JP2001206742A - Intermediate film for sandwich glass and sandwich glass - Google Patents

Intermediate film for sandwich glass and sandwich glass

Info

Publication number
JP2001206742A
JP2001206742A JP2000010537A JP2000010537A JP2001206742A JP 2001206742 A JP2001206742 A JP 2001206742A JP 2000010537 A JP2000010537 A JP 2000010537A JP 2000010537 A JP2000010537 A JP 2000010537A JP 2001206742 A JP2001206742 A JP 2001206742A
Authority
JP
Japan
Prior art keywords
polyvinyl acetal
acetal resin
film
laminated glass
polymerization
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP2000010537A
Other languages
Japanese (ja)
Other versions
JP4331846B2 (en
Inventor
Kiyobumi Toyama
清文 遠山
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sekisui Chemical Co Ltd
Original Assignee
Sekisui Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sekisui Chemical Co Ltd filed Critical Sekisui Chemical Co Ltd
Priority to JP2000010537A priority Critical patent/JP4331846B2/en
Publication of JP2001206742A publication Critical patent/JP2001206742A/en
Application granted granted Critical
Publication of JP4331846B2 publication Critical patent/JP4331846B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/10—Properties of the layers or laminate having particular acoustical properties
    • B32B2307/102—Insulating

Landscapes

  • Laminated Bodies (AREA)
  • Joining Of Glass To Other Materials (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Soundproofing, Sound Blocking, And Sound Damping (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain an intermediate film for sandwich glass which does not impair the basic performance necessary for the sandwich glass, such as transparency, weatherability, impact energy absorbability and adhesiveness to glass, has sufficient formability and handling quality and can exhibit excellent sound shielding performance over a wide temperature region. SOLUTION: At least one layer of polyvinyl acetal resin film of the intermediate film for sandwich glass consisting of a laminate composed of the plural plasticized polyvinyl acetal resin films contains the polyvinyl acetal resin (A) of 2,000 to 3,000 in average degree of polymerization and the polyvinyl acetal resin (B) of 300 to 600 in average degree of polymerization and >=1,500 in the difference in the average degree of polymerization from the polyvinyl acetal resin (A). The polyvinyl acetal resin (B) is mixed at a ratio of 3 to 8 pts.wt. per 100 pts.wt. polyvinyl acetal resin (A).

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】本発明は、例えば車両や建築
物の窓ガラスに用いられる合わせガラス用中間膜に関
し、より詳細には、優れた遮音性能を発揮する合わせガ
ラス用中間膜、該合わせガラス用中間膜を用いた合わせ
ガラス及びその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an interlayer film for laminated glass used, for example, for window glasses of vehicles and buildings, and more particularly, to an interlayer film for laminated glass exhibiting excellent sound insulation performance, and the laminated glass. TECHNICAL FIELD The present invention relates to a laminated glass using an interlayer film for use and a method for producing the same.

【０００２】[0002]

【従来の技術】合わせガラスは、一対のガラス板間に樹
脂膜をサンドイッチした構造を有する。破損時に破片が
飛散せず、安全性に優れているため、合わせガラスは、
例えば自動車用などの交通車両の窓板ガラスや建築物の
窓板ガラスに広く用いられている。2. Description of the Related Art A laminated glass has a structure in which a resin film is sandwiched between a pair of glass plates. Since broken pieces do not scatter at the time of breakage and are excellent in safety, laminated glass is
For example, it is widely used as window glass for traffic vehicles such as automobiles and window glass for buildings.

【０００３】上記合わせガラスにおいて、ガラス板間に
サンドイッチされる樹脂膜は、中間膜と称されている。
この中間膜を構成する材料としては、可塑剤の添加によ
り可塑化されたポリビニルブチラール樹脂膜が用いられ
ている。In the above laminated glass, the resin film sandwiched between the glass plates is called an intermediate film.
As a material constituting the intermediate film, a polyvinyl butyral resin film plasticized by adding a plasticizer is used.

【０００４】可塑化されたポリビニルブチラール樹脂膜
は、ガラスとの接着性に優れており、引張強度が高く、
高い透明性を備えている。従って、可塑化されたポリビ
ニルブチラール樹脂膜を中間膜として用いた合わせガラ
スは、車両用窓ガラスとして特に好適である。[0004] The plasticized polyvinyl butyral resin film has excellent adhesion to glass, high tensile strength,
Has high transparency. Therefore, a laminated glass using a plasticized polyvinyl butyral resin film as an intermediate film is particularly suitable as a window glass for vehicles.

【０００５】ところで、遮音性能は、周波数の変化に応
じた透過損失量で示され、該透過損失量は、ＪＩＳ Ａ
４７０８では、図１に実線で示すように、５００Ｈｚ以
上において遮音等級に応じてそれぞれ一定値で規定され
ている。ところで、ガラス板の遮音性能は、図１に破線
で示すように、２０００Ｈｚを中心とする周波数領域で
は、コインシデンス効果により著しく低下する。図１の
破線で示す特性の谷部がコインシデンス効果による遮音
性能の低下部分に相当し、２０００Ｈｚを中心とする周
波数領域では所定の遮音性能を有しないことがわかる。[0005] Incidentally, the sound insulation performance is represented by a transmission loss amount corresponding to a change in frequency.
In 4708, as shown by the solid line in FIG. 1, the constant is specified at 500 Hz or more according to the sound insulation class. By the way, the sound insulation performance of the glass plate is remarkably reduced due to the coincidence effect in a frequency region centered at 2000 Hz, as shown by a broken line in FIG. The valley of the characteristic shown by the broken line in FIG. 1 corresponds to a portion where the sound insulation performance is reduced due to the coincidence effect, and it can be seen that a predetermined sound insulation performance is not provided in a frequency region around 2000 Hz.

【０００６】なお、上記コインシデンス効果とは、ガラ
ス板に音波が入射した時に、ガラス板の剛性と慣性によ
り、ガラス面上を横波が伝搬し、横波と入射音とが共鳴
し、その結果、音が透過する現象をいう。[0006] The coincidence effect means that when a sound wave is incident on a glass plate, a transverse wave propagates on the glass surface due to the rigidity and inertia of the glass plate, and the transverse wave and the incident sound resonate. Refers to the phenomenon of transmission.

【０００７】上記の合わせガラスは、破片の飛散防止の
面においては優れているものの、２０００Ｈｚを中心と
する周波数領域において、上記コインシデンス効果によ
る遮音性能の低下が避けられず、この点の改善が強く求
められていた。[0007] Although the above laminated glass is excellent in preventing the scattering of fragments, it is inevitable that the sound insulation performance is reduced due to the coincidence effect in a frequency region centered at 2000 Hz, and this point is strongly improved. Was sought.

【０００８】他方、人間の聴覚は、等ラウドネス曲線か
ら、１０００〜６０００Ｈｚの範囲では他の周波数領域
に比べて非常に高い感度を示すことが知られている。従
って、コインシデンス効果による上記遮音性能の落ち込
みを解消することは、防音性を高める上で極めて重要で
あることがわかる。[0008] On the other hand, it is known from the equal loudness curve that human hearing exhibits a much higher sensitivity in the range of 1000 to 6000 Hz than in other frequency regions. Therefore, it is understood that resolving the drop in the sound insulation performance due to the coincidence effect is extremely important in improving the sound insulation.

【０００９】従って、合わせガラスの遮音性能を高める
には、上記コインシデンス効果による遮音性能の低下を
緩和し、コインシデンス効果によって生じる透過損失の
極小部（以下、この極小部の透過損失をＴＬ値と呼ぶ。
図１参照）の低下を防ぐ必要がある。Therefore, in order to enhance the sound insulation performance of the laminated glass, the decrease in the sound insulation performance due to the above-described coincidence effect is alleviated, and the minimum transmission loss caused by the coincidence effect (hereinafter, the transmission loss of this minimum portion is referred to as the TL value). .
(See FIG. 1).

【００１０】従来、ＴＬ値の低下を抑制する方法とし
て、合わせガラスの質量を増大させる方法、ガラス
を複層化する方法、ガラス面積を細分化する方法、
ガラス板支持手段を改善する方法など、種々の方法が提
案されている。しかしながら、これらのいずれの方法に
おいても、十分に満足し得る効果を得ることができず、
かつ合わせガラスのコストが高くつくという問題があっ
た。Conventionally, as a method of suppressing the decrease in TL value, a method of increasing the mass of a laminated glass, a method of forming a multilayer glass, a method of subdividing a glass area,
Various methods have been proposed, such as a method for improving a glass plate supporting means. However, in any of these methods, a sufficiently satisfactory effect cannot be obtained,
In addition, there is a problem that the cost of the laminated glass is expensive.

