JP6532469B2 - ポリマーフィルムを被覆するための組成物、被覆方法、及び得られる複合材料 - Google Patents
ポリマーフィルムを被覆するための組成物、被覆方法、及び得られる複合材料 Download PDFInfo
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- JP6532469B2 JP6532469B2 JP2016541171A JP2016541171A JP6532469B2 JP 6532469 B2 JP6532469 B2 JP 6532469B2 JP 2016541171 A JP2016541171 A JP 2016541171A JP 2016541171 A JP2016541171 A JP 2016541171A JP 6532469 B2 JP6532469 B2 JP 6532469B2
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Description
第1の形態によれば、本発明は、
・アクリル及び/又はメタクリルポリマーの全重量に対して少なくとも50重量%のゲル含量を有する少なくとも1種類のアクリル及び/又はメタクリルポリマー;
・少なくとも1種類の架橋剤;
・スルホニルオキシ基を有する少なくとも1種類の水溶性又は水分散性ポリエステル;
を含む被覆組成物に関する。
(a)基材を用い;
(b)場合によっては、基材の物理的表面処理を行い;
(c)基材の少なくとも1つの面を上記に記載の被覆組成物で被覆し;そして
(d)下塗り層を得るために被覆を架橋し、ここで下塗り層の表面における遊離酸官能基の残留レベルは、下塗り層中に含まれるポリマーの全重量に対して少なくとも5重量%である;
工程を実施することを特徴とする、結合プライマーの少なくとも1つの層で基材を被覆する方法にも関する。
本発明による被覆組成物は、
・アクリル及び/又はメタクリルポリマーの全重量に対して少なくとも50重量%のゲル含量を有する少なくとも1種類のアクリル及び/又はメタクリルポリマー;
・少なくとも1種類の架橋剤;
・スルホニルオキシ基を有する少なくとも1種類の水溶性又は水分散性ポリエステル;
を含む。
本発明によるアクリル及び/又はメタクリルポリマーは、アクリル及び/又はメタクリルモノマーを含む。これは、異なるタイプのもの:疎水性モノマー、親水性モノマー、及び部分的に親水性のモノマーであってよいモノマーで構成される。好ましくは、本発明によるアクリル及び/又はメタクリルポリマーは、
(i)アルキルアクリレート、アルキルメタクリレート、又はこの2つの混合物の少なくとも1種類の部分的に親水性のモノマー(これらのモノマーのアルキル基は1又は2個の炭素原子を含む);
(ii)アルキルアクリレート、アルキルメタクリレート、又はこの2つの混合物の少なくとも1種類の疎水性モノマー(これらのモノマーのアルキル基は線状又は分岐であり、少なくとも4個の炭素原子を含む);
(iii)少なくとも1種類の親水性モノマー;
を含む。
本発明において用いることができる親水性モノマーは、アルキルアクリレート又はアルキルメタクリレートモノマーと共重合させることができ、水溶性であるモノマーである。親水性モノマーは、モノオレフィン性モノカルボン酸、モノオレフィン性ジカルボン酸、及びこれらの混合物から選択することができる。親水性モノマーの例としては、アクリル酸、メタクリル酸、フマル酸、マレイン酸、イタコン酸、クロトン酸、アクリル酸のオリゴマー、及びこれらの混合物が挙げられるが、これらに限定されない。好ましい酸は、アクリル酸、メタクリル酸、及びこれらの混合物である。
上記に記載の疎水性、親水性、及び部分的に親水性のモノマーの合計重量は、好ましくは、本発明によるアクリル及び/又はメタクリルポリマーを構成するモノマーの全重量の少なくとも60%、より好ましくは少なくとも75%、より好ましくは少なくとも80%、更により好ましくは少なくとも90%を示す。これらの疎水性、親水性、及び部分的に親水性のモノマーと異なるモノマーの重量%は、モノマーの全重量に対して好ましくは20%未満、より好ましくは10%未満、更により好ましくは5%未満である。好ましくは、本発明によるアクリル及び/又はメタクリルポリマーは、上記に記載の疎水性、親水性、及び部分的に親水性のモノマーで構成されるか又は実質的に構成される。
