JPWO2019151325A1 - 合わせガラス用中間膜、ロール体及び合わせガラス - Google Patents
合わせガラス用中間膜、ロール体及び合わせガラス Download PDFInfo
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- JPWO2019151325A1 JPWO2019151325A1 JP2019515566A JP2019515566A JPWO2019151325A1 JP WO2019151325 A1 JPWO2019151325 A1 JP WO2019151325A1 JP 2019515566 A JP2019515566 A JP 2019515566A JP 2019515566 A JP2019515566 A JP 2019515566A JP WO2019151325 A1 JPWO2019151325 A1 JP WO2019151325A1
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- interlayer film
- laminated glass
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Images
Classifications
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- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10761—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing vinyl acetal
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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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、1層又は2層以上の構造を有する。
上記第1の層は、ポリ酢酸ビニル(以下、ポリ酢酸ビニル(1)と記載することがある)を含む。上記第1の層中のポリ酢酸ビニル(1)は特に限定されない。上記ポリ酢酸ビニル(1)は、一般的に熱可塑性樹脂である。上記ポリ酢酸ビニル(1)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。上記第1の層(単層の中間膜を含む)は、可塑剤(以下、可塑剤(1)と記載することがある)を含むことが好ましい。上記第2の層は、可塑剤(以下、可塑剤(2)と記載することがある)を含むことが好ましい。上記第3の層は、可塑剤(以下、可塑剤(3)と記載することがある)を含むことが好ましい。可塑剤の使用により、またポリビニルアセタール樹脂と可塑剤との併用により、耐貫通性により一層優れ、ポリビニルアセタール樹脂と可塑剤とを含む層の合わせガラス部材又は他の層に対する接着力が適度に高くなる。上記可塑剤は特に限定されない。上記可塑剤(1)と上記可塑剤(2)と上記可塑剤(3)とは同一であってもよく、異なっていてもよい。上記可塑剤(1)、上記可塑剤(2)及び上記可塑剤(3)はそれぞれ、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。上記第1の層は、遮熱性物質を含んでいてもよい。上記第2の層は、遮熱性物質を含んでいてもよい。上記第3の層は、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。上記第1の層は、上記金属塩Mを含んでいてもよい。上記第2の層は、上記金属塩Mを含んでいてもよい。上記第3の層は、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。上記第1の層は、紫外線遮蔽剤を含んでいてもよい。上記第2の層は、紫外線遮蔽剤を含んでいてもよい。上記第3の層は、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。上記第1の層は、酸化防止剤を含んでいてもよい。上記第2の層は、酸化防止剤を含んでいてもよい。上記第3の層は、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、上記第1の層、上記第2の層及び上記第3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。
図3は、図1に示す合わせガラス用中間膜を用いた合わせガラスの一例を模式的に示す断面図である。
ポリ酢酸ビニル:
(合成例1)
還流冷却器、滴下漏斗、温度計及び窒素導入口を備えるガラス製重合容器を用意した。この重合容器内に、酢酸ビニルモノマー100重量部と、3−メチル−3−ブテン−1−オール(MB)1.0重量部と、メタノール3.8重量部とを入れ、加熱及び攪拌して重合容器内を窒素置換した。次に、上記重合容器内の温度を60℃にして、重合開始剤であるtert−ブチルパーオキシネオデカネート0.02重量部と、酢酸ビニルモノマー150重量部と、3−メチル−3−ブテン−1−オール(MB)1.5重量部とを、4時間かけて滴下し、滴下終了後1時間重合させて、ポリ酢酸ビニル(1)を含む溶液を得た。この溶液を110℃のオーブンで3時間乾燥させることにより、ポリ酢酸ビニル(1)を得た。ポリ酢酸ビニル(1)では、上記比(0.06ppm以上0.3ppm以下に存在する全ピークのピーク強度/4.5ppm以上5.3ppm以下に存在する全ピークの強度)(ピーク比)は、0.042であった。
(合成例2)
