JPWO2018182029A1 - 熱可塑性樹脂膜及びガラス板含有積層体 - Google Patents
熱可塑性樹脂膜及びガラス板含有積層体 Download PDFInfo
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Abstract
Description
上記樹脂膜は、熱可塑性樹脂を含む。上記熱可塑性樹脂としては、ポリビニルアセタール樹脂、エチレン−酢酸ビニル共重合体樹脂、エチレン−アクリル酸共重合体樹脂、ポリウレタン樹脂、ポリビニルアルコール樹脂、アイオノマー樹脂及びシクロオレフィン樹脂等が挙げられる。
樹脂膜の接着力を適度に高める観点から、上記樹脂膜は、可塑剤を含むことが好ましい。ポリビニルアセタール樹脂と可塑剤との併用により、ガラス板、合わせガラス部材又は他の樹脂膜等に対する本発明に係る樹脂膜の接着力がより一層高くなる。上記可塑剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。
変色を抑える観点から、上記樹脂膜は、染料を含み、該染料のモル体積が200cm3/mol以上であることが好ましい。上記樹脂膜に含まれる染料は、モル体積が200cm3/mol以上である染料を含むことが好ましい。
上記樹脂膜は、光安定剤を含むことが好ましい。光安定剤の使用により、樹脂膜が長期間使用されたり、太陽光に晒されたりしても、変色がより一層抑えられ、可視光線透過率がより一層低下し難くなる。また、光照射後の色むら、及び変色を抑える観点から、上記樹脂膜は、上記染料とともに、上記光安定剤を含むことが好ましい。上記光安定剤は1種のみが用いられてもよく、2種以上が併用されてもよい。
上記樹脂膜は、マグネシウム塩、アルカリ金属塩又はアルカリ土類金属塩(以下、これらを併せて金属塩Mと記載することがある)を含むことが好ましい。上記金属塩Mの使用により、ガラス板、合わせガラス部材又は他の樹脂膜等に対する本発明に係る樹脂膜の接着力を制御することがより一層容易になる。上記金属塩Mは、1種のみが用いられてもよく、2種以上が併用されてもよい。
上記樹脂膜は、紫外線遮蔽剤を含むことが好ましい。上記紫外線遮蔽剤の使用により、樹脂膜が長期間使用されたり、高温下で使用されたりしても、変色がより一層抑えられ、可視光線透過率がより一層低下し難くなる。上記紫外線遮蔽剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。
上記樹脂膜は、酸化防止剤を含むことが好ましい。上記酸化防止剤の使用により、樹脂膜が長期間使用されたり、高温下で使用されたりしても、変色がより一層抑えられ、可視光線透過率がより一層低下し難くなる。上記酸化防止剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。
上記樹脂膜は、必要に応じて、難燃剤、帯電防止剤、耐湿剤、蛍光増白剤及び赤外線吸収剤等の添加剤を含んでいてもよい。これらの添加剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。
ガラス板含有積層体の耐貫通性を効果的に高める観点からは、上記樹脂膜のガラス転移温度は、好ましくは10℃以上、より好ましくは15℃以上、更に好ましくは20℃以上、好ましくは45℃以下、より好ましくは40℃以下、更に好ましくは35℃以下である。
図1は、本発明の一実施形態に係る熱可塑性樹脂膜を用いたガラス板含有積層体の一例を示す断面図である。
ポリビニルブチラール樹脂(PVB(1))(ポリビニルアルコールの重合度1700、水酸基の含有率30モル%、アセチル化度1モル%、アセタール化度(ブチラール化度)69モル%)
トリエチレングリコールジ−2−エチルヘキサノエート(3GO)
アントラキノン系染料(1)(CASNo.14233−37−5、モル体積262cm3/mol)
アントラキノン系染料(2)(CASNo.13676−91−0、モル体積303cm3/mol)
