JP3583587B2 - Vinyl chloride fiber and method for producing the same - Google Patents
Vinyl chloride fiber and method for producing the same Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は、かつら、ヘアピース、ブレード、エクステンションヘアー、アクセサリーヘアーなどの頭髪装飾用に用いられる人工毛髪、或いはドールヘアー等の人形用頭髪などとして使用される塩化ビニル系繊維およびその製造法に関するものである。
【０００２】
【従来の技術】
塩化ビニル系樹脂を紡糸して繊維状にしてなる塩化ビニル系繊維は、その優れた強度、伸度、カール保持性、スタイル性などの故に、頭髪装飾用などの人工毛髪用繊維として、あるいはドールヘアーなどの人形用頭髪繊維として多量に使用されている。
【０００３】
従来、一般的には、頭髪装飾用などの人工毛髪用繊維として、細繊度（断面積が小さく、細い繊維）の繊維を工業的に製造するには、塩化ビニル系樹脂に対する溶媒を使用する湿式紡糸法、または乾式紡糸法によって、細い繊度の塩化ビニル系繊維を製造する方法が工業的に実施されている。しかしながら、これらの方法は、溶媒を使用するが故に脱溶媒工程を必要とし、過大な設備投資が必要であり、その設備の維持管理にも多数の人手を必要とするという問題点がある。また、溶媒に対する溶解性を向上するべく、アクリロニトリルなどのコモノマーを共重合する為、繊維の初期着色性に弱点があり、乾燥工程での熱によって黄色味の強い毛髪になり易いという問題点、あるいは繊維のカール保持性が充分でないなどの問題点がある。
【０００４】
一方、溶媒を使用しない紡糸方法として、溶融紡糸法が知られているが、この方法にて、人毛に類似した半艶表面（艶の評価については、実施例に評価基準を示した。）、手触り触感性に優れた細繊度の繊維を製造するには、１ケの断面積が小さいノズル孔（０．５ｍｍ２以下）からストランドを溶融・流出せしめ、紡糸ドラフト比を出来得る限り小さくする（Ｄｒ比：２５以下）のが好ましい。逆に、大きな断面積のノズル孔から溶融・流出させて、細繊度の塩化ビニル繊維とすると、必然的に紡糸ドラフト比を大きくする必要があり、溶融紡糸時に、未延伸糸が極端に引き伸ばされることから、繊維（延伸糸）表面が平滑になり、光沢が出てきて、サラサラ触感がなくなり、人工毛髪用繊維としては品質的に不十分な繊維となる傾向がある。
【０００５】
しかしながら、１ケの断面積がより小さいノズル孔から流出させる場合は、ノズルにかかる圧力が高くなり、押出機の設計圧力をオーバーしてしまうという問題が発生しやすく、あるいは、その圧力を定格以下とするべく、押出量を低くすると、溶融紡糸生産性が低下するという問題、あるいは溶融粘度を低くする為に、溶融紡糸温度を高く設定すると、熱分解を起こしたり、ロングラン性が劣る結果となるという問題もあった。そのため、これらの問題を解決する為に組成物の見掛けの溶融粘度を低下するべく、カドミウムや鉛を使用するＣｄ−Ｐｂ系の熱安定剤、滑剤を使用する技術が従来技術として実施されている。
【０００６】
しかしながら、これらの配合剤は毒性が高く、製造上問題があるばかりでなく、頭髪装飾用として皮膚に触れる為、安全衛生上の問題がある。また、該頭髪装飾用品などが廃棄される場合、一般ゴミに混入して、環境を汚染するという問題もある。また、これらの配合剤を使用すると、ノズル圧力の問題、溶融紡糸生産性の問題などを解決できるものの、初期着色が大きく、黄色味の強い毛髪になる傾向があった。そこで、これらＣｄ−Ｐｂ系熱安定剤を主とした配合系の問題点を解決するべく、錫系熱安定剤あるいはＣａ−Ｚｎ系熱安定剤などを使用する方法などが提案されているが、ノズル圧力と溶融紡糸生産性とのバランスのレベルアップという観点では十分な解決には到っていない。例えば、特公昭５１−２１０９号公報では、塩素化塩化ビニル樹脂とメチルメタクリレート系樹脂を使用することにより、曳糸性を向上するという提案があるが、ノズル圧力が高くなる為、溶融粘度を低下するべく、ノズル温度を２００℃という高い温度に設定している。その為、繊維表面が平滑になり、光沢が発生し、人毛に類似した半艶表面からかけ離れたものになるばかりでなく、サラサラとした触感がなくなり、毛髪用繊維として品質的に不十分なものになるという問題があった。
【０００７】
【発明が解決しようとする課題】
本発明は、錫系熱安定剤などを使用した際に発生する「ノズル圧力が高くなる」という溶融紡糸上の課題ならびに「半艶表面性、手触り触感に劣る」という繊維品質上の課題等の従来技術の問題点を解決する為になされたものである。すなわち、本発明の第１の目的は、従来公知のＣｄ−Ｐｂ系の熱安定剤、滑剤を使用しなくとも、１ケのノズル断面積が小さいノズル孔から溶融紡糸する際の問題点を解決し、ノズル圧力と溶融紡糸生産性を高度にバランスした細繊度の塩化ビニル系樹脂繊維の製造法を提供することにあり、また第２の目的は、従来公知のＣｄ−Ｐｂ系の熱安定剤、滑剤を使用しなくても、初期着色性を大幅に改善しつつ、人毛に極めて類似した半艶表面、触感、柔軟性を保持し、また優れた強度、伸度、収縮性を保持した細繊度の塩化ビニル系繊維を提供することにある。さらに、第３の目的は、従来公知の錫系安定剤を使用した塩化ビニル系樹脂繊維の品質課題であるプラチック的触感、キラキラ感のある表面性、ゴワゴワとした指巻き触感、熱収縮性などが改善され、安全に、かつ安定的に生産できる細繊度の塩化ビニル系樹脂繊維の製造法を提供することにある。
【０００８】
【課題を解決する為の手段】
本発明者らは、上記課題を解決するべく組成物の配合系などについて鋭意研究を重ねた結果、塩化ビニル系樹脂及び／または塩素化塩化ビニル系樹脂からなる塩化ビニル系混合物に熱安定剤、滑剤ならびにノズル圧力低下剤としてフタル酸系可塑剤、トリメリット酸系可塑剤、ピロメリット酸系可塑剤、ポリエステル系可塑剤、および粘度平均重合度が４００〜８５０の塩化ビニル系樹脂から選択される１種または２種以上の可塑剤及び／樹脂を配合してなる塩化ビニル系樹脂組成物を用いることで、人毛に極めて類似した塩化ビニル系繊維を高い生産性を維持しながら得られることを見い出し、本発明を完成するに至った。
【０００９】
即ち、本発明は、粘度平均重合度が８５０〜１７００の塩化ビニル系樹脂１００〜６０重量％と塩素化塩化ビニル系樹脂０〜４０重量％からなる塩化ビニル系混合物１００重量部に対して、熱安定剤、滑剤、ならびに、ノズル圧力低下剤としてフタル酸系可塑剤、トリメリット酸系可塑剤、ピロメリット酸系可塑剤、ポリエステル系可塑剤から選択される１種または２種以上の可塑剤を１〜８重量部、および／または粘度平均重合度が４００〜８５０の塩化ビニル系樹脂を５〜３５重量部配合してなる塩化ビニル系樹脂組成物からなることを特徴とする塩化ビニル繊維である。
【００１０】
前記ノズル圧力低下剤は、フタル酸系、トリメリット酸系、ピロメリット酸系、ポリエステル系から選択される１種または２種以上の可塑剤であって、塩化ビニル系混合物１００重量部に対して、１〜８重量部配合して用いるのが好ましく、また、粘度平均重合度４００〜８５０の塩化ビニル系樹脂であって、塩化ビニル系混合物１００重量部に対して、５〜３５重量部配合して用いるのがより好ましく、塩化ビニル系混合物１００重量部に対してフタル酸系可塑剤を１〜５重量部および粘度平均重合度が４００〜８５０の塩化ビニル系樹脂を５〜１５重量部配合して用いる場合がさらに好ましい。
【００１１】
一方、本発明の製造法は、粘度平均重合度が８５０〜１７００の塩化ビニル系樹脂１００〜６０重量％と塩素化塩化ビニル系樹脂０〜４０重量％からなる塩化ビニル系混合物１００重量部に対して、熱安定剤、滑剤、ならびに、ノズル圧力低下剤としてフタル酸系可塑剤、トリメリット酸系可塑剤、ピロメリット酸系可塑剤、ポリエステル系可塑剤、および粘度平均重合度が４００〜８５０の塩化ビニル系樹脂から選択される１種または２種以上の可塑剤及び／または樹脂を配合してなる塩化ビニル系樹脂組成物を溶融紡糸することを特徴とする塩化ビニル系繊維の製造法であり、前記ノズル圧力低下剤は、フタル酸系、トリメリット酸系、ピロメリット酸系、ポリエステル系から選択される１種または２種以上の可塑剤であって、塩化ビニル系混合物１００重量部に対して、１〜８重量部配合して用いるのが好ましい。また、粘度平均重合度４００〜８５０の塩化ビニル系樹脂であって、塩化ビニル系混合物１００重量部に対して、５〜３５重量部配合して用いるのがより好ましく、塩化ビニル系混合物１００重量部に対してフタル酸系可塑剤を１〜５重量部および粘度平均重合度が４００〜８５０の塩化ビニル系樹脂を５〜１５重量部配合して用いるのがさらに好ましい。
【００１２】
また、溶融紡糸するに際し、１ケのノズル孔の断面積が０．５ｍｍ２以下のノズル孔から溶融・流出せしめることができる。
また、前記溶融紡糸するに際し、１ケのノズル孔の断面積が０．５ｍｍ２以下のノズル孔から溶融・流出せしめ、３００デニール以下の未延伸糸を製造し、次いで、この未延伸糸に延伸処理、熱処理を施して、１００デニール以下の繊維とすることもできる。
【００１３】