(i)メチルアクリレート、メチルメタクリレート、エチルアクリレート、及びこれらの混合物から選択される少なくとも30%の1種類又は複数の部分的に親水性のモノマー;
(ii)場合によっては、アルキルアクリレート、アルキルメタクリレート、又はこの2つの混合物の少なくとも1種類の疎水性モノマー(これらのモノマーのアルキル基は、線状又は分岐で、少なくとも4個の炭素原子を含む);
(iii)アクリル酸、メタクリル酸、及びこれらの混合物から選択される少なくとも10%の1種類又は複数の親水性モノマー;
を含む。
G(%)=[(Wf−Wc)×100]/Wi
(式中、
Wfは、カプセル及び不溶ポリマーの最終、即ち乾燥後の重量であり;
Wcは、カプセルの重量であり;そして
Wiは、乾燥したポリマーの重量である)
を用いて算出される。
である。
これらの樹脂はCytec Industries Inc.から販売されている。
最良の性能は、
・部分メチル化又は更に良好には高度にメチル化されているアミンベースの樹脂から選択される架橋剤;及び/又は
・80℃より高い温度で迅速に硬化させることができる架橋剤;及び/又は
・水性媒体中でアクリルポリマーと混合した後に、好ましくは48時間より長い長時間安定性を有する架橋剤;
によって得られる。
−SO3H又は(−SO3 −)nMn+
(式中、nは1又は2の値を有し、Mは、アルカリ金属イオン、アルカリ土類イオン、又は第4級アンモニウムを表す)
の基として定義される。
に対応していてよい。
スルホニルオキシ基を有する水溶性又は水分散性ポリエステルは、従来技術において、例えば特許出願EP−0260203において記載されている。更に、本発明において用いることができるポリエステルは商業的に入手できる。
被覆方法のための基材は、好ましくは可撓性の固体基材である。これは特にポリマーフィルムであってよい。特には、ポリエステルフィルムを用いる。ポリエステルは、1種類以上の芳香族ジカルボン酸(例えばテレフタル酸、イソフタル酸)又はそれらの誘導体(ハロゲン化物、エステル)と、少なくとも1種類のアルキレングリコール(例えば、エチレングリコール;プロパン−1,3−ジオール;ブタン−1,4−ジオール)との重縮合の生成物である。好ましくは、これらは、テレフタル酸又はテレフタル酸と他の芳香族ジカルボン酸(例えばイソフタル酸)の混合物から誘導されるポリエステルであり、混合物のテレフタル酸含量は、ポリマーが延伸後に実質的に結晶質であるのに十分なものである。
・ポリエチレンテレフタレートで構成されるか;
・又は、単独か若しくは混合して、エチレン単位に代えてシクロヘキシルジメチロール単位を含むポリエチレンテレフタレートコポリエステルで構成されるか;
・又は、単独か若しくは混合して、イソフタレート単位を有するポリエステル部分を有するポリエチレンテレフタレートコポリエステルで構成されるか;
・或いは、共押出によって得られる、上記に記載の異なる化学的性質を有するポリエステルの幾つかの層で構成される。
被覆された基材上の被覆の接着特性を更に向上させるために、被覆方法に、基材の物理的表面処理を行うことから構成される随意的な工程(b)を含ませることができる。この処理は被覆(工程c)の前に行う。基材の表面の一部又は全体を処理することができる。物理的処理は、コロナタイプの放電による処理、及びプラズマタイプの処理から選択することができる。かかるコロナタイプの処理は、大気圧の周囲空気下、又は好ましくは100mbar〜3000mbarの間の上昇した分圧、更により好ましくは大気圧の気体下におけるコロナ放電である。
