JP2015120819A - 樹脂組成物、2液型ラミネート用接着剤、積層フィルム及び太陽電池のバックシート - Google Patents
樹脂組成物、2液型ラミネート用接着剤、積層フィルム及び太陽電池のバックシート Download PDFInfo
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- JP2015120819A JP2015120819A JP2013265260A JP2013265260A JP2015120819A JP 2015120819 A JP2015120819 A JP 2015120819A JP 2013265260 A JP2013265260 A JP 2013265260A JP 2013265260 A JP2013265260 A JP 2013265260A JP 2015120819 A JP2015120819 A JP 2015120819A
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- Prior art keywords
- resin composition
- acid
- polyester polyurethane
- resin
- polyurethane polyol
- Prior art date
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E10/50—Photovoltaic [PV] energy
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Abstract
【解決手段】 分子内に分岐構造を有し、重量平均分子量が80,000〜150,000の範囲であり、かつ分子量分布が5.0〜30.0であるポリエステルポリウレタンポリオール(A)と、水酸基含有エポキシ樹脂(B)と、水酸基含有ポリカーボネート樹脂(C)と、粘着付与剤と、脂肪族ポリイソシアネートとを含有し、且つ前記ポリエステルポリウレタンポリオール(A)100質量部に対する前記粘着付与剤の配合比率が10〜30質量部であることを特徴とする樹脂組成物、これからなる接着剤、及び当該接着剤層を有する積層フィルムと太陽電池のバックシート。
【選択図】 なし
Description
カラム ;東ソー株式会社製 TSK−GUARDCOLUMN SuperHZ−L
+東ソー株式会社製 TSK−GEL SuperHZM−M×4
検出器 ;RI(示差屈折計)
データ処理;東ソー株式会社製 マルチステーションGPC−8020modelII
測定条件 ;カラム温度 40℃
溶媒 テトラヒドロフラン
流速 0.35ml/分
標準 ;単分散ポリスチレン
試料 ;樹脂固形分換算で0.2質量%のテトラヒドロフラン溶液をマイクロフィルターでろ過したもの(100μl)
カラム ;東ソー株式会社製 TSK−GUARDCOLUMN SuperHZ−L
+東ソー株式会社製 TSK−GEL SuperHZM−M×4
検出器 ;RI(示差屈折計)
データ処理;東ソー株式会社製 マルチステーションGPC−8020modelII
測定条件 ;カラム温度 40℃
溶媒 テトラヒドロフラン
流速 0.35ml/分
標準 ;単分散ポリスチレン
試料 ;樹脂固形分換算で0.2質量%のテトラヒドロフラン溶液をマイクロフィルターでろ過したもの(100μl)
攪拌棒、温度センサー、精留管を有するフラスコに、ネオペンチルグリコール641部、イソフタル酸417部、無水フタル酸194部、セバシン酸302部、無水トリメリット酸11部及び有機チタン化合物0.7部を仕込み、乾燥窒素をフラスコ内にフローさせ攪拌しながら230〜250℃に加熱しエステル化反応を行った。酸価が1.0mgKOH/g以下となったところで反応を停止し、100℃まで冷却後、酢酸エチルで固形分80%に希釈した。次いで、有機錫化合物を0.2部仕込み、ヘキサメチレンジイソシアヌレートのイソシアヌレート変性体(スミジュール N−3300;住化バイエルウレタン株式会社製)79部、ヘキサメチレンジイソシアネート29部を仕込み、乾燥窒素をフラスコ内にフローさせ攪拌しながら70〜80℃に加熱しウレタン化反応を行った。イソシアネート含有率0.03%以下となったところで反応を停止し、数平均分子量が11000、重量平均分子量103000、水酸基価10.0のポリエステルポリウレタンポリオールを得た。これに酢酸エチルとイソプロピルアルコールの混合溶剤を仕込み、希釈して得られた固形分50%の樹脂溶液をポリエステルポリウレタンポリオール(A1)の溶液とする。
攪拌棒、温度センサー、精留管を有するフラスコに、ネオペンチルグリコール311質量部、イソフタル酸215質量部、無水フタル酸99.7質量部、セバシン酸156質量部、無水トリメリット酸5.8質量部及びエステル化触媒として有機チタン化合物0.2質量部を仕込み、乾燥窒素をフラスコ内にフローさせ攪拌しながら230〜250℃に加熱しエステル化反応を行った。酸価が1.0mgKOH/g以下となったところで反応を停止し、100℃まで冷却後、酢酸エチルで固形分80%に希釈した。次いで、ヘキサメチレンジイソシアヌレートのイソシアヌレート変性体(住友バイエルウレタン株式会社製「スミジュールN3300」)10質量部、ヘキサメチレンジイソシアネート14質量部を仕込み、乾燥窒素をフラスコ内にフローさせ攪拌しながら70〜80℃に加熱しウレタン化反応を行った。イソシアネート含有率0.03%以下となったところで反応を停止し、数平均分子量が4600、重量平均分子量33000、水酸基価14.8のポリエステルポリウレタンポリオールを得た。これに酢酸エチルとイソプロピルアルコールの混合溶剤を仕込み、希釈して得られた固形分50%の樹脂溶液をポリエステルポリウレタンポリオール(a1)の溶液とする。
