JP3160578B2 - ポリマーフィルムの貼り合わせ方法 - Google Patents

ポリマーフィルムの貼り合わせ方法

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Publication number
JP3160578B2
JP3160578B2 JP26318298A JP26318298A JP3160578B2 JP 3160578 B2 JP3160578 B2 JP 3160578B2 JP 26318298 A JP26318298 A JP 26318298A JP 26318298 A JP26318298 A JP 26318298A JP 3160578 B2 JP3160578 B2 JP 3160578B2
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JP
Japan
Prior art keywords
polyester
diisocyanate
film
adhesive
melting point
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Expired - Lifetime
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JP26318298A
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English (en)
Other versions
JPH11148066A (ja
Inventor
チェン マイ
エイチ．デイッチ ジェフリー
Original Assignee
モートン インターナショナル，インコーポレイティド
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Publication of JPH11148066A publication Critical patent/JPH11148066A/ja
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
    • C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38—Pressure-sensitive adhesives [PSA]
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    • H01L2924/1025—Semiconducting materials
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    • H01L2924/10253—Silicon [Si]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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    • H01L2924/10—Details of semiconductor or other solid state devices to be connected
    • H01L2924/102—Material of the semiconductor or solid state bodies
    • H01L2924/1025—Semiconducting materials
    • H01L2924/1026—Compound semiconductors
    • H01L2924/1032—III-V
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Description

【発明の詳細な説明】
【０００１】
【発明の属する技術分野】本発明は、ポリマーフィルム
を接合するのに有用な貼り合わせ用接着剤に関し、特に
