JP2012012537A - 粘着剤組成物、および該粘着剤を用いた光学部材 - Google Patents
粘着剤組成物、および該粘着剤を用いた光学部材 Download PDFInfo
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- JP2012012537A JP2012012537A JP2010152122A JP2010152122A JP2012012537A JP 2012012537 A JP2012012537 A JP 2012012537A JP 2010152122 A JP2010152122 A JP 2010152122A JP 2010152122 A JP2010152122 A JP 2010152122A JP 2012012537 A JP2012012537 A JP 2012012537A
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- OTYIGDNQBJUCNI-UHFFFAOYSA-N tetraethyl silicate triethoxy(oxiran-2-ylmethoxymethyl)silane Chemical compound C(C)O[Si](OCC)(OCC)OCC.C(C1CO1)OC[Si](OCC)(OCC)OCC OTYIGDNQBJUCNI-UHFFFAOYSA-N 0.000 description 1
- KHULVWYNEIZLER-UHFFFAOYSA-N tetraethyl silicate triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound C(C)O[Si](OCC)(OCC)OCC.C(C1CO1)OCCC[Si](OCC)(OCC)OCC KHULVWYNEIZLER-UHFFFAOYSA-N 0.000 description 1
- UUUBKUHOEXOTFP-UHFFFAOYSA-N tetraethyl silicate;3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)OCC.CCO[Si](OCC)(OCC)CCCS UUUBKUHOEXOTFP-UHFFFAOYSA-N 0.000 description 1
- PFOWXDLDZSTNHE-UHFFFAOYSA-N tetraethyl silicate;3-triethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CCO[Si](OCC)(OCC)OCC.CCO[Si](OCC)(OCC)CCCOC(=O)C(C)=C PFOWXDLDZSTNHE-UHFFFAOYSA-N 0.000 description 1
- OTRAIGCCGQEMOG-UHFFFAOYSA-N tetraethyl silicate;3-triethoxysilylpropyl prop-2-enoate Chemical compound CCO[Si](OCC)(OCC)OCC.CCO[Si](OCC)(OCC)CCCOC(=O)C=C OTRAIGCCGQEMOG-UHFFFAOYSA-N 0.000 description 1
- NYWGPGGNZCFHDZ-UHFFFAOYSA-N tetraethyl silicate;3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS.CCO[Si](OCC)(OCC)OCC NYWGPGGNZCFHDZ-UHFFFAOYSA-N 0.000 description 1
- HRLAHSXHMIJXHV-UHFFFAOYSA-N tetraethyl silicate;3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CCO[Si](OCC)(OCC)OCC.CO[Si](OC)(OC)CCCOC(=O)C(C)=C HRLAHSXHMIJXHV-UHFFFAOYSA-N 0.000 description 1
- SJWDBDMRCPLUTI-UHFFFAOYSA-N tetraethyl silicate;3-trimethoxysilylpropyl prop-2-enoate Chemical compound CCO[Si](OCC)(OCC)OCC.CO[Si](OC)(OC)CCCOC(=O)C=C SJWDBDMRCPLUTI-UHFFFAOYSA-N 0.000 description 1