・エポキシ樹脂(B1):数平均分子量(Mn)470、エポキシ当量245g/eqのビスフェノールA型エポキシ樹脂(DIC株式会社製「EPICLON 860」)
・ポリカーボネートポリオール(C1):数平均分子量(Mn)1,000、水酸基価110mgKOH/gのポリカーボネートジオール(ダイセル化学社製「プラクセルCD210」)
前記合成例1及び2で得たポリエステルポリウレタンポリオール100質量部(固形分)、前記エポキシ樹脂(B1)、前記ポリカーボネートポリオール(C1)及び前記粘着付与剤およびポリイソシアネートを、表1〜2の配合比率で混合して樹脂組成物を得、下記の要領で評価サンプルを作成し、以下に示す方法で評価を行った。結果を表1〜2に示す。
125μm厚のPETフィルム(東レ株式会社製「X10S」)を基材とし、上記の各接着剤組成物を5〜6g/m2(乾燥質量)に塗装して、貼合用フィルムとして25μm厚のフッ素フィルム(旭硝子(株)アフレックス25PW)を用い、評価サンプルを得た。評価サンプルは、50℃、72時間、エージングした後、評価に供した。
前記した評価サンプルにて、フッ素フィルム側よりラミネート外観を目視評価。
○:フィルム表面が平滑
フィルム表面に若干のクレーターが存在
×:フィルム表面に多数のクレーター(凹み)が存在
前記した評価サンプルにて、引っ張り試験機(SHIMADZU社製;AGS500NG)で、剥離速度スピード300mm/minでの強度(N/15mm、T型剥離)を接着力として評価した。初期(エージング後)、及び、121℃℃100%環境下の25時間、50時間、75時間暴露後の接着力を測定した。
初期の接着力に対する121℃100%75時間後の接着力の保持率を、○:60%以上、△:60〜40%、×:40%未満として評価した。
Claims (12)
- 分子内に分岐構造を有し、重量平均分子量(Mw)が80,000〜150,000の範囲であり、かつ、分子量分布(Mw/Mn)が5.0〜30.0であるポリエステルポリウレタンポリオール(A)と、数平均分子量(Mn)が300〜5,000の範囲である水酸基含有エポキシ樹脂(B)と、数平均分子量(Mn)が300〜2,000の範囲である水酸基含有ポリカーボネート樹脂(C)と、粘着付与剤と、脂肪族ポリイソシアネートと、を必須の成分として含有し、且つ前記ポリエステルポリウレタンポリオール(A)100質量部に対する前記粘着付与剤の配合比率が10〜30質量部であることを特徴とする樹脂組成物。
- 前記ポリエステルポリウレタンポリオール(A)が、3官能以上のポリイソシアネート化合物(G2)を必須の成分として反応させて得られるものである請求項1記載の樹脂組成物。
- 前記ポリエステルポリウレタンポリオール(A)が、多塩基酸(E)と、多価アルコール(F)と、3官能以上のポリイソシアネート化合物(G2)とを必須の成分として反応させて得られるものである請求項1記載の樹脂組成物。
- 前記多価アルコール(F)が、ネオペンチルグリコールを50モル%以上で含有するものである請求項3記載の樹脂組成物。
- 前記ポリエステルポリウレタンポリオール(A)が、ジイソシアネート化合物(G1)と3官能以上のポリイソシアネート化合物(G2)とを、両者の質量比[(G1)/(G2)]が50/50〜5/95となる範囲で含有するポリイソシアネート(G)を必須の成分として反応させて得られるポリエステルポリウレタンポリオールである請求項1記載の樹脂組成物。
- 前記ポリエステルポリウレタンポリオール(A)の水酸基価が、5〜30mgKOH/gの範囲であり、且つ酸価が2.0以下である請求項1記載の樹脂組成物。
- 前記ポリエステルポリウレタンポリオール(A)100質量部に対し、前記エポキシ樹脂(B)を5〜20質量部の範囲で含有し、かつ、前記ポリカーボネート樹脂(C)を5〜20質量部の範囲で含有する請求項1記載の樹脂組成物。
- 前記ポリエステルポリウレタンポリオール(A)、前記エポキシ樹脂(B)及び前記ポリカーボネート樹脂(C)に含まれる水酸基の合計モル数[OH]と、前記ポリイソシアネートに含まれるイソシアネート基のモル数[NCO]との比[OH]/[NCO]が1/1〜1/2の範囲である請求項1記載の樹脂組成物。
- 前記粘着付与剤が、軟化点が80〜160℃のロジン系樹脂である請求項1記載の樹脂組成物。
- 請求項1〜9のいずれか1つに記載の樹脂組成物を含有する2液型ラミネート用接着剤。
- ポリエステルフィルム、フッ素フィルム、ポリオレフィンフィルム、金属箔からなる群から選ばれる1種類以上のフィルムと、請求項10記載の接着剤からなる接着層とを有する積層フィルム。
- 請求項10記載の接着剤からなる接着層を有する太陽電池のバックシート。
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JP7306380B2 (ja) | 2018-04-12 | 2023-07-11 | 東洋紡エムシー株式会社 | 耐候性接着剤組成物 |
WO2022208813A1 (ja) * | 2021-03-31 | 2022-10-06 | 株式会社寺岡製作所 | 樹脂組成物、接着剤層及び接着シート、並びに接着シートの製造方法 |
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