JP6343364B2 - 粘着剤組成物、及び粘着シート - Google Patents
粘着剤組成物、及び粘着シート Download PDFInfo
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- JP6343364B2 JP6343364B2 JP2017083001A JP2017083001A JP6343364B2 JP 6343364 B2 JP6343364 B2 JP 6343364B2 JP 2017083001 A JP2017083001 A JP 2017083001A JP 2017083001 A JP2017083001 A JP 2017083001A JP 6343364 B2 JP6343364 B2 JP 6343364B2
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- ISLMUNSNHGLMCV-UHFFFAOYSA-N tributyl(2-methoxyethyl)phosphanium Chemical compound CCCC[P+](CCCC)(CCCC)CCOC ISLMUNSNHGLMCV-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- MEJYOZOPFBOWNM-UHFFFAOYSA-N triethyl(heptyl)azanium Chemical compound CCCCCCC[N+](CC)(CC)CC MEJYOZOPFBOWNM-UHFFFAOYSA-N 0.000 description 1
- NFRBUOMQJKUACC-UHFFFAOYSA-N triethyl(pentyl)azanium Chemical compound CCCCC[N+](CC)(CC)CC NFRBUOMQJKUACC-UHFFFAOYSA-N 0.000 description 1
- WGYXSYLSCVXFDU-UHFFFAOYSA-N triethyl(propyl)azanium Chemical compound CCC[N+](CC)(CC)CC WGYXSYLSCVXFDU-UHFFFAOYSA-N 0.000 description 1
- JFZKOODUSFUFIZ-UHFFFAOYSA-N trifluoro phosphate Chemical compound FOP(=O)(OF)OF JFZKOODUSFUFIZ-UHFFFAOYSA-N 0.000 description 1
- IQZRBOPLVCXUST-UHFFFAOYSA-M trifluoromethanesulfonate;trimethyl(oxiran-2-ylmethyl)azanium Chemical compound C[N+](C)(C)CC1CO1.[O-]S(=O)(=O)C(F)(F)F IQZRBOPLVCXUST-UHFFFAOYSA-M 0.000 description 1
- NRZWQKGABZFFKE-UHFFFAOYSA-N trimethylsulfonium Chemical compound C[S+](C)C NRZWQKGABZFFKE-UHFFFAOYSA-N 0.000 description 1
- LAGQNGWYNLUQRI-UHFFFAOYSA-N trioctylmethylammonium bis(trifluoromethylsulfonyl)imide Chemical compound FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F.CCCCCCCC[N+](C)(CCCCCCCC)CCCCCCCC LAGQNGWYNLUQRI-UHFFFAOYSA-N 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
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Description
[式(A)中のRaは、炭素数4から20の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよく、RbおよびRcは、同一または異なって、水素または炭素数1から16の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。但し、窒素原子が2重結合を含む場合、Rcはない。]
[式(B)中のRdは、炭素数2から20の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよく、Re、Rf、およびRgは、同一または異なって、水素または炭素数1から16の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。]
