JP3895950B2 - Interlayer film for laminated glass - Google Patents

Interlayer film for laminated glass Download PDF

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Publication number
JP3895950B2
JP3895950B2 JP2001233643A JP2001233643A JP3895950B2 JP 3895950 B2 JP3895950 B2 JP 3895950B2 JP 2001233643 A JP2001233643 A JP 2001233643A JP 2001233643 A JP2001233643 A JP 2001233643A JP 3895950 B2 JP3895950 B2 JP 3895950B2
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Prior art keywords
main
laminated glass
interlayer film
convex
temperature
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JP2003048762A (en
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稔 中嶋
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Sekisui Chemical Co Ltd
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Sekisui Chemical Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06Layered 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
    • B32B17/10Layered 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
    • B32B17/10005Layered 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
    • B32B17/1055Layered 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
    • B32B17/10559Shape of the cross-section
    • B32B17/10577Surface roughness
    • B32B17/10587Surface roughness created by embossing

Description

【0001】
【発明の属する技術分野】
本発明は、微細な凹部と凸部とからなるエンボスが形成された合わせガラス用中間膜に関する。
【0002】
【従来の技術】
ガラス板の間に、可塑化ポリビニルブチラール樹脂のような熱可塑性樹脂を製膜してなる合わせガラス用中間膜を介在させ、接着させて一体化した合わせガラスは、自動車、航空機、建築物等の窓ガラスとして広く使用されている。
【0003】
この種の合わせガラスは、通常、少なくとも2枚のガラス板の間に中間膜を挟み、これをニップロールに通して扱くか又はゴムバックに入れて減圧吸引し、ガラス板と中間膜との間に残留する空気を脱気しながら予備圧着し、次いで、例えばオートクレーブ内で加熱加圧して本圧着を行うことにより製造される。
【0004】
上記中間膜には、透明性、接着性、耐貫通性、耐候性等の基本性能が良好であることの他に、保管中に中間膜同士がブロッキングしないこと、ガラス板の間に中間膜を挟む際の取扱い作業性が良好であること、更に空気の巻き込みによる気泡の発生をなくすために、予備圧着工程での脱気性が良好であること等が要求される。
【0005】
上記のような要求を満たすために、通常、中間膜の両面には微細な凹部と凸部とからなる多数のエンボスが形成されている。凹部と凸部の形態としては、例えば、多数の凸部とこれらの凸部に対する多数の凹部とからなる各種の凹凸模様や、多数の凸条とこれらの凸条に対する多数の凹溝とからなる各種の凹凸模様、粗さ、配置、大きさ等の種々の形状因子に関し多様な値を有するエンボス形状が開示されている。しかし、中間膜の両面に規則的なエンボスが形成されると、互いの回折面の干渉により、一般的にモアレ現象と呼称される縞状の回折像が出現する。
【0006】
上記モアレ現象は、外観の面から好ましくないばかりか、中間膜の裁断時や合わせ加工の作業時に、キラキラと目につく干渉縞の変化等により、作業者の目を疲れさせたり、乗物酔いのような症状を生じさせ、その結果、作業性の低下をもたらすという問題点がある。又、規則的に配置されたエンボスが片面のみに付与された中間膜の場合であっても、それを複数枚重ね合わせて作業する際には、やはりモアレ現象は出現し、同様に作業性の低下を来すという問題点がある。
【0007】
このため、例えば、特表平9−508078号公報等には、凹凸形状において溝形状を規則的に配置し、そのパターンを各面で交差角度25度以上に、より好ましくは交差角度90度にすることによってモアレ現象を解消する中間膜が開示されている。
【0008】
上述の方法において、モアレ現象を解消するために交差角度90度の刻線を付与した形状は、刻線角度45度のロールを用いて熱転写されることが公知である。しかし、ロールの刻線角度が大きくなるほど転写が容易でなくなる。一般には、転写流れに対して平行な縦刻線形状が最も容易に形成することができ、横刻線形状は転写の際に温度制御と高い圧力とを必要とする。
【0009】
又、上述の方法では、予備圧着工程における脱気開始時の温度を厳密に制御しないと、合わせガラス構成体(例えば、ガラス/中間膜/ガラス)の周縁部が先にシールされる周縁部シール先行現象が発生し、構成体内部の脱気が更に不充分になるという問題点がある。
【0010】
上記周縁部シール先行現象の発生を防止する手段として、溝形状の凹凸形状の大きさにより、脱気を開始するときの温度を管理し、脱気開始時の構成体圧着時にシール先行現象を防止したり、又、エンボスの粗さを大きくする方法もあるが、この場合、構成体の周縁部のシールを確実に行うためには予備圧着工程における予備圧着温度を大幅に高める必要が生じるという問題点がある。又、中間膜両面の刻線形状を成形性の観点から平行にすると、膜取扱い性、特に自着力においてその自着性が高くなるという問題点がある。
【0011】
【発明が解決しようとする課題】
本発明の目的は、上記問題点に鑑み、凹凸形状が表面に付与された中間膜において、予備圧着工程時に脱気開始温度の制御を厳密に行わなくとも周縁部シール先行現象が発生することがなく、優れた脱気性を発揮し、又、構成体の周縁部シールのために加熱温度を上げる必要がなく、更に、過酷な条件下においても気泡の発生による品質不良を殆ど生じることがない高品質の合わせガラスを得ることができる合わせガラス用中間膜を提供することにある。
【0012】
【課題を解決するための手段】