【００１１】遮音性能に対する要求は近年ますます高ま
っており、例えば建築用窓ガラスでは、常温付近で優れ
た遮音性能が要求されている。すなわち、温度に対して
ＴＬ値をプロットとすることにより求められた、遮音性
能が最も優れている温度（遮音性能最大温度＝ＴＬMAX
温度）が常温付近であり、かつ遮音性能の最大値（遮音
性能最大値＝ＴＬMAX 値）自体が大きいことが要求され
ている。同様に自動車用窓ガラスにおいても遮音性能が
高いことが求められ、高速走行時の風切り音及びエンジ
ン部からの振動等に対する遮音性が強く求められてい
る。[0011] In recent years, demands for sound insulation performance have been increasing more and more. For example, window glasses for construction are required to have excellent sound insulation performance near room temperature. In other words, the temperature at which the sound insulation performance is the best is obtained by plotting the TL value against the temperature (maximum temperature of the sound insulation performance = TL MAX).
Temperature) is around room temperature, and the maximum value of the sound insulation performance (the maximum value of the sound insulation performance = TL MAX value) itself is required to be large. Similarly, high sound insulation performance is required for window glass for automobiles, and sound insulation against wind noise during high-speed running, vibration from an engine unit, and the like is strongly required.

【００１２】また、実際に使用される状況を考慮する
と、これらの合わせガラスは、低温域から高温域までの
幅広い環境温度の変化にさらされる。すなわち、室温付
近のみならず、広い温度範囲にわたり、良好な遮音性能
を有することが要求される。Further, in consideration of the actual use, these laminated glasses are exposed to a wide range of environmental temperature changes from a low temperature range to a high temperature range. That is, it is required to have good sound insulation performance not only near room temperature but also over a wide temperature range.

【００１３】しかしながら、例えば、従来の可塑化ポリ
ビニルブチラール樹脂膜を用いた合わせガラスは、遮音
性能最大温度が室温より高く、常温付近では遮音性能が
十分でないという問題があった。However, for example, a laminated glass using a conventional plasticized polyvinyl butyral resin film has a problem that the maximum temperature of the sound insulation performance is higher than room temperature, and the sound insulation performance is not sufficient near normal temperature.

【００１４】上記のような合わせガラスの遮音性能を高
め得る中間膜の一例が、例えば、特開平２−２２９７４
２号公報に開示されている。ここでは、ガラス転移温度
１５℃以下の高分子膜、例えば塩化ビニル−エチレン−
グリシジルメタクリレート共重合体膜と、可塑化ポリビ
ニルアセタール膜との積層体からなる中間膜が記載され
ている。An example of an interlayer capable of improving the sound insulation performance of the laminated glass as described above is disclosed in, for example, Japanese Patent Laid-Open No. 22974/1990.
No. 2 discloses this. Here, a polymer film having a glass transition temperature of 15 ° C. or lower, for example, vinyl chloride-ethylene-
An intermediate film comprising a laminate of a glycidyl methacrylate copolymer film and a plasticized polyvinyl acetal film is described.

【００１５】しかしながら、ＪＩＳ Ａ４７０６による
遮音等級でＴｓ−３５等級を超える十分な遮音性は発揮
されず、遮音性を示す温度範囲が限定されており、広い
温度範囲で良好な遮音性能を発揮し得るものではなかっ
た。However, the sound insulation grade according to JIS A4706 does not exhibit sufficient sound insulation exceeding Ts-35 grade, and the temperature range showing the sound insulation is limited, so that good sound insulation performance can be exhibited in a wide temperature range. It was not something.

【００１６】また、特開昭５１−１０６１９０号公報に
は、ガラス転移温度が異なる２種以上の樹脂膜を金属板
に積層することにより、広い温度領域で制振性を発現す
る積層体が開示されている。この積層体では、広い温度
領域で制振性が改善される。しかしながら、特開昭５１
−１０６１９０号公報は、上記制振性を有する複合金属
板を開示しているに留まり、合わせガラスの中間膜とし
て用いた場合の必要な遮音性や透明性などに関しては言
及されていない。また、この先行技術に記載の積層体
は、安全ガラスとして必要な高い衝撃エネルギー吸収性
やガラス破損時の飛散防止性などの要件を満たすもので
はない。Japanese Patent Application Laid-Open No. 51-106190 discloses a laminated body which exhibits vibration damping properties over a wide temperature range by laminating two or more resin films having different glass transition temperatures on a metal plate. Have been. In this laminate, the vibration damping property is improved in a wide temperature range. However, JP
JP-A-106190 merely discloses the composite metal plate having the above-described vibration damping properties, but does not mention the necessary sound insulation and transparency when used as an interlayer film of laminated glass. Further, the laminated body described in the prior art does not satisfy requirements such as high impact energy absorption required for safety glass and scattering prevention upon glass breakage.

【００１７】本発明の目的は、透明性、耐候性、衝撃エ
ネルギー吸収性、及びガラスとの接着性等の合わせガラ
ス用中間膜として必要な基本的性能を損なうことなく、
かつ中間膜の成形性及び取扱性も損なうことなく、コイ
ンシデンス効果の緩和によりＴＬ値の低下を防ぎ、かつ
広い温度領域にわたり優れた遮音性能を長期間安定に発
揮し得る、合わせガラス用中間膜、該合わせガラス用中
間膜を用いた合わせガラス並びに該合わせガラスの製造
方法を提供することにある。An object of the present invention is to provide a laminated glass intermediate film having basic properties such as transparency, weather resistance, impact energy absorption, and adhesion to glass without impairing the basic properties.
An interlayer film for laminated glass, which can prevent a decrease in the TL value by relaxing the coincidence effect and can stably exhibit excellent sound insulation performance over a wide temperature range for a long time without impairing the moldability and handleability of the interlayer film, An object of the present invention is to provide a laminated glass using the interlayer film for a laminated glass and a method for producing the laminated glass.

【００１８】[0018]

【課題を解決するための手段】本願発明者らは、合わせ
ガラスの遮音性能が、中間膜の動的粘弾特性により左右
され、特に貯蔵弾性率と損失弾性率との比である損失正
接に最も影響されることを見出し、該知見に基づき、中
間膜の損失正接を制御すれば、広い温度範囲にわたり合
わせガラスの遮音性能を高め得るのではないかと考え、
鋭意検討した。Means for Solving the Problems The present inventors have found that the sound insulation performance of a laminated glass is affected by the dynamic viscoelastic properties of the interlayer film, and in particular, the loss tangent which is the ratio between the storage elastic modulus and the loss elastic modulus. Finding that it is most affected, based on the knowledge, if the loss tangent of the interlayer film is controlled, it is thought that the sound insulation performance of the laminated glass may be enhanced over a wide temperature range,
We studied diligently.

【００１９】その結果、特定の平均重合度を有する樹脂
膜を用いれば、損失係数が広い温度範囲にわたり、特に
低温域で良好となり、合わせガラスの遮音性能の高めら
れることが見出され、本発明をなすに至った。As a result, it has been found that when a resin film having a specific average degree of polymerization is used, the loss coefficient is improved over a wide temperature range, particularly in a low temperature range, and the sound insulating performance of the laminated glass is improved. Was reached.

【００２０】すなわち、本発明に係る合わせガラス用中
間膜は、可塑化された複数枚のポリビニルアセタール樹
脂膜よりなる積層体からなる合わせガラス用中間膜であ
って、少なくとも１層のポリビニルアセタール樹脂膜
が、平均重合度２０００〜３０００のポリビニルアセタ
ール樹脂（Ａ）と、平均重合度が３００〜６００であ
り、かつポリビニルアセタール樹脂（Ａ）との平均重合
度の差が１５００以上であるポリビニルアセタール樹脂
（Ｂ）とを含み、ポリビニルアセタール樹脂（Ｂ）がポ
リビニルアセタール樹脂（Ａ）１００重量部に対し、３
〜８重量％の割合で混合されていることを特徴とする。That is, the interlayer film for a laminated glass according to the present invention is an interlayer film for a laminated glass comprising a laminate of a plurality of plasticized polyvinyl acetal resin films, and at least one layer of a polyvinyl acetal resin film. Is a polyvinyl acetal resin (A) having an average degree of polymerization of 2000 to 3000, and a polyvinyl acetal resin having an average degree of polymerization of 300 to 600 and a difference in average degree of polymerization between the polyvinyl acetal resin (A) of 1500 or more ( B) and 100 parts by weight of the polyvinyl acetal resin (A).
-8% by weight.

