JP2019531363A - 低レベルのポリアミド66コモノマーを含有するポリアミド6樹脂 - Google Patents
低レベルのポリアミド66コモノマーを含有するポリアミド6樹脂 Download PDFInfo
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Abstract
Description
本出願は、米国特許法第119条(e)の下、各々の開示内容全体が明白に本明細書に援用される2016年12月15日に出願された「POLYAMIDE 6 RESINS CONTAINING A LOW LEVEL OF POLYAMIDE 66 COMONOMER」と題する米国仮特許出願第62/434,698号及び2016年7月28日に出願された「POLYAMIDE 6 RESINS CONTAINING A LOW LEVEL OF POLYAMIDE 66 COMONOMER」と題する米国仮特許出願第62/367,753号の利益を主張するものである。
本発明は、ポリアミド材料、特に、インフレーションフィルム用途に有用であるポリアミド6とポリアミド66とのコポリマーに関する。
本開示は、例えばインフレーションフィルムの製造に有用である、低レベルのポリアミド66コモノマーを含有するポリアミド樹脂の組成物を提供する。
例示的な配合物を、示差走査熱量測定を用いて試験し、ASTM D3418に従って融点温度(Tm)及び結晶化温度(Tc)を、ASTM E2070に従って等温結晶化時間(t1/2)を特定した。
図4を参照すると、様々な組成物の結晶化速度の対数を、温度の関数として特定した。実線は、実験データを示し、破線は、Sestak−Berggren方程式に基づいた結晶化速度の外挿値を示す。図4の上側の曲線に示されるように、PA6ホモポリマーの結晶化速度は、相対的に高い。
様々な量のカプロラクタム及びAH塩を含有するポリアミド組成物を、ペレットの形態で作製した。各組成物のペレットは、表1に示すカプロラクタム及びAH塩のモルパーセントに従って作製した。各サンプルにおいて、ポリアミド組成物は、カプロラクタム及びAH塩のモノマーから連続プロセスで作製した。各段階の温度は、260℃に設定し、流量は、約7000lb/時間とした。
実施例3
様々な量のカプロラクタム及びAH塩を含有するポリアミド組成物を、ペレットの形態で作製した。各組成物のペレットは、表2に示すカプロラクタム及びAH塩のモルパーセントに従って作製した。
以下の表3に示されるように、様々なコポリマーを、その対応する特性について試験し、70重量%のPA6ホモポリマーと30重量%のPA6/66コポリマーとのブレンド(比較例3)と比較した。コポリマーは、70重量%のB40 PA6ホモポリマーと30重量%のC40L PA6/66コポリマーとの物理的粉末ブレンド又は溶融ブレンドを、250℃の溶融温度で運転する一軸押出機に供給することによる連続溶融重合を用いて作製した。
様々な量のカプロラクタム及びAH塩を含有するポリアミド組成物を、ペレットの形態で作製した。核磁気共鳴(NMR)分光用のサンプルを、5mmのNMRチューブに調製した。各サンプルのおよそ25mgを秤量し、1mLの重水素化H2SO4に溶解して透明溶液を得た。この溶液を、0.2mLのCDCl3溶液又は0.2mLのCD3COCD3溶液のいずれかで外部からロックし、スペクトルを、100MHz(13C)NMR測定器で記録した。13C定量NMRスペクトルを、プログラム(例:Brukerパルスプログラム)を用いて取得した。
様々な量のカプロラクタム及びAH塩を含有するポリアミド組成物を、ペレットの形態で作製した。平行板流動性測定は、TA Instruments Discovery HR−2 Hybrid Rheometerなどのレオメーターで行った。4〜5グラムのサンプルを25mmローターの間に置き、ローター間のギャップを1mmに調節した。クロスオーバー実験のために、0.1ラジアン/秒〜700ラジアン/秒の範囲内の周波数スイープ実験を行った。100秒間にわたって50パスカル(Pa)の一定のせん断を掛け、モニタリングしてクリープ回復を測定した。試験は260℃の温度で行った。
様々な量のカプロラクタム及びAH塩を含有するポリアミド組成物を、ペレットの形態で作製した。溶融強度試験は、測定器(例:Gottfert Rheotens測定器)を測定器の取扱説明書に開示される標準的な手順に従って用いて行った。レオメーターは、直径2mm、長さ10mmのダイを用いて260℃で運転した。溶融押出し物を引取りホイールで加速し、溶融押出し物が破断した時点で得られた荷重を記録する。結果を図8及び以下の表5に示す。
