JP5976110B2 - 粘着剤組成物及びそれを用いた粘着テープ - Google Patents
粘着剤組成物及びそれを用いた粘着テープ Download PDFInfo
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- JP5976110B2 JP5976110B2 JP2014522283A JP2014522283A JP5976110B2 JP 5976110 B2 JP5976110 B2 JP 5976110B2 JP 2014522283 A JP2014522283 A JP 2014522283A JP 2014522283 A JP2014522283 A JP 2014522283A JP 5976110 B2 JP5976110 B2 JP 5976110B2
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- pressure
- sensitive adhesive
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- adhesive composition
- adhesive tape
- Prior art date
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
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- C08G18/622—Polymers of esters of alpha-beta ethylenically unsaturated carboxylic acids
- C08G18/6225—Polymers of esters of acrylic or methacrylic acid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
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Description
カルボキシル基含有モノマー(A2)3〜20質量%、
水酸基含有モノマー(A3)3〜20質量%、及び、
炭素原子数1〜3のアルキル基を有する(メタ)アクリル酸アルキルエステル(A4)3〜15質量%
を構成成分として含み、重量平均分子量が70万〜200万、理論Tgが−40℃以下である、ヒドロキシル基及びカルボキシル基を有するアクリル系共重合体(A)と、
架橋剤(B)と
を含有する粘着剤組成物であって、
カルボキシル基含有モノマー(A2)と水酸基含有モノマー(A3)の合計含有量が15質量%以上である粘着剤組成物である。
攪拌機、温度計、還流冷却器及び窒素ガス導入管を備えた反応装置に、表1に示す量(%)の成分(A1)〜(A4)と、酢酸エチル、連鎖移動剤としてn−ドデカンチオール及びラジカル重合開始剤としてラウリルパーオキサイド0.1部を仕込んだ。反応装置内に窒素ガスを封入し、攪拌しながら窒素ガス気流下で68℃、3時間、その後78℃、3時間で重合反応させた。その後、室温まで冷却し、酢酸エチルを添加した。これにより、固形分濃度30%のアクリル系共重合体(A)を得た。
表2に示す通り、製造例1〜17で得たアクリル系共重合体(A)の固形分100部に対して、架橋剤(B)としてイソシアネート系架橋剤(B1)又はエポキシ系架橋剤(B2)を加えて混合し、粘着剤組成物を調製した。
攪拌機、温度計、還流冷却器、UVランプ及び窒素ガス導入口を備えた反応容器に、表1に示す量(%)の成分(A1)〜(A4)と、連鎖移動剤としてn−ドデシルメルカプタン0.01部及び光重合開始剤(BASFジャパン社製、商品名ダロキュア1173)0.01部を添加し、窒素雰囲気下でUV光を照射してアクリルシロップを調製した。アクリルシロップ中のアクリルポリマー濃度は約13%、重量平均分子量は約150万であった。
製造例18で得たアクリルシロップ100部に対して、架橋剤(B)としてヘキサンジオールジアクリレート(新中村化学工業社製、商品名NKエステルA−HD−N)0.08部、追加の光重合開始剤(BASFジャパン社製、商品名ダロキュア1173)0.5部を添加して均一に撹拌した。撹拌混合時に混入した空気泡を脱泡操作により除去して、UV硬化型粘着剤組成物を調製した。
実施例1に記載の粘着剤組成物を、両面に約0.20mm厚のスキン層を有するPP発泡体(2.0mm厚)の両面に貼り合せた。そして23℃、50%Rhで7日間養生して、粘着テープを得た。
実施例1に記載の粘着剤組成物を、両面にスキン層を有しないPE発泡体の両面に貼り合せた。そして23℃、50%Rhで7日間養生して、粘着テープを得た。
実施例1に記載の粘着剤組成物を、両面にスキン層を有しないウレタンフォーム発泡体の両面に貼り合せた。そして23℃、50%Rhで7日間養生して、粘着テープを得た。
「2−EHA」:2−エチルヘキシルアクリレート、
「BA」:n−ブチルアクリレート、
「MA」:メチルアクリレート、
「AA」:アクリル酸、
「2−HEA」:2−ヒドロキシエチルアクリレート。
各実施例及び比較例で得た粘着テープを、以下の方法で評価した。結果を表3〜5に示す。