基材は、好ましくは延伸可能なフィルムである。好ましくは、これは1つ又は2つの直交する方向において延伸にかける。両方の方向において延伸する場合には、これは二次元延伸と呼ばれ、まず縦方向の延伸(縦方向延伸LS、LSの延伸度≧3.0)を行い、次に横方向の延伸(横方向延伸TS、TSの延伸度≧3.5)を行うことができる。平面延伸度(これらの延伸操作の順番に関係なく、縦方向延伸度と横方向延伸度の積として定義される)は、例えば1〜20の間、通常は12より大きい。延伸の順番は、本発明によって得られる特性に悪影響を与えることなく、用いる機械によって相違させることができる。例えば、所謂逆シーケンス又は多工程機、交互シーケンスを有する機械、或いは同時延伸のための機械等を有用に用いることができる。延伸温度は、例えば、縦方向及び横方向において、基材のガラス転移温度Tgと最高でTg+60℃に等しい温度の間である。縦方向延伸は例えば3〜6回行い、横方向延伸は例えば3〜5回行う。
・Cchargesは、ポリマー1gあたりのマイクロ当量(μeq/g−ポリマー)で表されるラテックス中の電荷の濃度を示し;
・[NaOH]及び[HCl]は、それぞれモル・L−1で表される滴定溶液中の水酸化ナトリウム及び塩酸の濃度を表し;
・VNaOH及びVHClは、それぞれリットルで表される、測定のために用いた水酸化ナトリウム及び塩酸の滴定溶液の体積を表し;
・mlatexは、グラムで表されるラテックスの重量を表し;そして
・TSは、希釈されたラテックス中の固形分含量を表す)
を用いて、ラテックス中の電荷の濃度を測定曲線から計算することができる。
・被覆組成物の固形分含量;及び/又は
・基材に被覆組成物を施すために用いる適用方法及びロールの寸法;
に伴って変化する可能性がある。
1.異なる条件下における基材から基材のコアへの定性的深さ分布プロファイル。これによって、下塗り層の厚さを浸食時間の関数として求め、同じ種類の異なるフィルムの間の比較分析を行うことが可能である。
・少なくとも1種類の金属及び/又は少なくとも1種類の金属酸化物の少なくとも1つの層;
・インクの少なくとも1つの層;及び
・接着剤の少なくとも1つの層;
から選択することができる。
幾つかの場合においては、これらの異なるタイプの被覆を組み合わせることを想到することができる。
被覆は、基材の一方又は両方の面の上に存在する下塗り層の上に施すことができる。
驚くべきことに、本発明による複合材料は基材と被覆の間の良好な接着特性、及び特に酸素及び水蒸気に対する非常に良好なバリヤ特性の両方を有することが見出された。これらの良好な特性は、高い温度及び湿度の条件下において有利に維持される。
更に、得られる複合材料は、有利には、湿潤条件下及び乾燥条件下において、従来技術におけるものと同等に良好であるか又はそれよりも更に良好である被覆の接着特性を有することができる。
グラフィックアートのためのフィルム又はシートに関しては、これらは、インクで被覆されているか又は被覆されていない印刷可能な基材であってよい。
DMS社によってBT-67の名称で販売されているアクリル及び/又はメタクリルポリマーを用いた。これは、水中に分散している(0〜15又は20%の乾燥抽出物)、その平均径が100nm未満である粒子の形態である。このポリマーは、下記において「ラテックスB」と示す。
4つの被覆組成物F1、F2、F3、及びF4を調製した。
・F1:ラテックスBのみ;
・F2:ラテックスB+架橋剤X−80/20のラテックス/架橋剤の重量比(乾燥抽出物/乾燥抽出物);
・F3:ラテックスB+架橋剤X−75/25のラテックス/架橋剤の重量比(乾燥抽出物/乾燥抽出物);
・F4:ラテックスB+架橋剤X−70/30のラテックス/架橋剤の重量比(乾燥抽出物/乾燥抽出物)。
次式:
のスルホニルオキシ基を有する水溶性ポリエステルを、上記記載の組成物に加えた。このポリマーは、下記において「PES」と示す。
・F5:ラテックスB
+架橋剤X−80/20のラテックス/架橋剤の重量比(乾燥抽出物/乾燥抽出物)
+ラテックスBの乾燥重量に対して乾燥重量で5%のPES;
・F6:ラテックスB
+架橋剤X−80/20のラテックス/架橋剤の重量比(乾燥抽出物/乾燥抽出物)
+ラテックスBの乾燥重量に対して乾燥重量で10%のPES;
・F7:ラテックスB