【００２１】本発明に係る合わせガラス用中間膜の特定
の局面では、前記ポリビニルアセタール樹脂がポリビニ
ルブチラール樹脂であり、可塑剤が、トリエチレングリ
コールジ２−エチルブチレート、トリエチレングリコー
ルジ２−エチルヘキサノエート及びトリエチレングリコ
ールジｎ−ヘプタノエートからなる群より選択した少な
くとも１種であることを特徴とする。In a specific aspect of the interlayer film for laminated glass according to the present invention, the polyvinyl acetal resin is a polyvinyl butyral resin, and the plasticizer is triethylene glycol di-2-ethyl butyrate or triethylene glycol di 2-ethyl. It is at least one selected from the group consisting of hexanoate and triethylene glycol di-n-heptanoate.

【００２２】本発明に係る合わせガラスは、少なくとも
一対の板状透明体間に、本発明に係る合わせガラス用中
間膜を介在させ、一体化させてなることを特徴とする。
以下、本発明の詳細を説明する。The laminated glass according to the present invention is characterized in that the interlayer film for laminated glass according to the present invention is interposed between at least a pair of transparent plates and integrated.
Hereinafter, details of the present invention will be described.

【００２３】本発明に係る合わせガラス用中間膜に用い
られるポリビニルアセタール樹脂を得る方法としては、
例えば、ポリビニルアルコールを熱水に溶解し、得られ
たポリビニル水溶液を所定温度に保持した後、これにア
ルデヒドと触媒を加え、アセタール化反応を進行させ、
しかる後、反応液を所定温度に保持した後、中和、水洗
及び乾燥の諸工程を経て樹脂粉末を得る方法が挙げられ
る。The method for obtaining the polyvinyl acetal resin used in the interlayer film for laminated glass according to the present invention includes:
For example, after dissolving polyvinyl alcohol in hot water and maintaining the obtained aqueous polyvinyl solution at a predetermined temperature, an aldehyde and a catalyst are added thereto, and the acetalization reaction proceeds,
Thereafter, a method of obtaining a resin powder through various steps of neutralization, washing with water and drying after maintaining the reaction solution at a predetermined temperature.

【００２４】本発明に係る合わせガラス用中間膜では、
広い温度範囲にわたり良好な遮音性能を得るために、複
数のポリビニルアセタール樹脂膜からなる積層体のうち
少なくとも１層が、平均重合度２０００〜３０００のポ
リビニルアセタール樹脂（Ａ）と、平均重合度が３００
〜６００のポリビニルアセタール樹脂（Ｂ）とを含む混
合体である。この平均重合度が２０００〜３０００の高
重合度のポリビニルアセタール樹脂（Ａ）を用いること
により、合わせガラスの遮音性能が、広い温度範囲にわ
たり、特に低温域で良好となる。この平均重合度が２０
００より低いと、良好な遮音性能を示す温度範囲が広く
ならず、３０００より高いと、遮音性能は広い温度範囲
にわたり良好であるが、高温での流動性が高くなり過
ぎ、成形性が悪くなる。In the interlayer film for laminated glass according to the present invention,
In order to obtain good sound insulation performance over a wide temperature range, at least one of the laminates composed of a plurality of polyvinyl acetal resin films has a polyvinyl acetal resin (A) having an average degree of polymerization of 2000 to 3000 and an average degree of polymerization of 300.
And a polyvinyl acetal resin (B). By using the polyvinyl acetal resin (A) having a high degree of polymerization having an average degree of polymerization of 2000 to 3000, the sound insulation performance of the laminated glass is improved over a wide temperature range, particularly in a low temperature range. This average degree of polymerization is 20
If it is lower than 00, the temperature range showing good sound insulation performance is not widened, and if it is higher than 3000, the sound insulation performance is good over a wide temperature range, but the fluidity at high temperatures becomes too high and the moldability deteriorates. .

【００２５】もっとも、２０００〜３０００の平均重合
度のポリビニルアセタール樹脂（Ａ）は、高温での流動
性が比較的高く、場合によっては成形性に悪影響を与え
る可能性がある。そこで、本発明では、平均重合度が３
００〜６００の低重合度のポリビニルアセタール樹脂
（Ｂ）を上記特定の割合で混合することにより、低重合
度のポリビニルアセタール樹脂（Ｂ）が可塑剤のように
作用し、高温域での高流動性を抑制することが可能とさ
れている。しかも、通常の低分子の可塑剤とは異なり、
ブリードアウト等の恐れもない。However, the polyvinyl acetal resin (A) having an average degree of polymerization of 2000 to 3000 has a relatively high flowability at a high temperature, and may adversely affect the moldability in some cases. Therefore, in the present invention, the average degree of polymerization is 3
By mixing the polyvinyl acetal resin (B) having a low degree of polymerization of 00 to 600 at the above specific ratio, the polyvinyl acetal resin (B) having a low degree of polymerization acts like a plasticizer, and has a high flow rate in a high temperature range. It is possible to suppress the nature. Moreover, unlike ordinary low-molecular plasticizers,
There is no fear of bleeding out.

【００２６】上記低重合度のポリビニルアセタール樹脂
（Ｂ）の重合度が３００より低い場合には、ＰＶＡの合
成が非常に困難であり、確実に量産することができず、
逆に６００より高いと、高重合度のポリビニルアセター
ル樹脂（Ａ）に対する可塑化効果が発現しない。When the degree of polymerization of the polyvinyl acetal resin (B) having a low degree of polymerization is lower than 300, it is very difficult to synthesize PVA, and mass production cannot be ensured.
Conversely, if it is higher than 600, the plasticizing effect on the polyvinyl acetal resin (A) having a high degree of polymerization will not be exhibited.

【００２７】低重合度のポリビニルアセタール樹脂
（Ｂ）の可塑化効果を高めるために、本発明では、ポリ
ビニルアセタール樹脂（Ａ）とポリビニルアセタール樹
脂（Ｂ）の平均重合度の差は１５００以上とされてい
る。この重合度の差が１５００より小さいと、低重合度
のポリビニルアセタール樹脂（Ｂ）による可塑化効果が
低くなる。In order to enhance the plasticizing effect of the polyvinyl acetal resin (B) having a low polymerization degree, in the present invention, the difference between the average polymerization degrees of the polyvinyl acetal resin (A) and the polyvinyl acetal resin (B) is 1500 or more. ing. If the difference in the degree of polymerization is less than 1500, the plasticizing effect of the polyvinyl acetal resin (B) having a low degree of polymerization will be low.

【００２８】低重合度のポリビニルアセタール樹脂
（Ｂ）は、高重合度のポリビニルアセタール樹脂（Ａ）
１００重量部に対し、３〜８重量部の割合で混合され
る。３重量％より混合割合が低いと、ポリビニルアセタ
ール樹脂（Ｂ）による可塑化効果が発現せず、８重量部
より高くなると、低重合度のポリビニルアセタール樹脂
（Ｂ）自身の働きが強くなり、高重合度のポリビニルア
セタール樹脂（Ａ）により得られる広い温度範囲にわた
る良好な遮音性能が失われる。The low polymerization degree polyvinyl acetal resin (B) is a high polymerization degree polyvinyl acetal resin (A).
It is mixed at a ratio of 3 to 8 parts by weight with respect to 100 parts by weight. If the mixing ratio is lower than 3% by weight, the plasticizing effect of the polyvinyl acetal resin (B) is not exhibited, and if the mixing ratio is higher than 8 parts by weight, the function of the polyvinyl acetal resin (B) having a low degree of polymerization becomes strong, and Good sound insulation performance over a wide temperature range obtained by the polyvinyl acetal resin (A) having a degree of polymerization is lost.

【００２９】上記ポリビニルアセタール樹脂（Ａ）及び
ポリビニルアセタール樹脂（Ｂ）の混合方法は特に限定
されないが、以下の２つの方法を例示することができ
る。まず第１の方法では、平均重合度が異なるポリビニ
ルアルコールを所定量混合した後、アセタール化反応を
行い、混合ポリビニルアセタール樹脂を得る方法であ
る。第２の方法は、平均重合度が異なる各ポリビニルア
ルコールをそれぞれアセタール化反応させて得られた各
ポリビニルアセタール樹脂を、所定量混合する方法であ
る。The method of mixing the polyvinyl acetal resin (A) and the polyvinyl acetal resin (B) is not particularly limited, but the following two methods can be exemplified. First, the first method is a method in which a predetermined amount of polyvinyl alcohols having different average degrees of polymerization are mixed and then an acetalization reaction is performed to obtain a mixed polyvinyl acetal resin. The second method is a method of mixing a predetermined amount of each polyvinyl acetal resin obtained by causing each polyvinyl alcohol having a different average polymerization degree to undergo an acetalization reaction.