本発明の塩化ビニル系樹脂組成物を使用することにより、溶融紡糸する際の樹脂温度を１９５℃以下という比較的低い温度条件下で、ノズル圧力を押出機の設計圧力である５００Ｋｇ／ｃｍ２以下とし、１ケのノズル孔の断面積が０．５ｍｍ２以下のノズル孔から、６．０Ｋｇ／Ｈｒｓ以上の押出量で溶融紡糸することが可能となり、優れた強伸度、収縮性を保持し、人毛に極めて類似した半艶表面性、手触り触感性を備えた細繊度の塩化ビニル系樹脂繊維を製造することが可能となる。
【００１４】
【発明の実施の形態】
以下、本発明を詳細に説明する。
本発明でいう粘度平均重合度が８５０〜１７００の塩化ビニル系樹脂とは、従来公知の塩化ビニルの単独重合物であるホモポリマー樹脂または従来公知の各種のコポリマー樹脂からなるものであり、特に限定されるものではない。該コポリマー樹脂としては、従来公知のコポリマー樹脂を使用でき、塩化ビニル−酢酸ビニルコポリマー樹脂、塩化ビニル−プロピオン酸ビニルコポリマー樹脂など塩化ビニルとビニルエステル類とのコポリマー樹脂、塩化ビニル−アクリル酸ブチルコポリマー樹脂、塩化ビニル−アクリル酸２エチルヘキシルコポリマー樹脂など塩化ビニルとアクリル酸エステル類とのコポリマー樹脂、塩化ビニル−エチレンコポリマー樹脂、塩化ビニル−プロピレンコポリマー樹脂など塩化ビニルとオレフィン類とのコポリマー樹脂、塩化ビニル−アクリロニトルコポリマー樹脂などが代表的に例示される。特に好ましくは、塩化ビニル単独樹脂、エチレン−塩化ビニルコポリマー樹脂、酢酸ビニル−塩化ビニルコポリマー樹脂である。
【００１５】
該コポリマー樹脂に於いて、コモノマーの含有量は特に限定されず、成形加工性、糸特性などの要求品質に応じて決めることができる。特に、コモノマーの含有量は、２〜３０％であることが好ましい。
本発明に使用する塩化ビニル系樹脂の粘度平均重合度は、８５０〜１７００であることが好ましく、８５０未満であると、繊維の特性、特にカール保持性などが不十分になりやすく好ましくない。逆に、１７００を越えると、溶融粘度が高くなる為、ノズル圧力が高くなり、押出量を低く抑える必要があり好ましくない。これら成形加工性と繊維特性とのバランスから、塩化ビニル単独樹脂を使用する場合は、粘度平均重合度が８５０〜１４５０の範囲が特に好ましく、コポリマーを使用する場合は、コモノマーの含有量にも依存するが、おおよそ粘度平均重合度は、１０００〜１７００の範囲が特に好ましい。
【００１６】
また塩化ビニル系樹脂は、乳化重合、塊状重合または懸濁重合などによって製造したものを使用できるが、繊維の初期着色性などを勘案して、懸濁重合によって製造したものを使用するのが好ましい。
本発明でいう塩素化塩化ビニル系樹脂とは、塩化ビニル系樹脂を原料とし、これに塩素を付加反応せしめ、塩素含有量を５８〜７２％に高めたものであり、本発明に於いては、主たる目的として、繊維の表面性、手触り触感をコントロールし、熱収縮率を低下せしめる為に使用する。
【００１７】
本発明に使用する塩素化塩化ビニル系樹脂の粘度平均重合度（原料塩化ビニル系樹脂の粘度平均重合度）は、３００〜１１００であることが好ましい。該粘度平均重合度が３００未満であると、繊維の熱収縮率を低下せしめることが不十分となる傾向がある。逆に、該粘度平均重合度が、１１００を越えると、溶融粘度が高くなり、紡糸時のノズル圧力が高くなり、押出量を低く抑える必要があるばかりでなく、溶融紡糸時の糸の破断（糸切れ）の頻度が著しくなり、安定操業が困難となる傾向がある。特に好ましくは、粘度平均重合度は、５００〜９００のものが好ましい。
【００１８】
該塩素化塩化ビニル系樹脂の原料となる塩化ビニル系樹脂は、前述の塩化ビニル系樹脂と同様であるが、塩化ビニルホモポリマー樹脂またはエチレン−塩化ビニルコポリマー樹脂を原料として使用している場合が特に好ましい。
本発明に使用する塩素化塩化ビニル系樹脂の塩素含有量は、５８〜７２％であることが好ましい。該塩素含有量が、５８％未満であると、繊維の熱収縮率を低下せしめることが不十分となる傾向がある。逆に、該塩素含有量が、７２％を越えると溶融粘度が高くなり、紡糸時のノズル圧力が高くなり、押出量を低く抑える必要があるばかりでなく、溶融紡糸時の糸切れ頻度が著しくなり、安定操業が困難となる傾向がある。
【００１９】
本発明に於いては、塩化ビニル系樹脂と塩素化塩化ビニル系樹脂の使用比率は（塩化ビニル系樹脂／塩素化塩化ビニル系樹脂）＝（１００〜６０重量％／０〜４０重量％）の塩化ビニル系混合物とすることが好ましい。前記塩化ビニル系樹脂の比率が６０重量％未満となると、塩素化塩化ビニル系樹脂が過剰となり、溶融粘度が高くなり、溶融紡糸時のノズル圧力が高くなるため、安全操業が困難になる傾向があり好ましくない。尚、塩化ビニル系樹脂の比率が高い場合には熱収縮率の高い繊維になる傾向があり、目的に応じて、使用比率は適宜調整するのが好ましいが、特に（塩化ビニル系樹脂／塩素化塩化ビニル系樹脂）＝（９０〜７５重量％／１０〜２５重量％）の塩化ビニル系混合物とするのが好ましい。
【００２０】
本発明でいうノズル圧力低下剤とは、溶融紡糸時のノズル圧力を低下せしめるのみならず、繊維の表面の均一性をレベルアップして、平滑性を向上出来るものを含むものである。該ノズル圧力低下剤としては、フタル酸系、トリメリット酸系、ピロメリット酸系、ポリエステル系から選択される１種または２種以上の可塑剤が好ましい。エポキシ系可塑剤、アジピン酸系可塑剤、シトロン酸系可塑剤などは、繊維の初期着色性が劣ったり、ブリードして繊維表面に「ベトツキ感」がでてきて好ましくない。
【００２１】
該可塑剤の添加量は、塩化ビニル系混合物１００重量部に対して、１〜８重量部が好ましい。該添加量が１重量部未満であると、ノズル圧力低下効果が小さく、好ましくない。逆に、８重量部を越えると、繊維の熱収縮率が高くなるばかりでなく、溶融紡糸時に可塑剤ミストの発生が著しくなる傾向があり好ましくない。これら溶融紡糸時の挙動、繊維の熱収縮率などの品質とのバランスから、特に好ましい可塑剤はイソノニルフタレート、ウンデシルフタレートなどのフタル酸系可塑剤、トリオクチルトリメリテートなどのトリメリット酸系可塑剤、テトラオクチルピロメリテートなどのピロメリット酸系可塑剤などが望ましい。
【００２２】
また、ノズル圧力低下剤としては粘度平均重合度が、４００〜８５０の塩化ビニル系樹脂が、より好ましく、該塩化ビニル系樹脂は従来公知の塩化ビニルの単独重合物であるホモポリマー樹脂または従来公知の各種のコポリマー樹脂を用いることができ、特に限定されるものではない。該樹脂を使用することで、表面凹凸の均一性をレベルアップして、繊維表面の平滑性を向上することができる。
【００２３】
該樹脂の粘度平均重合度が４００未満であると、繊維の熱収縮率が高くなる傾向があり、また溶融紡糸時の塩ビ系混合物のゲル化・溶融状態が不均一となり、糸切れ頻度が多くなる傾向があり好ましくない。逆に、該樹脂の粘度平均重合度が８５０を越えると、ノズル圧力低下効果がなく好ましくない。
該樹脂の添加量は、塩化ビニル系混合物１００重量部に対して、５〜３５重量部使用するのが好ましい。使用量が５重量部未満であるとノズル圧力低下効果が小さく、３５重量部を越えると繊維の熱収縮率が高くなり好ましくない。
【００２４】
特に好ましくは、粘度平均重合度が６００〜８５０の塩化ビニルホモポリマーまたはエチレン−塩化ビニル共重合樹脂、酢酸ビニル−塩化ビニル共重合樹脂のうち１種以上の樹脂を５〜１５重量部使用するのが良い。
さらに、ノズル圧力低下剤としては、塩ビ系混合物１００重量部に対して、フタル酸系可塑剤を１〜５重量部および粘度平均重合度が４００〜８５０の塩化ビニル系樹脂を５〜１５重量部併用すると溶融紡糸性能、繊維品質、生産性などが高度にバランスされた範囲となる。
【００２５】
本発明でいう熱安定剤とは、従来公知の熱安定剤を用いることができる。例えば、金属石鹸系熱安定剤、錫系熱安定剤、Ｃａ−Ｚｎ系熱安定剤、ハイドロタルサイト系熱安定剤、ゼオライト系熱安定剤などの熱安定剤から１種または２種以上の熱安定剤を選択し、塩化ビニル系混合物１００重量部に対して、０．５〜５．０重量部使用するのが好ましい。該熱安定剤は、成形時の熱分解、ロングラン性、繊維の色調を改良する効果があるが、特に好ましくは、紡糸時のノズル目脂（ノズル周囲のスケール等をいう）発生量の比較的少ない錫系熱安定剤が良く、中でもメルカプト錫系熱安定剤、マレエート錫系熱安定剤、ラウレート錫系熱安定剤から、１種または２種以上を使用するのが特に好ましい。例えば、ジメチルスズメルカプト、ジブチルスズメルカプト、ジオクチルスズメルカプトなどのメルカプト錫系熱安定剤、ジメチルスズマレエート、ジブチルスズマレエート、ジオクチルスズマレエート、ジオクチルスズマレエートポリマーなどのマレエート錫系熱安定剤、ジメチルラウレート、スズジブチルスズラウレート、ジオクチルスズラウレートなどのラウレート錫系熱安定剤が例示される。
【００２６】
該熱安定剤の使用量が、０．５重量部未満となると、成形時の熱分解防止効果が少なくなり好ましくない。逆に５．０重量部を越えると、紡糸時のノズル目脂発生が多くなり好ましくない。
繊維の初期着色を抑制し、顔料を含まないナチュラル組成物の白色度を高める為には、メルカプト錫系熱安定剤を塩ビ系混合物１００重量部に対して、少なくとも０．１〜１．４重量部使用し、他の熱安定剤と併用するのが特に好ましい。