本発明は、熱可塑性樹脂シートの両面に主凹部及び主凸部からなる多数のエンボスが形成された合わせガラス用中間膜であって、上記主凹部は、溝形状を有し、上記主凸部は、頭頂に上記主凹部及び主凸部より微細な副凹部及び副凸部が形成された平面部を有し、上記主凹部の溝深さ(Rzg)が10〜30μmであり、かつ主凸部頭頂の平面部に形成された副凹凸部の形状が0<Rvk/Rz≦0.35の関係を満たす合わせガラス用中間膜である。
以下に、本発明を詳述する。
【0013】
本発明の合わせガラス用中間膜は、熱可塑性樹脂シートの両面に主凹部及び主凸部からなる多数のエンボスが形成されている。
【0014】
上記熱可塑性樹脂シートとしては特に限定されず、例えば、可塑化ポリビニルアセタール系樹脂シート、ポリウレタン系樹脂シート、エチレン−酢酸ビニル系樹脂シート、エチレン−エチルアクリレート系樹脂シート、可塑化塩化ビニル系樹脂シート等の従来から中間膜用として用いられている熱可塑性樹脂シートが挙げられる。これらの熱可塑性樹脂シートは、接着性、耐候性、耐貫通性、透明性等の中間膜として必要な基本性能に優れており好適に用いられるが、なかでも可塑化ポリビニルブチラール樹脂シートに代表される可塑化ポリビニルアセタール系樹脂シートがより好適に用いられる。
【0015】
上記熱可塑性樹脂シートの膜厚は、合わせガラスとして必要な耐貫通性等を考慮して設定されれば良く、特に限定されるものではないが、従来の中間膜と同様に、0.2〜2mm程度であることが好ましい。
【0016】
本発明の合わせガラス用中間膜においては、熱可塑性樹脂シートの両面に主凹部及び主凸部からなる多数のエンボスが形成され、上記主凹部は、溝形状を有し、上記主凸部は、頭頂に主凹部及び主凸部より微細な副凹部及び副凸部が形成された平面部を有する。
【0017】
本発明の合わせガラス用中間膜における上記主凹部は溝形状を有し、上記主凹部の底辺は連続している。ガラス/中間膜/ガラス等の組み合わせからなる合わせガラス構成体(積層体)を予備圧着工程において脱気する際の空気の抜け易さは、主凹部の底辺の連続性及び平滑性と密接な関係があり、主凸部の間隔や配置には殆ど影響を受けない。従って、中間膜の主凹部の底辺を連続したものとすることにより、予備圧着工程における脱気性を効果的に向上させることが可能となる。
【0018】
一方、上記のエンボス形状において、予備圧着時のエンボスの潰れ易さ(潰れ性)には、エンボスの体積が大きく影響する。上記エンボスの体積は、主凸部の間隔や配置、主凸部頭頂の平面部の面積、及び、主凹部の溝深さによって決定される。
【0019】
即ち、エンボスを構成する主凸部の頭頂の平面部の面積が広いほどエンボスの体積は大きくなる。本発明の合わせガラス用中間膜は、溝形状を有している主凹部に対する主凸部の頭頂が平面形状を有しているので、換言すれば、主凸部の延長方向に対し直交する断面が台形状を有しているので、主凸部頭頂の平面部の面積は大きくなり、それに伴いエンボスの体積も大きくなり、予備圧着工程におけるガラス構成体の周縁部シール先行現象の発生を効果的に抑えることができる。従って、予備圧着工程において合わせガラス構成体の中央部近傍に存在する空気も効果的に脱気され得る。又、エンボスの体積を大きくすることにより、エンボスの平均表面粗さを相対的に小さくすることができる。予備圧着工程における周縁部シールに必要な温度では、合わせガラス用中間膜は充分に流動状態となり、エンボスの表面粗さがある一定の範囲にあれば、通常の温度で充分に周縁部シールを行うことが可能となる。
【0020】
本発明の合わせガラス用中間膜は、エンボスを構成する主凹部の溝深さ(Rzg)が10〜30μmであり、好ましくは15〜25μmである。主凹部の溝深さ(Rzg)が10μm未満であると、エンボスの体積が小さくなって、予備圧着工程におけるガラス構成体の周縁部シール先行現象が発生し、逆に主凹部の溝深さ(Rzg)が30μmを超えると、エンボスの体積が必要以上に大きくなり過ぎて、予備圧着工程においてガラス構成体の周縁部シールを行うために、より高い温度が必要となる。主凹部の溝深さ(Rzg)を10〜30μmとすることにより、エンボスの体積は適正な大きさとなり、ガラス構成体の周縁部シール先行現象を発生することなく、比較的低い予備圧着温度でガラス構成体の周縁部をシールすることができる。
【0021】
上記主凹部の溝深さ(Rzg)は、汎用の表面粗さ計を用いて測定されるデジタル信号をデータ処理することによって容易に得ることができるが、本発明においては、JIS B−0601「表面粗さ−定義及び表示」に規定される、粗さ曲線の平均線(粗さ曲線までの偏差の2乗和が最小になるように設定した線)を基準とする溝深さを算出し、測定した溝数の溝深さの平均値を主凹部の溝深さ(Rzg)とした。
【0022】
又、本発明の合わせガラス用中間膜では、主凸部頭頂の平面部には、主凹部及び主凸部より微細な副凹部及び副凸部が形成されている。主凸部の頭頂を平面形状にすることにより、中間膜の自着性が高くなることがあるが、平面部に主凹部及び主凸部より微細な副凹部及び副凸部が形成されていることにより、得られる中間膜の自着性を抑えることができ、膜取扱い性が良好となる。
【0023】
図1は、後述する実施例1及び実施例2で得られた中間膜のエンボスの模様(凹凸部の模様)を示す模式図であるが、図1において、aは主凸部の配置間隔(ピッチ)を表し、bは主凸部頭頂の平面部の幅を表す。
【0024】
本発明の合わせガラス用中間膜においては、主凸部の配置間隔{ピッチ(a)}に対する主凸部頭頂の平面部の幅(b)の比率(b/a)が20%以上であることが好ましい。
【0025】
上記b/aが20%未満であると、エンボスの体積向上効果及びそれに伴う周縁部シール先行現象の発生防止効果が充分に得られないことがある。上記b/aが100%になると実質的に主凹部がなくなるため、b/aは100%未満であることが好ましく、より好ましくは90%以下である。又、主凸部頭頂の平面部の幅(b)は、中間膜全域にわたって一定の幅であっても良いし、部分的に異なる幅、即ち、ランダムな幅であっても良い。
【0026】
又、本発明の合わせガラス用中間膜においては、その一方の面の主凹凸形状の間隔に対して他方の面の主凹凸形状の間隔が同一でないことが好ましい。上記両方の面の主凹凸形状の間隔が同一であると、モアレ現象が生じ易くなる。
【0027】
本発明の合わせガラス用中間膜においては、上記主凸部頭頂の平面部の平均表面粗さ(Ra)が2.5μm以上であることが好ましく、より好ましくは、上記Raが3.0μm以上である。上記Raが2.5μm以上であれば、中間膜同士を合わせて常法により保管しても、中間膜同士の接触面積を小さくすることができるので、自着性が問題のないレベルとなる。
【0028】
しかし、単に平面部の面積及び表面粗さを大きくすると、平面部に形成された副凹凸形状内の副凹部に空気溜まりを造ることになり、予備脱気時に微量な空気が残存し、その微量な残存空気により透過率の低下即ち透明性の低下が起こり得る。中間膜は充分な空気の溶解能力を有するので、透過率の低下自体は大きな問題にはならないが、予備圧着工程の管理という面からは透明性は高いほど好ましい。予備圧着時の透明性を充分に確保するためには、主凸部頭頂の平面部に無用な副凹部を設けないことが好ましい。
【0029】