+架橋剤X−75/25のラテックス/架橋剤の重量比(乾燥抽出物/乾燥抽出物)
+ラテックスBの乾燥重量に対して乾燥重量で5%のPES;
・F8:ラテックスB
+架橋剤X−75/25のラテックス/架橋剤の重量比(乾燥抽出物/乾燥抽出物)
+ラテックスBの乾燥重量に対して乾燥重量で10%のPES;
・F9:ラテックスB
+架橋剤X−70/30のラテックス/架橋剤の重量比(乾燥抽出物/乾燥抽出物)
+ラテックスBの乾燥重量に対して乾燥重量で5%のPES;
・F10:ラテックスB
+架橋剤X−70/30のラテックス/架橋剤の重量比(乾燥抽出物/乾燥抽出物)
+ラテックスBの乾燥重量に対して乾燥重量で10%のPES。
本発明の具体的態様は以下のとおりである。
[1]
・アクリル及び/又はメタクリルポリマーの全重量に対して少なくとも50重量%のゲル含量を有する少なくとも1種類のアクリル及び/又はメタクリルポリマー;
・少なくとも1種類の架橋剤;
・スルホニルオキシ基を有する少なくとも1種類の水溶性又は水分散性ポリエステル;
を含む被覆組成物。
[2]
アクリル及び/又はメタクリルポリマーが水相中に分散しているポリマー粒子の形態である、[1]に記載の被覆組成物。
[3]
架橋剤がアミンベースの樹脂、好ましくはメラミンアルデヒド、ベンゾグアナミンアルデヒド、又はその誘導体である、[1]及び[2]のいずれかに記載の被覆組成物。
[4]
架橋剤に対するアクリル及び/又はメタクリルポリマーの重量基準の割合(重量/重量)が、95/5〜70/30の間、より好ましくは90/10〜75/25の間、更により好ましくは85/15〜80/20の間である、[1]〜[3]のいずれかに記載の被覆組成物。
[5]
スルホニルオキシ基を有する水溶性又は水分散性ポリエステルの含量が、アクリル及び/又はメタクリルポリマーの乾燥重量に対して2〜30重量%の間、より好ましくは5〜20重量%の間、更により好ましくは8〜12重量%の間である、[1]〜[4]のいずれかに記載の被覆組成物。
[6]
以下の:
(a)基材を与え;
(b)場合によっては、基材の物理的表面処理を行い;
(c)基材の少なくとも1つの面を、[1]〜[5]のいずれかに記載の被覆組成物で被覆し;そして
(d)被覆を架橋して下塗り層を得て、ここで下塗り層の表面における遊離酸官能基の残留レベルは、下塗り層中に含まれるポリマーの全重量に対して少なくとも5重量%である;
工程を実施することを特徴とする、結合プライマーの少なくとも1つの層で基材を被覆する方法。
[7]
基材が、ポリエステルフィルム、好ましくはポリエチレンテレフタレート(PET)のフィルムであり、その厚さは、好ましくは150μm(マイクロメートル)以下、より好ましくは4μm〜100μmの間、より好ましくは4μm〜40μmの間、更により好ましくは4μm〜12μmの間である、[6]に記載の被覆方法。
[8]
基材上に得られる下塗り層が、200nm(ナノメートル)以下、より好ましくは40nm〜120nmの間、より好ましくは50nm〜100nmの間、更により好ましくは60nm〜90nmの間の厚さEを有する、[6]及び[7]のいずれかに記載の被覆方法。
[9]
基材の被覆をインラインで行う、[6]〜[8]のいずれかに記載の被覆方法。
[10]
[6]〜[9]のいずれかに記載の方法によって得られる下塗り層で被覆された基材の上に、下塗り層と反応させることができる被覆を施すことから構成される工程を含む、複合材料の製造方法。
[11]
被覆が、
・少なくとも1種類の金属及び/又は少なくとも1種類の金属酸化物の少なくとも1つの層;
・少なくとも1つのインクの層;及び
・少なくとも1つの接着剤の層;
から選択され;
好ましくは、被覆は少なくとも1種類の金属、特にアルミニウムの少なくとも1つの層から構成される、[10]に記載の複合材料の製造方法。
[12]
[10]又は[11]に記載の方法によって得られる複合材料。
[13]
被覆が、少なくとも1種類の金属及び/又は少なくとも1種類の金属酸化物の少なくとも1つの層であり、1cc/m 2 /日以下の酸素及び水蒸気透過速度を有する、[12]に記載の複合材料。
