JP6899689B2 - 金属積層用二軸延伸ポリエステルフィルム - Google Patents
金属積層用二軸延伸ポリエステルフィルム Download PDFInfo
- Publication number
- JP6899689B2 JP6899689B2 JP2017077546A JP2017077546A JP6899689B2 JP 6899689 B2 JP6899689 B2 JP 6899689B2 JP 2017077546 A JP2017077546 A JP 2017077546A JP 2017077546 A JP2017077546 A JP 2017077546A JP 6899689 B2 JP6899689 B2 JP 6899689B2
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- JP
- Japan
- Prior art keywords
- polyester film
- polyester
- outer layer
- weight
- layer
- 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.)
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- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
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- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0018—Combinations of extrusion moulding with other shaping operations combined with shaping by orienting, stretching or shrinking, e.g. film blowing
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- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
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- B29C48/911—Cooling
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- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/15—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
- B32B37/153—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state at least one layer is extruded and immediately laminated while in semi-molten state
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
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- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D43/00—Lids or covers for rigid or semi-rigid containers
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- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
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- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C—CHEMISTRY; METALLURGY
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- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
- C08L67/03—Polyesters derived from dicarboxylic acids and dihydroxy compounds the dicarboxylic acids and dihydroxy compounds having the carboxyl- and the hydroxy groups directly linked to aromatic rings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D201/00—Coating compositions based on unspecified macromolecular compounds
- C09D201/02—Coating compositions based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C09D201/10—Coating compositions based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing hydrolysable silane groups
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31678—Of metal
- Y10T428/31681—Next to polyester, polyamide or polyimide [e.g., alkyd, glue, or nylon, etc.]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31786—Of polyester [e.g., alkyd, etc.]
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Description
