JPWO2019151329A1 - 合わせガラス用中間膜及び合わせガラス - Google Patents
合わせガラス用中間膜及び合わせガラス Download PDFInfo
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- JPWO2019151329A1 JPWO2019151329A1 JP2019516005A JP2019516005A JPWO2019151329A1 JP WO2019151329 A1 JPWO2019151329 A1 JP WO2019151329A1 JP 2019516005 A JP2019516005 A JP 2019516005A JP 2019516005 A JP2019516005 A JP 2019516005A JP WO2019151329 A1 JPWO2019151329 A1 JP WO2019151329A1
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Abstract
Description
本発明に係る合わせガラス用中間膜(以下、中間膜と記載することがある)は、2層以上の構造を有する。
上記中間膜は、樹脂層を備える。
上記中間膜は、粘着付与樹脂を含むことが好ましい。上記硬化物を含む層は、粘着付与樹脂を含むことが好ましい。上記樹脂を含む層は、粘着付与樹脂を含むことが好ましい。上記第1の層は、粘着付与樹脂を含むことが好ましい。上記粘着付与樹脂は、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。
上記中間膜は、可塑剤を含むことが好ましい。遮音性を効果的に高める観点からは、上記樹脂層は、可塑剤を含むことが好ましい。上記樹脂を含む層は、可塑剤を含むことが好ましい。上記第1,第2,第3,第4,第5の層はそれぞれ、可塑剤を含むことが好ましい。可塑剤の使用により、各層間の接着力がより一層高くなる傾向がある。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。
上記中間膜は、遮熱性物質を含んでいてもよい。上記樹脂層は、遮熱性物質を含んでいてもよい。上記樹脂を含む層は、遮熱性物質を含んでいてもよい。上記第1,第2,第3,第4,第5の層はそれぞれ、遮熱性物質を含んでいてもよい。上記遮熱性物質は、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。
上記中間膜は、アルカリ金属塩、アルカリ土類金属塩及びマグネシウム塩の内の少なくとも1種の金属塩(以下、金属塩Mと記載することがある)を含んでいてもよい。上記硬化物を含む層は、上記金属塩Mを含んでいてもよい。上記樹脂を含む層は、上記金属塩Mを含んでいてもよい。上記第1,第2,第3,第4,第5の層はそれぞれ、上記金属塩Mを含んでいてもよい。上記金属塩Mの使用により、中間膜とガラス板などの合わせガラス部材との接着性又は中間膜における各層間の接着性を制御することが容易になる。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。
上記中間膜は、紫外線遮蔽剤を含んでいてもよい。上記硬化物を含む層は、紫外線遮蔽剤を含んでいてもよい。上記樹脂を含む層は、紫外線遮蔽剤を含んでいてもよい。上記第1,第2,第3,第4,第5の層はそれぞれ、紫外線遮蔽剤を含んでいてもよい。紫外線遮蔽剤の使用により、中間膜及び合わせガラスが長期間使用されても、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。
上記中間膜は、酸化防止剤を含んでいてもよい。上記樹脂層は、酸化防止剤を含んでいてもよい。上記樹脂を含む層は、酸化防止剤を含んでいてもよい。上記第1,第2,第3,第4,第5の層はそれぞれ、酸化防止剤を含んでいてもよい。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。
上記中間膜、上記樹脂層、上記樹脂を含む層、上記第1,第2,第3,第4,第5の層はそれぞれ、必要に応じて、カップリング剤、分散剤、界面活性剤、難燃剤、帯電防止剤、顔料、染料、金属塩以外の接着力調整剤、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。