- FJGOJSLDQKMJSD-UHFFFAOYSA-N tetraethyl silicate;triethoxysilylmethanethiol Chemical compound CCO[Si](CS)(OCC)OCC.CCO[Si](OCC)(OCC)OCC FJGOJSLDQKMJSD-UHFFFAOYSA-N 0.000 description 1
- BSTMSRIMJAEHTM-UHFFFAOYSA-N tetraethyl silicate;trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)OCC.CO[Si](OC)(OC)CCCOCC1CO1 BSTMSRIMJAEHTM-UHFFFAOYSA-N 0.000 description 1
- FZXUHBUNJYBPSF-UHFFFAOYSA-N tetraethyl silicate;trimethoxysilylmethanethiol Chemical compound CO[Si](CS)(OC)OC.CCO[Si](OCC)(OCC)OCC FZXUHBUNJYBPSF-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- KSFXBJJRUDMSCL-UHFFFAOYSA-N tetramethyl silicate;3-triethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)OC.CCO[Si](OCC)(OCC)CCCS KSFXBJJRUDMSCL-UHFFFAOYSA-N 0.000 description 1
- UMRRNLWGYGXKJT-UHFFFAOYSA-N tetramethyl silicate;3-triethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)OC.CCO[Si](OCC)(OCC)CCCOC(=O)C(C)=C UMRRNLWGYGXKJT-UHFFFAOYSA-N 0.000 description 1
- TYWOIFWGIPJOQP-UHFFFAOYSA-N tetramethyl silicate;3-triethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)OC.CCO[Si](OCC)(OCC)CCCOC(=O)C=C TYWOIFWGIPJOQP-UHFFFAOYSA-N 0.000 description 1
- XGFZGELZFRHQIU-UHFFFAOYSA-N tetramethyl silicate;3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)OC.CO[Si](OC)(OC)CCCS XGFZGELZFRHQIU-UHFFFAOYSA-N 0.000 description 1
- HKTUBAPEZVPPNP-UHFFFAOYSA-N tetramethyl silicate;3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)OC.CO[Si](OC)(OC)CCCOC(=O)C(C)=C HKTUBAPEZVPPNP-UHFFFAOYSA-N 0.000 description 1
- XWCXOVZGEZNJMY-UHFFFAOYSA-N tetramethyl silicate;3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)OC.CO[Si](OC)(OC)CCCOC(=O)C=C XWCXOVZGEZNJMY-UHFFFAOYSA-N 0.000 description 1
- JGASWBJDLLOTLH-UHFFFAOYSA-N tetramethyl silicate;triethoxysilylmethanethiol Chemical compound CO[Si](OC)(OC)OC.CCO[Si](CS)(OCC)OCC JGASWBJDLLOTLH-UHFFFAOYSA-N 0.000 description 1