アントラキノン系染料(3)(CASNo.17418−58−5、モル体積223cm3/mol)
アントラキノン系染料(4)(CASNo2475−44−7、モル体積477cm3/mol)
アミノケトン系染料(1)(CASNo.20749−68−2、モル体積246cm3/mol)
アントラキノン系染料(X)(CASNo.81−42−5、モル体積182cm3/mol)
インドール顔料(CASNo.5590−18−1)
Tinuvin765(BASF社製、N−C(アルキル基)型)
Tinuvin770(BASF社製、N−H(水素基)型)
Tinuvin123(BASF社製、N−O−R(アルコキシ基)型)
混合物(1)(酢酸マグネシウムと2−エチルヘキサン酸マグネシウムとの混合物)
Tinuvin326(BASF社製)
BHT(2,6−ジ−t−ブチル−p−クレゾール)
樹脂膜を形成するための組成物の作製:
PVB(1)に、3GOと、アントラキノン系染料(4)と、アントラキノン系染料(3)と、アントラキノン系染料(2)と、混合物(1)と、Tinuvin326と、BHTとを下記の表1に示す配合量となるように添加して、ミキシングロールで充分に混練し、組成物を得た。
樹脂膜を形成するための組成物を、押出機を用いて押出し、JIS B 0601:1994に準拠して測定される十点平均粗さRzが20μmとなるようにエンボスロールを用いて樹脂膜表面にエンボスを付与することにより、単層の樹脂膜(厚み780μm)を作製した。
得られた樹脂膜を、縦15cm×横15cmに切り出した。次に、JIS R3208に準拠した、厚み2mmの2枚のグリーンガラス(縦15cm×横15cm×厚み2mm)の間に樹脂膜を挟み込み、真空ラミネーターにて90℃で30分間保持し、真空プレスし、合わせガラスを得た。
組成物の配合成分の種類及び配合量を下記の表1〜3に示すように設定したこと以外は実施例1と同様にして、樹脂膜及び合わせガラスを得た。
(1)ガラス転移温度の測定
実施例及び比較例で得られた樹脂膜を、25℃及び相対湿度30%の条件で12時間放置した。12時間放置した後に、TA INSTRUMENTS社製のARES−G2を用いて、粘弾性を測定した。治具として、直径8mmのパラレルプレートを用いた。3℃/分の降温速度で100℃から−10℃まで温度を低下させる条件、及び周波数1Hz及び歪1%の条件で測定を行った。得られた測定結果において、損失正接のピーク温度をガラス転移温度Tg(℃)とした。
ヘーズメーター(東京電色社製「TC−HIIIDPK」)を用いて、JIS K6714に準拠して、得られた合わせガラスのヘーズ値を測定した。
JIS R3106:1998に準拠して、得られた合わせガラスの全光線透過率(TvD)を測定した。分光光度計(日立ハイテク社製「U−4100」)を用いて、透過した光線をすべて積分球に受光するよう積分球の開口部に、得られた合わせガラスを平行にかつ密着させ、分光透過率を測定した。得られた上記分光透過率から算出した可視光線透過率を、全光線透過率とした。
ゴムシート(硬度60、縦5cm、横5cm、厚み2mm)上に、より着色の少ない面がゴムシートと接するように実施例及び比較例で得られた樹脂膜(縦4cm、横4cm)を置いた。次に、色移り試験用ポリビニルブチラール樹脂膜(厚み760μm、縦4cm、横4cm、染料及び顔料は未使用)を用意した。上記色移り試験用ポリビニルブチラール樹脂膜の、JIS B 0601:1994に準拠して測定される表面の十点平均粗さRzは20μmである。上記色移り試験用ポリビニルブチラール樹脂膜は、ポリビニルブチラール樹脂(ポリビニルアルコールの重合度1700、水酸基の含有率30モル%、アセチル化度1モル%、ブチラール化度69モル%)100重量部及びトリエチレングリコールジ−2−エチルヘキサノエート(3GO)40重量部から構成される。実施例及び比較例で得られた樹脂膜上に色移り試験用ポリビニルブチラール樹脂膜、及び、グリーンガラス(JIS R3208に準拠、厚み2mm、縦4cm、横4cm)を載せて積層体を得た。得られた積層体のガラス板の上に、プレス機を用いて、200g/cm2の加重を均一にかけ、23℃及び湿度25%の条件で1週間放置した。放置後に、色移り試験用ポリビニルブチラール樹脂膜を取り出した。