【００２７】
本発明でいう滑剤とは、従来公知の滑剤を用いることができ、例えば、金属石鹸系滑剤、ポリエチレン系滑剤、高級脂肪酸系滑剤、ペンタエリスリトール系滑剤、高級アルコール系滑剤、モンタン酸ワックス系滑剤から選択される１種または２種以上の滑剤を塩化ビニル系混合物１００重量部に対して、０．２〜５．０重量部使用するのが好ましい。
【００２８】
該滑剤は、組成物の溶融状態、ならびに組成物と金属面との接着状態を制御する効果があり、繊維の表面状態、触感、糸切れ頻度、ノズル目脂発生頻度、ノズル圧力などに影響する。
比較的サラサラとした触感を得る為に、金属石鹸系滑剤を使用するのが好ましい。特に、衛生上の観点から、カドミウム石鹸以外の金属石鹸が好ましい。例えば、Ｎａ，Ｍｇ，Ａｌ，Ｃａ，Ｂａなどのステアレート、ラウレート、パルミテート、オレエートなどの金属石鹸が例示される。特に好ましくは、該金属石鹸系滑剤を０．５〜２．０重量部使用するのが良い。
【００２９】
ノズル目脂発生頻度を低下し、ノズル圧力を低く抑える為には、ポリエチレン系滑剤を使用するのが好ましく、従来公知のポリエチレン系滑剤を使用できるが、特に平均分子量が１５００〜４０００であり、密度が０．９１〜０．９７の非酸化タイプまたはごくわずかに極性を附加したタイプのポリエチレン系滑剤が好ましい。特に好ましくは、該ポリエチレン系滑剤を０．１〜１．３重量部使用するのが良い。
【００３０】
また、主として組成物の溶融状態を制御する為には、高級脂肪酸系滑剤、ペンタエリスリトール系滑剤、高級アルコール系滑剤、モンタン酸ワックス系滑剤が好ましい。高級脂肪酸系滑剤としては、例えば、ステアリン酸、パルミチン酸、ミリスチン酸、ラウリン酸、カプリン酸などの飽和脂肪酸、オレイン酸などの不飽和脂肪酸またはこれらの混合物などが例示される。ペンタエリスリトール系滑剤としては、ペンタエリスリトールまたはジペンタエリスリトールと高級脂肪酸とのモノエステル、ジエステル、トリエステル、テトラエステルまたはこれらの混合物などが例示される。高級アルコール系滑剤としては、ステアリルアルコール、パルミチルアルコール、ミリスチルアルコール、ラウリルアルコール、オレイルアルコールなどが例示される。さらに、モンタン酸ワックス系滑剤としては、モンタン酸とステアリルアルコール、パルミチルアルコール、ミリスチルアルコール、ラウリルアルコール、オレイルアルコールなどの高級アルコールとのエステル類が例示される。
【００３１】
本発明に於いて、該滑剤系の特に好ましい使用量の範囲は、塩化ビニル系混合物１００重量部に対して、カドミウム石鹸を含有しない金属石鹸系滑剤を０．５〜３．０重量部、ポリエチレン系滑剤を０．１〜１．８重量部、ペンタエリスリトール系滑剤を０．２〜１．０重量部併用するのが特に好ましい。
本発明に於いては、他に目的に応じて、塩化ビニル系組成物に使用される公知の配合剤、例えば、加工助剤、強化剤、紫外線吸収剤、酸化防止剤、、帯電防止剤、充填剤、難燃剤、顔料などを使用することができる。また、場合によっては、発泡剤、架橋剤、粘着性付与剤、親水性付与剤、導電性付与剤、香料など特殊な配合剤を使用することもできる。
【００３２】
前記加工助剤としては、公知のものを使用できる。例えば、メチルメタクリレートを主成分とするアクリル系加工助剤、または熱可塑性ポリエステルを主成分とするポエステル系加工助剤などを使用できる。該加工助剤の使用量としては、塩化ビニル系混合物１００重量部に対して、０．２〜１２重量部程度が好ましい。また、これらの加工助剤は、単独でも使用できるし、２種以上を併用しても良い。
【００３３】
本発明に使用できる充填剤としては、公知のものを使用できる。例えば、炭酸カルシウム、炭酸マグネシウム、酸化マグネシウム、酸化アルミニウム、水酸化マグネシウム、水酸化アルミニウム、タルク、マイカ、クレーなどを使用できる。該充填剤の使用量としては、塩化ビニル系混合物１００重量部に対して、０．２〜５重量部程度が好ましい。また、これらの充填剤は、単独でも使用できるし、２種以上を併用しても良い。
【００３４】
本発明に使用する塩化ビニル系樹脂組成物は、従来公知の混合機、例えば、ヘンシェルミキサー、スーパーミキサー、リボンブレンダーなどを使用して混合してなるパウダーコンパウンド、またはこれを溶融混合してなるペレットコンパウンドとして使用することができる。
該パウダーコンパウンドの製造は、従来公知の通常の条件で製造でき、ホットブレンドでもコールドブレンドでも良い。特に好ましくは、組成物中の揮発分を減少する為に、ブレンド時のカット温度を１０５〜１５５℃迄上げてなるホットブレンドを使用するのが良い。
【００３５】
該ペレットコンパウンドは、通常の塩化ビニル系ペレットコンパウンドの製造と同様にして製造できる。例えば、単軸押出機、異方向２軸押出機、コニカル２軸押出機、同方向２軸押出機、コニーダー、プラネタリーギアー押出機、ロール混練り機などの混練り機を使用して、ペレットコンパウンドとすることができる。該ペレットコンパウンドを製造する際の条件は、特に限定はされないが樹脂温度を１８５℃以下になる様に設定することが特に好ましい。
【００３６】
また、該ペレットコンパウンド中に混入し得る掃除用具の金属片などの異物を取り除く為に、目開きの細かいステンレスメッシュなどを混練り機内に設置したり、コールドカットの際、混入し得る「切り粉」などを除去する手段を取ったり、ホットカットを行うなどの方法は自在に可能であるが、特に好ましくは、「切り粉」混入の少ないホットカット法を使用するのが好ましい。
【００３７】
本発明に於いて、塩化ビニル系樹脂組成物を繊維状の未延伸糸にする際には、従来公知の押出機を使用できる。例えば、単軸押出機、異方向２軸押出機、コニカル２軸押出機などを使用できるが、例えば口径が３５〜８５ｍｍφ程度の単軸押出機、または口径が３５〜５０ｍｍφ程度のコニカル押出機を使用するのが好ましい。口径が大き過ぎると、押出量が多くなり、ノズル圧力が過大になったり、未延伸糸の流出速度が早過ぎて、巻取りが困難になる傾向があり好ましくない。
【００３８】
本発明の塩化ビニル系樹脂組成物を溶融紡糸するに場合に於いては、１ケのノズル孔の断面積が、０．５ｍｍ２以下のノズルをダイ先端部に取り付けて溶融紡糸を行なうのが好ましい。該断面積が０．５ｍｍ２を越えるノズルを使用すると、未延伸糸の繊度が太くなり、細繊度の繊維を得る為には、延伸処理の際、延伸倍率を大きくする必要がある。その為、延伸処理を施した後の細繊度の繊維（延伸糸）に光沢が出て、半艶〜七部艶状態を維持することが困難となる。また、繊維の触感が、ザラザラとしたり、キラキラ感がでたり、あるいはプラスチック的な滑り触感になる傾向があり好まくない。
【００３９】
更に、未延伸糸の繊度を３００デニール以下にすることで、延伸後の繊維の艶を半艶〜七部艶状態にすることが可能となる。該未延伸糸の繊度が３００デニールを越えると、細繊度の繊維を得る為には、延伸処理の際に延伸倍率を大きくする必要がある。そのため、延伸処理を施した後の細繊度の繊維（延伸糸）に光沢が出て、半艶〜七部艶状態を維持することが困難となる。また、プラスチック的な滑り触感になる傾向がある。
【００４０】
前記溶融紡糸で得られた未延伸糸に公知の方法で延伸処理・熱処理を施して、１００デニール以下の細繊度の繊維とすることができる。頭髪装飾用の繊維としては、２５〜１００デニールの範囲が特に好ましい。また、人形用頭髪の繊維としては、１０〜６５デニールの範囲が特に好ましい。延伸処理条件としては、延伸処理温度７０〜１５０℃の雰囲気下で、延伸倍率は、２００〜４５０％程度延伸することが特に好ましい。延伸処理温度が７０℃未満であると繊維の強度が低くなると共に、糸切れを発生し易く、１５０℃を越えると繊維の触感がプラスチック的な滑り触感になる傾向があり好ましくない。また、延伸倍率が２００％未満であると繊維の強度発現が不十分となりやすく、４５０％を越えると延伸処理時に、糸切れを発生し易く好ましくない。
【００４１】
さらに、延伸処理を施した繊維に熱処理を施して、２〜７５％の緩和率で繊維を緩和処理することにより熱収縮率を低下させることができる、また、繊維表面の凹凸を整えて、人毛に類似した触感、半艶〜七部艶表面とする為にも該緩和処理が好ましい。該緩和率の範囲を外れると人工毛髪用繊維として、あるいはドールヘアー用繊維として、品質が低下する傾向があり好ましくない。該熱処理は、延伸処理と連動して実施することもできるし、切り離して実施することもできる。熱処理温度条件としては、雰囲気温度８０〜１５０℃の雰囲気下で実施することが特に好ましい。また本発明に於いては、従来公知の溶融紡糸に関わる技術、例えば、各種ノズル断面形状に関わる技術、加熱筒に関わる技術、延伸処理に関わる技術、熱処理に関わる技術などは、自在に組み合わせて使用することが可能である。
【００４２】
【実施例】
次に、実施例をあげて、本発明のさらに詳細に説明するが、これらの実施例は、本発明の適用限界を明らかにする為に例示するものに過ぎず、本発明は、これらの実施例のみに限定されるものではない。
尚、表中の組成物等は、次のように略記する。
塩化ビニル樹脂：「ＰＶＣ」、塩素化塩化ビニル系樹脂：「ＣＰＶＣ」、粘度平均重合度：「Ｍ」、また表２、４〜５における、組成物での配合剤の数値は、ＰＶＣとＣＰＶＣの合計＝１００重量部に対する各配合剤の重量部を表すものである。
