JP6767923B2 - 透明なプラスチック・ホイルの被覆及びシールのための、直接接着性の透明なヒートシール可能結合剤 - Google Patents
透明なプラスチック・ホイルの被覆及びシールのための、直接接着性の透明なヒートシール可能結合剤 Download PDFInfo
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- JP6767923B2 JP6767923B2 JP2017098053A JP2017098053A JP6767923B2 JP 6767923 B2 JP6767923 B2 JP 6767923B2 JP 2017098053 A JP2017098053 A JP 2017098053A JP 2017098053 A JP2017098053 A JP 2017098053A JP 6767923 B2 JP6767923 B2 JP 6767923B2
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Description
本発明の目的は、適切なポリマーの開発及び調合を通して、様々なポット材料に対して、特に透明な外観を有するポリスチレン、ポリエステル又はPVCに対して、PETホイル及びPET被覆ホイルをシールするのに適した、PVC非含有のヒートシール可能なラッカーを提供することであった。
上記目的は、種々のタイプの基材のシールに適した、膜形成分散物を含んだヒートシール可能な被覆系によって達成され、この分散物は、全体で25質量%〜65質量%、好ましくは35質量%〜60質量%、特に好ましくは40質量%〜55質量%の、構成要素A、B及びCの混合物を含み、ここで分散物の全固形物量は、25〜70質量%であることを特徴とする。この混合物は、ここで、以下の組成によって特徴付けられる:
ポリマー・タイプAとして、15質量%〜50質量%、好ましくは25質量%〜45質量%、特に好ましくは30質量%〜40質量%のポリエステル又はポリエステル混合物、
ポリマー・タイプBとして、15質量%〜50質量%、好ましくは25質量%〜45質量%、特に好ましくは30質量%〜40質量%のポリ(メタ)アクリレート又は2つ若しくはそれ以上のポリ(メタ)アクリレートの混合物、及び、
ポリマー・タイプCとして、15質量%〜40質量%、好ましくは20質量%〜35質量%、特に好ましくは25質量%〜30質量%の、スチレン繰り返し単位を有する1つ又はそれ以上のゴム。
当業者であれば、本発明の被覆組成物に適したポリマー・タイプAのポリエステルの選択を原理的に容易にできる。ここで、非常に広範囲のポリエステルを使用することができる。当業者が使用できる選択基準は、特に、それぞれの溶媒に対するポリエステルの溶解度、及び食品に接触する用途のために、この構成要素の食管法のもとでの適切な認可である。
ポリマー・タイプBは例えば、本発明の分散物の製造中にグラフト・コポリマーABと一緒に形成することができる。任意の生成物構成成分AB内のこれらのB鎖の組成は、同じく以下の記述に対応する。同じことは任意構成成分CBのB鎖にも当てはまる。ここで、個々の構成要素Bが互いに異なることが完全に可能であり、及び/又は構成要素Bの複数の異なるポリマーが互いに一緒に存在することも同様に可能である。これらの構成成分Bの全ての組成に対して、以下のことが当てはまることが好ましい。
本発明により、ポリマー・タイプCは、SEBS、グラフトされたSEBS、SEB、主としてスチレンと、アルキル部分として少なくとも12個の炭素原子を有する(メタ)アクリレートとから構成されるコポリマー、又は少なくとも2つのこれらの構成要素の混合物である。
任意で存在するグラフト・ポリマーABの製造
グラフト・コポリマーABの製造のための本発明による方法は、具体的には、(メタ)アクリレートのフリーラジカル重合の反応中心を形成する、タイプAのポリマー内のイタコン酸繰り返し単位の二重結合を有する、グラフト可能な基に関して以下の後の段階で説明する、適切な開始剤の反応を特徴とする。「反応中心」という用語は、フリーラジカル重合のための1つ又はそれ以上の開始剤単位を含むポリマー鎖を意味する。これらの開始剤単位は同時に又は異なる時に形成することができる。従ってまた、イタコン酸単位が、他のイタコン酸単位において形成された他のフリーラジカルが停止反応によって非活性化された後にのみ、活性化される可能性も高い。
