JP2004523668A - Thermoplastic composition for fiber and film production - Google Patents

Abstract

The present invention provides a thermoplastic composition for use in the production of extruded fibers or films useful for applications such as carpets, rugs, woven fabrics, non-woven fabrics, spunbond fabrics, knits, clothes, and laminates.
A) 86-92 wt% of a thermoplastic polymer having a crystallization temperature higher than 160 ° C.,
b) A thermoplastic polymer composition comprising 14-8 wt% of a thermoplastic polymer having a crystallization temperature at least 5 ° C higher than a) and c) a compatibilizer.
[Selection diagram] Fig. 1

Description

を使用して計算できる。
好ましい繊維は２．７以下、最も好ましくは２．３以下の成分（ｂ）の粒子径分散をもつ。
【００６０】
前述のＤν及びＤ９９測定は繊維又はフィルム試料を吸蔵物の溶媒又はスウェル剤ではないマトリックスのための溶媒に溶解させることによって決定される。
シンジオタクチックビニル芳香族ポリマー吸蔵物の溶媒又はスウェル剤ではないポリアミドマトリックスのために好的な溶媒はギ酸又はギ酸水溶液である。マトリックスを溶解した後で、得られた分離吸蔵粒子材料をろ過で回収し、クロムでコートし、そして走査電子顕微鏡で写真を撮る。標準の、コンピューターによる粒子径分析技術は粒子径を測定するために使用される。
【００６１】
成分（ｂ）の吸蔵物粒子寸法及びこのようにして得られた繊維の性質を調節する技術はもしあれば、採用される相溶化剤、成分（ｃ）の種類と量；押し出し前の溶融状態で達成される混合の度合い；溶融熱可塑性ブレンド物の混合の完了と成分（ｂ）の凝集を許す条件下での繊維の押し出しとの間の時間遅れ量；もしあれば調合時に存在する核剤の種類と量、各成分（ａ）及び（ｂ）の相対粘度と熔融粘度、そしてその他のプロセス変数を含む。
【００６２】
本発明の利点は押し出し物又はフィラメントを同時に冷却する繊維の延伸又は紡糸の過程で、成分（ｂ）の吸蔵物は成分（ａ）に較べて延伸力の影響が少ないという事実によるものと信じられている。これはこの特許の目的のための差分延伸性と呼ばれる。本発明において好ましくは、成分（ａ）は押し出し及び繊維形成下で成分（ｂ）の吸蔵物より多く延伸される。より好ましくは、マトリックスポリマー（成分（ａ））は成分（ｂ）の吸蔵ポリマーより少なくとも２倍、より好ましくは少なくとも３倍多く延伸される。差分延伸性は全体の繊維又はフィルムの延伸：分散相の延伸の比を計ることによって決定される。全体の繊維又はフィルムの延伸は、粒子の質量保存の法則を仮定して、未延伸繊維又は未延伸フィルムと完全に延伸された繊維又は完全に延伸されたフィルムの断面積の比として定義される。分散相の延伸は未延伸繊維又は未延伸フィルム中の分散相と完全に延伸された繊維又は完全に延伸されたフィルム分散相の平均断面積の比として定義される。前述の差分延伸性の結果として、そのような吸蔵物部分は得られた繊維又はフィルムの表面から放出されるか、又はそのような吸蔵物が繊維又はフィルムの表面に近接しているために、マトリックス（成分（ａ））が吸蔵物より多くの度合いで延伸されるときにそれが大きな引落とし率を生ずるので、表面に突起、割れ目、又は他の不連続性又は不規則性を引き起こす。そのような粗い表面の繊維は望ましい低光沢、手触り、そして柔らかさ；天然繊維との類似性；そしてなお改良された紡糸性と延伸物性、高速な商業的繊維製造と繊維形成過程での摩擦力や引きずりを減少させる。金属との摩擦力が減少した繊維はさらに紡糸仕上のために採用される潤滑剤の使用量を減少させる。粗い表面のフィルムは同様にアンチブロック、少ない埃生成、及び製造過程での摩擦の減少のような望ましい性質をもつ。
【００６３】
差分延伸性は、本発明で強調したように、多くの変数によって影響を受ける。分散相のドメイン寸法は効果的な粗い表面を作ることができるために十分大きくなければならないが、しかし紡糸が困難になるレベルまで繊維の堅さを減少させるほど大きくてもいけない。分散相のドメイン寸法は溶融相で繊維紡糸の押し出し機又は分岐管中で過剰な合体が起こらない程度の滞留時間を与えるために安定でなければならない。分散相と連続相の間の界面の相溶化は繊維の紡糸性をドラマチックに減少させるしずくや破裂を防ぐ助けとなる。分散相と連続相の融点は両方の相が熔融してなお分解や繊維紡糸のために熱くなり過ぎないように十分近くなければならない。分散相と連続相のレオロジーは熔融混合の過程で望ましい粒子径を生成させるのに十分なだけ類似していなければならないが、しかし繊維紡糸の過程で異なった延伸性を許容するだけの差異がなければならない。結晶化の少量の発達はどちらの相の粘度もドラマチックに増大させる。結晶化力学は結晶化が始まる温度、最大結晶発達温度、又は温度に対する結晶化速度によって定量化できる。核剤又は結晶化抑制剤が結晶化力学を変化させるために使用することができる。いずれの相の粘度も又ポリマーの分子量変化又は流れ特性に影響を与える物質（例えば、可塑剤又は流れ促進剤）の添加によって増加させたり減少させたりすることができる。
【００６４】
連続相の分子量はまた分散相の延伸性を変えるために変化させることができる。同様に、流れ特性に影響を与えるための添加剤を連続相に添加してもよい。繊維紡糸における延伸力は繊維紡糸装置の延伸ゴデット（あて布）によって与えられる。延伸力は連続相を経由して分散相に与えられる。連続相の分子量が低いときは、容易に延伸できそして分散相には低い延伸力を与える。
【００６５】
押し出しフィルムの形成及びフィルムの単軸又は二軸延伸又はテンタリング（幅だし）
においても、得られるフィルムの表面に不規則性が形成されるという同様な現象が起こる。
そのようなフィルムは付着が少なくそしてブロッキング剤の添加を必要とせずに高速フィルム形成装置によって容易に処理することができる。さらに、そのようなフィルムは高速処理及び輸送プロセスの過程でダスト（埃）の生成が少ない。
【００６６】
繊維の性質における前述の利点は熱可塑性組成物中につや消し剤、特に二酸化チタンを含ませる必要なしで達成されるのではあるが、そのような添加物の添加が排除されるわけではないことを理解すべきである。もし存在するなら、その使用量は従来技術のナイロンベースの調合に較べて大幅に減らすことができる。使用する場合、つや消し剤の量は０．０１−０．３重量％そして好ましくは０．１重量％以下である。最も好ましくは、つや消し剤を使用しないことであり、それによって繊維、フィルム及び本発明に従った繊維又はフィルムを含む物品、特に二酸化チタンのようなつや消し剤が物理的性質に影響を与えるような射出成形品、ガラス繊維強化物品のリサイクル性を改良するのに有利である。
【００６７】
さらに、注文生産のダイ又はスピンナー（紡糸口金）の設計が、もし望むなら、改良された嵩をもつ繊維の製造をもたらす多突起形状を製造するために採用されてもよい。純粋なナイロン樹脂に比較したダイスエルの差異によって、特殊なダイの設計は本発明のポリマーブレンド組成物を最大限利用するために採用されることが好ましい。このダイの構造は図７に示され、そこでは細長い三つの突出物のあるダイ開口デザイン、７０、は一般的に平行な（図示したような）又は半円又は湾曲した末端、７２、で終わる収束面をもつ３個の等しい長さのスロット、７１、をもち、合計スロット長さ（三つの突出物の中心軸が交差する点のスロットの中心軸、７３、に沿って測定した）は０．０４５インチ（１．１４３ｍｍ）、スロット幅０．００７インチ（０．１７８ｍｍ）、キャピラリー長さ０．０４０インチ（１．０２ｍｍ）で１１．２のＭｏｄ率（ＭＲ）をもつ。好ましいダイは９から１２のＭｏｄ比をもつ。
【００６８】
ここで使用されるＭｏｄ比は多突起繊維又はダイの断面形状の二つの測定値の比を意味する。特に、それは二つの円の半径の比であり、その大きいほうは断面形状の中心に位置し全体の多突起形状に外接しそして小さいほうは多突起形状の内面に内接する。これは参照として図３に示され、そこでは多突起形状、３０、は三つの突起、３１、をもち、半径Ｒ１をもつ円３３に外接し、そして半径Ｒ２をもつ円、３３、に内接する。Ｍｏｄ比はＲ１／Ｒ２として定義される。本発明の繊維の好ましいＭｏｄ比は２．５−４である。
【００６９】
本発明に従った繊維及びフィラメントからなるヤーンは一般的に前述の要求に適合しない単独の熱可塑性ポリマー成分又はポリマーブレンド物として成分（ａ）を含むポリマー組成物から作られたヤーンと比較して高められた色透過性及び耐色あせ性、高められた染色保持性、改良された耐シミ性、改良された耐汚れ性、改良された寸法安定性、改良された染色安定性、及び減少した水分取り込みを示すことが見出された。成分（ｂ）の吸蔵物は繊維又はフィルムの表面エネルギーを低くしそして水溶液のシミでの表面濡れを減少させ、そして吸蔵物は成分（ａ）のように水分の影響を受けず、それによって水溶液流体のような外部物質の透過のためのより曲がりくねった道を与え、結果として大きな耐シミ性と染色保持性を生ずるものと考えられる。
【００７０】
さらに第一と第二の熱可塑性ポリマー成分が本発明に従った結晶化温度の観点から差異のある熱可塑性組成物の繊維から作られたヤーンは、工業においては互いに両立しないと思われていた良好な嵩高さと良好な耐久性の両方を示すことが見出された。ポリマーアロイ成分間の結晶化温度の差異は繊維の結晶化発達を調節する容易な手段を提供する。例えば、一つの相の結晶性はけん縮（ｃｒｉｍｐ）をセットするために使用することができ、一方他相の結晶性は撚糸ヒートセットＢＣＦヤーンにおいて撚りをセットするために使用することができた。本発明の熱可塑性組成物、特に熱可塑性成分（ａ）がポリアミドである、から作られたヤーンの追加された利点は、一成分、特に成分（ｂ）の結晶性は、撚糸のセッティングに使用するマトリックス中で結晶性が保持されつつ、延伸過程又は延伸とけん縮の過程のような１以上の工程でセットされるために、組成物のモルフォロジーと結晶性が繊維全体でより一致して作られることである。これは熟練した当業者にとって、仕上げられたカーペット中の染料取り込みの差異と付随する縞筋の問題を最小化するか取り除くための助けとなるであろう。さらに、衣類用繊維に関しては、もし繊維が延伸とテクスチャーリング工程を分離されるなら、繊維の緩和を減少させるか防止するために、十分な結晶性が紡糸や延伸工程においてセットされる。
【００７１】
前述の利点に従えば、優位性は、差分走査熱量計（ＤＳＣ）で測定したときの、その成分の結晶化温度の差異に基づいて熱可塑性ポリマー（ａ）と熱可塑性ポリマー（ｂ）を選択するときに見出される。 好ましくは、熱可塑性ポリマー（ａ）は熱可塑性ポリマー（ｂ）の結晶化温度よりも少なくとも２０℃小さい結晶化温度をもち、そして最も好ましくは熱可塑性ポリマー（ｂ）の結晶化温度よりも少なくとも４０℃小さい結晶化温度をもつ。特に好ましい態様においては、熱可塑性ポリマー（ａ）は好ましくは２５０℃を越えない、より好ましくは２４０℃を越えない、そして最も好ましくは２３０℃を越えない結晶化温度をもつ。特に好ましい態様においては、熱可塑性ポリマー（ｂ）は少なくとも１７０℃、より好ましくは少なくとも２００℃、最も好ましくは少なくとも２１５℃；好ましくは２８５℃を越えない、より好ましくは２８０℃を越えない、そして最も好ましくは２７５℃を越えない結晶化温度をもつ。
【００７２】
熱可塑性ポリマー（ａ）について
高度に好ましくは、熱可塑性ポリマー（ａ）は押し出し延伸ができ、又繊維に紡糸できるタクチックでないポリマーである。熱可塑性ポリマー（ａ）として使用するための典型的なポリマーとしては、ポリアミド、ポリエステル、ポリアクチン酸、ポリビニルシクロヘキサンのホモポリマー及びコポリマー、エチレン／スチレンインターポリマー、及びそれらの混合物が包含される。好適なポリエステルとしては、エチレングリコール、ポリエチレングリコール又はポリプロピレングリコールと芳香族ジカルボン酸、特にテレフタール酸、フタール酸、又はそれらの混合物との縮合コポリマーが包含される。好ましいポリエステルはポリエチレンテレフタレート（ＰＥＴ）又はポリエチレングリコールテレフタレート（ＰＥＧＴ）である。
【００７３】
熱可塑性ポリマー（ａ）として使用するための好ましいポリマーはポリアミド又はコポリアミドであり、またナイロン混合物を含むナイロンとも呼ばれる。好適なポリアミドとしては、例えば、４−１２の炭素原子をもつ脂肪族又は芳香族ジカルボン酸と２−１２の炭素原子をもつ脂肪族又は芳香族ジアミンの縮合によって得られる脂肪族及び芳香族のポリアミドを包含する。ここで使用されるポリアミドの合成での使用に好適な脂肪族ジカルボン酸の典型的なしかし網羅的ではないリストとしては、アジピン酸、ピメリン酸、アゼライン酸、スベリン酸、セバシン酸及びドデカンジオン酸が包含される。典型的な芳香族ジカルボン酸としては：フタール酸、イソフタール酸、テレフタール酸、及びナフタレンジカルボン酸が包含される。典型的な脂肪族ジアミンとしては、例えば、ヘキサメチレンジアミン及びオクタメチレンジアミンのようなアルキレンジアミンが包含される。好適な芳香族ジアミンは以下のものである：１，４−ジアミノベンゼン、１，３−ジアミノベンゼン、１，２−ジアミノベンゼンのようなジアミノベンゼン；２，４−ジアミノトルエン、
２，３−ジアミノトルエン、２，５−ジアミノトルエン、及び２，６−ジアミノトルエン
のようなジアミノトルエン；オルソ−、メタ−、及びパラ−キシレンジアミン；オルソ−、メタ−、及びパラ−２，２’−ジアミノジエチルベンゼン；４，４’−ジアミノビフェニル；４，４’−ジアミノビフェニル；４，４’−ジアミノジフェニルメタン；４，４’−ジアミノジフェニルエーテル；４，４’−ジアミノジフェニルチオエーテル；４，４’−ジアミノジフェニルケトン；及び４，４’−ジアミノジフェニルスルホンである。前述の脂肪族及び芳香族ジカルボン酸とジアミンの混合物もまたよく使用される。ラクタム又はω−アミノカルボン酸の自己縮合によるのと同様に、酸クロライドとアミン塩のような酸誘導体とアミン誘導体からポリアミドを製造することもまた可能である。そのようなラクタムの例としては、ε−カプロラクタム及びω−ラウロラクタムが包含される。そのようなω−アミノ酸の例としては、１１−アミノウンデカン酸、１２−アミノウンデカン酸、４−アミノフェニルカルボキシルメタン、１−（４−アミノフェニル）２−カルボキシルエタン、３−（４−アミノフェニル）１−カルボキシルプロパン、及びパラ−（３−アミノ−３’−ヒドロキシ）ジプロピルベンゼンが包含される。
【００７４】
成分（ａ）として好適な典型的な芳香族ポリアミドとしてはポリキシレンアジピン酸アミド；ポリヘキサメチレンテレフタール酸アミド；ポリフェニレンフタール酸アミド；ポリキシレンアジピン酸アミド／ヘキサメチレンアジピン酸アミド；ポリエステルアミドエラストマー；ポリエーテルアミドエラストマー；ポリエーテルエステルアミドエラストマー；及びダイマー状の酸共重合アミドが包含される。
【００７５】
熱可塑性ポリマー（ａ）として使用するのに好適な典型的な脂肪族ポリアミドとしては：ポリカプロラクタム（ナイロン−６）；ポリ（ヘキサメチレンアジピン酸アミド）（ナイロン６，６）；ナイロン−３，４；ナイロン−４；ナイロン−４，６；ナイロン−５，１０；ナイロン−６；ナイロン−６，６；ナイロン−６，９；ナイロン−６，１０；ナイロン−６，１２；ナイロン−１１；及びナイロン−１２が包含される。好ましい成分（ａ）のポリマーは脂肪族ポリアミド、特にナイロン６又はナイロン６，６、最も好ましくはナイロン６である。
【００７６】
熱可塑性ポリマー（ａ）は或る分子量と分子量分布（ＭＷＤ）をもつものが好適である。
ＭＷＤはＭｗ／Ｍｎの比として計算され、ここでＭｗは重量平均分子量でありＭｎは数平均分子量である。好ましい材料は１−２０、好ましくは１．５−１０のＭＷＤをもつ。ＡＳＴＭ Ｄ１２３８条件２３０℃／２．１６ｋｇで測定されるナイロン−６熱可塑性ポリマー（ａ）のメルトフローレートは、それらから製造される繊維又はフィルムの良好な加工性を達成するためには、高い吐出速度、及び引っ張り強さを測定したときの良好な機械的性質で証明されるように、望ましくは０．１−１００ｇ／１０分、より好ましくは０．２−５０ｇ／１０分、そして最も好ましくは０．３−１０ｇ／１０分である。成分（ａ）のための多くの好適なポリマーは分子量の指標として相対粘度を使用する。この測定方法を使用すると、好適なポリマーは２５−２５０、好ましくは３０−１８０、より好ましくは３５−１６０のＲＶ（相対粘度）をもつ。好ましくは熱可塑性ポリマー（ａ）は２５℃の広角Ｘ線回折で測定したとき１０％の結晶性、好ましくは少なくとも１５％の結晶性、より好ましくは２０％の結晶性をもつ。これと等しく望ましくは、熱可塑性ポリマー（ａ）は適切な結晶化度をもつ繊維又はフィルムが典型的な成形延伸及び成形配向プロセス条件を使用して製造されるような結晶化速度をもつ。結晶生成速度を増加又は減少させるための添加剤（結晶化促進剤）をもし望むなら成分（ａ）に取り込んでもよい。
【００７７】
すでに開示したように、成分（ａ）としての使用のために好ましいポリマーは、本発明の改良なしでもナイロン６はナイロン６，６に較べて繊維形成が一般的に劣るという驚くべき事実を示すナイロン６である。文献で公知なように、採用されるポリアミドは、容易に染色され且つ改善された色定着性をもつポリマーを生成するアミン末端基を不釣合いの量でもっている。そのようなポリアミド化合物はポリアミド中のアミン末端基：カルボン酸末端基の比が１より大きいという事実によって特徴付けられる。もし望むなら、アミン末端基の量は、公知の方法で、カルボン酸機能又は第一アミンと反応する他の機能をもつ化合物と反応させることによって修正することができる。
【００７８】
ここで使用する好ましいポリアミドはさらに望まれる繊維の最終用途に依存する。高度につや消しをした繊維のためには低粘度のポリアミド、例えば、２５−７５、より好ましくは３０−６０のＲＶをもつナイロン６樹脂が好ましい。紡糸の容易性を高めた（糸切れの少ない）繊維のためには高い粘度のナイロン６又はナイロン６，６、例えば１２０−２５０、より好ましくは１５０−１８０のＲＶをもつ樹脂が好ましい。
【００７９】
熱可塑性ポリマー（ｂ）について
熱可塑性ポリマー（ｂ）として使用するために適したポリマーは、本発明の目的が得られるならば、限定はしないが、アイソタクチック又はシンジオタクチックポリスチレン及びスチレンと１以上のコモノマー（ハロ−、Ｃ_１−４ アルコキシ−、Ｃ_１−４ アルキル−又はＣ_１−４ ハロアルキル−環置換されたスチレン、又は極性基−置換されたスチレンのような）とのアイソタクチック又はシンジオタクチックコポリマーを含むビニリデン芳香族モノマーのタクチックポリマー、ポリシクロヘキセンテレフタレートのような高温用ポリエステル、ポリイミド、液晶ポリマー；極性コモノマーでグラフト変性した前者の誘導体、特にスチレンと環状アルキル置換されたスチレン化合物とのアイソタクチック又はシンジオタクチックコポリマーの無水マレイン酸、フマール酸、又はマレイミドグラフト変性誘導体；又は前者の混合物から好適に選択される。
【００８０】
好ましくは熱可塑性ポリマー（ｂ）は２５℃の広角Ｘ線回折で測定したとき５％の結晶性、好ましくは少なくとも１０％の結晶性、より好ましくは１５％の結晶性をもつ。結晶生成速度を増加又は減少させるための添加剤（結晶化促進剤）をもし望むなら成分（ｂ）に取り込んでもよい。この材料は成分（ａ）に取り込まれる結晶化促進剤と同じでも異なっていてもよい。
【００８１】
より好ましくは、熱可塑性ポリマー（ｂ）は、１以上のビニリデン芳香族モノマーのステレオブロックコポリマーを含む、ビニリデン芳香族モノマーのシンジオタクチックホモポリマー又は極性官能基を含むモノマーとのグラフト共重合を含む共重合した１以上の前者のポリマー（ここでは以後“極性基変性”ポリマーと呼ぶ）である。“極性基”又は“極性官能基”はここではそのような基をもたない化合物に比較して化合物に大きな極性モーメントを与える基又は置換基として定義される。好ましい極性基としてはカルボン酸及びカルボン酸誘導体（例えばカルボン酸基の水素原子又はヒドロキシル基の置換から生ずる、酸アミド、酸無水物、酸アジド、酸エステル、酸ハライド、及び酸の塩）、スルホン酸及びスルホン酸誘導体（例えば、スルホン酸エステル、スルホン酸クロライド、スルホン酸アミド、及びスルホン酸塩）、エポキシ基、カーボネート基、アミノ基、イミド基、及びオキサゾリン基を包含する。
【００８２】
好適なビニリデン芳香族モノマーは式：Ｈ_２ Ｃ＝ＣＲ−Ａｒの化合物であり、ここでＲは水素又は１−４の炭素原子をもつアルキル基であり、そしてＡｒは６−１８の炭素原子からなる芳香族基又はアルキル−、ハロアルキル−、アルコキシ−又はハロ置換した芳香族基である。好ましい極性官能基は無水マレイン酸又はフマール酸との反応から生ずる極性残余物である。好ましいビニリデン芳香族モノマーはスチレン及びＣ_１−４ アルキル−、Ｃ_１−４ アルコキシ−、又はハロ−、環置換されたスチレン誘導体である。
【００８３】
典型的なビニリデン芳香族ポリマーとしては：ポリスチレン、ポリ（メチルスチレン）、
ポリ（エチルスチレン）、ポリ（イソプロピルスチレン）、ポリ（ｐ−ｔ−ブチルスチレン）；
ポリ（メトキシスチレン）、ポリ（ビニルナフタレン）、ポリ（ブロモスチレン）、ポリ（ジブロモスチレン）、ポリ（クロロスチレン）、ポリ（フルオロスチレン）、モノマー異性体の混合物を含むモノマー混合物を重合することによって得られるポリマーを含む前者のポリマー混合物（例えば、スチレン／ｐ−メチルスチレンコポリマー）、及び水素化された又は極性基変性されたそれらの誘導体を包含する。最も好ましいのはシンジオタクチック立体異性体構造をもつ前者のポリマー形態である。
【００８４】
熱可塑性ポリマー（ｂ）としての使用に最も好ましい熱可塑性樹脂はシンジオタクチックビニリデン芳香族ポリマー及び極性基で官能基化したそれらの誘導体である。シンジオタクチックビニリデン芳香族ポリマーを合成する重合プロセスは米国特許４，６８０，３５３号；米国特許５，０６６，７４１号；米国特許５，２０６，１９７号；米国特許５，２９４，６８５号；米国特許５，９９０，２１７号；及びその他に記載されている。シンジオタクチックビニル芳香族ポリマーはまたダウケミカル社から商標名Ｑｕｅｓｔｒａとして市販されている。熱可塑性ポリマー（ｂ）としての使用に最も好ましいポリマーはシンジオタクチックポリスチレン、０．００５−１５重量％、好ましくは０．０１−１０重量％のｐ−、ｍ−またはｏ−メチルスチレンモノマー、特にｐ−メチルスチレンを含むシンジオタクチックスチレン／ｐ−、ｍ−またはｏ−メチルスチレンコポリマー、及び０．００５−５重量％の機能性基を含む極性基で官能基化した前者の誘導体である。最も高度に好ましいポリマーはシンジオタクチックスチレン又は０．１−１０重量％のｐ−メチルスチレンと０．０１−１．５重量％の無水マレイン酸又はフマール酸を含む無水マレイン酸又はフマール酸でグラフトした又は共重合したスチレン／ｐ−メチルスチレンコポリマーである。後者のグラフトポリマーは熱可塑性ポリマー（ａ）と組み合わせてもよく、分離相溶化剤（ｃ）を添加することなしで繊維形成のための良好なポリマーモルフォロジーを達成する。
【００８５】
ゲルパーミエーションクロマトグラフィーで決定される、熱可塑性ポリマー（ｂ）の重量平均分子量、Ｍｗ、は臨界的ではないが、典型的には５，０００−５，０００，０００、より典型的には１０，０００−１，０００，０００、そして好ましくは２０，０００−５００，０００である。さらに、熱可塑性ポリマー（ｂ）の分子量分布は広い範囲で変化するが、しかし適切には１−２０、好ましくは１．５−１０である。
【００８６】
組成物中の熱可塑性ポリマー（ｂ）の量が望ましい量より少ないときは、それから得られる繊維は望ましい手触り又は柔らか味を示さない。組成物中の熱可塑性ポリマー（ｂ）の量が望ましい量より多いときは、フィラメント又は繊維は延伸又は紡糸において非常に糸切れし易くなる。ここで使用されるときは、用語“ドメイン形成”は特に成分（ａ）及び成分（ｂ）に関しては、それぞれのポリマーがお互いに部分的に相溶化し均一なブレンド物を形成することができると理解されているが、生ずる組成物中で区別できる領域又はドメインを形成することを意味する。しかし好ましくは、二つのポリマーは、せん断を与える熔融混合装置中での撹拌にも拘らず二つの成分の均一なブレンド物が生成しないようにお互いに実質上相溶化しないことである。
【００８７】
成分（ｃ）について
成分（ｃ）は、本発明で生ずるポリマードメイン間の改良された接着及び／又は減少した界面張力が望ましいところで利用される。さらに、相溶化剤の種類及び量はポリマーマトリックス中の小径粒子、よく分散した成分（ｂ）の吸蔵物の生成を助け、増加した繊維堅さと同様に改良された熔融張力と紡糸性をもつ組成物に導く。成分（ｂ）の吸蔵物の好適な小径ドメインは得られる繊維又はフィルムの改良された光学的性質と表面粗さを与える。好ましい相溶化剤は、芳香族の機能性と極性基の両方をもち、どちらかが組成物中に物理的に混合されるか又は１以上の熱可塑性成分（ａ）又は（ｂ）とグラフト又は界面重合によって反応するが、得られるブレンド物の黄色度には寄与しない、ポリマーである。
【００８８】
好適な相溶化剤としては、ビニリデン芳香族ホモポリマー及びコポリマー（ビニリデン芳香族モノマーのアタクチック、シンジオタクチック及びアイソタクチックホモポリマー又はコポリマー、同様にビニリデン芳香族モノマーとアクリロニトリル、無水マレイン酸、又はマレイミドとのコポリマーを含む）、ポリフェニレンエーテル、ポリ（ビニルエーテル）、ポリ（ビニルメタクリレート）、ポリオレフィン、ポリ（ジエン）、及び成分（ｃ）上で成分（ｂ）との混和性、部分溶解性、又は選択的親和性をもついくつかのポリマーを包含する。また、これらの材料にはブロックコポリマー（２以上の異なった繰り返し単位セグメントから構成されているポリマー）も含まれる。好適なブロックコポリマーは成分（ｃ）上で成分（ｂ）との混和性、部分溶解性、又は選択的親和性をもつセグメントを含んでいる。追加のセグメントは成分（ｃ）との混和性、溶解性、又は親和性の基準に適合してもしなくてもよい。このような材料の例は、他の繰り返し単位（例えば水素化されたポリ（スチレン−ブロック−エチレン−ブタジエンーブロック−スチレン）グラフト−無水マレイン酸）とビニリデン芳香族ポリマーとのブロックコポリマー及び以下のようないずれかのコポリマー：ビニリデン芳香族モノマーのアタクチック、シンジオタクチック及びアイソタクチックホモポリマー又はコポリマー、同様にビニリデン芳香族モノマーとアクリロニトリル、無水マレイン酸、又はマレイミドとのコポリマーを含む）、ポリフェニレンエーテル、ポリ（ビニルエーテル）、ポリ（ビニルメタクリレート）、ポリオレフィン、ポリ（ジエン）のようなグラフトした又はその他の機能性ポリマー誘導体である。
【００８９】
相溶化剤（ｃ）のポリマー鎖構造は好ましくは第一の熱可塑性ポリマー（ａ）の官能基と反応できる反応性極性基で修飾される。反応性極性基を含む好ましい反応物は、前に定義したように、望ましい極性基官能性に沿ってエチレン性不飽和のような不飽和結合を含む化合物である。好適な反応性極性基の例としては、カルボン酸、ジカルボン酸及びジカルボン酸誘導体（例えばカルボキシル基の水素原子又はヒドロキル基の置換から生ずる酸アミド、酸無水物、酸アジド、酸ハライド、酸の塩）、スルホン酸及びスルホン酸誘導体（例えば、スルホン酸エステル、スルホン酸クロライド、スルホン酸アミド、及びスルホン酸塩）、エポキシ基、カーボネート基、アミノ基、イミド基、及びオキサゾリン基を包含する。
【００９０】
好ましい反応性極性基含有不飽和反応物は不飽和カルボン酸及びジカルボン酸、不飽和カルボン酸及びジカルボン酸誘導体、不飽和エポキシ化合物、不飽和アルコール、不飽和アミン、及び不飽和イソシアネートである。反応性極性基含有不飽和反応物の特有の例としては、無水マレイン酸、フマール酸、マレイミド、マレイン酸ヒドラジド、及び無水マレイン酸とジアミンの反応性生物、無水１−メチルマレイン酸、無水ジクロロマレイン酸、
マレイン酸アミド、イタコン酸、無水イタコン酸、大豆油、桐油、ひまし油、亜麻に油、麻種油、綿種油、ゴマ油、菜種油、落花生油、つばき油、オリーブ油、ココナッツ油、及びサラダ油のような天然油脂又は天然油の酸；アクリル酸、ブテン酸、クロトン酸、ビニル酢酸、メタクリル酸、ペンテン酸、アンゲリカ酸、２−ペンテン酸、３−ペンテン酸、α−エチルアクリル酸、β−メチルクロトン酸、４−ペンテン酸、２−ヘキセン酸、２−メチル−２−ペンテン酸、３−メチル−２−ペンテン酸、α−エチルクロトン酸、２，２−ジメチル−３−ブテン酸、２−ヘプテン酸、２−オクテン酸、４−デセン酸、９−ウンデセン酸、１０−ウンデセン酸、４−ドデセン酸、５−ドデセン酸、４−テトラデセン酸、９−テトラデセン酸、９−ヘキサデセン酸、２−オクタデセン酸、９−オクタデセン酸、エイコセン酸、ドコセン酸、エルカ酸、テトラコセン酸、２，４−ペンタジエン酸、２，４−ヘキサジエン酸、ジアリル酢酸、ゼラニウム酸、２，４−デカジジエン酸、
２，４−ドデカジジエン酸、９，１２−ヘキサデカジジエン酸、９，１２−オクタデカジジエン酸、ヘキサデカトリエン酸、リノール酸、リノレン酸、オクタデカトリエン酸、エイコサジエン酸、エイコサトリエン酸、エイコサテトラエン酸、リシノール酸、エレオステアリン酸、オレイン酸、エイコサペンタエン酸、ドコサジエン酸、ドコサトリエン酸、
ドコサテトラエン酸、ドコサペンタエン酸、テトラコセン酸、ヘキサコセン酸、ヘキサコジエン酸、オクタコノン酸のような不飽和カルボン酸、及びこれら不飽和カルボン酸のエステル、酸アミド及び無水物；アリルアルコール、メチルビニルカルビノール、アリルカルビノール、メチルプロペニルカルビノール、４−ペンテン−１−オール、１０−ウンデカン−１−オール、プロパルギルアルコール、１，４−ペンタジエン−３−オール、１，４−ヘキサジエン−３−オール、３，５−ヘキサジエン−２−オール、２，４−ヘキサジエン−１−オール、のような不飽和アルコール、一般式：Ｃ_ｎＨ_２ｎ−５ＯＨ、Ｃ_ｎＨ_２ｎ−７ＯＨ、Ｃ_ｎＨ_２ｎ−９ＯＨ（ｎは正の整数）、３−ブテン−１，２−ジオール、２，５−ジメチル−３−ヘキセン−２，５−ジオール、１，５−ヘキサジエン−，４−ジオール、及び２，６−オクタジエン−４，５−ジオール、及びこれらの不飽和アルコールのＯＨ基をＮＨ_２ で置換して得られる不飽和アミンが包含される。
【００９１】
相溶化剤（ｃ）の酸性極性基は亜鉛、マグネシウム、マンガン、リチウム、又は他の金属カウンターイオン又は金属カウンターイオンの組み合わせによって完全に又は部分的に中和されていてもよい。中和した酸モノマー、例えば、相溶化剤（ｃ）を生成するためのグラフト重合又は機能化において、アクリル酸亜鉛を使用することもまた可能である。
【００９２】
エポキシ基をもつビニル化合物の例はグリシジルメタクリレート、グリシジルアクリレート、ビニルグリシジルエーテル、ヒドロキシアルキル（メタ）アクリレートのグリシジルエーテル、ポリアルキレングリコール（メタ）アクリレートのグリシジルエーテル、イタコン酸グリシジルであり、そのなかでもグリシジルメタクリレートが特に好ましい。相溶化剤（ｃ）は２以上の不飽和基と２以上の極性基（同じ又は異なった）、及び極性基又は多重極性基をもつ２以上の化合物を含むことができる。
【００９３】
とりわけ好適な相溶化剤（ｃ）は極性官能性をもつポリアリーレンエーテルと極性官能性をもつポリ（ビニリデン芳香族）ホモポリマー及びコポリマーである。極性官能性をもちそしてポリアリーレンエーテルとポリ（ビニリデン芳香族）ホモポリマー及びコポリマーのセグメントを含むブロックコポリマーもまた含まれる。そのような相溶化剤は従来からのポリマーを前述の極性基含有変性剤の一つで変性することによって得られる。変性方法は変性生成物が本発明の目的に従って使用することができる限り特に限定はしない。好適な塩基樹脂及び極性基含有反応物は溶融状態で、所望によりベンゾイルパーオキサイド、ジ−ｔ−ブチルパーオキサイド、ジクミルパーオキサイド、ｔ−ブチルパーオキシベンゾエート、アゾビスイソブチルロニトリル、アゾビスイソバレロニトリル、又は２，３−ジフェニル−２，３−ジメチルメタンのようなフリーラジカル発生剤又は他の開始剤の存在下で押し出し機又は同様な混合装置中で組み合わされる。ポリフェニレンエーテルは一般的には、２又は３位で置換されていることが好ましい１以上のフェノールの酸化カップリングによって製造することができる。好ましくは、銅−アミン錯体、特に一級、二級、三級アミンから導かれる銅−アミン錯体のような触媒が使用される。適切なポリフェニレンエーテルの例としては、ポリ（２，３−ジメチル−６−エチル−１，４−フェニレンエーテル）、ポリ（２−メチル−６−クロロメチル−１，４−フェニレンエーテル）、ポリ（２−メチル−６−ヒドロキシエチル−１，４−フェニレンエーテル）、ポリ（２−メチル−６−ｎ−ブチル−１，４−フェニレンエーテル）、ポリ（２−エチル−６−イソプロピル−１，４−フェニレンエーテル）、ポリ（２−エチル−６−ｎ−プロピル−１，４−フェニレンエーテル）、ポリ（２，３，６−トリメチル−１，４−フェニレンエーテル）、ポリ（２−（４’−メチルフェニル−１，４−フェニレンエーテル）、ポリ（２−ブロモ−６−フェニル−１，４−フェニレンエーテル）、ポリ（２−メチル−６−フェニル−１，４−フェニレンエーテル）、ポリ（２−フェニル−１，４−フェニレンエーテル）、ポリ（２−クロロ−１，４−フェニレンエーテル）、ポリ（２−メチル−１，４−フェニレンエーテル）、ポリ（２−クロロ−６−エチル−１，４−フェニレンエーテル）、ポリ（２−クロロ−６−ブロモ−１，４−フェニレンエーテル）、ポリ（２、６−ジ−ｎ−プロピル−１，４−フェニレンエーテル）、ポリ（２−メチル−６−イソプロピル−１，４−フェニレンエーテル）、ポリ（２−クロロ−６−メチル−１，４−フェニレンエーテル）、ポリ（２−メチル−６−エチル−１，４−フェニレンエーテル）、ポリ（２、６−ジ−ブロモ−１，４−フェニレンエーテル）、
ポリ（２、６−ジ−クロロ−１，４−フェニレンエーテル）、ポリ（２、６−ジエチル−１，４−フェニレンエーテル）、及びポリ（２、６−ジメチル−１，４−フェニレンエーテル）が包含される。ポリフェニレンエーテル製造のための好適な方法は米国特許３，３０６，８７４号、米国特許３，３０６，８７５号、米国特許３，２５７，３５７号、米国特許３，２５７，３５８号、及びその他に開示されている。ポリマーはまた容易に市販品から利用できる。
【００９４】
典型的には、成分（ｃ）の極性官能基の量は成分（ｃ）の重量基準で０．０１−１０重量％である。一般的には、もし０．０１％より少ない極性官能基しか存在しなければ、相溶化剤は希望の通り有効にはならない。採用される成分（ｃ）の量は、もし存在するなら、組成物重量基準で少なくとも０．１、より好ましくは少なくとも０．２重量％；典型的には５以下、好ましくは４．５以下、より好ましくは４．２以下、そして最も好ましくは４．０重量％以下である。
【００９５】
成分（ｃ）中の官能基の量は変化し、相溶化剤化合物中のそのような基の効率は変化し、
成分（ｂ）はまた成分（ａ）との相溶化を助ける官能性を含み、樹脂ブレンド物中にポリアミドのアミン末端基を中和し、又は生ずるポリマーの性質に影響を与える追加の成分が存在するので、希望する成分（ｂ）の効果的な利点を得るためには、成分（ｃ）の量が成分（ａ）と成分（ｂ）結合重量基準で０−５％の範囲で変化しそして成分（ｃ）（もし存在すれば）中の反応性官能基の合計量が、成分（ｂ）と成分（ｃ）との合計量基準で、０．００１−０．２５モル％、好ましくは０．０１−０．２４モル％であることが望ましい。
【００９６】
得られた繊維物品で測定すると、前述の範囲は以下のように変化する。
【００９７】
成分（ｃ）の量は成分（ａ）と成分（ｂ）結合重量基準で０−２４％の範囲で変化しそして成分（ｃ）（もし存在すれば）中の反応性官能基の合計量が、成分（ｂ）と成分（ｃ）との合計量基準で、０．００１−０．８モル％、好ましくは０．０１−０．５モル％の範囲であるべきである。
【００９８】
以下の計算において、官能化されると、成分（ｂ）は相溶化剤の全て（もし成分（ｃ）が調合中に存在しないなら）又は部分（もし調合が成分（ｃ）と成分（ｂ）の両方を含むなら）として見做される。前述の測定を行うために以下の式が使用される：
１．）ブレンド物中の官能性成分の重量％：
ｗ_（ｃ） ＝１００・ｍ_（ｃ） ／（ｍ_（ｂ）＋ｍ_（ａ）＋ｍ_（ｃ））
ここでｍ_（ｃ）＝機能性成分（成分（ｂ）もし官能化されているなら＋成分（ｃ））の質量、ｍ_（ｂ）＝成分（ｂ）の質量、ｍ_（ａ）＝成分（ａ）の質量である。
２．）ブレンド物中の官能性成分のモル％：
ｘ_（ｃ）＝（１００・ｍ_（ｃ） ／ＭＷ_（ｃ） ）／（ｍ_（ｂ）／ＭＷ_（ｂ） ＋ｍ_（ａ）／ＭＷ_（ａ）
＋ｍ_（ｃ））／ＭＷ_（ｃ） ）
ここでＭＷ_（ｃ） ＝成分（ｃ）繰り返し単位の平均分子量、ＭＷ_（ｂ） ＝成分（ｂ）繰り返し単位の分子量、ＭＷ_（ａ） ＝成分（ａ）繰り返し単位の分子量である。
３．）成分（ｂ）＋成分（ｃ）中の極性基の重量％：
ｗ_{Ｐｏｌａｒ，（ｂ）}＝（ｍ_（ｃ） ）（ｆ_{Ｐｏｌａｒ} ）／（ｍ_（ｂ）＋ｍ_（ｃ））
ここでｆ_{Ｐｏｌａｒ} ＝極性基又は官能基残余物（例えば、スチレン無水マレイン酸コポリマー中の無水マレイン酸残余物）である成分（ｃ）の重量％である。
４．）成分（ｂ）＋成分（ｃ）中の極性基のモル％：
ｘ_{Ｐｏｌａｒ} ＝［（ｍ_（ｃ） ）（ｆ_{Ｐｏｌａｒ} ）／ＭＷ_{Ｐｏｌａｒ} ］／［ｍ_（ｂ）／ＭＷ_（ｂ） ＋ｍ_（ｃ）／ＭＷ_（ｃ） ］
ここでＭＷ_{Ｐｏｌａｒ} ＝極性単位の分子量である。
５．）ブレンド物中の極性基の重量％：
ｗ_{Ｐｏｌａｒ，Ｂｌｅｎｄ}＝（ｍ_（ｃ） ）（ｆ_{Ｐｏｌａｒ} ）／［（ｍ_（ｂ）＋ｍ_（ｃ） ＋ｍ_（ａ） ］
６．）ブレンド物中の極性基のモル％：
ｘ_{Ｐｏｌａｒ、Ｂｌｅｎｄ} ＝［（ｍ_（ｃ） ）（ｆ_{Ｐｏｌａｒ} ）／ＭＷ_{Ｐｏｌａｒ} ］／［ｍ_（ｂ）／ＭＷ_（ｂ） ＋ｍ_（ｃ）／ＭＷ_（ｃ）＋ｍ_（ａ）／ＭＷ_（ａ） ］
採用される相溶化剤の前述の合計量の範囲内で、相溶化剤の理想的なレベルは得られる繊維又はフィルムの所望の性質にバランスするように決定される。使用される相溶化剤の量は究極的に、ポリアミドの残余のアミン末端基を含むブレンド物を減少させ、それが順番にそれから作られる繊維の繊維用途のための染色受け入れ性に影響するので、繊維の機械的性質を改良するために十分な量の、しかしアミン末端基の減少によって繊維の染色受け入れ性に負の影響を及ぼす量より少ない量の極性基を含む相溶化剤を採用することが望ましい。アミン末端基の初期モル量（開環反応によって生ずるポリアミドのための）は、順番にポリマーの分子量に依存する。利用できるアミン末端基を評価する式は公知である。ナイロン６及び開環反応（そして末端基濃度に影響を与えない方法で変性されていない）によって生成する他のポリアミドの場合、その式は：
Ｎ＝１・１０^６／Ｍ _ｎ ［＝］ミリ当量／ｇ
ここでＭ _ｎ ＝ポリアミドの数平均分子量である。
【００９９】
代替する方法としては、反応したアミン末端基の実際の量（モル）はそのようなポリマーに対して、相溶化剤の極性官能基と完全に反応することを仮定して、次式を使用することによって計算できる：
反応量＝ｍ_Ｃｏｍｐ ・ｆ_{Ｐｏｌａｒ} ／［１００・ＭＷ_{Ｐｏｌａｒ} ］
ここでｍ_Ｃｏｍｐ ＝相溶化剤の質量、ｆ_{Ｐｏｌａｒ} ＝相溶化剤中の極性官能基の重量％、そしてＭＷ_{Ｐｏｌａｒ} ＝極性官能基の分子量である。成分（ｂ）と成分（ｃ）の両方が極性官能基を含む場合は、調合によって設定される２成分の比を組み合わせて計算された官能基の平均重量％と平均分子量が上の式で使用される。
【０１００】
ポリマーブレンド物中に残っているアミン末端基の量は酸滴定又は他の適切な技術のような分析技術を使用して直接測定されるような極性官能基を含む試薬を添加する事によってまた減少する。特に、ナイロン６，６及び縮合ポリアミドの場合には、前述の方法による計算に従わないため、末端基含量は好ましくは直接測定される。
【０１０１】
ブレンド物中のアミン末端基を計算又は測定するために使用される方法に拘わらず、相溶化剤中の利用できるアミン末端基、Ｎ、：極性官能基の比は好ましくは７０：３０から９９：１、より好ましくは８０：２０から９６：４、そして最も好ましくは８５：１５から９３：７である。代わりに、ポリマー組成物の最終アミン末端基含量は成分（ｃ）又はもし成分（ｂ）が極性官能基を含むなら成分（ｂ）と成分（ｃ）の両方の極性基との反応によって５から２０％に減少する。成分（ｃ）としての好ましいポリマーはスチレン／無水マレイン酸コポリマー及び無水マレイン酸でグラフトしたスチレンとｐ−メチルスチレンとのシンジオタクチックコポリマーである。
【０１０２】
所望による成分（ｄ）について
本発明の組成物には、所望の性質又は最終製品が得られる範囲内で、追加の添加剤を存在させてもよい。追加の添加剤の種類と量は、もし存在するなら、公知の従来技術に従って選択される。典型的な追加の添加剤としては、つや消し剤、エラストマー、難燃剤、抗カビ剤、熱安定剤、光安定剤、抗酸化剤、顔料、染料、潤滑剤、ブロー剤、光学つや剤、及び静電気防止剤が包含される。そのような添加剤は成分（ａ）又は成分（ｂ）のどちらか又は両方に入れるか又は最初に成分（ａ）と成分（ｂ）のブレンド物を調製した後で生じた組成物中に入れてもよい。成分（ａ）に添加すると有害な添加物は成分（ｂ）のみに添加する事によって本発明に採用されてもよい。
【０１０３】
好適なつや消し剤は無機酸化物、チタネート、カーボネート及びシリケートであり、好ましくは二酸化チタンである。好ましいつや消し剤は微粒子又は微粉の形態であり、高度に好ましくは体積平均粒子径が１００μｍ以下、より好ましくは５０μｍ以下、最も好ましくは１０μｍ以下である。
【０１０４】
好適なエラストマーは組成物の耐衝撃性、硬さ又は伸びを増加させるものである。採用されるときは、エラストマーは合計組成物重量基準で典型的には０．５−５０、好ましくは０．７−３０そしてより好ましくは１．０−２０重量％の量で与えられる。組成物中に含まれてもよいエラストマーの例としては：天然ゴム、ポリブタジエン、ポリイソプレン、ポリイソブチレン、ネオプレン、ポリサルファイドゴム、ウレタンゴム、シリコーンゴム、エピクロルヒドリンゴム、スチレン−ブタジエンブロックコポリマー（ＳＢＲ）、水素化スチレン−ブタジエンブロックコポリマー（ＳＥＢ）、スチレン−ブタジエン−スチレンブロックコポリマー（ＳＢＳ）、水素化スチレン−ブタジエン−スチレンブロックコポリマー（ＳＥＢＳ）、スチレン−イソプレンブロックコポリマー（ＳＩＲ）、水素化スチレン−イソプレンブロックコポリマー（ＳＥＰ）、スチレン−イソプレン−スチレン−ブロックコポリマー（ＳＩＳ）、水素化スチレン−イソプレン−スチレン−ブロックコポリマー（ＳＥＰＳ）、
スチレン−ブタジエンランダムコポリマー、水素化スチレン−ブタジエンランダムコポリマー、スチレン−エチレン−プロピレンランダムコポリマー、スチレン−エチレン−ブチレンランダムコポリマー、エチレン−プロピレンゴム（ＥＰＲ）、エチレン−プロピレン−ジエン−ゴム（ＥＰＤＭ）、ブタジエン−アクリロニトリル−スチレンコアシェルゴム（ＡＢＳ）、メチルメタクリレート−ブタジエン−スチレンコアシェルゴム（ＭＢＳ）、メチルメタクリレート−ブチルアクリレート−スチレンコアシェルゴム（ＭＡＳ）、オクチルアクリレート−ブタジエン−スチレンコアシェルゴム（ＭＡＢＳ）、アルキルアクリレート−ブタジエン−アクリロニトリル−スチレンコアシェルゴム（ＡＡＢＳ）、ブタジエン−スチレンコアシェルゴム（ＳＢＲ）、及びメチルメタクリレート−ブチルアクリレート−シロキサンのようなシロキサンを含むコアシェルゴム、及びこれらのゴムの変性によって得られるゴムが包含される。
【０１０５】
着火紡糸添加剤とも呼ばれる難燃剤は実際の燃焼条件下で組成物の性能を反映するために意図されたものではない。この目的のための好適な添加剤としては、限定はしないが、臭素化ポリスチレン（臭素化シンジオタクチックポリスチレンを含む）、ヘキサブロモシクロドデカン、デカブロモジフェニルオキサイド、エチレン−ビス（テトラブロモフタールイミド）、エチレン−ビス（ジブロモボランジカルボキシイミド）、ペンタブロモジフェニルオキサイド、オクタタブロモジフェニルオキサイド、デカブロモジフェノキシエタン、ポリ−ジブロモフェニレンオキサイド、ハロゲン化リンエステル、無水テトラブロモフタール酸、ビス（無水トリブロモフタール酸）、テトラブロモビスフェノール−Ａビス（２−ヒドロキシエーテル）、テトラブロモビスフェノール−Ａビス（２、３−ジブロモプロピルエーテル）、ジブロモ−ネオペンチルグリコール、テトラデカブロモジフェノキシベンゼン、酸化アルミニウム３水和物、酸化アンチモン、アンチモン酸ナトリウム、ホウ酸亜鉛、及びテトラブロモビスフェノール−Ａのジアクリレートエステルが包含される。
【０１０６】
好適な熱及び光安定剤としては、限定はしないが、ステアリン酸カルシウム、フェノール及びヒンダードフェノール、酸化亜鉛、アリールエステル、ヒドロキシベンゾフェノン、及びヒドロキシベンゾトリアゾールが包含される。
【０１０７】
好適な抗酸化剤としてはリンベースの抗酸化剤、フェノール系抗酸化剤及び硫黄系抗酸化剤が包含される。リンベースの抗酸化剤の例はトリス（２，４−ジ−ｔ−ブチルフェニル）ホスファイト及びトリス（モノ／ジ−ノニルフェニル）ホスファイト、ジステアリルペンタエリスリトールジホスファイト；ジオクチルペンタエリスリトールジホスファイト；ジフェニルペンタエリスリトールジホスファイト；ビス（２，４−ジ−ｔ−ブチルフェニル）ペンタエリスリトールジホスファイト；ビス（２，６−ジ−ｔ−ブチル−４−メチルフェニル）ペンタエリスリトールジホスファイト、ジシクロヘキシペンタエリスリトールジホスファイト；トリス（２，４−ジ−ｔ−ブチルフェニル）ホスファイト；テトラキス（２，４−ジ−ｔ−ブチルフェニル）−４，４−ビフェニレンホスファイトのようなモノホスファイト及びジホスフェートが包含される。
【０１０８】
好適なフェノール系抗酸化剤としては、２，２’−メチレンビス（６−ｔ−ブチル−４−メチルフェノール）；１，１−ビス（５−ｔ−ブチル−４−ヒドロキシ−２−メチルフェニル）ブタン；２，２’−メチレンビス（４−メチル−６−シクロヘキシルフェノール）；
４，４’−チオビス（６−ｔ−ブチル−３−メチルフェノール）；２，２−ビス（５−ｔ−ブチル−４−ヒドロキシ−２−メチルフェノール）−４−ドデシルメルカプト−ブタン、２，６−ジ−ｔ−４−メチルフェノール；２，２’−メチレンビス（６−ｔ−ブチル−４−エチルフェノール）；２，２’−メチレンビス−４−メチル−６−（α−メチルシクロヘキシル）フェノール；２，２’−メチレンビス（４−メチル−６−ノニルフェノール）；１，１−ビス（３，５−ジメチル−２−ヒドロキシフェニル）−３−（ｎ−ドデシルチオ）−ブタン；１，３，５−トリス（３，５−ジ−ｔ−ブチル−４−ヒドロキシベンジル）−２，４，６−トリメチルベンゼン；２，２−ビス（３，５−ジ−ｔ−ブチル−４−ヒドロキシベンジル）ジオクタデシルマロネートエステル；ｎ−オクタデシル−３−（４−ヒドロキシ−３，５−ジ−ｔ−ブチルフェニル）プロピオネート、テトラキスメチレン（３，５−ジ−ｔ−ブチル−４−ヒドロキシヒドロシンナメート）メタン、３，９−ビス−１，１−ジメチル−２−（β−（３−ｔ−ブチル−４−ヒドロキシ−５−メチルフェニル）プロピオニルオキシ）エチル−２，４，８，１０−テトラオキサスピロ−５，５−ウンデカン、トリス−（３，５−ジ−ｔ−ブチル−４−ヒドロキシベンジル）イソシアヌレート、２，６−ジフェニル−４−メトキシフェノール、及びトリス−（４−ｔ−ブチル−２，６−ジメチル−３−ヒドロキシベンジル）イソシヌレートが包含される。
【０１０９】
好適な硫黄ベースの抗酸化剤としては：ジラウリル−３，３’−チオジプロピオネート；ジミリスチル−３，３’− チオジプロピオネート；ジステアリル−３，−３’−チオジプロピオネート；ペンタエリスリトール−テトラキス−（β−ラウリル−チオジプロピオネート）、ビス−２−メチル−４−（３−ｎ−アルキルチオプロピオニルオキシ）−５−ｔ−ブチルフェニルサルファイド、及び２−メルカプトベンズイミダゾールが包含される。
【０１１０】
有用な顔料は文献でよく知られておりそして、限定はしないが：カドミウム水銀オレンジ、カドミウムサルファイドイエロー、カドミウムスルホセレナイド、二酸化チタン、チタンイエロー、チタングリーン、チタンブルー、アルミン酸コバルト、マンガンブルー、マンガンバイオレット、ウルトラマリーンレッド、ウルトラマリーンブルー、及びウルトラマリーンバイオレットのような無機顔料；そしてパーマネントレッド２Ｂ、ペリレンレッド、キナクリドンレッド、ジアゾオレンジ、ジアゾイエロー、イソインドリノン、ハンザイエロー、フタロシアニングリーン、フタロシアニンブルー、キナクリドンバイオレット、及びドキサジンバイオレットのような有機顔料を含む。
【０１１１】
好適な抗カビ剤はポリマーにバクテリア、白カビ又はカビに対する抵抗を与える抗バクテリア性又はその他の薬剤である。好適な静電気防止剤は繊維に帯電防止性を与えることで知られている導電性又は両性イオンの物質を含む。
【０１１２】
一つの操作方法においては、好適なベースレジン中の顔料又は他の添加剤の濃縮物は１以上の組成物（ａ）及び（ｂ）と一緒に押し出し機に加えられる。代替方法としては、顔料又は他の添加剤はそのようなレジン中に予め組成物化されていてもよい。濃縮物の使用は添加剤の量の調節をしやすくしそして最終組成物中に添加剤を含ませる能力を改善する。顔料又は他の添加剤が主として組成物の一成分にのみ加えられてもよいことは熟練した当業者にとっては自明なことである。この態様の利点は、一成分に有害である顔料又は他の添加剤は主としてもう一方の成分にのみ含ませることができる点である。例えば、或る有機顔料はポリマーを架橋させるかもしれないし、それによってその熔融粘度を上げそして繊維を弱くする球状物を生成し、結果として紡糸工程での糸切れを引き起こすかもしれない。逆に、或る無機顔料はポリマーの解重合の触媒となり、染色敏感性に影響を与える機能性末端基の数を増加させそして粘度を減少させるかもしれない。そのような顔料を主として一相に含ませることによって、繊維形成プロセスの少なくとも最初の段階においては、前述の問題点のいくつか又は全てを減少させるか取り除くことができる。好ましい態様においては、添加剤を少量成分、特に物質が成分（ａ）より成分（ｂ）とより混じりあいやすい所に選択的に含ませることによって改良された性能を達成できる。さらに、添加剤を分散相にのみ濃縮させることによって、或る条件下では、少量の添加剤を使用して等価の性能を得ることができる。例えば、抗カビ剤を採用するときに、繊維表面の成分（ｂ）の吸蔵物の突起により、それは繊維又はフィルムの表面に多く露出しそして環境に触れやすくなるという事実によって、可能となる。
【０１１３】
高度に好ましい態様においては、成分（ｂ）は調合において望まれるいずれかの添加剤、特に相溶化剤（ｃ）、つや消し剤、着色剤、及び／又は他の添加剤を含むアロイ又は濃縮物として供給される。成分（ａ）の少量部分を含む濃縮物はそれから繊維又はフィルムの形成プロセスで使用される装置又は繊維やフィルム形成に適した完全に組成物化したポリマー混合物をダイ又は紡糸口金に供給するのに十分な分離押し出し機又は他の熔融混合装置中の成分（ａ）に熔融ブレンドされる。そのような条件下で十分な混合と十分な成分（ｂ）の粒子径を得るために、従来の繊維形成用押し出し機に組み込まれている好適な混合装置の例は、米国特許４，３３４，７８３号及び米国特許５，４５１，１０６号に開示されているような拡大流れ混合機である。
【０１１４】
特に好ましい態様においては、熔融ポリマーブレンド物は、押し出し機又はここで述べた希望する分散相粒子径を達成するために熔融ポリマーの適切な混合が得られるような、分散混合、拡大流れ混合、又はそれらの組み合わせを利用する分離して追加された混合装置内のいずれかのゾーンである撹拌ユニットを通過する。
【０１１５】
ポリマーのコンパウンド化においては、分配混合はスクリューフィーダーとダイの間でいわゆる“モーションレスミキサー”又は“スタティックミキサー”を使用することによって効果的になされる。たいていの場合、それらは温度調節手段の装備された管状ハウジング中に置かれたＮ個の右手回り及び左手回りの交互螺旋要素から構成されている。混合エネルギーは混合で発生する圧力低下によって与えられる。流れの飛散及び再結合は予測できる数の溝、２^Ｎ を生じる。分配混合における基本理論は流れの分配と再結合である。流れの分配はせん断タイプであるため、分配力は通常弱く、そして混合される液体が同じ粘度であるときに装置は最も有効に機能する。２液体の場合、この関係はλ＝η_ｄ／η_ｍ≒１で表される：
ここでη_ｄ 及びη_ｍ はそれぞれ分散相とマトリックスのせん断粘度である。これに対し、拡張流れ混合機中では、混合作用は粘度比の依存性が弱い。異なった粘度のニュートニアン液体又は非−ニュートニアン液体のどちらがせん断流れよりも拡張流れ中でより有効であるかは既に決定されてきた。
【０１１６】
拡張流れは流体が貯槽からキャピラリーに収束するときに起こる。一般的には、拡張流れは横長の楕円に変形させ、流れ分解の停止においては横長の楕円の小径の２倍の径の連続したミクロ液滴に変形させる傾向がある。多相系のマイナー相を制限された小径で収束又は分散した連続相をもつ系内で微小液滴に分散させることによって、良好な混合レベルが得られる。好適な拡張流れ混合機は流体導管に沿って置かれた連続した板からなる。これらの板で、流体混合物は収束と分散の連続を通って流される。連続的に増加する連続した収束及び分散強度を生じさせるために、これらの制限径が一定又は連続的に減少するように保たれるような設計が採用される。さらに、流体混合物が強い拡張流れ場に曝され、それぞれ半静止ゾーンが続き、押し出し機の通常流れの観点からそのような混合機の全体の流れ方向が軸方向より半径方向であり、そのような混合機の各開口部が穴よりはスリット形状であり、好ましくはその少なくともいくつかは異なった幅に調節できるようなスリットであるような領域を組み込む設計が強く望まれる。
【０１１７】
フィラメント、繊維及びヤーンの形成について
本発明の組成物は種々の成分及び添加物を、２以上の成分、そして好ましくは全ての成分を押し出し機又は他の熔融混合装置にブレンド物を供給する前にドライブレンドすることにより、又は希望のモルフォロジーをもつ組成物を調製するために実質上溶融状態にある間に十分な撹拌がなされる限り、どんな順序ででも、個々の成分を直接そのような押し出し機又は装置に供給するなどの種々の方法で結合させることによって形成される。組成物は、調製後にストランドやペレットに成形されるが、好ましい態様においては、組成物は押し出し機中でフィルムや繊維を製造するために使用されるダイ又は紡糸口金の操作により成形される。高度に望ましくは、成分（ａ）は最初に押し出し機に加えられ熔融可塑化される。その後で、押し出し機の１以上の追加ゾーンにおいて、好ましくは成分（ａ）の熔融物をその結晶融点以上に、所望により成分（ｂ）の結晶融点以上に加熱した後で、成分（ｂ）は組成物の他の構成成分と同時か、それらの添加の前に又はそれに引き続いて加えられる。熔融可塑化組成物はそれから、所望により成分（ａ）と（ｂ）の結晶融点の間の温度に冷却した後で、ダイ又は紡糸口金を通り、そして１以上の単位操作で繊維に成形される。組成物のコンパウンド化及びペレット化バージョンの前に再加熱及び再押し出しをしないことにより、ポリマー劣化は少なく、そして操作コストも減少する。