上記中間膜の厚みは特に限定されない。実用面の観点、並びに合わせガラスの耐貫通性及び曲げ剛性を充分に高める観点からは、中間膜の厚みは、好ましくは0.1mm以上、より好ましくは0.25mm以上、好ましくは3mm以下、より好ましくは1.5mm以下である。中間膜の厚みが上記下限以上であると、合わせガラスの耐貫通性及び曲げ剛性がより一層高くなる。中間膜の厚みが上記上限以下であると、中間膜の透明性がより一層良好になる。
本発明に係る合わせガラスは、第1の合わせガラス部材と、第2の合わせガラス部材と、上述した合わせガラス用中間膜とを備える。本発明に係る合わせガラスでは、上記第1の合わせガラス部材と上記第2の合わせガラス部材との間に、上記合わせガラス用中間膜が配置されている。
ポリビニルアセタール樹脂(1)(n−ブチルアルデヒドを使用、重合度1700、水酸基の含有率30.4モル%、アセチル化度0.9モル%、アセタール化度68.7モル%)
ポリビニルアセタール樹脂(A)(n−ブチルアルデヒドを使用、重合度3000、水酸基の含有率24.3モル%、アセチル化度12.5モル%、アセタール化度63.2モル%)
PETフィルム(1)(東洋紡社製「東洋紡エステルフィルム E5100」、厚み50μm)
PETフィルム(2)(東レ社製「ルミラー T60」、厚み50μm)
脂肪族ポリオレフィン(三井化学社製「アブソートマーEP−1001」;熱可塑性エラストマー)
下記の表1に示す配合組成を有する重合性組成物を、2枚の片面離型処理されたPETシート(ニッパ社製、厚み50μm)に挟み込むようにして、厚み100μmとなるように重合性組成物層を形成した。なお、2枚のPETシートの周囲にスペーサを配置した。ケミカルランプ(FL20SBL、東芝社製)を用いて、照射量3000mJ/cm2で紫外線を重合性組成物層に照射することにより、重合性組成物を反応により硬化させて、(メタ)アクリル重合体(1)〜(5)を得た。
トリエチレングリコールジ−2−エチルヘキサノエート(3GO)
パラフィンオイル(出光興産社製「ダイアナプロセスオイルPW−32」)
Mg混合物(2−エチル酪酸マグネシウムと酢酸マグネシウムとの50:50(重量比)混合物)
Tinuvin326(2−(2’−ヒドロキシ−3’−t−ブチル−5−メチルフェニル)−5−クロロベンゾトリアゾール、BASF社製「Tinuvin326」)
BHT(2,6−ジ−t−ブチル−p−クレゾール)
第1の層の作製:
上記で得られた(メタ)アクリル重合体(1)100重量部と可塑剤(3GO)25重量部とを含む第1の層(硬化物を含む層、厚み100μm)を用意した。
第2,第3の層として、PETフィルム(1)を用意した。
以下の配合成分を混合し、ミキシングロールで充分に混練し、第4,第5の層を形成するための組成物を得た。
可塑剤(3GO)35重量部
得られる第4,第5の層中で70ppmとなる量の金属塩M(Mg混合物)
得られる第4,第5の層中で0.2重量%となる量の紫外線遮蔽剤(Tinuvin326)
得られる第4,第5の層中で0.2重量%となる量の酸化防止剤(BHT)
第1の層を第2の層と第3の層とで挟み込んで、3層積層体を得た。この積層体の外側に第4の層及び第5の層を配置して、ロールラミネーター(アコ・ブランズ・ジャパン社製「GDRB316 A3」)を用いて、100℃及び速度設定3でラミネートすることにより、第4の層/第2の層/第1の層/第3の層/第5の層の構造を有する中間膜を得た。
得られた中間膜を幅25mm及び長さ300mmの大きさに切断した。第1の合わせガラス部材及び第2の合わせガラス部材として、2つのガラス板(クリアフロートガラス、幅25mm、長さ300mm及び厚さ2mm)を用意した。2枚のガラス板の間に、中間膜を挟み込み、積層体を得た。この積層体をゴムバック内に入れ、2.6kPaの真空度で20分間脱気した後、脱気したままオーブン内に移し、更に90℃で30分間保持して真空プレスし、積層体を予備圧着した。オートクレーブ中で135℃及び圧力1.2MPaの条件で、予備圧着された積層体を20分間圧着し、合わせガラスを得た。