[式(C)中のRhは、炭素数2から20の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよく、Ri、Rj、およびRkは、同一または異なって、水素または炭素数1から16の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。]
[式(D)中のZは、窒素、硫黄、またはリン原子を表し、Rl、Rm、Rn、およびRoは、同一または異なって、炭素数1から20の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。但しZが硫黄原子の場合、Roはない。]
[式(E)中のRPは、炭素数1から18の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。]
[式(a)中のR1は、水素または炭素数1から3の炭化水素基を表し、R2は、水素または炭素数1から5の炭化水素基を表す。]
[式(b)中のR3は、水素または炭素数1から3の炭化水素基を表し、R4は、水素または炭素数1から5の炭化水素基を表す。]
[式(c)中のR5は、水素または炭素数1から3の炭化水素基を表し、R6は、水素または炭素数1から5の炭化水素基を表す。]
[式(d)中のR7は、水素または炭素数1から3の炭化水素基を表し、R8は、水素または炭素数1から5の炭化水素基を表す。]
前記アクリルエマルション系重合体は、原料モノマーとして、(メタ)アクリル酸アルキルエステルを70〜99.5重量%、及びカルボキシル基含有不飽和モノマーを0.5〜10重量%から構成される重合体である。前記アクリルエマルション系重合体は、単独で又は2種以上組み合わせて使用することができる。なお、本発明では、「(メタ)アクリル」とは「アクリル」及び/又は「メタクリル」のことをいう。
本発明のアクリルエマルション系重合体のエマルション重合に用いる乳化剤としては、分子中にラジカル重合性官能基が導入された反応性乳化剤(ラジカル重合性官能基を含む反応性乳化剤)を用いることが好ましい。これらの乳化剤は単独でまたは2種以上が用いられる。
アクリルエマルション系重合体約0.1gを採取し、平均孔径0.2μmの多孔質テトラフルオロエチレンシート(商品名「NTF1122」、日東電工株式会社製)に包んだ後、凧糸で縛り、その際の重量を測定し、該重量を浸漬前重量とする。なお、該浸漬前重量は、アクリルエマルション系重合体(上記で採取したもの)と、テトラフルオロエチレンシートと、凧糸の総重量である。また、テトラフルオロエチレンシートと凧糸の合計重量も測定しておき、該重量を包袋重量とする。
溶剤不溶分(重量%)=(a−b)/(c−b)×100
(上記式中において、aは浸漬後重量であり、bは包袋重量であり、cは浸漬前重量である。)
GPC測定は、東ソー株式会社製GPC装置「HLC−8220GPC」を用いて行い、ポリスチレン換算値にて分子量を求める。測定条件は下記の通りである。
サンプル濃度:0.2重量%(THF溶液)
サンプル注入量:10μl
溶離液:THF
流速:0.6ml/min
測定温度:40℃
カラム:
サンプルカラム;TSKguardcolumn SuperHZ−H 1本+TSKgel SuperHZM−H 2本
リファレンスカラム;TSKgel SuperH−RC 1本
検出器:示差屈折計
本発明の粘着剤組成物は、HLB(Hydrophile−Lipophile−Blance)値が6以上のノニオン性界面活性剤を必須成分として含有する。なお、HLB値は、GriffinによるHydrophile−Lipophile Balanceであり、界面活性剤の水や油への親和性の程度を表す値である。HLB値の定義については、W.C.Griffin:J.Soc.Cosmetic Chemists,1,311(1949)や、高橋越民、難波義郎、小池基生、小林正雄共著、「界面活性剤ハンドブック」、第3版、工学図書株式会社出版、昭和47年11月25日、p179〜182などに記載されており、親水性と親油性の比を0〜20の間の数値で表したものである。
本発明の粘着剤組成物は、架橋剤を必須成分として含有する。前記アクリルエマルション系重合体を、前記架橋剤を用いて、適宜架橋することにより、より耐熱性に優れた粘着剤層(粘着シート)が得られる。本発明に用いられる架橋剤としては、イソシアネート化合物、エポキシ化合物、メラミン系樹脂、アジリジン誘導体、および金属キレート化合物などが用いられる。なかでも、主に適度な凝集力を得る観点から、イソシアネート化合物やエポキシ化合物が特に好ましく用いられる。これらの化合物は単独で使用してもよく、また2種以上を混合して使用してもよい。
同重量の水(25℃)と架橋剤を、攪拌機を用いて回転数300rpm、10分の条件で混合し、遠心分離により水相と油相に分ける。次いで、水相を採取し120℃で1時間乾燥して、乾燥減量から水相中の不揮発分(水100重量部に対する不揮発成分の重量部)を求める。
非水溶性架橋剤の有するカルボキシル基と反応しうる官能基のモル数=[非水溶性架橋剤の配合量(配合量)]/[官能基当量]=4/110
例えば、非水溶性架橋剤として、エポキシ当量が110(g/eq)のエポキシ系架橋剤を4g添加(配合)する場合、エポキシ系架橋剤の有するエポキシ基のモル数は、例えば、以下のように算出できる。