【０１１８】
組成物は好ましくは組成物が容易に流れることができるがしかし繊維又はフィルムの破壊を避けるのに十分な熔融張力を維持する温度でダイ又は紡糸口金を通り押し出し機から押し出される。好ましくは、ポリマー熔融物の温度は少なくとも成分（ａ）及び（ｂ）の分解温度、Ｔｄ、以下の範囲で維持される。Ｔｄは真空化で、ポリマーの重量減少速度が１％／分となるときの温度として定義される。本発明の押し出し及び紡糸のための好ましい温度は１７０−３４０℃、より好ましくは２００−３２０℃、そして最も好ましくは２５０−３００℃の範囲内である。押し出し機の温度は得られるフィラメント、フィルム又は繊維の希望する性質及び他の要因の中でもとりわけ希望する処理速度に基づいて選択される。
【０１１９】
紡糸口金はフィラメントに、例えば、三角形、多突起、五角形、等々を含む、業界で通常使用される希望の断面形状を与えるために設計される。フィラメントは１以上の軸方向空隙をもっている。さらに、フィラメントは単成分であるか多成分であり、即ち、フィラメントは１以上の長さ方向に同じ長さで接合したストランドからなる。多成分繊維の例としては、芯−鞘、並列、又は同じストランド配列をもつ繊維を含む。本発明の組成物はフィラメント、繊維、又はヤーンの希望する性質に応じてそのような多成分フィラメント又は全てのそのような成分の一成分をつくるために使用される。そのようなプロセスでは、多重供給ブロックダイが公知の手順で使用され、その例は米国特許６．０２４，５５６号、６，１６２，３８２号、及びその他に開示されている。
【０１２０】
カーペット用に特に適した繊維の製造においては、紡糸過程で、多数のフィラメントを形成する複数のオリフィスをもつ紡糸口金板が通常採用される。押し出しフィラメントが紡糸口金板から出るときに、フィラメントは十字流ガス、典型的には空気で急冷される。フィラメントはそれから延伸され、所望によりテクチャーライズ及び／又はけん縮され、所望により再加熱され、そして最終的に冷却され、ヤーンとして集積されそして巻き取りスプールに巻き取られる。けん縮はヤーンに大きな嵩を与えそして、これにより、カーペットに大きな嵩を与える。けん縮プロセスは繊維に１以上の曲げと変形を、好ましくは交互方向に、生じさせる。一般的には、けん縮繊維はそれから乾燥雰囲気又はスチーム存在下で熱に曝されポリマー成分の結晶性とけん縮“歪”を増加させる。
【０１２１】
本発明のさらなる例としては、特に成分（ａ）がナイロンであるときは、押し出し工程は：（ｉ）組成物を究極の温度、好ましくは２６０℃−３３０℃、より好ましくは２８５℃−２９５℃に上げるために、加熱、混合及び輸送ゾーン、又はそれらの組み合わせによって特徴付けられる押し出し機を通して組成物を輸送し；（ｉｉ）組成物を容量調節熔融ポンプ経由で希望のフィラメント形状に作られた多数の穴からなる紡糸口金群に供給し、そこでは紡糸口金は多数の押し出し繊維を製造するために調節されており；そして（ｉｉｉ）
押し出し物を、好ましくは１０℃−２０℃で操作される急冷ゾーンを通すことによって冷却する、諸工程からなる。
【０１２２】
押し出し後に、フィラメントは１回以上、好ましくは２回、延伸される。テクチャーライズ、けん縮、熱処理、染色、バルキング、絡まりあい化、コーティング、巻き取り、切断及びカーディングのような後成形処理が同様になされる。フィラメントはまたバルクの連続フィラメント、ステープル繊維、前者の組み合わせ、カーディングした及びカーディングしないヤーン又はストランド、及び多フィラメントヤーン、撚りのあるなしを含む既に公知の形態に処理されてもよい。本発明の繊維の粗い表面はより高い繊維−繊維内部摩擦を与えステープル繊維をヤーンに加工するのに有利である。
【０１２３】
既に述べたように、本発明の熱可塑性組成物は望ましくは成分（ａ）のマトリックス中に成分（ｂ）が吸蔵されている形態を生ずることである。本発明の繊維の延伸、又本発明に従ったフィルムの配向においては、前述の吸蔵物のいくつかはユニクにも繊維又はフィルムの表面に突起やこぶを形成する。好ましい態様においては、そのような吸蔵物は体積平均基準で０．２−３．０μｍの短軸、又は直径をもちそして粒子又は吸蔵物は実質上、体積平均の長さ：直径の比１−２０をもつ楕円形、球状、円筒状、長円状、又は“ソーセージ”形状である。そのような繊維のモルフォロジーは繊維及びフィルムに望ましい量の、好ましくは１以上の繊維又はフィルムの光学的又は物理的性質、又は成形又は製造特性を改良するのに十分な表面粗さをもたらすことが見出された。
【０１２４】
理論で縛られることは望まないが、特に上述の組成物を使用して繊維を製造するときに得られる利点は繊維形成過程で熱可塑性ポリマー（ａ）の連続マトリックス中に熱可塑性ポリマー（ｂ）が分散した、不連続なドメインを形成する能力に、少なくとも部分的には寄与しているものと考えられる。特に、熱可塑性ポリマー（ａ）の量に比較して低い量の、そして必須の熱的性質をもつ熱可塑性ポリマー（ｂ）を使用することによって、そのような分散した、不連続なドメインが典型的な繊維形成条件下で生成すると考えられる。もし高い濃度の熱可塑性ポリマー（ｂ）が採用されるなら、成分（ａ）の連続相に拡がっているそれらの原繊維のネットワーク又は成分（ａ）が成分（ｂ）のマトリックス中に分散している構造が生成しやすい。さらに、ポリマー（ｂ）の高い結晶化温度は繊維形成操作がポリマー（ａ）の冷却時の結晶化温度（Ｔｃ）より高い温度で起こり、それによってマトリックスの延伸糸又は連続相のポリマーが繊維の表面に突起を生ずるような延伸可能なマトリックス内で比較的結晶化した吸蔵物を生ずる事を確実にする。吸蔵相粒子の少量の延伸が同様に起こり、それによって堅さ及びけん縮のような繊維のいくつかの性質が成分（ａ）よりも成分（ｂ）の結晶化によって生ずる。
【０１２５】
結果として生ずる繊維のモルフォロジーは紡糸口金の設計、紡糸率、成分（ｃ）の量と効率、押し出し混合能力及び他の物理的及び操作変数によって影響を受ける。最も望ましくは、組成物は押し出し及び急冷の後で十分な熔融張力をもち、繊維が高い線速度で、適切には延伸後の速度で少なくとも１０００ｍ／分、好ましくは少なくとも１５００ｍ／分、より好ましくは少なくとも２０００ｍ／分、そして最も好ましくは少なくとも２５００ｍ／分の速度で調製される。更に好ましくは、得られる完全延伸繊維が少なくとも１．０ｇ／デニール、より好ましくは少なくとも１．８ｇ／デニールの堅さで特徴付けられることである。
【０１２６】
本発明の態様Ｋで既に開示したように、例えば、ポリマー（ａ）と同じである第一のポリマーが１以上の第二のポリマーの１以上の層でカプセル化又はコーティングされている第一のポリマー領域を形成するために採用されており、そのような層の少なくとも１が既に開示された組成物からなるような２成分又は多成分繊維又は２層又は多層フィルムを形成することには利点がある。本発明の態様においては、コーティング組成物の量は繊維の全体体積に比較して少ないので、組成物中の成分（ｂ）の量は単一成分の繊維又はフィルムで採用されるそれよりも２倍又は３倍、又はそれ以上増加する。即ち、そのような組成物中の成分（ｂ）の量は、既に開示したように９９重量％の高さにまで及ぶ。
【０１２７】
繊維又は得られるヤーンは後成形操作で染色される。好適な染料としては有機溶媒媒体染料（分散染料）又は酸性染料、予備中和染料、及びカチオン性染料のような水溶液染料が包含される。例としてはトリフェニルメタン、ピラゾロン、アジン、ニトロ及びキノリン染料と同様にモノ及びジスルホン酸染料を含む。好ましい染料はモノ及びジスルホン酸染料である。もし望むなら、１以上の染料を適用することもでき、もし望むなら、ヤーン又はストランド中の異なった繊維が別々に染色されてもよい。
【０１２８】
染色工程においては、フィラメント、繊維又はヤーンは好ましくは最初に通常ＮａＯＨ、ＫＯＨ又はＮＨ_４ ＯＨのような塩基を含む熱水で洗浄される。熱水洗浄温度は６０−１８０℃の範囲でそして残余の潤滑剤のような仕上げ油を取り除くのに十分な高温でなければならない。次にフィラメント、繊維又はヤーンは、染料浴に通され、所望により高められた温度で、好適には８０℃−１００℃の浴温で０．１−３０分間接触させ、所望により染料を定着させるために加熱され、洗浄し、リンスしそして乾燥する。染料浴は典型的には大気圧で操作される。
【０１２９】
合成繊維を、或る染料に対する繊維の親和性を増加させたり減少させたりするために、種々の薬剤で処理することは公知である。例えば、ポリマー鎖は追加の反応性基と置換されるか又はさらに末端基を与えるために短くされ、それによって増加した染料サイトの数と結果として起こる染色性の増加を提供する。代わりに、或る染料の染色性を減少させるために、ポリマーはキャッピング剤と反応して官能性末端基の数と有効性を減少させる。まずいことに、そのようなプロセスはポリマーの熔融特性と結晶性を変えてしまい、それによって繊維の紡糸性と後で繊維の性質を変性するための能力に影響を与える。本発明は必ずしも繊維の紡糸性又は繊維の変性特性に影響を与えることなしに形成される繊維の染色性を減少させる方法を提供する。本発明は在来の明るい染料や深みのある染料技術を使用して実施される。
【０１３０】
染料の取り込みは繊維の結晶構造により影響を受ける。非晶質のポリマー領域は一般的に結晶性ポリマー領域よりも容易に水ベースの染料を受け入れやすい。繊維中の大結晶の生成は大量の非晶質のポリマーと比較的吸蔵されていない非晶質の領域を生ずる。比較的小結晶の生成は一般的に吸蔵されていない非晶質領域の数と合計非晶質ポリマー量を減少させる。本発明に従った繊維においては、追加の成分（ｂ）の吸蔵領域は成分（ａ）による結晶構造とは独立している異なった結晶及び変更された結晶モルフォロジー（本来備わっている異なった水分輸送速度と平衡水分含量）を与え、それによって異なった繊維間の熱履歴の変化から生ずる繊維取り込み変化を修正する。特に、本発明の繊維は一般に完全に又は実質上成分（ａ）から作られた繊維に比較して減少したストライク速度をもつ。この理由から、本発明の繊維は本来改良された耐シミ性をもつ。
【０１３１】
望ましくは、フィラメント又は繊維は０．５デニール−６０デニール、そして好ましくは１デニール−３０デニールの範囲である。繊維はステープルファイバー、連続繊維、バルク連続フィラメント（“ＢＣＦ”）、又はこれらの混合物であるが；連続形態が好ましい。
ヤーンは前述のフィラメント又は繊維から公知の技術に従って製造する。
【０１３２】
コーティングもまた延伸前後のフィラメントに適用できる。好ましいコーティング剤としては潤滑剤、静電気防止剤、シーラント、及び金属光沢コーティング剤が包含される。本発明の繊維の本来備わった表面粗さと後加工プロセスで使用されるローラーやガイドに対する減少した摩擦により、本発明に従ったヤーンの加工においては一般的には必要となる潤滑剤の量を減少させるか又はまったく必要としなくなる。もし使うなら、仕上剤の量は一般的に合計繊維重量基準で０．５−２．５％である。
【０１３３】
本発明のフィラメントを延伸する一つの手段は（ｉ）急冷されたフィラメントを徐々に増加する速度で操作される多数組のゴデットに供給し、それによってフィラメントを所望の延伸比にする。好ましい態様においては、第一のゴデットは６００−１０００ｍ／分、好ましくは６００ｍ／分で操作しそして最終ゴデットは１２００−６０００ｍ／分、好ましくは少なくとも１８００ｍ／分で操作する。熟練した当業者なら、これらの延伸条件は本発明の操作性に影響を及ぼすことなしで変更できることを認識するであろう。
【０１３４】
繊維はいくつかの適切な技術を使用してテクチャライズ又はけん縮してもよい。そのようなプロセスの一つは繊維をけん縮するために熱空気を使用したテクスチャリングエアジェットを使用する。好ましくは、テクスチャリングエアジェットは３．０−１０．０バール（０．３−１．０ＭＰａ）の空気圧と１２０−１８０℃の温度で操作するスプリットタイプである。けん縮された繊維はざる又は多孔ドラムに取り込まれ空気を通して繊維を冷却しけん縮を定着させる。代わりに、又は所望により、多重フィラメントは織り交ぜエアジェットを通して、好ましくは１．０−８．０バール（０．１−０．８ＭＰａ）の空気圧力を使用してフィラメントを絡み合わせそして得られるヤーンに嵩を加える。最終操作において、繊維又はそれらの組み合わせは円筒状のパッケージ、ボビン又はスプールに巻き取られる。好ましくは、嵩高の繊維は１００−１０００のデニールをもつ。
【０１３５】
更なる態様においては、別々のパッケージに巻き取られた２以上の繊維は多重ヤーンを作るために撚り工程に送られる。好適な撚り工程は少なくとも２本の別々の、好ましくはけん縮した繊維を、Ｖｅｒｄｏｌ，Ｉｎｃ．又はＶｏｌｋｍａｎｎ，Ｉｎｃ．によって製造された撚り機で糸にすることからなる。好ましくは、インチ当たり２−９撚りの６００−８０００デニールの多重ヤーン、好ましくはインチ当たり３−６撚りの８００−１５００デニールの２重ヤーンが製造される。好適には、撚り機はスピンドル速度５０００−８０００回転／分で操作される。熟練した当業者なら、本発明の繊維はまた所望の性質をもつヤーンを製造するために１以上の繊維を撚りの有る又は無しで組み合わせてもよいことは理解するであろう。例えば、少なくとも２の異なった繊維タイプで、少なくとも１は本発明に従って製造された繊維からなる多重繊維が製造される。残りの繊維は従来の天然又は合成繊維又は本発明に従ったものとは異なる繊維である。
【０１３６】
或る用途、特にカーペット製造においては、ヤーンは繊維に最終レベルの結晶性を与えるために種々の熱処理に曝される。ヒートセットはヤーンに寸法安定性と改良された耐熱性を与える。撚り多重ヤーンの場合、ヒートセットは機械的な撚り応力を軽減させ、そのような撚りヤーンから製造されたカーペットの撚り保持や外観を改良する。一般的に、その工程はヤーンを適切な温度に、一般的には応力の存在なしで、ある時間及び所望のヤーンの性質を達成するための方法で加熱する事を含む。好適なヒートセットプロセスはスーペルバ（Ｓｕｐｅｒｂａ）又はスッセン（Ｓｕｅｓｓｅｎ）プロセスを含む。
【０１３７】
一般的には、ヒートセット工程における時間と温度の厳密な調節が均一な染色性をもつヤーンを製造するために必要である。さらに、多くのヤーンはヒートセット工程の結果として収縮し、それによってデニールのばらつきを増大させる。有利なことに、本発明に従ったヤーンは染色や光学縞筋に対する敏感性が少なくそしてそれゆえにヒートセット工程での変動により耐えられる。さらに、本発明のヤーン及びそれから製造された製品は従来のヤーンに比較してヒートセット、洗浄、染色、又は他の加工工程、そして使用時における収縮が少ない。好ましいヤーン、特に撚り、ヒートセットした、多重ヤーンは１３０℃１分間のヒートセットで１５％以下のデニール減少を示す。
【０１３８】
本発明に従った繊維は望ましくは成分（ａ）から単独に又は実質的に作られた繊維に比較して高い弾性率をもつ。本発明に従ったヤーンを含むカーペットは改良された耐シミ、耐汚染性と増大した耐久性によって特徴付けられる。この効果は特に成分（ａ）がポリエステルのような低弾性率の樹脂からなるときに強調される。本発明の繊維の比較的粗い表面は、粗い粒子は滑らかな繊維表面で起こるような繊維表面の大部分に接触することができないので、その高められた汚れを解き放つ性質に寄与する。さらに、繊維の粗い表面はヤーンの束又はカーペットパイル中で洗濯や真空洗浄によって容易に取り除くことのできる粗い粒子を多く含んでいる。
【０１３９】
本発明のヤーンは熟練した当業者に公知の標準編み込み技術を使用する衣類用途の布を織ったり編んだりするために使用される。本発明の繊維及びヤーンの使用によって得られる高い繊維間摩擦力によって、これらの繊維から作られる織物はより均一な織物構造、少ない縞筋、及び少ない布切れを与える。本発明に従ったヤーンの加工性は少なくとも部分的にはその表面の性質によって、減少した工程応力、改善された延伸性、及び減少したロール巻き込みを得られる利点がある。
【０１４０】
カーペット製造について
本発明のヤーンは容易にカーペット、マット、及び床や壁被覆用途用に加工できる。カーペットを製造するために、ヤーン、特に撚りヤーンがタフトされ、編みこまれ、又は裏打ちに熔融編み込みされる。“グレイジュ（ｇｒｅｉｇｅ）グッド”と呼ばれる得られたカーペットは適切な色に染色されてもよい。次に、カーペットの裏面をラテックスのような適切な接着剤又はシール剤でコートし、そしてタフトヤーンを第一の裏地に結合させるために乾燥する。もし望むなら、それから第二の裏打ちをカーペットの裏側に取り付ける。タフトヤーンをそれから所望によりループパイル、切断パイル又はループ及び切断パイルタイプのカーペットを形成するために公知の切断操作にかける。さらに、多重撚りヤーンの多重末端を織物裏地に含ませて所望のカーペットデザインを得るために表面のテクスチャ加工をする。
【０１４１】
カーペットの染色は繊維又はヤーンの染色に関して前に述べた染料を使用してバッチプロセス又は連続プロセスで行われる。従来の深み染色及び明るい染色技術、スペース染色技術、ニット−デニット染色技術など全て使用することができる。
【０１４２】
好ましくは、カーペットは、オッチング社又はクスター社から市販されているような水溶液染色ユニットを通すことによって染色される。カーペットはコンベアーの手段によってユニットを通過する。一般的に、カーペットは最初に、例えば、湿潤剤又は界面活性剤を加えた水を通すことによって予め濡らされる。カーペットはそれからニップロールの間を通り過剰の水を取り除きそれから染料と染色補助剤を含む“リカー”と呼ばれる媒体と接触する。典型的には、酸染料プロセスにおいては、リカーのｐＨは４．５−８に維持される。リカーはカーペットにスプレーされるか又は貯槽からブレード装置によって適用される。次に、カーペットはスチーム加熱された容器のような加熱室を通りカーペット上に染料を定着させる。カーペットはそれから残余のリカーをカーペットから取り除くために洗浄され、リンスされそして乾燥される。もし望むなら、耐シミ剤又はシミブロッカー、例えば、シラン化合物が染料リカー中に含まれていてもよいし、カーペットに同時に又は引き続く乾燥プロセスに適用されてもよい。従来からの耐シミ及び耐汚染技術が本発明の繊維、カーペット及び織物に使用することができる。
【０１４３】
本発明に従ったカーペット又は敷物は好ましくは以下の寄与の少なくとも一つを示す：減少した染料縞筋、減少した汚れ、洗濯時の改良された色定着性、紫外線に対する改良された色定着性、改良された手触り、改良された回収、又は改良された耐久性；どのケースにおいても熱可塑性ポリマー成分（ｂ）を含まない組成物から作られた繊維からなるカーペット又は敷物との比較である。
【０１４４】
要約
下記は、本明細書で完全に説明され開示された本発明の特定の態様のまとめである。
【０１４５】
１． （ａ）１６０℃より大きい結晶化温度、Ｔｃ、をもつ第一の熱可塑性ポリマー８６−９２重量％、
（ｂ）結晶化温度、Ｔｃ’、をもつ（ａ）とは化学的に異なる第二の熱可塑性ポリマー１４−８重量％、及び
（ｃ）（ａ）と（ｂ）用の相溶化剤、
ここで該％は（ａ）と（ｂ）の合計量基準であり、Ｔｃ はＴｃ’よりも少なくとも５℃小さい、からなることを特徴とする押出し繊維及びフィルムの製造に有用な熱可塑性ポリマー組成物。
【０１４６】
２． 第一の熱可塑性ポリマーがポリアミド又はコポリアミドでありそしてＴｃ’が１９５℃より大きい態様１記載の組成物。
【０１４７】
３． 第一の熱可塑性ポリマーがポリアミド又はコポリアミドでありそして第二の熱可塑性ポリマーがアイソタクチック又はシンジオタクチック立体構造をもつポリビニリデン芳香族ポリマーである態様１記載の組成物。
【０１４８】
４． 第一の熱可塑性ポリマーがナイロン６、ナイロン６，６、又はナイロン６とナイロン６，６のコポリマーでありそして第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様３記載の組成物。
【０１４９】
５． ポリアミドが３０−１８０の相対粘度をもつナイロン６である態様３記載の組成物。
【０１５０】
６． 第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−又はハロ−置換されたビニル芳香族モノマー又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換ビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様５記載の組成物。
【０１５１】
７． 第二の熱可塑性ポリマーが９５％より大きいタクチシティーと５０，０００より大きいＭｗをもつ態様５記載の組成物。
【０１５２】
８． １０．０より小さい黄色指数、ＹＩをもつ態様１記載の組成物。
【０１５３】
９． 合計組成物重量基準で０．１−１０％の相溶化剤ｃ）からなる態様１記載の組成物。
【０１５４】
１０． 相溶化剤が極性基変性ビニリデン芳香族ホモポリマー又はコポリマーである態様９記載の組成物。
【０１５５】
１１． 相溶化剤が極性基変性ポリスチレン、１以上のビニル芳香族モノマーと１以上の極性コモノマーとのコポリマー、又はスチレンと１以上の環状Ｃ_１−１０ アルキル−又はハロ−置換されたビニル芳香族モノマー又は極性基−置換されたビニル芳香族モノマーとの極性基変性コポリマーである態様１０記載の組成物。
【０１５６】
１２． 相溶化剤が無水マレイン酸変性又はフマール酸変性スチレンホモポリマー又はスチレンと１以上の環状Ｃ_１−１０ アルキル−置換されたスチレンとの無水マレイン酸変性又はフマール酸変性スチレンコポリマーであり、該相溶化剤が０．０１−５．０モル％の共重合した無水マレイン酸又はフマール酸官能性をもつ態様１１記載の組成物。
【０１５７】
１３． 繊維又はフィルムの形成後に、成分（ａ）のマトリックス中に成分（ｂ）が０．２μｍより大きい体積平均短軸径をもつ吸蔵粒子形態で存在する態様１−１２のいずれかに記載の組成物。
【０１５８】
１４． 繊維又はフィルムの形成後に、成分（ｂ）が０．３−２．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在する態様１３記載の組成物。
【０１５９】
１５． 繊維又はフィルムの形成後に、成分（ｂ）が３．０μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様１３記載の組成物。
【０１６０】
１６． 繊維又はフィルムの形成後に、成分（ｂ）が２．８μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様１４記載の組成物。
【０１６１】
１７． 繊維の形成後に、成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様１−１２のいずれかに記載の組成物。
【０１６２】
１８． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様１５記載の組成物。
【０１６３】
１９． 繊維の形成後に、成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様１−１２のいずれかに記載の組成物。
【０１６４】
２０． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様１５記載の組成物。
【０１６５】
２１． 成分（ｃ）の量が成分（ａ）と成分（ｂ）の結合重量基準で０−５％の範囲にありそして成分（ｃ）（もし存在するなら）中の反応性、官能性基の合計量が成分（ｂ）と成分（ｃ）の合計量基準で０．００１−０．２５モル％である態様１−１２のいずれかに記載の組成物。
【０１６６】
２２． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様１５記載の組成物。
【０１６７】
２３． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様１９記載の組成物。
【０１６８】
２４． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様２０記載の組成物。
【０１６９】
２５． さらに合計組成物重量基準で０．１−１０．０％のつや消し剤を含む態様１−１２のいずれかに記載の組成物。
【０１７０】
２６． （ａ）１６０℃より大きい結晶化温度、Ｔｃ、をもつ第一の熱可塑性ポリマー７６−９７重量％、
（ｂ）結晶化温度、Ｔｃ’、をもつ（ａ）とは化学的に異なる第二の熱可塑性ポリマー２４−３重量％、及び
（ｃ）（ａ）と（ｂ）用の相溶化剤、
ここで該％は（ａ）と（ｂ）の合計量基準であり、Ｔｃ はＴｃ’よりも少なくとも５℃小さい、からなることを特徴とする熱可塑性ポリマー組成物からなる押出し延伸繊維。
【０１７１】
２７． 第一の熱可塑性ポリマーがポリアミド又はコポリアミドでありそしてＴｃ’が１９５℃より大きい態様２６記載の繊維。
【０１７２】
２８． 第一の熱可塑性ポリマーがポリアミド又はコポリアミドでありそして第二の熱可塑性ポリマーがアイソタクチック又はシンジオタクチック立体構造をもつポリビニリデン芳香族ポリマーである態様２６記載の繊維。
【０１７３】
２９． 第一の熱可塑性ポリマーがナイロン６、ナイロン６，６、又はナイロン６とナイロン６，６のコポリマーでありそして第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様２８記載の繊維。
【０１７４】
３０． ポリアミドが３０−１８０の相対粘度をもつナイロン６である２７記載の繊維。
【０１７５】
３１． 第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−又はハロ−置換されたビニル芳香族モノマー又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基置換ビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様３０記載の繊維。
【０１７６】
３２． 第二の熱可塑性ポリマーが９５％より大きいタクチシティーと５０，０００より大きいＭｗをもつ態様３０記載の繊維。
【０１７７】
３３． １０．０より小さい黄色指数、ＹＩをもつ態様２６記載の繊維。
【０１７８】
３４． 合計組成物重量基準で０．１−１０％の相溶化剤ｃ）を含む態様２６記載の繊維。
【０１７９】
３５． 相溶化剤が極性基変性ポリスチレン、１以上のビニル芳香族モノマーと１以上の極性コモノマーとのコポリマー、スチレンと１以上の環状Ｃ_１−１０ アルキル−又はハロ−置換されたビニル芳香族モノマー又は極性基−置換されたビニル芳香族モノマーとの極性基変性コポリマーである態様３４記載の繊維。
３６． 相溶化剤が極性基変性ポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−又はハロ−置換されたビニル芳香族モノマー又は極性基−置換されたビニル芳香族モノマーとの極性基変性コポリマーである態様３５記載の繊維。
【０１８０】
３７． 相溶化剤が無水マレイン酸変性又はフマール酸変性スチレンホモポリマー又はスチレンと１以上の環状Ｃ_１−１０ アルキル−置換されたスチレンとの無水マレイン酸変性又はフマール酸変性スチレンコポリマーであり、該相溶化剤が０．０１−５．０モル％の共重合した無水マレイン酸又はフマール酸官能性をもつ態様３６記載の繊維。
【０１８１】
３８． 成分（ａ）のマトリックス中に成分（ｂ）が０．２μｍより大きい体積平均短軸径をもつ吸蔵粒子形態で存在する態様２６−３７のいずれかに記載の繊維。
【０１８２】
３９． 成分（ｂ）が０．３−２．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在する態様３８記載の繊維。
【０１８３】
４０． 成分（ｂ）が３．０μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様３８記載の繊維。
【０１８４】
４１． 成分（ｂ）が２．８μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様３９記載の繊維。
【０１８５】
４２． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様２６−３７のいずれかに記載の繊維。
【０１８６】
４３． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様４０記載の繊維。
【０１８７】
４４． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様２６−３７のいずれかに記載の繊維。
【０１８８】
４５． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様４０記載の繊維。
【０１８９】
４６． 成分（ｃ）の量が成分（ａ）と成分（ｂ）の結合重量基準で０−５％の範囲にありそして成分（ｃ）（もし存在するなら）中の反応性、官能性基の合計量が成分（ｂ）と成分（ｃ）の合計量基準で０．００１−０．２５モル％である態様２６−３７のいずれかに記載の繊維。
【０１９０】
４７． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様４０記載の繊維。
【０１９１】
４８． 組成物が成分（ａ）と成分（ｂ）の合計重量基準で８０−９５重量％の成分（ａ）；及び２０−５重量％の成分（ｂ）からなる態様２６−３７のいずれかに記載の繊維。
４９． 組成物が成分（ａ）と成分（ｂ）の合計重量基準で８６−９２重量％の成分（ａ）；及び１４−８重量％の成分（ｂ）からなる態様２６−３７のいずれかに記載の繊維。
５０． さらに合計組成物重量基準で０．１−１０．０％のつや消し剤を含む態様２６−３７のいずれかに記載の繊維。
【０１９２】
５１． （ａ）１６０℃より大きい結晶化温度、Ｔｃ、をもつ第一の熱可塑性ポリマー６５−９７重量％、及び
（ｂ）結晶化温度、Ｔｃ’、をもつ（ａ）とは化学的に異なりそして極性官能基をもつ第二の熱可塑性ポリマー３５−３重量％、及び所望により１以上の非−重合体添加物から本質的になることを特徴とする押出し繊維及びフィルムの製造に有用な熱可塑性ポリマー組成物。
【０１９３】
５２． 第一の熱可塑性ポリマーがポリアミド又はコポリアミドでありそしてＴｃ’が１９５℃より大きい態様５１記載の組成物。
【０１９４】
５３． ＴｃがＴｃ’より少なくとも５℃小さい態様５１記載の組成物。
【０１９５】
５４． 第一の熱可塑性ポリマーがナイロン６、ナイロン６，６、又はナイロン６とナイロン６，６のコポリマーでありそして第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様５１記載の組成物。
【０１９６】
５５． ポリアミドが３０−１８０の相対粘度をもつナイロン６である態様５２記載の組成物。
【０１９７】
５６． 第二の熱可塑性ポリマーがシンジオタクチックポリスチレン又はスチレンとｐ−メチルスチレンとのシンジオタクチックコポリマーの極性基変性誘導体である態様５１記載の組成物。
【０１９８】
５７． 第二の熱可塑性ポリマーが９５％より大きいタクチシティーと５０，０００より大きいＭｗをもつ態様５１記載の組成物。
【０１９９】
５８． １０．０より小さい黄色指数、ＹＩをもつ態様５１記載の組成物。
【０２００】
５９． ５．０−２０重量％の成分（ｂ）を必須成分として含む態様５１記載の組成物。
【０２０１】
６０． ８−１４重量％の成分（ｂ）を必須成分として含む態様５９記載の組成物。
【０２０２】
６１． 第二成分が無水マレイン酸変性又はフマール酸変性シンジオタクチックポリスチレン又は無水マレイン酸変性又はフマール酸変性したスチレンとｐ−メチルスチレンのシンジオタクチックコポリマーである態様５６記載の組成物。
【０２０３】
６２． 成分（ｂ）が０．０１−５．０モル％の共重合した無水マレイン酸又はフマール酸官能性をもつ態様６１記載の組成物。
【０２０４】
６３． 繊維又はフィルムの形成後に、成分（ｂ）のマトリックス中に成分（ｂ）が０．２μｍより大きい体積平均短軸径をもつ吸蔵粒子形態で存在する態様５１−６２のいずれかに記載の組成物。
【０２０５】
６４． 繊維又はフィルムの形成後に、成分（ｂ）が０．３−２．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在する態様６３記載の組成物。
【０２０６】
６５． 繊維又はフィルムの形成後に、成分（ｂ）が３．０μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様６３記載の組成物。
【０２０７】
６６． 繊維又はフィルムの形成後に、成分（ｂ）が２．８μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様６４記載の組成物。
【０２０８】
６７． 繊維の形成後に、成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様５１−６２のいずれかに記載の組成物。
【０２０９】
６８． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様６５記載の組成物。
【０２１０】
６９． 繊維の形成後に、成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様５１−６２のいずれかに記載の組成物。
【０２１１】
７０． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様６５記載の組成物。
【０２１２】
７１． 成分（ｂ）中の極性基が反応性極性官能基でありそして成分（ｂ）の０．００１−０．２５モル％の量で存在する態様５１−６２のいずれかに記載の組成物。
【０２１３】
７２． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様６５記載の組成物。
【０２１４】
７３． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様６９記載の組成物。
【０２１５】
７４． 繊維の形成後に、成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様７０記載の組成物。
【０２１６】
７５． さらに合計組成物重量基準で０．１−１０．０％のつや消し剤を含む態様５１−６２記載の組成物。
【０２１７】
７６． （ａ）１６０℃より大きい結晶化温度、Ｔｃ、をもつ第一の熱可塑性ポリマー６５−９７重量％、及び
（ｂ）結晶化温度、Ｔｃ’、をもつ（ａ）とは化学的に異なり、そして極性官能基を含む第二の熱可塑性ポリマー３５−３重量％、及び所望により１以上の非−重合体添加物から本質的になることを特徴とする押出し延伸繊維。
【０２１８】
７７． 第一の熱可塑性ポリマーがポリアミド又はコポリアミドでありそしてＴｃ’が１９５℃より大きい態様７６記載の繊維。
【０２１９】
７８． ＴｃがＴｃ’より少なくとも５℃小さい態様７６記載の繊維。
【０２２０】
７９． 第一の熱可塑性ポリマーがナイロン６、ナイロン６，６、又はナイロン６とナイロン６，６のコポリマーでありそして第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様７６記載の繊維。
【０２２１】
８０． ポリアミドが３０−１８０の相対粘度をもつナイロン６である態様７７記載の繊維。
【０２２２】
８１． 第二の熱可塑性ポリマーがシンジオタクチックポリスチレン又はスチレンとｐ−メチルスチレンとのシンジオタクチックコポリマーの極性基変性誘導体である態様７６記載の繊維。
【０２２３】
８２． 第二の熱可塑性ポリマーが９５％より大きいタクチシティーと５０，０００より大きいＭｗをもつ態様７６記載の繊維。
【０２２４】
８３． １０．０より小さい黄色指数、ＹＩをもつ態様７６記載の繊維。
【０２２５】
８４． ５．０−２０重量％の成分（ｂ）を必須成分として含む態様７６記載の繊維。
【０２２６】
８５． ８−１４重量％の成分（ｂ）を必須成分として含む態様８４記載の繊維。
【０２２７】
８６． 第二成分が無水マレイン酸変性又はフマール酸変性シンジオタクチックポリスチレン又は無水マレイン酸変性又はフマール酸変性したスチレンとｐ−メチルスチレンのシンジオタクチックコポリマーである態様８１記載の繊維。
【０２２８】
８７． 成分（ｂ）が０．０１−５．０モル％の共重合した無水マレイン酸又はフマール酸官能性をもつ態様８６記載の繊維。
【０２２９】
８８． 成分（ａ）のマトリックス中に成分（ｂ）が０．２μｍより大きい体積平均短軸径をもつ吸蔵粒子形態で存在する態様７６−８７のいずれかに記載の繊維。
【０２３０】
８９． 成分（ｂ）が０．３−２．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在する態様８８記載の繊維。
【０２３１】
９０． 成分（ｂ）が３．０μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様８８記載の繊維。
【０２３２】
９１． 成分（ｂ）が２．８μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様８９記載の繊維。
【０２３３】
９２． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様７６−８７のいずれかに記載の繊維。
【０２３４】
９３． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様９０記載の繊維。
【０２３５】
９４． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様７６−８７のいずれかに記載の繊維。
【０２３６】
９５． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様９０記載の繊維。
【０２３７】
９６． 成分（ｂ）中の極性基が反応性極性官能基でありそして成分（ｂ）の０．００１−０．２５モル％で存在する態様７６−８７記載の繊維。
【０２３８】
９７． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様９０記載の繊維。
【０２３９】
９８． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様９４記載の繊維。
９９． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様９５記載の繊維。
１００． さらに合計組成物重量基準で０．１−５．０％のつや消し剤を含む態様７６−８７のいずれかに記載の繊維。
【０２４０】
１０１． （ａ）１６０℃より大きい結晶化温度、Ｔｃ、をもつ第一の熱可塑性ポリマー６５−９７重量％、及び
（ｂ）結晶化温度、Ｔｃ’、をもつ（ａ）とは化学的に異なり、そして極性官能基を含む第二の熱可塑性ポリマー３５−３重量％、及び所望により１以上の非−重合体添加物から本質的になることを特徴とする押出し、延伸、及び縮れ繊維。
【０２４１】
１０２． 第一の熱可塑性ポリマーがポリアミド又はコポリアミドでありそしてＴｃ’が１９５℃より大きい態様１０１記載の繊維。
【０２４２】
１０３． ＴｃがＴｃ’より少なくとも１０℃小さい態様１０１記載の繊維。
【０２４３】
１０４． 第一の熱可塑性ポリマーがナイロン６、ナイロン６，６、又はナイロン６とナイロン６，６のコポリマーでありそして第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様１０１記載の繊維。
【０２４４】
１０５． ポリアミドが３０−１８０の相対粘度をもつナイロン６である態様１０２記載の繊維。
【０２４５】
１０６． 第二の熱可塑性ポリマーがシンジオタクチックポリスチレン又はスチレンとｐ−メチルスチレンとのシンジオタクチックコポリマーの極性基変性誘導体である態様１０１記載の繊維。
【０２４６】
１０７． 第二の熱可塑性ポリマーが９５％より大きいタクチシティーと５０，０００より大きいＭｗをもつ態様１０１記載の繊維。
【０２４７】
１０８． １０．０より小さい黄色指数、ＹＩをもつ態様１０１記載の繊維。
【０２４８】
１０９． ５．０−２０重量％の成分（ｂ）を必須成分として含む態様１０１記載の繊維。
【０２４９】
１１０． ８−１４重量％の成分（ｂ）を必須成分として含む態様１０９記載の繊維。
【０２５０】
１１１， 成分（ｂ）が無水マレイン酸変性又はフマール酸変性シンジオタクチックポリスチレン又は無水マレイン酸変性又はフマール酸変性したスチレンとｐ−メチルスチレンとのシンジオタクチックコポリマーである態様１０１記載の繊維。
【０２５１】
１１２． 成分（ｂ）が０．０１−５．０モル％の共重合した無水マレイン酸又はフマール酸官能性をもつ態様１１１記載の繊維。
【０２５２】
１１３． 成分（ａ）のマトリックス中に成分（ｂ）が０．２μｍより大きい体積平均短軸径をもつ吸蔵粒子形態で存在する態様１０１−１１２のいずれかに記載の繊維。
【０２５３】
１１４． 成分（ｂ）が０．３−２．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在する態様１１３記載の繊維。
【０２５４】
１１５． 成分（ｂ）が３．０μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様１１３記載の繊維。
【０２５５】
１１６． 成分（ｂ）が２．８μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様１１４記載の繊維。
【０２５６】
１１７． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様１０１−１１２のいずれかに記載の繊維。
【０２５７】
１１８． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様１１５記載の繊維。
【０２５８】
１１９． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様１０１−１１２のいずれかに記載の繊維。
【０２５９】
１２０． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様１１５記載の繊維。
【０２６０】
１２１． 成分（ｂ）中の極性基が反応性極性官能基でありそして成分（ｂ）の０．００１−０．２５モル％の量で存在する態様１０１−１１２のいずれかに記載の繊維。
【０２６１】
１２２． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様１１５記載の繊維。
【０２６２】
１２３． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様１１９記載の繊維。
【０２６３】
１２４． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様１２０記載の繊維。
【０２６４】
１２５． さらに合計組成物重量基準で０．１−１０．０％のつや消し剤を含む態様１０１−１１２のいずれかに記載の繊維。
【０２６５】
１２６． ２以上の縦方向長さのポリマードメインからなり、少なくとも１のドメインが（ａ）１６０℃より大きい結晶化温度、Ｔｃ、をもつ第一の熱可塑性ポリマー７６−９７重量％、
（ｂ）結晶化温度、Ｔｃ’、をもつ（ａ）とは化学的に異なる第二の熱可塑性ポリマー２４−３重量％、及び
（ｃ）（ａ）と（ｂ）用の相溶化剤、
ここで該％は（ａ）と（ｂ）の合計量基準であり、Ｔｃ はＴｃ’よりも少なくとも５℃小さい、からなることを特徴とする熱可塑性ポリマーブレンド物からなる多成分繊維。
【０２６６】
１２７． ブレンド物の第一の熱可塑性ポリマーがポリアミド又はコポリアミドでありそしてＴｃ’が１９５℃より大きい態様１２６記載の繊維。
【０２６７】
１２８． ブレンド物の第一の熱可塑性ポリマーがポリアミド又はコポリアミドでありそして第二の熱可塑性ポリマーがアイソタクチック又はシンジオタクチック立体構造をもつポリビニリデン芳香族ポリマーである態様１２６記載の繊維。
【０２６８】
１２９． ブレンド物の第一の熱可塑性ポリマーがナイロン６、ナイロン６，６、又はナイロン６とナイロン６，６のコポリマーでありそして第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様１２８記載の繊維。
【０２６９】
１３０． ポリアミドが３０−１８０の相対粘度をもつナイロン６である態様１２８記載の繊維。
【０２７０】
１３１． 第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−又はハロ−置換されたビニル芳香族モノマー又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基置換ビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様１３０記載の繊維。
【０２７１】
１３２． 第二の熱可塑性ポリマーが９５％より大きいタクチシティーと５０，０００より大きいＭｗをもつ態様１３０記載の繊維。
【０２７２】
１３３． 芯／鞘繊維でありそしてブレンド物が鞘からなる態様１２６記載の繊維。
【０２７３】
１３４． ブレンド物が合計組成物重量基準で０．１−１０％の相溶化剤ｃ）を含む態様１２６記載の繊維。
【０２７４】
１３５． 相溶化剤が極性基変性ポリスチレン、１以上のビニル芳香族モノマーと１以上の極性コモノマーとのコポリマー、又はスチレンと１以上の環状Ｃ_１−１０ アルキル−又はハロ−置換されたビニル芳香族モノマー又は極性基−置換されたビニル芳香族モノマーとの極性基変性コポリマーである態様１３４記載の繊維。
【０２７５】
１３６． 相溶化剤が極性基変性ポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−又はハロ−置換されたビニル芳香族モノマー又は極性基−置換されたビニル芳香族モノマーとの極性基変性コポリマーである態様１３５記載の繊維。
【０２７６】
１３７． 相溶化剤が無水マレイン酸変性又はフマール酸変性スチレンホモポリマー又はスチレンと１以上の環状Ｃ_１−１０ アルキル−置換されたスチレンとの無水マレイン酸変性又はフマール酸変性スチレンコポリマーであり、該相溶化剤が０．０１−５．０モル％の共重合した無水マレイン酸又はフマール酸官能性をもつ態様１３６記載の繊維。
【０２７７】
１３８． 成分（ａ）のマトリックス中に成分（ｂ）が０．２μｍより大きい体積平均短軸径をもつ吸蔵粒子形態で存在する態様１２６−１３７のいずれかに記載の繊維。
【０２７８】
１３９． 成分（ｂ）が０．３−２．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在する態様１３８記載の繊維。
【０２７９】
１４０． 成分（ｂ）が３．０μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様１３８記載の繊維。
【０２８０】
１４１． 成分（ｂ）が２．８μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様１３９記載の繊維。
【０２８１】
１４２． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様１２６−１３７のいずれかに記載の繊維。
【０２８２】
１４３． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様１４０記載の繊維。
【０２８３】
１４４． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様１２６−１３７のいずれかに記載の繊維。
【０２８４】
１４５． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様１４０記載の繊維。
【０２８５】
１４６． 成分（ｃ）の量が成分（ａ）と成分（ｂ）の結合重量基準で０−５％の範囲にありそして成分（ｃ）（もし存在するなら）中の反応性、官能性基の合計量が成分（ｂ）と成分（ｃ）の合計量基準で０．００１−０．２５モル％である態様１２６−１３７のいずれかに記載の繊維。
【０２８６】
１４７． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様１４０記載の繊維。
【０２８７】
１４８． ブレンド組成物が成分（ａ）と成分（ｂ）の合計量基準で成分（ａ）８０−９５重量％、及び成分（ｂ）２０−５重量％からなる態様１２６−１３７のいずれかに記載の繊維。
【０２８８】
１４９． 芯がナイロン６又はナイロン６，６からなる態様１３３記載の繊維。
【０２８９】
１５０． さらに合計組成物重量基準で０．１−１０．０％のつや消し剤を含む態様１２６−１３７のいずれかに記載の繊維。
【０２９０】
１５１． （ａ）１６０℃より大きい結晶化温度、Ｔｃ、をもつ第一の熱可塑性ポリマー７６−９７重量％、
（ｂ）結晶化温度、Ｔｃ’、をもつ（ａ）とは化学的に異なる第二の熱可塑性ポリマー２４−３重量％、及び所望により、
（ｃ）（ａ）と（ｂ）用の相溶化剤、
ここで該％は（ａ）と（ｂ）の合計量基準である、からなる熱可塑性ポリマー組成物からなることを特徴とし、且つ該熱可塑性ポリマー組成物が主として成分（ａ）からなる基本樹脂と主として成分（ｂ）及び所望により成分（ｃ）及びさらに所望により、少量の成分（ａ）からなる濃縮樹脂を溶融及び混合し；そして得られた溶融熱可塑性ポリマー組成物を繊維形態に押出し及び延伸するか又は得られた熱可塑性ポリマー組成物をフィルム形態に押出し又は延伸することによって製造される押出し延伸繊維又は押出し延伸フィルム。
【０２９１】
１５２． 熱可塑性組成物が伸張流れ混合を内包する溶融混合プロセスによって製造される態様１５１記載の繊維又はフィルム。
【０２９２】
１５３． ＴｃがＴｃ’より少なくとも１０℃小さい態様１５１記載の繊維又はフィルム。
【０２９３】
１５４． 第一の熱可塑性ポリマーがナイロン６、ナイロン６，６、又はナイロン６とナイロン６，６のコポリマーでありそして第二の熱可塑性ポリマーがシンジオタクチックポリスチレン、スチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマー、又はシンジオタクチックポリスチレン又はスチレンと１以上の環状Ｃ_１−１０ アルキル−、ハロ−、又は極性基−置換されたビニル芳香族モノマーとのシンジオタクチックコポリマーの極性基変性誘導体である態様１５１記載の繊維又はフィルム。
【０２９４】
１５５． ポリアミドが３０−１８０の相対粘度をもつナイロン６である態様１５４記載の繊維又はフィルム。
【０２９５】
１５６． 第二の熱可塑性ポリマーがシンジオタクチックポリスチレン又はスチレンとｐ−メチルスチレンとのシンジオタクチックコポリマーの極性基変性誘導体である態様１５１記載の繊維又はフィルム。
【０２９６】
１５７． 第二の熱可塑性ポリマーが９５％より大きいタクチシティーと５０，０００より大きいＭｗをもつ態様１５１記載の繊維又はフィルム。
【０２９７】
１５８． １０．０より小さい黄色指数、ＹＩをもつ態様１５１記載の繊維又はフィルム。
【０２９８】
１５９． ５．０−２０重量％の成分（ｂ）を必須成分として含む態様１５１記載の繊維又はフィルム。
【０２９９】
１６０． ８−１４重量％の成分（ｂ）を含む態様１５９記載の繊維又はフィルム。
【０３００】
１６１． 成分（ｂ）が無水マレイン酸変性又はフマール酸変性したスチレンホモポリマー又はスチレンとｐ−メチルスチレンとのコポリマーである態様１５１記載の繊維又はフィルム。
【０３０１】
１６２． 成分（ｂ）が０．０１−５．０モル％の共重合した無水マレイン酸又はフマール酸官能性をもつ態様１６１記載の繊維。
【０３０２】
１６３． 成分（ａ）のマトリックス中に成分（ｂ）が０．２μｍより大きい体積平均短軸径をもつ吸蔵粒子形態で存在する態様１５１−１６２のいずれかに記載の繊維又はフィルム。
【０３０３】
１６４． 成分（ｂ）が０．３−２．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在する態様１６３記載の繊維又はフィルム。
【０３０４】
１６５． 成分（ｂ）が３．０μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様１６３記載の繊維。
【０３０５】
１６６． 成分（ｂ）が２．８μｍより小さいＤ^９９短軸径をもつ吸蔵粒子形態で存在する態様１６４記載の繊維。
【０３０６】
１６７． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様１５１−１６２のいずれかに記載の繊維。
【０３０７】
１６８． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が０．２９以上のレーザー光散乱比又は標準繊維試料で決定された４．０以下の光沢審査員等級をもつ態様１６５記載の繊維。
【０３０８】
１６９． 成分（ａ）のマトリックス中に成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様１５１−１６２のいずれかに記載の繊維。
【０３０９】
１７０． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在し、そして該繊維が柔らかな手触りをもつ態様１６５記載の繊維。
【０３１０】
１７１． 成分（ｃ）の量が成分（ａ）と成分（ｂ）の結合重量基準で０−５％の範囲にありそして成分（ｃ）（もし存在するなら）中の反応性、官能性基の合計量が成分（ｂ）と成分（ｃ）の合計量基準で０．００１−０．２５モル％である態様１５１−１６２のいずれかに記載の繊維。
【０３１１】
１７２． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様１６５記載の繊維。
【０３１２】
１７３． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様１６９記載の繊維。
【０３１３】
１７４． 成分（ｂ）が０．２−３．０μｍの体積平均短軸径をもつ吸蔵粒子形態で存在しそして該繊維が柔らかな手触りと改良された耐久性をもつ態様１７０記載の繊維。
【０３１４】
１７５． さらに合計組成物重量基準で０．１−５．０％のつや消し剤を含む態様１５１−１６２のいずれかに記載の繊維。
【０３１５】
実施例
以下の実施例は説明のためになされたもので限定するためになされたものではなくそして追加の添加物又は成分の存在を排除するものではない。特に断らない限り本明細書をとおして全ての部及び％は重量基準である。実施例においては、以下の装置、方法と材料が使用された。
【０３１６】
コンパウンド化装置
ワーナープファイドラーＺＳＫ 直径４０ｍｍ、Ｌ／Ｄ比３４：１、長さ１．４ｍのベント付き二軸コンパウンド押し出し機を以下の実施例の組成物を調製するために使用した。標準コンパウンド押し出し機の設定は以下の通りである：
表Ａ アロイ製造のためのコンパウンド条件