グラフト・ポリマーCBは一般に、任意で適切な乳化剤を用いて、構成要素Cの分散物を製造し、これに、この目的に適した反応条件下で、ポリマー・タイプBをもたらすモノマーをグラフトすることによって、製造される。タイプCBの適切な乳化剤を製造するための方法はそれ自体が既知であり、例えば、転移グラフト法によって実施することが可能である(さらに、Houben−Weyl著、Methoden der Org. Chemie[有機化学の方法(Methods of organic chemistry)]1411巻、114ページ、及び、H.A.J.Battaerd, G.W.Tregear著、Polymer Reviews,16巻、Interscience (1967)を参照されたい)。
本発明の被覆組成物はまた、ポリマー・タイプA、B及びC、並びに任意でグラフト・ポリマーAB及びCB、並びにさらに任意で他の添加物質、と一緒に溶媒系Lを含む。
使用したホイル材料:
紙/アルミニウム/ポリエステル・ホイルの複合ホイル(例えば、Flexpap、Constantia)
PETホイル、厚さ36μm、両面未処理、透明。このホイル自体のヘイズ値は9.2%である。このホイルは、例えば、三菱ポリエステルフィルム(Mitsubishi Polyester Films)から入手可能である。
BOPPホイルはコンスタンチア(Constantia)から購入し、外側をコロナ前処理した。
フェルンホルツからの熱成形可能ポリスチレン・ホイル
フェルンホルツからの非晶質ポリエチレンテレフタレート(APET)
フェルンホルツからの熱成形可能ポリプロピレン(PP)ホイル
実験室におけるヒートシール可能溶液の塗布:
MTVメステクニーク(Messtechnik)からの手動塗装機(ドクターブレード系)を、ヒートシール可能溶液を塗布するのに使用した(濡れ層厚24μm及び20μm)。ここで、結果として得られた乾燥層厚は4μm〜7μm及び2μm〜4μmであった。
短時間(5〜10分)の空気乾燥の後、ホイルを対流式オーブン内で、120℃〜200℃において15秒間乾燥させた。
ブルッガー(Brugger)からのヒートシール装置(HSG/ET)を使用してシール法を実行した。
1. PSポット材料及びAPETポット材料に対する、紙/metPETホイル、アルミニウム・ホイル、AIPETホイル及びPET36ホイルのシール
温度 180℃
圧力 3bar
時間 0.5sec
シール面積 100mm×10mm
2. PPポット材料に対する、紙/metPETホイル、アルミニウム・ホイル、AIPETホイル及びPET36ホイルのシール
温度 200℃
圧力 6bar
時間 1sec
3. APET、PP及びPSポット材料に対する、BOPPホイルのシール
温度 160℃
圧力 3bar
時間 0.5sec
構成要素A(ポリエステル):
表1に、ここで構成要素Aの例として用いたコポリマー(タイプA1及びA2)の特性を載せてある。ここで材料は、ポリカルボン酸の総量に基づいてイタコン酸を有する及び有しない半芳香族線状コポリマーである。
エボニック・インダストリーズAGからのメチルメタクリレート(MMA)、>99%、非安定化
エボニック・インダストリーズAGからのn−ブチルメタクリレート(nBMA)、>99%、非安定化
エボニック・インダストリーズAGからのイソボルニルメタクリレート(IBOMA)
4500g/mol〜5000g/molのモル質量を有する水素化ヒドロキシプロピル末端ポリブタジエンのメタクリル酸エステル(サルトマ(Sartomer)から);ブレンタグ(Brenntag)からの、10〜15ppmのp−tert−ブチルカテコールで安定化されたスチレン。
使用したスチレンゴム材料
表2:使用したゴムタイプの性質の概観
MFI:メルトフロー・インデックス;ここでタイプ3及び4のMFIはまた200℃で計測されるとき1〜40g/10minであることに留意されたい。