食品、医薬品等のためのポリマーフィルム積層体を提供
することに関する。本発明の貼り合わせ用接着剤は、水
も有機溶剤も含まないという意味で「無溶剤型」の接着
剤である。この接着剤は、優れた酸素遮断性及び防湿性
を備えている。
【０００２】
【従来の技術及び発明が解決しようとする課題】酸素、
湿分及び他の気体は多くの食品及び医薬品の品質を劣化
させる傾向を有する。食品包装、医薬品包装等に有用な
多くのポリマーフィルムが、酸素及び湿分が比較的透過
しうるものである。遮断性を高めるために、ポリマーフ
ィルムは、高遮断性を有する接着剤層を使用して積層体
に形成される。
【０００３】現在のところ、遮断性のある貼り合わせ用
接着剤は主として水性又は溶剤型のポリ塩化ビニリデン
（ＰＶＤＣ）配合物である。溶液が水性である場合に
は、水を蒸発させるためにエネルギーを消費させる必要
がある。有機溶剤型配合物も、溶剤を除去するために若
干のエネルギー消費を伴い、さらに溶剤は作業場及び環
境に有害である。無溶剤型貼り合わせ機のみを所有する
包装業者は、ＰＶＤＣで予めコーティングされたフィル
ムを使用しなくてはならない。また、ＰＶＤＣ中の塩素
は環境汚染物質の発生原因である。
【０００４】もう１つ別の高遮断性材料にはエチレンビ
ニルアルコール（ＥＶＯＨ）があるが、これは典型的に
は水性接着剤配合物として適用される。ＥＶＯＨは塩素
を含まないが、配合物中の水はエネルギーの消費を必要
とする。ＥＶＯＨは高い融点、すなわち１５０℃よりも
高い融点を有する。そのような高い融点では、また殆ど
のポリマーフィルムが溶融する。従って、ＥＶＯＨを溶
剤型接着剤として適用することはできない。ＥＶＯＨは
酸素及び他の気体に対して優れた遮断性を有するが、不
十分な防湿性を有する。また、ＥＶＯＨは比較的高価で
ある。
【０００５】本発明は、貼り合わせに有用であり、かつ
酸素及び湿分の両方に対する高い遮断性を提供する無溶
剤型ウレタン接着剤に関する。殆どの商用の無溶剤型ウ
レタン接着剤は、それらがアモルファスポリマーとなる
傾向があるために、非常に不十分な酸素遮断性を有す
る。
【０００６】
【課題を解決するための手段】本発明の無溶剤型ウレタ
ン接着剤は、２〜１０個の炭素原子、好ましくは３〜６
個の炭素原子を有する１種の線状脂肪族ジオール及び１
種の線状ジカルボン酸から形成されたヒドロキシル末端
ポリエステル（Ａ）と１種の液状ジイソシアネート
（Ｂ）とが約１〜約１．１の間のＮＣＯ／ＯＨ比で反応
した反応生成物を含む。前記ポリエステル（Ａ）は、周
囲温度で結晶質であり、約８０℃以下、好ましくは約７
０℃以下、より好ましくは約６０℃以下、最も好ましく
は約５５℃以下の融点を有する。前記ポリエステルの数
平均分子量（Ｍn ）は、約３００〜約５０００の間、好
ましくは約５００〜約２０００の間である。結果として
得られるウレタンは、１種の線状ジオール、１種の線状
ジカルボン酸及び１種のジイソシアネートから形成され
るため、ポリウレタンは高い結晶性を有し、それに伴っ
て高い酸素遮断性及び高い防湿性を有する。前記ポリエ
ステルの低い融点はいかなる溶剤も必要とせずに低温で
の接着剤の適用を可能にするため、貼り合わされるポリ
マーフィルムは分解も変形もしない。
【０００７】前記ポリエステル（Ａ）の一部（Ａ’）を
前記イソシアネート（Ｂ）の全部又は一部（Ｂ’）と約
２〜約８のＮＣＯ／ＯＨ比で反応させてウレタンプレポ
リマー（Ｃ）を形成させ、その後にポリエステル（Ａ）
の残りの部分（Ａ''）をプレポリマー（Ｃ）及びイソシ
アネート（Ｂ）の残りの部分（Ｂ''）と混合してフィル
ムを貼り合わせるのに適する接着剤混合物を形成させる
ことは本発明の範囲内に含まれることであり、ある場合
に好ましい。そのような場合においても、（Ａ’）及び
（Ａ''）の両方を包含する（Ａ）に対する（Ｂ’）及び
（Ｂ''）を包含する（Ｂ）のＮＣＯ／ＯＨ比は約１〜約
１．１の間である。
【０００８】
【発明の実施の形態】前記ポリエステルを形成するのに
好ましい線状脂肪族ジオールは、Ｃ3 〜Ｃ6ジオールで
あり、優れた遮断性を有する接着剤を形成するという観