【００４３】
［実験１〜５（可塑剤添加量の効果）］
塩化ビニル系混合物１００重量部が４Ｋｇになる様に計量し、次いで、可塑剤（ジイソノニルフタレート）の添加量を変更しながら、表２に示す配合剤をそれぞれ計量して２０Ｌのヘンシェルミキサーに投入し、攪拌しながら、内容物の温度が１２５℃になる迄、攪拌・混合した。その後、冷却水をヘンシェルミキサーのジャケットに流しながら攪拌・混合を続け、内容物の温度が７５℃になる迄、冷却して、塩ビ系パウダーコンパウンドを得た。
【００４４】
該パウダーコンパウンドを表１（紡糸条件１）に示す条件にて、溶融紡糸実験に供した。
【００４５】
【表１】
溶融紡糸実験は、定常状態になってから、スクリュー回転数と押出量の関係を求め、押出量が７．５Ｋｇ／Ｈｒｓになる様にスクリュー回転数を決定した。ノズル圧力、ダイ圧計をノズル部に設置して測定した。鉛直方向にノズルから溶融・流出したストランドを加熱紡糸筒に導入し、ここで該ストランドを瞬間的に加熱溶解し、ノズル直下約３ｍの位置に設置した引取機にて、未延伸糸を一定速度で巻き取った。この際、該未延伸糸の繊度が約１６８デニール程度になる様に引取速度を調節した。
【００４７】
この未延伸糸を製造する段階で、糸切れの発生状況を目視観察し、次の様に評価した。
［溶融紡糸時の糸切れ発生状況］
◎： 全く糸切れが発生しない
○：１時間に３回以内発生する
△：１時間に４〜１５回発生する
またこの未延伸糸の着色状態を目視観察にて、次の様に評価した。
【００４８】
［未延伸糸の着色状態］
◎：乳白色で黄色味がない
○：乳白色であるが、わずかに黄色味がある
△：かなり強い黄色味がある
該未延伸糸を延伸・熱処理機に導入し、延伸処理、次いで、熱緩和処理を行い、延伸糸を製造した。この際、熱緩和処理は、３０％緩和に固定し、延伸処理は最終の延伸糸の繊度が６８デニールになる様に延伸倍率を若干調整した。
この延伸・熱処理時に発生する糸切れの発生状況を目視観察し、次の様に評価した。
【００４９】
［延伸・熱処理時の糸切れ発生状況］
◎：全く糸切れが発生しない
○：１時間に３回以内発生する
△：１時間に４〜１５回発生する
また、この延伸糸の表面艶・光沢を目視観察し、次の様に評価した。
【００５０】
［延伸糸の艶状態］
◎（半艶状態）：表面が平滑で、わずかに鈍い光沢があり、半艶状態を示す
○（七部艶状態）：表面が平滑で、鈍い光沢があり、七部艶状態を示す
●（完全艶消状態）：表面がザラザラで、光沢がなく、完全艶消状態を示す
×（艶有状態）： 表面が平滑で、全面的に光沢があり、輝き感がある
さらに、この延伸糸を手で触り、その手触り触感を、次の様に評価した。
【００５１】
［延伸糸の触感］
◎：表面が平滑で、サラサラとした触感がある
○：表面が平滑で、かすかに湿った触感があるが、サラサラ感がある
△（ザラザラ感）：表面がザラザラで、ザラザラとした触感がある
●（プラスチック感）：表面が平滑で、プラスチック的触感があり、滑り触感がある
またさらに、この延伸糸を指に数回巻き付け、その際の反発力、触感、柔軟性を、次の様に評価した。
【００５２】
［延伸糸のしなやかさ］
◎：指にやわらかく、しなやかに巻き取ることができる
○：かすかに反発触感があるが、しなやかに巻き取ることができる
●（ゴワゴワ感）：全体的に硬い感触で、かなり強い反発触感がある
△（ザラザラ感）：指にやわらかく巻けるが、ザラザラとした触感がある
該延伸糸を引張試験、熱収縮試験に供し、強度および熱収縮率を求めた。尚、延伸糸の熱収縮率の測定は、１００℃の雰囲気温度で、２５分熱収縮させ、計算は、次の様に行なった。
【００５３】
［熱収縮率］
（熱処理前の延伸糸長−熱処理後の延伸糸長）／熱処理前の延伸糸長×１００ ＝熱収縮率（％）
これらの評価結果を表２に示す。
【００５４】
【表２】
実験１〜５の比較から判る様に、可塑剤の配合比率が１重量部未満であると繊維の品質は良好であるが、ノズル圧力が５００Ｋｇ／ｃｍ２以上になり、押出機の設計圧力を超える状態になり、安全な生産ができなくなる傾向がある。一方、可塑剤の配合比率が８重量部を越えると組成の溶融状態が不均一となり、溶融紡糸時、延伸時の糸切れが著しくなる。また、繊維の表面がザラザラとした手触り触感になる。さらに、ノズル圧力を低下する為に、スクリュー回転数を低下すると、押出量が低下して、溶融紡糸生産性が低下する。これらの実験から、ノズル圧力と繊維品質のバランスが最適となる可塑剤の配合比率は、塩化ビニル系混合物１００重量部に対して、１〜８重量部の領域が最適であることが判る。
【００５６】
［実験６〜１０」（低重合度塩化ビニル系樹脂の添加効果）］
実験１〜５と同様に塩化ビニル系混合物１００重量部が４Ｋｇになる様に計量し、次いで、低重合度塩化ビニル系樹脂の添加量を変更し、表４に示す配合剤をそれぞれ計量して、２０Ｌのヘンシェルミキサーに投入し、攪拌しながら、内容物の温度が１０５℃になる迄、攪拌・混合した。その後、冷却水をヘンシェルミキサーのジャケットに流しながら攪拌・混合を続け、内容物の温度が７０℃になる迄、冷却して、塩ビ系パウダーコンパウンドを得た。尚、繊維の柔軟性を向上する為に、ＥＶＡ系樹脂（酢酸ビニル含有量＝２５％，メルトインデックス＝３）を使用した。該パウダーコンパウンドを表３（ペレット条件）に示した条件にて、ペレットコンパウンド とし、表１（紡糸条件１）と同様の条件にて、溶融紡糸実験に供した。
【００５７】
【表３】
該ペレットコンパウンドを、表１と同様の条件にて、溶融紡糸実験を行った。溶融紡糸実験は、定常状態になってから、スクリュー回転数と押出量の関係を求め、押出量が７．２Ｋｇ／Ｈｒｓになる様に、スクリュー回転数を決定した。
ノズル圧力、樹脂温度は、ダイ圧計ならびに樹脂温度センサーをノズル部に設置して測定した。鉛直方向にノズルから溶融・流出したストランドを加熱紡糸筒に導入し、ここで該ストランドを瞬間的に加熱溶解し、ノズル直下、約３ｍの位置に設置した引取機にて、未延伸糸を一定速度で巻き取った。この際、該未延伸糸の繊度が約１６８デニール程度になる様に引取速度を調節した。
【００５９】
また、その他の紡糸条件などは、実験１〜５に示した方法と同様に行い、評価方法なども実験１〜５に示した方法と全く同様に行なった。これらの評価結果を表４に示す。
【００６０】
【表４】
実験６〜１０の比較から判る様に、低重合度塩化ビニル系樹脂の配合比率が５重量部未満であると繊維の品質は良好であるが、ノズル圧力が５００Ｋｇ／ｃｍ２以上になり、押出機の設計圧力を超える状態になり、安全な生産ができなくなる。 一方、可塑剤の配合比率が３５重量部を越えるとノズル圧力は安全な領域を確保できるものの、繊維の熱収縮率が高くなる傾向にある。さらに、ノズル圧力を低下する為に、スクリュー回転数を低下すると、押出量が低下して、溶融紡糸生産性が低下する。これらの実験から、ノズル圧力と繊維品質のバランスが最適となる低重合度塩化ビニル系樹脂の配 合比率は、塩化ビニル系混合物１００重量部に対して、５〜３５重量部の領域が最適であることが判る。
【００６２】
［実験１１〜１５（低重合度塩化ビニル樹脂と可塑剤の併用効果）］
実験１〜５と同様、塩化ビニル系混合物１００重量部が４Ｋｇになる様に計量し、次いで、低重合度塩化ビニル樹脂、可塑剤の添加量ならびに種類を変更しながら、表５に示す配合剤をそれぞれ計量して、２０Ｌのヘンシェルミキサーに投入し、攪拌しながら、内容物の温度が１１５℃になる迄、攪拌・混合した。その後、冷却水をヘンシェルミキサーのジャケットに流しながら攪拌・混合を続け、内容物の温度が７５℃になる迄、冷却して、塩ビ系パウダーコンパウンドを得た。
【００６３】
該パウダーコンパウンドを実験１〜５に示した紡糸条件，延伸条件，加熱緩和処理条件と全く同様の条件にて、溶融紡糸・延伸・熱処理実験に供した。また、実験１〜５に示した試験方法、評価方法にて、未延伸糸、延伸糸の評価を全く同様に行なった。評価結果を表５に示す。
【００６４】
【表５】
実験１１〜１５の比較から判る様に、低重合度塩化ビニル樹脂と可塑剤を併用することにより、繊維品質とノズル圧力のバランスの優れる領域を容易に得ることができる。とりわけ、熱収縮率の点から、フタル酸可塑剤（ＤＩＮＰ）がもっとも良好な繊維品質となる。
【００６６】
【発明の効果】
以上のように、本発明の塩化ビニル系樹脂組成物を用いれば、品質に優れ、人毛に極めて類似した七部〜半艶表面の手触り触感を兼ね備えた塩化ビニル系繊維を得られ、また、本発明の製造法を用いれば、目的の塩化ビニル系繊維を、高い紡糸生産性を維持しながら、安全に製造することができる。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a vinyl chloride fiber used as artificial hair used for hair decoration such as a wig, a hairpiece, a blade, an extension hair, an accessory hair, or a doll hair such as a doll hair, and a method for producing the same. is there.