【００３０】積層体中において、他のポリビニルアセタ
ール樹脂膜については、合わせガラス用中間膜として一
般的な平均重合度を有するポリビニルアセタール樹脂膜
を用いて構成することができ、中間膜としての良好な機
械的強度及び成形性を得るには、平均重合度が１０００
〜２０００の範囲のポリビニルアセタール樹脂膜が好適
に用いられる。In the laminate, the other polyvinyl acetal resin film can be constituted by using a polyvinyl acetal resin film having a general average degree of polymerization as an interlayer film for laminated glass. To obtain mechanical strength and moldability, the average degree of polymerization is 1000
A polyvinyl acetal resin film in the range of 2000 is preferably used.

【００３１】上記ポリビニルアセタール樹脂の調製に用
いられるアルデヒドとしては、例えば、ホルムアルデヒ
ド、アセトアルデヒド、プロピオンアルデヒド、ｎ−ブ
チルアルデヒド、イソブチルアルデヒド、バレルアルデ
ヒド、ｎ−ヘキシルアルデヒド、２−エチルブチルアル
デヒド、ベンズアルデヒド、シンナムアルデヒドなどが
挙げられる。The aldehyde used for preparing the polyvinyl acetal resin includes, for example, formaldehyde, acetaldehyde, propionaldehyde, n-butyraldehyde, isobutyraldehyde, valeraldehyde, n-hexylaldehyde, 2-ethylbutyraldehyde, benzaldehyde, cinnaaldehyde And aldehyde.

【００３２】上記各種ポリビニルアセタール樹脂は単独
で用いられてもよく、２種以上併用されてもよい。中で
も、ｎ−ブチルアルデヒドでアセタール化して得られる
ポリビニルブチラール樹脂が好ましく用いられる。The above polyvinyl acetal resins may be used alone or in combination of two or more. Among them, a polyvinyl butyral resin obtained by acetalization with n-butyraldehyde is preferably used.

【００３３】ポリビニルアセタール樹脂の中でもポリビ
ニルブチラール樹脂を用いることにより、ポリビニルブ
チラール樹脂膜及び中間膜の透明性、耐侯性及びガラス
に対する接着性がより優れたものとなる。By using a polyvinyl butyral resin among the polyvinyl acetal resins, the transparency, weather resistance and adhesion to glass of the polyvinyl butyral resin film and the intermediate film are further improved.

【００３４】本発明において用いられるポリビニルアセ
タール樹脂膜は、可塑剤により可塑化されたものであ
る。可塑剤としては、特に限定されず、例えば一塩基酸
エステル系、多塩基酸エステル系などの有機エステル系
可塑剤；あるいは有機リン酸系、有機亜リン酸系などの
リン酸系可塑剤が好適に用いられる。The polyvinyl acetal resin film used in the present invention has been plasticized with a plasticizer. The plasticizer is not particularly limited, and is preferably, for example, an organic ester plasticizer such as a monobasic acid ester or a polybasic acid ester; or a phosphoric acid plasticizer such as an organic phosphoric acid or an organic phosphorous acid. Used for

【００３５】具体的には、一塩基酸エステル系可塑剤の
中では、トリエチレングリコール、トリプロピレングリ
コール、テトラエチレングリコール等のグリコールと、
酪酸、イソ酪酸、カプロン酸、２−エチル酪酸、ヘプタ
ン酸、２−エチルヘキシル酸等の有機酸との反応によっ
て得られたグリコール系エステル等が挙げられる。Specifically, among the monobasic acid ester-based plasticizers, glycols such as triethylene glycol, tripropylene glycol, and tetraethylene glycol;
Glycol esters obtained by reaction with organic acids such as butyric acid, isobutyric acid, caproic acid, 2-ethylbutyric acid, heptanoic acid and 2-ethylhexylic acid.

【００３６】多塩基酸エステル系可塑剤としては、例え
ば、単素数４〜８の直鎖状もしくは分岐状アルコール
と、アジピン酸、セバチン酸、アゼライン酸等の有機酸
との反応によって得られるエステル等が挙げられる。Examples of the polybasic acid ester-based plasticizer include esters obtained by reacting a linear or branched alcohol having 4 to 8 primates with an organic acid such as adipic acid, sebacic acid and azelaic acid. Is mentioned.

【００３７】また、リン酸系可塑剤としては、トリブト
キシエチルフォスフェート、イソデシルフェニルホスフ
ェート等が挙げられる。上記各種可塑剤の中でも、例え
ば、トリエチレングリコール−ジ−２−エチルブチレー
ト（３ＧＨ）、トリエチレングリコール−ジ−２−エチ
ルヘキサノエート（３ＧＯ）、トリエチレングリコール
−ジ−ｎ−ヘプタノエート（３Ｇ７）、トリエチレング
リコールジカプリレート、トリエチレングリコール−ジ
−ｎ−オクトエート、テトラエチレングリコール−ジ−
２−エチルブチレート、テトラエチレングリコール−ジ
−ｎ−ヘプタノエート、ジヘキシルアジペート、ジベン
ジルフタレート等が好適に用いられ、中でも特に好適に
用いられるのは、３ＧＨ、３ＧＯ、３Ｇ７等である。[0037] Examples of the phosphoric acid plasticizer include tributoxyethyl phosphate, isodecylphenyl phosphate and the like. Among the various plasticizers, for example, triethylene glycol-di-2-ethylbutyrate (3GH), triethylene glycol-di-2-ethylhexanoate (3GO), and triethylene glycol-di-n-heptanoate (3GO) 3G7), triethylene glycol dicaprylate, triethylene glycol di-n-octoate, tetraethylene glycol di-
2-ethyl butyrate, tetraethylene glycol-di-n-heptanoate, dihexyl adipate, dibenzyl phthalate and the like are preferably used, and particularly preferably used are 3GH, 3GO, 3G7 and the like.

【００３８】上記可塑剤は、単独で用いられても良い
し、２種類以上併用されても良い。上記ポリビニルアセ
タール樹脂に対する可塑剤の添加量は特に限定されない
が、ポリビニルアセタール樹脂１００重量部に対し、可
塑剤３０〜７０重量部の範囲とすることが望ましい。The above plasticizers may be used alone or in combination of two or more. The amount of the plasticizer added to the polyvinyl acetal resin is not particularly limited, but is preferably in the range of 30 to 70 parts by weight of the plasticizer based on 100 parts by weight of the polyvinyl acetal resin.

【００３９】可塑剤の添加割合が３０重量部未満では、
ポリビニルアセタール樹脂の可塑化が不十分となること
があり、逆に７０重量部を超えると、ポリビニルアセタ
ール樹脂膜及び中間膜の力学的特性やガラスに対する接
着力が不十分となることがある。If the addition ratio of the plasticizer is less than 30 parts by weight,
In some cases, the plasticization of the polyvinyl acetal resin is insufficient. On the other hand, when it exceeds 70 parts by weight, the mechanical properties of the polyvinyl acetal resin film and the interlayer film and the adhesive strength to glass may be insufficient.

【００４０】上記ポリビニルアセタール樹脂と可塑剤と
の組み合わせの中でも、ポリビニルアセタール樹脂とし
てポリビニルブチラール樹脂を用い、可塑剤として３Ｇ
Ｈ、３ＧＯ及び３Ｇ７からなる群より選択される少なく
とも１種を用いる組み合わせが、中間膜の力学特性及び
ガラスに対する接着性の上で特に好ましい。Among the combinations of the polyvinyl acetal resin and the plasticizer, a polyvinyl butyral resin is used as the polyvinyl acetal resin, and 3G is used as the plasticizer.
A combination using at least one selected from the group consisting of H, 3GO and 3G7 is particularly preferable in terms of the mechanical properties of the interlayer film and the adhesion to glass.