58.3gの酢酸ブチルと57.5gのマクロアルコール(macroalcohol)メタクリレートを、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器の中の、115℃における初期充填物として用い、10.0gの酢酸ブチルに溶解させた1.15gの3級ブチルペルオキシ2−エチルヘキサノエート(ペロキサン(Peroxan)PO)を用いて開始した。5分後、この溶液に、23.0gのスチレン、8.6gのMMA及び15.0gの酢酸ブチルの溶液を、60分間にわたって滴下した。3時間後、結果として得られた反応混合物に、35.4gのポリエステル・タイプA1、92.0gのポリエステル・タイプA2、及び175.1gの酢酸プロピルから構成されるポリエステル溶液287.5gを加えた。ひとたび内部温度を115℃に再設定した後、この系内に、25.9gのMMA、及び20.0gの酢酸ブチル中の0.63gのペロキサンPOの溶液を、60分間にわたって計量添加した。計量添加が終了した30分後及び90分後に、5.0gの酢酸ブチル中の0.23gのペロキサンPOを、いずれの場合にも、追加開始(post initiation)のために使用した。最後の追加開始の240分後、反応混合物を冷却し(<30℃)、ナイロン織物(メッシュ幅125μm)を通して濾過した。
58.7gのタイプ3のSEBSゴムを、65.6gのポリエステル・タイプA2、22.1gのポリエステル・タイプA1及び288.2gの酢酸プロピルの溶液の中に、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器の中で、98℃において2時間にわたって溶解させた。次に、溶液に、8.3gの酢酸プロピル中に溶解させた0.44gのペロキサンPOを加え、さらに5分後に、44.0gのMMA、44.0gのnBMA及び14.6gの酢酸プロピル中の1.32gのペロキサンPOの溶液の計量添加を、98℃において開始し、90分間続けた。この反応混合物に、30分後、90分後及び150分後に、いずれの場合にも8.3gの酢酸プロピルに溶解させたいずれの場合にも0.176gのペロキサンPOを98℃において加えることによって重合を完了させた。さらに180分後に、混合物を冷却し、ナイロン濾し器(メッシュ幅125μm)を通して濾過した。
製造プロセスには、発明実施例2において使用した手順及び原材料量を使用した。タイプ3のゴムの代わりに、51.8gのタイプ4のゴムを溶解させ、ポリエステル及びゴムを溶解させるための溶媒の量は、281.0gに調節した。
製造プロセスには、発明実施例2において使用した手順及び原材料量を使用した。タイプ3のゴムの代わりに、58.7gのタイプ2を用いた。
92.25gのタイプ2のSEBSゴムを、120.0gのポリエステル・タイプA2、18.4gのポリエステル・タイプA1及び464.8gの酢酸プロピルの溶液の中に、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器の中で、98℃において2時間にわたって溶解させた。次に、この溶液に、13.0gの酢酸プロピル中に溶解させた0.692gのペロキサンPOを加え、さらに5分後に、69.1gのMMA、69.1gのnBMA及び23.0gの酢酸プロピル中の2.076gのペロキサンPOの溶液の計量添加を、98℃において開始し、90分間続けた。反応混合物に、30分後、90分後及び150分後に、いずれの場合にも13gの酢酸プロピルに溶解させたいずれの場合にも0.277gのペロキサンPOを98℃において加えることによって重合を完了させた。さらに180分後に、混合物を冷却し、ナイロン濾し器(メッシュ幅125μm)を通して濾過した。
102.5gのタイプ2のSEBSゴムを、121.0gのポリエステル・タイプA2、32.8gのポリエステル・タイプA1及び511.0gの酢酸プロピルの溶液の中に、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器の中で、98℃において2時間にわたって溶解させた。次に、この溶液に、13.0gの酢酸プロピル中に溶解させた0.769gのペロキサンPOを加え、さらに5分後に、84.0gのMMA、69.7gのnBMA及び23.0gの酢酸プロピル中の2.306gのペロキサンPOの溶液の計量添加を、98℃において開始し、90分間続けた。反応混合物に、30分後、90分後及び150分後に、いずれの場合にも13gの酢酸プロピルに溶解させたいずれの場合にも0.308gのペロキサンPOを98℃において加えることによって重合を完了させた。さらに180分後に、混合物を冷却し、ナイロン濾し器(メッシュ幅125μm)を通して濾過した。