[0002]
[Prior art]
Polyvinyl chloride fiber, which is formed by spinning a vinyl chloride resin into a fibrous form, has excellent strength, elongation, curl retention, and styling properties. It is used in large quantities as hair fibers for dolls such as hair.
[0003]
Conventionally, in general, in order to industrially produce fibers of fineness (small cross-sectional area, fine fibers) as artificial hair fibers for hair decoration and the like, a wet process using a solvent for a vinyl chloride resin is required. 2. Description of the Related Art A method for producing vinyl chloride fibers having fineness by a spinning method or a dry spinning method is industrially practiced. However, these methods have a problem that a solvent is used, so that a desolvation step is required, an excessive capital investment is required, and maintenance and management of the equipment require a large number of people. Further, in order to improve the solubility in the solvent, to copolymerize a comonomer such as acrylonitrile, there is a weak point in the initial coloring of the fiber, there is a problem that the hair in the drying process is likely to become a strong yellowish hair, or There are problems such as insufficient curl retention of the fiber.
[0004]
On the other hand, a melt spinning method is known as a spinning method that does not use a solvent. In this method, a semi-gloss surface similar to human hair (for the evaluation of gloss, evaluation criteria are shown in Examples). In order to produce fine fibers with excellent touch feeling, a single nozzle hole (0.5 mm 2 It is preferred that the strands are melted and flown out of the following) to reduce the spinning draft ratio as much as possible (Dr ratio: 25 or less). Conversely, if vinyl chloride fibers are melted and flown out from the nozzle holes having a large cross-sectional area to produce fine fine vinyl fibers, the spinning draft ratio must necessarily be increased, and the undrawn yarn is extremely stretched during melt spinning. As a result, the fiber (drawn yarn) surface becomes smooth and glossy, the smooth feel is lost, and the fiber for artificial hair tends to be insufficient in quality.
[0005]
However, when one of the cross-sectional areas is made to flow out from a smaller nozzle hole, the pressure applied to the nozzle is increased, and the problem of exceeding the design pressure of the extruder is likely to occur. Therefore, if the extrusion rate is reduced, the melt spinning productivity decreases, or if the melt spinning temperature is set high in order to lower the melt viscosity, thermal decomposition occurs or the long run property is poor. There was also a problem. Therefore, in order to solve these problems, in order to reduce the apparent melt viscosity of the composition, a technology using a Cd-Pb-based heat stabilizer using cadmium or lead and a lubricant is used as a conventional technology. .
[0006]
However, these compounding agents are highly toxic and have problems not only in production but also in safety and hygiene because they come into contact with the skin for hair decoration. Further, when the hair ornaments are discarded, they are mixed with general garbage and pollute the environment. In addition, when these compounding agents are used, the problem of nozzle pressure, the problem of melt spinning productivity, and the like can be solved, but the hair tends to have large initial coloring and a strong yellow tint. Therefore, in order to solve the problems of the compounding system mainly including the Cd-Pb-based heat stabilizer, a method using a tin-based heat stabilizer or a Ca-Zn-based heat stabilizer has been proposed. A sufficient solution has not been reached from the viewpoint of improving the balance between nozzle pressure and melt spinning productivity. For example, Japanese Patent Publication No. Sho 51-2109 proposes to improve the spinnability by using a chlorinated vinyl chloride resin and a methyl methacrylate resin, but the melt viscosity is reduced because the nozzle pressure is increased. For this purpose, the nozzle temperature is set to a high temperature of 200 ° C. As a result, the fiber surface becomes smooth and glossy, not only is it far from a semi-glossy surface resembling human hair, but also loses a smooth feel and is insufficient in quality as a fiber for hair. There was a problem of becoming something.
[0007]
[Problems to be solved by the invention]
The present invention relates to a problem in melt spinning such as "nozzle pressure is increased" and a problem in fiber quality such as "semi-gloss surface property and inferior touch feeling" generated when a tin-based heat stabilizer or the like is used. The purpose of the present invention is to solve the problems of the prior art. That is, the first object of the present invention is to solve the problem of melt-spinning from one nozzle having a small nozzle cross-sectional area without using a conventionally known Cd-Pb-based heat stabilizer or lubricant. It is another object of the present invention to provide a method for producing a fine vinyl chloride resin fiber having a high balance between nozzle pressure and melt spinning productivity, and a second object of the present invention is to provide a conventionally known Cd-Pb-based heat stabilizer. Even without the use of lubricants, while maintaining a significantly improved initial coloring, while maintaining a semi-glossy surface, touch and flexibility very similar to human hair, and also maintaining excellent strength, elongation and shrinkage It is an object of the present invention to provide a fine vinyl chloride fiber. Further, the third object is a quality problem of a vinyl chloride-based resin fiber using a conventionally known tin-based stabilizer, such as a plastic touch feeling, a glittering surface property, a stiff finger touch feeling, a heat shrinkage property, and the like. It is an object of the present invention to provide a method for producing a fine vinyl chloride resin fiber which can be produced stably and stably.
[0008]
[Means for solving the problem]
The present inventors have conducted intensive studies on the compounding system of the composition and the like in order to solve the above problems, and as a result, a heat stabilizer was added to a vinyl chloride-based resin and / or a vinyl chloride-based mixture comprising a chlorinated vinyl chloride-based resin. The lubricant and the nozzle pressure reducing agent are selected from phthalic acid plasticizers, trimellitic acid plasticizers, pyromellitic acid plasticizers, polyester plasticizers, and vinyl chloride resins having a viscosity average polymerization degree of 400 to 850. By using a vinyl chloride resin composition containing one or more plasticizers and / or resins, it is possible to obtain vinyl chloride fibers very similar to human hair while maintaining high productivity. They have found and completed the present invention.
[0009]
That is, according to the present invention, 100 parts by weight of a vinyl chloride-based resin composed of 100 to 60% by weight of a vinyl chloride-based resin having a viscosity average polymerization degree of 850 to 1700 and 0 to 40% by weight of a chlorinated vinyl chloride-based resin is used. Phthalate plasticizer, trimellitic plasticizer, pyromellitic plasticizer, polyester plasticizer as stabilizer, lubricant, and nozzle pressure reducing agent 1 to 8 parts by weight of one or more plasticizers selected from ,and / Or A vinyl chloride resin having a viscosity average degree of polymerization of 400 to 850 5 to 35 parts by weight A vinyl chloride fiber comprising a vinyl chloride resin composition blended.
[0010]
The nozzle pressure reducing agent is one or more plasticizers selected from phthalic acid, trimellitic acid, pyromellitic acid, and polyester, and based on 100 parts by weight of the vinyl chloride mixture. , 1 to 8 parts by weight of a vinyl chloride resin having a viscosity average degree of polymerization of 400 to 850, and 5 to 35 parts by weight based on 100 parts by weight of the vinyl chloride mixture. More preferably, 1 to 5 parts by weight of a phthalic acid plasticizer and 5 to 15 parts by weight of a vinyl chloride resin having a viscosity average polymerization degree of 400 to 850 are added to 100 parts by weight of the vinyl chloride mixture. It is more preferable to use them.
[0011]
On the other hand, the production method of the present invention is based on 100 parts by weight of a vinyl chloride-based mixture comprising 100 to 60% by weight of a vinyl chloride-based resin having a viscosity average polymerization degree of 850 to 1700 and 0 to 40% by weight of a chlorinated vinyl chloride-based resin. A heat stabilizer, a lubricant, and a phthalic acid-based plasticizer, a trimellitic acid-based plasticizer, a pyromellitic acid-based plasticizer, a polyester-based plasticizer, and a viscosity average polymerization degree of 400 to 850 as a nozzle pressure reducing agent. A method for producing a vinyl chloride fiber, comprising melt-spinning a vinyl chloride resin composition comprising one or more plasticizers and / or resins selected from vinyl chloride resins. The nozzle pressure reducing agent is one or more plasticizers selected from phthalic acid, trimellitic acid, pyromellitic acid, and polyester; Relative system 100 parts by weight of a mixture, is preferably used by blending 1-8 weight parts. Further, it is a vinyl chloride resin having a viscosity average degree of polymerization of 400 to 850, more preferably 5 to 35 parts by weight based on 100 parts by weight of the vinyl chloride mixture, and 100 parts by weight of the vinyl chloride mixture. It is more preferable to use 1 to 5 parts by weight of a phthalic acid plasticizer and 5 to 15 parts by weight of a vinyl chloride resin having a viscosity average polymerization degree of 400 to 850.
[0012]
Also, when performing melt spinning, the cross-sectional area of one nozzle hole is 0.5 mm. 2 It can be melted and discharged from the following nozzle holes.
When the melt spinning is performed, the cross-sectional area of one nozzle hole is 0.5 mm. 2 The undrawn yarn having a density of 300 denier or less can be manufactured by melting and flowing out from the following nozzle holes, and then the undrawn yarn can be subjected to a stretching treatment and a heat treatment to obtain a fiber having a denier of 100 denier or less.