【００４１】本発明に係る合わせガラス用中間膜は、上
記のように、ポリビニルアセタール樹脂（Ａ）及びポリ
ビニルアセタール樹脂（Ｂ）との混合体からなる少なく
とも１層のポリビニルアセタール樹脂膜を含む積層体か
らなる。この場合、平均重合度が異なっているアセター
ル樹脂混合膜を「混合膜」と表現し、通常のポリビニル
アセタール樹脂膜を「通常膜」と表現した場合、次のよ
うな積層構造を採用することができる。As described above, the interlayer film for laminated glass according to the present invention is a laminate including at least one layer of a polyvinyl acetal resin film composed of a mixture of the polyvinyl acetal resin (A) and the polyvinyl acetal resin (B). Consists of In this case, when an acetal resin mixed film having a different average polymerization degree is expressed as a “mixed film”, and a normal polyvinyl acetal resin film is expressed as a “normal film”, the following laminated structure may be employed. it can.

【００４２】「通常膜」／「混合膜」、「通常膜」／
「混合膜」／「通常膜」、「通常膜」／「混合膜」／
「通常膜」／「混合膜」／「通常膜」、「混合膜」／
「通常膜」／「混合膜」などである。すなわち、通常膜
と混合膜の積層体については特に限定されない。また、
複数のポリビニルアセタール樹脂膜の積層数についても
特に限定されない。"Normal film" / "Mixed film", "Normal film" /
"Mixed film" / "Normal film", "Normal film" / "Mixed film" /
“Normal film” / “Mixed film” / “Normal film”, “Mixed film” /
"Normal film" / "mixed film". That is, the stacked body of the normal film and the mixed film is not particularly limited. Also,
The number of layers of a plurality of polyvinyl acetal resin films is not particularly limited.

【００４３】合わせガラス用中間膜の全体としての厚み
は、通常の合わせガラス用中間膜としての厚みである
０．３〜１．６ｍｍの範囲が好ましい。中間膜の厚みが
大きい程、遮音性能は高められるが、合わせガラスとし
て必要な耐貫通性を考慮すると、実用上、上記範囲とす
ることが好ましい。The total thickness of the interlayer film for laminated glass is preferably in the range of 0.3 to 1.6 mm, which is the thickness of an ordinary interlayer film for laminated glass. The greater the thickness of the interlayer, the higher the sound insulation performance. However, in consideration of the penetration resistance required as a laminated glass, the above range is practically preferable.

【００４４】合わせガラス用中間膜の成膜方法について
も特に限定されず、例えば、上記各ポリビニルアセター
ル樹脂膜をそれぞれ別途成形した後、一対の板状透明体
間に積層する方法、各ポリビニルアセタール樹脂膜を多
層成形機を用いて一体成形して合わせガラス用中間膜を
得る方法など、任意である。The method for forming the interlayer film for laminated glass is not particularly limited. For example, a method in which each of the above-mentioned polyvinyl acetal resin films is separately formed and then laminated between a pair of plate-shaped transparent bodies, Any method may be used, such as a method of integrally forming a film using a multilayer forming machine to obtain an interlayer film for laminated glass.

【００４５】合わせガラス用中間膜を板状透明体間に挟
持して合わせガラスを製造する方法についても、通常の
合わせガラスの製造方法を適宜採用することができる。
例えば、合わせガラス用中間膜を両側からガラス板で挟
み込み、熱圧プレスにより合わせガラスを製造する方法
を用いることができる。As for the method of manufacturing a laminated glass by sandwiching the interlayer film for a laminated glass between the plate-shaped transparent bodies, an ordinary method of manufacturing a laminated glass can be appropriately adopted.
For example, a method in which an interlayer film for laminated glass is sandwiched between glass plates from both sides and a laminated glass is manufactured by hot-pressing can be used.

【００４６】さらに、本発明においては、板状透明体と
しては、板ガラスの他、ガラス以外の透明体からなるも
の、例えばポリカーボネート樹脂からなるものも用いる
ことができ、すなわち上述したポリビニルアセタール樹
脂膜よりも剛性が高い適宜の板状透明体を用いることが
できる。Further, in the present invention, as the plate-shaped transparent body, one made of a transparent body other than glass, for example, one made of a polycarbonate resin can be used in addition to the plate glass. Also, an appropriate plate-shaped transparent body having high rigidity can be used.

【００４７】[0047]

【発明の実施の形態】以下、本発明の具体的な実施例及
び比較例を挙げることにより、本発明を明らかにする。
なお、以下において、合わせガラスの遮音性能の測定
は、下記の方法により行った。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be clarified by giving specific examples and comparative examples of the present invention.
In the following, the sound insulation performance of the laminated glass was measured by the following method.

【００４８】合わせガラスの遮音性能…所定温度におい
て、合わせガラスをダンピング試験用振動発生機（振研
社製加振機、品番：Ｇ２１−００５Ｄ）により加振し、
得られる振動特性を機械インピーダンスアンプ（リオン
社製、品番：ＸＧ−８１）により増幅し、得られた振動
スペクトルをＦＦＴアナライザー（横河ヒューレットパ
ッカー社製、商品名：ＦＦＴスペクトラムアナライザー
ＨＰ３５８２ＡＡ）にて解析した。このようにして得ら
れた損失係数と、ガラスとの共振周波数との比から透過
損失を算出した。この結果に基づき、周波数２０００Ｈ
ｚ近辺における極小の透過損失をＴＬ値とした。なお、
測定は０〜＋３０℃の間、１０℃間隔にて行った。ま
た、以下の実施例及び比較例では、合わせガラス用中間
膜の成形性を評価したが、評価方法は官能評価により行
った。Sound insulation performance of laminated glass: At a predetermined temperature, the laminated glass was vibrated by a vibration generator for vibration damping test (vibrator manufactured by Shinken Co., Ltd., product number: G21-005D).
The obtained vibration characteristics are amplified by a mechanical impedance amplifier (manufactured by Rion, product number: XG-81), and the obtained vibration spectrum is analyzed by an FFT analyzer (manufactured by Yokogawa Hewlett Packer, trade name: FFT Spectrum Analyzer HP3582AA). did. The transmission loss was calculated from the ratio between the thus obtained loss coefficient and the resonance frequency with glass. Based on this result, the frequency 2000H
The minimum transmission loss near z was taken as the TL value. In addition,
The measurement was performed at 10 ° C intervals between 0 and + 30 ° C. In the following Examples and Comparative Examples, the moldability of the interlayer film for laminated glass was evaluated, but the evaluation was performed by sensory evaluation.

【００４９】（実施例１）下記の２種類の可塑化ポリビ
ニルアセタール樹脂膜Ｘ，Ｙを作製し、これらを用いて
合わせガラス用中間膜を作製した。Example 1 The following two types of plasticized polyvinyl acetal resin films X and Y were produced, and an intermediate film for laminated glass was produced using these films.

【００５０】（樹脂膜Ｘの作製）ポリビニルブチラール
樹脂（以下、ＰＶＢと略す。平均重合度１７００、ブチ
ラール化度６５．９モル％、アセチル基量０．９モル
％）１００重量部に、可塑剤としてトリエチレングリコ
ール−ジ−２−エチルブチレート（３ＧＨ）を４０重量
部添加した。これらの混合物をミキシングロールで十分
に混練し、混練物の所定量をプレス成形機で１５０℃で
３０分間保持し、厚み０．２ｍｍのポリビニルブチラー
ル樹脂膜Ｘを作製した。(Preparation of Resin Film X) 100 parts by weight of a polyvinyl butyral resin (hereinafter abbreviated as PVB; average polymerization degree 1700, butyralization degree 65.9 mol%, acetyl group content 0.9 mol%), and a plasticizer And 40 parts by weight of triethylene glycol-di-2-ethyl butyrate (3GH). The mixture was sufficiently kneaded with a mixing roll, and a predetermined amount of the kneaded material was held at 150 ° C. for 30 minutes by a press molding machine to produce a polyvinyl butyral resin film X having a thickness of 0.2 mm.

【００５１】（樹脂膜Ｙの作製）予め、平均重合度＝２
８００のポリビニルアルコール（以下、ＰＶＡ）１００
重量部に対し、平均重合度＝５００のＰＶＡを５重量部
混合した。このＰＶＡ混合物から、ブチラール化度６
０．２モル％、アセチル基量１１．９モル％のＰＶＢ樹
脂を合成した。得られたＰＶＢ樹脂１００重量部に、可
塑剤として３ＧＨを６０重量部添加した。この混合物を
ミキシングロールで十分に混練し、混練物の所定量をプ
レス成形機で１５０℃で３０分間保持し、厚み０．４ｍ
ｍのポリビニルブチラール樹脂膜Ｙを作製した。(Preparation of Resin Film Y) An average degree of polymerization = 2
800 polyvinyl alcohol (PVA) 100
5 parts by weight of PVA having an average polymerization degree of 500 was mixed with the parts by weight. From this PVA mixture, a butyralization degree of 6
A PVB resin having 0.2 mol% and an acetyl group content of 11.9 mol% was synthesized. To 100 parts by weight of the obtained PVB resin, 60 parts by weight of 3GH was added as a plasticizer. This mixture is sufficiently kneaded with a mixing roll, and a predetermined amount of the kneaded material is held at 150 ° C. for 30 minutes by a press molding machine, and the thickness is 0.4 m
m of a polyvinyl butyral resin film Y was prepared.