熔融ポリマーブレンド物を多数の穴をもつダイを通して０．３２ｃｍ直径の円筒状ストランド（糸）に押し出し、水浴中で室温まで冷却し、そして飛沫水を除去するために２台のエアジェットの間を通した。ストランドをそれから切断機に供給して長さ２．８ｍｍで直径２．１ｍｍの円筒状チップに切断した。ブレンドしたチップを使用前に循環乾燥機中で９０℃で８−１２時間乾燥した。二つのコンパウンド化手順を使用した。マスターバッチ手段は第一のコンパウンド過程で分散相ポリマーと相溶化剤を混合することから構成される。得られたチップを最終ブレンドペレットを作るために連続相ポリマーとマスターバッチを混ぜる第二の過程の前に乾燥する。１回通過手段は；最終ブレンドペレットを作るために、分散相ポリマー、相溶化剤、そして連続相ポリマーの３成分全てを混合機（コンパウンダー）の１回通過で混合することから構成される。
【０３１７】
ワーナープファイドラーＺＳＫ 直径３０ｍｍ、Ｌ／Ｄ比３０：１、長さ０．９ｍのベント付き二軸コンパウンド押し出し機を以下の実施例の組成物を調製するために使用した。標準コンパウンド押し出し機の設定は以下の通りである：
表Ｂ アロイ製造のためのコンパウンド条件

熔融ポリマーブレンド物を多数の穴をもつダイを通して０．３２ｃｍ直径の円筒状ストランド（糸）に押し出し、水浴中で室温まで冷却し、そして飛沫水を除去するために２台のエアジェットの間を通した。ストランドをそれから切断機に供給して長さ２．８ｍｍｍで直径２．１ｍｍの円筒状チップに切断した。ブレンドしたチップを使用前に循環乾燥機中で９０℃で８−１２時間乾燥した。二つのコンパウンド化手順を使用した。マスターバッチ手段は第一のコンパウンド過程で分散相ポリマーと相溶化剤を混合することから構成される。得られたチップを最終ブレンドペレットを作るために連続相ポリマーとマスターバッチを混ぜる第二の過程の前に乾燥する。１回通過手段は；最終ブレンドペレットを作るために、分散相ポリマー、相溶化剤、そして連続相ポリマーの３成分全てを混合機（コンパウンダー）の１回通過で混合することから構成される。
【０３１８】
繊維成形装置
繊維製造のために、実験室規模と商業的規模の両方の多層フィラメント、繊維紡糸装置を使用した。ポリマー組成物を使用前に乾燥しそして乾燥窒素雰囲気下で押し出し機に加えた。延伸及びテキスチャーリング操作は指示通りに実施した。
【０３１９】
実験室連続フィラメント（ＣＦ）ライン
繊維成形押し出し機は長さ／直径比（Ｌ／Ｄ）３０：１で４個の電気ゾーン加熱器が付いた２５ｍｍ直径の単軸押し出し機である。押し出し機は定量ポンプと焼結金属フィルターをもつスピンパックに接続されている。スピンパックは２４個の丸い穴をもつ繊維紡糸口金に接続されている。フィラメントの流れをクロスフロー急冷室を通しそれから２個の加熱ゴデット上に巻き取る。２４本のフィラメントヤーンを標準巻き取り機を使用する円筒状パッケージ上に巻きつける。
【０３２０】
パイロットバルク連続フィラメント（ＢＣＦ）ライン
押し出し機は長さ／直径比（Ｌ／Ｄ）３０：１で４個の電気ゾーン加熱器が付いた３０ｍｍ直径単軸押出し機である。押し出し機は定量ポンプと焼結金属フィルターをもつスピンパックに接続されている。スピンパックは７２個の３突起形状をもつダイ（変性比が１．８−２．３の範囲の繊維を作り出す）をもつ繊維紡糸口金を装備している。押出し機の１−４のゾーン（供給口から供給末端まで）の温度、スピンパックの温度、そして生成物の熔融温度は熱電対手段で測定した。押出しに続き、熔融繊維はクロスフロー急冷室を通り固体化して未延伸連続フィラメントヤーンとなる。急冷は特に断りがなければ１５℃空気中である。未延伸の急冷された連続フィラメントヤーンをそれぞれが実施例で与えられる温度と表面速度をもつ遅い第一のゴデットロールと速い第二のゴデットロールの間で延伸する。延伸ヤーンをそれから熱空気テクスチャライザー管に導入しそこで加熱された乱流空気に曝されることで連続フィラメントからバルク連続フィラメント（ＢＣＦ）に転換させる。嵩高となったＢＣＦヤーンの“栓流”はテクスチャライザー管を出て多孔の冷却ドラムに入り、冷却ドラムは真空によって熱テクスチャ栓流を通して周囲の空気を吸い込む。冷却されたＢＣＦヤーンの束を絡まりヤーンを作るために織り交ぜジェットに移す。それからＢＣＦヤーンを１０００ｍ／分で操作する標準巻き取り機を使用する円筒状パッケージ上に巻きつける。
【０３２１】
パイロット連続フィラメント（ＣＦ）ライン
押し出し機は長さ／直径比（Ｌ／Ｄ）３０：１で４個の電気ゾーン加熱器が付いた３０ｍｍ直径単軸押出し機である。押し出し機は定量ポンプと焼結金属フィルターをもつスピンパックに接続されている。スピンパックは７２個の０．２５ｍｍ径の円形ダイをもつ繊維紡糸口金を装備している。押出し機の１−４のゾーン（供給口から供給末端まで）の温度、スピンパックの温度、そして生成物の熔融温度は熱電対手段で測定した。押出しに続き、熔融繊維はクロスフロー急冷室を通り固体化して未延伸連続フィラメントヤーンとなる。急冷は特に断りがなければ１５℃空気中である。未延伸の急冷された連続フィラメントヤーンをそれぞれが実施例で与えられる温度と表面速度をもつ遅い第一のゴデットロールと速い第二のゴデットロールの間で延伸する。延伸ヤーンをそれから標準巻き取り機を使用する円筒状パッケージ上に巻きつける。
【０３２２】
コマーシャルバルク連続フィラメント（ＢＣＦ）ライン
カーペット工業に共通の商業規模のＢＣＦ紡糸ラインで繊維を紡糸した。紡糸ラインは長さ／直径比（Ｌ／Ｄ）３０：１で５個の電気ゾーン加熱器が付いた７５ｍｍ直径単軸押出し機３台を使用する。各押し出し機は定量ポンプと焼結金属フィルターをもつスピンパックを装備している。スピンパックは５７個の３葉突起形状ダイをもつ繊維紡糸口金を装備している。各押し出し機の１−５のゾーン（供給口から供給末端まで）の温度勾配、スピンヘッド温度、そしてポリマー熔融温度は実施例中で与えられる。押出しに続き、熔融繊維はクロスフロー急冷室を通り固体化して未延伸連続フィラメントヤーンとなる。急冷は特に断りがなければ１５℃空気中である。未延伸の急冷された連続フィラメントヤーンをそれぞれが実施例で与えられる温度と表面速度をもつ遅い第一のゴデットロールと速い第二のゴデットロールの間で延伸する。
【０３２３】
延伸ヤーンをそれから熱空気テクスチャライザー管に導入しそこで加熱された乱流空気に曝されることで連続フィラメントからバルク連続フィラメントに転換させる。嵩高となったＢＣＦヤーンの“栓流”はテクスチャライザー管を出て多孔の冷却ドラムに入り、冷却ドラムは真空によって熱テクスチャ栓流を通して周囲の空気を吸い込む。冷却されたＢＣＦヤーンの束をタフトカーペットヤーンへの引き続く工程のために十分な絡まりを作るために織り交ぜジェットに移す。それからヤーンを標準巻き取り機を使用する円筒状パッケージ上に巻きつける。
【０３２４】
未処理材料
実施例で使用した未処理材料は以下のとおりである。
成分（ａ）
Ｎ−６ＲＶ１５１：ナイロン−６ホモポリマー（ＣＡＳ ２５０３８−５４−４）
相対粘度１５１、最大水分０．０８ｗｔ％、最大抽出可能水分１．５ｗｔ％、チップ寸法２．５ｘ２．５ｍｍをもつＤＳＭ社から市販されているタイプ２７００である。
【０３２５】
Ｎ−６ＲＶ３８：ナイロン−６ホモポリマー（ＣＡＳ ２５０３８−５４−４）
相対粘度３８をもつＤＳＭ社から市販されている商標名アクロンＫ２２２−Ｄである。
【０３２６】
Ｎ−６，６ＲＶ５０：ナイロン−６，６ホモポリマー（ＣＡＳ ３２１３１−１７−２）
Ｔｍ＝２６７℃をもつシグマーアルドリッチ社から市販されている製品番号１８１１２９である。
【０３２７】
Ｎ−６，６ＲＶ２５０：ナイロン−６，６ホモポリマー（ＣＡＳ ３２１３１−１７−２）
相対粘度２３０−２８０をもつ高粘度押し出しグレードのシグマーアルドリッチ社から市販されている製品番号４２９１７１である。
【０３２８】
Ｎ−６／６，６：ナイロン−６／ナイロン−６，６コポリマー（ＣＡＳ ２４９９３−０４−２）
Ｔｍ＝２５０℃をもつシグマーアルドリッチ社から市販されている製品番号４２９２４−４である。
成分（ｂ）
ＳＰＳ１：シンジオオタクチックポリスチレンホモポリマー
目的Ｍｗ＝２５０，０００（ゲルパーミエーションクロマトグラフィー）、メルトフローレート（ＭＦＲ）＝１３ｇ／１０分（ＡＳＴＭ Ｄ−１２３８：条件３００℃、１．２ｋｇ荷重）、そしてシンジオオタクチー＝９６％以上のダウケミカル社から市販されている、商標名クエストラＱＡ１０１である。
【０３２９】
ＳＰＳ２：シンジオオタクチックポリスチレンホモポリマー
目的Ｍｗ＝３５０，０００（ゲルパーミエーションクロマトグラフィー）、メルトフローレート（ＭＦＲ）＝４ｇ／１０分（ＡＳＴＭ Ｄ−１２３８：条件３００℃、１．２ｋｇ荷重）、そしてシンジオオタクチー＝９６％以上のダウケミカル社から市販されている、商標名クエストラＱＡ１０２である。
【０３３０】
ＳＰＭ１：スチレンと７ｗｔ％のｐ−メチルスチレンとのシンジオオタクチックコポリマー
目的Ｍｗ＝３２５，０００（ゲルパーミエーションクロマトグラフィー）をもつダウケミカル社から市販されている、商標名クエストラＭＡ４０６である。
【０３３１】
ＳＰＭ２：スチレンと４ｗｔ％のｐ−メチルスチレンとのシンジオオタクチックコポリマー、Ｔｃ＝２５７℃
ＳＰＭ３：スチレンと０．７ｗｔ％のｐ−メチルスチレンとのシンジオオタクチックコポリマー、
ＳＰＭ４：スチレンと１０ｗｔ％のｐ−メチルスチレンとのシンジオオタクチックコポリマー、Ｔｃ＝２４６℃
成分（ｂ）及び／又は成分（ｃ）
ＭＧＳＰＭ１：スチレンとｐ−メチルスチレンとのマレイン酸変性シンジオオタクチックコポリマー、
９５ｗｔ％のＳＰＭ１、３．０ｗｔ％のフマール酸、２．０ｗｔ％の２，３−ジメチル−２，３−ジフェニルブタン、及びフリーラジカル開始剤をＺＳＫ４０二軸押し出し機で３００℃で熔融混合して調製した。 得られた無水物基のグラフト含有量はフーリエ変換赤外分析（ＦＴＩＲ）で０．５ｗｔ％であった。
【０３３２】
ＭＧＳＰＭ２：スチレンとｐ−メチルスチレンとのマレイン酸変性シンジオオタクチックコポリマー、
９５ｗｔ％のＳＰＭ２、３．０ｗｔ％のフマール酸、２．０ｗｔ％の２，３−ジメチル−２，３−ジフェニルブタン、及びフリーラジカル開始剤をＺＳＫ４０二軸押し出し機で３００℃で熔融混合して調製した。 得られた無水物基のグラフト含有量はフーリエ変換赤外分析（ＦＴＩＲ）で０．３ｗｔ％であった。
【０３３３】
ＭＧＳＰＭ３：スチレンとｐ−メチルスチレンとのマレイン酸変性シンジオオタクチックコポリマー、
９５ｗｔ％のＳＰＭ３、３．０ｗｔ％のフマール酸、２．０ｗｔ％の２，３−ジメチル−２，３−ジフェニルブタン、及びフリーラジカル開始剤をＺＳＫ４０二軸押し出し機で３００℃で熔融混合して調製した。得られた無水物基のグラフト含有量はフーリエ変換赤外分析（ＦＴＩＲ）で０．２ｗｔ％であった。
【０３３４】
ＭＧＳＰＳ２：マレイン酸変性シンジオオタクチックホモポリマー、
９５ｗｔ％のＳＰＳ２、３．０ｗｔ％のフマール酸、２．０ｗｔ％の２，３−ジメチル−２，３−ジフェニルブタン、及びフリーラジカル開始剤をＺＳＫ４０二軸押し出し機で３００℃で熔融混合して調製した。得られたカルボニル基のグラフト含有量はフーリエ変換赤外分析（ＦＴＩＲ）で０．３４ｗｔ％であった。
【０３３５】
ＦＡＰＰＯ１：フマール酸グラフト変性ポリ（２，６−ジメチル−１，４−フェニレンエーテル）（ＰＰＯ）
グラフトしたフマール酸０．８ｗｔ％を含む。
【０３３６】
ＦＡＰＰＯ２：フマール酸グラフト変性ポリ（２，６−ジメチル−１，４−フェニレンエーテル）（ＰＰＯ）
グラフトしたフマール酸１．６ｗｔ％とシンジオオタクチックポリスチレン（ＳＰＳ１）１０ｗｔ％を含む。
【０３３７】
ＳＭＡ１：アタクチックスチレン／無水マレイン酸コポリマー（ＳＭＡ）（ＣＡＳ ９０１１−１３−６）
メルトインデックス＝１．７ｇ／１０分（ＡＳＴＭ Ｄ−１２３８、２３０℃／２．１６ｋｇ）をもちそして無水マレイン酸７ｗｔ％を含む。
【０３３８】
ＳＭＡ２：アタクチックスチレン／無水マレイン酸コポリマー
ＦＴＩＲ分析による無水マレイン酸含量０．２ｗｔ％を含む。
【０３３９】
ＳＭＡ３：アタクチックスチレン／無水マレイン酸コポリマー
ＦＴＩＲ分析による無水マレイン酸含量１．５ｗｔ％を含む。
【０３４０】
ＳＭＡ４：アタクチックスチレン／無水マレイン酸コポリマー
ＦＴＩＲ分析による無水マレイン酸含量０．５ｗｔ％を含む。
【０３４１】
上記の成分は追加的に少量の１以上の、抗酸化剤、潤滑剤、アンチ−ブロック剤、安定剤、核剤及び顔料のような添加剤を含む。
試験方法
特に指示がない限り、以下の試験方法が使用される。
【０３４２】
堅さはＡＳＴＭ Ｄ３８２２−９６に従って測定される。
【０３４３】
伸びはＡＳＴＭ Ｄ３８２２−９６に従って測定される。
【０３４４】
弾性率（ヤングモジュラス）はＡＳＴＭ Ｄ３８２２−９６に従って測定される。
【０３４５】
収縮は次式に従ってヒートセット前後の線密度の差異（デニール）から計算される：
収縮＝１００ｘ［（Ｄａｈｓ−Ｄｂｈｓ）／Ｄｂｈｓ］、
ここで、Ｄｂｈｓはヒートセット前の試料のデニールでＤａｈｓはヒートセット後の試料のデニールである。
【０３４６】
相対粘度はキャピラリー粘度計（キャノンウベロード、ＩＩ−タイプ、寸法２００Ａ）を使用し、２５℃に設定された一定温度浴中に粘度計を漬けて決定される。ポリマー溶液と溶媒の流れ時間はキャピラリー粘度計中で測定される。相対粘度は式：ηｒｅｌ．＝Ｔ／Ｔ_０ によって決定される。
ここでηｒｅｌ．＝相対粘度、Ｔ＝溶液の流れ時間（秒）、Ｔ_０ ＝溶媒の流れ時間（秒）。
【０３４７】
冷却時の結晶化温度（Ｔｃ）はＤＳＣで測定される。約１０ｍｇのポリマーペレットをアルミニウム製ＤＳＣパン中に計量し（０．００１ｍｇ）、ふたをしてそしてＴＡインスツルメンツモデル９２０オートサンプラー及びＴＡインスツルメンツユニバーサルＶ３．０Ｅソフトウエアを装備したＴＡインスツルメンツ差分走査熱量計、モデル９１０の試料セル中に置いた。ふた付きで空の同定用アルミニウムパンを対照セル中に置いた。試料を２０℃／分の速度で３２０℃まで加熱し、３２０℃で５分間保持し、それから２０分間で１５０℃まで冷却した。熱流（ワット／ｇ）：温度のプロットが得られる。
【０３４８】
以下の転移点（温度）が得られる：
Ｔｇ＝ガラス転移点、秒次元の転移
Ｔｃｈ＝固体結晶を加熱時の結晶化熱流ピーク温度、一次発熱転移
Ｔｍ＝固体結晶を加熱時の融解熱流ピーク温度、一次吸熱転移
Ｔｃ＝融解結晶を冷却時の結晶化熱流ピーク温度、一次発熱転移
前述の方法で試験した種々の材料のＴｃを表１に示す。
【０３４９】
【表１】

【実施例１】
【０３５０】
実施例１−３、レーザー光散乱によるＡ及びＢ−光沢の決定
バルク連続フィラメント繊維試料の光沢を評価するために５人の光沢審査員を使用した。
ＢＣＦ繊維を濃いオリーブグリーンに染色し、明るい白色等級ＢＣＦ繊維試験よりは易しい光沢評価を行った。５点の標準を数値等級スケールとして使用した。１等級（１）は典型的には羊毛繊維に見られると同様のフルダル（完全にくすんだ色）を示すのに使用された。５等級（５）はナイロン６試料のフルブライト(完全光沢)を示すのに使用された。２等級（２）、３等級（３）、そして４等級（４）をもつ標準は中間点として選ばれた。それぞれの繊維試料をここで開示したレーザー光散乱技術でもまた測定した。
【０３５１】
表２に開示した組成物を調製しそして繊維に紡糸した。実施例１及び２の組成物はマスターバッチ法を使用して４０ｍｍ二軸押し出し機で調製した。実施例３とＡはシングルパス法を使用して４０ｍｍ二軸押し出し機で調製した。
【０３５２】
【表２】

上記の組成物はパイロットＢＣＦ紡糸ラインを使用して７２本のフィラメントを含み約１２００デニールをもつヤーンに紡糸した。ヤーンはフルブライトからフルダルの範囲の光沢を示した。ヤーンは以下の光沢ランクで規定された：
５＝ナイロン６＝フルブライト(完全光沢)比較例Ｂ
４＝比較例Ａ
３＝実施例２
２＝実施例１
１＝フルダル(完全なくすみ)、実施例３
さらに、市販のＢＣＦ試料をレーザー光散乱によって分析した。これらの同じＢＣＦ繊維をまた濃いオリーブグリーンに染色しそして光沢審査員によって等級化した。採用された市販試料と対応する審査員による光沢等級は下記の通りであった：
Ｃ１^＊ ＤｕＰｏｎｔ１７１０−９４−０−８９６ＡＳ ＳｅｍｉＤｕｌｌ（光沢審査員等級＝２．９）
Ｃ２^＊ ＤｕＰｏｎｔ１１０５−１３６−０−６１５（光沢審査員等級＝１．８）
Ｃ３^＊ ＤｕＰｏｎｔ１３４０−６８−０−４１６Ａ（光沢審査員等級＝２．２）
Ｃ４^＊ ＤｕＰｏｎｔ１４３０−６８−０−Ｐ１３６９（光沢審査員等級＝４．１）
Ｃ５^＊ ＤｕＰｏｎｔ１４２５−１２４−０−Ｐ１３６５（光沢審査員等級＝１．９）
５点の審査員光沢標準と上記５点の市販ＢＣＦ試料の散乱比を表３に示す。光沢審査員等級とレーザー光散乱比のプロット（それから計算される直線適合性と一緒に）を図１２に示す。レーザー光散乱によって決定される散乱比、Ｒｓ、は光沢審査員によって決定される光沢と反比例の関係にある。特に、光沢＝（−１０．９０６）／Ｒｓ＋７．１６７５はＲ^２ ＝０．９０６５の直線適合性を与える。本発明に従った繊維は４以下の光沢審査員等級とそれに対応する散乱比０．２９以上をもつ。結果を表３に示す。
【０３５３】
【表３】

繊維分析のためのレーザー光散乱技術にさらに確証を与えるために、種々のレベルで公知のつや消し剤、ＴｉＯ_２ 、を含むナイロン６の数点のブレンド物を３０ｍｍ二軸押し出し機でコンパウンド化しそして実験室規模の連続フィラメントラインで本質的に前に述べそして分析したのと同じ条件を使用して繊維に成形した。組成物の詳細と結果を表４とまた図１３に示す。
【０３５４】
【表４】

ＴｉＯ_２ に対する散乱比、Ｒｓ、のプロットは良好な相関を示す。特に、次式：Ｒｓ＝１６４．６ｗ＋０．２３６４、ここでｗはＴｉＯ_２ の含有量（重量％）、への適合性は二乗相関係数Ｒ^２ ＝０．９８９５を与える。図において、散乱比０．２９はＴｉＯ_２ レベル
３２５ｐｐｍに対応することがわかる。
【０３５５】
実施例４−１５及びＥ 光沢及び堅さに及ぼす分散相レベルの影響
光沢及び堅さに及ぼす分散相含有量の影響を種々の組成物で測定した。実施例４−１５の組成物は表５に与えられる組成物を得るためにマスターバッチ法を使用して３０ｍｍ二軸押し出し機で調製した。本発明の実施例４−１５及び比較実施例Ｅの繊維を表６に与えられる条件を使用して実験室規模の連続フィラメントラインで紡糸した。
【０３５６】
【表５】

【０３５７】
【表６】

繊維の堅さ、弾性率、そして散乱比を表７に示す。０．２９の散乱比下限に基づくと、この技術はＦＡＰＰＯ１で相溶化するとＳＰＳ２レベル２％の光沢そしてＭＧＳＰＭ１相溶化剤を使用すると合計ＳＰＳレベル（ＳＰＳ２＋ＭＧＳＰＭ１）３％の光沢を示す。繊維紡糸のための堅さと能力に基づきこの技術のために要求される上限組成物は３５％のＳＰＳ２又はＳＰＳ２＋ＭＧＳＰＭ１である。より好ましいのは３０％以下のＳＰＳ２又はＳＰＳ２＋ＭＧＳＰＭ１そして最も好ましいのは２０％以下のＳＰＳ２又はＳＰＳ２＋ＭＧＳＰＭ１である。
【０３５８】
繊維の弾性率は、改良された耐久性、良好な寸法安定性、改良されたしわ回復性，又は改良された剛性に導くことができる分散相の性質を強化するＳＰＳ２含有量の増加と共に増大する。
【０３５９】
【表７】

既知長さの前述の繊維の一スケイン（かせ）を沸騰水に１５分間漬けた。繊維を取り出しそして７２時間空気乾燥にかけた。スケインの長さを再測定しそして一次スケイン収縮率を計算した。繊維はそれから物理的性質の試験をした。結果を表８に示す。
【０３６０】
一次スケイン収縮率は次のようにして測定される。試料をフックに吊るしそして２７５ｇの錘をスケインにぶら下げた。沸騰水に曝す前の長さを測定しそしてＬ_ｂ として記録した。沸騰水に浸漬し乾燥後の長さを測定しそしてＬ_ａ として記録した。一次スケイン収縮率はそれから次式に従って計算される。
【０３６１】
一次スケイン収縮％（ＬＳＳ）＝（（Ｌ_ｂ −Ｌ_ａ ）／Ｌ_ｂ ）ｘ１００
沸騰水暴露による一次スケイン収縮率は、カーペットにおける光学的縞筋の減少、織物の製造、染色、及び仕上過程における寸法安定性の改良、家庭での洗濯及び業者の洗濯過程での寸法安定性の改良、織物製造過程における収率の改善、ヒートセットの必要性を減少させる能力、及び衣服の形状維持能力を含む織物用途における多くの優位性をもつ本発明の寸法安定性を実証するＳＰＳ２含有量の増加と共に低下する。表７と表８の弾性率を比較すると、繊維の弾性率は沸騰水に曝された後でも良好に維持され、それは着心地や形状の維持が熱水に曝されるときに重要となる織物用途で優位性を発揮する。
【０３６２】
【表８】

実施例１６−２７ 光沢及び散乱比の吸蔵粒子径との関係
本発明に従った繊維は種々のブレンド物を典型的な紡糸条件を使用してパイロットＢＣＦ紡糸ラインで紡糸、延伸そして仕上げを行うことにより作られた。試料を室温のギ酸中に入れると、ナイロンマトリックスは溶解するが、ギ酸による影響を受けない吸蔵相の微粒子は分散状態が維持された。粒子をろ過し回収した。図１７、は実施例２５に従って作られた繊維中のそのような粒子の典型的な試料の走査電子顕微鏡像（ＳＥＭ）である。そのような繊維の典型的な試料を以下の手順に従って標準粒子径分析ソフトウエアを使用して画像化し解析した。
【０３６３】
繊維試料（０．０１２ｇ）をそれぞれ新しいねじ込みキャップのついた１０ｍｌガラスバイアルビンに入れた。２ｍｌの濃縮（９５−９７％）ギ酸を各試料バイアルに添加した。バイアルを２０秒間ゆっくりと振ってナイロンを溶解させそして２５℃で４時間静止状態に保持した。溶液を再度振ってギ酸溶液中にｓＰＳを一様に分散させた。新しい１ｍｌの樹脂製キャピラリーシリンジで各分散液のアリコート（分割量）（０．１ｍｌ）を採取し新しいねじ込みキャップのついた１０ｍｌガラスバイアルビンに入れた。それから４．９ｍｌのギ酸を各バイアルに加え各バイアル中で合計５ｍｌの分散液とした。或る溶液は写真でｓＰＳの分配を見るためにさらに必要なだけ希釈した。希釈分散液を２−３秒ゆっくりと振ってそれから約２ｍｌの溶液をシリンジで採取しそして０．１又は０．０２ミクロン孔径の無機メンブレンフィルターでろ過した。ろ過残査をギ酸で３回洗浄し残留ナイロンを除去した。
【０３６４】
分散したｓＰＳ粒子が集められたフィルターを簡単に空気乾燥しそしてアルミニウム製の走査電顕スタブに取り付けた。測定試料を高解像度クロムコーター中でクロムスパッターした。このようにして調製された試料を走査電子顕微鏡（日立（株）から市販されている日立Ｓ−４１００ＦＥＧ走査電子顕微鏡）で画像化した。４ＰＩ Ａｎａｌｙｓｉｓ社から市販されている４ＰＩデジタル画像システムで電子的に４０９６ｘ４０９６ピクセルの画像を採取した。
【０３６５】
コンピューター画像解析ソフトウエアを使用してｓＰＳ粒子の形状とサイズを解析した（シオン社から市販されている、ウインドウズオペレーティングシステムのパソコン用シオン画像解析アプリケーションソフトウエア） 。粒子は画像上でマニュアルで捕らえた。
それから画像を、各粒子の投影形状に楕円（長軸及び短軸）を適用して粒子の投影面積と周囲長さを測定するために使用した。たいていの粒子はモデルにうまく適合する楕円状又は長円球形状の外観をしているが、いくつかの粒子は投影形状でより長方形状（３次元的により円筒形状を示す）であることが認められたので、マニュアルで長さと幅の長方形モデルでの再適合を行った。試料によるが、４００−４０００粒子が各試料で解析された。用語短軸と投影短軸はここでは用語直径及び粒子径と置き換え可能なものとして使用されている。同様に、長軸と投影長軸はここでは用語長さ及び粒子長さと置き換え可能なものとして使用されている。
【０３６６】
ｓＰＳ粒子の長軸と投影短軸（直径）の平均値は、粒子の数、投影面積、評価された粒子体積、そして投影短軸の重みに基づいて計算した。重量平均決定の一般式は次式を使用した：
【０３６７】
【化２】

ここでｘ_ｗ はｗの重み係数（例えば、粒子体積）に基づいて計算された平均量（例えば、直径）、ｗ_ｉは粒子ｉの各重み係数（例えば、粒子ｉの評価体積）、そしてｘ_ｉは平均化された粒子寸法（例えば、粒子ｉの直径）である。体積重み平均から、粒子径の累積的な可能性は次式で計算された：
【０３６８】
【化３】

ここでＦ（ｊ）は粒子ｊの累積的な可能性、そしてＶ_ｉ は粒子ｉの評価体積であり、そして粒子は、粒子１は最小直径をもちそして粒子Ｎは最大直径をもつように最小径から最大径まで序列化される。この分布に基づいて、この体積基準分布の９９番目の百分位数の直径をもつ粒子を計算することが可能である。この粒子径は（Ｄ９９）と呼ばれる。Ｄ９９の物理的な意味は体積基準分布の９９番目の百分位数の粒子直径、即ち、評価合計粒子体積の９９％がＤ９９より小さな直径の粒子によって占有されていることを意味する。結果として、Ｄ９９は最大直径の概略値である。真の最大直径は無限の測定セットを必要とし、結果として、測定や解析のための実用的な量とはならない。Ｄ９９と体積平均粒子径を表９に示す。
【０３６９】
【表９】

繊維形成に使用する熱可塑性アロイはマスターバッチ法を使用して３０ｍｍ又は４０ｍｍ二軸押し出し機でコンパウンド化した。例外は、実施例２５で、シングルパス法を使用して４０ｍｍ二軸押し出し機でコンポウンド化した。全ての材料はパイロット規模のＢＣＦ紡糸ラインで繊維に成形した。全ての材料は約１０％の結晶性シンジオタクチックポリマー相（ＭＧＳＰＭ１を含む試料を包含する）を含む。体積平均の投影粒子短軸径と専門審査員によって決定されたＢＣＦヤーンの光沢のプロットを計算による適合直線と共に図１４に示す。直線関係（ｙ＝０．２５ｘ＋１．４）は体積平均の投影粒子短軸径（ｙ）と審査員によって測定された光沢（ｘ）の間に０．７９の相関係数の二乗、Ｒ^２ をもつことがわかった。特に、８−１４重量％の成分（ｂ）のレベルにおいて０．２０μｍより大きい、好ましくは０．２５μｍより大きい吸蔵粒子の体積平均短軸径が光沢の減少した繊維を製造するために望ましい。また、散乱比（ｘ−軸）によって測定されるときのＢＣＦヤーンの光沢を使用して同様の情報を図１５にプロットすると、体積平均の投影粒子短軸径（ｙ）と繊維の散乱比（ｘ）の間に０．６５の相関係数の二乗、Ｒ^２ をもつ直線相関（ｙ＝４．５ｘ−１．３）を得る。０．３３より大きい、より好ましくは０．３５より大きい前述の方法で決定される散乱比をもつ繊維は本発明にとって特に望ましい。
【０３７０】
堅さもまた投影粒子短軸径の９９番目の百分位数(体積百分位数基準)、それは最大粒子径の近似値である、と相関があることが見出された。堅さの関数としてプロットすると相関が観察される。特に、次式の直線関係が得られた：Ｄ９９粒子径＝−１．３ｘ＋４．２、
ここでｘは堅さ（ｇ／デニール）で、Ｒ^２ ＝０．６４の相関係数の二乗値をもつ。結果を図１６に示す。
【０３７１】
良好な繊維紡糸性能は少なくとも部分的には許容できる壊裂ダイナミックスをもつ繊維が生じていると思われる。この性質に影響を与える一因子は最大吸蔵粒子の短軸径であると思われる。このように、示された堅さとＤ９９短軸粒子径との相関関係は良好な繊維紡糸特性の指標となる。特に、３．０μｍより小さいＤ９９が非常に望ましい。
【０３７２】
実施例２８−３８ 種々の相溶化剤と２成分、自己相溶化ブレンド物の使用
表１０の組成物は実施例２８−３６の場合はマスターバッチ法を使用して３０ｍｍ又は４０ｍｍ二軸押し出し機で、そして実施例３７−３８の場合はシングルパス法を使用してコンパウンド化した。得られたブレンド物を、実施例２８−３６の場合は実験室規模の連続フィラメントラインでそして実施例３７−３８の場合はパイロット規模のＢＣＦ紡糸ラインで繊維に紡糸した。ＢＣＦ試料を光沢審査員によって光沢の等級付けをした。実施例２８−３６は１０％のＳＰＳ２を含んだ。実施例３７−３８は２成分のみを含んだ：ナイロン６とスチレンとｐ−メチルスチレンとのマレイン酸変性シンジオタクチックコポリマー。
【０３７３】
【表１０】

実施例３９−４６、Ｆ 黄色指数、ＹＩ試験
ＳＰＳ２、ナイロン−６、及び無水マレイン酸グラフトシンジオタクチックスチレン／ｐ−メチルスチレンコポリマー（ＭＧＳＰＭ１）、無水マレイン酸グラフトシンジオタクチックポリスチレン（ＭＧＳＰ２）、アタクチックスチレン／無水マレイン酸コポリマー（ＳＭＡ４）、又はフマール酸グラフトポリプロピレンオキサイド(ＦＡＰＰＯ１又はＦＡＰＰＯ２)を含む種々の相溶化剤(成分（ｃ）)の種々の重量比のドライ回転ブレンド物をマスターバッチ法を使用して３０ｍｍ又は４０ｍｍ二軸押し出し機でコンパウンド化した。さらに、ナイロンＮ−６成分（ａ）と無水マレイン酸グラフトスチレン／ｐ−メチルスチレンコポリマーのドライ回転ブレンド物をシングルパス法を使用して二軸押し出し機でコンパウンド化した。
【０３７４】
【表１１】

【０３７５】
実施例Ｆａ，３９ａ，４１ａ，４３ａ，４４ａ 未染色繊維の光安定性
上記の異なった組成物のＢＣＦ試料をＡｍｅｒｉｃａｎ Ａｓｓｏｃｉａｔｉｏｎ ｏｆ Ｃｈｅｍｉｓｔｓ ａｎｄ Ｃｏｒｏｒａｎｔｓ（ＡＡＴＣＣ）試験方法１６−１９９８、オプションＥに従ってＵＶ光に対する色安定性試験にかけた。試験のために３層厚みの白カードに巻き取った。全ての試験はＰｒｏｆｅｓｓｉｏｎａｌ Ｔｅｓｔｉｎｇ Ｌａｂｏｒａｔｏｒｙ ｏｆ Ｄａｌｔｎ ＧＡにより行った。試料を８０及び１６０時間高圧水銀ディスチャージライトに曝し、それから曝露のない対照試料と比較した。Ｄ６５，１０度色変化、△Ｅの結果を表１８に示す。表において、反射光の色変化、△Ｅ、を次式：△Ｅ＝(Ｌ_１−Ｌ_２)^２ ＋(ａ_１−ａ_２)^２ ＋(ｂ_１−ｂ_２)^２ ）^１／２ 、で計算した。
ここで１は初期状態そして２は最終状態、そしてＬ、ａ及びｂはそれぞれ赤／緑及び黄色／青の光度又は強度に関する反射光の測定値である。
【０３７６】
色変化は相溶化剤としてグラフトしたポリフェニレンオキサイドポリマーを使用した試料はナイロン比較例及びＭＧＳＰＳ２とＭＧＳＰＳ１相溶化剤を使用した実施例に比較して許容できない色定着性をもつことを示している。
【０３７７】
【表１２】

実施例４７とＧ 細いデニールで防止した衣類用繊維と織物試料のデモ
ＳＰＳ２、ＭＧＳＰＭ１、及びナイロンＮ−６の１０：３：８７重量比のブレンド物を
マスターバッチ法を使用して４０ｍｍ二軸押し出し機でコンパウンド化した。得られたブレンド物を以下の条件を使用してパイロット規模の連続フィラメントラインで紡糸した：
定量ポンプ供給量：１４．７ｇ／分
押し出し機バレル温度勾配：２９０℃／３２５℃／３２５℃／３１０℃
スピンヘッド温度：３１０℃
融点：３０２℃
充填圧力：３６３ｐｓｉｇ（２．６ＭＰａ）
クエンチング：１４℃空気中
低速ゴデット：７５℃及び４３４ｍ／分
高速ゴデット：１７５℃及び１３００ｍ／分
延伸比：３：１
ヤーンデニール：１００／７２、１．４ｄｐｆ
得られた１００／７２ヤーンの堅さは６５％伸びで２．４ｇ／デニールである。
【０３７８】
比較例Ｇの試料は純粋なナイロンＮ−６を使用して比較条件下で作った。押し出し機は長さ対直径比（Ｌ／Ｄ）が２４の３８ｍｍ径の単軸押し出し機で電気ゾーンヒーターを装備している。各押し出し機は定量ポンプと焼結金属フィルターをもつスピンパックに接続されている。スピンパックは６４個の０．３ｍｍ径の円形状ダイをもつ繊維紡糸口金を装備している。繊維紡糸条件は以下の通りである：
定量ポンプ供給量：８．３ｇ／分
押し出し機バレル温度勾配：２６０℃／２７５℃／２６０℃
スピンヘッド温度：２６０℃
融点：２５８℃
充填圧力：３８０ｐｓｉｇ（２．６ＭＰａ）
クエンチング：１３℃空気中
低速ゴデット：４０℃及び２３３ｍ／分
高速ゴデット：９０℃及び７５０ｍ／分
延伸比：３．２：１
ヤーンデニール：１００／６４、１．５６ｄｐｆ
得られた１００／６４ヤーンの堅さは７５％伸びで４．０ｇ／デニールである。
【０３７９】
２本の繊維を２撚り／インチで撚りそしてそれから４本の通糸つり索サテン織り構造の織物に織った。グレージュ繊維を沸騰水に浸漬しそれから空気乾燥させた。沸騰水曝露の前後の縦糸とフィル（ｆｉｌｌ）方向の寸法を測定した。それから収縮を縦糸とフィル方向の両方で計算した。結果を表１３に示す。
【０３８０】
【表１３】