3−メチル−3−ブテン−1−オール(MB)を、エチレングリコールモノビニルエーテル(HEVE)に変更し、かつ酢酸ビニルモノマー及びエチレングリコールモノビニルエーテル(HEVE)の配合量を変更したこと以外は合成例1と同様にして、ポリ酢酸ビニル(2)を得た。ポリ酢酸ビニル(2)では、上記ピーク比は、0.037であった。
(合成例3)
3−メチル−3−ブテン−1−オール(MB)を、エチレングリコールモノビニルエーテル(HEVE)に変更し、かつ酢酸ビニルモノマー及びエチレングリコールモノビニルエーテル(HEVE)の配合量を変更したこと以外は合成例1と同様にして、ポリ酢酸ビニル(3)を得た。ポリ酢酸ビニル(3)では、上記ピーク比は、0.02であった。
(合成例4)
3−メチル−3−ブテン−1−オール(MB)を、エチレングリコールモノビニルエーテル(HEVE)に変更し、かつ酢酸ビニルモノマー及びエチレングリコールモノビニルエーテル(HEVE)の配合量を変更したこと以外は合成例1と同様にして、ポリ酢酸ビニル(4)を得た。ポリ酢酸ビニル(4)では、上記ピーク比は、2.8であった。
(合成例5)
3−メチル−3−ブテン−1−オール(MB)を、モノメチルイタコン酸に変更し、かつ酢酸ビニルモノマー及びモノメチルイタコン酸の配合量を変更したこと以外は合成例1と同様にして、ポリ酢酸ビニル(5)を得た。ポリ酢酸ビニル(5)では、上記ピーク比は、0.025であった。
(合成例X1)
還流冷却器、滴下ロート、温度計及び窒素導入口を備えるガラス製重合容器を用意した。この重合容器内に、酢酸ビニルモノマー250重量部と、メタノール3.8重量部とを入れ、加熱及び攪拌して重合容器内を窒素置換した。次に、上記重合容器内の温度を60℃にして、重合開始剤であるtert−ブチルパーオキシネオデカネート0.02重量部を2.5時間かけて滴下し、滴下終了後2時間重合させて、ポリ酢酸ビニル(X1)を含む溶液を得た。この溶液を110℃のオーブンで3時間乾燥させることにより、ポリ酢酸ビニル(X1)を得た。
(合成例X2)
還流冷却器、滴下漏斗、温度計及び窒素導入口を備えるガラス製重合容器を用意した。この重合容器内に、酢酸ビニルモノマー100重量部と、エチレングリコールモノビニルエーテル0.3重量部と、メタノール3.8重量部とを入れ、加熱及び攪拌して重合容器内を窒素置換した。次に、上記重合容器内の温度を60℃にして、重合開始剤であるtert−ブチルパーオキシネオデカネート0.02重量部と、酢酸ビニルモノマー150重量部と、3−メチル−3−ブテン−1−オール0.45重量部とを、4時間かけて滴下し、滴下終了後1時間重合させて、ポリ酢酸ビニル(X2)を含む溶液を得た。この溶液を110℃のオーブンで3時間乾燥させることにより、ポリ酢酸ビニル(X2)を得た。ポリ酢酸ビニル(X2)では、上記ピーク比は、0.01であった。
(合成例X3)
還流冷却器、滴下漏斗、温度計及び窒素導入口を備えるガラス製重合容器を用意した。この重合容器内に、酢酸ビニルモノマー100重量部と、エチレングリコールモノビニルエーテル40重量部と、メタノール3.8重量部とを入れ、加熱及び攪拌して重合容器内を窒素置換した。次に、上記重合容器内の温度を60℃にして、重合開始剤であるtert−ブチルパーオキシネオデカネート0.02重量部と、酢酸ビニルモノマー150重量部と、3−メチル−3−ブテン−1−オール(MB)60重量部とを、4時間かけて滴下し、滴下終了後1時間重合させて、ポリ酢酸ビニル(X3)を含む溶液を得た。この溶液を110℃のオーブンで3時間乾燥させることにより、ポリ酢酸ビニル(X3)を得た。ポリ酢酸ビニル(X3)では、上記ピーク比は、4.0であった。
ポリビニルアセタール樹脂(表1,2中、PVB)(n−ブチルアルデヒドを使用、重合度1700、水酸基の含有率32モル%、アセチル化度1モル%、アセタール化度67モル%)
D931(アジピン酸ビス(2−ブトキシエチル))
DBA(ジブチルアジペート)
3GO(トリエチレングリコールジ−2−エチルヘキサノエート)
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の層を形成するための組成物の作製:
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(D931)70重量部
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)
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)
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(D931)35重量部
得られる第2,第3の層中でMgが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により押出して、第2の層(厚み370μm)/第1の層(厚み100μm)/第3の層(厚み370μm)の構造を有する中間膜を得た。
得られた中間膜を縦30cm×横2.5cm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(クリアガラス、縦30cm×横2.5cm×厚さ2.5mm)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。
ポリ酢酸ビニル、ポリビニルアセタール樹脂及び可塑剤の種類と、これらの配合量とを下記の表1,2に示すように変更し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)1H−NMRの測定