[14]
被覆が、少なくとも1種類の金属及び/又は少なくとも1種類の金属酸化物の少なくとも1つの層であり、湿潤及び乾燥条件下での被覆の接着力は少なくとも500gF/38mmである、[12]又は[13]のいずれかに記載の複合材料。
[15]
基材が、部分的に、基材それ自体、及び/又は被覆基材、及び/又は被覆され下塗り層が施された基材に由来するリサイクル製品を含む、[12]〜[14]のいずれかに記載の複合材料。
[16]
[12]〜[15]のいずれかに記載の複合材料、或いは[10]又は[11]のいずれかに記載の方法の結果として得られる複合材料を含むことを特徴とする、食品及び非食品包装材、グラフィックアート用のフィルム又はシート、装飾用のフィルム又はシート、基材保護用のフィルム又はシート、並びに建築部門において断熱及び湿気に対する保護のためのフィルム又はシートからなる群から選択される物品。
Claims (16)
- ポリマーフィルムの下塗り層として用いられる被覆組成物であって:
・アクリル及び/又はメタクリルポリマーの全重量に対して少なくとも50重量%のゲル含量を有し、高度に架橋されたラテックスの形態である、少なくとも1種類のアクリル及び/又はメタクリルポリマー;
・少なくとも1種類の架橋剤;
・スルホニルオキシ基を有する少なくとも1種類の水溶性又は水分散性ポリエステル;
を含み、
前記架橋剤は、高度に架橋されたアクリル及び/又はメタクリルポリマーに加えられ、粒子の形態の前記ポリマーの界面架橋を可能にし、
前記アクリル及び/又はメタクリルポリマーは、アクリル及び/又はメタクリルモノマーの全重量を基準として、60重量%未満の部分的に親水性のモノマーを含む、前記被覆組成物。 - アクリル及び/又はメタクリルポリマーが水相中に分散しているポリマー粒子の形態である、請求項1に記載の被覆組成物。
- 架橋剤がアミンベースの樹脂、好ましくはメラミンアルデヒド、ベンゾグアナミンアルデヒド、又はその誘導体である、請求項1及び2のいずれかに記載の被覆組成物。
- 架橋剤に対するアクリル及び/又はメタクリルポリマーの重量基準の割合(重量/重量)が、95/5〜70/30の間、より好ましくは90/10〜75/25の間、更により好ましくは85/15〜80/20の間である、請求項1〜3のいずれかに記載の被覆組成物。
- スルホニルオキシ基を有する水溶性又は水分散性ポリエステルの含量が、アクリル及び/又はメタクリルポリマーの乾燥重量に対して2〜30重量%の間、より好ましくは5〜20重量%の間、更により好ましくは8〜12重量%の間である、請求項1〜4のいずれかに記載の被覆組成物。
- 以下の:
(a)基材を与え;
(b)場合によっては、基材の物理的表面処理を行い;
(c)基材の少なくとも1つの面を、請求項1〜5のいずれかに記載の被覆組成物で被覆し;そして
(d)被覆を架橋して下塗り層を得て、ここで、下塗り層の中で、高度に架橋されたアクリル及び/又はメタクリルポリマーが粒子の形態で界面架橋され、下塗り層の表面における遊離酸官能基の残留レベルは、下塗り層中に含まれるポリマーの全重量に対して少なくとも5重量%である;
工程を実施することを特徴とする、下塗り層の少なくとも1つの層で基材を被覆する方法。 - 基材が、ポリエステルフィルム、好ましくはポリエチレンテレフタレート(PET)のフィルムであり、その厚さは、好ましくは150μm(マイクロメートル)以下、より好ましくは4μm〜100μmの間、より好ましくは4μm〜40μmの間、更により好ましくは4μm〜12μmの間である、請求項6に記載の被覆方法。
- 基材上に得られる下塗り層が、200nm(ナノメートル)以下、より好ましくは40nm〜120nmの間、より好ましくは50nm〜100nmの間、更により好ましくは60nm〜90nmの間の厚さEを有する、請求項6及び7のいずれかに記載の被覆方法。
- 基材の被覆をインラインで行う、請求項6〜8のいずれかに記載の被覆方法。
- 請求項6〜9のいずれかに記載の方法によって得られる下塗り層で被覆された基材の上に、下塗り層と反応させることができる被覆を施すことから構成される工程を含む、複合材料の製造方法。