得られた織物試料の前述の方法で処理後の試験は本発明(実施例４７)にしたがって作られた織物が比較例の織物に較べより満足できる手触り(柔らかな感触)と良好な範囲（よりくすんだ）をもつことを示した。
【０３８１】
実施例４８ マスターバッチブレンド及び拡張流れ混合を使用した繊維の製造
ＳＰＳ２とＦＡＰＰＯ１（０．８％のグラフトフマール酸を含むフマール酸変性ポリフェニレンオキサイド）の重量比７８．７４：２１．２６のドライ回転ブレンド物を２９０℃でワンパスでコンパウンド化し、円筒状のストランドに押し出しそして水浴中で室温に冷却した。ストランドを水フリーでブローしそして長さ２．８ｍｍで直径２．１ｍｍのチップに切断した。このチップ(マスターバッチチップと呼ぶ)を空気循環乾燥機中で９０℃で８時間乾燥し水分レベルを０．０８％以下とした。ナイロンＮ−６と前述のマスターバッチチップの重量比８７．３：１２．７のドライ回転ブレンド物をポリマー粒子製造用の図６に示すような６３．５ｍｍ径単軸押し出し機に供給した。押し出し機、６０、は単軸、６９、温度調節ゾーン、６１，６２、６３をもつ内部円筒状混合機本体、６５、からなる。入り口から出口までのゾーンの設定温度はそれぞれ２６０、３１５、そして３１５℃であった。移送ライン、６４、混合機本体、６５、及び円筒状ダイ、６６、を２９０℃に調節した。押し出し機の回転数を５０回転に設定し、正味の流速１３．６１ｋｇ／ｈｒで系内に供給した。ナイロン６とマスターバッチチップの混合を改善するために、押し出し機を出る熔融ポリマーをインライン拡張流れ混合装置、６７、（Ｅｘｔｅｎｓｉｏｎａｌ Ｆｌｏｗ Ｍｉｘｅｒ，Ｉｎｃ．Ｍｉｓｓｉｓｓａｕｇａ，Ｏｎｔａｒｉｏから市販されているモデルＥＦＭ−２５０スタティックミキサー）に供給した。混合装置の可変ギャップは３ｍｍに設定した。混合装置を出た材料を円筒状ストランド(糸)に押し出しそして水浴、６８で室温まで冷却した。ストランドをおおよそ長さ４ｍｍそして直径３ｍｍのチップに切断した。得られたペレットを空気循環乾燥機中で乾燥し水分レベルを０．０８％以下としてパイロット規模のＢＣＦ紡糸ラインで紡糸した。
【０３８２】
繊維の成形条件は以下の通りであった：
定量ポンプ供給量：１３５ｇ／分
押し出し機バレル温度勾配：３００℃／３２５℃／３２５℃／２９５℃
スピンヘッド温度：２９５℃
融点：２９０℃
充填圧力：７９５ｐｓｉｇ（５．６ＭＰａ）
クエンチング：１５℃空気中
低速ゴデット：７５℃及び３３４ｍ／分
高速ゴデット：１６０℃及び１０００ｍ／分
延伸比：３：１
テキスチャライザー温度と圧力：１９０℃と８０ｐｓｉｇ（０．６３ＭＰａ）
織り交ぜ圧力：４５ｐｓｉｇ（０．４０ＭＰａ）
ヤーンデニール：１００／６４、１．５６ｄｐｆ
得られたＢＣＦヤーンは延伸、テキスチャライジング、空気織り交ぜ及び巻き取りの後で、７２本のヤーン束に対して１１９７の合計デニールをもっていた。得られた１１９７／７２ヤーンの堅さは２．５ｇ／デニールである。光沢審査官等級は３．６であった。
【０３８３】
繊維紡糸装置はまた、実質的に前の項で記載したような拡張混合機、又はスタティックミキサーを押し出し機とスピンパックとの間に組み込むことができることは理解されるであろう。そように変更した繊維紡糸装置では、繊維の熔融押し出しの過程で種々の成分を合体させることによって、全ての成分のブレンド物又はアロイの初期コンパウンド化が必要ない程に、成分（ａ）中に成分（ｂ）及び成分（ｃ）の予備ブレンドしたペレットの十分な分散を達成することができる。
【０３８４】
実施例４９ ２成分繊維紡糸
ナイロンＮ−６、ＳＰＳ２及びＦＡＰＰＯ１（０．８％のグラフトフマール酸を含むフマール酸変性ポリフェニレンオキサイド）の重量比８７．３：１０：２．７のドライ回転ブレンド物を二軸押し出し機中でワンパスでコンパウンド化しそして乾燥した。
【０３８５】
２成分(芯／鞘)繊維は以下の紡糸条件で成形された。長さ対直径比（Ｌ／Ｄ）が３０：１で４個の電気ゾーンヒーターを装備している２台の単軸、３０ｍｍ径押し出し機（１台は鞘に使用されるブレンド物のためにそしてもう１台は芯として使用されるナイロン６を練るために）を使用した。各押し出し機は定量ポンプと焼結金属フィルターをもつスピンパックを装備している。スピンパックは７２個の３葉突起形状ダイをもつ繊維紡糸口金を装備しており、それぞれが３葉突起形状の孔で芯−鞘、２成分、共押し出し繊維を作ることができる。各押し出し機の１−４のゾーン（供給口から供給末端まで）とスピンの温度は熱電対によって測定される。各定量ポンプは６８ｇ／分で送給した。押し出し機バレル温度勾配は２９０℃／３２０℃／３１０℃／３００℃、ナイロン押し出し機バレル温度勾配は２６０℃／２８０℃／２７５℃／２７５℃、スピンヘッド温度は３００℃であった。充填圧力は７９５ｐｓｉｇ（５．６ＭＰａ）であった。鞘(本発明の熱可塑性ブレンド物から作られる)は合計繊維断面の体積で５０％からなり、残りは芯繊維からなる練ったナイロン６である。
【０３８６】
押出しに続き、熔融繊維はクロスフロー急冷室を通り固体化して部分延伸連続フィラメントヤーンとなる。急冷は特に断りがなければ１５℃空気中である。部分延伸の急冷された連続フィラメントヤーンをそれぞれが７５℃と１６０℃の温度をもち、それぞれの表面速度が３３９と９５０ｍ／分をもつ遅い第一のゴデットロールと速い第二のゴデットロールの間で延伸し、延伸比は２．８であった。
【０３８７】
冷却されたヤーンを９５０ｍ／分で操作する標準巻き取り機を使用する円筒状パッケージ上に巻きつける。得られた平らなヤーンは延伸と巻き取り後に７２の３突起フィラメントに対して１２５０合計デニールをもっていた。得られた１２５０／７２ヤーンの堅さは１．９ｇ／デニールであった。
【０３８８】
実施例５０ 商業的規模のＢＣＦ紡糸のデモ
ＳＰＳ２、ＦＡＰＰＯ１、及びナイロンＮ−６の１０：２．７：８７．３重量比のブレンド物をマスターバッチ法を使用して４０ｍｍ二軸押し出し機でコンパウンド化した。得られたブレンド物を以下の条件及び表１４の条件を使用してパイロット規模の連続フィラメントラインで紡糸した：
押し出し機バレル温度勾配：２７５℃，２８８℃，２８５℃，２８５℃，２８５℃
スピンヘッド温度：２８５℃
融点：２８５℃
充填圧力：１１０ｐｓｉｇ（０．８６ＭＰａ）
クエンチング：１６℃空気中
低速ゴデット：７５℃
高速ゴデット：１８０℃
テキスチャライザー温度と圧力：２１０℃と６．０バール（０．６ＭＰａ）
織り交ぜ圧力：３．０バール（０．３０ＭＰａ）
比較例Ｈ １００％成分（ａ） ( ナイロン−６ )
ナイロンＮ−６ポリマーのヤーンを作るために以下の条件及び表１４の条件を使用し、実施例５０の装置を使用して紡糸した。
【０３８９】
押し出し機バレル温度勾配：２４７℃，２５７℃，２５６℃，２５４℃，２５４℃
スピンヘッド温度：２６０℃
融点：２６０℃
充填圧力：１５５０ｐｓｉｇ（１０．８ＭＰａ）
クエンチング：１６℃空気中
低速ゴデット：７５℃
高速ゴデット：１８０℃
テキスチャライザー温度と圧力：２１０℃と６．０バール（０．６ＭＰａ）
織り交ぜ圧力：３．０バール（０．３０ＭＰａ）
比較例Ｉ：
スチロン６８５Ｄ（アタクチックポリスチレン）、ＳＭＡ１、及びナイロンＮ−６の１０：１：８９重量比のブレンド物をシングルパス法を使用して４０ｍｍ二軸押し出し機でコンパウンド化した。得られたブレンドペレットを以下の条件及び表１４の条件を使用してパイロット規模の連続フィラメントラインで紡糸した：
押し出し機バレル温度勾配：２６０℃，２８０℃，２７０℃，２７０℃，２７０℃
スピンヘッド温度：２７０℃
融点：２７０℃
充填圧力：１５００ｐｓｉｇ（１０．４ＭＰａ）
クエンチング：１６℃空気中
低速ゴデット：７５℃
高速ゴデット：１８０℃
テキスチャライザー温度と圧力：２１０℃と６．０バール（０．６ＭＰａ）
織り交ぜ圧力：３．０バール（０．３０ＭＰａ）
表１４のヤーンと紡糸条件を比較すると、比較例Ｈ及びＩに従った繊維及びヤーンと比較して本発明に従った組成物を使用して到達可能な紡糸性には改良が認められる。比較例Ｈ又はＩの繊維と比較して、同じデニール／フィラメントにおいて、実施例５０の繊維は成形し易くそして商業規模の成形装置において高い処理速度で紡糸できた。比較例Ｉは紡糸が難しくそして多くの糸切れを起こしたが、実施例５０の組成物を使用すると糸切れや繊維安定性の問題には遭遇しなかった。
【０３９０】
【表１４】

実施例５１−５３、Ｊ、Ｋ、及びＬ ヒートセット収縮の減少
実施例５１−５３の組成物はマスターバッチ法を使用して４０ｍｍ二軸押し出し機でコンパウンド化した。実施例Ｍの組成物はシングルパス法を使用して４０ｍｍ二軸押し出し機でコンパウンド化した。得られたブレンド物(表１５に示される)をパイロット規模のＢＣＦ紡糸ラインで表１６に与えられた条件を使用して繊維に紡糸した。繊維の走査電顕像を図１ａ(実施例５１)、１ｂ(実施例５２)、１ｃ(実施例５３)、２ａ（Ｋ）、及び２ｃ（Ｍ）に示す。
【０３９１】
【表１５】

【０３９２】
【表１６】

ヒートセットツイストヤーンの熱収縮
比較例Ｋ、Ｌ、及びＭそして実施例５１−５３で製造されたヤーンを、“Ｓ”方向で４．５ターン／インチ（１．７７ターン／ｃｍ）をもつツイストヤーン(撚糸)を作るために、ベルドールモデル４００、ケ−ブル撚り装置でスピンドル速度５２００ｒｐｍ及び巻き取り速度２７．８ｍ／分で撚糸した。それから撚糸をバッチオートクレーブを使用して回転及びヒートセットするために周囲長さ８９インチ(２．３ｍ)のリールに巻いた。ヒートセットを１３２℃で５４分間行った。ヒートセット前後の撚糸のデニールを撚り及びヒートセットヤーンのヒートセット時の収縮と堅さと共に表１７に示す。
【０３９３】
【表１７】

表１７に示されるように、実施例５１ａ−５３ａの繊維で作られたケーブルツイストヒートセットヤーンは比較例Ｌａ、Ｋａ、Ｍａの繊維で作ったヤーンと比較して収縮が少ないことを示している。特に、少なくとも５重量％のシンジオタクチックポリスチレンで作られたツイストヤーンの各実施例は１５％以下の収縮、少なくとも１０重量％のシンジオタクチックポリスチレンで作られたヤーンは１３％以下、そして１５重量％のシンジオタクチックポリスチレンで作られたヤーンは１０％以下の収縮を示した。
【０３９４】
色安定性
実施例５１ｂ、５２ｂ、５３ｂ、及びＪｂ（撚糸５１ｂ−５３ｂが作られたのと同じ方法で撚糸Ｊａによって作られる）の撚り及びヒートセットＢＣＦ繊維試料を以下の染色処方と手順に従って濃いオリーブグリーンにスケイン染色した。繊維試料はランジェリーバッグに入れそして以下の手順に従って洗濯した。
【０３９５】
染料処方
レベル酸染料処方−オリーブグリーン
商標名ダイアシッドイエロー３Ｒ ２００％：０．００３３８ｇ／ｇ繊維
商標名ダイアシッドレッド２Ｂ ２００％：０．０００２ｇ／ｇ繊維
商標名ダイアシッドブルー４Ｒ ２００％：０．００２５６ｇ／ｇ繊維
商標名ダイレブＡＣ ：０．０２ｇ／ｇ繊維
硫酸アンモニウム：０．０２ｇ／ｇ繊維
アンモニア：０．０１ｇ／ｇ繊維
チオ硫酸ナトリウム：０．００２５ｇ／ｇ繊維
商標名ダイレブＡＣ＝ダウケミカル社の商標名ダウファックス２Ａ１の４８％水溶液
商標名ダイアシッドイエロー３Ｒ ２００％＝ダルトンジョージアのダイシステム社から市販されている。
【０３９６】
商標名ダイアシッドレッド２Ｂ ２００％＝ダルトンジョージアのダイシステム社から市販されている。
【０３９７】
商標名ダイアシッドブルー４Ｒ ２００％＝ダルトンジョージアのダイシステム社から市販されている。
【０３９８】
染色手順
１． ３０：１−４０：１のリカー比を与えるために染料に水を加える。
【０３９９】
２． スケインを水と循環浴に加える。
【０４００】
３． 商標名ダイレブＡＣ、硫酸アンモニウム、アンモニア、及びチオ硫酸ナトリウムを秤量しそして染色される繊維の重量に比例して１１０リットルの水に加える。染料浴に加え１５分間循環させる。目的の初期ｐＨは８そして目的の最終ｐＨは６．５−７。
【０４０１】
４． 染色される繊維の重量に比例して染料溶液を加える。
【０４０２】
５． 混合物を撹拌しながら約４５分以上で９３℃に加熱する。
【０４０３】
６． 撹拌しながら１５分間９３℃に保持する。
【０４０４】
７． 浴を冷却しそして冷リンス水を加え、オーバーフローさせ、それから排出する。
【０４０５】
８． 冷水でリンスし、スケインを除去し、そして１２０℃で乾燥する。
洗濯手順
ヤーンをランジェリーバッグに入れた。各ヤーンの２組、各１５ｇを第一の３回洗浄サイクルのために標準住宅用洗濯機に入れた。３回洗浄サイクルの後で、各材料の１ヤーンを取り出しそして他のヤーンが別の３サイクルを続ける間保存した(合計６サイクル)。各洗浄サイクルの後でヤーンを従来からの住宅用乾燥機中で乾燥した。
【０４０６】
各洗浄サイクルのロード（負荷）当たり、約８５ｇの市販の洗濯用洗剤（Ｔｉｄｅ Ｄｅｅｐ Ｃｌｅａｎ Ｆｏｒｍｕｌａ，Ｍｏｕｎｔａｉｎ Ｓｐｒｉｎｇ ｌｉｑｕｉｄ ｌａｕｎｄｒｙ ｄｅｔｅｒｇｅｎｔ）を使用した。中間負荷設定は洗浄サイクルで約１６ガロンの温水そしてリンスサイクルで１７ガロンの冷水を使用した。合計洗浄サイクルは３０分であった。
【０４０７】
３回洗浄サイクル、６回洗浄サイクル、そして対照ヤーンをＡＡＴＣＣ法試験方法１６−１９９８の推奨に従って３層厚のカードに巻いた。ヤーンの色を測定し色定着性を次式：△Ｅ＝(Ｌ_１−Ｌ_２)^２ ＋(ａ_１−ａ_２)^２ ＋(ｂ_１−ｂ_２)^２ ）^１／２ 、で計算される反射光の色変化、△Ｅ、によって定量した。ここで１は初期状態そして２は最終状態、そしてＬ、ａ及びｂはそれぞれ赤／緑及び黄色／青の光度又は強度に関する反射光の測定値である。
【０４０８】
洗浄サイクルの色変化（△Ｅ）を表１８に示した。データは実施例５１ｂ−５３ｂからなるヤーンの６回洗浄後の色定着性は比較例のナイロン６対照（Ｊｂ^＊ ）のそれよりも良好であることを示している。ミリング酸染料やプリメタライズ染料のような他の酸染料技術を使用しても同様の結果が期待される。従来からの定着剤技術もまたさらに洗浄定着性を改良するために本発明と一緒に使用することができる。
【０４０９】
【表１８】

カットパイルカーペットの製造
実施例５１ａ−５３ａ及び比較例ＬａとＫａで作られたヤーンは、“Ｓ”方向で４．５ターン／インチ（１．６ターン／ｃｍ）をもつツイストヤーン(撚糸)を作るために、ベルドールモデル４００、ケ−ブル撚り装置でスピンドル速度５２００ｒｐｍ及び巻き取り速度３１．６ｍ／分で撚糸した。撚糸をバッチオートクレーブを使用して回転及びヒートセットするために周囲長さ８９インチ(２．３ｍ)のリールに巻いた。ヒートセットを１３２℃で５４分間行った。
【０４１０】
撚りそしてヒートセットしたヤーンを５／３２ゲージカットパイルタフト機で主カーペット裏地にタフトした。パイル高さは２０／３２インチ（１．６ｃｍ）でそしてカーペットの平方ヤード当たり４０オンス（１１３４ｇ）（１３５６ｇ／ｍ^２）のヤーンを使用した。
それからタフトカーペットを表１９の処方に従って以下の手順で染色した。
【０４１１】
１． 水の適当量を染料浴に加えカーペットが染料浴に十分覆われるようにした。
【０４１２】
２． 金属イオン封止剤のＥＤＴＡ、ダイイエローＡＣ、硫酸アンモニウム、及びチオ硫酸ナトリウムを染料浴に加えそしてｐＨを約６．５に調節した。
【０４１３】
３．グレージュ良好なカーペットを繊維を濡らすために染料浴に加えた。
【０４１４】
４． 染料を染料浴に加えた。
【０４１５】
５． それから染料浴をゆっくりかき混ぜながら３０−４５分で約９０℃に加熱した。
【０４１６】
６． 染料浴を撹拌しながら９０℃で３０分間保持した。
【０４１７】
７． それから染色されたカーペットを取り出し冷水でリンスし乾燥させた。
【０４１８】
【表１９】

乾燥後、カーペットをスチレン／ブタジエンラテックスでコーティングし、乾燥し、せん断をかけ、そしてコントラクトウォーカー評価用の試料に切断した。コントラクトウォーカー評価の目的はコントロールされた環境における歩行者の往来の結果としての床被覆パイルの外観保持を評価することである。試験はよく知られておりそして通常カーペット工業で採用されている。コントラクトウォーカー試験は以下の手順に従って、Ｐｒｏｆｅｓｓｉｏｎａｌ Ｔｅｓｔｉｎｇ Ｌａｂｏｒａｔｏｒｙ ｏｆ Ｄａｌｔｏｎ，ＧＡ，ＵＳＡによって実施された：
１． 長さと幅方向の両方から２３０ｍｍｘ５６０ｍｍの試料を切断し、歩行流れに垂直な長い距離の床に適切な手段で固定した。
【０４１９】
２． 歩行者は５０分間隔で歩く。全ての試料は往来が再開される前に毎時間電気掃除機をかける。予め決定された往来量が適用されたかを決定するために多重電子計数器を使用する。
【０４２０】
３． 予め決定された往来量が適用された後で再び電気掃除機をかけ最後の吸引で元のパイルの方向にする。全ての試料は技術審査員による等級付けの前に最低１２時間室温で回復させる。
【０４２１】
４． 試料はそれぞれカーペット及び敷物協会（ＣＲＩ）ＴＭ１０１に従ってＣＲＩ対照（リファランス）スケールを使用して等級付けされる。等級は平均化され最も近い０．１で報告される。等級が高ければ期待される性能は良好となる。等級は、５＝すりへりが認められない、４＝わずかにすりへり、３＝中庸のすりへり、２＝有意のすりへり、１＝激しいすりへり、である。
【０４２２】
５． 各試料はいずれも５０００サイクル等級付けしそして２０，０００サイクルが得られるまでさらに往来試験のために床に置かれる。
【０４２３】
外観試験の結果を表２０及び図４に示す。
【０４２４】
【表２０】

本発明のカーペットの耐久性は良好な手触りをもちながら比較例の対照に較べて改善されている。
【０４２５】
実施例５４−５５、Ｍｃ
実施例５１と５２の繊維成形条件がマスターバッチ法を使用して４０ｍｍ二軸押し出し機でコンパウンド化したナイロン−６、シンジオタクチックスチレン及び相溶化剤からなる本発明に従った組成物からの１３９０合計デニールの７２フィラメントヤーンを作るために繰り返された。実質的に純粋なナイロン６が比較例試料として含まれる。繊維成形条件は表２１に示す。
【０４２６】
【表２１】

紡糸口金は定量ポンプ流量１５０ｇ／分で供給された。第一及び第二ゴデットロールは、それぞれ８０℃／３０８ｍ／秒及び１５０℃／１０００ｍ／秒で操作され、延伸比３．２５を与えた。テキスチャライジングは加熱空気を使用して１７０℃、３５ｐｓｉｇ（２４１ｋＰａ）圧力で行われた。絡まりは織り交ぜジェットによって４４ｐｓｉｇ（３００ｋＰａ）の空気圧力で得られた。
【０４２７】
実施例５４と５５及び比較例Ｍで作られたヤーンを４．０ターン／インチで撚り、ヒートセットし、そしてカーペット裏地にタフトして４０オンス／スクエアヤード（１．４ｋｇ／ｍ^２ ）、５／８インチ（１６ｍｍ）パイル高さの５／３２ゲージカットパイルカーペットを作った。カーペットを二つのグループに分けた。第一グループは染色無しだがラテックス接着剤で裏打ちされ、せん断をかけられ、そして住宅用シミ試験用のグレージュ製品として本発明の耐シミ製の改良を強調するために残した。グレージュカーペットに１０の典型的なシミの標準量をたらしそして２４時間試料上に保持した。それからカーペットをマイルドな洗剤で洗濯しそして乾燥した。生じたシミを等級化するために、Ａｍｅｒｉｃａｎ Ａｓｓｏｃｉａｔｉｏｎ ｏｆ Ｃｈｅｍｉｓｔ ａｎｄ Ｃｏｒｏｒｉｓｔｓ（ＡＡＴＣＣ）シミ評価のグレ−スケールを使用した。等級は：５＝シミなし、４＝わずかのシミ、３＝認知できるシミ、２＝かなりのシミ、１＝ひどいシミである。シミ等級を図５に示す。実施例５４と５５のヤーンから作られたカーペットはコーラ、コーヒー、トマトジュース、オレンジジュース、及び赤ワインに対して比較例Ｍから作られたカーペットより少ないシミを示した。さらに、実施例５４と５５のヤーンから作られたカーペットのシミの拡がり度合いは比較例Ｍのヤーンで作られたカーペットより非常に少なく本発明の汚れの減少を際立たせた。
【０４２８】
裏打ち無しのグレージュカーペットの第二のグループは、コーティングとせん断の前に、前の実施例５１ｃ−５３ｃの手順と表２２の染料処方で黄色に染色した。
【０４２９】
【表２２】

比較例Ｍｂの撚り及びヒートセットしたヤーンから作られたカーペット（Ｍｃ）は色縞筋を示した。実施例５４の撚り及びヒートセットしたヤーンから作られた染色カーペットは色縞筋が少なくそして満足すべき手触りと少ない光沢をもっていた。実施例５５の撚り及びヒートセットしたヤーンから作られた染色カーペットは実施例５４及び比較例Ｍｃの染色カーペットに比較して色縞筋がなくそしてより満足すべき手触りと少ない光沢をもっていた。
【０４３０】
実施例５６−６５、Ｎ
表２３に与えられる組成物をシングルパス法を使用して３０ｍｍ二軸押し出し機で製造した。得られたブレンド物を繊維を延伸せず部分的に配向したヤーン（ＰＯＹ）として残すことを除き、実験室規模の連続フィラメントラインで紡糸した。繊維成形条件は表２３に示す。融点は３００℃。充填圧力は４３０ｐｓｉｇ（２．９６ＭＰａ）。定量ポンプ供給量は５．９ｇ／分で２４フィラメントヤーンに対して約１４５０の合計デニールの連続フィラメントヤーンを製造した。未延伸急冷連続フィラメントヤーンを中間車に引き出しそれから延伸しそしてレゾーナ巻き取り機を使用して１００ｍ／分で円筒状パッケージに巻き取り、延伸比約３：１を得た。結果を表２３に示す。
【０４３１】
高い繊維堅さと残留伸びが相溶化剤を含む本発明の組成物で観察された。弾性率の改善は１０重量％以上の成分（ｂ）を含む繊維調合で見られた。
【０４３２】
【表２３】

実施例６６、Ｏ 低分子量のナイロン６の使用
ＳＰＳ２、ＭＧＳＰＭ１、Ｎ−６ＲＶ３８の１０：３：８７比のブレンド物をマスターバッチ法を使用して３０ｍｍ二軸押し出し機でコンパウンド化した。高分子量ナイロンを使用しそして２．５５ｇ／デニールの堅さと２．５の光沢審査員等級をもつ本発明の実施例３５に対し、このブレンド物は低分子量ナイロンを使用する。ブレンド物を、比較例Ｏ、
Ｎ−６ＲＶ３８対照と一緒にパイロット規模のＢＣＦ紡糸ラインで紡糸した。クエンチング：１５℃空気中、低速ゴデットロール速度：３３４ｍ／分、高速ゴデットロール速度：１０００ｍ／分、テキスチャライザー温度と圧力：１９０℃と８０ｐｓｉｇ（０．５５ＭＰａ）、織り交ぜ圧力：４０ｐｓｉｇ（０．２８ＭＰａ）である。追加の紡糸条件と結果として得られた堅さを表２４に示す。両試料ともうまく紡糸できた。本発明の実施例６６の光沢審査員等級は１．４でナイロン分子量の低下によって減少を示した。比較例Ｏの
光沢審査員等級は５．０であった。
【０４３３】
【表２４】

発明の実施例６７−７２
ナイロンＮ−６(成分（ａ）)、ＳＰＳ２(成分（ｂ）)、ＳＭＡ１(成分（ｃ）)、及びオクタデカンアミド(成分（ｄ）)の表２５の重量比のブレンド物をマスターバッチ法を使用して３０ｍｍ二軸押し出し機でコンパウンド化した。これらの実施例ではＳＰＳ２、ＳＭＡ１及びオクタデカンアミドはマスターバッチで混合した。オクタデカンアミドの目的は
ＳＭＡ１をナイロンＮ−６に混合する前に無水マレイン酸基のいくつかを予備反応させることによってその無水マレイン酸基の量を減少させることである。このことはユーザーにとって市販の相溶化剤を使用可能にしそして相溶化剤と反応するナイロンアミン末端基の量を成分（ａ）及び（ｂ）の相溶化剤と同様に良好な染色性をもたせるために調節することを可能にさせる。
【０４３４】
【表２５】

得られたブレンド物を実験室規模の連続フィラメント紡糸ラインと表２６の繊維紡糸条件を使用して紡糸した。クエンチ温度は２３℃である。繊維の性質は表２６に示す。
【０４３５】
【表２６】

実施例７３
ＳＰＳ２、ＭＧＳＰＭ１、及びナイロン６；６，６の重量比１０：３：８７のブレンド物をマスターバッチ法を使用して３０ｍｍ二軸押し出し機でコンパウンド化した。得られたブレンド物をパイロット規模のＢＣＦ紡糸ラインを使用して繊維に紡糸した。繊維紡糸条件は以下の通りである：
押し出し機バレル温度勾配：２８５℃／３１０℃／３０５℃／３０５℃
スピンヘッド温度：３０５℃
融点：３００℃
充填圧力：１２００ｐｓｉｇ（８．４ＭＰａ）
クエンチング：１４℃空気中
低速ゴデット：７５℃及び３３４ｍ／分
高速ゴデット：１６０℃及び１０００ｍ／分
テキスチャライザー温度と圧力：１９０℃と８０ｐｓｉｇ（０．６６ＭＰａ）
織り交ぜ圧力：５０ｐｓｉｇ（０．４４ＭＰａ）
得られたＢＣＦヤーンは、延伸、テキスチャーライジング、空気織り混ぜ及び巻き取りの後で７２フィラメントに対して１２０２合計デニールをもっていた。得られた１２０２／７２ヤーンの堅さは２．４ｇ／デニールである。光沢審査員等級は３．０であった。
【０４３６】
本発明の実施例７４−７７、Ｐ 分散相としてのｓＰＳ−ＰＭＳコポリマーの使用
ＳＰＳ２、ＳＰＭ１、ＳＰＭ２、ＳＰＭ４、ＭＧＳＰＭ１、及びナイロンＮ−６のブレンド物をマスターバッチ法と表２７に与えられた重量比を使用して３０ｍｍ二軸押し出し機でコンパウンド化した。得られたブレンド物を表２８に与えられた紡糸条件を使用してパイロット規模のＢＣＦ紡糸ラインで繊維に紡糸した。これらの実施例は、特別設計のダイを使用しないで変性比を改善するために分散相として低融点ポリマーを使用できる能力を強調している。
【０４３７】
【表２７】

【０４３８】
【表２８】

ＳＰＳ２、ＭＧＳＰＭ１、ナイロンＮ−６，６ＲＶ５０及びナイロンＮ−６，６ＲＶ２５０のブレンド物を表２９に与えられた重量比でマスターバッチ法を使用して３０ｍｍ二軸押し出し機でコンパウンド化した。得られたブレンド物を実質上実施例７４−７７のそれと同じ紡糸条件を使用して実験室規模の連続フィラメントラインで繊維に紡糸した。散乱比を実質的に実施例１６−２７及び本明細書の他の箇所で開示したレーザー光バック散乱技術によって決定した。
【０４３９】
【表２９】