遮音性評価用の中間膜と同様にして、3層積層体を得た。次に、3層積層体と第4の層と第5の層とを縦30cm×横15cmの大きさに切断した。切断された第4の層及び第5の層において、第4の層及び第5の層の端部から縦方向にそれぞれ内側に向かって8cmの位置と、第4の層及び第5の層の端部から横方向にそれぞれ内側に向かって5cmの位置との交点4箇所に、直径6mmの貫通孔を作製した。なお、第4の層及び第5の層の両面にはエンボスが形成されており、そのエンボスの十点平均粗さは30μmであった。得られた中間膜は温度23℃の環境下にて、10時間保管した。
遮音性評価用の中間膜と同様にして、3層積層体を得た。得られた3層積層体の外側に第4の層及び第5の層を積層し、第4の層/第2の層/第1の層/第3の層/第5の層の構造を有する中間膜を得た。この中間膜を透明なフロートガラス(縦30cm×横15cm×厚さ2.5mm)2枚の間に挟み込み、積層体を得た。積層体の外周縁を、熱融着により端部から幅2cmをシール剤により封止することにより、エンボスに残留した空気及び貫通孔に残留した空気を封じ込めた。この積層体をオートクレーブ中で135℃及び圧力1.2MPaの条件で、20分間圧着することで、残留した空気を中間膜中に溶かし込み、発泡試験に用いる合わせガラスを得た。
配合成分の種類及び配合量を下記の表2に示すように設定したこと、かつ厚みを下記の表2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、中間膜を作製した。なお、第4,第5の層には、実施例1と同様の種類及び配合量で、金属塩M、紫外線遮蔽剤及び酸化防止剤を配合した(表2では省略)。
第1の層の作製:
上記で得られた(メタ)アクリル重合体(2)(硬化物を含む層、厚み100μm)を用意した。
以下の配合成分を混合し、ミキシングロールで充分に混練し、第2,第3の層を形成するための組成物を得た。
可塑剤(3GO)35重量部
得られる第2,第3の層中で70ppmとなる量の金属塩M(Mg混合物)
得られる第2,第3の層中で0.2重量%となる量の紫外線遮蔽剤(Tinuvin326)
得られる第2,第3の層中で0.2重量%となる量の酸化防止剤(BHT)
第1の層の外側に第2の層及び第3の層を配置して、ロールラミネーター(アコ・ブランズ・ジャパン社製「GDRB316 A3」)を用いて、100℃及び速度設定3でラミネートすることにより、第2の層/第1の層/第3の層の構造を有する中間膜を得た。
得られた中間膜を用いたこと以外は実施例1と同様にして、合わせガラスを得た。
実施例1の3層積層体の代わりに得られた第1の層を用い、第4の層及び第5の層の代わりに得られた第2の層及び第3の層を用いたこと以外は実施例1と同様にして、中間膜を得た。
実施例1の3層積層体の代わりに得られた第1の層を用い、第4の層及び第5の層の代わりに得られた第2の層及び第3の層を用いたこと以外は実施例1と同様にして、合わせガラスを得た。
第2の層/第1の層/第3の層の3層積層体の作製:
第2,第3の層として、PETフィルム(2)を用意した。
実施例1と同様の第4,第5の層を形成するための組成物を用意した。
実施例1と同様にして、第4の層/第2の層/第1の層/第3の層/第5の層の構造を有する中間膜を得た。
得られた中間膜を用いたこと以外は実施例1と同様にして、合わせガラスを得た。
得られた3層積層体と用意した第4の層と第5の層を用いたこと実施例1と同様にして中間膜を作製し、得られた中間膜を用いたこと以外は実施例1と同様にして、合わせガラスを得た。
第1の層の作製:
上記で得られた(メタ)アクリル重合体(4)(硬化物を含む層、厚み100μm)を用意した。以下の配合成分を酢酸エチルに溶解して混合した後、乾燥後に厚み100μmとなるように塗工し、100℃オーブンで30分乾燥して酢酸エチルをとばし、第1の層を形成するための組成物を得た。
可塑剤(3GO)50重量部
以下の配合成分を混合し、ミキシングロールで充分に混練し、第2,第3の層を形成するための組成物を得た。
可塑剤(3GO)30重量部
得られる第2,第3の層中で70ppmとなる量の金属塩M(Mg混合物)
得られる第2,第3の層中で0.2重量%となる量の紫外線遮蔽剤(Tinuvin326)
得られる第2,第3の層中で0.2重量%となる量の酸化防止剤(BHT)
実施例4と同様にして、第2の層/第1の層/第3の層の構造を有する中間膜を得た。
得られた中間膜を用いたこと以外は実施例4と同様にして、合わせガラスを得た。
実施例4と同様にして、中間膜を得た。
実施例4と同様にして、合わせガラスを得た。