- 被覆が、
・少なくとも1種類の金属及び/又は少なくとも1種類の金属酸化物の少なくとも1つの層;
・少なくとも1つのインクの層;及び
・少なくとも1つの接着剤の層;
から選択され;
好ましくは、被覆は少なくとも1種類の金属、特にアルミニウムの少なくとも1つの層から構成される、請求項10に記載の複合材料の製造方法。 - 請求項10又は請求項11に記載の方法によって得られる複合材料。
- 被覆が、少なくとも1種類の金属及び/又は少なくとも1種類の金属酸化物の少なくとも1つの層であり、1cc/m2/日以下の酸素及び水蒸気透過速度を有する、請求項12に記載の複合材料。
- 被覆が、少なくとも1種類の金属及び/又は少なくとも1種類の金属酸化物の少なくとも1つの層であり、湿潤及び乾燥条件下での被覆の接着力は少なくとも500gF/38mmである、請求項12又は13のいずれかに記載の複合材料。
- 基材が、部分的に、基材それ自体、及び/又は被覆基材、及び/又は被覆され下塗り層が施された基材に由来するリサイクル製品を含む、請求項12〜14のいずれかに記載の複合材料。
- 請求項12〜15のいずれかに記載の複合材料、或いは請求項10又は11のいずれかに記載の方法の結果として得られる複合材料を含むことを特徴とする、食品及び非食品包装材、グラフィックアート用のフィルム又はシート、装飾用のフィルム又はシート、基材保護用のフィルム又はシート、並びに建築部門において断熱及び湿気に対する保護のためのフィルム又はシートからなる群から選択される物品。
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2013
- 2013-12-19 FR FR1363002A patent/FR3015509B1/fr active Active
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2014
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- 2014-12-19 JP JP2016541171A patent/JP6532469B2/ja active Active
- 2014-12-19 KR KR1020167019226A patent/KR20160099677A/ko not_active Application Discontinuation
- 2014-12-19 US US15/103,513 patent/US10590300B2/en active Active
- 2014-12-19 PL PL14830842T patent/PL3083852T3/pl unknown
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Publication number | Publication date |
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FR3015509B1 (fr) | 2016-01-22 |
EP3083852A1 (fr) | 2016-10-26 |
KR20160099677A (ko) | 2016-08-22 |
WO2015092329A1 (fr) | 2015-06-25 |
US20160312056A1 (en) | 2016-10-27 |
US10590300B2 (en) | 2020-03-17 |
JP2017510666A (ja) | 2017-04-13 |
EP3083852B1 (fr) | 2017-11-15 |
MY178846A (en) | 2020-10-21 |
FR3015509A1 (fr) | 2015-06-26 |
PL3083852T3 (pl) | 2018-04-30 |
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