【産業上の利用可能性】
【０４４０】
本発明は、特殊な装置設計又は操作手順（低い延伸温度の使用のような）や仕上げ技術を必要とせずに高速紡糸、シミ抵抗、色定着性、少ない色縞、少ない光学的な縞、減少したシミ、改良された破壊抵抗又は耐久性、及び少ない水分取り込みをもつ工業的な合成繊維又はフィルムの製造法として、カーペット、敷物、織布、不織布、スパンボンド布地、編み物、衣服、ラミネート等の用途に有用である。
【図面の簡単な説明】
【０４４１】
【図１】図１（ａ）は実施例５１に従った９３．１重量％のナイロン６、５重量％のシンジオタクチックポリスチレン、１．９重量％の相溶化剤を含む熱可塑性組成物の走査電子顕微鏡像である。図１（ｂ）は実施例５２に従った８７．３重量％のナイロン６、１０重量％のシンジオタクチックポリスチレン、２．７重量％の相溶化剤を含む熱可塑性組成物の走査電子顕微鏡像である。 図１（ｃ）は実施例５３に従った８１．９重量％のナイロン６、１５重量％のシンジオタクチックポリスチレン、３．１重量％の相溶化剤を含む熱可塑性組成物の走査電子顕微鏡像である。
【図２】図２（ａ）は比較例Ｋに従ったナイロン６と０．２重量％のＴｉＯ_２ つや消し剤を含む熱可塑性組成物から製造された繊維の走査電子顕微鏡像である。図２（ｂ）は比較例Ｌに従ったナイロン６と０．４重量％のＴｉＯ_２ つや消し剤を含む熱可塑性組成物から製造された繊維の走査電子顕微鏡像である。図２（ｃ）は比較例Ｍに従った８９重量％のナイロン６、１０重量％のアタクチックポリスチレン、及び１重量％の相溶化剤を含む熱可塑性組成物から製造された繊維の走査電子顕微鏡像である。
【図３】図３は変性率（Ｍｏｄ ｒａｔｉｏ）を計算するための典型的な多重繊維のプロットである。
【図４】図４は実施例５１ｃ−５３ｃ、Ｋｃ及びＬｃの試料カーペットの外観保持等級のプロットである。
【図５】図５は実施例５４、５５、及びＭｃのヤーンから製造されたの試料カーペットのシミ等級を示す。
【図６】図６は実施例４８で使用された溶融混合の一要素と拡張装置として組み込まれた拡張流れ撹拌機の見取り図である。
【図７】図７は高いダイスウェルをもつ本発明に従ったポリマーブレンド組成物で使用した新規なダイ設計図である。
【図８】図８は繊維のレーザー光散乱比を測定するために使用した装置の関係を示すスキーム図である。
【図９】図９はレーザー光散乱比を測定するために使用した単一繊維マウントの見取り図である。
【図１０】図１０はレーザー光散乱比を測定するために使用した単一繊維マウントの側面図である。
【図１１】図１１はレーザー光散乱比を測定するために使用した単一繊維マウントの図１０の線１１方向で示した断面図である。
【図１２】図１２は実施例１−３、Ａ、Ｂ及びＣ１−Ｃ５の繊維のレーザー光バック散乱測定によって決定されるときの散乱比、Ｒｓの関数として光沢をプロットした図である。
【図１３】図１３は実施例Ｄ１−Ｄ６の種々の繊維のレーザー光バック散乱測定によって決定したときの散乱比、ＲｓをＴｉＯ_２ 含量の関数としてプロットした図である。
【図１４】図１４は実施例１６−２７の繊維の体積平均直径を審査員光沢の関数としてプロットした図である。
【図１５】図１５は実施例１６−２７の繊維の体積平均直径を散乱比の関数としてプロットした図である。
【図１６】図１６は実施例１６−２７の繊維の堅さの関数として百分位数第９９番目の吸蔵粒子の体積Ｄ９９をプロットした図である。
【図１７】図１７は実施例２５で製造された繊維からの成分（ｂ）の吸蔵粒子の走査電子顕微鏡像である。
【図１８】図１８は実施例Ｆ、３９ａ、４１ａ、４３ａ、及び４４ａで決定されたときのＵＶ光に曝された後での、未染色繊維のＤ６５、１０度色等級をプロットしたものである。
【図１９】図１９は実施例４８での繊維表面の走査電子顕微鏡像（ＳＥＭ）である。【Technical field】
[0001]
The present invention relates to a thermoplastic composition useful for producing filaments, fibers, molded films and / or other shaped compositions, and a method for producing the same. In addition, the present invention is intended for, but not limited to, yarns and fabrics used in carpets, wovens, rovings, nonwovens, and other uses, jackets, adhesive tapes, packaging materials, and other uses. The present invention relates to an article made of a filament, a fiber, or a film including the above film.
[Background Art]
[0002]
Natural fibers such as wool, cotton, and silk have long been used in yarn-, filament-, and yarn-based applications such as carpet and textile applications. However, natural fibers have a limited supply. Furthermore, the quality and properties of natural fibers vary widely depending on the origin of the natural fibers in living animals and plants. Such irregularities negatively affect the feel, appearance, and performance of the fibers, and articles incorporating such fibers.
[0003]
Synthetic fibers, such as nylon, polyester, and polypropylene fibers, do not have the supply limitations of natural fibers and are therefore less expensive than natural fibers. In addition, synthetic fibers have the advantage of being obtained from a controlled chemical reaction or physical molding environment, having a more uniform quality than natural fibers and having improved durability over natural fibers. However, because synthetic fibers are incompatible with the overall performance profile of natural fibers, particularly with respect to the softness, warmth, color depth, and hand of natural fibers, consumers have found that synthetic fibers are less suitable than their natural counterparts. They tend to be considered undesirable.
[0004]
Synthetic fibers extrude filaments of synthetic resin and render the synthetic resin into a product having desirable properties by drawing or spinning, shrinking, or other molding methods (hereinafter "synthetic fiber"). Thermoplastic polymers are desirable for use in such processes due to the fact that they can be easily extruded at temperatures above their melting point and may be shaped and shaped in a subsequent operation before or after cooling. The highly desirable thermoplastic polymers for the aforementioned end uses have sufficient crystallinity at normal use temperatures, especially at 20 ° C., which does not obey the laws of linear viscoelasticity applicable to amorphous polymers. More desirably, such polymers are cooled to a temperature below the crystalline melting point to provide sufficient crystallinity to provide sufficient elasticity and general mechanical properties suitable for use in fiber or film forming processes. It is desirable to form. That is, a suitable thermoplastic polymer should have a sufficient crystallization rate to be suitably used in such a process. Ultimately, the thermoplastic polymer is well below the depolymerization, decomposition or auto-ignition temperature so that it can be easily extruded without significant polymer decomposition, volatilization or smoke generation when extruded in the presence of oxygen. It is desirable to have a melting point, (Tm).
[0005]
Yarn is typically formed by bundling a number of fibers using a suitable integration technique. The enhanced physical properties are imparted to the yarn by a number of physical treatments, including heating, twisting, or otherwise physically or chemically modifying the fiber or yarn. Yarns made from thermoplastic polymers are particularly useful for forming carpets, fabrics (including woven, nonwoven or spunbond and knit fabrics) and other uses.
[0006]
The film is also extruded from a thermoplastic polymer through a die or orifice and then formed by uniaxial or biaxial stretching by the use of a tentering machine or expanded gas using compressed gas. Such films are applicable for many applications, including packaging, textiles, adhesive tapes and structural laminates. In some of these applications, a rough surface is desirable to reduce frictional forces and dust generation during the manufacturing process and to reduce blocking during storage and use.
[0007]
Suitable thermoplastics for forming filaments, fibers, films, and other structures include polyamides, polyesters, polyolefins, polyurethanes, and the like. Polyamides, especially nylon 6 and nylon 6,6, are highly desirable for use in making fibers, especially carpets, upholstery fabrics, and clothing. Generally, nylon synthetic fibers have much higher gloss and less color depth than natural fibers, especially wool and silk. The carpet industry has traditionally added titanium dioxide (TiO2) to molten polymers.₂ ) To give the nylon fibers a more wool-like sheen by including a small amount (typically 0.1-0.6% by weight) of a matting agent. However, the use of matting agents has several disadvantages. First, the presence of a matting agent in the thermoplastic composition reduces the color depth of the fibers and causes articles made from the fibers to have a faded chalk-like appearance. Further addition of the dye does not improve the color depth. Second, matting agents reduce the UV fixing of the fibers. TiO₂ Is known to cause nylon degradation. TiO₂ Also reflects incoming light and prevents the light from passing through the fiber as desired. This causes carpets, fabrics and other articles made from matte synthetic resins to fade faster than desired. In particular, light is prevented from penetrating deeply into the matte synthetic fiber, so that there is less fading inside the fiber, but this cannot compensate for the more faded surface.
[0008]
Synthetic fibers tend to have a smooth surface, which would lack the texture or 'feel', softness, and warmth of natural fibers. The textile industry has devised several means of modifying and / or processing fibers made from thermoplastics to provide a more natural or softer texture or hand. For example, it is well known to use special star- or multi-projection-shaped dies or spinners and special spinning conditions to give a softer, more wool-like feel to the fiber surface. As a disadvantage, such fiber designs often reduce the mechanical properties of the fiber, leading to a lack of durability. It is well known that forming fine denier fibers improves softness, but again at the expense of durability and fiber spinning economy.
[0009]
Nylon fibers have particularly additional disadvantages. For example, nylon fibers absorb water and are more susceptible to contamination by water-based stains than other fiber-forming materials such as polyester. Nylon fibers and yarns made therefrom can be easily dyed in aqueous media by this water absorption and also by their receptivity of the reactive amine end groups to the most common acid dyes used in the tufted carpet industry. The reactive amine end groups also make the nylon yarn very stainy. Special grade nylons with modified end groups are produced for this reason. In the case of resins containing a large number of amine end groups, expensive stain inhibitors are often employed to coat the amine end groups and provide stain resistance. Such additional processing will increase the cost of the resulting product. In addition, resins which are inherently stain resistant or have been modified to impart stain resistance often have the disadvantage of poor dyeing properties, in particular poor color fixability. In applications requiring repeated washing of carpets such as rugs and bath mats, improved color fixing properties are desired in the industry. It would be advantageous to be able to modify the water and stain absorption of the nylon fibers to improve stain resistance while retaining dyeability.
[0010]
In addition, carpets and fabrics made from nylon yarns are prone to streaking with dyes and light. Nylon fibers used for warp in woven and knitted fabrics have been carefully selected to ensure uniformity of dyeing and are sold at a higher price than regular nylon fibers. In the process of heating and cooling the fibers in synthetic carpet production, for example, the fibers or yarns undergo a process of twisting or shrinking. Despite extensive quality control efforts, nylon carpets obtained from the processing of fibers can undergo inconsistent heat treatment. Because dye penetration and uptake is affected by the morphology and crystallinity of the nylon fibers, uneven heat treatment can lead to carpet fibers with different levels of dye penetration and uptake, which in turn, allows for the final carpet. Light or dark streaks that cannot be formed may be formed. In addition, the yarns used in carpet manufacturing have varying shrinkage recovery powers, resulting in differences in carpet tuft width and height, providing streaks to color streaks. It would be a great advantage to be able to control the dyeing and shrinkage of nylon fibers in the process of reducing dye streaks and streaks. In addition, modern nylon grades require the use of partially drawn yarns or POY to reduce the time before spinning and texturing and on the other hand the fibers relax, if a significant time delay occurs on one side after spinning and drawing. It is difficult to use in the manufacture of garments, especially in the manufacture of garment fabrics. This is believed to be due to a change in the crystalline system of the polymer, especially from gamma to alpha crystal form. In fact, a single turn of a fiber made from a resin exhibiting this property is prone to breaking and is unacceptable for commercial use. The ability to spin a stable POY is an advantage when decoupling the spinning process from the drawing and texturing processes and allowing high speed spinning of garment yarns.
[0011]
A final known disadvantage of nylon resins is that they have a propensity to absorb unacceptable amounts of moisture and require careful drying during the manufacturing process before melting and extruding filaments therefrom. In addition, this property will also reduce carpet performance during use, such as absorbing undesirable cleaning solutions or spilled liquids and lack of color fixation in the resulting article.
[0012]
It is known to add small amounts of a second polymeric substance to a fiber-forming polymer to produce a rough surface fiber having an appearance similar to natural wool and reduced gloss. U.S. Pat. No. 4,518,744 teaches that fiber-forming polymers such as polyethylene terephthalate, nylon 6,6, or polypropylene are insoluble in the melt and have a particle size of 0.5 to 3 microns in the melt. Thermoplastic polymer blends are disclosed that form fibers containing between 0.1 and 10% by weight of the polymer. While providing improved surface texture and feel, the foregoing compositions did not exhibit improved melt spinning properties. This is believed to be due, at least in part, to poor compatibility between the polymer components.
[0013]
In U.S. Pat. No. 4,806,299, 0.1-5% by weight of a low molecular weight (200-40,000) polypropylene having a melting point above 120 DEG C. and a viscosity of 200-10,000 cp at 190 DEG C. was added. Nylon resin blends were employed for this purpose. Similar nylon blends containing amorphous polymers, polyethylene oxide (PEO) or polyethylene glycol (PEG) have been disclosed as well. Disadvantages are that such blends need to be drawn at spinning temperatures below the softening temperature of the polypropylene (50-120 ° C), and the amount of polypropylene is above 5% by weight to reduce the fiber stiffness I can't. In addition, both polypropylene and polyethylene oxide have a melting point (160 ° C. Tm or 66 ° C. Tm) lower than the melting point (Tm) of polyamide (220-260 ° C.), so that under typical fiber forming conditions, The formation of a discontinuous occlusion of the minor components of, a desirable morphology to produce matte fibers, is difficult or impossible. Finally, the water solubility of polyethylene oxide renders fibers made from blends containing it unacceptable for commercial use due to lack of color fixation, lack of stain resistance, and dye variability.
[0014]
In US Pat. No. 5,399,306, an increased composition comprising a comonomer, a metal salt, or a second component such as a molecularly dispersed polymer (eg, PEG dispersed in nylon 6,6 or nylon 6 dispersed in nylon 66). A nylon carpet or textile yarn made at a processing rate is disclosed.
[0015]
U.S. Pat. No. 6,024,556 discloses a multi-layer, co-extruded composite polymer fiber having improved optical properties, especially increased gloss and color depth, a fiber structure having a multi-layer fiber structure with optically controlled layers. A mechanical forming method has been disclosed.
[0016]
Certain references have suggested compositions comprising syndiotactic polystyrene (SPS) and nylon, or other polymeric compounds. In U.S. Pat. No. 5,914,370, a blend of nylon, SPS and various polar group containing compounds having low water absorption, including a maleic acid-modified syndiotactic copolymer of styrene and p-methylstyrene, is prepared and molded. Tested for use. Various component ratios down to 25% SPS and 5% maleic acid modified copolymer were tested (see Example 8). U.S. Pat. No. 5,270,353 discloses a blend of a polar functional polymer including SPS and nylon, and a polar group containing compatibilizing compound including maleated polyphenylene ether and a styrene / maleic anhydride copolymer. In particular, Example 5 comprises a 85/15 weight ratio of polyamide and syndiotactic polystyrene together with 5% styrene / maleic anhydride copolymer containing 1% maleic anhydride. It is believed that the amount of compatibilizer and polar groups in the blend is insufficient for use in fibers or films to achieve proper dispersion of the dispersed phase particles in the polyamide matrix.
[0017]
In a laboratory disclosure, 40258, published September 20, 1997, an industrial fabric made from syndiotactic polystyrene or blends thereof with nylon or other polymers, especially paper machine structures or other A yarn for use as a high temperature application is disclosed.
[0018]
In TW 40965A published February 8, 1999, (a) 50-10 parts by weight of a syndiotactic styrene-based polymer; (b) 1-50 parts by weight of a polyamide; and (c) a styrene-maleic anhydride phase. A polystyrene / polyamide composition having improved toughness and flexural strength comprising 0.01-20 parts by weight of a solubilizer is disclosed. Finally, U.S. Pat. No. 6,093,771 discloses thermoplastic polymer blends for use in fiber, film and molding applications.
[0019]
Blends of syndiotactic polyvinylidene aromatic polymer and polyamide polymer or copolymer are good if the syndiotactic polyvinylidene aromatic polymer is in excess, even if such a blend contains a compatibilizer. It has been found that they do not have good fiber-forming properties. In particular, such resins do not have sufficient fiber strength to be molded using high speed fiber molding equipment. Blends containing such polar group-modified polypropylene ethers as compatibilizers generally have a slightly yellow color. For many applications where light or white fibers are desired, such polymers have been found to be unacceptable. In addition, prior art blends containing polyethylene terephthalate, polypropylene or polyethylene oxide in a nylon matrix, even when matted, have generally unacceptable spinnability, tinting, and puncture resistance properties and are commercially available. It is unacceptable as a product.
DISCLOSURE OF THE INVENTION
[Problems to be solved by the invention]
[0020]
Accordingly, an object of the present invention is to provide a fiber comprising a syndiotactic polyvinylidene aromatic polymer which can be produced using a high-speed fiber molding apparatus, and furthermore, has the properties of high quality wool fiber, especially low gloss, good hand and softness. It is an object of the present invention to provide a synthetic fiber exhibiting low yellowness and good color depth. Furthermore, it is an object of the present invention to provide high-speed spinning, stain resistance, color fixation, low color streaks, without the need for special equipment designs or operating procedures (such as using low drawing temperatures) or finishing techniques. It is to provide an industrial synthetic fiber with less optical streaks, reduced stains, improved puncture resistance or durability and low moisture uptake.
[Means for Solving the Problems]
[0021]
A. Thus, the present invention:
(A) a first thermoplastic polymer 76-97, more preferably 80-95, and most preferably having a crystallization temperature, Tc, greater than 160 ° C., preferably greater than 165 ° C., most preferably greater than 170 ° C. Is 86-92% by weight,
(B) a second thermoplastic polymer 24-3 that is chemically different from (a) having a crystallization temperature, Tc ', more preferably 20-5, and most preferably 14-8% by weight, and
(C) optionally a compatibilizer for (a) and (b), wherein the percentages are based on the total amount of (a) and (b), and Tc is at least 5 ° C. There is provided a composition comprising at least 10 ° C, most preferably 20 ° C less.
[0022]
Preferably, the aforementioned composition has a yellow index, YI, of less than 10.0.
[0023]
B. In another aspect, the invention provides:
(A) a first thermoplastic polymer 76-97, more preferably 80-95, and most preferably having a crystallization temperature, Tc, greater than 160 ° C., preferably greater than 165 ° C., most preferably greater than 170 ° C. Is 86-92% by weight,
(B) a second thermoplastic polymer 24-3 that is chemically different from (a) having a crystallization temperature, Tc ', more preferably 20-5, and most preferably 14-8% by weight, and
(C) if desired, compatibilizers for (a) and (b), and
(D) 0.1-10.0, preferably 0.1-7.0, more preferably 0.2-5.0%, by weight of the total composition of the matting agent, wherein Tc is Tc '. At least 5 ° C, preferably at least 10 ° C, most preferably at least 20 ° C.
[0024]
Preferably the aforementioned composition B also has a yellow index, YI, of less than 10.0.
[0025]
C. In another aspect, the present invention comprises the aforementioned composition A or B, or a preferred embodiment thereof, wherein the first thermoplastic polymer is a polyamide, preferably a polyamide having a specific viscosity of 25-250, and more preferably Preferably, the polyamide is nylon 6.
[0026]
D. In yet another aspect, the invention comprises a composition A, B or C as described above, wherein the second thermoplastic polymer is a tactic conformation, preferably a homopolymer of a vinylidene aromatic monomer, one or more vinylidene aromatics. Or a derivative modified with a polar group thereof, wherein the second thermoplastic polymer has a syndiotactic steric structure, most preferably a syndiotacticity greater than 95%. It is a polyvinylidene aromatic homopolymer or copolymer.
[0027]
E. FIG. In another aspect, the present invention provides an extruded stretched fiber, or an extruded stretched film, preferably a stretched or oriented film, or a stretched fiber comprising the thermoplastic composition A, B, C, or D described above. Preferably, such a filament, fiber or film has a rough surface or comprises an occlusion of component (b) in a matrix of component (a), said occlusion being less than 0.2 μm D with a volume average minor axis diameter of large, preferably 0.3-2.0 μm, or smaller than 3.0 μm⁹⁹An extruded stretched fiber or an extruded stretched film having a minor axis diameter or having a laser light scattering ratio (defined below) of 0.29 or greater, or a gloss judge grade of 4.0 or less.
[0028]
F. In another aspect, the present invention relates to (1) a thermoplastic composition according to A, B, C or D wherein the thermoplastic composition comprises a continuous matrix of a first thermoplastic polymer and an occlusion of a second thermoplastic polymer. (2) occlusion of the second thermoplastic polymer is partially spread on the surface of the fiber or oriented film or causes perturbation on the surface of the fiber or film. As provided, there is provided a method for producing a fiber or film comprising the steps of drawing the filament of step (1) into drawn fibers or orienting the film of step (1) to an oriented film.
[0029]
G. FIG. In another aspect, the invention relates to a filament, fiber, yarn or extruded film as described above, carpet, rug, woven, nonwoven or spunbond fabric, knit, garment, laminate, made from either E or F. Provide structures or other commercial products.
[0030]
H. In another aspect, the present invention relates to (1) a method of preparing a thermoplastic composition according to A, B, C or D wherein the temperature at which the thermoplastic composition is extruded comprises both component (a) and component (b). (2) cooling the extrudate to a temperature between the crystallization temperatures of component (a) and component (b); or extruding the component (a) Cooled to a temperature below the crystallization temperature of component (b) and subsequently reheated to a temperature between the crystallization temperatures of component (a) and component (b), and (3) the filaments of step (1) or Provided is a method for producing a fiber or a film, comprising a step of stretching a film into a drawn fiber or an oriented film.
[0031]
I. In another aspect of the present invention, (1) extruding the thermoplastic composition according to A, B, C, or D as a number of fibers, (2) stretching the fibers, and (3) optionally texturing the fibers. Ring, shrink, dye, or partially or completely heat set, and (4) the fibers of (3) are combined with one or more yarns, optionally in a braid, dye, carding, or bulking process or even heat setting. (5) inserting the yarn into the yarn with backing and implantation; cutting or shaping the yarn as desired to form a rug or carpet, and (6) dyeing or finishing the rug or carpet as desired Producing a rug or carpet in steps comprising, where finishing comprises applying one or more stain or stain resistant treatments, rinsing, dyeing, or other steps To provide that way.
[0032]
J. In another embodiment of the present invention, a second thermoplastic polymer 24-3, different from (a) and having a crystallization temperature, Tc ', more preferably 20-5, and most preferably 14-8 weight. %, And (c) optionally a compatibilizer for (a) and (b), wherein said% is based on the total amount of (a) and (b), and Tc is at least 5 ° C. , Preferably at least 10 ° C, most preferably at least 20 ° C, less than 160 ° C, preferably greater than 165 ° C, comprising forming a polymer mixture and forming and drawing fibers from the polymer mixture. A method is provided for matting fibers of a first thermoplastic polymer (a) having a crystallization temperature, Tc, preferably greater than 170 ° C.
[0033]
K. As will be described in more detail below, in yet another aspect of the present invention, there is provided an extruded stretch, multicomponent fiber or extruded orientation, multicomponent film, or one or more components of such a multicomponent fiber or multicomponent film or Provided is a thermoplastic polymer composition in the form of a layer; wherein the composition consists of any of compositions A, B, C or D, or:
(A) a first thermoplastic polymer 99-51 having a crystallization temperature, Tc, greater than 160 ° C., more preferably 97-76, and most preferably 92-86% by weight;
(B) a second thermoplastic polymer 1-49, different from (a), having a crystallization temperature, Tc ', more preferably 3-24, and most preferably 8-14% by weight, and (c) a desired The compatibilizer for (a) and (b), wherein the% is based on the total amount of (a) and (b), and Tc is at least 5 ° C., preferably at least 10 ° C. Most preferably 20 ° C less.
[0034]
L. Another aspect of the present invention is a thermoplastic polymer composition useful in the manufacture of extruded fibers and films, the composition comprising (a) a first thermal crystallization temperature, Tc, having a crystallization temperature, Tc, greater than 160 ° C. 65-97% by weight of a thermoplastic polymer, (b) 35-3% by weight of a second thermoplastic polymer chemically different from (a) having a crystallization temperature, Tc ′, and containing polar functional groups, and Contains one or more non-polymer additives.
[0035]
M. In a final embodiment, the polymer composition melts the base resin consisting mainly of component (a) and simultaneously or subsequently mainly comprises component (b) and optionally components (c) and / or (d) and, if desired, a small amount of Mixing with it a concentrated resin consisting of component (a); and extruding the resulting molten thermoplastic polymer composition into a fiber form and optionally stretching or extruding the optionally obtained thermoplastic polymer composition into a film form. And the above-mentioned article (extruded drawn fiber or extruded drawn film) manufactured by drawing is provided. A preferred method for obtaining the aforementioned well-mixed compositions is to introduce a mixing device or element that provides static or extended mixing to the polymer melt during or after the melt mixing or extrusion process.
【The invention's effect】
[0036]
According to the present invention, a fiber comprising a syndiotactic polyvinylidene aromatic polymer produced using a high-speed fiber molding apparatus can be produced, and further, the properties of high-quality wool fiber, particularly low gloss, good touch and softness, and low yellowness Synthetic fibers exhibiting taste and good color depth can be produced.
Furthermore, the present invention allows for high speed spinning, spot resistance, color fixation, low color fringing, and low optics without the need for special equipment designs or operating procedures (such as using low draw temperatures) or finishing techniques. Industrial synthetic fibers can be produced with good streaking, reduced spots, improved puncture resistance or durability, and low moisture uptake.
BEST MODE FOR CARRYING OUT THE INVENTION
[0037]
For the purposes of United States patent practice, the patent application or publication referred to herein is hereby incorporated by reference in its entirety, particularly with respect to the disclosure of analytical or synthetic techniques and the general knowledge of the literature. The term “consisting of” and derivatives thereof, whether or not disclosed herein, are not intended to exclude the presence of any additional components, steps, or means. For the avoidance of doubt, all compositions defined in the claims using the term "comprising", unless otherwise specified, whether or not they are polymers or additional additives , Adjuvants, or compounds. In particular, the blends of the present invention characterized using the term "consisting of" comprise in component (a), (b) and (c) one or more thermoplastic polymers meeting the requirements of the claims. It may be. In contrast, the term "consisting essentially of" excludes any other component, step or means from the point of view of any reference, except that it is not essential for operation. Finally, the term "consisting of" excludes any component, step or means not specifically described or listed.
[0038]
The term "polymer" as used herein refers to the reaction of a homopolymer, i.e., a polymer derived from a single reactive compound, with a copolymer, i.e., at least two polymer-forming reactive monomeric compounds. And the polymer obtained by the above method. The term “crystalline” refers to polymers that exhibit an X-ray diffraction pattern at 25 ° C. and have a temporary transition point or crystalline melting point (Tm). This term is used interchangeably with the term "semi-crystalline." The term "chemically different" means that the major repeating groups of the two polymers are functionally different than the difference in the size of the repeating units.
[0039]
The term "fiber" means a strand of thermoplastic material having a relatively large length / thickness ratio, including continuous fibers. The cross-section of the fibers may be any desired closed shape, including round or curved, polygonal or multi-projection shapes. In addition, the cross-section may include voids of any shape, continuous or discontinuous, which result in fibers containing depressions, partially depressions or cells. Also included are continuous or discontinuous single fibers or yarns made therefrom. Preferably, the fibers have a maximum cross-sectional dimension of 2.0 mm, more preferably 1.0 mm, and most preferably 0.5 mm. Preferably, the fibers are characterized by having a length at least 100 times their diameter or cross-sectional dimension. For use in yarn and fiber production, the fibers should be at least 5 mm long and have sufficient strength and flexibility to be useful for this application. Draw fiber is an article made by drawing or spinning the aforementioned fiber, thereby stretching the fiber and providing improved tensile strength and other physical properties. Generally, drawing gives a large orientation to the crystal structure of one or more polymer components of the fiber. Preferred drawn fibers are those drawn in a ratio of at least 2: 1, preferably at least 2.3: 1 and most preferably 2.6: 1. In the above definition, draw ratio means the ratio of the respective linear velocities of the fibers as measured at the end and at the beginning of the drawing process. The fibers may be crimped, dyed or physically or chemically modified before or after bonding to other fibers and yarns or tows.
[0040]
The term "filament" as used herein generally refers to endless or very long fibers. Relatively short lengths of fibers are called "staples". "Tow" means the combination of several fibers without a distinct twist or other modification. Individual fibers may also be brought together by fiber entanglement or crimping. The term "yarn" refers to a combination of one or more fibers or filaments, including further physically or chemically modified derivatives, such as interlaced, dyed or heat-treated derivatives of such fibers or filaments. Means Tow called zero twist yarn is also included. Twisting generally gives yarns improved strength, cohesion and uniformity through improved entanglement.
[0041]
The term "film" means a solid, free-standing, generally planar structure having an average width of 1.0 mm and a thickness of 50% or less of the average thickness.
[0042]
"Compatibilizers" increase interfacial adhesion between the different phases of a multi-component mixture, reduce interfacial tension, or both increase interfacial adhesion and decrease interfacial tension. Polymeric compatibilizers are one of several types:
a) Compatibilizers consist of separation zones or "blocks" having different physical and chemical properties. The polymer can be a linear block polymer having two or more blocks, a radial copolymer containing many arms protruding from a central core, or a "star" or dendritic structure containing discrete regions of similar chemical structure. it can. The blocks, arms or regions are mixed or have an affinity for one or more components of the mixture.
[0043]
b) the compatibilizer has the ability to mix or have an affinity for one or more of the components of the mixture and to react and bind with one or more of the remaining components.
[0044]
c) The compatibilizer has at least two functions. One is that it can react and bind with at least one of the components of the mixture, and one or more of the remaining functionality is that it can react with and bind with at least one of the remaining components of the mixture.
[0045]
Increased interfacial adhesion can be evidenced by an increase in tensile strength of the sample containing the compatibilizer as determined according to ASTM D638 after conditioning according to ASTM D618A. Domains are identifiable regions of each polymer determined using microscopy, optionally stains, or can be evidenced by some other morphological analysis technique. Separation domains result in incomplete or heterogeneous mixing of the respective polymers. Domains exist in the form of polymers occluded in other polymer matrices, or enter a network where each polymer is in a continuous or semi-continuous phase. For use herein, a thermoplastic polymer is a material in which the blend is non-homogeneous if the two polymers are mixed at a temperature above the melting point of both polymers, i.e., microscopic examination, or some other morphology. One or all of the polymers identifiable by analytical techniques are considered to be incompatible if they produce a material characterized by a separation domain. Preferably, the compositions of the present invention result in the formation of occlusions of component (b) in a continuous matrix of component (a) and the filaments or fibers of the present invention comprise components (b) in a continuous matrix of component (a). Is characterized by the presence of occlusions.
[0046]
The preferred compatibilizer (component (c)) used herein is a thermoplastic polymer having both olefinic functionality, preferably organic, aromatic functionality, and relatively polar functionality. Exemplary thermoplastic compatibilizers used herein include polar group-modified polyphenylene ethers, polar group-modified vinylidene aromatic polymers, polar group-modified block copolymers of one or more vinylidene aromatic monomers and one or more conjugated dienes (thereof). Including partially or fully hydrogenated derivatives of such polymers or block copolymers) and mixtures of the former. Preferred aromatic monomers include styrene, C_1-4 Cyclic alkyl- or halo-substituted styrenes (especially all isomers of vinyltoluene and mixtures thereof) and α-methylstyrene are included. Preferred compatibilizers are ethylenically unsaturated, polar group-containing compounds, especially graft copolymers of maleic anhydride or fumaric acid with preformed polyphenylene ethers; polar comonomers, especially maleic anhydride, fumaric acid, N-methylmaleimide, methyl methacrylate, acrylonitrile or acrylamide and vinyl aromatic polymers or copolymers, especially atactic or syndiotactic polystyrene, styrene and one or more cyclic alkyl-substituted styrenes, especially styrene and p-methylstyrene, o-methylstyrene, graft copolymers with copolymers, including syndiotactic copolymers with m-methylstyrene or mixtures thereof; or block copolymers of styrene and conjugated dienes; Family monomers, copolymers of styrene is particularly encompassed.
[0047]
In embodiments A-M of the invention described above, component (b) is analogous to a polar group-modified crystalline polymer, such as the compounds of the preceding list of components suitable for component (c), Reactive polar group-modified syndiotactic vinylidene aromatic homopolymers or copolymers are repeated here for clarity. In such embodiments of the present invention, the separation compatibilizer (component (c)) need not necessarily be included in the composition. As an example of such an embodiment, a composition consisting solely of 97-76% of component (a) and 3-24% of such a polar group-modified syndiotactic vinylidene aromatic homopolymer or copolymer is particularly preferred for the present invention. . More preferably, such a composition comprises a polar group graft-modified syndiotactic copolymer of styrene and one or more cyclomethylated styrenes, especially p-methylstyrene, wherein the copolymer comprises a polymerized styrene-methylstyrene linkage. Comprising 99.5-95.0% styrene and 0.01-5.0% of the cyclic methylated styrene by weight; and 0.01-3% by weight of grafted polarity based on total graft polymer weight. Contains comonomer residues.
[0048]
As used herein, the term “tactic”^ThirteenC means a polymer having an isotactic or syndiotactic stereoregular structure greater than 90% of the racemic triad, preferably greater than 95% of the racemic triad, as determined by nuclear magnetic resonance spectroscopy. . The terms "isotactic" and "syndiotactic" refer to such a tactic polymer having an isotactic or syndiotactic configuration, respectively. The "specific viscosity" value, RV, is a dimensionless number, unless otherwise noted, in an 8.5% by weight polymer solution in formic acid for nylon or in another suitable solvent for other polymers according to ASTM D2857. Based on viscosity measurement at 25 ° C.
[0049]
The yellow index, YI, is a dimensionless number determined on both polymer and article samples (fibers) and determined according to ASTM E-313-00. The preferred YI rating of the compositions and fibers according to the invention is 8 or less, and most preferably 6 or less.
[0050]
Fiber gloss, especially in the textile industry, was determined by a professional judge comparing samples with known standards made from wool for dull or matte fibers and pure nylon fibers for bright high gloss standards. It has been qualitatively tested for a long time. A similar examiner approach is used in this patent for fibers of grades 1 (dull, wool) to 5 (glossy, non-matte). On the downside, this test is subjective because it reflects the gloss determined by the human eye. In order to be able to apply to the fiber itself and provide a more quantitative gloss test than the judge test, we have described "Experimental Studies of Fiber Surface Roughness by Laser Back-scattering", J. Am. Polym. Sci. Phys. Ed. , 28, 1771 (1990) and "Computer Simulation of Laser Backscattering from Fiber Surfaces" J. Am. Polym. Sci. Phys. Ed. C., 28, 1755. Luo and R.S. R. Laser light back scattering analysis technology based on Breese's published technology has been developed to determine the surface structure of woven fibers.
[0051]
The above technique shows that high gloss fibers exhibit high directional (low isotropic solid angle) radiant emission, while low gloss fibers exhibit low directional (higher isotropic solid angle). It takes advantage of the fact that it exhibits radiative divergence. The scattered radiation ratio is measured and quantified using fixed solid angle sensing optics and image analysis. A known method of optically matting fibers is to impart a surface roughness to the fibers. (Other means include adding internal means to scatter the diffraction index boundaries of the object or fiber). Regardless of the matting mechanism, the collimated collimated light emits from the fiber at a very elevated solid angle. The image obtained from the emission is converted to the spatial frequency domain for subsequent analysis using Fourier transform techniques. In the aforementioned technique, the roughness coefficient, RC, is obtained from this analysis and is used to quantify the gloss of various fibers.
[0052]
To determine the gloss of each fiber sample according to the present invention, the following procedure and technique (herein referred to as laser light backscattering technique) was developed based on the aforementioned prior art.
An apparatus for measuring scattered laser irradiation from a single fiber according to the present technology is shown in FIG.
It comprises four main parts: laser light source, 4, light beam generator, 2, fiber mounting (installation) and orientation means, 20, recording / analyzing means such as a digital camera connected to a digital processor or computer, A backlight strobe unit for synchronizing with the measurement of the scattered laser light by the light beam means; A preferred laser light source has a wavelength of 632.8 mm and about 0.78 mm 1 / e² Helium-neon gas laser-generated TEM with randomly localized light source of beam diameter₀₀(Model LSR2P laser commercially available from Aerotech). The laser is mounted on an attenuated, adjustable table, such as the 443 variant, commercially available from Newport, Irvine, CA, and provides fine adjustment of height and coarse adjustment of angle of incidence and θ. Fine adjustment of the angle of incidence is made by adjusting the travel using a precision rail system (PRC-3 transporter and PRL-36 rail available from Newport, Irvine, CA). A linear variable intermediate density filter (31W00ML.1, Newport, Inc.) is attached to the laser to adjust the power of the incident laser beam, 2.
[0053]
The fiber mount, with a perspective view in FIG. 9, an end view in FIG. 10, and a cross-sectional view along line A in FIG. 11, exhibits elasticity in fiber orientation and shape. The mount comprises a frame 21 consisting of holders 21a and 21b which are attached to the substrate 1c by a clamping machine 21d and has a circular opening for receiving the rings 22a and 22b. Core rings 22a and 22b are held in holders 21a and 21b by means of locking devices 23a and 23b, respectively. The fiber locking clamps 24a and 24b for mounting the end 1 of the fiber, respectively, are located outside the core rings 22a and 22b. The rings 22a and 22b can rotate together or independently about the major axis of the fiber. When the locking devices 23a and 23b are released, the mandrel rotates together by connecting with the mandrel support 24. The core ring 22a further includes an inner core ring 28 containing a central shaft portion 29 and is connected concentrically to the core ring holder 27 so that it can rotate around the fiber axis of the core ring holder 27.
The inner ring 28 is fixed to the shaft of the ring holder 27 by independent locking means such as a fixing screw. By opening the independent locking means 23c and rotating the inner ring 28, and by interfering with the movement of the ring holder 27 by locking the ring screw 23a, the fibers have a random surface texture before being measured. Twisted many times to make. The fiber mount frame is releasably connected to a height adjustment means, such as a post, which is not shown here, which mates with the connection port 26.
[0054]
8, the detector 30, 30 comprises a video camera, such as a model XC-55 / 55BB video camera available from Sony Corporation (Japan). This camera includes a sensor array of 659 × 494 (horizontal / vertical) pixels operated in 8-bit grayscale, and a 4 × zoom lens that produces a spatial resolution of 4.022 μm / pixel. To provide backside illumination and synchronize to camera exposure, a fiber optic connected flashlamp, such as the LS-1102 flashlamp, available from EG & G Optoelectronics, Salem, MA, is placed on the other side of the fiber from the camera.
[0055]
The fibers to be analyzed are carefully washed with hot, deionized water to remove the finished coating and dust, dried, and kept in a dust-free environment before and during the analysis. The fibers are twisted to randomize the surface texture and placed under tension for analysis. Images are acquired and analyzed using an IBM personal computer equipped with an Intel, Pentium (III) microprocessor, video capture board, and image analysis software (Speedview 850, Greenfield Instruments, Greenfield, MA). Will be implemented.
[0056]
Images of the fiber collected with or without laser light are processed to obtain a measure of the scattered laser intensity emanating from the fiber. Quantitation of the amount of scattered light is achieved by analyzing the grayscale image in a histogram format, whereby the reflected fiber-, background- and scatter-irradiation peaks are recorded. The integrated intensity of these peaks, pixels (area), gives the fiber area and the scattered illumination intensity. Since the fiber diameter is known to affect the scattering intensity and the fibers analyzed are of different diameters, the measurement of the scattering intensity is normalized to the fiber diameter by the following formula: R_s= I_s/ A_f        (1)
Where R_sIs the scattering ratio, I_sIs the intensity of the scattered light collected and A_f Is the area of the fiber. The scattering ratio, also called the laser light back scattering ratio, has been found to be a quantitative number that is inversely proportional to the appearance contribution of gloss. As disclosed in Examples 1-3, A, B, C1-C5 and D6, the laser light scattering technique for this gloss measurement is based on the results of a gloss judge and a matting agent (TiO2).₂ ) Has been shown to be in good agreement empirically with the gloss values obtained with known amounts of. Highly desirably in the present invention, the fiber has a scattering ratio, R, of at least 0.29, preferably at least 0.33, as measured by this laser light back scattering technique._s With. Alternatively or additionally, the fibers have a corresponding gloss judge value of 4 or less, more preferably 3.5 or less.
[0057]
The term "occlusions" means a region of discontinuous or substantially discontinuous component (b) surrounded or partially surrounded by component (a), called a matrix. The size of component (b) and the distribution of the solid occlusion determine the ultimate fiber properties, especially gloss and spinnability. It was determined that there was a good correlation between gloss and volume average minor axis diameter. Preferred are occlusion products of component (b) of greater than 0.2 μm, preferably 0.25-3.0 μm, more preferably 0.3-2.0 μm, most preferably 0.4-1.6 μm. It is a fiber having a volume average short axis diameter, Dν. Furthermore, the absence of large occluded particles is highly desirable to improve fiber stiffness and avoid fiber breakage, a property indicative of spinnability. Particularly preferred are fibers whose component (b) occluded material has a short axis diameter of 99% or less and D99 of D99. Having a narrow particle size distribution is highly preferred because minimum gloss and maximum firmness are achieved at the volume average particle size.
[0058]
The particle size dispersion, P, is calculated using the two measured diameters of the occluded particles of component (b) as follows:
[0059]
Embedded image