点及び経済的観点からｎ−ブタンジオール及びｎ−ヘキ
サンジオールが好ましいジオールである。
【０００９】アジピン酸は本発明のポリエステルを形成
するのに好ましいジカルボン酸であるが、他の適切なジ
カルボン酸が使用されてもよい。このような適切なジカ
ルボン酸としてはアゼライン酸及びセバシン酸がある
が、これらに限定されない。
【００１０】現在のところ、最も好ましいポリエステル
は、１，６−ヘキサンジオール又は１，４−ブタンジオ
ールとアジピン酸との反応生成物である。
【００１１】約２０〜約３５０、好ましくは約１００〜
約２５０のＯＨ価を有するヒドロキシル末端ポリエステ
ルが形成するようにジオールを反応させる。
【００１２】好ましいジイソシアネートは、脂肪族ジイ
ソシアネート、特に線状ジイソシアネートであり、高分
子量ヘキサメチレンジイソシアネート（ＨＤＩ）が挙げ
られる。
【００１３】しかしながら、メチレンジフェニルジイソ
シアネート（ＭＤＩ）、ジシクロヘキシルメタン４，
４’−ジイソシアネート（Ｈ12ＭＤＩ）及びトルエンジ
イソシアネート（ＴＤＩ）を包含する他のジイソシアネ
ートが使用されてもよい。ジイソシアネートは、概し
て、ポリエステルよりも小さな割合で線状ポリウレタン
鎖を構成する。そのため、ジイソシアネートの選択はポ
リエステルの性質よりも概して厳密ではない。遮断性が
非常に優れた遮断層を形成する観点から、高分子量ＨＤ
Ｉが現在のところ好ましい。しかしながら、高分子量Ｈ
ＤＩは比較的高価な材料であり、遮断性に対する要求が
あまり厳しくない場合にはＭＤＩのようなあまり高価で
ないジイソシアネートを使用することができる。
【００１４】本発明において有用なジイソシアネート
は、周囲温度、すなわち２０〜２５℃で液状である。本
発明の低分子量ポリエステルは非常に結晶性が高いが、
それらの分子量が小さいために比較的低い温度で溶融す
る。ポリエステルは、周囲温度よりもほんの僅か高い温
度であるが積層体を形成するポリマーフィルムが分解又
は変形しない温度で接着剤を適用することができるよう
に、周囲温度よりもほんの僅か高い低温で溶融すること
が必要である。このことは、当然のことながらポリマー
フィルムの個々の性質に依存するが、より感熱性の高い
フィルムに対してはポリエステルが約８０℃以下の温度
で溶融することが望ましい。
【００１５】高速貼り合わせ機を使用する適用、例え
ば、６００ft／分（１８３ｍ／分）以上の速度での適用
に対しては、ジイソシアネート／ポリエステル混合物の
粘度は貼り合わせ温度で約３００〜約２０００ｃｐｓで
あることが好ましく、貼り合わせ温度で約４００〜約１
０００ｃｐｓであることがより好ましい。貼り合わせ温
度は、好ましくは８０℃以下、より好ましくは７０℃以
下、さらに好ましくは６０℃以下、最も好ましくは５５
℃以下である。すなわち、参考までに述べると、個々の
適用に依存して、上記粘度は、先に列挙した温度のうち
の少なくとも１つの温度、すなわち８０℃、７０℃、６
０℃又は５５℃での粘度に該当すべきである。
【００１６】本発明の接着剤は、ポリプロピレン、ポリ
エチレン、ポリエステル、ポリアミドのフィルム及び同
時押出フィルムを包含する種々のポリマーフィルムを接
着するのに有用である。当然のことながら、この接着剤
は、不十分な遮断性を有するフィルムを接着させて高遮
断性積層体を提供することにおいて最も有用である。２
枚のフィルム同士の間の接着性は非常に優れ、このウレ
タン接着剤から形成される積層体は剥離性でない。
【００１７】概して、貼り合わせ前、すなわち貼り合わ
せ前の約１分以内に２つの接着剤成分が混合される。溶
融ポリエステルは液状ジイソシアネートと混合され、接
着剤混合物組成物が形成される。接着剤混合物組成物
は、ポリマーフィルムのうちの１枚に適用され、両方の
フィルムがニップに通され、そしてその結果として得ら
れる積層体がリールに巻き取られる。塗布量は、典型的
には１〜３ポンド毎連（１．６〜４．９ｇ／ｍ2 ）、好
ましくは約１．５ポンド毎連（２．４ｇ／ｍ2 ）であ
