JP7060515B2 - 樹脂膜及びガラス板含有積層体 - Google Patents
樹脂膜及びガラス板含有積層体 Download PDFInfo
- Publication number
- JP7060515B2 JP7060515B2 JP2018546712A JP2018546712A JP7060515B2 JP 7060515 B2 JP7060515 B2 JP 7060515B2 JP 2018546712 A JP2018546712 A JP 2018546712A JP 2018546712 A JP2018546712 A JP 2018546712A JP 7060515 B2 JP7060515 B2 JP 7060515B2
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- Prior art keywords
- layer
- resin film
- resin
- weight
- glass plate
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Description
本発明に係る樹脂膜は、1層の構造又は2層以上の構造を有する。
上記樹脂膜は、熱可塑性樹脂、又は、光硬化性化合物もしくは湿気硬化性化合物を硬化させた硬化物である樹脂成分を含む。上記樹脂膜は、テルペンフェノール樹脂とは異なる樹脂として、上記樹脂成分(熱可塑性樹脂、又は、光硬化性化合物もしくは湿気硬化性化合物を硬化させた硬化物)を含む。上記第1の層(単層の樹脂膜を含む)は、上記樹脂成分(以下、樹脂成分(1)と記載することがある)を含む。
上記樹脂膜は、可塑剤を含むことが好ましい。上記第1の層(単層の樹脂膜を含む)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。
上記樹脂膜は、テルペンフェノール樹脂を含む。上記第1の層(単層の樹脂膜を含む)は、テルペンフェノール樹脂を含む。上記テルペンフェノール樹脂は、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。
上記樹脂膜は、遮熱性物質(遮熱性化合物)を含むことが好ましい。上記第1の層(単層の樹脂膜を含む)は、遮熱性物質を含むことが好ましい。上記第2の層は、遮熱性物質を含むことが好ましい。上記第3の層は、遮熱性物質を含むことが好ましい。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。
上記樹脂膜は、フタロシアニン化合物、ナフタロシアニン化合物又はアントラシアニン化合物である成分Xを含むことが好ましい。上記第1の層(単層の樹脂膜を含む)は、上記成分Xを含むことが好ましい。上記第2の層は、上記成分Xを含むことが好ましい。上記第3の層は、上記成分Xを含むことが好ましい。上記成分Xは遮熱性物質である。上記成分X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、遮熱粒子を含むことが好ましい。上記第1の層(単層の樹脂膜を含む)は、上記遮熱粒子を含むことが好ましい。上記第2の層は、上記遮熱粒子を含むことが好ましい。上記第3の層は、上記遮熱粒子を含むことが好ましい。上記遮熱粒子は遮熱性物質である。遮熱粒子の使用により、赤外線(熱線)を効果的に遮断できる。上記遮熱粒子は、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、アルカリ金属塩、アルカリ土類金属塩又はマグネシウム塩(以下、これらを金属塩Mと記載することがある)を含むことが好ましい。上記第1の層(単層の樹脂膜を含む)は、上記金属塩Mを含むことが好ましい。上記第2の層は、上記金属塩Mを含むことが好ましい。上記第3の層は、上記金属塩Mを含むことが好ましい。上記金属塩Mの使用により、樹脂膜と合わせガラス部材との接着性又は樹脂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。
上記樹脂膜は、紫外線遮蔽剤を含むことが好ましい。上記第1の層(単層の樹脂膜を含む)は、紫外線遮蔽剤を含むことが好ましい。上記第2の層は、紫外線遮蔽剤を含むことが好ましい。上記第3の層は、紫外線遮蔽剤を含むことが好ましい。紫外線遮蔽剤の使用により、樹脂膜及びガラス板含有積層体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。
上記樹脂膜は、酸化防止剤を含むことが好ましい。上記第1の層(単層の樹脂膜を含む)は、酸化防止剤を含むことが好ましい。上記第2の層は、酸化防止剤を含むことが好ましい。上記第3の層は、酸化防止剤を含むことが好ましい。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。
上記樹脂膜、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、他の成分を含んでいてもよい。上記他の成分としては、ケイ素、アルミニウム又はチタンを含むカップリング剤、分散剤、界面活性剤、難燃剤、帯電防止剤、フィラー、顔料、染料、接着力調整剤、耐湿剤、蛍光増白剤及び赤外線吸収剤等が挙げられる。上記他の成分は、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、ガラス板に貼り合わされて用いられる樹脂膜であることが好ましい。