112.8gのタイプ2のSEBSゴムを、110.7gのポリエステル・タイプA2、36.9gのポリエステル・タイプA1及び393.9gの酢酸プロピルの溶液の中に、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器の中で、98℃において2時間にわたって溶解させた。次に、この溶液に、13.0gの酢酸プロピル中に溶解させた0.748gのペロキサンPOを加え、さらに5分後に、74.8gのMMA、74.8gのnBMA及び23.0gの酢酸プロピル中の2.245gのペロキサンPOの溶液の計量添加を、98℃において開始し、90分間続けた。反応混合物に、30分後、90分後及び150分後に、いずれの場合にも13gの酢酸プロピルに溶解させたいずれの場合にも0.299gのペロキサンPOを98℃において加えることによって重合を完了させた。さらに180分後に、混合物を冷却し、117.2gの酢酸エチルで希釈し、ナイロン濾し器(メッシュ幅125μm)を通して濾過した。
112.8gのタイプ2のSEBSゴムを、115.2gのポリエステル・タイプA2、32.8gのポリエステル・タイプA1及び511.0gの酢酸プロピルの溶液の中に、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器の中で、98℃において2時間にわたって溶解させた。次に、この溶液に、13.0gの酢酸プロピル中に溶解させた0.746gのペロキサンPOを加え、さらに5分後に、54.1gのMMA、74.6gのnBMA、20.5gのIBOMA及び23.0gの酢酸プロピル中の2.239gのペロキサンPOの溶液の計量添加を、98℃において開始し、90分間続けた。反応混合物に、30分後、90分後及び150分後に、いずれの場合にも13gの酢酸プロピルに溶解させたいずれの場合にも0.298gのペロキサンPOを98℃において加えることによって重合を完了させた。さらに180分後に、混合物を冷却し、ナイロン濾し器(メッシュ幅125μm)を通して濾過した。
65.0gのドゥトラル(Dutral)CO 043、26.0gのタイプA1のポリエステル、及び104.0gのタイプA2のポリエステル、及びさらに120.0gの適切な乳化剤を、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器中の335gの酢酸プロピル及びさらに60.0gのシクロヘキサン(CH:cyclohexane)中への初期充填物として用い、混合物を95℃において、全ての材料が溶解するまで撹拌した。次に、2.60gの3級ブチルペルオキシ2−エチルヘキサノエートを、64.9gのメチルメタクリレートと64.9gのブチルメタクリレートとの混合物と混合し、結果として得られた混合物を系中に、軽量ポンプを用いて95℃で1.5時間にわたって計量添加した。ひとたび添加が終了すると、さらに0.26gの3級ブチルペルオキシ2−エチルヘキサノエートを、1時間離れた2つの時点の各々において加え、さらに2時間、混合物を撹拌した。反応混合物を冷却し、ナイロン・フィルター(メッシュ幅125μm)を通して濾過した。
製造プロセスには、発明実施例2に使用された手順及び原材料量を使用した。タイプ3のゴムの代わりに、58.7gのタイプ1のゴム(SBSゴム)を用いた。
113.4gのポリエステル・タイプA2及び20.0gのポリエステル・タイプA1を、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器内で、300.0gの酢酸プロピルに98℃で溶解させた。次に、66.6gのタイプ2のSEBSゴムを加え、混合物の溶解をさらに2時間続けた。反応混合物は、冷却後ナイロン・フィルター(メッシュ幅125μm)で濾過することができなかった。
136.5gのタイプ2のSEBSゴムを、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器内で、98℃において2時間にわたって溶解させた。この溶液に、13.0gの酢酸プロピルに溶解させた1.367gのペロキサンPOを加え、5分後に、136.5gのMMA、136.9gのnBMA及び23.0gの酢酸プロピルに溶解させた4.012gのペロキサンPOの計量添加を開始し、90分間続けた。反応混合物に、30分後、90分後及び150分後に、いずれの場合にも13gの酢酸プロピルに溶解させたいずれの場合にも0.547gのペロキサンPOを98℃において加えることによって重合を完了させた。さらに180分後に、混合物を冷却し、粘度調節のために267.5gの酢酸プロピルでさらに希釈し、次いで、ナイロン濾し器(メッシュ幅125μm)を通して濾過した。