【００５２】（積層膜及び合わせガラスの作製）上記の
ように得られたポリビニルブチラール樹脂膜Ｘ，Ｙを、
図１に示すように積層構成がポリビニルブチラール樹脂
膜Ｘ／ポリビニルブチラール樹脂膜Ｙ／ポリビニルブチ
ラール樹脂膜Ｘとなるように積層し、３層構造の合わせ
ガラス用中間膜１を得た。(Preparation of Laminated Film and Laminated Glass) The polyvinyl butyral resin films X and Y obtained as described above were
As shown in FIG. 1, the laminated structure was a polyvinyl butyral resin film X / polyvinyl butyral resin film Y / polyvinyl butyral resin film X to obtain an interlayer film 1 for laminated glass having a three-layer structure.

【００５３】次に、上記中間膜を、一辺が３００ｍｍで
ある正方形の厚み３ｍｍのフロートガラス２枚で両側か
らサンドイッチし、この未圧着サンドイッチ体をゴムバ
ッグに入れ、２．６７ｋＰａの真空度で２０分間脱気し
た。しかる後脱気状態のまま９０℃のオーブンに移し、
３０分間保持した。このようにして真空プレスにより、
仮接着されたサンドイッチ体を、次に、オートクレーブ
内で圧力１１７０ｋＰａ及び温度１３５℃で熱圧着し、
透明な合わせガラスを作製した。得られた合わせガラス
を用い、上述した評価方法に従って、遮音性能を評価し
た。合わせガラス用中間膜の構成及び評価結果を下記の
表１に示す。Next, the above-mentioned intermediate film was sandwiched from both sides with two square 3 mm-thick float glasses each having a side of 300 mm, and this unpressed sandwich body was put into a rubber bag, and the sandwich was placed at a degree of vacuum of 2.67 kPa. Degassed for a minute. After that, transfer it to a 90 ° C oven while keeping it in a degassed state.
Hold for 30 minutes. Thus, by the vacuum press,
Next, the sandwich body temporarily bonded is thermocompression-bonded in an autoclave at a pressure of 1170 kPa and a temperature of 135 ° C.
A transparent laminated glass was produced. Using the obtained laminated glass, the sound insulation performance was evaluated according to the evaluation method described above. The structure and evaluation results of the interlayer film for laminated glass are shown in Table 1 below.

【００５４】（実施例２） （ＰＶＢ樹脂膜Ｘの作製）ＰＶＢ樹脂（平均重合度＝１
７００、ブチラール化度＝６８．９モル％、アセチル基
量＝０．９モル％）１００重量部に、可塑剤としてトリ
エチレングリコール−ジ−２−エチルヘキサノエート
（３ＧＯ）３９重量部を添加した。混合物を用いたこと
を除いては、実施例１と同様にして、厚み０．２ｍｍの
ＰＶＢ樹脂膜Ｘを作製した。(Example 2) (Preparation of PVB resin film X) PVB resin (average degree of polymerization = 1)
700, butyralization degree = 68.9 mol%, acetyl group content = 0.9 mol%), and triethylene glycol-di-2-ethylhexanoate (3GO) 39 parts by weight as a plasticizer is added to 100 parts by weight. did. Except that a mixture was used, a PVB resin film X having a thickness of 0.2 mm was produced in the same manner as in Example 1.

【００５５】（ＰＶＢ樹脂膜Ｙの作製）予め、平均重合
度＝２８００ＰＶＡに平均重合度＝５００のＰＶＡを実
施例１と同様に５重量％混合してなる混合物を用意し、
該混合物からブチラール化度６４．０モル％及びアセチ
ル基量１３．５モル％のＰＶＢ樹脂を合成した。得られ
たＰＶＢ樹脂１００重量部に、可塑剤として３ＧＯを６
０重量部添加した。これを実施例１と同様にして、厚み
０．４ｍｍのＰＶＢ樹脂膜Ｙを作製した。得られたＰＶ
Ｂ樹脂膜Ｘ，Ｙを用い、実施例１と同様にして３層構造
の中間膜を作製した後、合わせガラスを作製し、評価し
た。(Preparation of PVB Resin Film Y) A mixture was prepared in advance by mixing 5% by weight of PVA having an average degree of polymerization of 500 with 2800 PVA in the same manner as in Example 1.
From the mixture, a PVB resin having a butyralization degree of 64.0 mol% and an acetyl group content of 13.5 mol% was synthesized. To 100 parts by weight of the obtained PVB resin, 6 GO as a plasticizer was added.
0 parts by weight were added. In the same manner as in Example 1, a PVB resin film Y having a thickness of 0.4 mm was produced. Obtained PV
Using the B resin films X and Y, an intermediate film having a three-layer structure was manufactured in the same manner as in Example 1, and then a laminated glass was manufactured and evaluated.

【００５６】（実施例３） （ＰＶＢ樹脂膜Ｘの作製）実施例２と同様にしてＰＶＢ
樹脂膜Ｘを作製した。(Example 3) (Preparation of PVB resin film X)
A resin film X was produced.

【００５７】（ＰＶＢ樹脂膜Ｙの作製）平均重合度＝２
４００のＰＶＡ１００重量部に、平均重合度＝５００の
ＰＶＡを３重量部混合し、得られたＰＶＡ混合物から、
ブチラール化度＝６４．０モル％、アセチル基量＝１
３．５モル％のＰＶＢ樹脂を合成した。得られたＰＶＢ
樹脂１００重量部に、可塑剤として３ＧＯを６０重量部
添加した。この混合物を用い、実施例１と同様にして、
厚み０．４ｍｍのＰＶＢ樹脂膜Ｙを作製した。得られた
ＰＶＢ樹脂膜Ｘ，Ｙを用い、実施例１と同様にして３層
構造の中間膜を作製した後、合わせガラスを作製し、評
価した。(Preparation of PVB Resin Film Y) Average Degree of Polymerization = 2
To 100 parts by weight of PVA of 400, 3 parts by weight of PVA having an average degree of polymerization of 500 was mixed, and from the obtained PVA mixture,
Butyralization degree = 64.0 mol%, acetyl group content = 1
A 3.5 mol% PVB resin was synthesized. PVB obtained
60 parts by weight of 3GO as a plasticizer was added to 100 parts by weight of the resin. Using this mixture, in the same manner as in Example 1,
A 0.4 mm thick PVB resin film Y was produced. Using the obtained PVB resin films X and Y, an intermediate film having a three-layer structure was produced in the same manner as in Example 1, and then a laminated glass was produced and evaluated.

【００５８】（実施例４） （ＰＶＢ樹脂膜Ｘの作製）平均重合度＝２４００のＰＶ
Ａ１００重量部に対し、平均重合度＝５００ＰＶＡを３
重量部混合した。このＰＶＡ混合物から、ブチラール化
度＝６８．９モル％及びアセチル基量＝０．９モル％の
ＰＶＢ樹脂を合成した。Example 4 (Preparation of PVB Resin Film X) PV of Average Degree of Polymerization = 2400
Average polymerization degree = 500 PVA per 100 parts by weight of A
Parts by weight were mixed. From this PVA mixture, a PVB resin having a butyralization degree of 68.9 mol% and an acetyl group content of 0.9 mol% was synthesized.

【００５９】得られたＰＶＢ樹脂１００重量部に、可塑
剤としてトリエチレングリコール−ジ−ｎ−ヘプタネー
ト（３Ｇ７）を４０重量部添加した。この混合物を用
い、実施例１と同様にして厚み０．２ｍｍのＰＶＢ樹脂
膜Ｘを作製した。To 100 parts by weight of the obtained PVB resin, 40 parts by weight of triethylene glycol-di-n-heptane (3G7) was added as a plasticizer. Using this mixture, a PVB resin film X having a thickness of 0.2 mm was produced in the same manner as in Example 1.