本発明の合わせガラス用中間膜においては、主凹部の平均表面粗さ(Ra:B)と主凸部の平均表面粗さ(Ra:A)との関係がB/A=0.5〜2.0を満たすことが好ましい。尚、上記Ra:A及びRa:Bは、JIS B−0601に規定される、粗さ曲線の平均線を基準とする表面粗さであり、例えば、デジタル型触針電気式表面粗さ計(例えば、商品名「Perthometer S3P」、Feinpuf Perthen GMBH社製)や、デジタル型触針電気式表面粗さ測定器(例えば、商品名「SE−2000」、小坂研究所社製)等を用いて測定することができる。本発明においては、上記デジタル型触針電気式表面粗さ計「Perthometer S3P」を用いて、Ra:Aの場合は、触針の先端幅200μm、対面角90°の条件で、又、Ra:Bの場合は、触針の先端幅5μm、対面角90°の条件で、触針を先端幅に対して直交する方向に移動させて測定した。
【0030】
上記B/Aが0.5未満であると、予備圧着時に脱気開始温度の制御を厳密に行う必要が生じることがあり、換言すれば、予備圧着時にシール条件を緩和することが困難となることがあり、逆に上記B/Aが2.0を超えると、予備圧着時の脱気性が不充分となることがある。
【0031】
本発明の合わせガラス用中間膜においては、主凸部頭頂の平面部に形成された副凹凸部の形状が0<Rvk/Rz≦0.35の関係を満たすことが好ましい。ここで、Rvkは副凹凸部の中心領域から落ち込んでいる谷部分の平均粗さを意味し、Rzは副凹凸部の平均深さを意味する。
【0032】
上記Rvk/Rzが0.35を超えると、予備圧着工程で予備圧着した後の合わせガラス積層体の透明性が低下する現象が発生し易くなる。
【0033】
本発明において、合わせガラス用中間膜の両面に上記のような多数のエンボスを形成する方法としては特に限定されず、例えば、エンボスロール法、カレンダーロール法、異形押出法等が挙げられ、なかでも定量的に一定の微細な凹部及び凸部からなるエンボスを形成することができるエンボスロール法が好ましい。
【0034】
上記エンボスロール法で用いられるエンボスロールとしては特に限定されず、、例えば、金属ロール表面に酸化アルミニウムや酸化珪素等の研削材を用いてブラスト処理を行い、次いで表面の過大ピークを減少させるためにバーチカル研削等を用いてラッピングを行うことにより、ロール表面に微細なエンボス模様(凹凸模様)を形成したもの、彫刻ミル(マザーミル)を用い、この彫刻ミルの凹凸模様を金属ロール表面に転写することにより、ロール表面に微細な凹凸模様を形成したもの、エッチング(蝕刻)によりロール表面に微細な凹凸模様を形成したもの等が挙げられる。
【0035】
本発明の合わせガラス用中間膜における上記エンボス模様(主凹凸部の模様)としては特に限定されず、例えば、刻線状、格子状、放射状、半球状等が挙げられる。
【0036】
上記主凹部及び主凸部の配置(分布)としては特に限定されず、規則的に分布していても良いし、不規則的に分布していても良いが、規則的に分布していることが好ましい。
【0037】
上記主凸部の高さは、全て同じであっても良いし、異なっていても良い。又、主凸部に対する主凹部の溝深さ(Rzg)も10〜30μmの範囲のなかで、全て同じであっても良いし、異なっていても良い。
【0038】
上記主凸部の本来の形状(頭頂に平面部が設けられる前の形状)としては特に限定されず、例えば、三角錐、四角錐、円錐などの錐体、截頭三角錐、截頭四角錐、截頭円錐などの截頭錐体、頭部が山型や半球状となった擬錐体等が挙げられる。又、上記主凹部の形状としては、主凸部に対応した形状等が挙げられる。
【0039】
上記主凸部の寸法としては特に限定されず、主凸部の配置間隔(ピッチ)は10〜2000μmであることが好ましく、より好ましくは50〜1000μmである。又、主凸部の底辺の長さは30〜1000μmであることが好ましい。
【0040】
本発明の合わせガラス用中間膜の製造に際し、主凸部頭頂の平面部に副凹凸部を形成する温度より低い温度で主凹凸部を形成することが好ましい。
【0041】
本発明の合わせガラス用中間膜を得るために、熱可塑性樹脂シートの両面に主凹凸部を形成する方法としては特に限定されず、例えば、主凹凸部に対応する刻線を有するエンボスロールを用いて、予め副凹凸部が形成されている熱可塑性樹脂シートに転写すれば良いが、主凹凸部の転写条件(温度や圧力)が高すぎると、副凹凸部が主凹凸部の転写時に消滅することがある。しかし、主凹凸部の形成温度(転写温度)を副凹凸部の形成温度(転写温度)より低くすることにより、主凹凸部の形成(転写)後でも主凸部頭頂の平面部に主凹凸部より微細な副凹凸部を残存させることができる。
【0042】
本発明の合わせガラス用中間膜は、合わせガラスに好適に用いられる。上記合わせガラスの構成としては、本発明の合わせガラス用中間膜が少なくとも一対のガラス板の間に挟まれていれば特に限定されず、ガラス板/中間膜/ガラス板からなる通常の三層構造のみならず、ガラス板/中間膜/ガラス板/中間膜/ガラス板等よりなる多層構造でも良い。
【0043】
合わせガラスに用いられるガラス板としては特に限定されず、例えば、通常の無機ガラス板や、ポリカーボネート板、ポリメチルメタクリレート板等の有機ガラス板等が挙げられる。
【0044】
本発明の合わせガラス用中間膜を用いて合わせガラスを製造する方法としては特に限定されず、通常の合わせガラスの製造方法の場合と同様に、少なくとも一対のガラス板間に中間膜を挟み、まず予備圧着を行って脱気及び仮接着をした後、例えばオートクレーブ内で本圧着を行うことにより、所望の合わせガラスを得ることができる。
【0045】
例えば、合わせガラス用中間膜として、可塑化ポリビニルブチラール樹脂シートからなる中間膜を用いて合わせガラスを製造する場合は、具体的には、次のように予備圧着と本圧着とを行えば良い。
【0046】
予備圧着は、2枚の透明な無機ガラス板の間に本発明の合わせガラス用中間膜を挟み、この積層体をニップロールに通し、例えば、圧力約196〜980kPa、温度約50〜100℃の条件で扱いて脱気しながら予備圧着する方法(扱き脱気法)、又は、上記積層体をゴムバッグに入れ、ゴムバッグを排気系に接続して約−53〜−100kPaの減圧度(絶対圧力48〜1kPa)となるように吸引減圧しながら温度を上げ、温度約60〜100℃で予備圧着する方法(減圧脱気法)等により行われる。
【0047】
次いで、予備圧着された積層体は、常法によりオートクレーブを用いるか、又は、プレスを用いて、例えば、温度約120〜150℃、圧力約196〜1470kPaの条件で本圧着され、合わせガラスが製造される。
【0048】
【作用】
本発明の合わせガラス用中間膜は、上述のような構成からなるので、予備圧着工程において優れた脱気性を発揮する。又、予備圧着工程における合わせガラス構成体の周縁部シール先行現象の発生は効果的に抑制される。従って、合わせガラス構成体の中央部近傍に存在する空気も効果的に脱気される。
【0049】
【発明の実施の形態】
本発明をさらに詳しく説明するため以下に実施例を挙げるが、本発明はこれら実施例のみに限定されるものではない。
【0050】
(実施例1〜実施例3)並びに(比較例1及び比較例2)
(1)合わせガラス用中間膜の作製
種々のエンボス形状が付与できるように、種々のエンボスロールを用意した。熱可塑性樹脂シートとして、主凸部頭頂に種々の形状の副凹凸部が形成された平面部を有するRZN膜(可塑化ポリビニルブチラール樹脂シート、積水化学工業社製)を用意した。エンボスロールとゴムロールとからなる一対のロールを凹凸形状転写装置として用い、上記RZN膜をこの凹凸形状転写装置に下記転写条件で通し、両面にエンボス形状を有する合わせガラス用中間膜を作製した。