[0013]
By using the vinyl chloride-based resin composition of the present invention, the nozzle pressure is set to 500 Kg / cm, which is the design pressure of the extruder, under the condition that the resin temperature during melt spinning is relatively low, such as 195 ° C. or less. 2 The cross-sectional area of one nozzle hole is 0.5 mm 2 From the following nozzle holes, it becomes possible to perform melt spinning at an extrusion rate of 6.0 Kg / Hrs or more, maintain excellent strong elongation and shrinkage, and have semi-glossy surface properties and hand-feel tactility very similar to human hair It is possible to produce a vinyl chloride-based resin fiber having a fine fineness provided with:
[0014]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, the present invention will be described in detail.
The vinyl chloride resin having a viscosity average polymerization degree of 850 to 1700 in the present invention is a homopolymer resin which is a homopolymer of a conventionally known vinyl chloride or a conventionally known various copolymer resin, and is particularly limited. It is not done. As the copolymer resin, conventionally known copolymer resins can be used, such as vinyl chloride-vinyl acetate copolymer resin, vinyl chloride-vinyl propionate copolymer resin, a copolymer resin of vinyl chloride and vinyl esters, and a vinyl chloride-butyl acrylate copolymer. Resin, copolymer resin of vinyl chloride and acrylates such as vinyl chloride-ethyl hexyl acrylate copolymer resin, vinyl chloride-ethylene copolymer resin, copolymer resin of vinyl chloride and olefins such as vinyl chloride-propylene copolymer resin, vinyl chloride Acrylonitrile polymer resin and the like are typically exemplified. Particularly preferred are vinyl chloride alone resin, ethylene-vinyl chloride copolymer resin, and vinyl acetate-vinyl chloride copolymer resin.
[0015]
In the copolymer resin, the content of the comonomer is not particularly limited, and can be determined according to required quality such as moldability and yarn characteristics. In particular, the comonomer content is preferably 2 to 30%.
The viscosity average degree of polymerization of the vinyl chloride resin used in the present invention is preferably 850 to 1700, and if it is less than 850, the properties of the fiber, particularly the curl retention, tend to be insufficient, which is not preferable. Conversely, if it exceeds 1,700, the melt viscosity becomes high, so that the nozzle pressure becomes high, and it is necessary to keep the extrusion amount low, which is not preferable. From the balance between the moldability and the fiber properties, when using vinyl chloride alone resin, the viscosity average degree of polymerization is particularly preferably in the range of 850 to 1450, and when using a copolymer, it also depends on the comonomer content. However, the viscosity average polymerization degree is particularly preferably in the range of 1,000 to 1,700.
[0016]
Further, the vinyl chloride resin can be used those produced by emulsion polymerization, bulk polymerization or suspension polymerization, but it is preferable to use those produced by suspension polymerization in consideration of the initial coloring properties of the fibers and the like. .
The chlorinated vinyl chloride resin referred to in the present invention is a vinyl chloride resin as a raw material, to which chlorine is added and reacted to increase the chlorine content to 58 to 72%. The main purpose is to control the surface properties and feel of the fibers and to reduce the heat shrinkage.
[0017]
The chlorinated vinyl chloride resin used in the present invention preferably has a viscosity average degree of polymerization (viscosity average degree of polymerization of the starting vinyl chloride resin) of 300 to 1100. If the viscosity-average degree of polymerization is less than 300, it tends to be insufficient to lower the heat shrinkage of the fiber. Conversely, if the viscosity average degree of polymerization exceeds 1100, the melt viscosity increases, the nozzle pressure during spinning increases, and it is necessary not only to reduce the extrusion rate but also to break the yarn during melt spinning ( The frequency of thread breakage) becomes remarkable, and stable operation tends to be difficult. Particularly preferably, the viscosity average polymerization degree is from 500 to 900.
[0018]
The vinyl chloride resin used as a raw material of the chlorinated vinyl chloride resin is the same as the above-mentioned vinyl chloride resin, except that a vinyl chloride homopolymer resin or an ethylene-vinyl chloride copolymer resin is used as a raw material. Particularly preferred.
The chlorinated vinyl chloride resin used in the present invention preferably has a chlorine content of 58 to 72%. If the chlorine content is less than 58%, it tends to be insufficient to reduce the heat shrinkage of the fiber. Conversely, if the chlorine content exceeds 72%, the melt viscosity increases, the nozzle pressure during spinning increases, and not only does the extrusion rate need to be kept low, but also the frequency of yarn breakage during melt spinning becomes extremely high. And stable operation tends to be difficult.
[0019]
In the present invention, the usage ratio of the vinyl chloride resin to the chlorinated vinyl chloride resin is (vinyl chloride resin / chlorinated vinyl chloride resin) = (100 to 60% by weight / 0 to 40% by weight). It is preferable to use a vinyl chloride-based mixture. When the ratio of the vinyl chloride resin is less than 60% by weight, the chlorinated vinyl chloride resin becomes excessive, the melt viscosity increases, and the nozzle pressure during melt spinning increases. There is not preferred. When the ratio of the vinyl chloride resin is high, the fiber tends to have a high heat shrinkage, and it is preferable to appropriately adjust the usage ratio according to the purpose. It is preferable to use a vinyl chloride-based mixture of (vinyl chloride-based resin) = (90 to 75% by weight / 10 to 25% by weight).
[0020]
The term "nozzle pressure reducing agent" as used in the present invention includes those which can not only lower the nozzle pressure during melt spinning but also improve the uniformity of the fiber surface and improve the smoothness. As the nozzle pressure reducing agent, one or more plasticizers selected from phthalic acid, trimellitic acid, pyromellitic acid, and polyester are preferable. Epoxy plasticizers, adipic acid plasticizers, citronic acid plasticizers and the like are not preferred because the initial coloring properties of the fibers are poor, or the fibers bleed to give a "sticky feeling" on the fiber surface.
[0021]
The amount of the plasticizer is preferably 1 to 8 parts by weight based on 100 parts by weight of the vinyl chloride-based mixture. If the amount is less than 1 part by weight, the effect of lowering the nozzle pressure is small, which is not preferable. Conversely, if the amount exceeds 8 parts by weight, not only is the thermal shrinkage of the fiber increased, but also the plasticizer mist tends to be significantly generated during melt spinning, which is not preferable. Particularly preferred plasticizers are phthalic acid-based plasticizers such as isononyl phthalate and undecyl phthalate, and trimellitic acid such as trioctyl trimellitate, in view of the balance between the behavior during melt spinning and the quality such as the heat shrinkage of the fiber. A plasticizer, a pyromellitic plasticizer such as tetraoctyl pyromellitate, and the like are preferable.
[0022]
Further, as the nozzle pressure lowering agent, a vinyl chloride resin having a viscosity average polymerization degree of 400 to 850 is more preferable, and the vinyl chloride resin is a conventionally known homopolymer resin which is a homopolymer of vinyl chloride or a conventionally known vinyl chloride resin. Can be used, and is not particularly limited. By using the resin, the uniformity of the surface irregularities can be improved, and the smoothness of the fiber surface can be improved.
[0023]
When the viscosity-average degree of polymerization of the resin is less than 400, the heat shrinkage of the fiber tends to be high, and the gelation / melting state of the PVC-based mixture during melt spinning becomes non-uniform, and the frequency of yarn breakage is high. This is not preferred. Conversely, if the viscosity average polymerization degree of the resin exceeds 850, the effect of lowering the nozzle pressure is not obtained, which is not preferable.
The addition amount of the resin is preferably 5 to 35 parts by weight based on 100 parts by weight of the vinyl chloride mixture. If the amount is less than 5 parts by weight, the effect of lowering the nozzle pressure is small, and if it exceeds 35 parts by weight, the heat shrinkage of the fiber is undesirably high.
[0024]
Particularly preferably, 5 to 15 parts by weight of one or more resins of a vinyl chloride homopolymer or an ethylene-vinyl chloride copolymer resin or a vinyl acetate-vinyl chloride copolymer resin having a viscosity average polymerization degree of 600 to 850 is used. Is good.
Further, as the nozzle pressure reducing agent, 1 to 5 parts by weight of a phthalic acid-based plasticizer and 5 to 15 parts by weight of a vinyl chloride resin having a viscosity average polymerization degree of 400 to 850 with respect to 100 parts by weight of a PVC mixture. When used together, the melt spinning performance, fiber quality, productivity, etc., are in a highly balanced range.
[0025]
As the heat stabilizer in the present invention, a conventionally known heat stabilizer can be used. For example, heat stabilizers such as metal soap heat stabilizers, tin heat stabilizers, Ca-Zn heat stabilizers, hydrotalcite heat stabilizers, and zeolite heat stabilizers may be used. It is preferable to select a stabilizer and use 0.5 to 5.0 parts by weight based on 100 parts by weight of the vinyl chloride-based mixture. The heat stabilizer has an effect of improving thermal decomposition, long run property and color tone of the fiber at the time of molding, and particularly preferably, has a relatively small amount of nozzle grease (such as scale around the nozzle) generated during spinning. A small amount of a tin-based heat stabilizer is preferred, and among these, one or more of a mercaptotin-based heat stabilizer, a maleate tin-based heat stabilizer, and a laurate tin-based heat stabilizer are particularly preferably used. For example, dimethyltin mercapto, dibutyltin mercapto, mercaptotin-based heat stabilizers such as dioctyltin mercapto, dimethyltin maleate, dibutyltin maleate, dioctyltin maleate, maleate tin-based heat stabilizers such as dioctyltin maleate polymer, dimethyl Examples thereof include tin laurate-based heat stabilizers such as laurate, tin dibutyltin laurate, and dioctyltin laurate.
[0026]
If the amount of the heat stabilizer is less than 0.5 parts by weight, the effect of preventing thermal decomposition during molding is undesirably reduced. Conversely, if the amount exceeds 5.0 parts by weight, undesired nozzle grease during spinning increases.
In order to suppress the initial coloring of the fiber and increase the whiteness of the pigment-free natural composition, at least 0.1 to 1.4 parts by weight of the mercaptotin-based heat stabilizer is added to 100 parts by weight of the PVC-based mixture. It is particularly preferable to use the heat stabilizer in combination with another heat stabilizer.
[0027]
As the lubricant in the present invention, a conventionally known lubricant can be used. It is preferable to use one or more selected lubricants in an amount of 0.2 to 5.0 parts by weight based on 100 parts by weight of the vinyl chloride mixture.