エポキシ系架橋剤の有するエポキシ基のモル数=[エポキシ系架橋剤の配合量(配合量)]/[エポキシ当量]=4/110
本発明の粘着剤組成物は、イオン性化合物を必須成分として含有する。前記イオン性化合物としては、特に制限されないが、例えば、前記イオン性化合物が、フッ素原子を含むアニオンや、窒素原子を含むアニオン、スルホニル基を有するアニオンを含有することが好ましく、より好ましくは、イオン液体、及び/又は、アルカリ金属塩である。これらのイオン性化合物を含有することにより、優れた帯電防止性を付与することができる。
[式(a)中のR1は、水素または炭素数1から3の炭化水素基を表し、R2は、水素または炭素数1から7の炭化水素基を表す。]
[式(b)中のR3は、水素または炭素数1から3の炭化水素基を表し、R4は、水素または炭素数1から7の炭化水素基を表す。]
[式(c)中のR5は、水素または炭素数1から3の炭化水素基を表し、R6は、水素または炭素数1から7の炭化水素基を表す。]
[式(d)中のR7は、水素または炭素数1から3の炭化水素基を表し、R8は、水素または炭素数1から7の炭化水素基を表す。]
ニウムトリフルオロメタンスルホネート、N,N−ジエチル−N−メチル−N−(2−メトキシエチル)アンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジエチル−Nメチル−N−(2−メトキシエチル)アンモニウムビス(ペンタフルオロエタンスルホニル)イミド、グリシジルトリメチルアンモニウムトリフルオロメタンスルホネート、グリシジルトリメチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、グリシジルトリメチルアンモニウムビス(ペンタフルオロエタンスルホニル)イミド、テトラオクチルホスホニウムトリフルオロメタンスルホネート、テトラオクチルホスホニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−エチル−N−プロピルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−エチル−N−ブチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−エチル−N−ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−エチル−N−へキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−エチル−N−ヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−エチル−N−ノニルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N,N−ジプロピルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−プロピル−N−ブチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−プロピル−N−ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−プロピル−N−ヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−プロピル−N−ヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−ブチル−N−ヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−ブチル−N−ヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N−ペンチル−N−ヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジメチル−N,N−ジヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリメチルヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジエチル−N−メチル−N−プロピルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジエチル−N−メチル−N−ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジエチル−N−メチル−N−ヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジエチル−N−プロピル−N−ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリエチルプロピルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリエチルペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリエチルヘプチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジプロピル−N−メチル−N−エチルアンモニウムビス(トリフルオロメダンスルホニル)イミド、N,N−ジプロピル−N−メチル−N−ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジプロピル−N−ブチル−N−へキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジプロピル−N,N−ジヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジブチル−N−メチル−N−ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N,N−ジブチル−N−メチル−N−ヘキシルアンモニウムビス(トリフルオロメタンスルホニル)イミド、トリオクチルメチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、N−メチル−N−エチル−N−プロピル−N−ペンチルアンモニウムビス(トリフルオロメタンスルホニル)イミド、1−ブチルピリジニウム(トリフルオロメタンスルホニル)トリフルオロアセトアミド、1−ブチル−3−メチルピリジニウム(トリフルオロメタンスルホニル)トリフルオロアセトアミド、1−エチル−3−メチルイミダゾリウム(トリフルオロメタンスルホニル)トリフルオロアセトアミド、N−エチル−N−メチルモルフォリニウムチオシアネート、4−エチル−4−メチルモルフォリニウムメチルカーボネート、1−エチル−3−メチルイミダゾリウムチオシアネート、1−ブチル−3−メチルイミダゾリウムチオシアネート、1−エチル−3−メチルイミダゾリウムテトラシアノボレート、1−エチル−3−メチルイミダゾリウムトリス(ペンタフルオロエチル)トリフルオロホスフェート、1−エチル−3−メチルイミダゾリウムビス(フルオロフルホニル)イミド、トリエチルスルホニウムビス(トリフルオロメチルスルホニル)イミドなどがあげられる。
前記水分散型アクリル系粘着剤組成物には、更に、エーテル基含有ポリシロキサン(アルキレンオキシド含有ポリシロキサン)を含有することができる。前記エーテル基含有ポリシロキサン(アルキレンオキシド含有ポリシロキサン)を含有することにより、より優れた帯電防止性が発現できる。帯電防止性が発現されるメカニズムの詳細は定かでないが、エーテル基は、空気中の水分と親和性が高いため、空気中への電荷の移動が容易に起こり易く、また、エーテル基は分子運動の自由度が高く、剥離時に生じる電荷を空気中へ効率的に移動し易いため、優れた帯電防止性が発現されているものと推察される。なお、シリコーン(ポリシロキサン)骨格は、低表面張力のため少量でも高い界面吸着性を持つので、被着体(被保護体)から粘着シートを剥離する際に被着体表面へ均一に微量転写でき、被着体表面に生じた電荷の移動を効率的に起こすことができ、優れた帯電防止性が発現される。
(式中、R1は1価の有機基、R2,R3及びR4はアルキレン基、もしくはR5はヒドロキシル基もしくは有機基、m及びnは0〜1000の整数。但し、m,nが同時に0となることはない。a及びbは0〜100の整数。但し、a,bが同時に0となることはない。)
本発明の粘着剤組成物は、上述の通り、本発明のアクリルエマルション系重合体、架橋剤、イオン性化合物、および特定のHLB値を有するノニオン性界面活性剤を必須の構成成分として含有する。さらに、必要に応じて、その他の各種添加剤を含有してよい。例えば、汚染性に影響を与えない範囲であれば、各種添加剤として、顔料、充填剤、レベリング剤、分散剤、可塑剤、安定剤、酸化防止剤、紫外線吸収剤、紫外線安定剤、老化防止剤、防腐剤、消泡剤などが挙げられる。
本発明の粘着剤層(粘着シート)は、前記粘着剤組成物により形成される。粘着剤層の形成方法は特に限定されず、公知慣用の粘着剤層の形成方法を用いることができる。粘着剤層の形成は、基材又は剥離フィルム(剥離ライナー、セパレータ)上に、前記粘着剤組成物を塗布した後、乾燥することより形成することができる。なお、粘着剤層を剥離(離型)フィルムに形成した場合には、前記粘着剤層を、基材に貼り合せて転写する。
次に、前記の架橋皮膜をテトラフルオロエチレンシートで包み、凧糸で縛ったもの(「サンプル」と称する)を、酢酸エチルで満たした50ml容器に入れ、23℃にて7日間静置した。その後、容器からサンプル(酢酸エチル処理後)を取り出して、アルミニウム製カップに移し、130℃で2時間、乾燥機中で乾燥して酢酸エチルを除去した後、重量を測定し、該重量を浸漬後重量とした。そして、下記の式から溶剤不溶分を算出した。
溶剤不溶分(重量%)=(d−e)/(f−e)×100
(上記式中において、dは浸漬後重量であり、eは包袋重量であり、fは浸漬前重量である。)