〔転写条件〕
RZN膜の温度:常温、RZN膜の副凹凸部の転写温度:130℃、エンボスロール温度:130℃、線速:10m/分、プレス線圧:500kPa
【0051】
実施例1〜実施例3、並びに、比較例1及び比較例2で得られた合わせガラス用中間膜のエンボスの形状(凹凸部の形状)を表1に示した。又、図1に、実施例1及び実施例2で得られた合わせガラス用中間膜のエンボスの模様(凹凸部の模様)を模式的に示し、図2に、実施例3で得られた合わせガラス用中間膜のエンボスの模様(凹凸部の模様)を模式的に示した。
【0052】
実施例1〜実施例3、並びに、比較例1及び比較例2で得られた合わせガラス用中間膜について、下記の方法でRz及びRvkを測定した。その結果は表1に示すとおりであった。
【0053】
〔Rz及びRvkの測定方法〕
前記デジタル型触針電気式表面粗さ計「Perthometer S3P」及び上記表面粗さ計仕様の表面形状解析装置(商品名「SAS−2010」、名伸工機社製)を用い、JIS B−0601に準拠して、触針の先端幅200μm、対面角90°の条件でRz及びRvkを測定した。
【0054】
(2)合わせガラスの作製
実施例1〜実施例3、並びに、比較例1及び比較例2で得られた合わせガラス用中間膜を使用して、以下に示すように、減圧脱気法により予備圧着を行い、次いで本圧着を行って、合わせガラスを作製した。
【0055】
〔減圧脱気法〕
合わせガラス用中間膜を2枚の透明なフロートガラス板(縦30cm×横30cm×厚さ30cm)の間に挟み、はみ出た部分を切取り、合わせガラス積層体を作製した。得られた合わせガラス積層体をゴムバッグに移した。ゴムバッグを吸引減圧系に接続し、外気加熱温度で加熱すると同時に−60kPa(絶対圧力41kPa)の減圧下で10分間保持し、合わせガラス積層体の温度(予備圧着温度)が70℃となるように加熱した後、大気圧に戻して、予備圧着を終了した合わせガラス積層体を作製した。尚、予備圧着時の脱気開始温度は、40℃、50℃及び60℃の3条件で行った。
【0056】
〔本圧着〕
上記方法で予備圧着された合わせガラス積層体をオートクレーブ内に入れ、温度140℃、圧力1300kPaの条件下で10分間保持した後、50℃まで温度を下げ、大気圧に戻すことにより本圧着を終了して、合わせガラスを作製した。
【0057】
(3)評価
上記で得られた合わせガラスについてベークテストを下記の方法で行って、予備圧着工程での脱気性を評価した。その結果は表1に示すとおりであった。
【0058】
〔合わせガラスのベークテスト〕
合わせガラスを140℃のオーブン内で2時間加熱した。次いで、オーブンから取り出して3時間放冷した後、合わせガラスの外観を目視で観察し、合わせガラスに発泡(気泡)が生じた枚数を調べて、脱気性を評価した。尚、テスト枚数は、各100枚とした。
【0059】
【表1】

Figure 0003895950
【0060】
表1から明らかなように、実施例1〜実施例3の合わせガラス用中間膜を用いて作製した実施例1〜実施例3の合わせガラスは、いずれも減圧脱気法による予備圧着時の脱気開始温度が40℃、50℃及び60℃のいずれの場合でもベークテスト時の気泡による発泡枚数(不良枚数)が極めて少なかった。これは、予備圧着工程において、脱気開始温度を厳密に制御しなくても、又、予備圧着温度を特に高めることなく通常の予備圧着温度(70℃)でも、優れた脱気性を発揮したことを示している。
【0061】
これに対し、主凹部の溝深さ(Rzg)が10μm未満(9.5μm)であった比較例1の合わせガラス用中間膜を用いて作製した比較例1の合わせガラス及び主凹部の溝深さ(Rzg)が30μmを超えていた(31.6μm)比較例2の合わせガラス用中間膜を用いて作製した比較例2の合わせガラスは、実施例11〜実施例3の合わせガラスに比較して、いずれもベークテスト時の気泡による発泡枚数(不良枚数)が多かった。これは、予備圧着工程において、合わせガラス積層体の周縁部シール先行現象が発生し、合わせガラス積層体の中央部近傍に存在する空気が充分に脱気され難かったことを示している。
【0062】
【発明の効果】
以上述べたように、本発明の合わせガラス用中間膜は、予備圧着工程において脱気開始温度を厳密に制御する必要がないにもかかわらず、周縁部シール先行現象を発生することがなく、優れた脱気性を発揮する。従って、合わせガラス作製時の作業性に優れると共に、過酷な条件下においても気泡の発生による品質不良を殆ど生じない高品質の合わせガラスを得ることができる。
【0063】
又、上記本発明の合わせガラス用中間膜を用いて作製された合わせガラスは、過酷な条件下においても気泡の発生による品質不良を殆ど生じない高品質のものであり、自動車、車輌、航空機、建築物等の窓ガラス用として好適に用いられる。
【図面の簡単な説明】
【図1】実施例1及び実施例2で得られた合わせガラス用中間膜のエンボスの模様(凹凸部の模様)を示す模式図である。
【図2】実施例3で得られた合わせガラス用中間膜のエンボスの模様(凹凸部の模様)を示す模式図である。
【符号の説明】
a 主凸部の配置間隔(ピッチ)
b 主凸部頭頂の平面部の幅
c 主凹部の幅[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an interlayer film for laminated glass in which an emboss made of fine concave portions and convex portions is formed.
[0002]
[Prior art]
Laminated glass, which is formed by interposing an interlayer film for laminated glass formed by forming a thermoplastic resin such as plasticized polyvinyl butyral resin between glass plates and bonding them, is a window glass for automobiles, aircraft, buildings, etc. As widely used.
[0003]
In this type of laminated glass, an intermediate film is usually sandwiched between at least two glass plates, and this is handled through a nip roll or placed in a rubber bag and sucked under reduced pressure, and remains between the glass plate and the intermediate film. It is manufactured by pre-compression while deaeration of the air to be performed, and then performing main compression by heating and pressurizing in an autoclave, for example.