【００６０】（ＰＶＢ樹脂膜Ｙの作製）実施例３のＰＶ
Ｂ樹脂膜作製において、可塑剤として３ＧＯに代えて、
３Ｇ７を用いたことを除いては、実施例３のＰＶＢ樹脂
膜Ｙの製造方法と同様にして、厚み０．４ｍｍのＰＶＢ
樹脂膜Ｙを得た。得られたＰＶＢ樹脂膜Ｘ，Ｙを用い、
実施例１と同様にして３層構造の中間膜を作製した後、
合わせガラスを作製し、評価した。(Preparation of PVB Resin Film Y)
In producing the B resin film, instead of 3GO as a plasticizer,
Except that 3G7 was used, a 0.4 mm-thick PVB resin film Y was manufactured in the same manner as in the method of manufacturing the PVB resin film Y of Example 3.
A resin film Y was obtained. Using the obtained PVB resin films X and Y,
After producing an intermediate film having a three-layer structure in the same manner as in Example 1,
Laminated glass was produced and evaluated.

【００６１】（比較例１） （ＰＶＢ樹脂膜Ｘの作製）ＰＶＢ樹脂（平均重合度＝１
７００、ブチラール化度＝６８．９モル％、アセチル基
量＝０．９モル％）１００重量部に、可塑剤として３Ｇ
Ｏを３９重量部添加した。この混合物を用い、実施例１
のＰＶＢ樹脂膜Ｘの製造方法と同様にして、厚み０．２
ｍｍのＰＶＢ樹脂膜Ｘを作製した。(Comparative Example 1) (Preparation of PVB resin film X) PVB resin (average degree of polymerization = 1)
700, butyral degree = 68.9 mol%, acetyl group content = 0.9 mol%)
39 parts by weight of O was added. Example 1 using this mixture
In the same manner as in the method for producing the PVB resin film X of
mm of PVB resin film X was produced.

【００６２】（ＰＶＢ樹脂膜Ｙの作製）ＰＶＢ樹脂（平
均重合度＝１７００、ブチラール化度＝６４．０モル
％、アセチル基量＝１３．５モル％）１００重量部に、
可塑剤として３ＧＯを６０重量部添加し、この混合物を
用い、実施例１と同様にして、厚み０．４ｍｍのＰＶＢ
樹脂膜Ｙを作製した。得られたＰＶＢ樹脂膜Ｘ，Ｙを用
い、実施例１と同様にして３層構造の中間膜を作製した
後、合わせガラスを作製し、評価した。(Preparation of PVB Resin Film Y) To 100 parts by weight of PVB resin (average degree of polymerization = 1700, butyralization degree = 64.0 mol%, acetyl group content = 13.5 mol%)
As a plasticizer, 60 parts by weight of 3GO was added, and this mixture was used.
A resin film Y was produced. Using the obtained PVB resin films X and Y, an intermediate film having a three-layer structure was produced in the same manner as in Example 1, and then a laminated glass was produced and evaluated.

【００６３】（比較例２） （ＰＶＢ樹脂膜Ｘの作製）比較例１と同様にしてＰＶＢ
樹脂膜Ｘを作製した。(Comparative Example 2) (Preparation of PVB Resin Film X)
A resin film X was produced.

【００６４】（ＰＶＢ樹脂膜Ｙの作製）ＰＶＢ樹脂（平
均重合度＝２８００、ブチラール化度＝６４．０モル
％、アセチル基量＝１３．５モル％）１００重量部に対
し、可塑剤として３ＧＯを６０重量部添加した。これを
用い、実施例１と同様にして、厚み０．４ｍｍのＰＶＢ
樹脂膜Ｙを作製した。得られたＰＶＢ樹脂膜Ｘ，Ｙを用
い、実施例１と同様にして３層構造の中間膜を作製した
後、合わせガラスを作製し、評価した。(Preparation of PVB Resin Film Y) 100 parts by weight of PVB resin (average degree of polymerization = 2800, degree of butyralization = 64.0 mol%, acetyl group content = 13.5 mol%), and 3GO as a plasticizer were used. Was added in an amount of 60 parts by weight. Using this, in the same manner as in Example 1, a 0.4 mm thick PVB
A resin film Y was produced. Using the obtained PVB resin films X and Y, an intermediate film having a three-layer structure was produced in the same manner as in Example 1, and then a laminated glass was produced and evaluated.

【００６５】（比較例３） （ＰＶＢ樹脂膜Ｘの作製）実施例１と同様にしてＰＶＢ
樹脂膜Ｘを作製した。(Comparative Example 3) (Preparation of PVB resin film X)
A resin film X was produced.

【００６６】（ＰＶＢ樹脂膜Ｙの作製）平均重合度＝２
８００のＰＶＡ樹脂１００重量部に、平均重合度＝１７
００のＰＶＡを５重量部混合し、得られたＰＶＡ混合物
から、ブチラール化度＝６０．２モル％、アセチル基量
＝１１．９モル％のＰＶＢ樹脂を合成した。(Preparation of PVB Resin Film Y) Average Degree of Polymerization = 2
100 parts by weight of 800 PVA resin, average degree of polymerization = 17
Then, 5 parts by weight of PVA No. 00 were mixed, and a PVB resin having a butyralization degree of 60.2 mol% and an acetyl group content of 11.9 mol% was synthesized from the obtained PVA mixture.

【００６７】得られたＰＶＢ樹脂１００重量部に、可塑
剤として３ＧＨを６０重量部添加した。この混合物を用
い、実施例１と同様にして、厚み０．４ｍｍのＰＶＢ樹
脂膜Ｙを作製した。To 100 parts by weight of the obtained PVB resin, 60 parts by weight of 3GH was added as a plasticizer. Using this mixture, a PVB resin film Y having a thickness of 0.4 mm was produced in the same manner as in Example 1.

【００６８】得られたＰＶＢ樹脂膜Ｘ，Ｙを用い、実施
例１と同様にして３層構造の中間膜を作製した後、合わ
せガラスを作製し、評価した。Using the obtained PVB resin films X and Y, an intermediate film having a three-layer structure was produced in the same manner as in Example 1, and then a laminated glass was produced and evaluated.

【００６９】[0069]

【表１】 [Table 1]

【００７０】表１から明らかなように、比較例１の合わ
せガラス用中間膜を用いた場合、−１０℃の低温域で、
ＴＬ値が低下し、十分な遮音性能が得られなかった。ま
た、比較例２の合わせガラス用中間膜を用いた場合、や
はり−１０℃でＴＬ値が３３ｄＢと若干低く、かつ成形
性が十分でないためか、合わせガラス用中間膜の膜厚に
ばらつきが生じた。As is clear from Table 1, when the interlayer film for laminated glass of Comparative Example 1 was used, at a low temperature range of -10 ° C.,
The TL value was lowered, and sufficient sound insulation performance was not obtained. Also, when the interlayer film for laminated glass of Comparative Example 2 was used, the TL value at -10 ° C. was slightly lower at 33 dB, and the moldability was not sufficient. Was.

【００７１】これに対して、実施例１〜４の各合わせガ
ラス用中間膜では、成形性が良好であり、膜厚のばらつ
きも見られず、かつ−１０℃〜＋３０℃の広い温度範囲
にわたり、ＴＬ値の低下が見られず、良好な遮音性能を
示すことが確かめられた。On the other hand, in each of the interlayer films for laminated glass of Examples 1 to 4, the moldability was good, there was no variation in the film thickness, and over a wide temperature range from -10 ° C. to + 30 ° C. , TL value was not reduced, and good sound insulation performance was confirmed.