図3は、図1に示す樹脂膜を用いたガラス板含有積層体の一例を模式的に示す断面図である。
樹脂膜(第1の層)を形成するための組成物の作製:
以下の成分を配合し、樹脂膜を形成するための組成物を得た。
トリエチレングリコールジ-2-エチルヘキサノエート(3GO)50重量部
テルペンフェノール樹脂(ヤスハラケミカル社製「N125」)40重量部
得られる樹脂膜中で金属元素濃度(Mg濃度)が70ppmとなる量の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)
得られる樹脂膜中で0.2重量%となる量の紫外線遮蔽剤(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)
得られる樹脂膜中で0.2重量%となる量の酸化防止剤(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を、押出機を用いて押出しすることにより、樹脂膜(厚み800μm)を作製した。
得られた樹脂膜を縦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、樹脂膜を挟み込み、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。
以下の変更をしたこと以外は参考例1と同様にして、樹脂膜及び合わせガラスを得た。
3GOの配合量を60重量部に変更
テルペンフェノール樹脂40重量部を、テルペンフェノール樹脂(ヤスハラケミカル社製「G125」)50重量部に変更
以下の変更をしたこと以外は参考例1と同様にして、樹脂膜及び合わせガラスを得た。
3GOの配合量を70重量部に変更
テルペンフェノール樹脂40重量部を、テルペンフェノール樹脂(ヤスハラケミカル社製「ポリスターNH」)70重量部に変更
以下の変更をしたこと以外は参考例1と同様にして、樹脂膜及び合わせガラスを得た。
テルペンフェノール樹脂40重量部を、ロジン樹脂(荒川化学社製「D160」)70重量部に変更
以下の変更をしたこと以外は参考例1と同様にして、樹脂膜及び合わせガラスを得た。
3GOの配合量を60重量部に変更
テルペンフェノール樹脂40重量部を、ロジン樹脂(荒川化学社製「D125」)50重量部に変更
以下の変更をしたこと以外は参考例1と同様にして、樹脂膜及び合わせガラスを得た。
3GOの配合量を70重量部に変更
テルペンフェノール樹脂40重量部を、配合しないように変更
ポリ酢酸ビニルの作製:
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(HEVE)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、エチレングリコールモノビニルエーテル(HEVE)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、ポリ酢酸ビニルを得た。ポリ酢酸ビニルでは、HEVEに由来する構造単位の割合は、0.2モル%であった。ポリ酢酸ビニルの重量平均分子量は699000であった。
3GO50重量部を、アジピン酸ビス(2-ブトキシエチル)(D931)40重量部に変更
テルペンフェノール樹脂40重量部を、テルペンフェノール樹脂(ヤスハラケミカル社製「ポリスターNH」)30重量部に変更
(メタ)アクリロイル重合体の作製:
還流冷却器、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。この重合容器内に以下の成分を入れ、加熱及び攪拌して重合容器内を窒素置換した。
ポリオキシエチレンスチレン化プロペニルフェニルエーテル硫酸エステルアンモニウム(第一工業製薬社製「AR-30」)0.1重量部
エチレンオキサイド・プロピレンオキサイド共重合体(明成化学工業社製「EP-10」)0.005重量部
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)(BzA)5重量部
(2ーメチル-2-エチル-1,3-ジオキソラン-4-イル)メチルアクリレート(大阪有機化学工業社製)(MEDOL-10)10重量部
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)(HPA)15重量部
イソボルニルアクリレート(日本触媒社製、IBOA)70重量部
3GOの配合量を40重量部に変更
テルペンフェノール樹脂40重量部を、テルペンフェノール樹脂(ヤスハラケミカル社製「ポリスターNH」)20重量部に変更
(1)遮音性(低温側のtanδのピークの最大値)
得られた樹脂膜を直径8mmの円形に切り抜いた。この樹脂膜について、粘弾性装置(レオメトリックス社製「ARES」)を用いてせん断法にて、ひずみ1%及び周波数1Hzの条件で、昇温速度5℃/分で動的粘弾性測定を行った。最も低温側に現れる損失正接の最大値(極大値)を測定した。
得られた合わせガラスについて、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、ヘーズ値を測定した。
第1の層を形成するための組成物:
参考例1で得られた第1の層を形成するための組成物を用意した。
以下の成分を配合し、第2の層及び第3の層を形成するための組成物を得た。
トリエチレングリコールジ-2-エチルヘキサノエート(3GO)37.5重量部
得られる樹脂膜中で金属元素濃度(Mg濃度)が70ppmとなる量の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)