[0004]
In addition to good basic performance such as transparency, adhesion, penetration resistance, weather resistance, etc., the interlayer film does not block between interlayer films during storage, and when the interlayer film is sandwiched between glass plates In order to eliminate the generation of bubbles due to entrainment of air, it is required that the deaeration property in the precompression bonding process is good.
[0005]
In order to satisfy the above requirements, a large number of embosses composed of fine concave portions and convex portions are usually formed on both surfaces of the intermediate film. As a form of a recessed part and a convex part, for example, it consists of various uneven | corrugated patterns which consist of many convex parts and many recessed parts with respect to these convex parts, or many convex stripes and many concave grooves with respect to these convex stripes. Embossed shapes having various values regarding various shape factors such as various uneven patterns, roughness, arrangement, and size are disclosed. However, when regular embossing is formed on both surfaces of the intermediate film, a fringe-shaped diffraction image generally called a moire phenomenon appears due to the interference of the diffraction surfaces of each other.
[0006]
The above moire phenomenon is not preferable from the viewpoint of appearance, and when the intermediate film is cut or combined, the eyes of the operator may become tired due to changes in the interference fringes that are noticeable. There is a problem that such symptoms are caused, and as a result, workability is lowered. Even in the case of an intermediate film in which regularly arranged embosses are provided only on one side, when working with a plurality of stacked layers, the moire phenomenon still appears, and the workability is also reduced. There is a problem of causing a decline.
[0007]
For this reason, for example, in Japanese translations of PCT publication No. 9-5008078, etc., the groove shape is regularly arranged in the concavo-convex shape, and the pattern has an intersection angle of 25 degrees or more on each surface, more preferably an intersection angle of 90 degrees. An intermediate film that eliminates the moire phenomenon is disclosed.
[0008]
In the above-described method, it is known that a shape provided with engraved lines having an intersecting angle of 90 degrees in order to eliminate the moire phenomenon is thermally transferred using a roll having an engraved angle of 45 degrees. However, transfer becomes more difficult as the engraving angle of the roll increases. In general, a vertical line shape parallel to the transfer flow can be most easily formed, and the horizontal line shape requires temperature control and high pressure during transfer.
[0009]
Further, in the above-described method, if the temperature at the start of deaeration in the pre-bonding step is not strictly controlled, the peripheral edge seal in which the peripheral edge of the laminated glass structure (for example, glass / intermediate film / glass) is sealed first. There is a problem that the preceding phenomenon occurs and the deaeration inside the structure is further insufficient.
[0010]
As a means to prevent the occurrence of the peripheral seal prior phenomenon, the temperature at the start of deaeration is controlled by the size of the groove-shaped unevenness, and the seal prior phenomenon is prevented at the time of pressure bonding of the component at the start of deaeration There is also a method of increasing the roughness of the emboss, but in this case, it is necessary to significantly increase the pre-compression temperature in the pre-compression process in order to securely seal the peripheral portion of the structure. There is a point. In addition, when the engraved shapes on both surfaces of the intermediate film are made parallel from the viewpoint of moldability, there is a problem that the self-adhesive property is enhanced in terms of the film handling property, particularly the self-adhesive force.
[0011]
[Problems to be solved by the invention]
In view of the above problems, an object of the present invention is that an intermediate film having a concavo-convex shape on its surface may cause a peripheral seal advance phenomenon without strictly controlling the deaeration start temperature during the pre-bonding process. Excellent degassing performance, no need to raise the heating temperature for sealing the peripheral edge of the structure, and high quality with almost no poor quality due to the generation of bubbles even under severe conditions An object of the present invention is to provide an interlayer film for laminated glass from which quality laminated glass can be obtained.
[0012]
[Means for Solving the Problems]
The present invention is an interlayer film for laminated glass in which a large number of embosses composed of main concave portions and main convex portions are formed on both surfaces of a thermoplastic resin sheet, wherein the main concave portions have a groove shape, and the main convex portions has the main recess and the flat portion vice recess and Fukutotsu portion formed fine than the main projections on top, the groove depth of the main recesses (rzg) is Ri 10~30μm der, and mainly The intermediate film for laminated glass satisfies the relationship of 0 <Rvk / Rz ≦ 0.35 in the shape of the sub-concavo-convex portion formed on the flat portion at the top of the convex portion .
The present invention is described in detail below.
[0013]
In the interlayer film for laminated glass of the present invention, a large number of embosses composed of main concave portions and main convex portions are formed on both surfaces of a thermoplastic resin sheet.
[0014]
The thermoplastic resin sheet is not particularly limited. For example, plasticized polyvinyl acetal resin sheet, polyurethane resin sheet, ethylene-vinyl acetate resin sheet, ethylene-ethyl acrylate resin sheet, plasticized vinyl chloride resin sheet The thermoplastic resin sheet conventionally used for intermediate films, such as these, is mentioned. These thermoplastic resin sheets are excellent in basic performance required as an intermediate film such as adhesiveness, weather resistance, penetration resistance and transparency, and are preferably used, but among them are represented by plasticized polyvinyl butyral resin sheets. A plasticized polyvinyl acetal resin sheet is more preferably used.
[0015]
The film thickness of the thermoplastic resin sheet may be set in consideration of the penetration resistance required for laminated glass and the like, and is not particularly limited. It is preferably about 2 mm.
[0016]
In the interlayer film for laminated glass of the present invention, a large number of embosses composed of main concave portions and main convex portions are formed on both surfaces of the thermoplastic resin sheet, the main concave portions have a groove shape, and the main convex portions are The top of the head has a planar portion in which a sub-recess and a sub-projection that are finer than the main recess and the main protrusion are formed.
[0017]
The main recess in the interlayer film for laminated glass of the present invention has a groove shape, and the bottom of the main recess is continuous. The ease of air removal when degassing a laminated glass structure (laminate) composed of a combination of glass / interlayer / glass, etc., is closely related to the continuity and smoothness of the bottom of the main recess. There is almost no influence on the interval and arrangement of the main projections. Therefore, by making the bottom side of the main concave portion of the intermediate film continuous, it is possible to effectively improve the deaeration property in the pre-compression bonding step.
[0018]
On the other hand, in the above-mentioned embossed shape, the embossed volume greatly affects the crushability (collapseability) of the emboss during pre-bonding. The volume of the emboss is determined by the spacing and arrangement of the main convex portions, the area of the flat portion at the top of the main convex portions, and the groove depth of the main concave portions.
[0019]
That is, the volume of the emboss increases as the area of the flat surface of the top of the main convex portion constituting the emboss increases. In the interlayer film for laminated glass of the present invention, the top of the main convex portion with respect to the main concave portion having the groove shape has a planar shape, in other words, a cross section orthogonal to the extending direction of the main convex portion. Because of the trapezoidal shape, the area of the flat part of the top of the main convex part increases, and the volume of the embossment increases accordingly, which effectively causes the peripheral seal prior phenomenon of the glass component in the pre-compression process. Can be suppressed. Therefore, air existing in the vicinity of the central portion of the laminated glass structure in the pre-bonding step can be effectively deaerated. Moreover, by increasing the volume of the emboss, the average surface roughness of the emboss can be relatively reduced. The intermediate film for laminated glass is in a sufficiently fluid state at the temperature required for the peripheral edge seal in the pre-crimping step, and if the surface roughness of the emboss is within a certain range, the peripheral edge seal is sufficiently performed at a normal temperature. It becomes possible.