[0028]
The lubricant has an effect of controlling the molten state of the composition, and the state of adhesion between the composition and a metal surface, and affects the surface state of the fiber, tactile sensation, frequency of thread breakage, frequency of occurrence of nozzle grease, nozzle pressure, and the like. .
In order to obtain a relatively smooth feel, it is preferable to use a metal soap-based lubricant. Particularly, from the viewpoint of hygiene, metal soaps other than cadmium soap are preferable. For example, metal soaps such as stearate such as Na, Mg, Al, Ca and Ba, laurate, palmitate and oleate are exemplified. Particularly preferably, 0.5 to 2.0 parts by weight of the metal soap lubricant is used.
[0029]
In order to reduce the frequency of occurrence of nozzle grease and to keep the nozzle pressure low, it is preferable to use a polyethylene-based lubricant. Conventionally known polyethylene-based lubricants can be used, and particularly, the average molecular weight is 1500 to 4000, and the density is high. Is preferably a non-oxidized type or a slightly-polarized type polyethylene-based lubricant having a ratio of 0.91 to 0.97. Particularly preferably, the polyethylene lubricant is used in an amount of 0.1 to 1.3 parts by weight.
[0030]
In order to mainly control the molten state of the composition, a higher fatty acid lubricant, a pentaerythritol lubricant, a higher alcohol lubricant, and a montanic acid wax lubricant are preferred. Examples of the higher fatty acid-based lubricant include saturated fatty acids such as stearic acid, palmitic acid, myristic acid, lauric acid, and capric acid, unsaturated fatty acids such as oleic acid, and mixtures thereof. Examples of the pentaerythritol-based lubricant include monoesters, diesters, triesters, tetraesters of pentaerythritol or dipentaerythritol and higher fatty acids, and mixtures thereof. Examples of the higher alcohol lubricant include stearyl alcohol, palmityl alcohol, myristyl alcohol, lauryl alcohol, oleyl alcohol and the like. Further, examples of the montanic acid wax-based lubricant include esters of montanic acid with higher alcohols such as stearyl alcohol, palmityl alcohol, myristyl alcohol, lauryl alcohol, and oleyl alcohol.
[0031]
In the present invention, a particularly preferable range of the amount of the lubricant system used is such that 0.5 to 3.0 parts by weight of a metal soap-based lubricant containing no cadmium soap and 100 parts by weight of a vinyl chloride-based mixture, It is particularly preferable to use 0.1 to 1.8 parts by weight of a system lubricant and 0.2 to 1.0 part by weight of a pentaerythritol system lubricant.
In the present invention, according to other purposes, known compounding agents used in the vinyl chloride composition, for example, processing aids, reinforcing agents, ultraviolet absorbers, antioxidants, antistatic agents, Fillers, flame retardants, pigments and the like can be used. In some cases, a special compounding agent such as a foaming agent, a cross-linking agent, a tackifier, a hydrophilicity-imparting agent, a conductivity-imparting agent, or a fragrance may be used.
[0032]
Known processing aids can be used. For example, an acrylic processing aid mainly composed of methyl methacrylate, or a polyester processing aid mainly composed of thermoplastic polyester can be used. The amount of the processing aid used is preferably about 0.2 to 12 parts by weight based on 100 parts by weight of the vinyl chloride mixture. These processing aids can be used alone or in combination of two or more.
[0033]
Known fillers can be used in the present invention. For example, calcium carbonate, magnesium carbonate, magnesium oxide, aluminum oxide, magnesium hydroxide, aluminum hydroxide, talc, mica, clay and the like can be used. The amount of the filler used is preferably about 0.2 to 5 parts by weight based on 100 parts by weight of the vinyl chloride mixture. These fillers can be used alone or in combination of two or more.
[0034]
The vinyl chloride resin composition used in the present invention may be a powder compound obtained by mixing using a conventionally known mixer, for example, a Henschel mixer, a super mixer, a ribbon blender, or a pellet obtained by melt-mixing the powder compound. Can be used as a compound.
The powder compound can be produced under conventionally known ordinary conditions, and may be a hot blend or a cold blend. It is particularly preferable to use a hot blend in which the cutting temperature at the time of blending is raised to 105 to 155 ° C. in order to reduce volatile components in the composition.
[0035]
The pellet compound can be produced in the same manner as in the production of an ordinary vinyl chloride pellet compound. For example, using a kneading machine such as a single-screw extruder, a bidirectional twin-screw extruder, a conical twin-screw extruder, a co-axial twin-screw extruder, a co-kneader, a planetary gear extruder, and a roll kneader, pellets are used. It can be a compound. The conditions for producing the pellet compound are not particularly limited, but it is particularly preferable to set the resin temperature to 185 ° C. or lower.
[0036]
Further, in order to remove foreign substances such as metal pieces of a cleaning tool that can be mixed in the pellet compound, a stainless mesh with a fine opening is installed in a kneading machine, or `` cut powder '' which can be mixed in a cold cut. , Etc., or a method such as hot cutting can be freely used, but a hot cutting method with less mixing of “cutting chips” is particularly preferable.
[0037]
In the present invention, when the vinyl chloride-based resin composition is converted into a fibrous undrawn yarn, a conventionally known extruder can be used. For example, a single-screw extruder, a bidirectional twin-screw extruder, a conical twin-screw extruder, or the like can be used. For example, a single-screw extruder having a diameter of about 35 to 85 mmφ, or a conical extruder having a diameter of about 35 to 50 mmφ is used. It is preferred to use. If the diameter is too large, the amount of extrusion increases, the nozzle pressure becomes excessive, or the outflow speed of the undrawn yarn tends to be too fast, which tends to make winding difficult.
[0038]
When melt-spinning the vinyl chloride resin composition of the present invention, the cross-sectional area of one nozzle hole is 0.5 mm 2 It is preferable to perform the melt spinning by attaching the following nozzle to the tip of the die. The cross-sectional area is 0.5mm 2 When a nozzle exceeding is used, the fineness of the undrawn yarn becomes large, and in order to obtain a fine fiber, it is necessary to increase the draw ratio during the drawing treatment. For this reason, the fiber (drawn yarn) having a fine fineness after the drawing treatment is glossy, and it is difficult to maintain a semi-gloss to seven-part gloss state. In addition, the texture of the fibers tends to be rough, glittery, or has a plastic-like sliding feel, which is not preferred.
[0039]
Furthermore, by setting the fineness of the undrawn yarn to 300 denier or less, it is possible to make the gloss of the drawn fiber half-gloss to seven-part gloss. If the fineness of the undrawn yarn exceeds 300 denier, it is necessary to increase the draw ratio during the drawing process in order to obtain a fine fiber. For this reason, the fibers (drawn yarns) having a fine fineness after the drawing treatment are glossy, and it is difficult to maintain a semi-gloss to seven-part gloss state. Also, it tends to have a plastic-like sliding feel.
[0040]
The undrawn yarn obtained by the melt spinning can be subjected to a drawing treatment and a heat treatment by a known method to obtain a fiber having a fineness of 100 denier or less. The fiber for hair decoration is particularly preferably in the range of 25 to 100 denier. Further, the fiber of the doll's hair is particularly preferably in the range of 10 to 65 denier. As the stretching treatment conditions, it is particularly preferable that the stretching is performed at a stretching ratio of about 200 to 450% in an atmosphere at a stretching treatment temperature of 70 to 150 ° C. If the stretching treatment temperature is lower than 70 ° C., the strength of the fiber is lowered, and yarn breakage is apt to occur. If the temperature is higher than 150 ° C., the feel of the fiber tends to be a plastic-like sliding feel, which is not preferable. On the other hand, if the draw ratio is less than 200%, the strength of the fiber tends to be insufficiently expressed, and if it exceeds 450%, yarn breakage is apt to occur during the stretching treatment, which is not preferable.
[0041]
Furthermore, the heat-shrinkage rate can be reduced by subjecting the drawn fiber to a heat treatment to relax the fiber at a relaxation rate of 2 to 75%. The relaxation treatment is also preferable in order to obtain a texture similar to hair and a semi-glossy to seven-part gloss surface. If the relaxation ratio is out of the range, the quality tends to deteriorate as a fiber for artificial hair or a fiber for doll hair, which is not preferable. The heat treatment can be carried out in conjunction with the stretching treatment or can be carried out separately. As the heat treatment temperature condition, it is particularly preferable to perform the heat treatment in an atmosphere at an ambient temperature of 80 to 150 ° C. Further, in the present invention, conventionally known techniques related to melt spinning, for example, techniques related to various nozzle cross-sectional shapes, techniques related to a heating cylinder, techniques related to a stretching process, techniques related to a heat treatment, and the like can be freely combined. It is possible to use.
[0042]
【Example】
Next, the present invention will be described in more detail with reference to examples. However, these examples are merely examples for clarifying the application limit of the present invention, and the present invention is not limited to these examples. It is not limited to examples only.
The compositions and the like in the table are abbreviated as follows.
Vinyl chloride resin: "PVC", chlorinated vinyl chloride resin: "CPVC", viscosity average degree of polymerization: "M". In Tables 2, 4 to 5, the numerical values of the compounding agents in the compositions are PVC and CPVC. Represents 100 parts by weight of the total amount of the components.
[0043]
[Experiments 1 to 5 (Effect of Plasticizer Addition Amount)]
100 parts by weight of the vinyl chloride-based mixture was weighed so as to become 4 kg, and then, while changing the addition amount of the plasticizer (diisononyl phthalate), the compounding agents shown in Table 2 were respectively weighed and put into a 20 L Henschel mixer. While stirring, the contents were stirred and mixed until the temperature of the contents reached 125 ° C. Thereafter, stirring and mixing were continued while cooling water was passed through the jacket of the Henschel mixer, and the contents were cooled until the temperature of the contents reached 75 ° C. to obtain a PVC powder compound.
[0044]
The powder compound was subjected to a melt spinning experiment under the conditions shown in Table 1 (spinning conditions 1).