Can be calculated using
Preferred fibers have a particle size distribution of component (b) of 2.7 or less, most preferably 2.3 or less.
[0060]
The aforementioned Dv and D99 measurements are determined by dissolving the fiber or film sample in an occlusion solvent or solvent for the matrix that is not a swelling agent.
A preferred solvent for the polyamide matrix which is not a solvent for the syndiotactic vinyl aromatic polymer occluder or a swelling agent is formic acid or an aqueous solution of formic acid. After dissolving the matrix, the resulting separated occluded particulate material is recovered by filtration, coated with chromium, and photographed with a scanning electron microscope. Standard, computer-based particle size analysis techniques are used to measure particle size.
[0061]
Techniques, if any, for adjusting the occlusion particle size of component (b) and the properties of the fiber thus obtained, the type and amount of compatibilizer employed, component (c); the molten state before extrusion The amount of mixing achieved in the process; the amount of time delay between the completion of mixing of the molten thermoplastic blend and the extrusion of the fibers under conditions that permit agglomeration of component (b); nucleating agent, if any, present at the time of compounding And the relative and melt viscosities of each component (a) and (b), as well as other process variables.
[0062]
The advantage of the present invention is believed to be due to the fact that occlusions of component (b) are less affected by the drawing force as compared to component (a) during the drawing or spinning of the fiber, which simultaneously cools the extrudate or filament. ing. This is called differential stretchability for the purposes of this patent. Preferably in the present invention, component (a) is stretched more than the occluded component (b) during extrusion and fiber formation. More preferably, the matrix polymer (component (a)) is stretched at least 2 times, more preferably at least 3 times more than the occlusion polymer of component (b). Differential drawability is determined by measuring the draw ratio of the whole fiber or film to the draw of the dispersed phase. Stretching of the entire fiber or film is defined as the ratio of the cross-sectional area of the undrawn fiber or undrawn film to the fully drawn fiber or fully drawn film, assuming the law of conservation of mass of the particles. . Stretching of the dispersed phase is defined as the ratio of the average cross-sectional area of the dispersed phase in the unstretched fiber or unstretched film to the fully stretched fiber or fully stretched film. As a result of the aforementioned differential stretchability, such occluded portions are released from the surface of the resulting fiber or film, or because such occluded materials are in close proximity to the surface of the fiber or film, When the matrix (component (a)) is stretched to a greater degree than the occlusion, it causes large pull-down rates, causing protrusions, cracks, or other discontinuities or irregularities in the surface. Such rough surface fibers may have desirable low gloss, hand and softness; similarity to natural fibers; and still improved spinnability and draw properties, high speed commercial fiber production and frictional forces during fiber formation. And reduce drag. Fibers with reduced friction with metals further reduce the amount of lubricant employed for spin finish. Rough surface films also have desirable properties such as anti-blocking, low dust generation, and reduced friction during manufacturing.
[0063]
Differential stretchability is affected by many variables, as highlighted in the present invention. The domain size of the dispersed phase must be large enough to be able to create an effective rough surface, but not so large as to reduce fiber stiffness to a level that makes spinning difficult. The domain size of the dispersed phase must be stable to provide a residence time that does not cause excessive coalescence in the fiber spinning extruder or branch in the melt phase. Compatibilization of the interface between the dispersed and continuous phases helps to dramatically reduce fiber spinnability and prevent dripping and bursting. The melting points of the dispersed phase and the continuous phase must be close enough so that both phases do not melt and still become too hot for decomposition and fiber spinning. The rheology of the dispersed and continuous phases must be similar enough to produce the desired particle size during the melt-mixing process, but must be sufficiently different to allow for different drawability during the fiber spinning process. Must. A small amount of crystallization development dramatically increases the viscosity of both phases. Crystallization mechanics can be quantified by the temperature at which crystallization begins, the maximum crystal development temperature, or the rate of crystallization versus temperature. Nucleating agents or crystallization inhibitors can be used to alter the crystallization dynamics. The viscosity of either phase can also be increased or decreased by the addition of substances (eg, plasticizers or flow enhancers) that affect the molecular weight change or flow properties of the polymer.
[0064]
The molecular weight of the continuous phase can also be varied to change the stretchability of the dispersed phase. Similarly, additives to affect the flow properties may be added to the continuous phase. The drawing force in fiber spinning is given by a drawing godet (address cloth) of a fiber spinning device. Stretching force is applied to the dispersed phase via the continuous phase. When the molecular weight of the continuous phase is low, it can be easily stretched and imparts a low stretching force to the dispersed phase.
[0065]
Extruded film formation and uniaxial or biaxial stretching or tentering of the film
A similar phenomenon occurs that irregularities are formed on the surface of the obtained film.
Such films have low adhesion and can be easily processed by high speed film formers without the need for the addition of blocking agents. Further, such films produce less dust during high speed processing and transport processes.
[0066]
Although the aforementioned advantages in fiber properties are achieved without the need to include a matting agent, particularly titanium dioxide, in the thermoplastic composition, it should be noted that the addition of such additives is not excluded. You should understand. If present, its use can be greatly reduced compared to prior art nylon-based formulations. When used, the level of matting agent is from 0.01 to 0.3% by weight and preferably less than 0.1% by weight. Most preferably, no matting agent is used, whereby fibers, films and articles comprising fibers or films according to the present invention, especially injection, where matting agents such as titanium dioxide affect physical properties. This is advantageous for improving the recyclability of molded articles and glass fiber reinforced articles.
[0067]
In addition, custom die or spinner designs may be employed, if desired, to produce multi-projection shapes that result in the production of fibers with improved bulk. Due to the differences in die swell compared to pure nylon resin, a particular die design is preferably employed to make the best use of the polymer blend composition of the present invention. The structure of this die is shown in FIG. 7, where a die opening design with three elongated protrusions, 70, terminates generally at a parallel (as shown) or semicircular or curved end, 72. The total slot length (measured along the central axis of the slot, 73, at the point where the central axes of the three protrusions intersect) has three equal length slots, 71, with converging surfaces. It has a Mod Rate (MR) of 11.2 with a 0.045 inch (1.143 mm), a slot width of 0.007 inch (0.178 mm) and a capillary length of 0.040 inch (1.02 mm). Preferred dies have a Mod ratio of 9 to 12.
[0068]
Mod ratio as used herein refers to the ratio of two measurements of the cross-sectional shape of a multi-projection fiber or die. In particular, it is the ratio of the radii of two circles, the larger of which is located at the center of the cross-sectional shape and circumscribes the entire multi-projection shape and the smaller one inscribes the inner surface of the multi-projection shape. This is shown in FIG. 3 as a reference, where the multi-projection shape, 30, has three projections, 31, circumscribes a circle 33 having a radius R1 and inscribes a circle 33 having a radius R2. . The Mod ratio is defined as R1 / R2. The preferred Mod ratio of the fibers of the present invention is 2.5-4.
[0069]
Yarns composed of fibers and filaments according to the invention generally do not meet the aforementioned requirements as compared to yarns made from a single thermoplastic polymer component or a polymer composition comprising component (a) as a polymer blend. Increased color transmission and fade resistance, increased stain retention, improved stain resistance, improved stain resistance, improved dimensional stability, improved dye stability, and reduced moisture It was found to show uptake. The occlusion of component (b) lowers the surface energy of the fiber or film and reduces the surface wetting of the aqueous solution with stains, and the occlusion is not affected by moisture as in component (a), and It is believed to provide a more serpentine path for permeation of extraneous materials such as fluids, resulting in greater stain resistance and stain retention.
[0070]
Furthermore, yarns made from fibers of a thermoplastic composition in which the first and second thermoplastic polymer components differ in terms of the crystallization temperature according to the present invention were considered to be incompatible with one another in the industry. It has been found to exhibit both good bulk and good durability. The difference in crystallization temperature between the polymer alloy components provides an easy means to control the crystallization development of the fiber. For example, the crystallinity of one phase could be used to set crimp, while the crystallinity of the other phase could be used to set twist in a twisted heat set BCF yarn. . An additional advantage of yarns made from the thermoplastic composition of the present invention, especially the thermoplastic component (a) is a polyamide, is that the crystallinity of one component, particularly component (b), is used in setting the twist yarn. The morphology and crystallinity of the composition is more consistent throughout the fiber because it is set in one or more steps, such as the drawing process or the drawing and crimping process, while maintaining the crystallinity in the matrix. Is to be done. This will assist the skilled artisan in minimizing or eliminating dye uptake differences in the finished carpet and the associated streaking problems. Further, for garment fibers, if the fibers are separated from the drawing and texturing steps, sufficient crystallinity is set in the spinning and drawing steps to reduce or prevent fiber relaxation.
[0071]
According to the aforementioned advantages, the advantage is that the thermoplastic polymer (a) and the thermoplastic polymer (b) are selected based on the difference in the crystallization temperature of the component as measured by a differential scanning calorimeter (DSC). Found when Preferably, the thermoplastic polymer (a) has a crystallization temperature that is at least 20 ° C. less than the crystallization temperature of thermoplastic polymer (b), and most preferably at least 40 ° C. below the crystallization temperature of thermoplastic polymer (b). It has a low crystallization temperature. In a particularly preferred embodiment, the thermoplastic polymer (a) preferably has a crystallization temperature not exceeding 250 ° C, more preferably not exceeding 240 ° C, and most preferably not exceeding 230 ° C. In a particularly preferred embodiment, the thermoplastic polymer (b) is at least 170 ° C, more preferably at least 200 ° C, most preferably at least 215 ° C; preferably not more than 285 ° C, more preferably not more than 280 ° C, and most preferably Preferably it has a crystallization temperature not exceeding 275 ° C.
[0072]
About thermoplastic polymer (a)
Highly preferably, the thermoplastic polymer (a) is a non-tactic polymer that can be extruded and spun into fibers. Typical polymers for use as thermoplastic polymer (a) include homopolymers and copolymers of polyamide, polyester, polyactinic acid, polyvinylcyclohexane, ethylene / styrene interpolymers, and mixtures thereof. Suitable polyesters include condensation copolymers of ethylene glycol, polyethylene glycol or polypropylene glycol with aromatic dicarboxylic acids, especially terephthalic acid, phthalic acid, or mixtures thereof. A preferred polyester is polyethylene terephthalate (PET) or polyethylene glycol terephthalate (PEGT).
[0073]
Preferred polymers for use as the thermoplastic polymer (a) are polyamides or copolyamides, also called nylons, including nylon mixtures. Suitable polyamides include, for example, aliphatic and aromatic polyamides obtained by condensation of an aliphatic or aromatic dicarboxylic acid having 4-12 carbon atoms with an aliphatic or aromatic diamine having 2-12 carbon atoms. Is included. A typical but non-exhaustive list of aliphatic dicarboxylic acids suitable for use in synthesizing the polyamides used herein includes adipic acid, pimelic acid, azelaic acid, suberic acid, sebacic acid and dodecandioic acid. Included. Typical aromatic dicarboxylic acids include: phthalic acid, isophthalic acid, terephthalic acid, and naphthalenedicarboxylic acid. Typical aliphatic diamines include, for example, alkylenediamines such as hexamethylene diamine and octamethylene diamine. Suitable aromatic diamines are: diaminobenzenes such as 1,4-diaminobenzene, 1,3-diaminobenzene, 1,2-diaminobenzene; 2,4-diaminotoluene;
2,3-diaminotoluene, 2,5-diaminotoluene, and 2,6-diaminotoluene
Ortho-, meta-, and para-xylylenediamine; ortho-, meta-, and para-2,2'-diaminodiethylbenzene; 4,4'-diaminobiphenyl; 4,4'-diaminobiphenyl 4,4'-diaminodiphenylmethane; 4,4'-diaminodiphenylether; 4,4'-diaminodiphenylthioether; 4,4'-diaminodiphenylketone; and 4,4'-diaminodiphenylsulfone. Mixtures of the aforementioned aliphatic and aromatic dicarboxylic acids and diamines are also frequently used. As well as by self-condensation of lactams or ω-aminocarboxylic acids, it is also possible to prepare polyamides from acid chlorides and acid derivatives such as amine salts and amine derivatives. Examples of such lactams include ε-caprolactam and ω-laurolactam. Examples of such ω-amino acids include 11-aminoundecanoic acid, 12-aminoundecanoic acid, 4-aminophenylcarboxylmethane, 1- (4-aminophenyl) 2-carboxylethane, and 3- (4-aminophenyl ) 1-carboxylpropane, and para- (3-amino-3'-hydroxy) dipropylbenzene.
[0074]
Typical aromatic polyamides suitable as component (a) include polyxylene adipamide; polyhexamethylene terephthalamide; polyphenylene phthalamide; polyxylene adipamide / hexamethylene adipamide; polyester amide elastomers Polyether amide elastomers; polyether ester amide elastomers; and dimeric acid copolymerized amides.
[0075]
Typical aliphatic polyamides suitable for use as the thermoplastic polymer (a) include: polycaprolactam (nylon-6); poly (hexamethylene adipamide) (nylon 6,6); nylon-3,4 Nylon-4; Nylon-4,6; Nylon-5,10; Nylon-6; Nylon-6,6; Nylon-6,9; Nylon-6,10; Nylon-6,12; Nylon-11; Nylon-12 is included. Preferred polymers of component (a) are aliphatic polyamides, especially nylon 6 or nylon 6,6, most preferably nylon 6.
[0076]
The thermoplastic polymer (a) preferably has a certain molecular weight and molecular weight distribution (MWD).
MWD is calculated as the ratio of Mw / Mn, where Mw is the weight average molecular weight and Mn is the number average molecular weight. Preferred materials have a MWD of 1-20, preferably 1.5-10. The melt flow rates of the nylon-6 thermoplastic polymers (a) measured at 230 ° C / 2.16 kg under ASTM D1238 conditions require high discharge rates to achieve good workability of the fibers or films made therefrom. Desirably 0.1-100 g / 10 min, more preferably 0.2-50 g / 10 min, and most preferably, as evidenced by good mechanical properties when measuring speed and tensile strength 0.3-10 g / 10 min. Many suitable polymers for component (a) use relative viscosity as a measure of molecular weight. Using this measurement method, suitable polymers have an RV (relative viscosity) of 25-250, preferably 30-180, more preferably 35-160. Preferably, the thermoplastic polymer (a) has a crystallinity of 10%, preferably at least 15%, more preferably 20% as measured by wide angle X-ray diffraction at 25 ° C. Equally desirably, the thermoplastic polymer (a) has a crystallization rate such that fibers or films with appropriate crystallinity are produced using typical forming and forming process conditions. Additives (crystallization promoters) to increase or decrease the rate of crystallization may be incorporated into component (a) if desired.
[0077]
As already disclosed, the preferred polymer for use as component (a) is a nylon, which shows the surprising fact that nylon 6 generally has less fiber formation than nylon 6,6 without the improvement of the present invention. 6. As is known in the literature, the polyamide employed has a disproportionate amount of amine end groups which produces a polymer that is easily dyed and has improved color fixation. Such polyamide compounds are characterized by the fact that the ratio of amine end groups: carboxylic acid end groups in the polyamide is greater than 1. If desired, the amount of amine end groups can be modified in a known manner by reacting with a compound having a carboxylic acid function or other function that reacts with a primary amine.
[0078]
The preferred polyamides used herein further depend on the desired end use of the fiber. For highly matte fibers low viscosity polyamides, such as nylon 6 resin having an RV of 25-75, more preferably 30-60 are preferred. For fibers with enhanced ease of spinning (less breakage), high viscosity nylon 6 or nylon 6,6, for example, resins having an RV of 120-250, more preferably 150-180 are preferred.
[0079]
About thermoplastic polymer (b)
Polymers suitable for use as the thermoplastic polymer (b), without limitation, are isotactic or syndiotactic polystyrene and styrene with one or more comonomers (halo-, C_1-4 Alkoxy-, C_1-4 Alkyl- or C_1-4 High temperature polyesters such as polycyclohexene terephthalate, tactic polymers of vinylidene aromatic monomers, including isotactic or syndiotactic copolymers (such as haloalkyl-ring-substituted styrene or polar-substituted styrene). A derivative of the former graft-modified with a polar comonomer, especially a maleic anhydride, fumaric acid, or maleimide graft-modified derivative of an isotactic or syndiotactic copolymer of styrene and a cyclic alkyl-substituted styrene compound; Alternatively, it is suitably selected from the former mixture.
[0080]
Preferably, the thermoplastic polymer (b) has a crystallinity of 5%, preferably at least 10%, more preferably 15% as measured by wide angle X-ray diffraction at 25 ° C. An additive (crystallization accelerator) for increasing or decreasing the rate of crystallization may be incorporated into component (b) if desired. This material may be the same or different from the crystallization promoter incorporated in component (a).
[0081]
More preferably, the thermoplastic polymer (b) comprises a syndiotactic homopolymer of vinylidene aromatic monomer or a graft copolymerization with a monomer containing polar functional groups, including a stereoblock copolymer of one or more vinylidene aromatic monomers. One or more of the former polymers that have been copolymerized (hereinafter referred to as "polar group modified" polymers). A "polar group" or "polar functional group" is defined herein as a group or substituent that imparts a greater polar moment to a compound as compared to a compound without such a group. Preferred polar groups include carboxylic acids and carboxylic acid derivatives (eg, acid amides, acid anhydrides, acid azides, acid esters, acid halides, and acid salts resulting from substitution of a hydrogen atom or a hydroxyl group of the carboxylic acid group), sulfones Includes acids and sulfonic acid derivatives (eg, sulfonic acid esters, sulfonic acid chlorides, sulfonic acid amides, and sulfonic acid salts), epoxy groups, carbonate groups, amino groups, imide groups, and oxazoline groups.
[0082]
Suitable vinylidene aromatic monomers have the formula: H₂ C is a compound of CR-Ar, where R is hydrogen or an alkyl group having 1-4 carbon atoms, and Ar is an aromatic group consisting of 6-18 carbon atoms or an alkyl-, haloalkyl-, Alkoxy- or halo-substituted aromatic groups. Preferred polar functional groups are polar residues resulting from reaction with maleic anhydride or fumaric acid. Preferred vinylidene aromatic monomers are styrene and C_1-4 Alkyl-, C_1-4 It is an alkoxy- or halo-, ring-substituted styrene derivative.
[0083]
Typical vinylidene aromatic polymers include: polystyrene, poly (methylstyrene),
Poly (ethylstyrene), poly (isopropylstyrene), poly (pt-butylstyrene);
By polymerizing a monomer mixture including poly (methoxystyrene), poly (vinylnaphthalene), poly (bromostyrene), poly (dibromostyrene), poly (chlorostyrene), poly (fluorostyrene), and a mixture of monomer isomers Includes the former polymer mixtures (e.g., styrene / p-methylstyrene copolymer), including the resulting polymers, and hydrogenated or polar group modified derivatives thereof. Most preferred is the former polymer form having a syndiotactic stereoisomer structure.
[0084]
Most preferred thermoplastic resins for use as thermoplastic polymer (b) are syndiotactic vinylidene aromatic polymers and their derivatives functionalized with polar groups. US Pat. No. 4,680,353; US Pat. No. 5,066,741; US Pat. No. 5,206,197; US Pat. No. 5,294,685; US Pat. Patent 5,990,217; and others. Syndiotactic vinyl aromatic polymers are also commercially available from Dow Chemical Company under the trade name Questra. The most preferred polymer for use as thermoplastic polymer (b) is syndiotactic polystyrene, 0.005 to 15% by weight, preferably 0.01 to 10% by weight of p-, m- or o-methylstyrene monomer, especially Syndiotactic styrene containing p-methylstyrene / p-, m- or o-methylstyrene copolymer and derivatives of the former functionalized with polar groups containing 0.005-5% by weight of functional groups. The most highly preferred polymers are grafted with syndiotactic styrene or maleic anhydride or fumaric acid containing 0.1-10% by weight p-methylstyrene and 0.01-1.5% by weight maleic anhydride or fumaric acid. Or copolymerized styrene / p-methylstyrene copolymer. The latter graft polymer may be combined with the thermoplastic polymer (a) to achieve good polymer morphology for fiber formation without adding a separating compatibilizer (c).
[0085]
The weight average molecular weight, Mw, of the thermoplastic polymer (b), as determined by gel permeation chromatography, is not critical, but is typically 5,000-5,000,000, more typically 10 2,000-1,000,000, and preferably 20,000-500,000. Furthermore, the molecular weight distribution of the thermoplastic polymer (b) varies over a wide range, but is suitably 1-20, preferably 1.5-10.
[0086]
When the amount of thermoplastic polymer (b) in the composition is less than the desired amount, the fibers obtained therefrom do not exhibit the desired hand or soft taste. If the amount of thermoplastic polymer (b) in the composition is higher than desired, the filaments or fibers will be very liable to break during drawing or spinning. As used herein, the term "domain formation", particularly with respect to component (a) and component (b), refers to the fact that the respective polymers can be partially compatible with each other to form a homogeneous blend. It is understood that it means forming distinct regions or domains in the resulting composition. Preferably, however, the two polymers do not substantially compatibilize with each other, despite the agitation in the melt-mixing device providing shear, such that a homogeneous blend of the two components is not formed.
[0087]
About component (c)
Component (c) is utilized where improved adhesion and / or reduced interfacial tension between polymer domains resulting from the present invention is desired. In addition, the type and amount of compatibilizer aids the formation of small particles in the polymer matrix, well dispersed occlusions of component (b), and compositions having improved fiber tension as well as improved melt tension and spinnability. Guide to things. The preferred small domain of the occlusion of component (b) provides improved optical properties and surface roughness of the resulting fiber or film. Preferred compatibilizers have both aromatic functionality and polar groups, either physically mixed into the composition or grafted with one or more thermoplastic components (a) or (b). A polymer that reacts by interfacial polymerization but does not contribute to the yellowness of the resulting blend.
[0088]
Suitable compatibilizers include vinylidene aromatic homopolymers and copolymers (atactic, syndiotactic and isotactic homopolymers or copolymers of vinylidene aromatic monomers, as well as vinylidene aromatic monomers and acrylonitrile, maleic anhydride, or maleimide , Poly (vinyl ether), poly (vinyl methacrylate), polyolefin, poly (diene), and miscibility, partial solubility, or selection with component (b) on component (c). Includes several polymers with high affinity. These materials also include block copolymers (polymers composed of two or more different repeating unit segments). Suitable block copolymers comprise a segment that is miscible, partially soluble, or selectively compatible with component (b) on component (c). The additional segments may or may not meet miscibility, solubility, or affinity criteria with component (c). Examples of such materials include block copolymers of other repeating units (e.g., hydrogenated poly (styrene-block-ethylene-butadiene-block-styrene) graft-maleic anhydride) and vinylidene aromatic polymers and the following: Any such copolymers: including atactic, syndiotactic and isotactic homopolymers or copolymers of vinylidene aromatic monomers, as well as copolymers of vinylidene aromatic monomers with acrylonitrile, maleic anhydride, or maleimide), polyphenylene ethers Grafted or other functional polymer derivatives such as poly (vinyl ether), poly (vinyl methacrylate), polyolefin, poly (diene).
[0089]
The polymer chain structure of the compatibilizer (c) is preferably modified with reactive polar groups capable of reacting with the functional groups of the first thermoplastic polymer (a). Preferred reactants containing a reactive polar group are compounds containing an unsaturated bond, such as an ethylenic unsaturation, along with the desired polar group functionality, as defined above. Examples of suitable reactive polar groups include carboxylic acids, dicarboxylic acids and dicarboxylic acid derivatives (eg acid amides, anhydrides, azides, acid halides, acid salts resulting from the substitution of a hydrogen atom or a hydroxyl group of a carboxyl group) ), Sulfonic acids and sulfonic acid derivatives (eg, sulfonic acid esters, sulfonic acid chlorides, sulfonic acid amides, and sulfonic acid salts), epoxy groups, carbonate groups, amino groups, imide groups, and oxazoline groups.
[0090]
Preferred unsaturated reactants containing a reactive polar group are unsaturated carboxylic acids and dicarboxylic acids, unsaturated carboxylic acids and dicarboxylic acid derivatives, unsaturated epoxy compounds, unsaturated alcohols, unsaturated amines, and unsaturated isocyanates. Specific examples of reactive polar group-containing unsaturated reactants include maleic anhydride, fumaric acid, maleimide, maleic hydrazide, and reactive products of maleic anhydride and diamine, 1-methylmaleic anhydride, dichloromaleic anhydride. acid,
Such as maleic amide, itaconic acid, itaconic anhydride, soybean oil, tung oil, castor oil, linseed oil, hemp seed oil, cotton seed oil, sesame oil, rapeseed oil, peanut oil, tsubaki oil, olive oil, coconut oil, and salad oil Natural fats or acids of natural oils; acrylic acid, butenoic acid, crotonic acid, vinyl acetic acid, methacrylic acid, pentenoic acid, angelic acid, 2-pentenoic acid, 3-pentenoic acid, α-ethylacrylic acid, β-methylcrotonic acid , 4-pentenoic acid, 2-hexenoic acid, 2-methyl-2-pentenoic acid, 3-methyl-2-pentenoic acid, α-ethylcrotonic acid, 2,2-dimethyl-3-butenoic acid, 2-heptenoic acid 2-octenoic acid, 4-decenoic acid, 9-undecenoic acid, 10-undecenoic acid, 4-dodecenoic acid, 5-dodecenoic acid, 4-tetradecenoic acid, 9-tetradecenoic acid, 9-f Sadecenoic acid, 2-octadecenoic acid, 9-octadecenoic acid, eicosenoic acid, docosenoic acid, erucic acid, tetracosenoic acid, 2,4-pentadienoic acid, 2,4-hexadienoic acid, diallylacetic acid, geranium acid, 2,4-decadiediene acid,
2,4-dodecadiedienoic acid, 9,12-hexadecadienoic acid, 9,12-octadecadienoic acid, hexadecatrienoic acid, linoleic acid, linolenic acid, octadecatrienoic acid, eicosadienoic acid, eicosatrienoic acid , Eicosatetraenoic acid, ricinoleic acid, eleostearic acid, oleic acid, eicosapentaenoic acid, docosadienoic acid, docosatrienoic acid,
Unsaturated carboxylic acids such as docosatetraenoic acid, docosapentaenoic acid, tetracosenoic acid, hexacosenoic acid, hexacodienoic acid and octacononic acid, and esters, acid amides and anhydrides of these unsaturated carboxylic acids; allyl alcohol, methyl vinyl carbyl Ol, allylcarbinol, methylpropenylcarbinol, 4-penten-1-ol, 10-undecane-1-ol, propargyl alcohol, 1,4-pentadien-3-ol, 1,4-hexadien-3-ol, Unsaturated alcohols such as 3,5-hexadien-2-ol and 2,4-hexadien-1-ol;_nH_2n-5OH, C_nH_2n-7OH, C_nH_2n-9OH (n is a positive integer), 3-butene-1,2-diol, 2,5-dimethyl-3-hexene-2,5-diol, 1,5-hexadiene-, 4-diol, and 2,6 -Octadiene-4,5-diol and the unsaturated alcohols of these unsaturated alcohols₂ And unsaturated amines obtained by substitution with
[0091]
The acidic polar groups of the compatibilizer (c) may be completely or partially neutralized by zinc, magnesium, manganese, lithium or other metal counterions or combinations of metal counterions. It is also possible to use zinc acrylate in graft polymerization or functionalization to produce neutralized acid monomers, for example compatibilizer (c).
[0092]
Examples of the vinyl compound having an epoxy group include glycidyl methacrylate, glycidyl acrylate, vinyl glycidyl ether, glycidyl ether of hydroxyalkyl (meth) acrylate, glycidyl ether of polyalkylene glycol (meth) acrylate, and glycidyl itaconate. Methacrylate is particularly preferred. The compatibilizer (c) can include two or more compounds having two or more unsaturated groups and two or more polar groups (same or different), and a polar group or multiple polar groups.
[0093]
Particularly suitable compatibilizers (c) are polyarylene ethers having polar functionality and poly (vinylidene aromatic) homopolymers and copolymers having polar functionality. Also included are block copolymers having polar functionality and comprising segments of polyarylene ether and poly (vinylidene aromatic) homopolymers and copolymers. Such a compatibilizer can be obtained by modifying a conventional polymer with one of the polar group-containing modifiers described above. The modification method is not particularly limited as long as the modified product can be used according to the object of the present invention. Suitable base resins and reactants containing polar groups are in the molten state, optionally benzoyl peroxide, di-t-butyl peroxide, dicumyl peroxide, t-butyl peroxybenzoate, azobisisobutyl lonitrile, azobisiso Combined in an extruder or similar mixing device in the presence of a free radical generator or other initiator such as valeronitrile or 2,3-diphenyl-2,3-dimethylmethane. Polyphenylene ethers can generally be prepared by oxidative coupling of one or more phenols, preferably substituted at the 2- or 3-position. Preferably, a catalyst is used, such as a copper-amine complex, especially a copper-amine complex derived from primary, secondary and tertiary amines. Examples of suitable polyphenylene ethers include poly (2,3-dimethyl-6-ethyl-1,4-phenylene ether), poly (2-methyl-6-chloromethyl-1,4-phenylene ether), poly ( 2-methyl-6-hydroxyethyl-1,4-phenylene ether), poly (2-methyl-6-n-butyl-1,4-phenylene ether), poly (2-ethyl-6-isopropyl-1,4) -Phenylene ether), poly (2-ethyl-6-n-propyl-1,4-phenylene ether), poly (2,3,6-trimethyl-1,4-phenylene ether), poly (2- (4 ′ -Methylphenyl-1,4-phenylene ether), poly (2-bromo-6-phenyl-1,4-phenylene ether), poly (2-methyl-6-phenyl-1,4-) Phenylene ether), poly (2-phenyl-1,4-phenylene ether), poly (2-chloro-1,4-phenylene ether), poly (2-methyl-1,4-phenylene ether), poly (2 -Chloro-6-ethyl-1,4-phenylene ether), poly (2-chloro-6-bromo-1,4-phenylene ether), poly (2,6-di-n-propyl-1,4-phenylene) Ether), poly (2-methyl-6-isopropyl-1,4-phenylene ether), poly (2-chloro-6-methyl-1,4-phenylene ether), poly (2-methyl-6-ethyl-1) , 4-phenylene ether), poly (2,6-di-bromo-1,4-phenylene ether),
Poly (2,6-di-chloro-1,4-phenylene ether), poly (2,6-diethyl-1,4-phenylene ether), and poly (2,6-dimethyl-1,4-phenylene ether) Is included. Suitable methods for making polyphenylene ethers are disclosed in U.S. Pat. Nos. 3,306,874, 3,306,875, 3,257,357, 3,257,358, and others. Have been. Polymers are also readily available from commercial sources.
[0094]
Typically, the amount of polar functional groups in component (c) is 0.01-10% by weight based on the weight of component (c). In general, if less than 0.01% of polar functional groups are present, the compatibilizer will not be as effective as desired. The amount of component (c) employed, if present, is at least 0.1, more preferably at least 0.2% by weight, based on the weight of the composition; typically no more than 5, preferably no more than 4.5, It is more preferably at most 4.2, and most preferably at most 4.0% by weight.
[0095]
The amount of functional groups in component (c) varies, the efficiency of such groups in the compatibilizer compound varies,
Component (b) also contains functionality that aids compatibilization with component (a), and there are additional components in the resin blend that neutralize the amine end groups of the polyamide or affect the properties of the resulting polymer. In order to obtain the desired effective benefits of component (b), the amount of component (c) varies in the range of 0-5% based on the combined weight of components (a) and (b); The total amount of reactive functional groups in component (c) (if present) is from 0.001 to 0.25 mol%, preferably 0, based on the total amount of component (b) and component (c). It is desirably 0.011 to 0.24 mol%.
[0096]
When measured on the obtained fiber article, the above range changes as follows.
[0097]
The amount of component (c) varies from 0 to 24% based on the combined weight of components (a) and (b) and the total amount of reactive functional groups in component (c) (if present) Should be in the range of 0.001-0.8 mol%, preferably 0.01-0.5 mol%, based on the total amount of component (b) and component (c).
[0098]
In the following calculations, when functionalized, component (b) will contain all (if component (c) is not present during formulation) or a portion (if formulation is component (c) and component (b)) of the compatibilizer. If both are included). The following equation is used to make the above measurements:
1. ))% By weight of the functional component in the blend:
w_(C) = 100m_(C) / (M_(B)+ M_(A)+ M_(C))
Where m_(C)= Mass of functional component (component (b) if functionalized + component (c)), m_(B)= Mass of component (b), m_(A)= Mass of component (a).
2. ) Mol% of the functional component in the blend:
x_(C)= (100m_(C) / MW_(C) ) / (M_(B)/ MW_(B) + M_(A)/ MW_(A)
+ M_(C)) / MW_(C) )
Where MW_(C) = Average molecular weight of component (c) repeating unit, MW_(B) = Molecular weight of component (b) repeating unit, MW_(A) = Molecular weight of component (a) repeating unit.
3. ) Component (b) + weight percent of polar groups in component (c):
w_{Polar, (b)}= (M_(C) ) (F_Polar ) / (M_(B)+ M_(C))
Where f_Polar = Weight percent of component (c), which is a polar or functional residue (eg, a maleic anhydride residue in a styrene maleic anhydride copolymer).
4. ) Mol% of polar group in component (b) + component (c):
x_Polar = [(M_(C) ) (F_Polar ) / MW_Polar ] / [M_(B)/ MW_(B) + M_(C)/ MW_(C) ]
Where MW_Polar = Molecular weight of polar units.
5. )) Weight percent of polar groups in the blend:
w_{Polar, Blend}= (M_(C) ) (F_Polar ) / [(M_(B)+ M_(C) + M_(A) ]
6. ) Mole% of polar groups in the blend:
x_{Polar, Blend} = [(M_(C) ) (F_Polar ) / MW_Polar ] / [M_(B)/ MW_(B) + M_(C)/ MW_(C)+ M_(A)/ MW_(A) ]
Within the aforementioned total amounts of compatibilizer employed, the ideal level of compatibilizer is determined to balance the desired properties of the resulting fiber or film. The amount of compatibilizer used ultimately reduces the blend containing residual amine end groups of the polyamide, which in turn affects the dye acceptability of the fiber made therefrom for fiber applications, It is possible to employ a compatibilizer containing a polar group in an amount sufficient to improve the mechanical properties of the fiber, but less than the amount that has a negative effect on the dye acceptability of the fiber due to the reduction of amine end groups. desirable. The initial molar amount of amine end groups (for polyamides resulting from ring opening reactions) in turn depends on the molecular weight of the polymer. Formulas for evaluating available amine end groups are known. For nylon 6 and other polyamides formed by a ring opening reaction (and not modified in a manner that does not affect end group concentration), the formula is:
N = 1.10⁶/M _n [=] Milliequivalent / g
hereM _n = Number average molecular weight of the polyamide.
[0099]
Alternatively, use the following formula, assuming that the actual amount (moles) of reacted amine end groups reacts completely with the polar functional groups of the compatibilizer for such polymers. Can be calculated by:
Reaction amount = m_Comp ・ F_Polar / [100 ・ MW_Polar ]
Where m_Comp = Mass of compatibilizer, f_Polar = Weight percent of polar functional groups in the compatibilizer, and MW_Polar = Molecular weight of polar functional group. When both component (b) and component (c) contain polar functional groups, the average weight% and average molecular weight of the functional groups calculated by combining the ratios of the two components set by the formulation are used in the above formula. Is done.
[0100]
The amount of amine end groups remaining in the polymer blend is also reduced by adding reagents containing polar functional groups as measured directly using analytical techniques such as acid titration or other suitable techniques. I do. In particular, in the case of nylon 6,6 and condensed polyamide, the terminal group content is preferably measured directly since the calculation by the above-mentioned method is not followed.
[0101]
Regardless of the method used to calculate or determine the amine end groups in the blend, the ratio of available amine end groups, N,: polar functional groups in the compatibilizer is preferably from 70:30 to 99:99. 1, more preferably from 80:20 to 96: 4, and most preferably from 85:15 to 93: 7. Alternatively, the final amine end group content of the polymer composition is from 5 by reaction of component (c) or, if component (b) contains polar functional groups, with both polar groups of component (b) and component (c). Reduce to 20%. Preferred polymers as component (c) are styrene / maleic anhydride copolymers and syndiotactic copolymers of styrene and p-methylstyrene grafted with maleic anhydride.
[0102]
Optional component (d)
Additional additives may be present in the compositions of the present invention as long as the desired properties or end product is obtained. The type and amount of additional additives, if present, are selected according to known prior art. Typical additional additives include matting agents, elastomers, flame retardants, antifungal agents, heat stabilizers, light stabilizers, antioxidants, pigments, dyes, lubricants, blowing agents, optical matting agents, and static electricity Inhibitors are included. Such additives may be included in either or both of component (a) or component (b) or in the resulting composition after first preparing a blend of component (a) and component (b). You may. Additives that are harmful when added to component (a) may be employed in the present invention by being added only to component (b).
[0103]
Suitable matting agents are inorganic oxides, titanates, carbonates and silicates, preferably titanium dioxide. Preferred matting agents are in the form of fine particles or fine powder, and highly preferably have a volume average particle size of 100 μm or less, more preferably 50 μm or less, most preferably 10 μm or less.
[0104]
Suitable elastomers are those that increase the impact resistance, hardness or elongation of the composition. When employed, the elastomer is typically provided in an amount of 0.5-50, preferably 0.7-30, and more preferably 1.0-20% by weight based on the total composition weight. Examples of elastomers that may be included in the composition include: natural rubber, polybutadiene, polyisoprene, polyisobutylene, neoprene, polysulfide rubber, urethane rubber, silicone rubber, epichlorohydrin rubber, styrene-butadiene block copolymer (SBR), hydrogen Styrene-butadiene block copolymer (SEB), styrene-butadiene-styrene block copolymer (SBS), hydrogenated styrene-butadiene-styrene block copolymer (SEBS), styrene-isoprene block copolymer (SIR), hydrogenated styrene-isoprene block copolymer (SEP), styrene-isoprene-styrene-block copolymer (SIS), hydrogenated styrene-isoprene-styrene-block copolymer (SEPS) ,
Styrene-butadiene random copolymer, hydrogenated styrene-butadiene random copolymer, styrene-ethylene-propylene random copolymer, styrene-ethylene-butylene random copolymer, ethylene-propylene rubber (EPR), ethylene-propylene-diene-rubber (EPDM), butadiene -Acrylonitrile-styrene core-shell rubber (ABS), methyl methacrylate-butadiene-styrene core-shell rubber (MBS), methyl methacrylate-butyl acrylate-styrene core-shell rubber (MAS), octyl acrylate-butadiene-styrene core-shell rubber (MABS), alkyl acrylate- Butadiene-acrylonitrile-styrene core shell rubber (ABS), butadiene-styrene core shell rubber (SBR), and methyl methacrylate - butyl acrylate - core shell rubbers containing siloxanes such as siloxanes, and rubber obtained by modification of these rubbers are included.
[0105]
Flame retardants, also called ignitable spin additives, are not intended to reflect the performance of the composition under actual combustion conditions. Suitable additives for this purpose include, but are not limited to, brominated polystyrene (including brominated syndiotactic polystyrene), hexabromocyclododecane, decabromodiphenyl oxide, ethylene-bis (tetrabromophthalimide). ), Ethylene-bis (dibromoboranedicarboximide), pentabromodiphenyl oxide, octabromodiphenyl oxide, decabromodiphenoxyethane, poly-dibromophenylene oxide, halogenated phosphorus ester, tetrabromophthalic anhydride, bis ( Tribromophthalic anhydride), tetrabromobisphenol-A bis (2-hydroxy ether), tetrabromobisphenol-A bis (2,3-dibromopropyl ether), dibromo-neopentyl glycol Tetra Decabromodiphenyl diphenoxybenzene, aluminum oxide trihydrate, antimony oxide, sodium antimonate, zinc borate, and diacrylate esters of tetrabromobisphenol -A encompassed.
[0106]
Suitable heat and light stabilizers include, but are not limited to, calcium stearate, phenol and hindered phenol, zinc oxide, aryl esters, hydroxybenzophenone, and hydroxybenzotriazole.
[0107]
Suitable antioxidants include phosphorus based antioxidants, phenolic antioxidants and sulfur based antioxidants. Examples of phosphorus-based antioxidants are tris (2,4-di-t-butylphenyl) phosphite and tris (mono / di-nonylphenyl) phosphite, distearylpentaerythritol diphosphite; dioctylpentaerythritol diphosphite. Phyte; diphenylpentaerythritol diphosphite; bis (2,4-di-t-butylphenyl) pentaerythritol diphosphite; bis (2,6-di-t-butyl-4-methylphenyl) pentaerythritol diphosphite , Dicyclohexylpentaerythritol diphosphite; tris (2,4-di-t-butylphenyl) phosphite; tetrakis (2,4-di-t-butylphenyl) -4,4-biphenylene phosphite Includes monophosphite and diphosphate
[0108]
Suitable phenolic antioxidants include 2,2′-methylenebis (6-tert-butyl-4-methylphenol); 1,1-bis (5-tert-butyl-4-hydroxy-2-methylphenyl) Butane; 2,2'-methylenebis (4-methyl-6-cyclohexylphenol);
4,4'-thiobis (6-tert-butyl-3-methylphenol); 2,2-bis (5-tert-butyl-4-hydroxy-2-methylphenol) -4-dodecylmercapto-butane, 2, 6-di-t-4-methylphenol; 2,2′-methylenebis (6-t-butyl-4-ethylphenol); 2,2′-methylenebis-4-methyl-6- (α-methylcyclohexyl) phenol 2,2′-methylenebis (4-methyl-6-nonylphenol); 1,1-bis (3,5-dimethyl-2-hydroxyphenyl) -3- (n-dodecylthio) -butane; 1,3,5 -Tris (3,5-di-t-butyl-4-hydroxybenzyl) -2,4,6-trimethylbenzene; 2,2-bis (3,5-di-t-butyl-4-hydroxybenzyl) dioc Decyl malonate ester; n-octadecyl-3- (4-hydroxy-3,5-di-tert-butylphenyl) propionate, tetrakismethylene (3,5-di-tert-butyl-4-hydroxyhydrocinnamate) methane , 3,9-bis-1,1-dimethyl-2- (β- (3-t-butyl-4-hydroxy-5-methylphenyl) propionyloxy) ethyl-2,4,8,10-tetraoxaspiro -5,5-undecane, tris- (3,5-di-t-butyl-4-hydroxybenzyl) isocyanurate, 2,6-diphenyl-4-methoxyphenol, and tris- (4-t-butyl-2 , 6-dimethyl-3-hydroxybenzyl) isocinurate.
[0109]
Suitable sulfur-based antioxidants include: dilauryl-3,3'-thiodipropionate; dimyristyl-3,3'-thiodipropionate; distearyl-3, -3'-thiodipropionate; Erythritol-tetrakis- (β-lauryl-thiodipropionate), bis-2-methyl-4- (3-n-alkylthiopropionyloxy) -5-t-butylphenyl sulfide, and 2-mercaptobenzimidazole are included. You.
[0110]
Useful pigments are well known in the literature and include, but are not limited to: cadmium mercury orange, cadmium sulfide yellow, cadmium sulfoselenide, titanium dioxide, titanium yellow, titanium green, titanium blue, cobalt aluminate, manganese blue, Inorganic pigments such as manganese violet, ultramarine red, ultramarine blue, and ultramarine violet; and permanent red 2B, perylene red, quinacridone red, diazo orange, diazo yellow, isoindolinone, hansa yellow, phthalocyanine green, phthalocyanine blue Quinacridone violet, and organic pigments such as doxazine violet.
[0111]
Suitable antifungal agents are antibacterial or other agents that impart resistance to the polymer to bacteria, mildew or mold. Suitable antistatic agents include conductive or zwitterionic substances known to impart antistatic properties to the fibers.
[0112]
In one mode of operation, a concentrate of pigments or other additives in a suitable base resin is added to an extruder along with one or more compositions (a) and (b). Alternatively, pigments or other additives may be pre-composed in such resins. The use of a concentrate facilitates control of the amount of additive and improves the ability to include the additive in the final composition. It is obvious to a skilled person that pigments or other additives may be added mainly to only one component of the composition. The advantage of this embodiment is that pigments or other additives that are detrimental to one component can be included primarily only in the other component. For example, certain organic pigments may crosslink the polymer, thereby producing spheroids that increase its melt viscosity and weaken the fibers, resulting in thread breaks in the spinning process. Conversely, some inorganic pigments may catalyze the depolymerization of the polymer, increasing the number of functional end groups that affect dye sensitivity and reducing viscosity. By including such pigments primarily in one phase, some or all of the aforementioned problems can be reduced or eliminated, at least at the beginning of the fiber forming process. In a preferred embodiment, improved performance can be achieved by selectively including additives in minor components, especially where the substance is more miscible with component (b) than with component (a). Further, by concentrating the additive only in the dispersed phase, under certain conditions, equivalent performance can be obtained using a small amount of additive. For example, when employing antifungal agents, the protrusions of the occlusions of component (b) on the fiber surface are made possible by the fact that they are more exposed on the surface of the fiber or film and are more accessible to the environment.
[0113]
In a highly preferred embodiment, component (b) is as an alloy or concentrate containing any additives desired in the formulation, especially compatibilizers (c), matting agents, colorants, and / or other additives. Supplied. The concentrate containing a minor portion of component (a) is then sufficient to feed the equipment used in the fiber or film forming process or a fully formulated polymer mixture suitable for fiber or film formation to a die or spinneret. Melt blended with component (a) in a separate extruder or other melt mixing device. In order to obtain sufficient mixing and particle size of component (b) under such conditions, an example of a suitable mixing device incorporated in a conventional fiber-forming extruder is disclosed in US Pat. No. 783 and U.S. Pat. No. 5,451,106.
[0114]
In a particularly preferred embodiment, the molten polymer blend is extruded or dispersed mixed, expanded flow mixed, or so that proper mixing of the molten polymer is achieved to achieve the desired dispersed phase particle size described herein. Pass through a stirrer unit, which is any zone in the separately added mixing device utilizing their combination.
[0115]
In compounding polymers, distributive mixing is effectively done by using a so-called "motionless mixer" or "static mixer" between a screw feeder and a die. In most cases, they consist of N right-handed and left-handed alternating spiral elements placed in a tubular housing equipped with temperature control means. Mixing energy is provided by the pressure drop created by mixing. The splattering and recombination of the flow is a^N Will occur. The basic theory in distributed mixing is flow distribution and recombination. Since the flow distribution is of the shear type, the distribution forces are usually weak and the device works best when the liquids being mixed have the same viscosity. For two liquids, this relationship is λ = η_d/ Η_mRepresented by $ 1:
Where η_d And η_m Is the shear viscosity of the dispersed phase and the matrix, respectively. In contrast, in an extended flow mixer, the mixing action is less dependent on the viscosity ratio. It has already been determined whether Newtonian or non-Newtonian liquids of different viscosities are more effective in extended flow than in shear flow.
[0116]
Expanded flow occurs when fluid converges from the reservoir to the capillary. In general, the expanded flow tends to transform into a horizontally elongated ellipse, and at the end of flow decomposition, tends to transform into a continuous microdroplet having a diameter twice the small diameter of the horizontally elongated ellipse. Good dispersion levels are obtained by dispersing the minor phase of a multiphase system into microdroplets in a system having a contiguous or dispersed continuous phase with a limited small diameter. A preferred extended flow mixer comprises a continuous plate placed along a fluid conduit. With these plates, the fluid mixture is flowed through a series of convergence and dispersion. In order to produce a continuously increasing convergence and dispersion intensity that increases continuously, a design is employed in which these limiting diameters are kept constant or continuously decreasing. In addition, the fluid mixture is exposed to a strong expanding flow field, each followed by a semi-stationary zone, wherein the overall flow direction of such a mixer is more radial than axial in view of the normal flow of the extruder, such that A design that incorporates an area in which each opening of the mixer is slit-shaped rather than a hole, preferably at least some of which are slits that can be adjusted to different widths, is highly desirable.
[0117]
About the formation of filaments, fibers and yarns
The compositions of the present invention can be obtained by dry blending the various components and additives prior to feeding the blend to two or more components, and preferably all components, to an extruder or other melt mixing device, or In any order, the individual components can be fed directly to such an extruder or apparatus, as long as sufficient agitation is provided while in the molten state to prepare a composition having the morphology of Formed by the above method. The composition is formed into strands or pellets after preparation, but in a preferred embodiment, the composition is formed by the operation of a die or spinneret used to make films and fibers in an extruder. Highly desirably, component (a) is first added to the extruder and melt plasticized. Thereafter, in one or more additional zones of the extruder, after heating the melt of component (a), preferably above its crystalline melting point, and optionally above the crystalline melting point of component (b), component (b) It is added at the same time as the other components of the composition, before or after their addition. The molten plasticized composition is then passed through a die or spinneret, optionally after cooling to a temperature between the crystalline melting points of components (a) and (b), and formed into fibers in one or more unit operations. . By not reheating and re-extruding prior to compounding and pelletizing versions of the composition, polymer degradation is reduced and operating costs are reduced.
[0118]
The composition is preferably extruded from the extruder through a die or spinneret at a temperature that allows the composition to flow easily but maintains sufficient melt tension to avoid fiber or film breakage. Preferably, the temperature of the polymer melt is maintained at least in the range of the decomposition temperature of components (a) and (b), Td, below. Td is defined as the temperature at which the rate of weight loss of the polymer is 1% / min under vacuum. Preferred temperatures for the extrusion and spinning of the present invention are in the range of 170-340C, more preferably 200-320C, and most preferably 250-300C. The extruder temperature is selected based on the desired properties of the resulting filament, film or fiber and, among other factors, the desired processing speed.
[0119]
The spinneret is designed to give the filament the desired cross-sectional shape commonly used in the industry, including, for example, triangles, multi-projections, pentagons, and the like. The filament has one or more axial voids. Further, the filaments may be mono- or multi-component, i.e., the filaments may comprise strands joined at one or more lengths with the same length. Examples of multicomponent fibers include fibers having core-sheath, side-by-side, or the same strand arrangement. The compositions of the present invention are used to make such multicomponent filaments or one component of all such components depending on the desired properties of the filaments, fibers, or yarns. In such processes, multiple feed block dies are used in known procedures, examples of which are disclosed in U.S. Patent Nos. 6,024,556, 6,162,382, and others.
[0120]
In the production of fibers particularly suitable for carpets, spinnerets having a plurality of orifices forming a large number of filaments are usually employed during the spinning process. As the extruded filament exits the spinneret, the filament is quenched with cross-flow gas, typically air. The filament is then drawn, optionally textured and / or crimped, optionally reheated, and finally cooled, collected as a yarn and wound onto a take-up spool. Crimp imparts a high bulk to the yarn, and thus a high bulk to the carpet. The crimping process causes the fiber to undergo one or more bends and deformations, preferably in alternating directions. Generally, the crimped fibers are then exposed to heat in a dry atmosphere or in the presence of steam to increase the crystallinity and crimp "strain" of the polymer component.
[0121]
As a further example of the invention, particularly when component (a) is nylon, the extrusion step comprises: (i) bringing the composition to the ultimate temperature, preferably 260-330 ° C, more preferably 285-295 ° C. Transporting the composition through an extruder characterized by heating, mixing and transport zones, or a combination thereof, to raise the composition to a desired filament shape via a volumetric melt pump. Feed to a group of spinnerets consisting of holes, wherein the spinnerets are adjusted to produce multiple extruded fibers; and (iii)
Cooling the extrudate by passing it through a quench zone, preferably operating at 10-20 ° C.
[0122]
After extrusion, the filament is drawn one or more times, preferably twice. Post-forming processes such as texture rise, crimp, heat treatment, dyeing, bulking, entanglement, coating, winding, cutting and carding are likewise performed. The filaments may also be processed into already known forms, including bulk continuous filaments, staple fibers, combinations of the former, carded and uncarded yarns or strands, and multifilament yarns, twisted or untwisted. The rough surface of the fibers of the present invention provides higher fiber-fiber internal friction and is advantageous for processing staple fibers into yarn.
[0123]
As already mentioned, the thermoplastic composition of the present invention desirably produces a form in which component (b) is occluded in a matrix of component (a). In the drawing of the fibers of the present invention, and in the orientation of the film according to the present invention, some of the above-mentioned occlusions also form protrusions and bumps on the surface of the fiber or film. In a preferred embodiment, such occlusions have a minor axis, or diameter, of 0.2-3.0 μm on a volume average basis and the particles or occlusions have a substantially volume average length: diameter ratio of 1-. 20 with an oval, spherical, cylindrical, oval, or "sausage" shape. The morphology of such fibers may result in the desired amount of fibers and films, preferably a surface roughness sufficient to improve the optical or physical properties, or the molding or manufacturing properties of one or more fibers or films. Was found.
[0124]
While not wishing to be bound by theory, the advantage gained, especially when manufacturing fibers using the above-described composition, is that the thermoplastic polymer (b) is incorporated into the continuous matrix of the thermoplastic polymer (a) during the fiber formation process. Are thought to contribute, at least in part, to the ability to form dispersed, discontinuous domains. In particular, by using a lower amount of the thermoplastic polymer (b) compared to the amount of the thermoplastic polymer (a) and having the essential thermal properties, such dispersed, discontinuous domains are typical. It is believed that it forms under typical fiber forming conditions. If a high concentration of thermoplastic polymer (b) is employed, those fibril networks or components (a) extending into the continuous phase of component (a) are dispersed in the matrix of component (b). Structure that is easy to generate. In addition, the high crystallization temperature of polymer (b) is such that the fiber-forming operation occurs at a temperature above the crystallization temperature (Tc) of the polymer (a) upon cooling, so that the drawn yarn of the matrix or the polymer of the continuous phase can Ensuring that relatively crystallized occlusions are formed in the stretchable matrix, such as to produce protrusions on the surface. A small amount of drawing of the occlusion phase particles likewise occurs, whereby some properties of the fiber, such as stiffness and crimp, result from the crystallization of component (b) rather than component (a).
[0125]
The resulting fiber morphology is affected by spinneret design, spin rate, amount and efficiency of component (c), extrusion mixing capability, and other physical and operating variables. Most desirably, the composition has sufficient melt tension after extrusion and quenching so that the fiber has a high linear velocity, suitably at a speed after drawing, at least 1000 m / min, preferably at least 1500 m / min, more preferably It is prepared at a speed of at least 2000 m / min, and most preferably at least 2500 m / min. Even more preferably, the resulting fully drawn fiber is characterized by a stiffness of at least 1.0 g / denier, more preferably at least 1.8 g / denier.
[0126]
As already disclosed in aspect K of the present invention, for example, a first polymer that is the same as polymer (a) is encapsulated or coated with one or more layers of one or more second polymers. There are advantages to forming bi- or multi-component fibers or bi- or multi-layer films such that at least one of such layers is comprised of the composition disclosed above, which has been employed to form the polymeric regions. is there. In embodiments of the present invention, the amount of component (b) in the composition is two times less than that employed in a single component fiber or film because the amount of the coating composition is small compared to the total volume of the fiber. Increase by a factor of three or three or more. That is, the amount of component (b) in such compositions ranges as high as 99% by weight, as previously disclosed.
[0127]
The fiber or the resulting yarn is dyed in a post-forming operation. Suitable dyes include organic solvent vehicle dyes (disperse dyes) or aqueous dyes such as acid dyes, pre-neutralized dyes, and cationic dyes. Examples include mono- and disulfonic acid dyes as well as triphenylmethane, pyrazolone, azine, nitro and quinoline dyes. Preferred dyes are mono and disulfonic acid dyes. If desired, one or more dyes can be applied and, if desired, different fibers in the yarn or strand can be separately dyed.
[0128]
In the dyeing process, the filaments, fibers or yarns are preferably firstly usually treated with NaOH, KOH or NH.₄ It is washed with hot water containing a base such as OH. The hot water wash temperature must be in the range of 60-180 ° C and high enough to remove residual oils such as lubricants. The filaments, fibers or yarns are then passed through a dye bath and contacted at an optionally elevated temperature, preferably at a bath temperature of 80 ° C-100 ° C for 0.1-30 minutes to fix the dye, if desired. Heated, washed, rinsed and dried. Dye baths are typically operated at atmospheric pressure.
[0129]
It is known to treat synthetic fibers with various agents to increase or decrease the fiber's affinity for certain dyes. For example, the polymer chains can be replaced with additional reactive groups or shortened to provide additional end groups, thereby providing an increased number of dye sites and a consequent increase in dyeability. Instead, the polymer reacts with a capping agent to reduce the dyeability of certain dyes, reducing the number and effectiveness of the functional end groups. Unfortunately, such processes alter the melting properties and crystallinity of the polymer, thereby affecting the spinnability of the fiber and its ability to later modify the properties of the fiber. The present invention provides a method for reducing the dyeability of fibers formed without necessarily affecting the spinnability or denaturing properties of the fibers. The present invention is practiced using conventional bright dye and deep dye techniques.
[0130]
Dye uptake is affected by the crystal structure of the fiber. Amorphous polymer regions are generally easier to accept water-based dyes than crystalline polymer regions. The formation of large crystals in the fiber results in a large amount of amorphous polymer and relatively non-occluded amorphous regions. The formation of relatively small crystals generally reduces the number of non-occluded amorphous regions and the total amount of amorphous polymer. In the fibers according to the invention, the storage area of the additional component (b) is a different crystal independent of the crystal structure according to component (a) and a modified crystal morphology (an inherently different water transport). Rate and equilibrium moisture content), thereby correcting fiber uptake changes resulting from changes in thermal history between different fibers. In particular, the fibers of the present invention generally have a reduced strike rate as compared to fibers made entirely or substantially from component (a). For this reason, the fibers of the present invention have inherently improved stain resistance.
[0131]
Desirably, the filaments or fibers range from 0.5 denier to 60 denier, and preferably 1 denier to 30 denier. The fibers are staple fibers, continuous fibers, bulk continuous filaments ("BCF"), or mixtures thereof; continuous forms are preferred.
The yarn is produced from the aforementioned filaments or fibers according to known techniques.
[0132]
Coatings can also be applied to the filament before and after drawing. Preferred coatings include lubricants, antistatics, sealants, and metallic luster coatings. The inherent surface roughness of the fibers of the present invention and the reduced friction on rollers and guides used in the post-processing process reduce the amount of lubricant generally required when processing yarns according to the present invention. Or no need at all. If used, the amount of finish is generally 0.5-2.5% based on total fiber weight.
[0133]
One means of drawing the filaments of the present invention is (i) feeding the quenched filaments to multiple sets of godets operated at gradually increasing speeds, thereby bringing the filaments to the desired draw ratio. In a preferred embodiment, the first godet operates at 600-1000 m / min, preferably 600 m / min and the final godet operates at 1200-6000 m / min, preferably at least 1800 m / min. The skilled artisan will recognize that these stretching conditions can be varied without affecting the operability of the present invention.
[0134]
The fibers may be textured or crimped using any suitable technique. One such process uses a texturing air jet using hot air to crimp the fibers. Preferably, the texturing air jet is of the split type operating at an air pressure of 3.0-10.0 bar (0.3-1.0 MPa) and a temperature of 120-180 ° C. The crimped fibers are taken up in a zigzag or perforated drum to cool the fibers through air and fix the crimp. Alternatively, or if desired, the multifilaments are entangled with the filaments through interlaced air jets, preferably using an air pressure of 1.0-8.0 bar (0.1-0.8 MPa) and the resulting yarn Add bulk. In a final operation, the fibers or a combination thereof are wound on a cylindrical package, bobbin or spool. Preferably, the bulky fibers have a denier of 100-1000.
[0135]
In a further embodiment, two or more fibers wound into separate packages are sent to a twisting process to make multiple yarns. A suitable twisting process comprises the steps of combining at least two separate, preferably crimped fibers with Verdol, Inc. Or Volkmann, Inc. Into a yarn with a twisting machine manufactured by the company. Preferably, multiple yarns of 600-8000 denier with 2-9 twists per inch, preferably double yarns of 800-1500 denier with 3-6 twists per inch are produced. Preferably, the twister is operated at a spindle speed of 5000-8000 revolutions / minute. Those skilled in the art will appreciate that the fibers of the present invention may also combine one or more fibers, with or without twist, to produce a yarn having the desired properties. For example, multiple fibers are produced comprising at least two different fiber types, at least one of which is produced according to the present invention. The remaining fibers are conventional natural or synthetic fibers or fibers different from those according to the invention.
[0136]
In some applications, particularly carpet making, the yarn is subjected to various heat treatments to give the fibers a final level of crystallinity. Heat setting gives the yarn dimensional stability and improved heat resistance. In the case of twisted multiple yarns, heat setting reduces mechanical twisting stresses and improves the twist retention and appearance of carpets made from such twisted yarns. Generally, the process involves heating the yarn to an appropriate temperature, generally without the presence of stress, for a period of time and in a manner to achieve the desired yarn properties. Suitable heat setting processes include the Superba or Sussen process.
[0137]
Generally, strict control of the time and temperature in the heat setting process is necessary to produce yarns with uniform dyeability. In addition, many yarns shrink as a result of the heat setting process, thereby increasing denier variability. Advantageously, the yarns according to the invention are less susceptible to dyeing and streaks and are therefore more tolerant of variations in the heat setting process. In addition, the yarns of the present invention and products made therefrom have less shrinkage during heat setting, washing, dyeing, or other processing steps, and use than conventional yarns. Preferred yarns, especially twisted, heat set, multiple yarns, show less than 15% denier reduction on heat setting at 130 ° C. for 1 minute.
[0138]
The fibers according to the invention desirably have a high modulus compared to fibers made alone or substantially from component (a). Carpets containing yarns according to the invention are characterized by improved stain resistance, stain resistance and increased durability. This effect is particularly emphasized when component (a) comprises a resin having a low elastic modulus such as polyester. The relatively rough surface of the fiber of the present invention contributes to its enhanced soil release properties because the coarse particles cannot contact most of the fiber surface as occurs with a smooth fiber surface. In addition, the rough surface of the fiber is rich in coarse particles that can be easily removed by washing or vacuum washing in a yarn bundle or carpet pile.
[0139]
The yarns of the present invention are used to weave or knit garment fabrics using standard knitting techniques known to those skilled in the art. Due to the high interfiber frictional forces obtained by using the fibers and yarns of the present invention, fabrics made from these fibers provide a more uniform fabric structure, less streaks, and fewer rags. The processability of the yarn according to the invention has the advantage that, due at least in part to the nature of its surface, a reduced process stress, an improved stretchability and a reduced roll winding can be obtained.
[0140]
About carpet manufacturing
The yarns of the present invention can be easily processed for carpet, mat, and floor and wall covering applications. To make carpets, yarns, especially twisted yarns, are tufted, braided, or melt knitted into a backing. The resulting carpet, called "greige good", may be dyed to a suitable color. Next, the back of the carpet is coated with a suitable adhesive or sealant, such as latex, and dried to bond the tufted yarn to the first backing. If desired, then attach a second backing to the back of the carpet. The tufted yarn is then optionally subjected to known cutting operations to form loop pile, cut pile or loop and cut pile type carpets. In addition, multiple ends of the multiply yarns are included in the textile backing to texture the surface to obtain the desired carpet design.
[0141]
Dyeing of carpet is carried out in a batch or continuous process using the dyes mentioned above for dyeing fibers or yarns. Conventional deep dyeing and bright dyeing techniques, space dyeing techniques, knit-denit dyeing techniques, etc. can all be used.
[0142]
Preferably, the carpet is dyed by passing through an aqueous dyeing unit such as is commercially available from Otching or Couster. The carpet passes through the unit by means of a conveyor. Generally, the carpet is first pre-wetted, for example, by passing water with a wetting agent or surfactant. The carpet then passes between nip rolls to remove excess water and then comes into contact with a medium called "liquor" containing dyes and dyeing aids. Typically, in the acid dye process, the pH of the liquor is maintained at 4.5-8. Liquor is sprayed onto the carpet or applied by a blade device from a reservoir. The carpet then passes through a heating chamber, such as a steam heated container, to fix the dye on the carpet. The carpet is then washed, rinsed and dried to remove residual liquor from the carpet. If desired, a stain resistant or stain blocker, such as a silane compound, may be included in the dye liquor or may be applied to the carpet simultaneously or in a subsequent drying process. Conventional stain and stain resistant techniques can be used for the fibers, carpets and fabrics of the present invention.
[0143]
The carpet or rug according to the invention preferably exhibits at least one of the following contributions: reduced dye streaking, reduced soiling, improved color fixability when washing, improved color fixability to UV light, Improved hand, improved recovery, or improved durability; comparison in each case to a carpet or rug consisting of fibers made from a composition that does not contain the thermoplastic polymer component (b).
[0144]
wrap up
The following is a summary of certain aspects of the invention fully described and disclosed herein.
[0145]
1. (A) 86-92% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C.
(B) 14-8% by weight of a second thermoplastic polymer chemically different from (a) having a crystallization temperature, Tc ', and
(C) a compatibilizer for (a) and (b),
Wherein the percentage is based on the total amount of (a) and (b), and Tc is at least 5 ° C. less than Tc ′, wherein the thermoplastic polymer composition is useful for producing extruded fibers and films. object.
[0146]
2. The composition according to embodiment 1, wherein the first thermoplastic polymer is a polyamide or copolyamide and Tc 'is greater than 195C.
[0147]
3. The composition of embodiment 1 wherein the first thermoplastic polymer is a polyamide or copolyamide and the second thermoplastic polymer is a polyvinylidene aromatic polymer having an isotactic or syndiotactic steric structure.
[0148]
4. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl-, halo-, or polar-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 The composition according to embodiment 3, which is a polar group-modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar-substituted vinyl aromatic monomer.
[0149]
5. The composition according to embodiment 3, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180.
[0150]
6. The second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl- or halo-substituted vinyl aromatic monomers or polar group-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 The composition according to embodiment 5, which is a polar group modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar group-substituted vinyl aromatic monomer.
[0151]
7. The composition according to embodiment 5, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000.
[0152]
8. The composition according to embodiment 1, having a yellow index, YI, of less than 10.0.
[0153]
9. The composition according to embodiment 1, comprising 0.1-10% of compatibilizer c) based on the total composition weight.
[0154]
10. The composition according to embodiment 9, wherein the compatibilizer is a polar group-modified vinylidene aromatic homopolymer or copolymer.
[0155]
11. The compatibilizer is a polar group-modified polystyrene, a copolymer of one or more vinyl aromatic monomers and one or more polar comonomers, or styrene and one or more cyclic C_1-10 The composition of embodiment 10, which is a polar group-modified copolymer of an alkyl- or halo-substituted vinyl aromatic monomer or a polar group-substituted vinyl aromatic monomer.
[0156]
12. The compatibilizer is a maleic anhydride-modified or fumaric acid-modified styrene homopolymer or styrene and at least one cyclic C_1-10 A maleic anhydride- or fumaric-acid-modified styrene copolymer with an alkyl-substituted styrene, wherein the compatibilizer has 0.01-5.0 mol% of copolymerized maleic anhydride or fumaric acid functionality. 12. The composition according to 11.
[0157]
13. 13. The composition according to any of embodiments 1-12, wherein after formation of the fiber or film, component (b) is present in the matrix of component (a) in the form of occluding particles having a volume average short axis diameter greater than 0.2 μm. .
[0158]
14． 14. The composition according to embodiment 13, wherein after formation of the fiber or film, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.3-2.0 μm.
[0159]
15. After formation of the fiber or film, component (b) is less than 3.0 μm D⁹⁹14. The composition according to embodiment 13, which is in the form of occluded particles having a short axis diameter.
[0160]
16. After formation of the fiber or film, component (b) has a D of less than 2.8 μm.⁹⁹15. The composition according to embodiment 14, which is in the form of occluded particles having a short axis diameter.
[0161]
17． After formation of the fiber, component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber is a laser having a particle size of at least 0.29. 13. The composition according to any of embodiments 1-12, having a light scattering ratio or a gloss judge rating of 4.0 or less as determined on a standard fiber sample.
[0162]
18. After fiber formation, component (b) is present in the form of occluded particles with a volume average minor axis diameter of 0.2-3.0 μm and the fiber is determined by a laser light scattering ratio or a standard fiber sample of 0.29 or greater. 16. The composition according to aspect 15, wherein the composition has a gloss judge rating of 4.0 or less.
[0163]
19. An embodiment in which, after the formation of the fibers, component (b) is present in the matrix of component (a) in the form of occluding particles having a volume-average minor axis diameter of 0.2-3.0 μm and the fibers have a soft hand 13. The composition according to any one of 1-12.
[0164]
20. 16. The composition according to embodiment 15, wherein after formation of the fibers, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fibers have a soft hand.
[0165]
21. The amount of component (c) is in the range of 0-5% based on the combined weight of components (a) and (b) and the sum of the reactive, functional groups in component (c) (if present) 13. The composition according to any of aspects 1-12, wherein the amount is 0.001-0.25 mol%, based on the total amount of component (b) and component (c).
[0166]
22. Embodiment 15. The fiber according to embodiment 15, wherein after formation of the fiber, component (b) is present in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability. Composition.
[0167]
23. After formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability. Composition.
[0168]
24. Aspect 20. After the formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability. Composition.
[0169]
25. 13. The composition according to any of aspects 1-12, further comprising 0.1-10.0% of the matting agent based on the total composition weight.
[0170]
26. (A) 76-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C.
(B) 24-3% by weight of a second thermoplastic polymer chemically different from (a) having a crystallization temperature, Tc ', and
(C) a compatibilizer for (a) and (b),
Here, the percentage is based on the total amount of (a) and (b), and Tc is at least 5 ° C. smaller than Tc ′. An extruded drawn fiber comprising a thermoplastic polymer composition.
[0171]
27. 27. The fiber of embodiment 26, wherein the first thermoplastic polymer is a polyamide or copolyamide and has a Tc 'of greater than 195C.
[0172]
28. 27. The fiber of embodiment 26, wherein the first thermoplastic polymer is a polyamide or copolyamide and the second thermoplastic polymer is a polyvinylidene aromatic polymer having an isotactic or syndiotactic steric structure.
[0173]
29. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl-, halo-, or polar-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 29. The fiber of embodiment 28 which is a polar group modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar-substituted vinyl aromatic monomer.
[0174]
30. 28. The fiber according to 27, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180.
[0175]
31. The second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl- or halo-substituted vinyl aromatic monomers or polar group-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 Embodiment 31. The fiber of embodiment 30, which is a polar group modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar group-substituted vinyl aromatic monomer.
[0176]
32. The fiber of embodiment 30, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000.
[0177]
33. 27. The fiber of embodiment 26 having a yellow index, YI, of less than 10.0.
[0178]
34. 27. The fiber of embodiment 26 comprising 0.1-10% of compatibilizer c) based on the total composition weight.
[0179]
35. The compatibilizer is a polar group-modified polystyrene, a copolymer of at least one vinyl aromatic monomer and at least one polar comonomer, styrene and at least one cyclic C_1-10 35. The fiber of embodiment 34 which is a polar group modified copolymer of an alkyl- or halo-substituted vinyl aromatic monomer or a polar group-substituted vinyl aromatic monomer.
36. When the compatibilizer is a polar group-modified polystyrene or styrene and at least one cyclic C_1-10 The fiber of embodiment 35, which is a polar group-modified copolymer of an alkyl- or halo-substituted vinyl aromatic monomer or a polar group-substituted vinyl aromatic monomer.
[0180]
37. The compatibilizer is a maleic anhydride-modified or fumaric acid-modified styrene homopolymer or styrene and at least one cyclic C_1-10 A maleic anhydride- or fumaric-acid-modified styrene copolymer with an alkyl-substituted styrene, wherein the compatibilizer has 0.01-5.0 mol% of copolymerized maleic anhydride or fumaric acid functionality. 36. The fiber according to 36.
[0181]
38. 38. The fiber according to any of aspects 26-37, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter greater than 0.2 µm.
[0182]
39. The fiber of embodiment 38, wherein component (b) is present in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 μm.
[0183]
40. D in which the component (b) is smaller than 3.0 μm⁹⁹The fiber of embodiment 38, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0184]
41. D in which the component (b) is smaller than 2.8 μm⁹⁹The fiber of embodiment 39, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0185]
42. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. 38. The fiber according to any of aspects 26-37, having a gloss judge rating of 4.0 or less as determined on the fiber sample.
[0186]
43. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. The fiber of embodiment 40, having the following gloss judge grade:
[0187]
44. Any of embodiments 26-37, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a soft hand. The fiber described in the crab.
[0188]
45. 41. The fiber of embodiment 40, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm, and wherein the fiber has a soft hand.
[0189]
46. The amount of component (c) is in the range of 0-5% based on the combined weight of components (a) and (b) and the sum of the reactive, functional groups in component (c) (if present) 38. The fiber according to any of aspects 26-37, wherein the amount is 0.001-0.25 mol%, based on the total amount of component (b) and component (c).
[0190]
47. The fiber of embodiment 40, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability.
[0191]
48. Aspect 38-37, wherein the composition comprises 80-95% by weight of component (a); and 20-5% by weight of component (b), based on the total weight of component (a) and component (b). Fiber.
49. 38. Any of embodiments 26-37, wherein the composition comprises 86-92% by weight of component (a); and 14-8% by weight of component (b), based on the total weight of component (a) and component (b). Fiber.
50. 38. The fiber of any of embodiments 26-37, further comprising 0.1-10.0% of the matting agent based on the total composition weight.
[0192]
51. (A) 65-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C., and
(B) 35-3% by weight of a second thermoplastic polymer which is chemically different from (a) and has polar functional groups with a crystallization temperature, Tc ', and optionally one or more non-polymer additions A thermoplastic polymer composition useful in the manufacture of extruded fibers and films, characterized by consisting essentially of a product.
[0193]
52. 52. The composition according to embodiment 51, wherein the first thermoplastic polymer is a polyamide or copolyamide and Tc 'is greater than 195C.
[0194]
53. 52. The composition according to embodiment 51, wherein Tc is at least 5 <0> C lower than Tc '.
[0195]
54. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl-, halo-, or polar-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 52. The composition according to embodiment 51, which is a polar group modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar group-substituted vinyl aromatic monomer.
[0196]
55. 53. The composition according to embodiment 52, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180.
[0197]
56. 52. The composition according to embodiment 51, wherein the second thermoplastic polymer is a syndiotactic polystyrene or a polar group modified derivative of a syndiotactic copolymer of styrene and p-methylstyrene.
[0198]
57. The composition according to embodiment 51, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000.
[0199]
58. 52. The composition according to embodiment 51, having a Yellow Index, YI, of less than 10.0.
[0200]
59. The composition according to embodiment 51, comprising 5.0-20% by weight of component (b) as an essential component.
[0201]
60. The composition according to embodiment 59, comprising 8-14% by weight of component (b) as an essential component.
[0202]
61. 57. The composition according to embodiment 56, wherein the second component is a maleic anhydride- or fumaric acid-modified syndiotactic polystyrene or a maleic anhydride- or fumaric acid-modified syndiotactic copolymer of styrene and p-methylstyrene.
[0203]
62. The composition according to embodiment 61, wherein component (b) has a copolymerized maleic anhydride or fumaric acid functionality of 0.01-5.0 mol%.
[0204]
63. 63. The composition according to any of embodiments 51-62, wherein after formation of the fiber or film, component (b) is present in the matrix of component (b) in the form of occluded particles having a volume average short axis diameter greater than 0.2 μm. .
[0205]
64. 64. The composition according to embodiment 63, wherein after formation of the fiber or film, component (b) is present in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 μm.
[0206]
65. After formation of the fiber or film, component (b) is less than 3.0 μm D⁹⁹The composition according to embodiment 63, wherein the composition is in the form of occluded particles having a short axis diameter.
[0207]
66. After formation of the fiber or film, component (b) has a D of less than 2.8 μm.⁹⁹The composition according to embodiment 64, wherein the composition is in the form of occluded particles having a minor axis diameter.
[0208]
67. After formation of the fiber, component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber is a laser having a particle size of at least 0.29. 63. The composition according to any of embodiments 51-62, having a light scattering ratio or a gloss judge rating of 4.0 or less as determined on a standard fiber sample.
[0209]
68. After fiber formation, component (b) is present in the form of occluded particles with a volume average minor axis diameter of 0.2-3.0 μm and the fiber is determined by a laser light scattering ratio or a standard fiber sample of 0.29 or greater. The composition of embodiment 65, wherein the composition has a gloss judge rating of 4.0 or less.
[0210]
69. An embodiment in which, after the formation of the fibers, component (b) is present in the matrix of component (a) in the form of occluding particles having a volume-average minor axis diameter of 0.2-3.0 μm and the fibers have a soft hand The composition according to any one of 51 to 62.
[0211]
70. 66. The composition according to embodiment 65, wherein after formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand.
[0212]
71. 63. The composition according to any of embodiments 51-62, wherein the polar group in component (b) is a reactive polar functional group and is present in an amount of 0.001-0.25 mol% of component (b).
[0213]
72. 67. The composition according to embodiment 65, wherein after formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability. Composition.
[0214]
73. 70. The composition according to embodiment 69, wherein after formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability. Composition.
[0215]
74. 70. The composition according to embodiment 70, wherein after formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability. Composition.
[0216]
75. 63. The composition according to embodiments 51-62, further comprising 0.1-10.0% of the matting agent based on the total composition weight.
[0217]
76. (A) 65-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C., and
(B) 35-3% by weight of a second thermoplastic polymer which is chemically different from (a) and has polar functional groups, having a crystallization temperature, Tc ', and optionally one or more non-polymers Extruded drawn fiber characterized by consisting essentially of additives.
[0218]
77. 77. The fiber of embodiment 76, wherein the first thermoplastic polymer is a polyamide or copolyamide and has a Tc 'of greater than 195C.
[0219]
78. 77. The fiber of embodiment 76, wherein Tc is at least 5C lower than Tc '.
[0220]
79. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl-, halo-, or polar-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 77. The fiber of embodiment 76, which is a polar group modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar-substituted vinyl aromatic monomer.
[0221]
80. The fiber of embodiment 77, wherein the polyamide is nylon 6 having a relative viscosity of 30-180.
[0222]
81. 77. The fiber of embodiment 76, wherein the second thermoplastic polymer is a syndiotactic polystyrene or a polar group modified derivative of a syndiotactic copolymer of styrene and p-methylstyrene.
[0223]
82. 77. The fiber of embodiment 76, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000.
[0224]
83. 77. The fiber of embodiment 76 having a yellow index, YI, of less than 10.0.
[0225]
84. The fiber of embodiment 76, comprising 5.0-20% by weight of component (b) as an essential component.
[0226]
85. The fiber of embodiment 84, comprising 8-14% by weight of component (b) as an essential component.
[0227]
86. The fiber according to embodiment 81, wherein the second component is maleic anhydride-modified or fumaric acid-modified syndiotactic polystyrene or a maleic anhydride-modified or fumaric acid-modified styrene and p-methylstyrene syndiotactic copolymer.
[0228]
87. The fiber of embodiment 86, wherein component (b) has a copolymerized maleic anhydride or fumaric acid functionality of 0.01-5.0 mol%.
[0229]
88. 88. The fiber according to any of aspects 76-87, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter greater than 0.2 μm.
[0230]
89. The fiber of embodiment 88, wherein component (b) is present in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 μm.
[0231]
90. D in which the component (b) is smaller than 3.0 μm⁹⁹The fiber of embodiment 88, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0232]
91. D in which the component (b) is smaller than 2.8 μm⁹⁹The fiber of embodiment 89, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0233]
92. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. 88. The fiber according to any of aspects 76-87, having a gloss judge rating of 4.0 or less as determined on the fiber sample.
[0234]
93. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. The fiber of embodiment 90, having the following gloss judge grade:
[0235]
94. Any of embodiments 76-87, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fibers have a soft hand. The fiber described in the crab.
[0236]
95. 90. The fiber of embodiment 90, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm, and wherein the fiber has a soft hand.
[0237]
96. 88. The fiber of embodiments 76-87, wherein the polar groups in component (b) are reactive polar functional groups and are present at 0.001-0.25 mol% of component (b).
[0238]
97. 90. The fiber according to embodiment 90, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm, and wherein the fiber has a soft hand and improved durability.
[0239]
98. 95. The fiber of embodiment 94, wherein component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand and improved durability.
99. The fiber of embodiment 95, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability.
100. 88. The fiber of any of embodiments 76-87, further comprising 0.1-5.0% of the matting agent, based on the total composition weight.
[0240]
101. (A) 65-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C., and
(B) 35-3% by weight of a second thermoplastic polymer which is chemically different from (a) and has polar functional groups, having a crystallization temperature, Tc ', and optionally one or more non-polymers Extruded, drawn, and crimped fibers characterized by consisting essentially of additives.
[0241]
102. The fiber of embodiment 101, wherein the first thermoplastic polymer is a polyamide or copolyamide and has a Tc 'of greater than 195C.
[0242]
103. Embodiment 101. The fiber of embodiment 101, wherein Tc is at least 10C lower than Tc '.
[0243]
104. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl-, halo-, or polar-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 The fiber of embodiment 101, which is a polar group modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar group-substituted vinyl aromatic monomer.
[0244]
105. The fiber of embodiment 102, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180.
[0245]
106. The fiber of embodiment 101, wherein the second thermoplastic polymer is a syndiotactic polystyrene or a polar group modified derivative of a syndiotactic copolymer of styrene and p-methylstyrene.
[0246]
107. The fiber of embodiment 101, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000.
[0247]
108. The fiber of embodiment 101, having a Yellow Index, YI, of less than 10.0.
[0248]
109. The fiber according to embodiment 101, comprising 5.0-20% by weight of component (b) as an essential component.
[0249]
110. The fiber of embodiment 109, comprising 8-14% by weight of component (b) as an essential component.
[0250]
111. The fiber of embodiment 101, wherein component (b) is maleic anhydride modified or fumaric acid modified syndiotactic polystyrene or a maleic anhydride modified or fumaric acid modified styrene and a syndiotactic copolymer of p-methylstyrene.
[0251]
112. 111. The fiber of embodiment 111, wherein component (b) has a copolymerized maleic anhydride or fumaric acid functionality of 0.01-5.0 mol%.
[0252]
113. 113. The fiber according to any of aspects 101-112, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter greater than 0.2 μm.
[0253]
114. The fiber of embodiment 113, wherein component (b) is present in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 μm.
[0254]
115. D in which the component (b) is smaller than 3.0 μm⁹⁹The fiber of embodiment 113, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0255]
116. D in which the component (b) is smaller than 2.8 μm⁹⁹The fiber of embodiment 114, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0256]
117. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. 113. The fiber according to any of aspects 101-112, having a gloss judge rating of 4.0 or less as determined on the fiber sample.
[0257]
118. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. The fiber of embodiment 115, having the following gloss judge grade:
[0258]
119. Any of embodiments 101-112, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a soft hand. The fiber described in the crab.
[0259]
120. 115. The fiber according to embodiment 115, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm, and wherein the fiber has a soft hand.
[0260]
121. The fiber of any of embodiments 101-112, wherein the polar group in component (b) is a reactive polar functional group and is present in an amount of 0.001-0.25 mol% of component (b).
[0261]
122. The fiber of embodiment 115, wherein component (b) is present in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability.
[0262]
123. The fiber of embodiment 119, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability.
[0263]
124. The fiber of embodiment 120, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability.
[0264]
125. The fiber of any of embodiments 101-112, further comprising 0.1-10.0% of the matting agent based on the total composition weight.
[0265]
126. 76-97% by weight of a first thermoplastic polymer consisting of two or more longitudinally-long polymer domains, wherein at least one domain has (a) a crystallization temperature, Tc, greater than 160 ° C;
(B) 24-3% by weight of a second thermoplastic polymer chemically different from (a) having a crystallization temperature, Tc ', and
(C) a compatibilizer for (a) and (b),
Here, the percentage is based on the total amount of (a) and (b), and Tc is at least 5 ° C. smaller than Tc ′, wherein the multicomponent fiber comprises a thermoplastic polymer blend.
[0266]
127. 127. The fiber of embodiment 126, wherein the first thermoplastic polymer of the blend is a polyamide or copolyamide and has a Tc 'of greater than 195C.
[0267]
128. 127. The fiber of embodiment 126, wherein the first thermoplastic polymer of the blend is a polyamide or copolyamide and the second thermoplastic polymer is a polyvinylidene aromatic polymer having an isotactic or syndiotactic steric structure.
[0268]
129. The first thermoplastic polymer of the blend is nylon 6, nylon 6,6 or a copolymer of nylon 6 and nylon 6,6 and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl-, halo-, or polar-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 The fiber of embodiment 128, which is a polar group modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar-substituted vinyl aromatic monomer.
[0269]
130. The fiber of embodiment 128, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180.
[0270]
131. The second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl- or halo-substituted vinyl aromatic monomers or polar group-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 Aspect 130. The fiber of aspect 130, which is a polar group modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar group-substituted vinyl aromatic monomer.
[0271]
132. The fiber of embodiment 130, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000.
[0272]
133. 127. The fiber of embodiment 126, wherein the fiber is a core / sheath fiber and the blend comprises a sheath.
[0273]
134. 127. The fiber of embodiment 126, wherein the blend comprises 0.1-10%, based on total composition weight, of compatibilizer c).
[0274]
135. The compatibilizer is a polar group-modified polystyrene, a copolymer of one or more vinyl aromatic monomers and one or more polar comonomers, or styrene and one or more cyclic C_1-10 The fiber of embodiment 134, which is a polar group-modified copolymer of an alkyl- or halo-substituted vinyl aromatic monomer or a polar group-substituted vinyl aromatic monomer.
[0275]
136. When the compatibilizer is a polar group-modified polystyrene or styrene and at least one cyclic C_1-10 135. The fiber of embodiment 135, which is a polar group-modified copolymer of an alkyl- or halo-substituted vinyl aromatic monomer or a polar group-substituted vinyl aromatic monomer.
[0276]
137. The compatibilizer is a maleic anhydride-modified or fumaric acid-modified styrene homopolymer or styrene and at least one cyclic C_1-10 A maleic anhydride- or fumaric-acid-modified styrene copolymer with an alkyl-substituted styrene, wherein the compatibilizer has 0.01-5.0 mol% of copolymerized maleic anhydride or fumaric acid functionality. 136. The fiber according to 136.
[0277]
138. The fiber according to any of embodiments 126-137, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter greater than 0.2 μm.
[0278]
139. The fiber of embodiment 138, wherein component (b) is present in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 μm.
[0279]
140. D in which the component (b) is smaller than 3.0 μm⁹⁹139. The fiber of embodiment 138, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0280]
141. D in which the component (b) is smaller than 2.8 μm⁹⁹139. The fiber of embodiment 139, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0281]
142. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. The fiber according to any of aspects 126-137, having a gloss judge rating of 4.0 or less as determined on the fiber sample.
[0282]
143. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. The fiber of embodiment 140, having the following gloss judge grade:
[0283]
144. Any of embodiments 126-137, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fibers have a soft hand. The fiber described in the crab.
[0284]
145. The fiber of embodiment 140, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm, and wherein the fiber has a soft hand.
[0285]
146. The amount of component (c) is in the range of 0-5% based on the combined weight of components (a) and (b) and the sum of the reactive, functional groups in component (c) (if present) The fiber according to any of aspects 126-137, wherein the amount is 0.001-0.25 mol%, based on the total amount of component (b) and component (c).
[0286]
147. The fiber of embodiment 140, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability.
[0287]
148. Aspects 126-137, wherein the blend composition comprises 80-95% by weight of component (a) and 20-5% by weight of component (b) based on the total amount of component (a) and component (b). fiber.
[0288]
149. The fiber according to embodiment 133, wherein the core comprises nylon 6 or nylon 6,6.
[0289]
150. Aspect 135. The fiber of any of aspects 126-137, further comprising 0.1-10.0%, by weight of the total composition, of the matting agent.
[0290]
151. (A) 76-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C.
(B) 24-3% by weight of a second thermoplastic polymer that is chemically different from (a) with a crystallization temperature, Tc ', and, if desired,
(C) a compatibilizer for (a) and (b),
Here, the% is based on the total amount of (a) and (b), characterized in that the thermoplastic resin composition comprises a thermoplastic resin composition, and the thermoplastic resin composition comprises a base resin mainly comprising the component (a). Melting and mixing a concentrated resin consisting primarily of component (b) and optionally component (c) and, optionally, small amounts of component (a); and extruding the resulting molten thermoplastic polymer composition into fiber form and Extruded stretched fibers or extruded stretched films produced by stretching or extruding or stretching the resulting thermoplastic polymer composition into film form.
[0291]
152. 152. The fiber or film of embodiment 151, wherein the thermoplastic composition is produced by a melt mixing process that includes elongational flow mixing.
[0292]
153. The fiber or film of embodiment 151, wherein Tc is at least 10 ° C. less than Tc ′.
[0293]
154. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C_1-10 Syndiotactic copolymers of alkyl-, halo-, or polar-substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic C_1-10 153. The fiber or film of embodiment 151 which is a polar group modified derivative of a syndiotactic copolymer with an alkyl-, halo-, or polar group-substituted vinyl aromatic monomer.
[0294]
155. 154. The fiber or film of embodiment 154, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180.
[0295]
156. The fiber or film of embodiment 151, wherein the second thermoplastic polymer is a syndiotactic polystyrene or a polar group-modified derivative of a syndiotactic copolymer of styrene and p-methylstyrene.
[0296]
157. The fiber or film of embodiment 151, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000.
[0297]
158. The fiber or film of embodiment 151, having a Yellow Index, YI, of less than 10.0.
[0298]
159. Aspect 151. The fiber or film of aspect 151, comprising 5.0-20% by weight of component (b) as an essential component.
[0299]
160. The fiber or film of embodiment 159, comprising 8-14% by weight of component (b).
[0300]
161. The fiber or film of embodiment 151, wherein component (b) is a maleic anhydride- or fumaric-acid-modified styrene homopolymer or a copolymer of styrene and p-methylstyrene.
[0301]
162. Embodiment 161. The fiber of embodiment 161 wherein component (b) has a copolymerized maleic anhydride or fumaric acid functionality of 0.01-5.0 mol%.
[0302]
163. 163. The fiber or film according to any of aspects 151-162, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter greater than 0.2 μm.
[0303]
164. 163. The fiber or film of embodiment 163, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 μm.
[0304]
165. D in which the component (b) is smaller than 3.0 μm⁹⁹163. The fiber of aspect 163, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0305]
166. D in which the component (b) is smaller than 2.8 μm⁹⁹164. The fiber of embodiment 164, wherein the fiber is in the form of occluded particles having a short axis diameter.
[0306]
167. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. 163. The fiber of any of aspects 151-162, having a gloss judge rating of 4.0 or less as determined on the fiber sample.
[0307]
168. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. The fiber of embodiment 165, having the following gloss judge grade:
[0308]
169. Any of embodiments 151-162, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fibers have a soft hand. The fiber described in the crab.
[0309]
170. The fiber of embodiment 165, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm, and wherein the fiber has a soft hand.
[0310]
171. The amount of component (c) is in the range of 0-5% based on the combined weight of components (a) and (b) and the sum of the reactive, functional groups in component (c) (if present) 163. The fiber according to any of aspects 151-162, wherein the amount is 0.001-0.25 mol%, based on the total amount of component (b) and component (c).
[0311]
172. The fiber of embodiment 165, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability.
[0312]
173. The fiber of embodiment 169, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability.
[0313]
174. The fiber of embodiment 170, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber has a soft hand and improved durability.
[0314]
175. 163. The fiber of any of embodiments 151-162, further comprising 0.1-5.0% of the matting agent based on the total composition weight.
[0315]
Example
The following examples are given by way of illustration and not by way of limitation and do not exclude the presence of additional additives or ingredients. Unless stated otherwise, all parts and percentages are by weight throughout the specification. In the examples, the following devices, methods and materials were used.
[0316]
Compounding equipment
A Warnerp Fiddler ZSK vented twin screw compound extruder of 40 mm diameter, 34: 1 L / D ratio, 1.4 m length was used to prepare the compositions of the following examples. The settings for the standard compound extruder are as follows:
Table A Compound conditions for alloy production