[0020]
In the interlayer film for laminated glass of the present invention, the groove depth (Rzg) of the main recess constituting the emboss is 10 to 30 μm, preferably 15 to 25 μm. If the groove depth (Rzg) of the main recess is less than 10 μm, the volume of the embossing becomes small, and the peripheral edge seal precedent phenomenon of the glass structure in the pre-compression process occurs, and conversely the groove depth ( When Rzg) exceeds 30 μm, the volume of the emboss becomes excessively larger than necessary, and a higher temperature is required to perform the peripheral portion sealing of the glass structure in the pre-compression bonding step. By setting the groove depth (Rzg) of the main concave portion to 10 to 30 μm, the volume of the emboss becomes an appropriate size, and a relatively low pre-compression temperature does not occur before the peripheral seal of the glass structure occurs. The periphery of the glass structure can be sealed.
[0021]
The groove depth (Rzg) of the main recess can be easily obtained by data processing of a digital signal measured using a general-purpose surface roughness meter. In the present invention, JIS B-0601 “ Calculate the groove depth based on the average line of the roughness curve (line set so that the sum of squares of the deviation to the roughness curve is the minimum) specified in “Surface Roughness-Definition and Display”. The average value of the groove depth of the measured number of grooves was defined as the groove depth (Rzg) of the main recess.
[0022]
Further, in the interlayer film for laminated glass of the present invention, sub-concave portions and sub-convex portions that are finer than the main concave portion and the main convex portion are formed on the flat surface of the top of the main convex portion. Although the self-adhesion property of the intermediate film may be increased by making the top of the main convex part into a planar shape, sub-recesses and sub-protrusions that are finer than the main concave part and the main convex part are formed in the flat part. As a result, the self-adhesiveness of the obtained intermediate film can be suppressed, and the film handleability is improved.
[0023]
FIG. 1 is a schematic view showing an embossed pattern (uneven portion pattern) of an intermediate film obtained in Example 1 and Example 2 to be described later. In FIG. Pitch), and b represents the width of the flat surface of the top of the main convex portion.
[0024]
In the interlayer film for laminated glass of the present invention, the ratio (b / a) of the width (b) of the plane part of the top of the main convex part to the arrangement interval {pitch (a)} of the main convex part is 20% or more. Is preferred.
[0025]
If the b / a is less than 20%, the effect of improving the volume of embossing and the effect of preventing the occurrence of the peripheral seal prior phenomenon may not be sufficiently obtained. When the b / a is 100%, the main concave portion is substantially eliminated. Therefore, the b / a is preferably less than 100%, and more preferably 90% or less. Further, the width (b) of the flat portion at the top of the main convex portion may be a constant width over the entire intermediate film, or may be a partially different width, that is, a random width.
[0026]
In the interlayer film for laminated glass of the present invention, it is preferable that the interval between the main concavo-convex shapes on the other surface is not the same as the interval between the main concavo-convex shapes on the one surface. If the distance between the main concavo-convex shapes on both the surfaces is the same, moire phenomenon is likely to occur.
[0027]
In the interlayer film for laminated glass of the present invention, the average surface roughness (Ra) of the flat portion at the top of the main convex portion is preferably 2.5 μm or more, and more preferably, the Ra is 3.0 μm or more. is there. If the Ra is 2.5 μm or more, even if the interlayer films are combined and stored by a conventional method, the contact area between the interlayer films can be reduced, so that the self-adhesiveness is at a level where there is no problem.
[0028]
However, simply increasing the area and surface roughness of the flat surface part creates an air pool in the sub-recessed part in the sub-recessed shape formed on the flat part, and a minute amount of air remains during preliminary deaeration. The residual air may cause a decrease in transmittance, that is, a decrease in transparency. Since the interlayer film has a sufficient ability to dissolve air, a decrease in the transmittance itself is not a big problem, but it is preferable that the transparency is higher in terms of management of the pre-compression process. In order to ensure sufficient transparency at the time of pre-bonding, it is preferable not to provide an unnecessary sub-recess in the flat part of the top of the main protrusion.
[0029]
In the interlayer film for laminated glass of the present invention, the relationship between the average surface roughness (Ra: B) of the main concave portion and the average surface roughness (Ra: A) of the main convex portion is B / A = 0.5-2. 0.0 is preferably satisfied. The Ra: A and Ra: B are surface roughnesses based on the average line of the roughness curve defined in JIS B-0601. For example, a digital stylus electric surface roughness meter ( For example, measurement is performed using a trade name “Persomemeter S3P”, manufactured by Feinpf Perthen GMBH, or a digital stylus electric surface roughness measuring instrument (eg, trade name “SE-2000”, manufactured by Kosaka Laboratory). can do. In the present invention, using the digital stylus electric surface roughness meter “Permeter S3P”, in the case of Ra: A, the tip width of the stylus is 200 μm, the facing angle is 90 °, and Ra: In the case of B, the measurement was performed by moving the stylus in a direction orthogonal to the tip width under the conditions of the tip width of the stylus of 5 μm and the facing angle of 90 °.
[0030]
When the B / A is less than 0.5, it may be necessary to strictly control the degassing start temperature at the time of preliminary pressure bonding. In other words, it becomes difficult to relax the sealing conditions at the time of preliminary pressure bonding. On the other hand, if the above B / A exceeds 2.0, the deaeration at the time of pre-compression may be insufficient.
[0031]
In the interlayer film for laminated glass of the present invention, it is preferable that the shape of the sub-concave portion formed on the flat surface at the top of the main convex portion satisfies the relationship 0 <Rvk / Rz ≦ 0.35. Here, Rvk means the average roughness of the valley portion falling from the central region of the sub uneven portion, and Rz means the average depth of the sub uneven portion.
[0032]
When the Rvk / Rz exceeds 0.35, a phenomenon that the transparency of the laminated glass laminate after pre-pressing in the pre-pressing step is likely to occur is likely to occur.
[0033]
In the present invention, the method for forming a large number of embosses on both surfaces of the interlayer film for laminated glass is not particularly limited, and examples thereof include an emboss roll method, a calender roll method, and a profile extrusion method. An embossing roll method capable of quantitatively forming embossing composed of fine concave and convex portions is preferable.
[0034]
The embossing roll used in the embossing roll method is not particularly limited. For example, in order to reduce the excessive peak of the surface by performing a blasting process using a grinding material such as aluminum oxide or silicon oxide on the surface of the metal roll. Using a carving mill (mother mill) with a fine embossed pattern (uneven pattern) formed on the roll surface by lapping using vertical grinding etc., transferring the uneven pattern of this engraving mill to the metal roll surface In this case, a fine concavo-convex pattern is formed on the roll surface, and a fine concavo-convex pattern is formed on the roll surface by etching (etching).