- PWYOLUNMUKEIMH-UHFFFAOYSA-N tetramethyl silicate;trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical group CO[Si](OC)(OC)OC.CO[Si](OC)(OC)CCCOCC1CO1 PWYOLUNMUKEIMH-UHFFFAOYSA-N 0.000 description 1
- JZWSKHZDUIDXBM-UHFFFAOYSA-N tetramethyl silicate;trimethoxysilylmethanethiol Chemical compound CO[Si](CS)(OC)OC.CO[Si](OC)(OC)OC JZWSKHZDUIDXBM-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- 239000003017 thermal stabilizer Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 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
- 239000013638 trimer Substances 0.000 description 1
- LFBULLRGNLZJAF-UHFFFAOYSA-N trimethoxy(oxiran-2-ylmethoxymethyl)silane Chemical compound CO[Si](OC)(OC)COCC1CO1 LFBULLRGNLZJAF-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- QJOOZNCPHALTKK-UHFFFAOYSA-N trimethoxysilylmethanethiol Chemical compound CO[Si](CS)(OC)OC QJOOZNCPHALTKK-UHFFFAOYSA-N 0.000 description 1
- JPPHEZSCZWYTOP-UHFFFAOYSA-N trimethoxysilylmethyl prop-2-enoate Chemical compound CO[Si](OC)(OC)COC(=O)C=C JPPHEZSCZWYTOP-UHFFFAOYSA-N 0.000 description 1
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 description 1
- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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Abstract
【解決手段】本発明によれば、(1)92〜99.7質量部の(メタ)アクリル酸エステルモノマーと、0.3〜8質量部のカルボキシル基含有モノマーおよびヒドロキシ基含有(メタ)アクリル酸モノマーの少なくとも一方とからなり、重量平均分子量が500,000〜2,000,000である(メタ)アクリル共重合体100質量部;(2)カルボジイミド硬化剤0.01〜1.0質量部;および(3)シランカップリング剤オリゴマー0.02〜1.0質量部;を含む粘着剤組成物が提供される。
【選択図】なし
Description
(1)92〜99.7質量部の(メタ)アクリル酸エステルモノマーと、0.3〜8質量部のカルボキシル基含有モノマーおよびヒドロキシ基含有(メタ)アクリル酸モノマーの少なくとも一方とからなり、重量平均分子量が500,000〜2,000,000である(メタ)アクリル共重合体100質量部;
(2)カルボジイミド硬化剤0.01〜1.0質量部;および
(3)シランカップリング剤オリゴマー0.02〜1.0質量部;
を含む粘着剤組成物を完成するに至った。
(メタ)アクリル共重合体は、本発明の粘着剤組成物、後に粘着剤層を構成する主要な成分である。本発明に使用される(メタ)アクリル共重合体は、92〜99.7質量部の(メタ)アクリル酸エステルモノマーと、0.3〜8質量部のカルボキシル基含有モノマーおよびヒドロキシ基含有(メタ)アクリル酸モノマーの少なくとも一方とからなり、重量平均分子量が500,000〜2,000,000である。