粘着テープを幅5mmで40mm×50mmの枠状に裁断し、一方の離型紙を剥離して2.0mm厚のガラス板に貼り合せ、更にもう一方の離型紙を剥離して2.0mm厚のガラス板を貼り合せた。このサンプルに対して、オートクレーブを用いて23℃で1時間の加圧処理(0.5Mpa)を行い、その後JIS IPX7(防水規格)に基づき一時的に水没させて、以下の基準で防水性を評価した。また、このサンプルに対して、オートクレーブを用いて23℃で1時間の加圧処理(0.1Mpa、0.25Mpa、0.5Mpa)を行い、その後JIS IPX8(防水規格)に基づき水深10cmの水中に沈め、以下の基準で防水性を評価した。
「○」:枠内に水が浸入しなかった。
「×」:枠内に水が浸入した。
粘着テープを幅5mmで40mm×50mmの枠状に裁断し、一方の離型紙を剥離して2.0mm厚のガラス板に貼り合せ、更にもう一方の離型紙を剥離して2.0mm厚のガラス板を貼り合せた。そして、オートクレーブを用いて23℃、0.5Mpa、1時間の加圧処理を行った。このサンプルを、人工皮脂(トリオレイン33.3%、オレイン酸20.0%、スクワレン13.3%、ミリスチルオクタドデシレート33.4%)又は人工汗油に1時間浸漬した。その後サンプルを取り出し、85℃、85%Rhの雰囲気下で72時間静置し、その後通常の雰囲気下に240時間放置した。そのサンプルを目視観察し、以下の基準で耐人工皮脂・人工肝油性を評価した。
「○」:テープの剥れ無し。
「×」:テープの剥れ有り。
粘着テープを25mm×25mmのサイズに裁断し、一方の離型紙を剥離した。そして図1示すように、フック2に粘着テープ1(基材1a、粘着層1b)を貼り合せ、次いでもう一方の離型紙を剥離し、被着体3に貼り合せた。この被着体3としては、SUS304、ポリカーボネート板、アクリル板、EGI鋼板、ガルバリウム鋼板、ガラス板を用いた。そしてフック2に1kgfの荷重(錘4)をかけ、85℃で60分間保持し、以下の基準で耐荷重性を評価した。
「○」:60分間フック2は落下しなかった。
「×」:60分以内にフック2が落下した。
粘着テープを5mm×125mmのサイズで10本に細断した状態のまま、65℃、80%Rh雰囲気下に1日放置した。そして1本毎に180°方向に離型紙ごと剥離し、隣接した部分との癒着を目視にて確認し、以下の基準で加工性を評価した。
「○」:隣接した部分との癒着がほとんど無く、隣接部分を剥すことなく剥離できた。
「×」:隣接した部分に著しい癒着があり、隣接部分が同時に剥れてしまった。
粘着テープを幅5mmで40mm×50mmの枠状に裁断し、一方の離型紙を剥離して、4mm厚のポリカーボネート板に貼り合せ、更にもう一方の剥離紙を剥離し、4mm厚のアクリル板に貼り合せ、20分間養生した。このサンプルを23℃、50%Rh下で、デュポン式衝撃試験機にて300gの錘を高さ600mmから落下させ、テープが剥離した時の落下させた回数を測定し、以下の基準で耐衝撃性を評価した。
「○」:テープが剥離した時に錘を落下させた回数が5回以上。
「×」:テープが剥離した時に錘を落下させた回数が5回未満。
175倍のマイクロスコープにて、基材である発泡体のスキン層の厚さを測定した。
粘着テープを25mm×25mmにサイズに裁断し、一方の離型紙を剥離した。そして図2示すように、フック2に粘着テープ1(基材1a、粘着層1b)を貼り合せ、次いでもう一方の離型紙を剥離し、被着体3に貼り合せた。そしてフック2を上方向に50mm/minの速度で引張り、発泡体が切れた時の強度[N/cm2]を測定した。
1a 基材
1b 粘着層
2 フック
3 被着体
4 錘
Claims (7)
- 炭素原子数が4〜12のアルキル基を有する(メタ)アクリル酸アルキルエステル(A1)50〜90質量%、
カルボキシル基含有モノマー(A2)3〜20質量%、
水酸基含有モノマー(A3)3〜20質量%、及び、
炭素原子数1〜3のアルキル基を有する(メタ)アクリル酸アルキルエステル(A4)3〜15質量%
を構成成分として含み、重量平均分子量が70万〜200万、理論Tgが−40℃以下である、ヒドロキシル基及びカルボキシル基を有するアクリル系共重合体(A)と、
架橋剤(B)と
を含有する粘着剤組成物であって、
カルボキシル基含有モノマー(A2)と水酸基含有モノマー(A3)の合計含有量が15質量%以上である粘着剤組成物。 - 架橋剤(B)が、少なくともイソシアネート系架橋剤(B1)を含む請求項1記載の粘着剤組成物。
- 架橋剤(B)が、少なくともエポキシ系架橋剤(B2)を含む請求項1又は2に記載の粘着剤組成物。
- 遮光性フィラー又は顔料を含む請求項1から3のいずれか1項に記載の粘着剤組成物。
- 基材の片面又は両面に、請求項1から4のいずれか1項に記載の粘着剤組成物から形成された粘着剤層を有する片面又は両面粘着テープ。
- 粘着剤層の厚さが5〜100μmである請求項5記載の片面又は両面粘着テープ。
- 基材が、両面にスキン層を有する発泡体であり、該スキン層の厚さは発泡体の全体厚に対して0.5%〜15%であり、かつ該発泡体の厚さ方向の割裂力が15N/cm2以上である請求項5又は6に記載の片面又は両面粘着テープ。
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