[0035]
The embossed pattern (pattern of the main concavo-convex portion) in the interlayer film for laminated glass of the present invention is not particularly limited, and examples thereof include engraved lines, grids, radials, and hemispheres.
[0036]
The arrangement (distribution) of the main concave portion and the main convex portion is not particularly limited, and may be regularly distributed or irregularly distributed, but regularly distributed. Is preferred.
[0037]
The main projections may all have the same height or different heights. Further, the groove depth (Rzg) of the main concave portion relative to the main convex portion may be all the same or different in the range of 10 to 30 μm.
[0038]
There is no particular limitation on the original shape of the main convex portion (the shape before the flat portion is provided on the top of the head). For example, a pyramid such as a triangular pyramid, a quadrangular pyramid, and a cone, a truncated triangular pyramid, and a truncated quadrangular pyramid And truncated cones such as truncated cones, pseudo cones with a head-shaped or hemispherical head, and the like. In addition, examples of the shape of the main concave portion include a shape corresponding to the main convex portion.
[0039]
The dimensions of the main projections are not particularly limited, and the arrangement interval (pitch) of the main projections is preferably 10 to 2000 μm, more preferably 50 to 1000 μm. Moreover, it is preferable that the length of the base of a main convex part is 30-1000 micrometers.
[0040]
In the production of the interlayer film for laminated glass of the present invention, it is preferable to form the main concavo-convex portion at a temperature lower than the temperature at which the sub concavo-convex portion is formed on the flat portion at the top of the main convex portion.
[0041]
In order to obtain the interlayer film for laminated glass of the present invention, the method for forming the main concavo-convex portions on both surfaces of the thermoplastic resin sheet is not particularly limited. For example, an embossing roll having engraved lines corresponding to the main concavo-convex portions is used. However, if the transfer condition (temperature or pressure) of the main uneven portion is too high, the sub uneven portion disappears when the main uneven portion is transferred. Sometimes. However, by making the formation temperature (transfer temperature) of the main concavo-convex part lower than the formation temperature (transfer temperature) of the sub concavo-convex part, the main concavo-convex part remains on the top of the main convex part even after the main concavo-convex part (transfer) Finer sub uneven portions can be left.
[0042]
The interlayer film for laminated glass of the present invention is suitably used for laminated glass. The structure of the laminated glass is not particularly limited as long as the interlayer film for laminated glass of the present invention is sandwiched between at least a pair of glass plates, and only a normal three-layer structure composed of a glass plate / intermediate film / glass plate is used. Alternatively, a multilayer structure composed of glass plate / intermediate film / glass plate / intermediate film / glass plate or the like may be used.
[0043]
It does not specifically limit as a glass plate used for laminated glass, For example, organic glass plates, such as a normal inorganic glass plate, a polycarbonate plate, a polymethylmethacrylate board, etc. are mentioned.
[0044]
The method for producing a laminated glass using the interlayer film for laminated glass of the present invention is not particularly limited, and in the same manner as in the ordinary laminated glass producing method, an interlayer film is sandwiched between at least a pair of glass plates, After performing pre-bonding and deaeration and temporary bonding, a desired laminated glass can be obtained by performing main bonding in an autoclave, for example.
[0045]
For example, when producing a laminated glass using an intermediate film made of a plasticized polyvinyl butyral resin sheet as an intermediate film for laminated glass, specifically, pre-bonding and main-bonding may be performed as follows.
[0046]
In the pre-compression, the laminated glass interlayer film of the present invention is sandwiched between two transparent inorganic glass plates, and this laminate is passed through a nip roll, for example, under conditions of a pressure of about 196 to 980 kPa and a temperature of about 50 to 100 ° C. A method of pre-pressing while degassing (handling degassing method), or putting the laminate in a rubber bag and connecting the rubber bag to an exhaust system to reduce the degree of vacuum (absolute pressure 48- 1 kPa) is performed by a method of increasing the temperature while reducing the pressure by suction and pre-pressing at a temperature of about 60 to 100 ° C. (vacuum degassing method).
[0047]
Next, the pre-pressed laminate is subjected to main press bonding under conditions of, for example, a temperature of about 120 to 150 ° C. and a pressure of about 196 to 1470 kPa using an autoclave or a press by a conventional method to produce a laminated glass. Is done.
[0048]
[Action]
Since the interlayer film for laminated glass according to the present invention has the above-described configuration, it exhibits excellent degassing properties in the preliminary press-bonding step. In addition, the occurrence of the peripheral seal prior phenomenon of the laminated glass structure in the pre-bonding step is effectively suppressed. Therefore, the air existing in the vicinity of the center portion of the laminated glass structure is also effectively deaerated.
[0049]
DETAILED DESCRIPTION OF THE INVENTION
In order to describe the present invention in more detail, examples are given below, but the present invention is not limited to these examples.
[0050]
(Examples 1 to 3) and (Comparative Examples 1 and 2)
(1) Preparation of interlayer film for laminated glass Various embossing rolls were prepared so that various embossed shapes could be imparted. As a thermoplastic resin sheet, an RZN film (plasticized polyvinyl butyral resin sheet, manufactured by Sekisui Chemical Co., Ltd.) having a planar portion in which sub-irregular portions of various shapes were formed on the top of the main convex portion was prepared. A pair of rolls composed of an embossing roll and a rubber roll was used as a concavo-convex shape transfer device, and the RZN film was passed through the concavo-convex shape transfer device under the following transfer conditions to produce an intermediate film for laminated glass having an embossed shape on both sides.
(Transfer conditions)
RZN film temperature: normal temperature, RZN film sub-concave portion transfer temperature: 130 ° C., embossing roll temperature: 130 ° C., linear velocity: 10 m / min, press linear pressure: 500 kPa
[0051]
Table 1 shows the embossed shapes (shapes of the concavo-convex portions) of the interlayer films for laminated glass obtained in Examples 1 to 3 and Comparative Examples 1 and 2. FIG. 1 schematically shows an embossed pattern (uneven portion pattern) of the interlayer film for laminated glass obtained in Example 1 and Example 2, and FIG. The embossed pattern (pattern on the concavo-convex part) of the interlayer film for glass is schematically shown.
[0052]
For the interlayer films for laminated glass obtained in Examples 1 to 3 and Comparative Examples 1 and 2, Rz and Rvk were measured by the following methods. The results are shown in Table 1.
[0053]
[Measurement method of Rz and Rvk]
Using the digital stylus electric surface roughness meter “Perometer S3P” and the surface shape analyzer of the surface roughness meter specification (trade name “SAS-2010”, manufactured by Nashin Koki Co., Ltd.), JIS B-0601 In accordance with the above, Rz and Rvk were measured under the condition that the tip width of the stylus was 200 μm and the facing angle was 90 °.