(メタ)アクリル酸エステルモノマー(以下、単に「成分(a−1)」とも称する)は、分子中にヒドロキシ基を有さない(メタ)アクリル酸のエステルである。(メタ)アクリル酸エステルモノマーの具体例としては、以下に制限されないが、メチル(メタ)アクリレート、エチル(メタ)アクリレート、プロピル(メタ)アクリレート、イソプロピル(メタ)アクリレート、n−ブチル(メタ)アクリレート、イソブチル(メタ)アクリレート、tert−ブチル(メタ)アクリレート、イソアミル(メタ)アクリレート、n−ヘキシル(メタ)アクリレート、n−ヘプチル(メタ)アクリレート、n−オクチル(メタ)アクリレート、tert−オクチル(メタ)アクリレート、2−エチルヘキシル(メタ)アクリレート、デシル(メタ)アクリレート、イソデシル(メタ)アクリレート、トリデシル(メタ)アクリレート、ステアリル(メタ)アクリレート、イソステアリル(メタ)アクリレート、フェニル(メタ)アクリレート、ベンジル(メタ)アクリレート、ドデシル(メタ)アクリレート、テトラヒドロフルフリル(メタ)アクリレート、シクロヘキシル(メタ)アクリレート、4−n−ブチルシクロヘキシル(メタ)アクリレート、2−エチルヘキシルジグリコール(メタ)アクリレート、ブトキシエチル(メタ)アクリレート、ブトキシメチル(メタ)アクリレート、3−メトキシブチル(メタ)アクリレート、2−(2−メトキシエトキシ)エチル(メタ)アクリレート、2−(2−ブトキシエトキシ)エチル(メタ)アクリレート、4−ブチルフェニル(メタ)アクリレート、フェニル(メタ)アクリレート、2,4,5−テトラメチルフェニル(メタ)アクリレート、フェノキシメチル(メタ)アクリレート、フェノキシエチル(メタ)アクリレート、ポリエチレンオキシドモノアルキルエーテル(メタ)アクリレート、ポリエチレンオキシドモノアルキルエーテル(メタ)アクリレート、ポリプロピレンオキシドモノアルキルエーテル(メタ)アクリレート、トリフルオロエチル(メタ)アクリレート、ペンタデカフルオロオキシエチル(メタ)アクリレート、2−クロロエチル(メタ)アクリレート、2,3−ジブロモプロピル(メタ)アクリレート、トリブロモフェニル(メタ)アクリレート等が挙げられる。これらは、単独で使用してもよいし2種以上組み合わせて使用してもよい。
本発明に係るカルボキシル基含有モノマー(以下、単に「成分(a−2)」とも称する)は、分子中に少なくとも1個のカルボキシル基を有する不飽和モノマーである。カルボキシル基含有モノマーの具体例としては、以下に制限されないが、(メタ)アクリル酸、マレイン酸、無水マレイン酸、フマル酸、無水フマル酸、クロトン酸、イタコン酸、無水イタコン酸、ミリストレイン酸、パルミトレイン酸、およびオレイン酸などが挙げられる。これらは、単独で使用してもよいし2種以上組み合わせて使用してもよい。
本発明に係るヒドロキシ基含有(メタ)アクリルモノマー(以下、単に「成分(a−3)」とも称する)は、分子中にヒドロキシ基を有するアクリルモノマーである。ヒドロキシ基含有(メタ)アクリルモノマーの具体例としては、以下に制限されないが、2−ヒドロキシエチル(メタ)アクリレート、4−ヒドロキシブチル(メタ)アクリレート、1,6−ヘキサンジオールモノ(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、ジペンタエリスリトールペンタ(メタ)アクリレート、ネオペンチルグリコールモノ(メタ)アクリレート、トリメチロールプロパンジ(メタ)アクリレート、トリメチロールエタンジ(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−ヒドロキシブチル(メタ)アクリレート、2−ヒドロキシ−3−フェニルオキシプロピル(メタ)アクリレート、4−ヒドロキシシクロヘキシル(メタ)アクリレート、N−2−ヒドロキシエチル(メタ)アクリルアミド、シクロヘキサンジメタノールモノアクリレート等が挙げられ、さらに、アルキルグリシジルエーテル、アリルグリシジルエーテル、グリシジル(メタ)アクリレート等のグリシジル基含有化合物と、(メタ)アクリル酸との付加反応により得られる化合物等が挙げられる。これらは、単独で使用してもよいし2種以上組み合わせて使用してもよい。