本発明の粘着剤組成物は、帯電防止性、粘着性(接着性)、再剥離性(軽剥離性、易剥離性)、及び、外観特性に優れ、再剥離が可能な粘着剤層を形成しうる粘着剤組成物であり、再剥離される用途に用いられる粘着剤層を形成するために用いられる。即ち、前記粘着剤層を有する粘着シートは再剥離される用途[例えば、建築養生用マスキングテープ、自動車塗装用マスキングテープ、電子部品(リードフレーム、プリント基板等)用マスキングテープ、サンドブラスト用マスキングテープなどのマスキングテープ類、アルミサッシ用表面保護フィルム、光学プラスチック用表面保護フィルム、光学ガラス用表面保護フィルム、自動車保護用表面保護フィルム、金属板用表面保護フィルムなどの表面保護フィルム類、バックグラインドテープ、ペリクル固定用テープ、ダイシング用テープ、リードフレーム固定用テープ、クリーニングテープ、除塵用テープ、キャリアテープ、カバーテープなどの半導体・電子部品製造工程用粘着テープ類、電子機器や電子部品の梱包用テープ類、輸送時の仮止めテープ類、結束用テープ類、ラベル類]等に好ましく用いられる。
(アクリルエマルション系重合体の調製)
容器に、水90重量部、及び、表1に示すように、アクリル酸2−エチルヘキシル(2EHA)92重量部、アクリル酸(AA)4重量部、メタクリル酸メチル(MMA)4重量部、反応性ノニオンアニオン系乳化剤[(第一工業製薬(株)製、商品名「アクアロンHS−1025」]2重量部を配合した後、ホモミキサーにより撹拌混合し、モノマーエマルションを調製した。
前記アクリルエマルション系重合体の水分散液に、アクリルエマルション系重合体(固形分)100重量部に対して、非水溶性架橋剤であるエポキシ系架橋剤[三菱ガス化学(株)製、商品名「TETRAD−C」、1,3−ビス(N,N−ジグリシジルアミノメチル)シクロヘキサン、エポキシ当量:110、官能基数:4]1.8重量部、1−エチル−3−メチルイミダゾリウムビスフルオロスルフォニルイミド[第一工業製薬(株)製、商品名「エレクセルAS−110」、有効成分100重量%]1重量部、エーテル基含有ポリシロキサン[信越シリコーン(株)製、商品名「KF−353」、有効成分100重量%]0.32重量部、HLB値が8のアセチレンジオール系化合物(組成物)[エアープロダクツ社製、商品名「サーフィノール440」、有効成分100重量%]1重量部を、攪拌機を用いて、23℃、2000rpm、10分の攪拌条件で攪拌混合し、再剥離用水分散型アクリル系粘着剤組成物を調製した。
さらに、前記再剥離用水分散型アクリル系粘着剤組成物を、PETフィルム(三菱樹脂(株)製、商品名「T100M38」、厚さ:38μm)のコロナ処理面上に、テスター産業(株)製アプリケーターを用いて、乾燥後の厚さが20μmとなるように塗布(コーティング)し、その後、熱風循環式オーブンで、120℃で2分間乾燥させ、さらにその後、50℃で1日間養生(エージング)して、粘着シートを得た。
表1に示すように、原料モノマーやノニオン性界面活性剤(アセチレンジオール系化合物)等の種類、配合量等を変更し、実施例1と同様にして、粘着剤組成物および粘着シートを得た。なお、表中に記載のない添加剤については、実施例1と同様の配合量で調製した。
実施例および比較例で得られた水分散型アクリル系粘着剤組成物および粘着シートについて、下記の測定方法又は評価方法により評価を行った。なお、評価結果については、表2に示した。
前記エマルションの平均粒子径の測定には、BECKMANCOULTER社製 LS1332レーザ散乱回折法粒度分布測定装置を用いた。ポンプスピードは30%、測定時間は90秒で行った。10倍希釈したエマルション粘着剤をセットし測定を行った。
作製した粘着シートを幅70mm、長さ120mmのサイズにカットし、セパレータを剥離した後、あらかじめ除電しておいたアクリル板(三菱レイヨン社製、アクリライト、厚み:1mm、幅:70mm、長さ:100mm)に貼り合わせた偏光板(日東電工(株)製、商品名「SEG1425DU」、「AGS1」、及び、「ARC150T」表面に、片方の端部が20mmはみ出すようにハンドローラーにて圧着した。続いて、20℃×25±2%RHの環境下に一日放置した後、図1に示すように所定の位置にサンプルをセットする。20mmはみ出した片方の端部を自動巻取り機に固定し、剥離角度150°、剥離速度30m/minとなるように剥離した。このときに発生する偏光板表面の電位を所定の位置に固定してある電位測定機(春日電機社製、KSD−0103)にて測定した。サンプルと電位測定機との距離はアクリル板表面測定時100mmとした。測定は20℃×25±2%RH、及び、23℃×50±2%RHの環境下で行った。なお、前記商品名「SEG1425DU」、「AGS1」、及び、「ARC150T」のそれぞれの性質としては、SEG1425DUは処理なし、AGS1はアンチグレア処理したもの、ARC150Tはアンチリフレクション処理したものである。
作製した粘着シートを幅25mm、長さ100mmのサイズにカットし、セパレータを剥離した後、貼り合わせ機(テスター産業(株)製、小型貼り合わせ機)を用いて、偏光板(日東電工社製、SEG1425DU、幅:70mm、長さ:100mm)に0.25MPa、0.3m/minの条件でラミネートし、評価サンプルを作製した。ラミネート後、23℃×50%RHの環境下に30分間放置した後、万能引張試験機にて剥離速度0.3m/min、剥離角度180°で剥離したときの剥離力(粘着力)(N/25mm)を測定し、「対DU初期剥離力」とした。測定は23℃×50%RHの環境下で行った。