[0054]
(2) Preparation of laminated glass Using the interlayer films for laminated glass obtained in Examples 1 to 3 and Comparative Example 1 and Comparative Example 2, as shown below, preliminarily prepared by a vacuum degassing method. Bonding was performed and then main pressing was performed to produce a laminated glass.
[0055]
[Vacuum degassing method]
An interlayer film for laminated glass was sandwiched between two transparent float glass plates (length 30 cm × width 30 cm × thickness 30 cm), and the protruding portion was cut out to produce a laminated glass laminate. The obtained laminated glass laminate was transferred to a rubber bag. The rubber bag is connected to a suction pressure reducing system and heated at the outside air heating temperature, and simultaneously held for 10 minutes under a reduced pressure of −60 kPa (absolute pressure 41 kPa) so that the temperature of the laminated glass laminate (preliminary pressure bonding temperature) becomes 70 ° C. Then, the pressure was returned to atmospheric pressure to produce a laminated glass laminate that had been subjected to pre-compression bonding. In addition, the deaeration start temperature at the time of preliminary press bonding was performed under three conditions of 40 ° C., 50 ° C., and 60 ° C.
[0056]
[Main crimping]
The laminated glass laminate preliminarily pressed by the above method is put in an autoclave, held for 10 minutes under conditions of a temperature of 140 ° C. and a pressure of 1300 kPa, then the temperature is lowered to 50 ° C. and returned to atmospheric pressure to complete the main pressure bonding. And the laminated glass was produced.
[0057]
(3) Evaluation The laminated glass obtained above was subjected to a baking test by the following method to evaluate the deaeration property in the preliminary press bonding step. The results are shown in Table 1.
[0058]
[Laminated glass baking test]
The laminated glass was heated in an oven at 140 ° C. for 2 hours. Subsequently, after taking out from oven and allowing to cool for 3 hours, the external appearance of the laminated glass was observed visually, the number of foaming (bubbles) produced in the laminated glass was examined, and deaeration was evaluated. The number of test sheets was 100 for each.
[0059]
[Table 1]
Figure 0003895950
[0060]
As is clear from Table 1, the laminated glasses of Examples 1 to 3 produced using the interlayer films for laminated glass of Examples 1 to 3 are all removed at the time of pre-compression by the vacuum degassing method. In any case where the gas start temperature was 40 ° C., 50 ° C. or 60 ° C., the number of foamed bubbles (number of defects) due to bubbles during the baking test was extremely small. This is because, in the pre-compression process, even if the degassing start temperature is not strictly controlled and the pre-compression temperature is not particularly increased, the deaeration performance is excellent even at the normal pre-compression temperature (70 ° C). Is shown.
[0061]
In contrast, the laminated glass of Comparative Example 1 manufactured using the interlayer film for laminated glass of Comparative Example 1 in which the groove depth (Rzg) of the main recessed portion was less than 10 μm (9.5 μm) and the groove depth of the main recessed portion. (Rzg) exceeded 30 μm (31.6 μm) The laminated glass of Comparative Example 2 produced using the interlayer film for laminated glass of Comparative Example 2 was compared with the laminated glasses of Example 11 to Example 3. In all cases, the number of foams (number of defects) due to bubbles during the baking test was large. This indicates that in the pre-bonding step, the peripheral seal prior phenomenon of the laminated glass laminate occurred, and the air existing near the center of the laminated glass laminate was not sufficiently deaerated.
[0062]
【The invention's effect】
As described above, the interlayer film for laminated glass according to the present invention is superior in that it does not cause a peripheral seal prior phenomenon even though it is not necessary to strictly control the degassing start temperature in the pre-compression process. Degassed. Therefore, it is possible to obtain a high-quality laminated glass that is excellent in workability at the time of producing a laminated glass and hardly causes quality defects due to the generation of bubbles even under severe conditions.
[0063]
Further, the laminated glass produced using the interlayer film for laminated glass of the present invention is of a high quality that hardly causes a quality defect due to the generation of bubbles even under severe conditions, such as automobiles, vehicles, aircraft, It is suitably used as a window glass for buildings and the like.
[Brief description of the drawings]
FIG. 1 is a schematic diagram showing an embossed pattern (pattern of irregularities) of an interlayer film for laminated glass obtained in Example 1 and Example 2. FIG.
FIG. 2 is a schematic view showing an embossed pattern (uneven portion pattern) of the interlayer film for laminated glass obtained in Example 3. FIG.
[Explanation of symbols]
a Arrangement interval (pitch) of main projections
b Width of flat surface of main convex part c Width of main concave part

Claims (3)

熱可塑性樹脂シートの両面に主凹部及び主凸部からなる多数のエンボスが形成された合わせガラス用中間膜であって、上記主凹部は、溝形状を有し、上記主凸部は、頭頂に上記主凹部及び主凸部より微細な副凹部及び副凸部が形成された平面部を有し、上記主凹部の溝深さ(Rzg)が10〜30μmであり、かつ主凸部頭頂の平面部に形成された副凹凸部の形状が0<Rvk/Rz≦0.35の関係を満たすことを特徴とする合わせガラス用中間膜。An interlayer film for laminated glass in which a large number of embossments composed of main concave portions and main convex portions are formed on both surfaces of a thermoplastic resin sheet, wherein the main concave portion has a groove shape, and the main convex portions are formed on the top of the head. the main recess and has a planar portion which sub recesses and Fukutotsu unit fine is formed from the main protrusion, the main recess of the groove depth (rzg) is 10~30μm der is, and the Shutotsu portion parietal An interlayer film for laminated glass, wherein the shape of the sub-concave portion formed on the flat portion satisfies a relationship of 0 <Rvk / Rz ≦ 0.35 . 主凸部の配置間隔(ピッチ)に対する主凸部頭頂の平面部の幅の比率が20%以上であることを特徴とする請求項1に記載の合わせガラス用中間膜。  2. The interlayer film for laminated glass according to claim 1, wherein the ratio of the width of the flat portion of the top of the main convex portion to the arrangement interval (pitch) of the main convex portion is 20% or more. 上記合わせガラス用中間膜の製造に際し、主凸部頭頂の平面部に副凹凸部を形成する温度より低い温度で主凹凸部を形成することを特徴とする請求項1または2に記載の合わせガラス用中間膜。The laminated glass according to claim 1 or 2, characterized in that formed in the production of the laminated glass interlayer film for a main uneven portion at a temperature lower than the temperature for forming the sub uneven portion to the plane portion of the main protrusions parietal Interlayer film.
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US7351468B2 (en) * 2000-10-26 2008-04-01 E. I. Du Pont De Nemours And Company Interlayers for laminated safety glass with superior de-airing and laminating properties and process for making the same
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RU2721199C2 (en) 2015-07-31 2020-05-18 Секисуй Кемикал Ко., Лтд. Interlayer film for multilayer glass, method of producing interlayer film for multilayer glass and multilayer glass
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