得られる樹脂膜中で0.2重量%となる量の紫外線遮蔽剤(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)
得られる樹脂膜中で0.2重量%となる量の酸化防止剤(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と、第2の層及び第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することにより、第2の層(厚み350μm)/第1の層(厚み100μm)/第3の層(厚み350μm)の積層構造を有する樹脂膜(厚み800μm)を作製した。
以下の変更をしたこと以外は実施例6と同様にして、樹脂膜及び合わせガラスを得た。
実施例8:第1の層を形成するための組成物を、参考例3で得られた第1の層を形成するための組成物に変更。第2,3の層を形成するための組成物におけるポリビニルアセタール樹脂の種類及び可塑剤の配合量を表2に示すように変更。第2,3の層の厚みを表2に示すように変更。
実施例9:第1の層を形成するための組成物を、参考例4で得られた第1の層を形成するための組成物に変更。第2,3の層を形成するための組成物におけるポリビニルアセタール樹脂の種類及び可塑剤の種類、配合量を表2に示すように変更。第2,3の層の厚みを表2に示すように変更。
実施例10:第1の層を形成するための組成物を、参考例5で得られた第1の層を形成するための組成物に変更。第2,3の層を形成するための組成物におけるポリビニルアセタール樹脂の種類及び可塑剤の配合量を表2に示すように変更。第2,3の層の厚みを表2に示すように変更。
比較例4:第1の層を形成するための組成物を、比較例1で得られた第1の層を形成するための組成物に変更。
比較例5:第1の層を形成するための組成物を、比較例2で得られた第1の層を形成するための組成物に変更。
比較例6:第1の層を形成するための組成物を、比較例3で得られた第1の層を形成するための組成物に変更。第2,3の層を形成するための組成物におけるポリビニルアセタール樹脂の種類及び可塑剤の配合量を表2に示すように変更。第2,3の層の厚みを表2に示すように変更。
多層の樹脂膜について、単層の樹脂膜と同様の評価を行った。実施例6~10の樹脂膜は、参考例1~5と同様の組成を有する第1の層を備える。このため、実施例6~10の樹脂膜は、比較例4~6の樹脂膜と比べて、遮音性及び透明性に優れていた。
実施例7~10及び比較例6で得られた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…樹脂膜
11A…樹脂膜(第1の層)
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…ガラス板含有積層体
31A…ガラス板含有積層体
Claims (8)
- 2層以上の構造を有する樹脂膜であって、
熱可塑性樹脂、又は、光硬化性化合物もしくは湿気硬化性化合物を硬化させた硬化物である樹脂成分と、テルペンフェノール樹脂とを含む第1の層を備え、
熱可塑性樹脂と、可塑剤とを含む第2の層を備え、
前記第2の層は、前記第1の層の第1の表面側に配置されており、
自動車用、鉄道車両用、航空機用、船舶用又は建築物用のガラス板含有積層体を得るためにガラス板に貼り合わされて用いられる、樹脂膜。 - 前記第1の層中の前記樹脂成分が、ポリビニルアセタール樹脂、ポリ酢酸ビニル、又は(メタ)アクリロイル重合体である、請求項1に記載の樹脂膜。
- 前記第1の層が、前記ポリビニルアセタール樹脂又は前記ポリ酢酸ビニルを含む場合に、前記第1の層が可塑剤を含む、請求項2に記載の樹脂膜。
- 前記テルペンフェノール樹脂の水酸基価が、50mgKOH/g以上200mgKOH/g以下である、請求項1~3のいずれか1項に記載の樹脂膜。
- 前記第1の層において、前記樹脂成分100重量部に対して、前記テルペンフェノール樹脂の含有量が10重量部以上150重量部以下である、請求項1~4のいずれか1項に記載の樹脂膜。
- 熱可塑性樹脂と、可塑剤とを含む第3の層を備え、
前記第3の層は、前記第1の層の前記第1の表面とは反対の第2の表面側に配置されている、請求項1~5のいずれか1項に記載の樹脂膜。 - 自動車用、鉄道車両用、航空機用、船舶用又は建築物用のガラス板含有積層体であって、
第1のガラス板と、
請求項1~6のいずれか1項に記載の樹脂膜とを備え、
前記第1のガラス板に、前記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、前記樹脂膜が配置されている、請求項7に記載のガラス板含有積層体。
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| EP3747846A4 (en) * | 2018-02-02 | 2021-11-03 | Sekisui Chemical Co., Ltd. | INTERMEDIATE FILM FOR LAMINATED GLASS, ROLLED BODY AND LAMINATED GLASS |
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| JP7245691B2 (ja) * | 2019-03-25 | 2023-03-24 | 株式会社日本触媒 | 樹脂粒子及び樹脂粒子の製造方法 |
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