The molten polymer blend is extruded through a multi-hole die into a 0.32 cm diameter cylindrical strand, cooled to room temperature in a water bath, and passed between two air jets to remove splashing water. I passed. The strands were then fed to a cutter and cut into cylindrical chips 2.8 mm long and 2.1 mm in diameter. The blended chips were dried in a circulating drier at 90 ° C. for 8-12 hours before use. Two compounding procedures were used. The masterbatch means comprises mixing the dispersed phase polymer and the compatibilizer in a first compounding step. The resulting chips are dried before the second step of mixing the continuous phase polymer and the masterbatch to make the final blend pellets. The single pass means consists of mixing all three components of the dispersed phase polymer, the compatibilizer, and the continuous phase polymer in a single pass through a mixer to make the final blended pellets.
[0317]
A Warnerp Fiddler ZSK vented twin screw compound extruder having a diameter of 30 mm, an L / D ratio of 30: 1 and a length of 0.9 m was used to prepare the compositions of the following examples. The settings for the standard compound extruder are as follows:
Table B Compound conditions for alloy production

The molten polymer blend is extruded through a multi-hole die into a 0.32 cm diameter cylindrical strand, cooled to room temperature in a water bath, and passed between two air jets to remove splashing water. I passed. The strands were then fed to a cutter and cut into cylindrical chips 2.8 mm in length and 2.1 mm in diameter. The blended chips were dried in a circulating drier at 90 ° C. for 8-12 hours before use. Two compounding procedures were used. The masterbatch means comprises mixing the dispersed phase polymer and the compatibilizer in a first compounding step. The resulting chips are dried before the second step of mixing the continuous phase polymer and the masterbatch to make the final blend pellets. The single pass means consists of mixing all three components of the dispersed phase polymer, the compatibilizer, and the continuous phase polymer in a single pass through a mixer to make the final blended pellets.
[0318]
Fiber molding equipment
For fiber production, both laboratory and commercial scale multi-layer filament, fiber spinning equipment was used. The polymer composition was dried before use and added to the extruder under a dry nitrogen atmosphere. Stretching and texturing operations were performed as indicated.
[0319]
Laboratory continuous filament (CF) line
The fiber forming extruder is a 25 mm diameter single screw extruder with a length / diameter ratio (L / D) of 30: 1 and four electric zone heaters. The extruder is connected to a spin pack with a metering pump and a sintered metal filter. The spin pack is connected to a fiber spinneret having 24 round holes. The filament stream is passed through a cross-flow quench chamber and then wound onto two heated godets. Twenty-four filament yarns are wound onto a cylindrical package using a standard winder.
[0320]
Pilot bulk continuous filament (BCF) line
The extruder is a 30 mm diameter single screw extruder with a length / diameter ratio (L / D) of 30: 1 and 4 electric zone heaters. The extruder is connected to a spin pack with a metering pump and a sintered metal filter. The spin pack is equipped with a fiber spinneret having 72 three-projection dies (producing fibers with a modification ratio in the range of 1.8-2.3). The temperature of the extruder's 1-4 zones (from feed port to feed end), the temperature of the spin pack, and the melting temperature of the product were measured by thermocouple means. Following extrusion, the molten fibers are solidified through a cross-flow quench chamber into undrawn continuous filament yarns. The quenching is at 15 ° C in air unless otherwise specified. The undrawn quenched continuous filament yarn is drawn between a slow first godet roll and a fast second godet roll, each having the temperature and surface speed given in the examples. The drawn yarn is then introduced into a hot air texturizer tube where it is converted from continuous filament to bulk continuous filament (BCF) by exposure to heated turbulent air. The "plug stream" of the bulked BCF yarn exits the texture riser tube and enters the perforated cooling drum, which draws in ambient air through the thermal texture plug stream by vacuum. The cooled bundle of BCF yarns is transferred to a weaving jet to entangle and make the yarn. The BCF yarn is then wound onto a cylindrical package using a standard winder operating at 1000 m / min.
[0321]
Pilot continuous filament (CF) line
The extruder is a 30 mm diameter single screw extruder with a length / diameter ratio (L / D) of 30: 1 and 4 electric zone heaters. The extruder is connected to a spin pack with a metering pump and a sintered metal filter. The spin pack is equipped with a fiber spinneret having 72 round dies of 0.25 mm diameter. The temperature of the extruder's 1-4 zones (from feed port to feed end), the temperature of the spin pack, and the melting temperature of the product were measured by thermocouple means. Following extrusion, the molten fibers are solidified through a cross-flow quench chamber into undrawn continuous filament yarns. The quenching is at 15 ° C in air unless otherwise specified. The undrawn quenched continuous filament yarn is drawn between a slow first godet roll and a fast second godet roll, each having the temperature and surface speed given in the examples. The drawn yarn is then wound on a cylindrical package using a standard winder.
[0322]
Commercial bulk continuous filament (BCF) line
The fibers were spun on a commercial scale BCF spinning line common to the carpet industry. The spinning line uses three 75 mm diameter single screw extruders with a length / diameter ratio (L / D) of 30: 1 and 5 electric zone heaters. Each extruder is equipped with a metering pump and a spin pack with a sintered metal filter. The spin pack is equipped with a fiber spinneret having 57 trilobal dies. The temperature gradient, spinhead temperature, and polymer melt temperature of zones 1-5 (from feed port to feed end) of each extruder are given in the examples. Following extrusion, the molten fibers are solidified through a cross-flow quench chamber into undrawn continuous filament yarns. The quenching is at 15 ° C in air unless otherwise specified. The undrawn quenched continuous filament yarn is drawn between a slow first godet roll and a fast second godet roll, each having the temperature and surface speed given in the examples.
[0323]
The drawn yarn is then introduced into a hot air texturizer tube where it is converted from a continuous filament to a bulk continuous filament by exposure to heated turbulent air. The "plug stream" of the bulked BCF yarn exits the texture riser tube and enters the perforated cooling drum, which draws in ambient air through the thermal texture plug stream by vacuum. The cooled bundle of BCF yarn is transferred to an interweaving jet to create sufficient entanglement for subsequent processing into tufted carpet yarn. The yarn is then wound onto a cylindrical package using a standard winder.
[0324]
Unprocessed material
The untreated materials used in the examples are as follows.
Component (a)
N-6RV151: Nylon-6 homopolymer (CAS 25038-54-4)
Type 2700 commercially available from DSM with a relative viscosity of 151, a maximum water content of 0.08 wt%, a maximum extractable water content of 1.5 wt%, and a chip size of 2.5 × 2.5 mm.
[0325]
N-6RV38: Nylon-6 homopolymer (CAS 25038-54-4)
Akron K222-D commercially available from DSM with a relative viscosity of 38.
[0326]
N-6,6RV50: Nylon-6,6 homopolymer (CAS 32131-17-2)
Product number 181129, commercially available from Sigma-Aldrich with Tm = 267 ° C.
[0327]
N-6,6RV250: Nylon-6,6 homopolymer (CAS 32131-17-2)
No. 429171, commercially available from Sigma-Aldrich, a high viscosity extrusion grade having a relative viscosity of 230-280.
[0328]
N-6 / 6,6: Nylon-6 / nylon-6,6 copolymer (CAS 24993-04-2)
Product number 42924-4, commercially available from Sigma-Aldrich with Tm = 250 ° C.
Component (b)
SPS1： Syndiotactic polystyrene homopolymer
Objective Mw = 250,000 (gel permeation chromatography), melt flow rate (MFR) = 13 g / 10 min (ASTM D-1238: condition 300 ° C., 1.2 kg load), and syndiotacticity = 96% or more Questra QA101, commercially available from Dow Chemical Company.
[0329]
SPS2： Syndiotactic polystyrene homopolymer
Objective Mw = 350,000 (gel permeation chromatography), melt flow rate (MFR) = 4 g / 10 min (ASTM D-1238: condition 300 ° C., 1.2 kg load), and syndiotacticity = 96% or more Questra QA102, commercially available from Dow Chemical Company.
[0330]
SPM1: Syndiotactic copolymer of styrene and 7 wt% p-methylstyrene
Questra MA406 trade name, commercially available from Dow Chemical Co., with a target Mw = 325,000 (gel permeation chromatography).
[0331]
SPM2: Syndiotactic copolymer of styrene and 4% by weight of p-methylstyrene, Tc = 257 ° C.
SPM3: A syndiotactic copolymer of styrene and 0.7 wt% p-methylstyrene,
SPM4: Syndiotactic copolymer of styrene and 10% by weight of p-methylstyrene, Tc = 246 ° C.
Component (b) and / or component (c)
MGSPM1: Maleic acid-modified syndiotactic copolymer of styrene and p-methylstyrene,
95 wt% SPM1, 3.0 wt% fumaric acid, 2.0 wt% 2,3-dimethyl-2,3-diphenylbutane, and a free radical initiator are melt mixed at 300 ° C. in a ZSK40 twin screw extruder. Prepared. The graft content of the obtained anhydride group was 0.5 wt% by Fourier transform infrared analysis (FTIR).
[0332]
MGSPM2: Maleic acid-modified syndiotactic copolymer of styrene and p-methylstyrene,
95 wt% SPM2, 3.0 wt% fumaric acid, 2.0 wt% 2,3-dimethyl-2,3-diphenylbutane and free radical initiator are melt mixed at 300 ° C. in a ZSK40 twin screw extruder. Prepared. The graft content of the obtained anhydride group was 0.3 wt% by Fourier transform infrared analysis (FTIR).
[0333]
MGSPM3: Maleic acid-modified syndiotactic copolymer of styrene and p-methylstyrene,
95 wt% of SPM3, 3.0 wt% of fumaric acid, 2.0 wt% of 2,3-dimethyl-2,3-diphenylbutane, and a free radical initiator are melt mixed at 300 ° C. in a ZSK40 twin screw extruder. Prepared. The graft content of the obtained anhydride group was 0.2 wt% by Fourier transform infrared analysis (FTIR).
[0334]
MGSPS2: Maleic acid-modified syndiotactic homopolymer,
95 wt% of SPS2, 3.0 wt% of fumaric acid, 2.0 wt% of 2,3-dimethyl-2,3-diphenylbutane, and a free radical initiator are melt-mixed at 300 ° C. in a ZSK40 twin screw extruder. Prepared. The graft content of the obtained carbonyl group was 0.34 wt% by Fourier transform infrared analysis (FTIR).
[0335]
FAPPO1: Fumaric acid graft-modified poly (2,6-dimethyl-1,4-phenylene ether) (PPO)
Contains 0.8 wt% of grafted fumaric acid.
[0336]
FAPPO2: Fumaric acid graft-modified poly (2,6-dimethyl-1,4-phenylene ether) (PPO)
Contains 1.6 wt% of grafted fumaric acid and 10 wt% of syndiotactic polystyrene (SPS1).
[0337]
SMA1: Atactic styrene / maleic anhydride copolymer (SMA) (CAS 9011-13-6)
Melt index = 1.7 g / 10 min (ASTM D-1238, 230 ° C / 2.16 kg) and contains 7 wt% maleic anhydride.
[0338]
SMA2： Atactic styrene / maleic anhydride copolymer
Contains 0.2 wt% maleic anhydride content by FTIR analysis.
[0339]
SMA3： Atactic styrene / maleic anhydride copolymer
Contains 1.5 wt% maleic anhydride content by FTIR analysis.
[0340]
SMA4： Atactic styrene / maleic anhydride copolymer
Contains 0.5 wt% maleic anhydride content by FTIR analysis.
[0341]
The above components additionally contain small amounts of one or more additives such as antioxidants, lubricants, anti-blocking agents, stabilizers, nucleating agents and pigments.
Test method
The following test methods are used unless otherwise indicated.
[0342]
Firmness is measured according to ASTM D3822-96.
[0343]
Elongation is measured according to ASTM D3822-96.
[0344]
Modulus of elasticity (Young's modulus) is measured according to ASTM D3822-96.
[0345]
Shrinkage is calculated from the difference in densities (denier) before and after heat setting according to the following formula:
Shrinkage = 100 × [(Dahs−Dbhs) / Dbhs],
Here, Dbhs is the denier of the sample before heat setting, and Dahs is the denier of the sample after heat setting.
[0346]
The relative viscosity is determined by using a capillary viscometer (Canon Ubelod, II-type, size 200A) and immersing the viscometer in a constant temperature bath set at 25 ° C. The flow times of the polymer solution and the solvent are measured in a capillary viscometer. The relative viscosity has the formula: ηrel. = T / T₀ Is determined by
Here, ηrel. = Relative viscosity, T = solution flow time (seconds), T₀ = Solvent flow time (seconds).
[0347]
The crystallization temperature during cooling (Tc) is measured by DSC. Approximately 10 mg of polymer pellets are weighed (0.001 mg) into an aluminum DSC pan, capped and TA Instruments differential scanning calorimeter equipped with TA Instruments Model 920 autosampler and TA Instruments Universal V3.0E software, Placed in model 910 sample cell. An empty aluminum pan with lid was placed in the control cell. The sample was heated at a rate of 20 ° C / min to 320 ° C, held at 320 ° C for 5 minutes, and then cooled to 150 ° C in 20 minutes. Heat flow (watts / g): A plot of temperature is obtained.
[0348]
The following transition points (temperatures) are obtained:
Tg = glass transition point, second order transition
Tch = crystallization heat flow peak temperature when heating a solid crystal, primary exothermic transition
Tm = peak temperature of heat of fusion when heating solid crystal, first-order endothermic transition
Tc = Peak temperature of crystallization heat flow when molten crystal is cooled, primary exothermic transition
Table 1 shows the Tc of various materials tested in the manner described above.
[0349]
[Table 1]

Embodiment 1
[0350]
Example 1-3, Determination of A and B-Glossy by Laser Light Scattering
Five gloss judges were used to evaluate the gloss of the bulk continuous filament fiber sample.
The BCF fibers were dyed in a dark olive green and evaluated for gloss more easily than the bright white grade BCF fiber test. A five point standard was used as a numerical rating scale. Grade 1 (1) was typically used to exhibit the same full darling (completely dull color) as found in wool fibers. Grade 5 (5) was used to indicate Fulbright (perfect gloss) of a nylon 6 sample. Standards with grades 2 (2), 3 (3), and 4 (4) were chosen as midpoints. Each fiber sample was also measured with the laser light scattering technique disclosed herein.
[0351]
The compositions disclosed in Table 2 were prepared and spun into fibers. The compositions of Examples 1 and 2 were prepared on a 40 mm twin screw extruder using the masterbatch method. Examples 3 and A were prepared on a 40 mm twin screw extruder using the single pass method.
[0352]
[Table 2]

The above composition was spun into a yarn containing 72 filaments and having about 1200 denier using a pilot BCF spinning line. The yarn exhibited a gloss ranging from Fulbright to Fuldal. The yarn was defined by the following gloss ranks:
5 = Nylon 6 = Fulbright (perfect gloss) Comparative Example B
4 = Comparative example A
3 = Example 2
2 = Example 1
1 = Fuldal (completely dull), Example 3
In addition, commercially available BCF samples were analyzed by laser light scattering. These same BCF fibers were also dyed dark olive green and graded by a gloss judge. The commercial samples employed and the corresponding gloss ratings by the judges were as follows:
C1^* DuPont 1710-94-0-896AS SemiDull (gloss judge grade = 2.9)
C2^* DuPont 1105-136-0-615 (gloss judge grade = 1.8)
C3^* DuPont 1340-68-0-416A (gloss judge grade = 2.2)
C4^* DuPont 1430-68-0-P1369 (gloss judge grade = 4.1)
C5^* DuPont 1425-124-0-P1365 (gloss judge grade = 1.9)
Table 3 shows the scattering ratio of the five judge gloss standards and the five commercially available BCF samples. A plot of gloss judge grade and laser light scattering ratio (along with the linear fit calculated therefrom) is shown in FIG. The scattering ratio, Rs, determined by laser light scattering is inversely related to the gloss determined by the gloss judge. In particular, gloss = (-10.906) /Rs+7.1675 is R² = 0.9065 linear fit. The fibers according to the invention have a gloss judge rating of 4 or less and a corresponding scattering ratio of 0.29 or more. Table 3 shows the results.
[0353]
[Table 3]

To further validate the laser light scattering technique for fiber analysis, a known matting agent, TiO, at various levels₂ Are blended in a 30 mm twin screw extruder and formed into fibers using a lab scale continuous filament line using essentially the same conditions as described and analyzed above. . The composition details and results are shown in Table 4 and also in FIG.
[0354]
[Table 4]

TiO₂ The plot of the scattering ratio, Rs, for shows a good correlation. In particular, the following equation: Rs = 164.6w + 0.2364, where w is TiO₂ The content (% by weight) of is the square correlation coefficient R² = 0.9895. In the figure, the scattering ratio 0.29₂ level
It turns out that it corresponds to 325 ppm.
[0355]
Examples 4-15 and E Effect of Disperse Phase Level on Gloss and Hardness
The effect of dispersed phase content on gloss and firmness was measured for various compositions. The compositions of Examples 4-15 were prepared on a 30 mm twin screw extruder using the masterbatch method to obtain the compositions given in Table 5. The fibers of Inventive Examples 4-15 and Comparative Example E were spun on a laboratory scale continuous filament line using the conditions given in Table 6.
[0356]
[Table 5]

[0357]
[Table 6]

Table 7 shows the fiber stiffness, elastic modulus, and scattering ratio. Based on a scattering ratio lower limit of 0.29, this technique shows an SPS2 level of 2% gloss when compatibilized with FAPPO1 and a total SPS level (SPS2 + MGSPM1) 3% gloss using the MGSPM1 compatibilizer. The upper limit composition required for this technology based on stiffness and capacity for fiber spinning is 35% SPS2 or SPS2 + MGSPM1. More preferred is less than 30% SPS2 or SPS2 + MGSPM1 and most preferred is less than 20% SPS2 or SPS2 + MGSPM1.
[0358]
The modulus of the fiber increases with increasing SPS2 content which enhances the properties of the dispersed phase, which can lead to improved durability, good dimensional stability, improved wrinkle recovery, or improved stiffness. .
[0359]
[Table 7]

One skein of the aforementioned fiber of known length was immersed in boiling water for 15 minutes. The fiber was removed and air dried for 72 hours. The skane length was remeasured and the primary skane shrinkage was calculated. The fiber was then tested for physical properties. Table 8 shows the results.
[0360]
The primary skeleton shrinkage is measured as follows. The sample was hung on a hook and a 275 g weight was hung on the skein. Measure the length before exposure to boiling water and L_b Recorded as. Measure the length after immersion in boiling water and drying._a Recorded as. The primary skein shrinkage is then calculated according to the following equation:
[0361]
Primary skein shrinkage% (LSS) = ((L_b -L_a ) / L_b ) X100
Primary skein shrinkage due to boiling water exposure reduces optical streaks in carpets, improves dimensional stability in fabric manufacturing, dyeing, and finishing processes, dimensional stability in home laundering and trade laundering processes. SPS2 content demonstrating the dimensional stability of the present invention with many advantages in textile applications including improvements, improved yields in the textile manufacturing process, the ability to reduce the need for heat setting, and the ability to maintain garment shape It decreases with the increase. Comparing the elastic moduli of Tables 7 and 8, the elastic modulus of the fibers is well maintained even after exposure to boiling water, which is important for maintaining comfort and shape when exposed to hot water. Demonstrates superiority in applications.
[0362]
[Table 8]

Examples 16-27 Relationship between Gloss and Scattering Ratio and Occluded Particle Size
Fibers according to the present invention were made by spinning, drawing and finishing various blends on a pilot BCF spinning line using typical spinning conditions. When the sample was placed in formic acid at room temperature, the nylon matrix was dissolved, but the fine particles of the occlusion phase, which were not affected by formic acid, remained in a dispersed state. The particles were collected by filtration. FIG. 17 is a scanning electron micrograph (SEM) of a typical sample of such particles in a fiber made according to Example 25. A typical sample of such fibers was imaged and analyzed using standard particle size analysis software according to the following procedure.
[0363]
Fiber samples (0.012 g) were each placed in a 10 ml glass vial with a new screw cap. 2 ml of concentrated (95-97%) formic acid was added to each sample vial. The vial was shaken gently for 20 seconds to dissolve the nylon and kept stationary at 25 ° C. for 4 hours. The solution was shaken again to evenly disperse the sPS in the formic acid solution. An aliquot (0.1 ml) of each dispersion was taken with a fresh 1 ml resin capillary syringe and placed in a 10 ml glass vial with a new screw cap. Then, 4.9 ml of formic acid was added to each vial to make a total of 5 ml of dispersion in each vial. Certain solutions were diluted as necessary to see the distribution of sPS in the photograph. The diluted dispersion was shaken gently for 2-3 seconds, then about 2 ml of the solution was taken with a syringe and filtered through a 0.1 or 0.02 micron pore size inorganic membrane filter. The filtration residue was washed three times with formic acid to remove residual nylon.
[0364]
The filter with the dispersed sPS particles collected was briefly air dried and mounted on an aluminum scanning electron microscope stub. The measurement sample was chromium sputtered in a high resolution chrome coater. The sample thus prepared was imaged with a scanning electron microscope (Hitachi S-4100 FEG scanning electron microscope commercially available from Hitachi, Ltd.). An image of 4096 × 4096 pixels was electronically acquired with a 4PI digital imaging system available from 4PI Analysis.
[0365]
The shape and size of the sPS particles were analyzed using computer image analysis software (Sion image analysis application software for a Windows operating system personal computer, commercially available from Sion). Particles were captured manually on the image.
The images were then used to measure the projected area and perimeter of the particles by applying ellipses (long and short axes) to the projected shape of each particle. Although most particles have an elliptical or ellipsoidal appearance that fits well with the model, some particles are found to be more rectangular in shape (indicating a more cylindrical shape in three dimensions). As a result, we manually re-fitted the length and width rectangle models. Depending on the sample, 400-4000 particles were analyzed in each sample. The terms minor axis and projected minor axis are used herein interchangeably with the terms diameter and particle size. Similarly, the long axis and projected long axis are used interchangeably herein with the terms length and particle length.
[0366]
The average of the major axis and the minor axis of projection (diameter) of the sPS particles was calculated based on the number of particles, the projected area, the estimated particle volume, and the weight of the minor axis of the projection. The general formula for determining the weight average used the following formula:
[0367]
Embedded image

Where x_w Is the average quantity (eg, diameter) calculated based on the weighting factor of w (eg, particle volume), w_iIs each weighting factor for particle i (eg, the estimated volume of particle i), and x_iIs the averaged particle size (eg, the diameter of particle i). From the volume weighted average, the cumulative probability of particle size was calculated as:
[0368]
Embedded image

Where F (j) is the cumulative probability of particle j and V_i Is the estimated volume of particle i, and the particles are ordered from smallest to largest such that particle 1 has the smallest diameter and particle N has the largest diameter. Based on this distribution, it is possible to calculate the particles with the 99th percentile diameter of this volume based distribution. This particle size is called (D99). The physical meaning of D99 means that the 99th percentile particle diameter of the volume-based distribution, ie, 99% of the estimated total particle volume, is occupied by particles of a smaller diameter than D99. As a result, D99 is an approximation of the maximum diameter. The true maximum diameter requires an infinite set of measurements, and as a result, is not a practical quantity for measurement or analysis. Table 9 shows D99 and the volume average particle diameter.
[0369]
[Table 9]

The thermoplastic alloy used for fiber formation was compounded with a 30 mm or 40 mm twin screw extruder using the masterbatch method. The exception was Example 25, which was compounded on a 40 mm twin screw extruder using the single pass method. All materials were formed into fibers on a pilot scale BCF spinning line. All materials contain about 10% crystalline syndiotactic polymer phase (including samples containing MGSPM1). A plot of the volume average projected particle minor axis diameter and the gloss of the BCF yarn determined by the expert judge is shown in FIG. 14 along with a calculated fit line. The linear relationship (y = 0.25x + 1.4) is the square of the correlation coefficient of 0.79 between the volume average projected particle minor axis diameter (y) and the gloss (x) measured by the judge, R² It was found to have. In particular, at the level of component (b) of 8-14% by weight, a volume average short axis diameter of the occluding particles greater than 0.20 μm, preferably greater than 0.25 μm, is desirable for producing fibers with reduced gloss. Also plotting similar information in FIG. 15 using the gloss of the BCF yarn as measured by the scattering ratio (x-axis), the volume average projected particle short axis diameter (y) and the fiber scattering ratio ( x) the square of the correlation coefficient of 0.65 during R), R² Is obtained (y = 4.5x-1.3). Fibers having a scattering ratio determined by the foregoing method of greater than 0.33, more preferably greater than 0.35, are particularly desirable for the present invention.
[0370]
Firmness was also found to correlate with the 99th percentile (based on volume percentile) of the minor axis diameter of the projected particle, which is an approximation of the maximum particle size. A correlation is observed when plotted as a function of firmness. In particular, the following linear relationship was obtained: D99 particle size = -1.3x + 4.2,
Where x is hardness (g / denier) and R² = 0.64. FIG. 16 shows the results.
[0371]
Good fiber spinning performance appears to result, at least in part, in fibers having acceptable bursting dynamics. One factor affecting this property appears to be the minor axis diameter of the largest occluded particles. Thus, the correlation between the indicated hardness and the D99 minor axis particle size is an indicator of good fiber spinning properties. In particular, D99 smaller than 3.0 μm is very desirable.
[0372]
Examples 28-38 Use of Two-Component, Self-Compatibilizing Blends with Various Compatibilizers
The compositions in Table 10 were compounded on a 30 mm or 40 mm twin screw extruder using the masterbatch method for Examples 28-36 and the single pass method for Examples 37-38. The resulting blends were spun into fibers on a laboratory scale continuous filament line for Examples 28-36 and a pilot scale BCF spinning line for Examples 37-38. The BCF samples were gloss graded by a gloss judge. Examples 28-36 contained 10% SPS2. Examples 37-38 contained only two components: a maleic acid modified syndiotactic copolymer of nylon 6, styrene and p-methylstyrene.
[0373]
[Table 10]

Examples 39-46, F Yellow Index, YI Test
SPS2, nylon-6, and maleic anhydride grafted syndiotactic styrene / p-methylstyrene copolymer (MGSPMl), maleic anhydride grafted syndiotactic polystyrene (MGSP2), atactic styrene / maleic anhydride copolymer (SMA4), or Dry spinning blends of various compatibilizers (component (c)) containing fumaric acid-grafted polypropylene oxide (FAPPO1 or FAPPO2) in various weight ratios are compounded on a 30 mm or 40 mm twin screw extruder using the masterbatch method. It has become. Further, a dry spinning blend of nylon N-6 component (a) and maleic anhydride grafted styrene / p-methylstyrene copolymer was compounded with a twin screw extruder using a single pass method.
[0374]
[Table 11]

[0375]
Examples Fa, 39a, 41a, 43a, 44a Light stability of undyed fibers
BCF samples of the different compositions described above were subjected to a UV light color stability test according to the American Association of Chemists and Colorants (AATCC) Test Method 16-1998, Option E. It was wound on a three-layer thick white card for testing. All tests were performed by Professional Testing Laboratory of Daltn GA. The samples were exposed to a high pressure mercury discharge light for 80 and 160 hours and then compared to a control sample without exposure. Table 18 shows the results of D65, 10-degree color change, and ΔE. In the table, the color change of the reflected light, ΔE, is expressed by the following equation: ΔE = (L₁-L₂)² + (A₁-A₂)² + (B₁-B₂)² )^1/2 , Was calculated.
Where 1 is the initial state, 2 is the final state, and L, a and b are the measurements of the reflected light with respect to the luminosity or intensity of red / green and yellow / blue, respectively.
[0376]
The color change shows that the sample using the grafted polyphenylene oxide polymer as the compatibilizer has unacceptable color fixability as compared to the nylon comparative example and the examples using the MGSPS2 and MGSPS1 compatibilizers.
[0377]
[Table 12]

Example 47 and G Demonstration of Cloth Fiber and Fabric Samples Prevented by Fine Denier
A 10: 3: 87 weight ratio blend of SPS2, MGSPM1, and Nylon N-6 was prepared.
Compounded with a 40 mm twin screw extruder using the masterbatch method. The resulting blend was spun on a pilot scale continuous filament line using the following conditions:
Metering pump supply: 14.7 g / min
Extruder barrel temperature gradient: 290 ° C / 325 ° C / 325 ° C / 310 ° C
Spin head temperature: 310 ° C
Melting point: 302 ° C
Filling pressure: 363 psig (2.6 MPa)
Quenching: 14 ° C in air
Low speed godet: 75 ° C and 434 m / min
High speed godet: 175 ° C and 1300m / min
Stretch ratio: 3: 1
Yarn denier: 100/72, 1.4dpf
The resulting 100/72 yarn has a firmness of 2.4 g / denier at 65% elongation.
[0378]
The sample of Comparative Example G was made using pure nylon N-6 under comparative conditions. The extruder is a 38 mm diameter single screw extruder with a length to diameter ratio (L / D) of 24 and equipped with an electric zone heater. Each extruder is connected to a spin pack with a metering pump and a sintered metal filter. The spin pack is equipped with a fiber spinneret having 64 0.3 mm diameter circular dies. The fiber spinning conditions are as follows:
Metering pump supply: 8.3 g / min
Extruder barrel temperature gradient: 260 ° C / 275 ° C / 260 ° C
Spin head temperature: 260 ° C
Melting point: 258 ° C
Filling pressure: 380 psig (2.6 MPa)
Quenching: 13 ° C in air
Low speed godet: 40 ° C and 233 m / min
High speed godet: 90 ° C and 750m / min
Stretch ratio: 3.2: 1
Yarn denier: 100/64, 1.56dpf
The resulting 100/64 yarn has a firmness of 4.0 g / denier at 75% elongation.
[0379]
The two fibers were twisted at 2 twists / inch and then woven into a four thread sling satin woven fabric. Greige fibers were soaked in boiling water and then allowed to air dry. The warp and fill dimensions before and after boiling water exposure were measured. The shrinkage was then calculated in both the warp and fill directions. Table 13 shows the results.
[0380]
[Table 13]

Testing of the resulting fabric sample after treatment in the manner described above shows that the fabric made according to the present invention (Example 47) has a more satisfactory hand (soft feel) and better range (more (Dull).
[0381]
Example 48 Production of Fibers Using Masterbatch Blend and Extended Flow Mixing
A dry spinning blend of SPS2 and FAPPO1 (fumaric acid-modified polyphenylene oxide containing 0.8% grafted fumaric acid) at a weight ratio of 78.74: 21.26 is compounded in one pass at 290 ° C. and extruded into cylindrical strands. Then cooled to room temperature in a water bath. The strands were blown free of water and cut into 2.8 mm long and 2.1 mm diameter chips. The chips (referred to as master batch chips) were dried in an air circulating drier at 90 ° C. for 8 hours to reduce the moisture level to 0.08% or less. A dry spinning blend of 87.3: 12.7 weight ratio of nylon N-6 and the aforementioned masterbatch chips was fed to a 63.5 mm diameter single screw extruder as shown in FIG. 6 for the production of polymer particles. The extruder, 60, comprises a single shaft, 69, an internal cylindrical mixer body 65 having a temperature control zone, 61, 62, 63, 65. The set temperatures of the zone from inlet to outlet were 260, 315, and 315 ° C., respectively. The transfer line, 64, mixer body, 65, and cylindrical die, 66, were adjusted to 290 ° C. The number of revolutions of the extruder was set to 50, and the extruder was fed into the system at a net flow rate of 13.61 kg / hr. To improve the mixing of the nylon 6 and masterbatch chips, the molten polymer exiting the extruder is passed through an in-line extended flow mixer, 67, (Model EFM-250 Static Mixer, commercially available from Extension Flow Mixer, Inc. Mississauga, Ontario). ). The variable gap of the mixing device was set at 3 mm. The material exiting the mixing device was extruded into a cylindrical strand (yarn) and cooled to room temperature in a water bath, 68. The strand was cut into chips approximately 4 mm long and 3 mm in diameter. The resulting pellets were dried in a circulating air dryer to a moisture level of 0.08% or less and spun on a pilot scale BCF spinning line.
[0382]
The fiber molding conditions were as follows:
Metering pump supply: 135 g / min
Extruder barrel temperature gradient: 300 ° C / 325 ° C / 325 ° C / 295 ° C
Spin head temperature: 295 ° C
Melting point: 290 ° C
Filling pressure: 795 psig (5.6 MPa)
Quenching: 15 ° C in air
Low speed godet: 75 ° C and 334 m / min
High speed godet: 160 ° C and 1000m / min
Stretch ratio: 3: 1
Texturizer temperature and pressure: 190 ° C and 80 psig (0.63 MPa)
Interweaving pressure: 45 psig (0.40 MPa)
Yarn denier: 100/64, 1.56dpf
The resulting BCF yarn had a total denier of 1197 for a 72 yarn bundle after stretching, texturing, air weaving and winding. The resulting 1197/72 yarn has a firmness of 2.5 g / denier. The gloss examiner rating was 3.6.
[0383]
It will be appreciated that the fiber spinning apparatus may also incorporate an extended mixer, or a static mixer, substantially as described in the previous section, between the extruder and the spin pack. In such a modified fiber spinning apparatus, the various components are combined in the process of melt extrusion of the fibers, so that the initial compounding of the blend or alloy of all the components is not necessary. Sufficient dispersion of the pre-blended pellets of component (b) and component (c) can be achieved.
[0384]
Example 49 Bicomponent fiber spinning
One-pass dry rotary blend of nylon N-6, SPS2 and FAPPO1 (fumaric acid-modified polyphenylene oxide containing 0.8% grafted fumaric acid) at a weight ratio of 87.3: 10: 2.7 in a twin screw extruder. And dried.
[0385]
The bicomponent (core / sheath) fiber was formed under the following spinning conditions. Two single-screw, 30 mm diameter extruders equipped with four electric zone heaters with a length to diameter ratio (L / D) of 30: 1 (one for the blend used for the sheath) The other was used to knead the nylon 6 used as the core. Each extruder is equipped with a metering pump and a spin pack with a sintered metal filter. The spin pack is equipped with a fiber spinneret having 72 trilobal dies, each of which can produce core-sheath, bicomponent, coextruded fibers with trilobal holes. The temperature of the 1-4 zones (from feed port to feed end) and spin of each extruder is measured by thermocouple. Each metering pump delivered at 68 g / min. The extruder barrel temperature gradient was 290 ° C / 320 ° C / 310 ° C / 300 ° C, the nylon extruder barrel temperature gradient was 260 ° C / 280 ° C / 275 ° C / 275 ° C, and the spin head temperature was 300 ° C. The filling pressure was 795 psig (5.6 MPa). The sheath (made from the thermoplastic blend of the present invention) comprises 50% by volume of the total fiber cross-section, the remainder being kneaded nylon 6 consisting of core fibers.
[0386]
Following extrusion, the molten fibers solidify through a cross-flow quenching chamber to become partially drawn continuous filament yarns. The quenching is at 15 ° C in air unless otherwise specified. The partially drawn quenched continuous filament yarn is drawn between a slow first godet roll and a fast second godet roll, each having a temperature of 75 ° C. and 160 ° C., and having respective surface velocities of 339 and 950 m / min. The stretching ratio was 2.8.
[0387]
The cooled yarn is wound onto a cylindrical package using a standard winder operating at 950 m / min. The resulting flat yarn had a total denier of 1250 for 72 3-projection filaments after drawing and winding. The resulting 1250/72 yarn had a firmness of 1.9 g / denier.
[0388]
Example 50 Demonstration of commercial-scale BCF spinning
A 10: 2.7: 87.3 weight ratio blend of SPS2, FAPPO1, and Nylon N-6 was compounded on a 40 mm twin screw extruder using the masterbatch method. The resulting blend was spun on a pilot scale continuous filament line using the following conditions and the conditions in Table 14:
Extruder barrel temperature gradient: 275 ° C, 288 ° C, 285 ° C, 285 ° C, 285 ° C
Spin head temperature: 285 ° C
Melting point: 285 ° C
Filling pressure: 110 psig (0.86 MPa)
Quenching: 16 ° C in air
Low speed godet: 75 ℃
High speed godet: 180 ℃
Texturizer temperature and pressure: 210 ° C and 6.0 bar (0.6 MPa)
Interweaving pressure: 3.0 bar (0.30 MPa)
Comparative Example H 100% component (a) ( Nylon-6 )
The following conditions and the conditions in Table 14 were used to make a nylon N-6 polymer yarn and spun using the apparatus of Example 50.
[0389]
Extruder barrel temperature gradient: 247 ° C, 257 ° C, 256 ° C, 254 ° C, 254 ° C
Spin head temperature: 260 ° C
Melting point: 260 ° C
Filling pressure: 1550 psig (10.8 MPa)
Quenching: 16 ° C in air
Low speed godet: 75 ℃
High speed godet: 180 ℃
Texturizer temperature and pressure: 210 ° C and 6.0 bar (0.6 MPa)
Interweaving pressure: 3.0 bar (0.30 MPa)
Comparative Example I:
A 10: 1: 89 weight ratio blend of Styron 685D (Atactic Polystyrene), SMA1, and Nylon N-6 was compounded on a 40 mm twin screw extruder using the single pass method. The resulting blend pellets were spun on a pilot scale continuous filament line using the following conditions and the conditions in Table 14:
Extruder barrel temperature gradient: 260 ° C, 280 ° C, 270 ° C, 270 ° C, 270 ° C
Spin head temperature: 270 ° C
Melting point: 270 ° C
Filling pressure: 1500 psig (10.4 MPa)
Quenching: 16 ° C in air
Low speed godet: 75 ℃
High speed godet: 180 ℃
Texturizer temperature and pressure: 210 ° C and 6.0 bar (0.6 MPa)
Interweaving pressure: 3.0 bar (0.30 MPa)
A comparison of the spinning conditions with the yarns of Table 14 shows an improvement in the spinnability achievable using the composition according to the invention compared to the fibers and yarns according to Comparative Examples H and I. At the same denier / filament as compared to the fibers of Comparative Examples H or I, the fibers of Example 50 were easier to mold and could be spun at higher processing speeds on a commercial scale molding machine. Comparative Example I was difficult to spin and caused many breaks, but no breaks or fiber stability problems were encountered using the composition of Example 50.
[0390]
[Table 14]