本発明の(メタ)アクリル共重合体には、必要に応じて、上記成分(a−1)〜(a−3)と共重合可能なその他のモノマーをさらに用いてもよい。その他のモノマーは特に制限されず、具体的な例としては、例えば、グリシジル(メタ)アクリレート、メチルグリシジル(メタ)アクリレート等のエポキシ基を有するアクリルモノマー;ジメチルアミノエチル(メタ)アクリレート、ジエチルアミノエチル(メタ)アクリレート、N−tert−ブチルアミノエチル(メタ)アクリレート、メタクリルオキシエチルトリメチルアンモニウムクロライド(メタ)アクリレート等のアミノ基を有するアクリルモノマー;(メタ)アクリルアミド、N−メチロール(メタ)アクリルアミド、N−メトキシメチル(メタ)アクリルアミド、N,N−メチレンビス(メタ)アクリルアミド等のアミド基を有するアクリルモノマー;2−メタクリロイルオキシエチルジフェニルホスフェート(メタ)アクリレート、トリメタクリロイルオキシエチルホスフェート(メタ)アクリレート、トリアクリロイルオキシエチルホスフェート(メタ)アクリレート等のリン酸基を有するアクリルモノマー;スルホプロピル(メタ)アクリレートナトリウム、2−スルホエチル(メタ)アクリレートナトリウム、2−アクリルアミド−2−メチルプロパンスルホン酸ナトリウム等のスルホン酸基を有するアクリルモノマー;ウレタン(メタ)アクリレート等のウレタン基を有するアクリルモノマー;p−tert−ブチルフェニル(メタ)アクリレート、o−ビフェニル(メタ)アクリレート等のフェニル基を有するアクリルビニルモノマー;、2−アセトアセトキシエチル(メタ)アクリレート、ビニルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリス(β−メトキシエチル)シラン、ビニルトリアセチルシラン、メタクリロイルオキシプロピルトリメトキシシラン等のシラン基を有するビニルモニマー;スチレン、クロロスチレン、α―メチルスチレン、ビニルトルエン、塩化ビニル、酢酸ビニル、プロピオン酸ビニル、アクリロニトリル、ビニルピリジン等が挙げられる。これらその他のモノマーは、単独で使用してもよいし2種以上組み合わせて使用してもよい。
重量平均分子量が500,000未満であると、耐熱性が不足する。一方、重量平均分子量が2,000,000を超えると、タックが低く、貼合性が低下する。
本発明の粘着剤組成物は、カルボジイミド硬化剤を含む。カルボジイミド硬化剤は、上記の(メタ)アクリル共重合体中のヒドロキシ基および/またはカルボキシル基と反応・結合し、主として架橋構造を形成する。上述のように、偏光板は周囲の温度等の環境変化によって膨張や収縮する等変形し易い傾向がある。本発明の粘着剤組成物による粘着剤層は、カルボジイミド硬化剤を添加することにより、このような偏光板の変形に追随でき、環境変化にさらされても偏光板の浮きや剥れ、粘着剤層の発泡を防止することができる。
本発明の粘着剤組成物は、シランカップリング剤オリゴマーを必須の成分として含む。シランカップリング剤オリゴマーは、少なくともアルコキシ基を有するシラン化合物が2個以上縮合して−Si−O−Si−構造を形成し、そのケイ素原子には少なくとも1個のアルコキシ基が結合し、さらに、分子内に有機官能基を有する化合物である。
本発明の粘着剤組成物は、カルボジイミド硬化剤に加えて、さらにイソシアネート硬化剤を含んでもよい。本発明において架橋構造を形成する主たる成分はカルボジイミド硬化剤であるため、イソシアネート硬化剤は補助的な役割であるが、イソシアネート硬化剤を添加することにより、得られる粘着層のフィルムに対する基材密着性および架橋性が向上する。
本発明の感光性樹脂組成物は、必要に応じて他の添加剤を加えてもよい。添加剤としては、硬化促進剤、無機充填剤、軟化剤、酸化防止剤、老化防止剤、安定剤、粘着付与樹脂、改質樹脂(ポリオール樹脂、フェノール樹脂、アクリル樹脂、ポリエステル樹脂、ポリオレフィン樹脂、エポキシ樹脂、エポキシ化ポリブタジエン樹脂等)、レベリング剤、消泡剤、可塑剤、染料、顔料(着色顔料、体質顔料等)、処理剤、粘度調整剤、蛍光増白剤、分散剤、熱安定剤、光安定剤、帯電防止剤、滑剤および溶剤が挙げられる。
本発明の粘着剤組成物は、(メタ)アクリル共重合体、カルボジイミド硬化剤、シランカップリング剤オリゴマー、および必要に応じてイソシアネート硬化剤やその他の添加剤を添加し、攪拌・混合することにより得られる。特に、前記(メタ)アクリル共重合体を、溶液重合法を用いて得た場合には、(メタ)アクリル共重合体を単離・精製することなく、そのまま溶液の状態で粘着剤組成物の製造に用いることができ好適である。
