JP5071750B1 - ヒートシール剤、それを用いた積層体及び太陽電池モジュール - Google Patents
ヒートシール剤、それを用いた積層体及び太陽電池モジュール Download PDFInfo
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- JP5071750B1 JP5071750B1 JP2012526213A JP2012526213A JP5071750B1 JP 5071750 B1 JP5071750 B1 JP 5071750B1 JP 2012526213 A JP2012526213 A JP 2012526213A JP 2012526213 A JP2012526213 A JP 2012526213A JP 5071750 B1 JP5071750 B1 JP 5071750B1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
本発明は、水性ウレタン樹脂(A)、水性ポリオレフィン樹脂(B)、架橋剤(C)及び水性媒体(D)を含有し、前記架橋剤(C)がアルキル化メチロールメラミン樹脂(c1)とエポキシ化合物(c2)とを含有し、前記アルキル化メチロールメラミン樹脂(c1)が5質量%〜50質量%の範囲で含まれ、前記水性ウレタン樹脂(A)及び水性ポリオレフィン樹脂(B)のいずれか一方または両方が、エポキシ基と反応しうる官能基[X]を有し、かつ、前記官能基[X]の合計物質量に対する前記エポキシ化合物(c2)の有するエポキシ基の物質量の割合が5/1〜1/5であるヒートシール剤に関する。
【選択図】なし
Description
本発明では、前記架橋剤(C)として、前記アルキル化メチロールメラミン樹脂(c1)を必須成分として使用し、かつ、前記エポキシ化合物(c2)を、前記アルキル化メチロールメラミン樹脂(c1)と組み合わせ使用することが、優れた耐湿熱性と各種基材に対する優れた密着性とを両立したヒートシール剤を得るうえで重要である。
本発明で使用する水性媒体(D)として、例えば、水、水と混和する有機溶剤、及び、これらの混合物が挙げられる。水と混和する有機溶剤としては、例えば、メタノール、エタノール、n−及びイソプロパノール等のアルコール類;アセトン、メチルエチルケトン等のケトン類;エチレングリコール、ジエチレングリコール、プロピレングリコール等のポリアルキレングリコール類;ポリアルキレングリコールのアルキルエーテル類;N-メチル-2-ピロリドン等のラクタム類、等が挙げられる。本発明では、水のみを用いても良く、また水及び水と混和する有機溶剤との混合物を用いても良く、水と混和する有機溶剤のみを用いても良い。安全性や環境に対する負荷の点から、水のみ、又は、水及び水と混和する有機溶剤との混合物が好ましく、水のみが特に好ましい。
温度計、窒素ガス導入管、攪拌機を備えた反応器中で窒素ガスを導入しながら、テレフタル酸830質量部、イソフタル酸830質量部、エチレングリコール374質量部、ネオペンチルグリコール604質量部及びジブチル錫オキサイド0.5質量部を仕込み180〜230℃で5時間エステル化した後、酸価が1未満になるまで260℃で6時間重縮合反応することによって、酸価0.2、水酸基価74.5のポリエステルポリオール(a1’)を得た。
温度計、窒素ガス導入管、攪拌機を備えた反応器中で窒素ガスを導入しながら、ニッポラン980R(日本ポリウレタン工業(株)製、ポリカーボネートジオール、数平均分子量2,000)を1000質量部を混合し、80℃まで冷却した後、メチルエチルケトン671質量部を加え十分に攪拌し溶解させ、2,2’−ジメチロールプロピオン酸75質量部とヘキサメチレンジイソシアネート178質量部とを加えて75℃で8時間反応させた。
温度計、窒素ガス導入管、攪拌機を備えた反応器中で窒素ガスを導入しながら、ポレスターVS−1236(星光PMC株式会社製、無水マレイン酸変性ポリオレフィンの水分散体、重量平均分子量70000)を1000質量部入れ、80℃で3時間攪拌し溶融させ、次いで50℃まで冷却し、トリエチルアミン180質量部加えて中和した後、水2153質量部を加えて水溶化することにより、不揮発分30質量%の組成物(III)を得た。
調製例1で得た組成物(I)を100質量部と、調製例3で得た組成物(III)を44質量部と混合した。次いで、ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)を7質量部と、ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)を8質量部とを添加、攪拌し、水を加えることによって、不揮発分20質量%の水性樹脂組成物(X−1)からなるヒートシール剤(X−1)を得た。
調製例1で得た組成物(I)100質量部の代わりに、調製例2で得た組成物(II)を100質量部使用すること以外は、実施例1と同様の方法で水性樹脂組成物(X−2)からなるヒートシール剤(X−2)を得た。
ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)の使用量を7質量部から2質量部に変更すること以外は、実施例1と同様の方法で水性樹脂組成物(X−3)からなるヒートシール剤(X−3)を得た。
ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分80質量%)の使用量を8質量部を16質量部に変更すること以外は、実施例1と同様の方法で水性樹脂組成物(X−4)からなるヒートシール剤(X−4)を得た。
ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分80質量%)の使用量を8質量部から2質量部に変更すること以外は、実施例1と同様の方法で水性樹脂組成物(X−5)からなるヒートシール剤(X−5)を得た。
調製例1で得た組成物(I)72質量部と調製例3で得た組成物(III)72質量部とを混合及び攪拌し、次いで、ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)7質量部と、ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)10質量部とを添加、混合し、水を加えることによって、不揮発分20質量%の水性樹脂組成物(X−6)からなるヒートシール剤(X−6)を得た。
調製例1で得た組成物(I)100質量部の代わりに、調製例1で得た組成物(I)50質量部と調製例2で得た組成物(II)50質量部を使用すること以外は、実施例1と同様の方法で水性樹脂組成物(X−7)からなるヒートシール剤(X−7)を得た。
ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)7質量部の代わりに、ベッカミンJ−101(DIC株式会社製、ヘキサメトキシメチロール型メラミン樹脂、不揮発分80質量%)7質量部使用すること以外は、実施例1と同様の方法で水性樹脂組成物(X−8)からなるヒートシール剤(X−8)を得た。
ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)8質量部の代わりに、デナコールEX−321(ナガセケムテックス株式会社製、トリメチロールプロパンポリグリシジルエーテル、不揮発分100質量%)5質量部使用すること以外は、実施例1と同様の方法で水性樹脂組成物(X−9)からなるヒートシール剤(X‘−9)を得た。
調製例1で得た組成物(I)100質量部と、調製例3で得た組成物(III)44質量部とを混合、攪拌し、水を加えることによって、不揮発分20質量%の水性樹脂組成物(X’−1)からなるヒートシール剤(X’−1)を得た。
調製例1で得た組成物(I)100質量部と、調製例3で得た組成物(III)44質量部とを混合及び攪拌し、次いで、ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)8質量部と混合し、水を加えることによって、不揮発分20質量%の水性樹脂組成物(X’−2)からなるヒートシール剤(X’−2)を得た。
調製例1で得た組成物(I)100質量部に、調製例3で得た組成物(III)を44質量部混合及び攪拌し、次いで、ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)7質量部と混合し、水を加えることによって、不揮発分20質量%の水性樹脂組成物(X’−3)からなるヒートシール剤(X’−3)を得た。
調製例1で得られた組成物(I)144質量部と、ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)7質量部及びウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)3質量部とを混合、攪拌し、水を加えることによって、不揮発分20質量%の水性樹脂組成物(X’−4)からなるヒートシール剤(X’−4)を得た。
調製例3で得られた組成物(III)144質量部と、ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)7質量部及びウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)18質量部とを混合、攪拌し、水を加えることによって、不揮発分20質量%の水性樹脂組成物(X’−5)からなるヒートシール剤(X’−5)を得た。
ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基含有エポキシ樹脂、不揮発分100質量%)8質量部の代わりに、アクアネート210(日本ポリウレタン工業株式会社製、水分散性ポリイソシアネート架橋剤、不揮発分100質量%)を8質量部使用すること以外は、実施例1と同様の方法で水性樹脂組成物(X’−7)からなるヒートシール剤(X’−7)を得た。
ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)7質量の代わりに、アクアネート210(日本ポリウレタン工業株式会社製、水分散性ポリイソシアネート架橋剤、不揮発分100質量%)を8質量部使用すること以外は、実施例1と同様の方法で水性樹脂組成物(X’−8)からなるヒートシール剤(X’−8)を得た。
ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)8質量部の代わりに、ハイドランアシスターCS−7(DIC株式会社製、水分散性カルボジイミド化合物、不揮発分40質量%)を30質量部使用すること以外は、実施例1と同様の方法で水性樹脂組成物(X’−9)からなるヒートシール剤(X’−9)を得た。
ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)7質量部の代わりに、CR−5L(DIC株式会社製、水溶性エポキシ化合物、不揮発分100質量%)を5質量部と、ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)8質量部の代わりに、アクアネート210(日本ポリウレタン工業株式会社製、水分散性ポリイソシアネート架橋剤、不揮発分100質量%)を8質量部使用すること以外は、実施例1と同様の方法で水性樹脂組成物(X’−10)からなるヒートシール剤(X’−10)を得た。
ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)の使用量を7質量部から2質量部に変更すること以外は、実施例1と同様の方法で水性樹脂組成物(X’−11)からなるヒートシール剤(X’−11)を得た。
ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)の使用量を7質量部から23質量部に変更すること以外は、実施例1と同様の方法で水性樹脂組成物(X’−12)からなるヒートシール剤(X’−12)を得た。
ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)の使用量を8質量部から46質量部に変更すること以外は、実施例1と同様の方法で水性樹脂組成物(X’−12)からなるヒートシール剤(X’−12)を得た。
ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基を有するエポキシ化合物、不揮発分100質量%)の使用量を8質量部から1質量部に変更すること以外は、実施例1と同様の方法で水性樹脂組成物(X’−13)からなるヒートシール剤(X’−13)を得た。
極性基材であるポリエチレンテレフタレートフィルムの表面に、乾燥膜厚が5μmとなるよう、前記実施例及び比較例で得たヒートシール剤を塗布し、150℃の条件で5分間乾燥することによって、前記フィルム用面に架橋した樹脂硬化層(ヒートシール層)が設けられた積層体を得た。
前記方法で製造した直後の積層体の密着性は、引張り試験機(株式会社 島津製作所製オートグラフ)を用いT型剥離試験(1000Nセル)によって評価した。前記密着性は、ヒートシール層と、前記エチレン−酢酸ビニルからなるフィルムとの間の密着性に基づいて評価した。
前記で得た積層体を120℃×100%RHの条件に設定された恒温恒湿機内に72時間静置し湿熱試験を行った。前記静置後の積層体の密着力を、前記と同様の方法によって測定し評価した。
「M−3」;ベッカミンM−3(DIC株式会社製、トリメトキシメチロール型メラミン樹脂、不揮発分80質量%)
「WSA−950」;ウォーターゾールWSA-950(DIC株式会社製、加水分解性シリル基含有エポキシ樹脂、不揮発分100質量%)
「CR−5L」;CR−5L(DIC株式会社製、水溶性エポキシ化合物、不揮発分100質量%)
「アクアネート210」;アクアネート210(日本ポリウレタン工業株式会社製、水分散性ポリイソシアネート架橋剤、不揮発分100質量%)
「J−101」;ベッカミンJ−101(DIC株式会社製、ヘキサメトキシメチロール型メラミン樹脂、不揮発分80質量%)
「CS−7」;ハイドランアシスターCS−7(DIC株式会社製、水分散性カルボジイミド化合物、不揮発分40質量%)
「アルキル化メチロールメラミン樹脂(c1)の含有量[質量%]」;水性ウレタン樹脂及び水性ポリオレフィン樹脂の合計質量に対するアルキル化メチロールメラミン樹脂の質量割合を表す。
Claims (9)
- 水性ウレタン樹脂(A)、水性ポリオレフィン樹脂(B)、架橋剤(C)及び水性媒体(D)を含有するヒートシール剤であって、前記架橋剤(C)がアルキル化メチロールメラミン樹脂(c1)とエポキシ化合物(c2)とを含有し、前記アルキル化メチロールメラミン樹脂(c1)が、前記水性ウレタン樹脂(A)及び前記水性ポリオレフィン樹脂(B)の合計質量に対して5質量%〜50質量%の範囲で含まれ、前記水性ウレタン樹脂(A)及び水性ポリオレフィン樹脂(B)のいずれか一方または両方が、エポキシ基と反応しうる官能基[X]を有し、かつ、前記官能基[X]の合計物質量に対する前記エポキシ化合物(c2)の有するエポキシ基の物質量の割合〔エポキシ基の物質量/官能基[X]の合計物質量〕が5/1〜1/5であることを特徴とするヒートシール剤。
- 前記水性ウレタン樹脂(A)及び水性ポリオレフィン樹脂(B)のいずれか一方または両方が有する前記官能基[X]が、カルボキシル基、水酸基及びアミノ基からなる群より選ばれる1種以上である請求項1に記載のヒートシール剤。
- 前記水性ウレタン樹脂(A)が、芳香族環構造含有ポリエステルポリオール、及び、ポリカーボネートポリオールからなる群より選ばれる1種以上を含むポリオール(a1)と、ポリイソシアネート(a2)とを反応させることによって得られるものである請求項1に記載のヒートシール剤。
- 前記エポキシ化合物(c2)が、加水分解性シリル基を有するエポキシ化合物、または、トリメチロールプロパンポリグリシジルエーテル、または、グリセリントリグリシジルエーテルである請求項1に記載のヒートシール剤。