る。高い遮断性を達成するには、速度が遅いウレタン形
成反応が最も望ましく、貼り合わせ後に、積層体は巻き
取られ、そのリールは周囲温度でイソシアネートとポリ
エステルのヒドロキシル基の間の反応を完了させるのに
十分な時間貯蔵される。周囲温度で少なくとも１週間の
貯蔵が望ましい。
【００１８】低粘度イソシアネートキャップドプレポリ
マーが形成されるようにジイソシアネートをポリエステ
ルの一部と予備反応させ、ポリエステルの残りをプレポ
リマーと反応させること、及び適用の時点でＮＣＯ／Ｏ
Ｈ比が約１〜約１．１であることも本発明の範囲内に含
まれる。いずれの場合においても、高結晶性であり、そ
のため酸素、湿分及び他の気体に対して高遮断性である
接着剤層を提供するために、１種のジオール、ジカルボ
ン酸及び好ましくはジイソシアネートが使用される。プ
レポリマーが形成される場合には、プレポリマーを形成
する際に約２〜約８の間のＮＣＯ／ＯＨ比が概して使用
される。ポリエステルの一部をジイソシアネートと予備
反応させたプレポリマーを形成させることの主な理由
は、接着剤混合物組成物の粘度が適用温度で低くなりす
ぎないようにするためである。概して、この方法に従う
場合には、ジイソシアネートの全部がポリエステルの適
切な割合の一部と反応する。しかしながら、ジイソシア
ネートの２５重量％がポリエステルの適切な割合の一部
と予備反応したとしても、粘度の実質的な調節が確認さ
れる。粘度調節のためにウレタンプレポリマーが望まし
い場合には、ポリエステルの少なくとも５０重量％を予
備反応させることが望ましい。
【００１９】ポリエステルをジイソシアネートと反応さ
せる場合であってもウレタンプレポリマーをポリエステ
ルと反応させる場合であっても、ポリエステルをイソシ
アネートと反応させる際に１のＮＣＯ／ＯＨ比が理論的
に望ましい。しかしながら、ポリエステルがポリエステ
ル縮合反応に由来する若干の残留水を含みうるため、約
１．１のＮＣＯ／ＯＨ比まで僅かに過剰のジイソシアネ
ートが典型的には使用される。特定の実施例によって本
発明をより詳細に説明する。
【００２０】
【実施例】実施例１〜５ 実施例１：１，４−ブタンジオールアジペート（ＯＨ価
２２５）のポリエステル１３重量部（ｐｂｗ）を１０重
量部の高分子量ＨＤＩと混合した。混合物を１．６ポン
ド毎連（２．６ｇ／ｍ2 ）の塗布量で１ミル（２５ミク
ロン）の透明延伸ポリプロピレン（ＯＰＰ）フィルム上
にコーティングした。コーティングされたフィルムを１
６０°Ｆ（７１℃）のニップ温度でもう１枚の１ミル
（２５ミクロン）ＯＰＰフィルムに貼り合わせた。
【００２１】実施例２：２６．４ｐｂｗの１，６−ヘキ
サンジオールアジペート（ＯＨ価１１２）を１０ｐｂｗ
のＨＤＩポリイソシアネートと混合した。接着剤を２ポ
ンド／連（３．２５ｇ／ｍ2 ）の塗布量で１ミルの低密
度ポリエチレン（ＬＤＰＥ）フィルム上にコーティング
した。コーティングされたフィルムを１６０°Ｆ（７１
℃）のニップ温度でもう１枚の１ミル（２５ミクロン）
ＬＤＰＥフィルムに貼り合わせた。
【００２２】実施例３：４０ｐｂｗの１，６−ヘキサン
ジオールアジペート（ＯＨ価１１２）を１０ｐｂｗの
２，４’−４，４’−メチレンジフェニルジイソシアネ
ート（ＭＤＩ）と混合した。混合物を使用し、１６０°
Ｆ（７１℃）のニップ温度で２枚の１ミル（２５ミクロ
ン）同時押出（ＣＯＥＸ）フィルムを貼り合わせた。
【００２３】比較例４：４０ｐｂｗのジエチレングリコ
ールアジペート（ＯＨ価１１２）を１０ｐｂｗの２，
４’−４，４’−ＭＤＩと混合し、実施例３におけるよ
うに積層体を形成することに使用した。
【００２４】比較例５：従来のアモルファスウレタン接
着剤を使用し、実施例２におけるように２枚の１ミル
（２５ミクロン）ＬＤＰＥフィルムを貼り合わせた。
【００２５】参考のため、実施例において使用した接着
剤層を有していない１ミル（２５ミクロン）の各フィル
ム層は湿度０％、７５°Ｆ（２３．９℃）で次の酸素透
過度（ＯＴＲ）（単位： cc/in2/日）を有していた：Ｌ
ＤＰＥ ４７９．０；ＯＰＰ９８．０；ＣＯＥＸ ８