本発明のフィルムのベース層は結晶性であり、融点が通常250℃未満、好ましくは245℃未満である。この結晶性はフィルムに良好な機械的強度を付与し、フィルムの製造加工において費用効率が高くなる。
ベース層Bに共押出しされて積層される非晶性外層Aは、19重量%以上、好ましくは23重量%以上、更に好ましくは27重量%以上のエチレンイソフタレート誘導単位と、81重量%以下、好ましくは77重量%以下、更に好ましくは73重量%以下のエチレンテレフタレート誘導単位から成る(外層A中のポリエステルの総重量を基準とする)。残余のモノマー単位は、ベース層中に取り入れられる脂肪族、脂環式または芳香族のジオールとジカルボン酸とから誘導される。
他に使用できるポリマーとしては、結晶性外層Cは、基本的に上述の結晶性ベース層Bで使用されるものと同じある。
本発明のフィルムは、アルミニウムとの密着性を改良するために、外層(A)上に機能性シランの塗布層を有していてもよい。官能基としては一級アミンが好ましい。アミノ官能基シランは、加水分解していない状態で以下の一般式で示される。
ポリエステルフィルムの製造方法は、例えば「Handbook of Thermoplastic Polyesters, Ed.S.Fakirov,Wiley−VCH,2002」又は「Encyclopedia of Polymer Science and Engineering,Vol.12,John Wiley & Sons,1988」の「Polyesters,Films」の章に記載されており、参照により本発明に引用する。本発明のフィルムの好ましい方法は、以下の工程による。原料をそれぞれの層に対応する押出機内で溶融し、3層フラットフィルムダイを介して冷却引取りロール上に押出す。得られたシートを再加熱し、機械方向(長手方向、MD)又は横方向(TD)の何れかの少なくとも1方向に延伸配向する。好ましくは長手方向およびまたは横方向および長手方向に延伸する。延伸工程におけるフィルム温度は、通常使用するポリエステルのガラス転移温度Tgより10〜60℃上の温度であり、長手方向の延伸比は通常2.5〜5.0、好ましくは3.0〜4.5であり、横方向の延伸比は通常3.0〜5.0、好ましくは3.5〜4.5である。長手方向延伸は横方向延伸と同時に行ってもよく(同時延伸)またいかなる考えられ得る連続的な延伸法で行ってもよい。次いで、フィルムは、通常180〜235℃、好ましくは210〜230℃のオーブン温度で熱固定される。次いで、フィルムは冷却され、巻取られる。
外層Aのポリエステルのガラス転移温度Tg及び融点は、DIN 53765に従い、DSC装置(Perkin−Elmer Pyris 1)を使用して測定した。20K/分の昇温速度で試料を300℃まで加熱し、この温度で10分間保持した。次いで、試料を可能な限り素早く20℃まで冷却した(500K/分)。試料を20℃で10分間保持した後、20K/分の昇温速度で試料を300℃まで加熱した。2回目の加熱工程から得られる値の方が再現性が良いために使われた。
フィルムの長手方向および横方向に対して弾性係数、最大抗張力、引張破断強度およびF5値を測定した。測定は、引張歪み試験機(Zwick社製010型(ドイツ))を使用してISO 527−1及び527−3に準拠して行った。
標準粘度SVは、DIN 53726に従い、ジクロロ酢酸(DCA)の1重量%溶液を調製し、ウベローデ型粘度計を使用して2℃で測定した。無次元SV値は、相対粘度(ηrel)から以下の式によって算出できる。
熱収縮率は、1辺10cmの正方形フィルムサンプルで測定した。サンプルは1辺が機械方向に平行に、もう1辺が機械方向に垂直になるように切り出した。サンプルの長さを正確に測定し(1辺の長さをL0とし、それぞれの方向TD及びMDをL0TD及びL0MDとする)、対流乾燥オーブン内で、収縮が起こる温度に15分間加熱する(この場合150℃)。サンプルを取り出し、室温において長さを正確に測定する(1辺の長さLTD及びLMD)。収縮率は以下の式により算出される。
収縮率[%]TD = 100×(L0TD−LTD)/L0TD
フィルム片180℃に予備加熱されている対流オーブン内に配置する。フィルムはワイヤーメッシュ上に配置した(メッシュ幅:0.25〜2cm)。フィルムを180℃で90分間オーブン内に放置した。機械的性質、収縮率、色およびSVについて測定された。
Cr(III)で前処理したアルミニウムシートを200℃に加熱し、フィルムをこの金属シート上に加圧して積層した。積層体は、次いで250℃で10秒間加熱した。このサンプルは、次いで100℃で30分間加熱して3%酢酸に接触させた。DIN EN ISO 2409に従いクロスカットテストをフィルム側に行った。結果は、0(非常に良好)〜5(非常に悪い)で評価した。
それぞれのフィルム側の結晶化度は、1040cm−1及び1337cm−1におけるATRスペクトル(ATR=減衰全反射)の強度比により決定した。強度は1117cm−1における強度を基準に規格化した。1040cm−1の帯域は非晶ポリエステルに対応し、1337cm−1の帯域は結晶ポリエステルに対応する(Polymer Letters Edition, Vol.12(1974),pp.13−19に記載)。
色特性L*、a*、b*は、Byk−Gardner社性(米国)Color−Sphere装置を使用し、DIN 1674又はASTM D2244に準拠して個々の層および包装層の透過率を測定した。使用した形状は光沢を有するd/8で、測定波長幅は400〜700nmであり、スペクトル分解能は20nmであり、使用した光源はD65であり、観測角度は10°であり、開口プレートの径は30mmである。
各層の構成を以下の表1に示す。
原料組成を以下の表3に示すように変更した以外は実施例1と同じ製造条件でフィルムを製造した。
原料組成を以下の表4に示すように変更した以外は実施例1と同じ製造条件でフィルムを製造した。
欧州特許第312304号に記載の厚さ20μmのフィルムを製造した。使用した原料を以下の表5に示す。外層A上の塗布層を設けなかったこと以外は実施例1と同じ製造条件でフィルムを製造した。
Claims (19)
- ベース層Bのポリエステルが、ポリエステルの総重量を基準として85重量%以上のエチレンテレフタレート誘導単位と2〜15重量%のエチレンイソフタレート誘導単位とから成る請求項1に記載のポリエステルフィルム。