66.6gのタイプ2のSEBSゴムを、サーモスタット、還流冷却器、翼攪拌器及び内部温度計を装着したジャケット付き容器内の300.0gの酢酸プロピル内への初期充填物として用い、そこに、133.4gのポリエステル・タイプA2をゆっくり加えた。この混合物を98℃に加熱し、次いで240分間にわたって均質にした。反応混合物は、冷却後ナイロン・フィルター(メッシュ幅125μm)で濾過することができなかった。
dl=フィルム材料からのシール可能層の剥離。
Claims (12)
- 様々なタイプの基材のシールに適した、フィルム形成分散物を備えるヒートシール可能な被覆系において、前記分散物は全体で25質量%〜65質量%の、構成要素A、B及びCの混合物を含み、前記混合物は、いずれの場合にもポリマー・タイプA、B及びCの組成物全体に基づいて
15質量%〜50質量%の、ポリマー・タイプAとしてのポリエステル、又はポリエステルの混合物と、
15質量%〜50質量%の、ポリマー・タイプBとしてのポリ(メタ)アクリレート、又は2つ若しくはそれ以上のポリ(メタ)アクリレートの混合物と、
15質量%〜40質量%の、ポリマー・タイプCとしてのスチレン繰り返し単位を含む1つ又はそれ以上のゴムと、
から構成され、構成要素A、B及び/又はCはさらに、完全に又はある程度、グラフト・コポリマーAB又はCBの形態を取ることができ、
ポリマー・タイプCは、SEBS、グラフトされたSEBS、SEB、主としてスチレンと、アルキル部分として少なくとも12個の炭素原子を有する(メタ)アクリレートとから構成されるコポリマー、又は少なくとも2つのこれら構成要素の混合物であり、
前記分散物の固形物量は25〜70質量%である、
ことを特徴とする、前記被覆系。 - 前記ポリマー・タイプAは、
・700〜5000g/molの数平均モル質量Mnを有し、イタコン酸の共重縮合によって製造されるポリエステルA1、
・5000〜50000g/molの数平均モル質量Mnを有し、二重結合を有さないポリエステルA2、又は
・前記2つのポリエステルA1とA2の混合物、
であることを特徴とする、請求項1に記載の被覆系。 - 前記2つのポリエステルA1とA2の混合物が存在し、前記ポリエステルA1の数平均モル質量Mnが2000〜4000g/molであり、前記ポリエステルA2の数平均モル質量Mnが10000〜35000g/molであり、前記被覆系は、潜在的な構成成分AB及びCBを含めた前記ポリマー・タイプA、B、Cの組成物全体に基づいて、1質量%〜15質量%の前記ポリエステルA1及び10質量%〜50質量%の前記ポリエステルA2を含むことを特徴とする、請求項2に記載の被覆系。
- 前記イタコン酸含有ポリエステルA1は、使用するポリカルボン酸の総量に基づいて、0.1〜20mol%、好ましくは2〜8mol%の割合のイタコン酸を含むことを特徴とする、請求項2又は3のいずれか1項に記載の被覆系。
- 前記ポリマー・タイプAB及びCBは、ポリエステルでできている主鎖、及びゴムでできている主鎖をそれぞれ有し、かつポリ(メタ)アクリレートでできているペンダント鎖を有する、グラフト・コポリマーであることを特徴とする、請求項1から4のいずれか1項に記載の被覆系。
- 構成要素CはSEBSであるか、アクリル酸、メタクリル酸、マレイン酸及び/又は無水マレイン酸でグラフトされたSEBSであるか、SEBSとSEBの混合物であるか、或いは、主としてスチレンと、少なくとも12個の炭素原子を有する脂肪アルコール又は水素化ヒドロキシ末端ポリブタジエンの(メタ)アクリレートエステルとから構成されるコポリマーであることを特徴とする、請求項1から5のいずれか1項に記載の被覆系。
- 構成要素Cは、8〜45質量%の割合のスチレン繰り返し単位を含むことを特徴とする、請求項6に記載の被覆系。
- ISO1133−1に従い、温度200℃で5kg負荷によって計測される、構成要素Cのメルトフロー・インデックスが、1〜40g/10min、好ましくは4〜10g/10minであることを特徴とする、請求項6又は7に記載の被覆系。
- 前記分散物は、全体で、35質量%〜60質量%の、構成要素A、B及びCの混合物を含み、前記混合物は、いずれの場合にも前記ポリマー・タイプA、B及びCの組成物全体に基づいて、
25質量%〜45質量%の、ポリマー・タイプAとしてのポリエステル、又はポリエステルの混合物と、
25質量%〜45質量%の、ポリマー・タイプBとしてのポリ(メタ)アクリレート、又は2つ若しくはそれ以上のポリ(メタ)アクリレートの混合物と、