【００７２】[0072]

【発明の効果】本発明に係る合わせガラス用中間膜で
は、複数枚の可塑化されたポリビニルアセタール樹脂膜
よりなり、少なくとも１層のポリビニルアセタール樹脂
膜が、平均重合度２０００〜３０００のポリビニルアセ
タール樹脂（Ａ）と、平均重合度が３００〜６００の範
囲にあり、かつポリビニルアセタール樹脂（Ａ）との平
均重合度の差が１５００以上であるポリビニルアセター
ル樹脂（Ｂ）との混合体からなり、ポリビニルアセター
ル樹脂（Ｂ）は、ポリビニルアセタール樹脂（Ａ）１０
０重量部に対し、３〜８重量部の割合で混合されてい
る。従って、高重合度のポリビニルアセタール樹脂
（Ａ）により広い温度範囲にわたり良好な遮音性能が発
揮され、しかも低重合度のポリビニルアセタール樹脂
（Ｂ）が上記特定の割合で混合されているので、成形性
が損なわれることもない。よって、可塑化されたポリビ
ニルアセタール樹脂膜からなり、機械的強度やガラスに
対する接着性などの合わせガラス用中間膜としての基本
的な性能を満たしつつ、広い温度範囲にわたり、特に低
温域において良好な遮音性能を発現する合わせガラス用
中間膜を提供することが可能となる。The interlayer film for laminated glass according to the present invention comprises a plurality of plasticized polyvinyl acetal resin films, and at least one layer of the polyvinyl acetal resin film has an average degree of polymerization of 2000 to 3000. A mixture of (A) and a polyvinyl acetal resin (B) having an average degree of polymerization in the range of 300 to 600 and having a difference in average degree of polymerization of at least 1500 from the polyvinyl acetal resin (A); Acetal resin (B) is a polyvinyl acetal resin (A) 10
It is mixed at a ratio of 3 to 8 parts by weight with respect to 0 parts by weight. Therefore, good sound insulation performance is exhibited over a wide temperature range by the polyvinyl acetal resin (A) having a high degree of polymerization, and the polyvinyl acetal resin (B) having a low degree of polymerization is mixed in the above-described specific ratio, so that the moldability is improved. Is not impaired. Therefore, it is made of a plasticized polyvinyl acetal resin film and has good sound insulation over a wide temperature range, especially in the low temperature range, while satisfying the basic performance as an interlayer film for laminated glass such as mechanical strength and adhesion to glass. It is possible to provide an interlayer film for laminated glass that exhibits performance.

【００７３】特に、ポリビニルアセタール樹脂としてポ
リビニルブチラール樹脂を用いた場合には、中間膜の透
明性、耐候性、及びガラスに対する接着性をより優れた
ものとすることができ、かつ可塑剤としてトリエチレン
グリコール−ジ−２−エチルブチレート、トリエチレン
グリコール−ジ−２−エチルヘキサノエート及びトリエ
チレングリコール−ジ−ｎ−ヘプタネートからなる群か
ら選択した少なくとも１種を用いた場合には、中間膜の
力学特性及びガラスに対する接着性をより優れたものと
することができる。In particular, when a polyvinyl butyral resin is used as the polyvinyl acetal resin, the transparency, weather resistance, and adhesion to glass of the interlayer can be further improved, and triethylene is used as the plasticizer. When at least one selected from the group consisting of glycol-di-2-ethylbutyrate, triethylene glycol-di-2-ethylhexanoate and triethylene glycol-di-n-heptanoate is used, the intermediate film Can have better mechanical properties and better adhesion to glass.

【００７４】本発明に係る合わせガラスは、少なくとも
一対の板状透明体間に本発明に係る合わせガラス用中間
膜を介在させて一体化させているため、本発明に係る合
わせガラス用中間膜の作用により、透明性、耐候性及び
衝撃エネルギー吸収性などの合わせガラスに必要な基本
性能を損なうことなく、コインシデンス効果が緩和され
てＴＬ値の低下が防止され、従って広い温度域にわた
り、特に低温域において優れた遮音性能を発現し得る合
わせガラスを提供することが可能となる。Since the laminated glass according to the present invention is integrated by interposing the interlayer film for laminated glass according to the present invention between at least a pair of transparent plates, the interlayer film for laminated glass according to the present invention is integrated. The action reduces the coincidence effect and prevents a decrease in TL value without impairing the basic performance required for laminated glass such as transparency, weather resistance and impact energy absorption, and thus prevents a decrease in TL value. It is possible to provide a laminated glass that can exhibit excellent sound insulation performance.

【図面の簡単な説明】[Brief description of the drawings]

【図１】本発明に係る合わせガラス用中間膜の構造を説
明するための略図的断面図。FIG. 1 is a schematic sectional view for explaining the structure of an interlayer film for laminated glass according to the present invention.

【図２】板ガラスの遮音性能を説明するための図。FIG. 2 is a diagram for explaining the sound insulation performance of a sheet glass.

【符号の説明】[Explanation of symbols]

１…合わせガラス用中間膜 Ｘ，Ｙ…ポリビニルアセタール樹脂膜 1: Interlayer film for laminated glass X, Y: Polyvinyl acetal resin film

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ０８Ｌ 29/14 Ｃ０８Ｌ 29/14 Ｇ１０Ｋ 11/162 Ｇ１０Ｋ 11/16 Ａ Ｆターム(参考） 4F071 AA30 AA81 AC10 AE04 AF50 BA01 BB03 4F100 AG00C AG00D AG00E AH02H AK23A AK23B AK23C AK23D AK23E AL05A AL05B AL05C AL05D AL05E BA02 BA03 BA04 BA05 BA10A BA10C BA10D BA10E BA13 CA04 EC03 EC032 EJ17 EJ172 GB08 GB33 JA07A JA07B JA07C JA07D JA07E JK10 JL09 JN01 YY00A YY00B YY00C YY00D YY00E 4G061 AA11 BA01 BA02 CB05 CB19 CD02 CD18 4J002 BE061 BE062 EH046 FD026 GF00 5D061 AA06 AA12 BB31 BB37 DD06──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI theme coat ゛ (Reference) C08L 29/14 C08L 29/14 G10K 11/162 G10K 11/16 A F term (Reference) 4F071 AA30 AA81 AC10 AE04 AF50 BA01 BB03 4F100 AG00C AG00D AG00E AH02H AK23A AK23B AK23C AK23D AK23E AL05A AL05B AL05C AL05D AL05E BA02 BA03 BA04 BA05 BA10A BA10C BA10D BA10E BA13 CA04 EC03 EC032 EJ17 EJ172 GB08 GB33 JA07A JA07B JA07C JA07D JA07E JK10 JL09 JN01 YY00A YY00B YY00C YY00D YY00E 4G061 AA11 BA01 BA02 CB05 CB19 CD02 CD18 4J002 BE061 BE062 EH046 FD026 GF00 5D061 AA06 AA12 BB31 BB37 DD06

Claims (3)

【特許請求の範囲】[Claims] 【請求項１】 可塑化された複数枚のポリビニルアセタ
ール樹脂膜よりなる積層体からなる合わせガラス用中間
膜であって、 少なくとも１層のポリビニルアセタール樹脂膜が、平均
重合度２０００〜３０００のポリビニルアセタール樹脂
（Ａ）と、平均重合度が３００〜６００であり、かつポ
リビニルアセタール樹脂（Ａ）との平均重合度の差が１
５００以上であるポリビニルアセタール樹脂（Ｂ）とを
含み、ポリビニルアセタール樹脂（Ｂ）がポリビニルア
セタール樹脂（Ａ）１００重量部に対し、３〜８重量部
の割合で混合されていることを特徴とする合わせガラス
用中間膜。1. An intermediate film for laminated glass comprising a laminate comprising a plurality of plasticized polyvinyl acetal resin films, wherein at least one layer of the polyvinyl acetal resin film has an average degree of polymerization of 2000 to 3000. The average degree of polymerization of the resin (A) is 300 to 600, and the difference of the average degree of polymerization of the polyvinyl acetal resin (A) is 1
A polyvinyl acetal resin (B) of 500 or more, wherein the polyvinyl acetal resin (B) is mixed at a ratio of 3 to 8 parts by weight with respect to 100 parts by weight of the polyvinyl acetal resin (A). Interlayer for laminated glass. 【請求項２】 前記ポリビニルアセタール樹脂がポリビ
ニルブチラール樹脂であり、 可塑剤が、トリエチレングリコール−ジ−２−エチルブ
チレート、トリエチレングリコール−ジ−２−エチルヘ
キサノエート及びトリエチレングリコール−ジ−ｎ−ヘ
プタノエートからなる群より選択した少なくとも１種で
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 polyvinyl acetal resin is a polyvinyl butyral resin, and the plasticizer is triethylene glycol-di-2-ethyl butyrate, triethylene glycol-di-2-ethylhexanoate and triethylene glycol-diethyl. The interlayer film for laminated glass according to claim 1, wherein the interlayer film is at least one selected from the group consisting of -n-heptanoate. 【請求項３】 少なくとも１対の板状透明体間に請求項
１または２に記載の合わせガラス用中間膜が介在され
て、一体化されていることを特徴とする合わせガラス。3. A laminated glass, wherein the interlayer film for laminated glass according to claim 1 is interposed between at least one pair of plate-shaped transparent bodies, and is integrated.
JP2000010537A 2000-01-19 2000-01-19 Laminated glass interlayer film and laminated glass Expired - Lifetime JP4331846B2 (en)

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