○○:ΔEが4.3以下
○:ΔEが4.3を超え4.5以下
△:ΔEが4.5を超え7以下
×:ΔEが7を超える
実施例及び比較例で得られた縦15cm×横15cmの合わせガラスに対して、合わせガラスのどちらかの面を光源側とし、光源から230mmの距離に合わせガラスを設置した。さらに、合わせガラスの四辺のうち二辺が光に曝されるように、残る二辺が固定枠で光から隠れるように設置した。スガ試験機社製「H75」を用いて、ブラックパネル温度50℃、照射強度70W/m2(波長300nmから400nm)に設定し、ブラックパネル温度50℃にて、光を1000時間照射した。目視観察により色むらを以下の基準で判定した。なお、図3に、色むらが発生した合わせガラスを示した。
○○:光に曝された二辺の縁部と、縁部の内側の縁部から5mm〜25mmの範囲とで色調が同じであり、色むらが発生していない
○:光に曝された二辺の縁部と、縁部の内側の縁部から5mm〜25mmの範囲とで色調が異なり、かなり薄く色むらが発生している
△:光に曝された二辺の縁部と、縁部の内側の縁部から5mm〜25mmの範囲とで色調が異なり、薄く色むらが発生している
×:光に曝された二辺の縁部と、縁部の内側の縁部から5mm〜25mmの範囲とで色調が異なり、濃く色むらが発生している
実施例及び比較例で用いた染料のモル体積を、ソフトウェアHSPiP 4th Edition 4.1.07を用いて計算した。
染料に関しては熱可塑性樹脂膜を溶媒にて溶解後、HPLCで染料を分取し、分取した溶媒を除去した後、NMRやMALDI−TOF−MS、TOF−SIMS、LC−MS、GC―MS、IR、UV−Visスペクトル測定などを用いて同定した。顔料に関しては、熱可塑性樹脂膜から二酸化炭素による超臨界抽出や有機溶媒によるソックスレー抽出などをした後、抽出後の熱可塑性樹脂膜を熱分解GC、MALDI−TOF−MS、TOF−SIMS、LC−MS、GC―MS、TEM−EDS、NMRで分析した。他にも、上記ソックスレー抽出後の熱可塑性樹脂膜を溶媒にて溶解し、再沈殿法などで熱可塑性樹脂のみを取り出した後、沈殿に用いた溶媒を留去して得られた着色成分をXRD、NMR、MALDI−TOF−MS、TOF−SIMS、LC−MS、GC―MS、IR法、UV−Visスペクトル測定などを用いて同定した。顔料が複数存在する場合は、HPLCやGPCなどで分取した。同定後、定量方法として、HPLCのピーク面積を用いて検量線を作成し同定する方法や、UV−Visスペクトルを用いて検量線を作成する方法を使用した。
2…樹脂膜
2a…第1の表面
2b…第2の表面
11…ガラス板含有積層体(合わせガラス)
12…樹脂膜
13…第1の層(樹脂膜)
14…第2の層(樹脂膜)
15…第3の層(樹脂膜)
13a…外側の表面
15a…外側の表面
21…第1の合わせガラス部材(第1のガラス板)
22…第2の合わせガラス部材
Claims (17)
- 熱可塑性樹脂膜であって、
熱可塑性樹脂と、染料とを含み、
硬度60のゴムシート上に、前記熱可塑性樹脂膜、色移り試験用ポリビニルブチラール樹脂膜、及びJIS R3208に準拠した、厚み2mmのグリーンガラスをこの順に積層した積層体に、23℃及び湿度25%の条件で200g/cm2の加重を1週間かけた後に、JIS K8781−4:2013に準拠して、前記色移り試験用ポリビニルブチラール樹脂膜の加重前後の色調変化を測定した際の色差ΔEが4.3以下である、熱可塑性樹脂膜。 - 前記染料が、モル体積が200cm3/mol以上である染料を含む、請求項1記載の熱可塑性樹脂膜。
- 顔料を含む、請求項1又は2記載の熱可塑性樹脂膜。
- 前記熱可塑性樹脂がポリビニルアセタール樹脂である、請求項1〜3のいずれか1項に記載の熱可塑性樹脂膜。