- ベース層Bのポリエステルが3〜10重量%のエチレンイソフタレート誘導単位から成る請求項1又は2に記載のポリエステルフィルム。
- エチレンテレフタレート誘導単位とエチレンイソフタレート誘導体の総重量がポリエステルの95重量%以上である請求項1〜3の何れかに記載のポリエステルフィルム。
- 非晶性外層Aが、外層A中のポリエステルの総重量を基準として19重量%以上のエチレンイソフタレート誘導単位と、81重量%以下のエチレンテレフタレート誘導単位から成る請求項1〜4の何れかに記載のポリエステルフィルム。
- 外層Cが0.05重量%以上の不活性粒子を含む請求項1〜5の何れかに記載のポリエステルフィルム。
- ポリエステルフィルムがチタン系触媒を使用して製造される請求項1〜6の何れかに記載のポリエステルフィルム。
- フィルムが50〜10000ppmのフリーラジカル捕捉剤を含む請求項1〜7の何れかに記載のポリエステルフィルム。
- 外層Cが300ppm以上のフリーラジカル捕捉剤を含む請求項1〜7の何れかに記載のポリエステルフィルム。
- フリーラジカル捕捉剤が、1,3,5−トリメチル−2,4,6−tris(3,5−di−tert−ブチル−4−ヒドロキシベンジル)ベンゼン(CAS番号1709−70−2)、2,6−ditert−ブチル−4−(ジオクタデコキシホスホリルメチル)フェノール(CAS番号3135−18−0)、アンチオキシダント1010(CAS番号6683−19−8)及びbis[2−tert−ブチル−6−[(3−tert−ブチル−2−ヒドロキシ−5−メチルフェニル)メチル]−4−メチルフェニル]ベンゼン−1,4−ジカルボキシレート(CAS番号57569−40−1)から選択される1種以上の化合物である請求項8又は9に記載のポリエステルフィルム。
- 外層A上に官能シラン塗布層を有する請求項1〜10の何れかに記載のポリエステルフィルム。
- 官能シランが加水分解されていないアミノ官能シランである請求項11に記載のポリエステルフィルム。
- 官能シランが(R1)aSi(R2)b(R3)cで示される化合物であり、R1は少なくとも1つの一級アミノ基を有する加水分解されない官能基であり、R2は低級のアルコキシ基、アセトキシ基またはハロゲン化基から選択される加水分解性官能基であり、R3は低級アルキル基またはフェニル基から選択される非反応性で加水分解されない官能基であり、a≧1、b≧1、c≧0、a+b+c=4であり、低級アルキル基および低級アルコキシ基の炭素数は1〜4であり、ハロゲン化基のハロゲンがフッ素、塩素、臭素およびヨウ素から選択される請求項12に記載のポリエステルフィルム。
- フィルムの厚さが5〜20μmである請求項1〜13の何れかに記載のポリエステルフィルム。
- 請求項1に記載のポリエステルフィルムの製造方法であって、外層A、ベース層B及び外層Cに対応するポリエステル混合物をそれぞれの押出機内で圧縮して溶融する工程と、溶融体を共押出ダイを介して溶融押出シートとして押出し、冷却ロール及び1つ以上の引取りロールで引取りプレフィルムを製造する工程と、プレフィルムを冷却し、固化した後に二軸延伸する工程とから成ることを特徴とするポリエステルフィルムの製造方法。
- 更に、シラン系塗布層を形成するための塗布液を二軸延伸工程中に外層A上に塗布する工程を有する請求項15に記載のポリエステルフィルムの製造方法。
- 請求項1〜14の何れかのポリエステルフィルムと金属シートから成る積層体。
- 金属シートがアルミニウムシートである請求項17に記載の積層体。
- 請求項17又は18に記載の積層体から成る飲料缶の蓋。
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US3871947A (en) | 1973-01-15 | 1975-03-18 | Minnesota Mining & Mfg | Biaxially oriented polyethylene terephthalate film having a surface suitable for writing thereon |
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-
2016
- 2016-04-08 DE DE102016205913.0A patent/DE102016205913A1/de not_active Withdrawn
-
2017
- 2017-03-29 ES ES17163508T patent/ES2848099T3/es active Active
- 2017-03-29 EP EP17163508.9A patent/EP3228456B1/de active Active
- 2017-04-06 US US15/480,807 patent/US11208528B2/en active Active
- 2017-04-06 KR KR1020170044796A patent/KR20170115961A/ko not_active Application Discontinuation
- 2017-04-07 CN CN201710226949.7A patent/CN107263973B/zh active Active
- 2017-04-10 JP JP2017077546A patent/JP6899689B2/ja active Active
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EP3228456A1 (de) | 2017-10-11 |
DE102016205913A1 (de) | 2017-10-12 |
US11208528B2 (en) | 2021-12-28 |
US20170291987A1 (en) | 2017-10-12 |
ES2848099T3 (es) | 2021-08-05 |
KR20170115961A (ko) | 2017-10-18 |
CN107263973B (zh) | 2021-04-09 |
DE102016205913A8 (de) | 2017-12-28 |
JP2017185810A (ja) | 2017-10-12 |
EP3228456B1 (de) | 2020-10-21 |
CN107263973A (zh) | 2017-10-20 |
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