実施例および比較例で得られた粘着シートの、粘着剤層表面の状態を目視で観察した。縦10cm×横10cmの観察範囲内の欠点(凹み及びゲル物)の個数を測定し、以下の基準で評価した。
欠点個数が0〜100個:外観が良好である(○)。
欠点個数が101個以上:外観が悪い(×)。
2EHA:アクリル酸2−エチルヘキシル
AA:アクリル酸
MMA:メタクリル酸メチル
HS−1025:第一工業製薬(株)製、商品名「アクアロンHS−1025」(反応性ノニオンアニオン系乳化剤)
T/C:三菱ガス化学(株)製、商品名「TETRAD−C」(1,3−ビス(N,N−ジグリシジルアミノメチル)シクロヘキサン、エポキシ当量:110、官能基数:4)(非水溶性架橋剤)
AS−110:第一工業製薬(株)製、商品名「エレクセルAS−110」(1−エチル−3−メチルイミダゾリウムビスフルオロスルフォニルイミド、有効成分100重量%)(イオン液体)
KF−353:信越シリコーン(株)製、商品名「KF−353」
サーフィノール420:エアープロダクツ社製、商品名「サーフィノール420」(HLB値:4、有効成分100重量%、アセチレンジオール系化合物)
サーフィノール440:エアープロダクツ社製、商品名「サーフィノール440」(HLB値:8、有効成分100重量%、アセチレンジオール系化合物)
サーフィノール465:エアープロダクツ社製、商品名「サーフィノール465」(HLB値:13、有効成分100重量%、アセチレンジオール系化合物)
サーフィノール485:エアープロダクツ社製、商品名「サーフィノール485」(HLB値:17、有効成分100重量%、アセチレンジオール系化合物)
アセチレノールE60:川研ファインケミカル社製、商品名「アセチレノールE60」(HLB値:11〜12、有効成分98重量%以上、アセチレングリコール系化合物)
アセチレノールE81:川研ファインケミカル社製、商品名「アセチレノールE81」(HLB値:12.2、有効成分98重量%以上、アセチレングリコール系化合物)
アセチレノールE100:川研ファインケミカル社製、商品名「アセチレノールE100」(HLB値:13〜14、有効成分98重量%以上、アセチレングリコール系化合物)
2 粘着シート
3 偏光板
4 アクリル板
5 サンプル固定台
Claims (3)
- (メタ)アクリル酸アルキルエステル70〜99.5重量%、及び、カルボキシル基含有不飽和モノマー0.5〜10重量%を、モノマー成分として構成されるアクリルエマルション系重合体、架橋剤、イオン性化合物、及び、HLB値が6以上のノニオン性界面活性剤を含有することを含有し、
前記イオン性化合物が、イオン液体であり、
前記イオン液体が、下記式(A)〜(E)で表わされるカチオンからなる群より選択される少なくとも1種のカチオンを含有することを特徴とする再剥離用水分散型アクリル系粘着剤組成物。
[式(A)中のRaは、炭素数4から20の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよく、RbおよびRcは、同一または異なって、水素または炭素数1から16の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。但し、窒素原子が2重結合を含む場合、Rcはない。]
[式(B)中のRdは、炭素数2から20の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよく、Re、Rf、およびRgは、同一または異なって、水素または炭素数1から16の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。]
[式(C)中のRhは、炭素数2から20の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよく、Ri、Rj、およびRkは、同一または異なって、水素または炭素数1から16の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。]
[式(D)中のZは、窒素、硫黄、またはリン原子を表し、Rl、Rm、Rn、およびRoは、同一または異なって、炭素数1から20の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。但しZが硫黄原子の場合、Roはない。]
[式(E)中のRPは、炭素数1から18の炭化水素基を表し、前記炭化水素基の一部がヘテロ原子で置換された官能基であってもよい。] - 前記ノニオン性界面活性剤が、アセチレン構造を含んでいることを特徴とする請求項1に記載の再剥離用水分散型アクリル系粘着剤組成物。
- 基材の少なくとも片面側に、請求項1又は2に記載の再剥離用水分散型アクリル系粘着剤組成物から形成された粘着剤層を有することを特徴とする粘着シート。
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