20質量%〜35質量%の、ポリマー・タイプCとしてのスチレン繰り返し単位を含む1つ又はそれ以上のゴムと、
から構成されることを特徴とする、請求項1から8のいずれか1項に記載の被覆系。 - 前記分散物は、全体で、40質量%〜55質量%の、構成要素A、B及びCの混合物を含み、前記混合物は、いずれの場合にも前記ポリマー・タイプA、B及びCの組成物全体に基づいて、
30質量%〜40質量%の、ポリマー・タイプAとしてのポリエステル、又はポリエステルの混合物と、
30質量%〜40質量%の、ポリマー・タイプBとしてのポリ(メタ)アクリレート、又は2つ若しくはそれ以上のポリ(メタ)アクリレートの混合物と、
25質量%〜30質量%の、ポリマー・タイプCとしてのスチレン繰り返し単位を含む1つ又はそれ以上のゴムと、
から構成されることを特徴とする、請求項1から9のいずれか1項に記載の被覆系。 - 前記ポリマー・タイプBは、(メタ)アクリル酸、ヒドロキシエチル(メタ)アクリレート、ヒドロキシプロピル(メタ)アクリレート、メチル(メタ)アクリレート、n−及び/又はイソプロピル(メタ)アクリレート、n−ブチル(メタ)アクリレート、及び(メタ)アクリル酸のC8−〜C22−脂肪アルコールエステル、のうちから選択された構成要素から構成されるモノマー混合物の共重合によって得られるコポリマーであることを特徴とする、請求項1から10のいずれか1項に記載の被覆系。
- ポリスチレン、ポリエステル及びポリ塩化ビニルに対するポリエステル・ホイル又はPET被覆ホイルをシールする方法において、前記ホイルは請求項1から11のいずれか1項に記載の被覆系で被覆され、前記被覆は乾燥され、シールされる材料の上に配置される前記ホイルの被覆される側は、ポリスチレン、ポリエステル又はPVCでできており、120〜220℃の温度において、1〜6MPaの圧力下で、0.1〜1.5sの間にシールされることを特徴とする、前記方法。
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2017
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- 2017-05-16 CN CN201710341104.2A patent/CN107384145B/zh active Active
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Also Published As
Publication number | Publication date |
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BR102017010356A2 (pt) | 2019-02-19 |
BR102017010356B1 (pt) | 2022-11-16 |
EP3246370B1 (de) | 2019-08-07 |
ES2747759T3 (es) | 2020-03-11 |
US20170335141A1 (en) | 2017-11-23 |
RU2017117050A (ru) | 2018-11-19 |
CA2967493A1 (en) | 2017-11-17 |
CN107384145A (zh) | 2017-11-24 |
US10195829B2 (en) | 2019-02-05 |
KR102368744B1 (ko) | 2022-02-28 |
RS59233B1 (sr) | 2019-10-31 |
EP3246370A1 (de) | 2017-11-22 |
HK1247228A1 (zh) | 2018-09-21 |
CN107384145B (zh) | 2021-05-18 |
RU2748348C2 (ru) | 2021-05-24 |
RU2017117050A3 (ja) | 2020-05-18 |
CA2967493C (en) | 2023-12-12 |
KR20170129621A (ko) | 2017-11-27 |
JP2017206694A (ja) | 2017-11-24 |
BR102017010356A8 (pt) | 2022-07-26 |
PL3246370T3 (pl) | 2020-02-28 |
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