保護偏光フィルム、画像表示装置およびその連続製造方法 |
CN112119332A (zh) * | 2018-06-26 | 2020-12-22 | 日东电工株式会社 | 带粘合剂层的单侧保护偏振膜、图像显示装置及其连续制造方法 |
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