単層のサンプルフィルムを、3つの押出機を含むインフレーションフィルム装置によって作製した。表7に示され、本明細書で考察される貫入抵抗などのフィルムの様々な特性を測定した。
サンプルフィルムを、工業的熱成形加工のシミュレーションとして試験した。試験は、図9に示される実験用熱成形機で行った。475mm×380mmのサイズのシートを、400Fで30秒間予備加熱した。シートを、真空を用いて金型で深絞りした。金型は、型の基部の長方形の周囲が23.75インチ、型の上部の長方形の周囲が21.5インチ、各長辺側の基部の直線エッジの長さが5.75インチ、各短辺側の基部の直線エッジの長さが3インチ、各長辺側の上部の直線エッジの長さが5インチ、各短辺側の上部の直線エッジの長さが3インチ、及び型の高さが1.4375インチであった。試験すべきフィルムを金型上で伸長し、次にフィルムが図9に示されるような形状となるように、金型の下から真空吸引を施すことによって金型上にドローダウンさせた。フィルムの成形後、図9に示されるように、「0」で示される金型の中央に対して測定したフィルムに沿った様々な位置(−4、−2、0、2、4)でフィルムの厚さを測定した。
(伸長フィルム厚さ/元のフィルム厚さ)×100
図11に示されるように、実施例3Dは、熱成形後、95.6%の最も高い残肉厚さを有することから、最も一定の厚さプロファイルを示す。さらに、図11から、実施例3B〜3Dは、比較例3よりも高い残肉厚さ(熱成形後の%)を有する。
Claims (15)
- インフレーションフィルムを形成する方法であって、
ポリアミドコポリマーを押出してポリアミドフィルムを形成することを含み、
前記ポリアミドコポリマーは、カプロラクタム及びヘキサメチレンジアミンアジペートの混合物から形成され、前記カプロラクタムは、カプロラクタム及びヘキサメチレンジアミンアジペートの合計モル数の85モル%乃至99モル%を占める、
方法。 - 前記ポリアミドコポリマーが、連続重合の一連の過程で、カプロラクタム及びヘキサメチレンジアミンアジペートの前記混合物を重合することによって形成される、請求項1に記載の方法。
- ポリエチレンポリマーを押出してポリエチレンフィルムを形成すること、及び
前記ポリアミドフィルム及びポリエチレンフィルムを組み合わせて多層フィルムを形成すること、
をさらに含む、請求項1に記載の方法。 - 前記ポリアミドコポリマーを押出すことが、吹込みポートを通して空気を吹込むことによって、前記押出されたポリアミドコポリマー中にバブルを形成すること、及び、前記押出されたポリアミドコポリマーを1又は複数のローラーで巻き取って前記ポリアミドフィルムとすること、を含む、請求項1に記載の方法。
- 前記ポリアミドコポリマーが、170℃で1.25分乃至12分の等温結晶化時間を有する、請求項1に記載の方法。
- 前記ポリアミドコポリマーが、170℃で1.0分から乃至14分の等温結晶化時間を有する、請求項1に記載の方法。
- 前記ポリアミドコポリマーが、0.95乃至1.1のランダム度を有する、請求項1に記載の方法。
- 前記ポリアミドコポリマーが、55in−lbf乃至95in−lbfの貫入抵抗を有する、請求項1に記載の方法。
- ポリアミド層を含むインフレーションフィルムであって、前記ポリアミド層は、カプロラクタム及びヘキサメチレンジアミンアジペートの混合物から形成されたポリアミドコポリマーを含み、前記カプロラクタムは、カプロラクタム及びヘキサメチレンジアミンアジペートの合計モル数の85モル%乃至99モル%を占める、インフレーションフィルム。
- 前記ポリアミドコポリマーが、140℃乃至170℃の結晶化温度を有する、請求項9に記載のインフレーションフィルム。
- 前記ポリアミドコポリマーが、55in−lbf乃至95in−lbfの貫入抵抗を有する、請求項9に記載のインフレーションフィルム。
- カプロラクタム及びヘキサメチレンジアミンアジペートの混合物から形成されるポリアミドコポリマーであって、前記カプロラクタムは、カプロラクタム及びヘキサメチレンジアミンアジペートの合計モル数の85モル%乃至99モル%を占め、前記コポリマーは、190℃乃至205℃の融点を有する、ポリアミドコポリマー。
- 前記コポリマーが、0.95乃至1.1のランダム度を有する、請求項12に記載のポリアミドコポリマー。
- 前記コポリマーが、85%乃至97%の残肉厚さを有する、請求項12に記載のポリアミドコポリマー。
- 前記コポリマーが、55in−lbf乃至95in−lbfの貫入抵抗を有する、請求項12に記載のポリアミドコポリマー。
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