本発明の粘着剤組成物は、種々の基材の貼り合わせに使用することができる。ここで使用できる基材としては、ガラス、プラスチックフィルム、紙または金属箔等が挙げられる。ガラスとしては、一般的な無機ガラスが挙げられる。プラスチックフィルムにおける、プラスチックとしては、例えばポリ塩化ビニル樹脂、ポリ塩化ビニリデン、セルロース系樹脂、アクリル系樹脂、シクロオレフィン系樹脂、非結晶性ポリオレフィン系樹脂、ポリエチレン、ポリプロピレン、ポリスチレン、ABS樹脂、ポリアミド、ポリエステル、ポリカーボネート、ポリウレタン、ポリビニルアルコール、エチレン−酢酸ビニル共重合体および塩素化ポリプロピレン等が挙げられる。非結晶性ポリオレフィン系樹脂は、通常、ノルボルネンや多環ノルボルネン系モノマーのような環状ポリオレフィンの重合単位を有するものであり、環状オレフィンと鎖状環状オレフィンとの共重合体であってもよい。市販されている非結晶性ポリオレフィン系樹脂として、JSR株式会社の商品名アートン、日本ゼオン株式会社のZEONEX(登録商標)、ZEONOR(登録商標)、三井化学株式会社のAPO、アペル(登録商標)などがある。非結晶性ポリオレフィン系樹脂を製膜してフィルムにするには、溶剤キャスト法、溶融押出法など、公知の方法が適宜用いられる。また、紙としては、模造紙、上質紙、クラフト紙、アートコート紙、キャスターコート紙、純白ロール紙、パーチメント紙、耐水紙、グラシン紙および段ボール紙等を挙げることができ。金属箔としては、例えばアルミニウム箔等を挙げることができる。
重合体溶液 約1gを、精秤したガラス皿に精秤する。105℃で1時間乾燥した後室温に戻し、ガラス皿と残存固形分との合計の質量を精秤する。ガラス皿の質量をX、乾燥する前のガラス皿とポリマー溶液との合計の質量をY、ガラス皿と残存固形分との合計の質量Zとして、下記数式1により固形分を算出した。
ガラス瓶に入れたポリマー溶液を25℃に温調し、ブルックフィールド社粘度計DV−II+Pro(スピンドルNo.63、回転数12rpm)により測定した。
還流器および攪拌機を備えたフラスコに、n−ブチルアクリレート(株式会社日本触媒製)98質量部、アクリル酸(株式会社日本触媒製)2質量部、および酢酸エチル150質量部を投入した。次いで、窒素置換を行いながら65℃まで加熱し、アゾビスイソブチロニトリル(AIBN)0.1質量部を加え、65℃を維持しつつ6時間重合を行った。重合反応終了後、酢酸エチル 83質量部を加えて希釈を行い、アクリル共重合体の溶液を得た。得られたアクリル共重合体溶液の固形分は28.0質量%、粘度は5.0Pa・s、アクリル共重合体の重量平均分子量は60万であった。
上記の粘着剤層付き偏光板を120mm(偏光板MD方向)×60mmに裁断し、ガラス基板(コーニングジャパン株式会社製イーグル2000、0.7mm厚)に貼り合せた。貼り合わせた試料は、50℃、0.49MPa(5kg/cm2)の条件で、20分間オートクレーブ処理を行った。その後、80℃の環境下で、120時間放置し、その後の外観を目視により観察した。下記表2中、評価結果は以下のように示した。
×:欠点あり(浮き、剥れ、発泡がある)
<耐湿熱性試験>
上記の粘着剤層付き偏光板を120mm(偏光板MD方向)×60mmに裁断し、ガラス板(コーニングジャパン株式会社製イーグル2000、0.7mm厚)に貼り合わせた。貼り合わせた試料は、50℃、0.49MPa(5kg/cm2)の条件で20分間オートクレーブ処理を行った。その後、60℃、90%RHの環境下で、120時間放置し、その後の外観を目視により観察した。下記表2中、評価結果は以下のように示した。
△:微欠点あり(わずかな浮き、剥れ、発泡がある)
×:欠点あり(浮き、剥れ、発泡がある)
<光漏れ試験>
上記の粘着剤層付き偏光板を、120mm(偏光板MD方向)×60mmに裁断した試料と、120mm×60mm(偏光板MD方向)に裁断した試料とを、ガラス基板(コーニングジャパン株式会社製イーグル2000、0.7mm厚)の各面に重なり合うように貼り合せた。貼り合わせた試料は、80℃の環境下で、120時間放置し、その後の外観を目視により観察した。下記表2中、評価結果は以下のように示した。
○:良好(光漏れがほとんどない)
×:欠点あり(光漏れがある)
<粘着力測定>
上記の粘着剤層付き偏光板を25mm幅に裁断した試料を、ガラス基板(コーニングジャパン株式会社製イーグル2000、0.7mm厚)に貼り合わせて、50℃、0.49MPa(5kg/cm2)で、20分間オートクレーブ処理を行った。その後、貼り合わせた試料を、引っ張り試験機を用いて、20℃、50%RHの環境下で、剥離角90度、剥離速度0.3m/minで、JIS Z0237(2000年)に記載の粘着テープ・粘着シート試験方法に準じて粘着力の測定を行った。また、同時に剥離状態の観察を行った。下記表2中、剥離状態の評価結果は下記のように示した。
×:ガラス表面に粘着剤起因の汚れあり
(実施例2)