[0045]
[Table 1]
In the melt spinning experiment, the relationship between the screw rotation speed and the extrusion amount was determined after the steady state was reached, and the screw rotation speed was determined so that the extrusion amount became 7.5 kg / Hrs. Nozzle pressure and a die pressure gauge were installed in the nozzle part and measured. The strands that have melted and flowed out of the nozzle in the vertical direction are introduced into a heated spinning cylinder, where the strands are instantaneously heated and melted. Rolled up. At this time, the take-up speed was adjusted so that the fineness of the undrawn yarn was about 168 denier.
[0047]
At the stage of producing this undrawn yarn, the occurrence of yarn breakage was visually observed and evaluated as follows.
[Yarn breakage during melt spinning]
◎: No thread breakage occurs
○: occurs within 3 times in one hour
△: 4 to 15 times per hour
The coloring state of the undrawn yarn was visually observed and evaluated as follows.
[0048]
[Coloring state of undrawn yarn]
◎: Milky white with no yellow color
：: Milky white, but slightly yellowish
△: fairly strong yellow color
The undrawn yarn was introduced into a drawing / heat treatment machine, subjected to a drawing treatment, and then subjected to a heat relaxation treatment to produce a drawn yarn. At this time, the heat relaxation treatment was fixed at 30% relaxation, and the stretching treatment was slightly adjusted in the draw ratio so that the fineness of the final drawn yarn was 68 denier.
The state of occurrence of yarn breakage generated during the stretching and heat treatment was visually observed and evaluated as follows.
[0049]
[Yarn breakage during drawing and heat treatment]
：: No thread breakage occurs
○: occurs within 3 times in one hour
△: 4 to 15 times per hour
Further, the surface gloss and gloss of the drawn yarn were visually observed and evaluated as follows.
[0050]
[Gloss of drawn yarn]
◎ (semi-gloss state): Smooth surface, slightly dull gloss, showing semi-gloss state
○ (Seven-part gloss state): The surface is smooth and has a dull gloss, indicating a seven-part gloss state
● (Complete matte state): The surface is rough, has no luster and shows a completely matte state
× (Glossy state): The surface is smooth, glossy over the entire surface, and has a shining feeling
Further, the drawn yarn was touched by hand, and the touch feeling was evaluated as follows.
[0051]
[Tactile sensation of drawn yarn]
◎: The surface is smooth and has a smooth touch
：: The surface is smooth and has a slightly damp feel, but has a smooth feeling
△ (rough feeling): the surface is rough, and there is a rough touch
● (Plastic feeling): The surface is smooth, has a plastic touch, and has a sliding touch
Further, the drawn yarn was wound around a finger several times, and the resilience, tactile sensation and flexibility at that time were evaluated as follows.
[0052]
[Flexibility of drawn yarn]
◎: Soft and flexible
：: There is a slight repulsive feeling, but it can be rewound gently
● (Rough feeling): Hard feeling on the whole, with quite strong repulsive feeling
△ (rough feeling): softly wrapped around the finger, but with a rough touch
The drawn yarn was subjected to a tensile test and a heat shrink test to determine the strength and the heat shrinkage. In addition, the measurement of the heat shrinkage of the drawn yarn was performed by heat shrinking at 100 ° C. atmosphere temperature for 25 minutes, and the calculation was performed as follows.
[0053]
[Heat shrinkage]
(Stretched yarn length before heat treatment-Stretched yarn length after heat treatment) / Stretched yarn length before heat treatment × 100 = heat shrinkage (%)
Table 2 shows the evaluation results.
[0054]
[Table 2]
As can be seen from the comparison of Experiments 1 to 5, when the blending ratio of the plasticizer is less than 1 part by weight, the fiber quality is good, but the nozzle pressure is 500 kg / cm. 2 As described above, the pressure exceeds the design pressure of the extruder, and there is a tendency that safe production cannot be performed. On the other hand, if the blending ratio of the plasticizer exceeds 8 parts by weight, the molten state of the composition becomes non-uniform, and the yarn breakage during melt spinning and stretching becomes remarkable. In addition, the surface of the fiber has a rough touch feeling. Further, when the screw rotation speed is reduced to lower the nozzle pressure, the extrusion amount is reduced, and the melt spinning productivity is reduced. From these experiments, it can be seen that the blending ratio of the plasticizer that optimizes the balance between the nozzle pressure and the fiber quality is optimal in the range of 1 to 8 parts by weight with respect to 100 parts by weight of the vinyl chloride mixture.
[0056]
[Experiments 6 to 10] (Effect of addition of low polymerization degree vinyl chloride resin)]
In the same manner as in Experiments 1 to 5, 100 parts by weight of the vinyl chloride-based mixture was weighed so as to become 4 kg, and then the amount of the low-polymerization degree vinyl chloride-based resin was changed. , A 20 L Henschel mixer, and stirred and mixed with stirring until the temperature of the contents reached 105 ° C. Thereafter, stirring and mixing were continued while flowing cooling water through the jacket of the Henschel mixer, and the contents were cooled until the temperature of the contents reached 70 ° C. to obtain a PVC-based powder compound. In order to improve the flexibility of the fiber, an EVA resin (vinyl acetate content = 25%, melt index = 3) was used. The powder compound was used as a pellet compound under the conditions shown in Table 3 (pellet conditions) and subjected to a melt spinning experiment under the same conditions as in Table 1 (spinning conditions 1).
[0057]
[Table 3]
The pellet compound was subjected to a melt spinning experiment under the same conditions as in Table 1. In the melt spinning experiment, the relationship between the screw rotation speed and the extrusion amount was determined after the steady state was reached, and the screw rotation speed was determined so that the extrusion amount became 7.2 kg / Hrs.
The nozzle pressure and the resin temperature were measured by installing a die pressure gauge and a resin temperature sensor in the nozzle portion. The strands that have melted and flowed out of the nozzle in the vertical direction are introduced into a heated spinning tube, where the strands are instantaneously heated and melted. Winded up at speed. At this time, the take-up speed was adjusted so that the fineness of the undrawn yarn was about 168 denier.
[0059]
Other spinning conditions and the like were performed in the same manner as in the methods shown in Experiments 1 to 5, and the evaluation method and the like were performed in exactly the same manner as in the methods shown in Experiments 1 to 5. Table 4 shows the evaluation results.
[0060]
[Table 4]
As can be seen from the comparison of Experiments 6 to 10, when the blending ratio of the vinyl chloride resin having a low polymerization degree is less than 5 parts by weight, the quality of the fiber is good, but the nozzle pressure is 500 kg / cm. 2 As a result, the pressure exceeds the design pressure of the extruder, and safe production cannot be performed. On the other hand, if the blending ratio of the plasticizer exceeds 35 parts by weight, the nozzle pressure can secure a safe region, but the thermal shrinkage of the fiber tends to increase. Further, when the screw rotation speed is reduced to lower the nozzle pressure, the extrusion amount is reduced, and the melt spinning productivity is reduced. From these experiments, it is found that the ratio of the vinyl chloride resin having a low polymerization degree at which the balance between the nozzle pressure and the fiber quality is optimum is optimally in the range of 5 to 35 parts by weight with respect to 100 parts by weight of the vinyl chloride mixture. It turns out that there is.
[0062]
[Experiments 11 to 15 (Effects of Using Vinyl Chloride Resin with Low Polymerization Degree and Plasticizer)]
In the same manner as in Experiments 1 to 5, 100 parts by weight of the vinyl chloride-based mixture was weighed so as to become 4 kg, and then, while changing the addition amount and type of the low-polymerization degree vinyl chloride resin and the plasticizer, Was weighed, charged into a 20 L Henschel mixer, and stirred and mixed with stirring until the content temperature reached 115 ° C. Thereafter, stirring and mixing were continued while cooling water was passed through the jacket of the Henschel mixer, and the contents were cooled until the temperature of the contents reached 75 ° C. to obtain a PVC powder compound.
[0063]
The powder compound was subjected to a melt spinning / drawing / heat treatment experiment under exactly the same conditions as the spinning conditions, stretching conditions and heat relaxation treatment conditions shown in Experiments 1 to 5. The undrawn yarn and the drawn yarn were evaluated in exactly the same manner by the test methods and evaluation methods shown in Experiments 1 to 5. Table 5 shows the evaluation results.
[0064]
[Table 5]
As can be seen from the comparison of Experiments 11 to 15, a region in which the balance between the fiber quality and the nozzle pressure is excellent can be easily obtained by using a low polymerization degree vinyl chloride resin and a plasticizer in combination. In particular, phthalic acid plasticizer (DINP) has the best fiber quality in terms of heat shrinkage.
[0066]
【The invention's effect】
As described above, by using the vinyl chloride-based resin composition of the present invention, it is possible to obtain a vinyl chloride-based fiber having excellent touch quality and a touch feeling of a seven-part to semi-gloss surface very similar to human hair, According to the production method of the present invention, the desired vinyl chloride fiber can be produced safely while maintaining high spinning productivity.
Claims (6)
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| JP22028797A JP3583587B2 (en) | 1997-08-15 | 1997-08-15 | Vinyl chloride fiber and method for producing the same |
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| KR100780134B1 (en) * | 2003-04-04 | 2007-11-28 | 덴끼 가가꾸 고교 가부시키가이샤 | Polyvinyl chloride fiber, process for producing the same, and use thereof |
| CN100336950C (en) * | 2003-04-04 | 2007-09-12 | 电气化学工业株式会社 | Polyvinyl chloride fiber, process for producing the same, and use thereof |
| KR101162784B1 (en) | 2003-10-03 | 2012-07-04 | 덴끼 가가꾸 고교 가부시키가이샤 | Polyvinyl chloride fiber for artificial hair, method and apparatus for producing the same |
| JP2005116593A (en) | 2003-10-03 | 2005-04-28 | Ube Ind Ltd | Thermoelectric transducer |
| KR101044900B1 (en) * | 2006-02-28 | 2011-06-28 | 덴끼 가가꾸 고교 가부시키가이샤 | Vinyl chloride resin fiber and method for producing same |
| WO2018221348A1 (en) * | 2017-05-30 | 2018-12-06 | デンカ株式会社 | Artificial hair fiber |
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