ポリ酢酸ビニル100mgを少量のクロロホルムで膨潤させた後、トリメチルシリル化剤(N,O−ビス(トリメチルシリル)トリフルオロアセトアミド:BSTFA)を250μL加えて1時間振とう器で攪拌した。重クロロホルム溶媒を250μL添加し、さらに1時間振とう器で攪拌することで、TMS化ポリ酢酸ビニルを得た。
上記第1の層と上第2の層に共通して含まれる可塑剤と、上記第2の層中の上記熱可塑性樹脂(2)と、上記第1の層中の上記ポリ酢酸ビニル(1)との組み合わせについて、上記した曇点の評価を実施した。
第1の層を形成するための組成物を、コロナ処理を施したPETフィルム(厚さ70μm)上に塗布し、厚さ100μmの第1の層を形成し、第1の積層体を得た。
上記(3)の接着力の評価で得られた試験サンプルを用意した。この試験サンプルを180度にふたつ折りにして元に戻し、折り目の部分に剥離が生じているか否かを評価した。比較例1では1cmの剥離が生じたのに対して、実施例2では剥離が生じなかった。
得られた合わせガラスを室温(25℃)で2週間放置した。放置後の合わせガラスを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、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」)により解析した。
1a…第1の表面
1b…第2の表面
2…第2の層
2a…外側の表面
3…第3の層
3a…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
51…ロール体
61…巻き芯
Claims (16)
- 1層又は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、ポリ酢酸ビニルを含む第1の層を備え、
前記ポリ酢酸ビニルをN,O−ビス(トリメチルシリル)トリフルオロアセトアミドの存在下でトリメチルシリル化させた化合物のクロロホルム−d中での1H−NMRを測定したときに、トリメチルシリル基の水素ピークが0.06ppm以上0.3ppm以下に存在し、0.06ppm以上0.3ppm以下に存在する全ピークのピーク強度の、4.5ppm以上5.3ppm以下に存在する全ピークの強度に対する比が、0.02以上3以下を満足する、合わせガラス用中間膜。 - 前記ポリ酢酸ビニルの重量平均分子量が30万以上である、請求項1に記載の合わせガラス用中間膜。
- 前記第1の層が可塑剤を含む、請求項1又は2に記載の合わせガラス用中間膜。
- 前記第1の層中での前記ポリ酢酸ビニル100重量部に対する前記可塑剤の含有量が30重量部以上である、請求項3に記載の合わせガラス用中間膜。
- 前記中間膜は、第2の層を備え、
前記第1の層の第1の表面に、前記第2の層が積層されている、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。 - 前記第2の層が、熱可塑性樹脂を含む、請求項5に記載の合わせガラス用中間膜。
- 前記第2の層中の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6に記載の合わせガラス用中間膜。
- 前記第1の層が可塑剤を含み、
前記第2の層が可塑剤を含む、請求項6又は7に記載の合わせガラス用中間膜。 - 前記第2の層中の最も含有量が多い可塑剤と前記第1の層中の最も含有量が多い可塑剤が同一であり、
前記第2の層中の最も含有量が多い可塑剤と、前記第2の層中の前記熱可塑性樹脂と、前記第1の層中の最も含有量が多い可塑剤と、前記第1の層中の前記ポリ酢酸ビニルとの組み合わせは、以下の構成を満足する組み合わせである、請求項8に記載の合わせガラス用中間膜。
構成:前記第2の層中の前記可塑剤の中で最も含有量が多い可塑剤100重量部に前記第2の層中の前記熱可塑性樹脂8重量部を混合した液を用いて測定される曇点は、前記第1の層中の前記可塑剤の中で最も含有量が多い可塑剤100重量部に前記第1の層中の前記ポリ酢酸ビニル8重量部を混合した液を用いて測定される曇点よりも30℃以上高い - 前記中間膜は、第3の層を備え、
前記第1の層の前記第1の表面とは反対の第2の表面に、前記第3の層が積層されている、請求項5〜9のいずれか1項に記載の合わせガラス用中間膜。 - 前記第3の層が、熱可塑性樹脂を含む、請求項10に記載の合わせガラス用中間膜。
- 前記第3の層中の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11に記載の合わせガラス用中間膜。
- 前記第1の層が可塑剤を含み、
前記第2の層が可塑剤を含み、
前記第3の層が可塑剤を含む、請求項10〜12のいずれか1項に記載の合わせガラス用中間膜。 - 前記第2の層が熱可塑性樹脂を含み、
前記第3の層が熱可塑性樹脂を含み、
前記第1の層中での前記ポリ酢酸ビニル100重量部に対する前記可塑剤の含有量が、前記第2の層中での前記熱可塑性樹脂100重量部に対する前記可塑剤の含有量よりも多く、
前記第1の層中での前記ポリ酢酸ビニル100重量部に対する前記可塑剤の含有量が、前記第3の層中での前記熱可塑性樹脂100重量部に対する前記可塑剤の含有量よりも多い、請求項13に記載の合わせガラス用中間膜。 - 巻き芯と、
請求項1〜14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、
前記合わせガラス用中間膜が、前記巻き芯の外周に巻かれている、ロール体。 - 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1〜14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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