- 前記染料として、アントラキノン系染料、アゾ系染料又はアミノケトン系染料を含む、請求項1〜4のいずれか1項に記載の熱可塑性樹脂膜。
- 光安定剤を含む、請求項1〜5のいずれか1項に記載の熱可塑性樹脂膜。
- 前記光安定剤が、ヒンダードアミン光安定剤である、請求項6に記載の熱可塑性樹脂膜。
- 前記ヒンダードアミン光安定剤が、ピペリジン構造の窒素原子にアルキル基又はアルコキシ基が結合しているヒンダードアミン光安定剤である、請求項7に記載の熱可塑性樹脂膜。
- 前記染料は、熱可塑性樹脂膜に含まれる全着色剤成分のうち、重量基準での含有量が4番目までに多い成分である、請求項1〜8のいずれか1項に記載の熱可塑性樹脂膜。
- JIS R3208に準拠した、厚み2mmの2枚のグリーンガラスの間に熱可塑性樹脂膜を挟み込んでガラス板含有積層体を得たときに、得られた前記ガラス板含有積層体のヘーズ値が3%以下である、請求項1〜9のいずれか1項に記載の熱可塑性樹脂膜。
- JIS R3208に準拠した、厚み2mmの2枚のグリーンガラスの間に熱可塑性樹脂膜を挟み込んでガラス板含有積層体を得たときに、得られた前記ガラス板含有積層体の全光線透過率が50%以下である、請求項1〜10のいずれか1項に記載の熱可塑性樹脂膜。
- ガラス転移温度が25℃以上40℃以下である、請求項1〜11のいずれか1項に記載の熱可塑性樹脂膜。
- 前記熱可塑性樹脂膜に含まれる染料全体での平均モル体積が280cm3/mol以上である、請求項1〜12のいずれか1項に記載の熱可塑性樹脂膜。
- 前記染料を3種以上含み、かつ顔料を1種以上含む、請求項1〜13のいずれか1項に記載の熱可塑性樹脂膜。
- ガラス板に貼り合わされて用いられる熱可塑性樹脂膜である、請求項1〜14のいずれか1項に記載の熱可塑性樹脂膜。
- 第1のガラス板と、
請求項1〜15のいずれか1項に記載の熱可塑性樹脂膜とを備え、
前記第1のガラス板に、前記熱可塑性樹脂膜が貼り合わされている、ガラス板含有積層体。 - 第1の合わせガラス部材として前記第1のガラス板と、
前記熱可塑性樹脂膜と、
第2の合わせガラス部材とを備え、
前記第1のガラス板に、前記熱可塑性樹脂膜が貼り合わされており、
前記第2の合わせガラス部材に、前記熱可塑性樹脂膜が貼り合わされており、
前記第1のガラス板と前記第2の合わせガラス部材との間に、前記熱可塑性樹脂膜が配置されている、請求項16に記載のガラス板含有積層体。
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WO2015046586A1 (ja) * | 2013-09-30 | 2015-04-02 | 積水化学工業株式会社 | 合わせガラス用中間膜及び合わせガラス |
WO2015147302A1 (ja) * | 2014-03-28 | 2015-10-01 | 積水化学工業株式会社 | 合わせガラス用中間膜及び合わせガラス |
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WO2018182029A1 (ja) | 2018-10-04 |
TWI757466B (zh) | 2022-03-11 |
US20200009837A1 (en) | 2020-01-09 |
CN109890776A (zh) | 2019-06-14 |
EP3604249A1 (en) | 2020-02-05 |
MX2019011439A (es) | 2019-11-18 |
CN109890776B (zh) | 2022-08-05 |
KR20190132981A (ko) | 2019-11-29 |
EP3604249A4 (en) | 2020-12-23 |
JP6974314B2 (ja) | 2021-12-01 |
TW201841863A (zh) | 2018-12-01 |
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