５．６。結果（湿度０％、７５°Ｆ（２３．９℃）での
ＯＴＲ(cc/in2/日））は次の通りである：
【００２６】
【表１】
【００２７】実施例１の透湿度は０．１３cc/100in2/日
であり、これに対して１ミル（２５ミクロン）のＯＰＰ
層の透湿度は０．４０cc/100in2/日であった。
───────────────────────────────────────────────────── フロントページの続き (72)発明者 ジェフリー エイチ．デイッチ アメリカ合衆国，イリノイ 60012，ク リスタル レイク，レキシントン トレ イル 6912 (56)参考文献 特開 平８−291279（ＪＰ，Ａ) 特開 平３−26772（ＪＰ，Ａ) 特開 平４−103687（ＪＰ，Ａ) 特開 平２−274787（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C09J 1/00 - 201/10 C08K 1/00 - 13/08 C08L 1/00 - 101/14

Claims (9)

    (57)【特許請求の範囲】
  1. 【請求項１】 ポリマー材料の第１フィルムをポリマー
    材料の第２フィルムに貼り合わせる方法であって、 末端ヒドロキシル基及び２〜１０個の炭素原子を有する
    １種の線状脂肪族ジオールと１種の線状ジカルボン酸か
    ら形成された溶融状態にある無溶剤ヒドロキシル末端ポ
    リエステルであって、３００〜５０００の数平均分子量
    及び８０℃以下の融点を有するポリエステル（Ａ）を準
    備する工程； 液体状態にある１種のジイソシアネート（Ｂ）を準備す
    る工程； 前記ジイソシアネート（Ｂ）と前記ポリエステル（Ａ）
    を１〜１．１の間のＮＣＯ／ＯＨ比で混合して接着剤混
    合物（Ｉ）を形成させるか、又は前記ジイソシアネート
    （Ｂ）の全部若しくは一部（Ｂ’）を前記ポリエステル
    （Ａ）の一部（Ａ’）と２〜８の間のＮＣＯ／ＯＨ比で
    反応させてウレタンプレポリマー（Ｃ）を形成させ、前
    記ポリエステル（Ａ）の残りの部分（Ａ''）及びもし存
    在するならば前記ジイソシアネート（Ｂ）の残りの部分
    （Ｂ''）と前記ウレタンプレポリマー（Ｃ）とを混合
    し、（Ｂ）に対する（Ａ）のＮＣＯ／ＯＨ比が１〜１．
    １の間である接着剤混合物（ＩＩ）を形成させる工程；前記第１フィルムと第２フィルムを接着させる直前に形
    成された 前記接着剤混合物（Ｉ）又は（ＩＩ）により前
    記第１フィルムと第２フィルムを接着させる工程；並び
    に前記ジイソシアネート（Ｂ）及び前記ポリエステル
    （Ａ）を完全に反応させる工程； を含む方法。
  2. 【請求項２】 前記ジオールが３〜６個の炭素原子を有
    する請求項１記載の方法。
  3. 【請求項３】 前記ポリエステルが５００〜２０００の
    間の数平均分子量を有する請求項１記載の方法。
  4. 【請求項４】 前記ポリエステルが７０℃以下の融点を
    有する請求項１記載の方法。
  5. 【請求項５】 前記ポリエステルが６０℃以下の融点を
    有する請求項１記載の方法。
  6. 【請求項６】 前記ポリエステルが５０℃以下の融点を
    有する請求項１記載の方法。
  7. 【請求項７】 前記接着剤がその粘度が３００〜２００
    ０ｃｐｓに及ぶ温度で適用される請求項１記載の方法。
  8. 【請求項８】 前記接着剤がその粘度が４００〜１００
    ０ｃｐｓに及ぶ温度で適用される請求項１記載の方法。
  9. 【請求項９】 請求項１記載の方法に従って製造される
    積層体。
JP26318298A 1997-09-17 1998-09-17 ポリマーフィルムの貼り合わせ方法 Expired - Lifetime JP3160578B2 (ja)

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