第1の層の作製:
上記で得られた(メタ)アクリル重合体(5)(硬化物を含む層、厚み100μm)を用意した。以下の配合成分を混合し、ミキシングロールで充分に混練し、第1の層を形成するための組成物を得た。
可塑剤(3GO)45重量部
以下の配合成分を混合し、ミキシングロールで充分に混練し、第2,第3の層を形成するための組成物を得た。
可塑剤(3GO)32重量部
得られる第2,第3の層中で70ppmとなる量の金属塩M(Mg混合物)
得られる第2,第3の層中で0.2重量%となる量の紫外線遮蔽剤(Tinuvin326)
得られる第2,第3の層中で0.2重量%となる量の酸化防止剤(BHT)
実施例4と同様にして、第2の層/第1の層/第3の層の構造を有する中間膜を得た。
得られた中間膜を用いたこと以外は実施例4と同様にして、合わせガラスを得た。
実施例4と同様にして、中間膜を得た。
実施例4と同様にして、合わせガラスを得た。
配合成分の種類及び配合量を下記の表3に示すように設定したこと、かつ厚みを下記の表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、中間膜を作製した。なお、第4,第5の層には、実施例1と同様の種類及び配合量で、金属塩M、紫外線遮蔽剤及び酸化防止剤を配合した(表3では省略)。
第1の層の作製:
ポリビニルアセタール樹脂(A)100重量部と、可塑剤(3GO)75重量部と、得られる第1の層中で0.2重量%となる量の紫外線遮蔽剤(Tinuvin326)と、得られる第1の層中で0.2重量%となる量の酸化防止剤(BHT)とを混合し、ミキシングロールで充分に混練し、第1の層を形成するための組成物を得た。
以下の配合成分を混合し、ミキシングロールで充分に混練し、第2,第3の層を形成するための組成物を得た。
可塑剤(3GO)37.5重量部
得られる第2,第3の層中で70ppmとなる量の金属塩M(Mg混合物)
得られる第2,第3の層中で0.2重量%となる量の紫外線遮蔽剤(Tinuvin326)
得られる第2,第3の層中で0.2重量%となる量の酸化防止剤(BHT)
得られた第1の層を形成するための組成物と、得られた第2,第3の層を形成するための組成物とを、共押出機を用いて共押出して、第2の層/第1の層/第3の層の構造を有する中間膜を得た。
得られた中間膜を用いたこと以外は実施例1と同様にして、合わせガラスを得た。
(1)動的粘弾性測定
遮音性評価用の中間膜を作製するのと同様にして第1の層を作製した。この第1の層を任意に切断し、重ね合わせることによって、厚みが0.5mmの試験片を用意した。この試験片を用いて、粘弾性測定を行った。第1の層が熱可塑性樹脂層である場合は、得られた組成物をプレス成型機でプレス成型して、厚さが0.5mmの試験片を作成してもよい。得られた試験片を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インスツルメント社製「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−20℃まで温度を低下させる条件、並びに周波数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。得られた測定結果から、Tgにおける損失正接tanδの値と、−5℃での貯蔵弾性率G’の値とを読み取った。
得られた合わせガラスは室温23±2℃、湿度25±5%の環境下で保管した。オートクレーブ完了から1ヶ月後に、得られた合わせガラスを20℃の恒温槽内でダンピング試験用の振動発生機(振研社製「加振機G21−005D」)により加振した。そこから得られた振動特性を機械インピーダンス測定装置(リオン社製「XG−81」)にて増幅した。振動スペクトルをFFTスペクトラムアナライザー(リオン社製「FFTアナライザー SA−01A2」)により解析し、共振周波数と損失係数を測定した。
○○:一次損失係数が0.25以上である温度範囲が、10℃〜30℃の温度領域中の20℃の温度範囲
○:一次損失係数が0.25以上である温度範囲が、10℃〜30℃の温度領域中の15℃以上20℃未満の温度範囲
×:一次損失係数が0.25以上である温度範囲が、10℃〜30℃の温度領域中の15℃未満の温度範囲
発泡試験に用いる合わせガラス10枚を、50℃のオーブン内に100時間放置した。放置後の合わせガラスにおいて、発泡の有無を下記の判定基準で判定した。