- 極性基材(I)の表面に、請求項1〜4のいずれか1項に記載のヒートシール剤を塗布し乾燥することによって形成されるヒートシール層を設け、前記ヒートシール層表面に非極性基材(II)を載置し、次いで80℃〜180℃で加熱することによって得られる積層体。
- 前記極性基材(I)がポリエチレンテレフタレート基材、ポリプロピレン基材、ポリカーボネート基材またはポリアミド基材であり、かつ、前記非極性基材(II)がエチレン−酢酸ビニル共重合体からなる基材である請求項5に記載の積層体。
- 極性基材(I)表面に、請求項1〜4のいずれか1項に記載のヒートシール剤を塗布し乾燥することによって、前記水性ウレタン樹脂(A)及び前記水性ポリオレフィン樹脂(B)のいずれか一方または両方が有する官能基[X]と、前記エポキシ化合物(c2)が有するエポキシ基とを反応させるとともに、
前記アルキル化メチロールメラミン樹脂(c1)の自己架橋反応、
及び/または、
前記官能基[X]と前記エポキシ化合物(c2)との反応によって生成した水酸基と前記アルキル化メチロールメラミン樹脂(c1)との反応
を進行させることによってヒートシール層を設け、次いで、前記ヒートシール層表面に非極性基材(II)を載置し、次いで80℃〜180℃で加熱することによって、前記極性基材(I)及び非極性基材(II)を接着することを特徴とする積層体の製造方法。 - 太陽電池を構成する受光面に対して反対側の、エチレン−酢酸ビニル共重合体からなる基材表面上に、請求項1〜4のいずれか1項に記載のヒートシール剤を用いて形成されるヒートシール層を有し、該ヒートシール層上に、ポリエチレンテレフタレート基材、ポリプロピレン基材、ポリカーボネート基材またはポリアミド基材からなるバックシート層を有することを特徴とする太陽電池モジュール。
- ポリエチレンテレフタレート基材、ポリプロピレン基材、ポリカーボネート基材またはポリアミド基材からなるシート表面に、請求項1〜4のいずれか1項に記載のヒートシール剤を用いて形成されるヒートシール層を備えた積層シートを、
太陽電池を構成する受光面に対して反対側の面を構成するエチレン−酢酸ビニル共重合体からなる基材表面に、
前記積層シートのヒートシール層と前記エチレン−酢酸ビニル共重合体からなる基材表面とが接触するように載置し、加熱することを特徴とする太陽電池モジュールの製造方法。
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- 2012-02-23 US US14/004,265 patent/US20130340816A1/en not_active Abandoned
- 2012-02-23 WO PCT/JP2012/054359 patent/WO2012124445A1/ja active Application Filing
- 2012-02-23 CN CN201280012825.4A patent/CN103429694B/zh active Active
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2014007119A1 (ja) * | 2012-07-04 | 2014-01-09 | Dic株式会社 | ヒートシール剤、それを用いた積層体及び太陽電池モジュール |
JP5522500B1 (ja) * | 2012-07-04 | 2014-06-18 | Dic株式会社 | ヒートシール剤、それを用いた積層体及び太陽電池モジュール |
KR20150030647A (ko) * | 2012-07-04 | 2015-03-20 | 디아이씨 가부시끼가이샤 | 히트 시일제, 그것을 사용한 적층체 및 태양 전지 모듈 |
KR102020257B1 (ko) | 2012-07-04 | 2019-09-10 | 디아이씨 가부시끼가이샤 | 히트 시일제, 그것을 사용한 적층체 및 태양 전지 모듈 |
KR20180006381A (ko) | 2015-05-15 | 2018-01-17 | 스미또모 가가꾸 가부시끼가이샤 | 수성 분산체 혼합물 |
US10344156B2 (en) | 2015-05-15 | 2019-07-09 | Sumitomo Chemical Company, Limited | Aqueous dispersion mixture |
Also Published As
Publication number | Publication date |
---|---|
EP2684931A4 (en) | 2014-09-03 |
KR101882291B1 (ko) | 2018-07-27 |
CN103429694A (zh) | 2013-12-04 |
JPWO2012124445A1 (ja) | 2014-07-17 |
WO2012124445A1 (ja) | 2012-09-20 |
EP2684931A1 (en) | 2014-01-15 |
TW201245329A (en) | 2012-11-16 |
KR20140012640A (ko) | 2014-02-03 |
TWI591124B (zh) | 2017-07-11 |
US20130340816A1 (en) | 2013-12-26 |
CN103429694B (zh) | 2016-05-18 |
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