還流器および攪拌機を備えたフラスコに、n−ブチルアクリレート(株式会社日本触媒製)98質量部、アクリル酸(株式会社日本触媒製)2質量部、および酢酸エチル125質量部を投入した。次いで、窒素置換を行いながら、65℃まで加熱し、アゾビスイソブチロニトリル(AIBN)0.05部を加え、65℃を維持しつつ6時間重合を行った。重合反応終了後、酢酸エチル 275部を加えて希釈を行い、アクリル共重合体の溶液を得た。得られたアクリル共重合体溶液の固形分は18.0質量%、粘度は7.0Pa・s、アクリル共重合体の重量平均分子量は120万であった。
還流器および攪拌機を備えたフラスコに、n−ブチルアクリレート(株式会社日本触媒製)98質量部、アクリル酸(株式会社日本触媒製)2質量部、および酢酸エチル115質量部を投入した。次いで、窒素置換を行いながら、65℃まで加熱し、アゾビスイソブチロニトリル(AIBN)0.04部を加え、65℃を維持しつつ6時間重合を行った。重合反応終了後、酢酸エチル 285部を加えて希釈を行い、アクリル共重合体の溶液を得た。得られたアクリル共重合体溶液の固形分は15.0%、粘度は6.0Pa・s、アクリル共重合体の重量平均分子量は160万であった。
還流器および攪拌機を備えたフラスコに、n−ブチルアクリレート(株式会社日本触媒製)98質量部、アクリル酸(株式会社日本触媒製)2質量部、および酢酸エチル100質量部を投入した。次いで、窒素置換を行いながら、65℃まで加熱し、アゾビスイソブチロニトリル(AIBN)0.04部を加え、65℃を維持しつつ6時間重合を行った。重合反応終了後、酢酸エチル 300部を加えて希釈を行い、アクリル共重合体の溶液を得た。得られたアクリル共重合体溶液の固形分は13.0%、粘度は5.0Pa・s、アクリル共重合体の重量平均分子量180万であった。
実施例5は実施例1と同様にして、実施例6〜8、11〜16は実施例2と同様にして、実施例9、10は実施例3と同様にして、後掲の表2〜4に示す配合量の材料を使用した以外は、本発明の粘着剤組成物および粘着剤層付き偏光板を製造し、評価を行った。評価結果は材料、配合量および物性等と併せて表2〜4に示す。
還流器および攪拌機を備えたフラスコに、n−ブチルアクリレート(株式会社日本触媒製)97.9質量部、アクリル酸(株式会社日本触媒製)2質量部、2−ヒドロキシエチルアクリレート0.1部および酢酸エチル140質量部を投入した。次いで、窒素置換を行いながら、65℃まで加熱し、アゾビスイソブチロニトリル(AIBN)0.1部を加え、65℃を維持しつつ6時間重合を行った。重合反応終了後、酢酸エチル 160部を加えて希釈を行い、アクリル共重合体の溶液を得た。得られたアクリル共重合体溶液の固形分は23.0質量%、粘度は8.0Pa・s、アクリル共重合体の重量平均分子量は100万であった。
還流器および攪拌機を備えたフラスコに、n−ブチルアクリレート(株式会社日本触媒製)97.9質量部、アクリル酸(株式会社日本触媒製)2質量部、2−ヒドロキシエチルアクリレート0.1部および酢酸エチル160質量部を投入した。次いで、窒素置換を行いながら、65℃まで加熱し、アゾビスイソブチロニトリル(AIBN)0.1部を加え、65℃を維持しつつ6時間重合を行った。重合反応終了後、酢酸エチル 140部を加えて希釈を行い、アクリル共重合体の溶液を得た。得られたアクリル共重合体溶液の固形分は22.8質量%、粘度は2.8Pa・s、アクリル共重合体の重量平均分子量は80万であった。
比較例1は実施例1と同様にして、比較例2、比較例4、5、比較例7〜10は実施例2と同様にして、比較例3、比較例6は実施例3と同様にして、後掲の表5または6に示す配合量の材料を使用した以外は、粘着剤組成物および粘着剤層付き偏光板を製造し、評価を行った。評価結果は材料、配合量および物性等と併せて表5または6に示す。
Claims (4)
- (1)92〜99.7質量部の(メタ)アクリル酸エステルモノマーと、0.3〜8質量部のカルボキシル基含有モノマーおよびヒドロキシ基含有(メタ)アクリル酸モノマーの少なくとも一方とからなり、重量平均分子量が500,000〜2,000,000である(メタ)アクリル共重合体100質量部;
(2)カルボジイミド硬化剤0.01〜1.0質量部;および
(3)シランカップリング剤オリゴマー0.02〜1.0質量部;
を含む粘着剤組成物。 - さらに、イソシアネート硬化剤0.05〜3.8質量部を含む請求項1に記載の粘着剤組成物。
- 前記(メタ)アクリル共重合体の重量平均分子量が600,000〜1,800,000である請求項1または2に記載の粘着剤組成物。
- 請求項1〜3のいずれか一項に記載の粘着剤組成物から形成される粘着層を備える光学部材。
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