○:目視で発泡が観察された合わせガラスが10枚中0枚である
△:目視で発泡が観察された合わせガラスが10枚中1枚以上9枚以下である
×:目視で発泡が観察された合わせガラスが10枚中10枚である
BzA:アクリル酸ベンジル(大阪有機化学工業社製、ビスコート#160)
THF−A:テトラヒドロフルフリルアクリレート(大阪有機化学工業社製、ビスコート#150)
HPA:ヒドロキシプロピルアクリレート(大阪有機化学工業社製)
CTFA(♯200):環状トリメチロールプロパンホルマールアクリレート(大阪有機化学工業社製、ビスコート#200)
IBOA:イソボルニルアクリレート(日本触媒社製)
4HBA:4−ヒドロキシブチルアクリレート(大阪有機化学工業社製)
IRGACURE 184:2,2−ジメトキシ−1,2−ジフェニルエタン−1−オン(BASF社製)
1a…第1の表面
1b…第2の表面
2,2A…第2の層
2a…外側の表面
3,3A…第3の層
3a…外側の表面
4A…第4の層
4a…外側の表面
5A…第5の層
5a…外側の表面
11,11A…中間膜
11a…第1の表面
11b…第2の表面
21…第1の合わせガラス部材
22…第2の合わせガラス部材
31,31A…合わせガラス
Claims (12)
- 2層以上の構造を有する合わせガラス用中間膜であり、
前記中間膜は、樹脂層を備え、
前記樹脂層のガラス転移温度が−10℃以上0℃以下であり、前記樹脂層のガラス転移温度でのtanδが2.5以上であり、
前記樹脂層の−5℃での貯蔵弾性率G’が3.0×104Pa以上5.0×106Pa以下である、合わせガラス用中間膜。 - 前記樹脂層が、硬化物又はポリオレフィン樹脂を含む層であり、
前記硬化物が、光硬化性化合物又は湿気硬化性化合物を硬化させた硬化物である、請求項1に記載の合わせガラス用中間膜。 - 前記硬化物が、光硬化性化合物を硬化させた硬化物である、請求項2に記載の合わせガラス用中間膜。
- 2層以上の構造を有する合わせガラス用中間膜であり、
前記中間膜は、樹脂層を備え、
前記樹脂層が、硬化物又はポリオレフィン樹脂を含む層であり、
前記硬化物が、(メタ)アクリロイル基を有する硬化性化合物を硬化させた硬化物であり、
前記硬化物又はポリオレフィン樹脂を含む層のガラス転移温度が−10℃以上0℃以下であり、前記硬化物又はポリオレフィン樹脂を含む層のガラス転移温度でのtanδが2.5以上であり、
前記硬化物又はポリオレフィン樹脂を含む層の−5℃での貯蔵弾性率G’が3.0×104Pa以上2.0×106Pa以下である、合わせガラス用中間膜。 - 前記樹脂層が、可塑剤を含む、請求項1〜4のいずれか1項に記載の合わせガラス用中間膜。
- 前記樹脂層は、前記中間膜における表面層ではない層である、請求項1〜5のいずれか1項に記載の合わせガラス用中間膜。
- 前記硬化物及び前記ポリオレフィン樹脂の双方とは異なる樹脂を含む層を備える、請求項2〜4のいずれか1項に記載の合わせガラス用中間膜。
- 前記硬化物及び前記ポリオレフィン樹脂の双方とは異なる樹脂を含む層として、ポリエステル樹脂を含む層を備える、請求項7に記載の合わせガラス用中間膜。
- 前記硬化物及び前記ポリオレフィン樹脂の双方とは異なる樹脂を含む層として、ポリビニルアセタール樹脂を含む層を備える、請求項2〜4のいずれか1項に記載の合わせガラス用中間膜。
- 前記硬化物及び前記ポリオレフィン樹脂の双方とは異なる樹脂を含む層として、ポリエステル樹脂を含む層と、ポリビニルアセタール樹脂を含む層とを備える、請求項9に記載の合わせガラス用中間膜。
- 前記硬化物又はポリオレフィン樹脂を含む層中の前記硬化物100重量部又は前記ポリオレフィン樹脂100重量部に対する可塑剤の含有量は、前記ポリビニルアセタール樹脂を含む層中の前記ポリビニルアセタール樹脂100重量部に対する可塑剤の含有量よりも少ない、請求項9又は10に記載の合わせガラス用中間膜。
- 第1の合わせガラス部材と、
第2の合わせガラス部材と、
請求項1〜11のいずれか1項に記載の合わせガラス用中間膜とを備え、
前記第1の合わせガラス部材と前記第2の合わせガラス部材との間に、前記合わせガラス用中間膜が配置されている、合わせガラス。
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