Examples 51-53, J, K, and L Reduce Heat Set Shrinkage
The compositions of Examples 51-53 were compounded with a 40 mm twin screw extruder using the masterbatch method. The composition of Example M was compounded on a 40 mm twin screw extruder using the single pass method. The resulting blend (shown in Table 15) was spun into fibers on a pilot scale BCF spinning line using the conditions given in Table 16. Scanning electron microscope images of the fibers are shown in FIGS. 1a (Example 51), 1b (Example 52), 1c (Example 53), 2a (K), and 2c (M).
[0391]
[Table 15]

[0392]
[Table 16]

Heat shrinkage of heat set twist yarn
The yarns produced in Comparative Examples K, L, and M and Examples 51-53 were used to make a twist yarn having 4.5 turns / inch (1.77 turns / cm) in the "S" direction. Then, the yarn was twisted with a Bell Doll model 400 using a cable twisting apparatus at a spindle speed of 5200 rpm and a winding speed of 27.8 m / min. The twisted yarn was then wound onto a 89 inch (2.3 m) circumference reel for spinning and heat setting using a batch autoclave. Heat set was performed at 132 ° C. for 54 minutes. Table 17 shows the denier of the twisted yarn before and after the heat setting, together with the shrinkage and hardness of the twisted and heat set yarns during heat setting.
[0393]
[Table 17]

As shown in Table 17, the cable twist heat set yarns made with the fibers of Examples 51a-53a show less shrinkage than the yarns made with the fibers of Comparative Examples La, Ka, and Ma. . In particular, each example of a twist yarn made of at least 5% by weight of syndiotactic polystyrene has a shrinkage of less than 15%, a yarn made of at least 10% by weight of syndiotactic polystyrene has less than 13%, and 15% Yarns made from 10% syndiotactic polystyrene exhibited shrinkage of 10% or less.
[0394]
Color stability
Twist and heat set BCF fiber samples of Examples 51b, 52b, 53b, and Jb (made by twisted yarn Ja in the same way that twisted yarns 51b-53b were made) to dark olive green according to the following dyeing recipe and procedure: Skein staining was performed. The fiber samples were placed in lingerie bags and washed according to the following procedure.
[0395]
Dye formulation
Level Acid Dye Formulation-Olive Green
Brand name Diacid Yellow 3R 200%: 0.00338 g / g fiber
Brand name Diacid Red 2B 200%: 0.0002 g / g fiber
Brand name Diacid Blue 4R 200%: 0.00256 g / g fiber
Brand name Direb AC: 0.02 g / g fiber
Ammonium sulfate: 0.02 g / g fiber
Ammonia: 0.01 g / g fiber
Sodium thiosulfate: 0.0025 g / g fiber
Trade name DIREV AC = 48% aqueous solution of Dowfax 2A1 trade name of Dow Chemical Company
200% brand name Diacid Yellow 3R = commercially available from Dye System, Dalton, Georgia.
[0396]
Trade name Diacid Red 2B 200% = commercially available from Die System Co., Dalton, Georgia.
[0397]
Trade name Diacid Blue 4R 200% = commercially available from Dye System Co., Dalton, Georgia.
[0398]
Staining procedure
1. Water is added to the dye to give a liquor ratio of 30: 1-40: 1.
[0399]
2. Add the skein to the water and circulating bath.
[0400]
3. Weigh Daleb AC, ammonium sulfate, ammonia, and sodium thiosulfate and add to 110 liters of water in proportion to the weight of the fiber to be dyed. Add to dye bath and circulate for 15 minutes. The desired initial pH is 8 and the desired final pH is 6.5-7.
[0401]
4. The dye solution is added in proportion to the weight of the fiber to be dyed.
[0402]
5. The mixture is heated to 93 ° C. over about 45 minutes with stirring.
[0403]
6. Hold at 93 ° C. for 15 minutes with stirring.
[0404]
7. The bath is cooled and cold rinse water is added, overflow, and then drain.
[0405]
8. Rinse with cold water, remove scale, and dry at 120 ° C.
Washing procedure
The yarn was put in a lingerie bag. Two sets of each yarn, 15 g each, were placed in a standard residential washing machine for the first three wash cycles. After three wash cycles, one yarn of each material was removed and stored while the other yarn continued for another three cycles (6 cycles total). After each wash cycle, the yarn was dried in a conventional residential dryer.
[0406]
Approximately 85 g of a commercial laundry detergent (Tide Deep Clean Formula, Mountain Spring liquid required detector) was used per load for each wash cycle. Intermediate load settings used about 16 gallons of hot water for the wash cycle and 17 gallons of cold water for the rinse cycle. The total wash cycle was 30 minutes.
[0407]
Three wash cycles, six wash cycles, and the control yarn were wound onto a three layer thick card according to the recommendations of AATCC test method 16-1998. The color of the yarn is measured, and the color fixability is determined by the following equation: ΔE = (L₁-L₂)² + (A₁-A₂)² + (B₁-B₂)² )^1/2 , Quantified by the color change of the reflected light, ΔE, calculated by Where 1 is the initial state, 2 is the final state, and L, a and b are the measurements of the reflected light with respect to the luminosity or intensity of red / green and yellow / blue, respectively.
[0408]
Table 18 shows the color change (ΔE) of the washing cycle. The data show that the color fixability of the yarns of Examples 51b-53b after six washes was comparable to the nylon 6 control (Jb^* ). Similar results are expected using other acid dye techniques such as milling acid dyes and premetallized dyes. Conventional fixer technology can also be used with the present invention to further improve wash fixability.
[0409]
[Table 18]

Manufacture of cut pile carpet
The yarns made of Examples 51a-53a and Comparative Examples La and Ka were made of Belldoll to make a twisted yarn having 4.5 turns / inch (1.6 turns / cm) in the "S" direction. Model 400 was twisted with a cable twisting apparatus at a spindle speed of 5200 rpm and a winding speed of 31.6 m / min. The twisted yarn was wound on a reel having a circumference of 89 inches (2.3 m) for spinning and heat setting using a batch autoclave. Heat set was performed at 132 ° C. for 54 minutes.
[0410]
The twisted and heat set yarn was tufted to the main carpet backing on a 5/32 gauge cut pile tufting machine. The pile height is 20/32 inches (1.6 cm) and 40 oz (1134 g) (1356 g / m2) per square yard of carpet.²) Yarns were used.
The tufted carpet was then dyed according to the recipe in Table 19 by the following procedure.
[0411]
1. An appropriate amount of water was added to the dye bath to ensure that the carpet was well covered by the dye bath.
[0412]
2. The metal ion sealants EDTA, Dye Yellow AC, ammonium sulfate, and sodium thiosulfate were added to the dyebath and the pH was adjusted to about 6.5.
[0413]
3. Greige good carpet was added to the dye bath to wet the fibers.
[0414]
4. The dye was added to the dye bath.
[0415]
5. The dye bath was then heated to about 90 DEG C. in 30-45 minutes with gentle stirring.
[0416]
6. The dye bath was kept at 90 ° C. for 30 minutes with stirring.
[0417]
7. The dyed carpet was then removed and rinsed with cold water and dried.
[0418]
[Table 19]

After drying, the carpet was coated with styrene / butadiene latex, dried, sheared, and cut into samples for contract walker evaluation. The purpose of the contract walker assessment is to assess the appearance retention of the floor covering pile as a result of pedestrian traffic in a controlled environment. Testing is well known and is commonly employed in the carpet industry. The contract walker test was performed by the Professional Testing Laboratory of Dalton, GA, USA according to the following procedure:
1. A 230 mm × 560 mm sample was cut from both the length and width directions and secured by suitable means to a long distance floor perpendicular to the walking flow.
[0419]
2. Pedestrians walk at 50 minute intervals. All samples are vacuumed every hour before traffic is resumed. A multiple electronic counter is used to determine if a predetermined traffic volume has been applied.
[0420]
3. After the predetermined traffic volume has been applied, vacuum again to return to the original pile orientation at the last suction. All samples are allowed to recover at room temperature for a minimum of 12 hours before grading by a technical judge.
[0421]
4. The samples are each graded using a CRI reference scale according to the Carpet and Rug Association (CRI) TM101. The grade is averaged and reported to the nearest 0.1. The higher the grade, the better the expected performance. The rating is: 5 = no grinding, 4 = slight grinding, 3 = medium grinding, 2 = significant grinding, 1 = severe grinding.
[0422]
5. Each sample was graded for 5000 cycles and placed on the floor for further traffic testing until 20,000 cycles were obtained.
[0423]
The results of the appearance test are shown in Table 20 and FIG.
[0424]
[Table 20]

The durability of the carpet of the present invention is improved compared to the control of the comparative example while having a good hand.
[0425]
Examples 54-55, Mc
The fiber molding conditions of Examples 51 and 52 were 1390 from the composition according to the invention consisting of nylon-6, syndiotactic styrene and a compatibilizer compounded in a 40 mm twin screw extruder using the masterbatch method. This was repeated to make a total denier 72 filament yarn. Substantially pure nylon 6 is included as a comparative sample. Table 21 shows the fiber molding conditions.
[0426]
[Table 21]

The spinneret was fed at a metering pump flow rate of 150 g / min. The first and second godet rolls were operated at 80 ° C./308 m / s and 150 ° C./1000 m / s, respectively, to give a draw ratio of 3.25. Texturing was performed using heated air at 170 ° C. and 35 psig (241 kPa) pressure. Entanglement was obtained with an interwoven jet at an air pressure of 44 psig (300 kPa).
[0427]
The yarns made in Examples 54 and 55 and Comparative Example M were twisted at 4.0 turns / inch, heat set, and tufted to a carpet backing to 40 oz / square yard (1.4 kg / m).² 5.) A 5/8 inch (16 mm) pile height 5/32 gauge cut pile carpet was made. The carpet was divided into two groups. The first group was undyed but backed with a latex adhesive, sheared, and left to emphasize the stain resistant improvement of the present invention as a greige product for residential stain testing. A standard amount of 10 typical stains was applied to the Greige carpet and kept on the sample for 24 hours. The carpet was then washed with a mild detergent and dried. The gray scale of the American Association of Chemist and Colorists (AATCC) stain rating was used to grade the resulting stain. The grades are: 5 = no stain, 4 = slight stain, 3 = perceptible stain, 2 = significant stain, 1 = severe stain. The stain rating is shown in FIG. The carpets made from the yarns of Examples 54 and 55 showed less stain for cola, coffee, tomato juice, orange juice, and red wine than the carpet made from Comparative Example M. In addition, the degree of stain spread on the carpets made from the yarns of Examples 54 and 55 was much less than the carpet made with the yarns of Comparative Example M, highlighting the reduction in soiling of the present invention.
[0428]
A second group of unlined Greige carpets was dyed yellow prior to coating and shearing with the procedure of Examples 51c-53c above and the dye formulation of Table 22.
[0429]
[Table 22]

Carpets (Mc) made from twisted and heat set yarns of Comparative Example Mb exhibited streaks. The dyed carpet made from the twisted and heat set yarn of Example 54 had low color streaks and had a satisfactory hand and low gloss. The dyed carpet made from the twisted and heat set yarn of Example 55 was free of color streaks and had a more satisfactory hand and less gloss compared to the dyed carpet of Example 54 and Comparative Example Mc.
[0430]
Examples 56-65, N
The compositions given in Table 23 were prepared on a 30 mm twin screw extruder using the single pass method. The resulting blend was spun on a laboratory scale continuous filament line, except that the fiber was not drawn and remained as partially oriented yarn (POY). Table 23 shows the fiber molding conditions. Melting point is 300 ° C. The filling pressure is 430 psig (2.96 MPa). A metering pump feed rate of 5.9 g / min produced a continuous filament yarn of about 1450 total denier for 24 filament yarns. The undrawn quenched continuous filament yarn was drawn into an intermediate wheel and then drawn and wound into a cylindrical package at 100 m / min using a Resonator winder to give a draw ratio of about 3: 1. The results are shown in Table 23.
[0431]
High fiber stiffness and residual elongation have been observed with compositions of the present invention that include a compatibilizer. An improvement in modulus was seen with fiber formulations containing 10% by weight or more of component (b).
[0432]
[Table 23]

Example 66 O Use of low molecular weight nylon 6
A blend of SPS2, MGSPM1, N-6RV38 in a 10: 3: 87 ratio was compounded on a 30 mm twin screw extruder using the masterbatch method. For Example 35 of the invention, which uses high molecular weight nylon and has a firmness of 2.55 g / denier and a gloss judge rating of 2.5, this blend uses low molecular weight nylon. The blend was prepared as Comparative Example O,
Spun on a pilot scale BCF spinning line with N-6RV38 control. Quenching: 15 ° C. in air, low speed godet roll speed: 334 m / min, high speed godet roll speed: 1000 m / min, texturer temperature and pressure: 190 ° C. and 80 psig (0.55 MPa), interwoven pressure: 40 psig (0.28 MPa) It is. Table 24 shows the additional spinning conditions and the resulting stiffness. Both samples were successfully spun. The gloss judge rating of Example 66 of the present invention was 1.4, indicating a decrease due to a decrease in nylon molecular weight. Comparative Example O
The gloss judge rating was 5.0.
[0433]
[Table 24]

Inventive Embodiments 67-72
A blend of nylon N-6 (component (a)), SPS2 (component (b)), SMA1 (component (c)), and octadecaneamide (component (d)) in a weight ratio shown in Table 25 was subjected to a master batch method. It was compounded with a 30 mm twin screw extruder. In these examples, SPS2, SMA1 and octadecanamide were mixed in a masterbatch. The purpose of octadecamide is
The purpose is to reduce the amount of maleic anhydride groups by pre-reacting some of the maleic anhydride groups before mixing SMA1 with nylon N-6. This makes it possible for the user to use commercially available compatibilizers and to make the amount of nylonamine end groups that react with the compatibilizer as good as the compatibilizers of components (a) and (b) for good dyeability. To be adjusted.
[0434]
[Table 25]

The resulting blend was spun using a laboratory scale continuous filament spinning line and the fiber spinning conditions in Table 26. The quench temperature is 23 ° C. The properties of the fibers are shown in Table 26.
[0435]
[Table 26]

Example 73
A blend of SPS2, MGSPM1, and nylon 6; 6,6 in a weight ratio of 10: 3: 87 was compounded using a masterbatch method on a 30 mm twin screw extruder. The resulting blend was spun into fibers using a pilot scale BCF spinning line. The fiber spinning conditions are as follows:
Extruder barrel temperature gradient: 285 ° C / 310 ° C / 305 ° C / 305 ° C
Spin head temperature: 305 ° C
Melting point: 300 ° C
Filling pressure: 1200 psig (8.4 MPa)
Quenching: 14 ° C in air
Low speed godet: 75 ° C and 334 m / min
High speed godet: 160 ° C and 1000m / min
Texturizer temperature and pressure: 190 ° C and 80 psig (0.66 MPa)
Interwoven pressure: 50 psig (0.44 MPa)
The resulting BCF yarn had 1202 total denier for 72 filaments after drawing, texturizing, air weaving and winding. The resulting 1202/72 yarn has a firmness of 2.4 g / denier. The gloss judge rating was 3.0.
[0436]
Inventive Examples 74-77, P Use of sPS-PMS Copolymer as Dispersed Phase
The blend of SPS2, SPM1, SPM2, SPM4, MGSPM1, and Nylon N-6 was compounded on a 30 mm twin screw extruder using the masterbatch method and the weight ratios given in Table 27. The resulting blend was spun into fibers on a pilot scale BCF spinning line using the spinning conditions given in Table 28. These examples highlight the ability to use a low melting polymer as a dispersed phase to improve the modification ratio without using a specially designed die.
[0437]
[Table 27]

[0438]
[Table 28]

A blend of SPS2, MGSPM1, Nylon N-6,6RV50 and Nylon N-6,6RV250 was compounded on a 30 mm twin screw extruder using the masterbatch method at the weight ratios given in Table 29. The resulting blend was spun into fibers on a laboratory scale continuous filament line using spinning conditions substantially the same as those of Examples 74-77. The scattering ratio was determined by the laser light back scattering technique substantially as disclosed in Examples 16-27 and elsewhere herein.
[0439]
[Table 29]

[Industrial applicability]
[0440]
The present invention provides high speed spinning, spot resistance, color fixation, low color fringes, low optical fringes, reduction without the need for special equipment designs or operating procedures (such as using low draw temperatures) or finishing techniques. Industrial synthetic fibers or films with improved stains, improved puncture resistance or durability and low moisture uptake include carpets, rugs, woven fabrics, nonwovens, spunbond fabrics, knits, garments, laminates, etc. Useful for applications.
[Brief description of the drawings]
[0441]
FIG. 1 (a) shows a thermoplastic composition comprising 93.1% by weight of nylon 6, 5% by weight of syndiotactic polystyrene, 1.9% by weight of a compatibilizer according to Example 51. It is a scanning electron microscope image. FIG. 1 (b) is a scanning electron microscope image of a thermoplastic composition comprising 87.3% by weight nylon 6, 10% by weight syndiotactic polystyrene, and 2.7% by weight of a compatibilizer according to Example 52. It is. FIG. 1 (c) is a scanning electron microscope image of a thermoplastic composition comprising 81.9% by weight nylon 6, 15% by weight syndiotactic polystyrene, and 3.1% by weight of a compatibilizer according to Example 53. It is.
FIG. 2 (a) shows nylon 6 according to Comparative Example K and 0.2% by weight of TiO.₂ 1 is a scanning electron microscope image of a fiber produced from a thermoplastic composition containing a matting agent. FIG. 2 (b) shows nylon 6 according to Comparative Example L and 0.4% by weight of TiO.₂ 1 is a scanning electron microscope image of a fiber produced from a thermoplastic composition containing a matting agent. FIG. 2 (c) shows a scanning electron microscope of a fiber made from a thermoplastic composition comprising 89% by weight of nylon 6, 10% by weight of atactic polystyrene and 1% by weight of a compatibilizer according to comparative example M. It is a statue.
FIG. 3 is a plot of a typical multiple fiber for calculating the Mod ratio.
FIG. 4 is a plot of the appearance retention rating of the sample carpets of Examples 51c-53c, Kc and Lc.
FIG. 5 shows the stain rating of sample carpets made from yarns of Examples 54, 55 and Mc.
FIG. 6 is a sketch of one element of the melt mixing used in Example 48 and an extended flow stirrer incorporated as an expansion device.
FIG. 7 is a novel die design used in a polymer blend composition according to the present invention having a high die swell.
FIG. 8 is a scheme diagram showing the relationship between the devices used to measure the laser light scattering ratio of the fiber.
FIG. 9 is a sketch of a single fiber mount used to measure laser light scattering ratio.
FIG. 10 is a side view of a single fiber mount used to measure laser light scattering ratio.
FIG. 11 is a cross-sectional view of the single fiber mount used to measure the laser light scattering ratio, taken along line 11 of FIG.
FIG. 12 is a plot of gloss as a function of scattering ratio, Rs, as determined by laser light backscattering measurements of fibers of Examples 1-3, A, B, and C1-C5.
FIG. 13 shows the scattering ratio, Rs, of the various fibers of Examples D1-D6, as determined by laser light back scattering measurements, as TiO.₂ FIG. 3 is a plot plotted as a function of content.
FIG. 14 is a plot of the volume average diameter of the fibers of Examples 16-27 as a function of judge gloss.
FIG. 15 is a plot of the volume average diameter of the fibers of Examples 16-27 as a function of scattering ratio.
FIG. 16 is a plot of the volume D99 of the 99th percentile storage particle as a function of fiber stiffness for Examples 16-27.
FIG. 17 is a scanning electron microscope image of occluded particles of the component (b) from the fiber produced in Example 25.
FIG. 18 plots the D65, 10 degree color grade of unstained fibers after exposure to UV light as determined in Examples F, 39a, 41a, 43a, and 44a. is there.
FIG. 19 is a scanning electron microscope image (SEM) of the fiber surface in Example 48.

Claims (175)

(A) 86-92% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C.
(B) 14-8% by weight of a second thermoplastic polymer chemically different from (a) having a crystallization temperature, Tc ', and (c) a compatibilizer for (a) and (b);
Wherein the percentage is based on the total amount of (a) and (b), and Tc is at least 5 ° C. less than Tc ′, wherein the thermoplastic polymer composition is useful for producing extruded fibers and films. object. The composition of claim 1 wherein the first thermoplastic polymer is a polyamide or copolyamide and has a Tc 'of greater than 195C. The composition of claim 1 wherein the first thermoplastic polymer is a polyamide or copolyamide and the second thermoplastic polymer is a polyvinylidene aromatic polymer having an isotactic or syndiotactic steric structure. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic _C1-10. Alkyl-, halo-, or polar groups-syndiotactic copolymers with substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic _C1-10 alkyl-, halo-, or polar groups- The composition according to claim 3, which is a polar group-modified derivative of a syndiotactic copolymer with a substituted vinyl aromatic monomer. The composition of claim 3 wherein the polyamide is Nylon 6 having a relative viscosity of 30-180. The second thermoplastic polymer is syndiotactic polystyrene, syndiotactic of styrene and one or more cyclic C _1-10 alkyl- or halo-substituted vinyl aromatic monomers or polar group-substituted vinyl aromatic monomers. copolymers, or syndiotactic polystyrene or styrene and one or more cyclic C _1-10 alkyl -, halo -, or a polar group - claim 5, wherein the polar group-modified derivative of syndiotactic copolymers of substituted vinyl aromatic monomers Composition. The composition of claim 5, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000. The composition of claim 1 having a yellow index, YI, of less than 10.0. A composition according to claim 1, comprising 0.1-10% of compatibilizer c) based on the total composition weight. The composition according to claim 9, wherein the compatibilizer is a polar group-modified vinylidene aromatic homopolymer or copolymer. The compatibilizer is a polar group-modified polystyrene, a copolymer of one or more vinyl aromatic monomers and one or more polar comonomers, or styrene and one or more cyclic C _1-10 alkyl- or halo-substituted vinyl aromatic monomers or The composition according to claim 10, which is a polar group-modified copolymer with a polar group-substituted vinyl aromatic monomer. The compatibilizer is a maleic anhydride-modified or fumaric acid-modified styrene homopolymer or a maleic anhydride-modified or fumaric acid-modified styrene copolymer of styrene and one or more cyclic C _1-10 alkyl-substituted styrenes. 12. The composition of claim 11, wherein the agent has a copolymerized maleic anhydride or fumaric acid functionality of 0.01-5.0 mole percent. 13. The composition according to claim 1, wherein after formation of the fiber or film, component (b) is present in the matrix of component (a) in the form of occluded particles having a volume-average minor axis diameter of greater than 0.2 [mu] m. object. 14. The composition of claim 13, wherein after formation of the fiber or film, component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.3-2.0 [mu] m. After formation of the fiber or film composition of claim 13 which component (b) is present in occluding particle form having a 3.0μm smaller D ⁹⁹ minor axis. After formation of the fiber or film composition of claim 14, where component (b) is present in occluding particle form having a 2.8μm smaller D ⁹⁹ minor axis. After formation of the fiber, component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber is a laser having a particle size of at least 0.29. 13. The composition according to any of the preceding claims, having a light judge rating of 4.0 or less as determined by light scattering ratio or standard fiber sample. After fiber formation, component (b) is present in the form of occluded particles with a volume average minor axis diameter of 0.2-3.0 μm and the fiber is determined by a laser light scattering ratio or a standard fiber sample of 0.29 or greater. 16. The composition of claim 15 having a gloss judge rating of 4.0 or less. After formation of the fibers, component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm, and the fibers have a soft hand. Item 13. The composition according to any one of Items 1 to 12. 16. The composition according to claim 15, wherein after formation of the fibers, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fibers have a soft hand. The amount of component (c) is in the range of 0-5% based on the combined weight of components (a) and (b) and the sum of the reactive, functional groups in component (c) (if present) The composition according to any one of claims 1 to 12, wherein the amount is 0.001 to 0.25 mol% based on the total amount of component (b) and component (c). 16. The fiber of claim 15, wherein after formation of the fiber, component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand and improved durability. Composition. 20. After formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand and improved durability. Composition. 21. After formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand and improved durability. Composition. 13. The composition of any of claims 1-12, further comprising 0.1-10.0% of the matting agent based on the total composition weight. (A) 76-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C.
(B) 24-3% by weight of a second thermoplastic polymer chemically different from (a) having a crystallization temperature, Tc ′, and (c) a compatibilizer for (a) and (b);
Here, the percentage is based on the total amount of (a) and (b), and Tc is at least 5 ° C. smaller than Tc ′. An extruded drawn fiber comprising a thermoplastic polymer composition. 27. The fiber of claim 26, wherein the first thermoplastic polymer is a polyamide or copolyamide and Tc 'is greater than 195C. 27. The fiber of claim 26, wherein the first thermoplastic polymer is a polyamide or copolyamide and the second thermoplastic polymer is a polyvinylidene aromatic polymer having an isotactic or syndiotactic steric structure. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic _C1-10. Alkyl-, halo-, or polar groups-syndiotactic copolymers with substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic _C1-10 alkyl-, halo-, or polar groups- 29. The fiber of claim 28 which is a polar group modified derivative of a syndiotactic copolymer with a substituted vinyl aromatic monomer. 28. The fiber of claim 27, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180. The second thermoplastic polymer is syndiotactic polystyrene, syndiotactic of styrene and one or more cyclic C _1-10 alkyl- or halo-substituted vinyl aromatic monomers or polar group-substituted vinyl aromatic monomers. copolymers, or syndiotactic polystyrene or styrene and one or more cyclic C _1-10 alkyl -, halo -, or according to claim 30, wherein the polar group is a polar group-modified derivative of syndiotactic copolymers of substituted vinyl aromatic monomers fiber. 31. The fiber of claim 30, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000. 27. The fiber of claim 26 having a yellow index, YI, of less than 10.0. 27. The fiber of claim 26 comprising 0.1-10% of a compatibilizer c) based on the total composition weight. The compatibilizer is a polar group-modified polystyrene, a copolymer of one or more vinyl aromatic monomers and one or more polar comonomers, styrene and one or more cyclic C _1-10 alkyl- or halo-substituted vinyl aromatic monomers or polar 35. The fiber of claim 34 which is a polar group modified copolymer with a group-substituted vinyl aromatic monomer. Compatibilizer polar group-modified polystyrene or styrene and one or more cyclic C _1-10 alkyl - or halo - substituted vinyl aromatic monomer or a polar group - is a polar group-modified copolymer of substituted vinyl aromatic monomers 36. The fiber of claim 35. The compatibilizer is a maleic anhydride-modified or fumaric acid-modified styrene homopolymer or a maleic anhydride-modified or fumaric acid-modified styrene copolymer of styrene and one or more cyclic C _1-10 alkyl-substituted styrenes. 37. The fiber of claim 36, wherein the agent has 0.01-5.0 mole percent copolymerized maleic anhydride or fumaric acid functionality. 38. The fiber according to any one of claims 26 to 37, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter greater than 0.2 [mu] m. 39. The fiber of claim 38, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 [mu] m. Fibers according to claim 38 wherein component (b) is present in occluding particle form having a 3.0μm smaller ^{D 99} minor axis. Fibers according to claim 39 wherein component (b) is present in occluding particle form having a 2.8μm smaller ^{D 99} minor axis. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. 38. The fiber of any of claims 26-37, having a gloss judge rating of 4.0 or less as determined on the fiber sample. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. 41. The fiber of claim 40 having the following gloss judge grade: 38. The process of claims 26-37, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 [mu] m and the fibers have a soft hand. The fiber according to any one of the above. 41. The fiber of claim 40, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m, and said fiber has a soft hand. The amount of component (c) is in the range of 0-5% based on the combined weight of components (a) and (b) and the sum of the reactive, functional groups in component (c) (if present) The fiber according to any one of claims 26 to 37, wherein the amount is 0.001 to 0.25 mol% based on the total amount of the component (b) and the component (c). 41. The fiber of claim 40, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand and improved durability. 38. Any of claims 26-37 wherein the composition comprises 80-95% by weight of component (a); and 20-5% by weight of component (b), based on the combined weight of component (a) and component (b). The described fiber. 38. The composition of any of claims 26-37, wherein the composition comprises 86-92% by weight of component (a); and 14-8% by weight of component (b), based on the combined weight of component (a) and component (b). The described fiber. 38. The fiber of any of claims 26-37, further comprising 0.1-10.0% of the matting agent based on the total composition weight. (A) 65-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C., and (b) chemically different from (a) having a crystallization temperature, Tc ′, and Thermoplastics useful in the manufacture of extruded fibers and films, characterized in that they consist essentially of 35-3% by weight of a second thermoplastic polymer with polar functional groups, and optionally one or more non-polymeric additives. Polymer composition. 52. The composition of claim 51, wherein the first thermoplastic polymer is a polyamide or copolyamide and has a Tc 'of greater than 195C. 52. The composition of claim 51, wherein Tc is at least 5 <0> C lower than Tc '. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic _C1-10. Alkyl-, halo-, or polar groups-syndiotactic copolymers with substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic _C1-10 alkyl-, halo-, or polar groups- 52. The composition of claim 51 which is a polar group modified derivative of a syndiotactic copolymer with a substituted vinyl aromatic monomer. 53. The composition of claim 52, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180. 52. The composition of claim 51, wherein the second thermoplastic polymer is a syndiotactic polystyrene or a polar group modified derivative of a syndiotactic copolymer of styrene and p-methylstyrene. 52. The composition of claim 51, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000. 52. The composition of claim 51 having a yellow index, YI, of less than 10.0. 52. The composition of claim 51 comprising 5.0-20% by weight of component (b) as an essential component. 60. The composition according to claim 59, comprising 8-14% by weight of component (b) as an essential component. 57. The composition according to claim 56, wherein the second component is maleic anhydride- or fumaric acid-modified syndiotactic polystyrene or a maleic anhydride- or fumaric acid-modified syndiotactic copolymer of styrene and p-methylstyrene. 63. The composition of claim 61, wherein component (b) has a copolymerized maleic anhydride or fumaric acid functionality of 0.01-5.0 mol%. 63. The composition according to any of claims 51 to 62, wherein after formation of the fiber or film, component (b) is present in the matrix of component (b) in the form of occluded particles having a volume average short axis diameter greater than 0.2 µm. object. 64. The composition of claim 63, wherein after formation of the fiber or film, component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.3-2.0 [mu] m. After formation of the fiber or film, component (b) composition of claim 63 which is present in the absorbing particle form having a 3.0μm smaller D ⁹⁹ minor axis. After formation of the fiber or film composition according to claim 64, wherein the component (b) is present in occluding particle form having a 2.8μm smaller D ⁹⁹ minor axis. After formation of the fiber, component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm and the fiber is a laser having a particle size of at least 0.29. 63. The composition of any of claims 51-62, having a gloss judge rating of 4.0 or less as determined by light scattering ratio or standard fiber sample. After fiber formation, component (b) is present in the form of occluded particles with a volume average minor axis diameter of 0.2-3.0 μm and the fiber is determined by a laser light scattering ratio or a standard fiber sample of 0.29 or greater. 66. The composition of claim 65 having a gloss judge rating of 4.0 or less. After formation of the fibers, component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 μm, and the fibers have a soft hand. Item 63. The composition according to any one of Items 51 to 62. 66. The composition of claim 65, wherein after formation of the fiber, component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m, and the fiber has a soft hand. 63. The composition according to any of claims 51-62, wherein the polar groups in component (b) are reactive polar functional groups and are present in an amount of 0.001-0.25 mol% of component (b). 66. After formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand and improved durability. Composition. 70. After formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand and improved durability. Composition. 71. After formation of the fiber, component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand and improved durability. Composition. 63. The composition of any of claims 51-62, further comprising 0.1-10.0% of the matting agent based on the total composition weight. (A) 65-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C .; and (b) chemically different from (a), having a crystallization temperature, Tc ′, An extruded drawn fiber, which consists essentially of 35-3% by weight of a second thermoplastic polymer containing polar functional groups, and optionally one or more non-polymer additives. 77. The fiber of claim 76, wherein the first thermoplastic polymer is a polyamide or copolyamide and has a Tc 'of greater than 195C. 77. The fiber of claim 76, wherein Tc is at least 5C less than Tc '. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic _C1-10. Alkyl-, halo-, or polar groups-syndiotactic copolymers with substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic _C1-10 alkyl-, halo-, or polar groups- 77. The fiber of claim 76 which is a polar group modified derivative of a syndiotactic copolymer with a substituted vinyl aromatic monomer. 78. The fiber of claim 77, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180. 77. The fiber of claim 76, wherein the second thermoplastic polymer is a syndiotactic polystyrene or a polar group modified derivative of a syndiotactic copolymer of styrene and p-methylstyrene. 77. The fiber of claim 76, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000. 77. The fiber of claim 76 having a yellow index, YI, of less than 10.0. 77. The fiber of claim 76 comprising 5.0-20% by weight of component (b) as an essential component. 85. The fiber of claim 84, comprising 8-14% by weight of component (b) as an essential component. 82. The fiber of claim 81, wherein the second component is a maleic anhydride modified or fumaric acid modified syndiotactic polystyrene or a maleic anhydride modified or fumaric acid modified styrene and p-methylstyrene syndiotactic copolymer. 87. The fiber of claim 86, wherein component (b) has a copolymerized maleic anhydride or fumaric acid functionality of 0.01-5.0 mol%. 88. The fiber of any of claims 76-87, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter greater than 0.2 µm. 89. The fiber of claim 88, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 [mu] m. Fibers according to claim 88 wherein component (b) is present in occluding particle form having a 3.0μm smaller ^{D 99} minor axis. Fibers according to claim 89 wherein component (b) is present in occluding particle form having a 2.8μm smaller ^{D 99} minor axis. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. 88. The fiber of any of claims 76-87 having a gloss judge rating of 4.0 or less as determined on the fiber sample. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. 90. The fiber of claim 90 having the following gloss judge grade: 87. The composition of claim 76-87, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fibers have a soft hand. The fiber according to any one of the above. 91. The fiber of claim 90, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand. 88. The fiber of any of claims 76-87, wherein the polar groups in component (b) are reactive polar functional groups and are present at 0.001-0.25 mol% of component (b). 90. The fiber of claim 90, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand and improved durability. 95. The fiber of claim 94, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand and improved durability. 97. The fiber of claim 95, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand and improved durability. 88. The fiber of any of claims 76-87, further comprising 0.1-5.0% of the matting agent based on the total composition weight. (A) 65-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C .; and (b) chemically different from (a), having a crystallization temperature, Tc ′, Extruded, drawn, and crimped fibers characterized in that they consist essentially of 35-3% by weight of a second thermoplastic polymer containing polar functional groups, and optionally one or more non-polymer additives. The fiber of claim 101, wherein the first thermoplastic polymer is a polyamide or copolyamide and Tc 'is greater than 195C. 103. The fiber of claim 101, wherein Tc is at least 10 <0> C lower than Tc '. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic _C1-10. Alkyl-, halo-, or polar groups-syndiotactic copolymers with substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic _C1-10 alkyl-, halo-, or polar groups- 103. The fiber of claim 101, which is a polar group modified derivative of a syndiotactic copolymer with a substituted vinyl aromatic monomer. 103. The fiber of claim 102, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180. The fiber of claim 101, wherein the second thermoplastic polymer is a syndiotactic polystyrene or a polar group modified derivative of a syndiotactic copolymer of styrene and p-methylstyrene. The fiber of claim 101, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000. 103. The fiber of claim 101, having a yellow index, YI, of less than 10.0. The fiber according to claim 101, comprising 5.0-20% by weight of component (b) as an essential component. 110. The fiber of claim 109, comprising 8-14% by weight of component (b) as an essential component. 102. The fiber of claim 101, wherein component (b) is maleic anhydride- or fumaric acid-modified syndiotactic polystyrene or a maleic anhydride- or fumaric acid-modified syndiotactic copolymer of styrene and p-methylstyrene. 111. The fiber of claim 111, wherein component (b) has a copolymerized maleic anhydride or fumaric acid functionality of 0.01-5.0 mol%. The fiber according to any of claims 101-112, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of greater than 0.2 µm. 114. The fiber of claim 113, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 [mu] m. Fibers according to claim 113 wherein component (b) is present in occluding particle form having a 3.0μm smaller ^{D 99} minor axis. Fibers according to claim 114 wherein component (b) is present in occluding particle form having a 2.8μm smaller ^{D 99} minor axis. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. 113. The fiber of any of claims 101-112, having a gloss judge rating of 4.0 or less as determined on the fiber sample. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. 115. The fiber of claim 115 having the following gloss judge grade: 112. The component of claims 101-112, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fibers have a soft hand. The fiber according to any one of the above. 116. The fiber of claim 115, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.2-3.0 [mu] m, and the fiber has a soft hand. 113. The fiber of any of claims 101-112, wherein the polar groups in component (b) are reactive polar functional groups and are present in an amount of 0.001-0.25 mol% of component (b). 115. The fiber of claim 115, wherein component (b) is present in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand and improved durability. 120. The fiber of claim 119, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand and improved durability. 121. The fiber of claim 120, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand and improved durability. 113. The fiber of any of claims 101-112, further comprising 0.1-10.0% of the matting agent based on the total composition weight. 76-97% by weight of a first thermoplastic polymer consisting of two or more longitudinally-long polymer domains, wherein at least one domain has (a) a crystallization temperature, Tc, greater than 160 ° C;
(B) 24-3% by weight of a second thermoplastic polymer chemically different from (a) having a crystallization temperature, Tc ′, and (c) a compatibilizer for (a) and (b);
Here, the percentage is based on the total amount of (a) and (b), and Tc is at least 5 ° C. smaller than Tc ′, wherein the multicomponent fiber comprises a thermoplastic polymer blend. 127. The fiber of claim 126, wherein the first thermoplastic polymer of the blend is a polyamide or copolyamide and Tc 'is greater than 195C. 127. The fiber of claim 126, wherein the first thermoplastic polymer of the blend is a polyamide or copolyamide and the second thermoplastic polymer is a polyvinylidene aromatic polymer having an isotactic or syndiotactic configuration. The first thermoplastic polymer of the blend is nylon 6, nylon 6,6 or a copolymer of nylon 6 and nylon 6,6 and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic C _1-10 alkyl-, halo-, or polar group-substituted syndiotactic copolymers with vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic _C1-10 alkyl-, halo-, or 129. The fiber of claim 128, which is a polar group modified derivative of a syndiotactic copolymer with a polar group-substituted vinyl aromatic monomer. 129. The fiber of claim 128, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180. The second thermoplastic polymer is syndiotactic polystyrene, syndiotactic of styrene and one or more cyclic C _1-10 alkyl- or halo-substituted vinyl aromatic monomers or polar group-substituted vinyl aromatic monomers. copolymers, or syndiotactic polystyrene or styrene and one or more cyclic C _1-10 alkyl -, halo -, or according to claim 130, wherein the polar group is a polar group-modified derivative of syndiotactic copolymers of substituted vinyl aromatic monomers fiber. 131. The fiber of claim 130, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000. 127. The fiber of claim 126, wherein the fiber is a core / sheath fiber and the blend comprises a sheath. 127. The fiber of claim 126, wherein the blend comprises 0.1-10%, based on total composition weight, of compatibilizer c). The compatibilizer is a polar group-modified polystyrene, a copolymer of one or more vinyl aromatic monomers and one or more polar comonomers, or styrene and one or more cyclic C _1-10 alkyl- or halo-substituted vinyl aromatic monomers or 135. The fiber of claim 134, wherein the fiber is a polar group-modified copolymer of a polar group-substituted vinyl aromatic monomer. Compatibilizer polar group-modified polystyrene or styrene and one or more cyclic C _1-10 alkyl - or halo - substituted vinyl aromatic monomer or a polar group - is a polar group-modified copolymer of substituted vinyl aromatic monomers 135. The fiber of claim 135. The compatibilizer is a maleic anhydride-modified or fumaric acid-modified styrene homopolymer or a maleic anhydride-modified or fumaric acid-modified styrene copolymer of styrene and one or more cyclic C _1-10 alkyl-substituted styrenes. 139. The fiber of claim 136, wherein the agent has 0.01-5.0 mol% of copolymerized maleic anhydride or fumaric acid functionality. The fiber according to any of claims 126 to 137, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter greater than 0.2 µm. 139. The fiber of claim 138, wherein component (b) is in the form of occluded particles having a volume average short axis diameter of 0.3-2.0 [mu] m. Fibers according to claim 138 wherein component (b) is present in occluding particle form having a 3.0μm smaller ^{D 99} minor axis. Fibers according to claim 139 wherein component (b) is present in occluding particle form having a 2.8μm smaller ^{D 99} minor axis. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. 138. The fiber of any of claims 126-137 having a gloss judge rating of 4.0 or less as determined on the fiber sample. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. 141. The fiber of claim 140 having the following gloss judge grade: 142. The component of claims 126-137, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fibers have a soft hand. The fiber according to any one of the above. 141. The fiber of claim 140, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand. The amount of component (c) is in the range of 0-5% based on the combined weight of components (a) and (b) and the sum of the reactive, functional groups in component (c) (if present) The fiber according to any one of claims 126 to 137, wherein the amount is 0.001 to 0.25 mol% based on the total amount of component (b) and component (c). 141. The fiber of claim 140, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand and improved durability. 137. The blend composition of any of claims 126-137, wherein the blend composition comprises 80-95% by weight of component (a) and 20-5% by weight of component (b) based on the total amount of component (a) and component (b). Fiber. 133. The fiber of claim 133, wherein the core comprises nylon 6 or nylon 6,6. 138. The fiber of any of claims 126-137, further comprising 0.1-10.0% of the matting agent based on the total composition weight. (A) 76-97% by weight of a first thermoplastic polymer having a crystallization temperature, Tc, greater than 160 ° C.
(B) 24-3% by weight of a second thermoplastic polymer that is chemically different from (a) with a crystallization temperature, Tc ′, and, if desired,
(C) a compatibilizer for (a) and (b),
Here, the% is based on the total amount of (a) and (b), characterized in that the thermoplastic resin composition comprises a thermoplastic resin composition, and the thermoplastic resin composition comprises a base resin mainly comprising the component (a). Melting and mixing a concentrated resin consisting primarily of component (b) and optionally component (c) and, optionally, small amounts of component (a); and extruding the resulting molten thermoplastic polymer composition into fiber form and Extruded stretched fibers or extruded stretched films produced by stretching or extruding or stretching the resulting thermoplastic polymer composition into film form. 153. The fiber or film of claim 151, wherein the thermoplastic composition is made by a melt mixing process that includes extensional flow mixing. 152. The fiber or film of claim 151, wherein Tc is at least 10C lower than Tc '. The first thermoplastic polymer is nylon 6, nylon 6,6, or a copolymer of nylon 6 and nylon 6,6, and the second thermoplastic polymer is syndiotactic polystyrene, styrene and one or more cyclic _C1-10. Alkyl-, halo-, or polar groups-syndiotactic copolymers with substituted vinyl aromatic monomers, or syndiotactic polystyrene or styrene and one or more cyclic _C1-10 alkyl-, halo-, or polar groups- 151. The fiber or film of claim 151 which is a polar group modified derivative of a syndiotactic copolymer with a substituted vinyl aromatic monomer. 155. The fiber or film of claim 154, wherein the polyamide is Nylon 6 having a relative viscosity of 30-180. 151. The fiber or film of claim 151, wherein the second thermoplastic polymer is a syndiotactic polystyrene or a polar group modified derivative of a syndiotactic copolymer of styrene and p-methylstyrene. 151. The fiber or film of claim 151, wherein the second thermoplastic polymer has a tacticity greater than 95% and a Mw greater than 50,000. 152. The fiber or film of claim 151, having a yellow index, YI, of less than 10.0. 152. The fiber or film of claim 151, comprising 5.0-20% by weight of component (b) as an essential component. 160. The fiber or film of claim 159, comprising 8-14% by weight of component (b). 151. The fiber or film according to claim 151, wherein component (b) is a maleic anhydride- or fumaric-acid-modified styrene homopolymer or a copolymer of styrene and p-methylstyrene. 163. The fiber or film of claim 161, wherein component (b) has a copolymerized maleic anhydride or fumaric acid functionality of 0.01-5.0 mol%. 163. The fiber or film according to any of claims 151-162, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average short axis diameter greater than 0.2 µm. 163. The fiber of claim 163, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.3-2.0 [mu] m. Fibers according to claim 163 wherein component (b) is present in occluding particle form having a 3.0μm smaller ^{D 99} minor axis. Fibers according to claim 164 wherein component (b) is present in occluding particle form having a 2.8μm smaller ^{D 99} minor axis. Component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 μm and the fibers have a laser light scattering ratio or standard of 0.29 or greater. 163. The fiber of any of claims 151-162, having a gloss judge rating of 4.0 or less as determined on the fiber sample. Component (b) is present in the form of occluded particles with a volume-average minor axis diameter of 0.2-3.0 μm and the fiber has a laser light scattering ratio of greater than 0.29 or 4.0 determined on a standard fiber sample. 165. The fiber of claim 165 having the following gloss judge grade: 163. The process of claims 151-162, wherein component (b) is present in the matrix of component (a) in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fibers have a soft hand. The fiber according to any one of the above. 170. The fiber of claim 165, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand. The amount of component (c) is in the range of 0-5% based on the combined weight of components (a) and (b) and the sum of the reactive, functional groups in component (c) (if present) 163. The fiber according to any of claims 151 to 162, wherein the amount is 0.001-0.25 mol% based on the total amount of component (b) and component (c). 165. The fiber of claim 165, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand and improved durability. 169. The fiber of claim 169, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and the fiber has a soft hand and improved durability. 170. The fiber of claim 170, wherein component (b) is in the form of occluded particles having a volume average minor axis diameter of 0.2-3.0 [mu] m and said fiber has a soft hand and improved durability. 163. The fiber of any of claims 151-162, further comprising 0.1-5.0% of the matting agent based on the total composition weight.