JPH0123571B2 - - Google Patents

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Publication number
JPH0123571B2
JPH0123571B2 JP59209628A JP20962884A JPH0123571B2 JP H0123571 B2 JPH0123571 B2 JP H0123571B2 JP 59209628 A JP59209628 A JP 59209628A JP 20962884 A JP20962884 A JP 20962884A JP H0123571 B2 JPH0123571 B2 JP H0123571B2
Authority
JP
Japan
Prior art keywords
yarn
aromatic polyamide
producing
stretching
aromatic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
JP59209628A
Other languages
Japanese (ja)
Other versions
JPS6189317A (en
Inventor
Yukikage Matsui
Shozaburo Hiratsuka
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Teijin Ltd
Original Assignee
Teijin Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Teijin Ltd filed Critical Teijin Ltd
Priority to JP20962884A priority Critical patent/JPS6189317A/en
Publication of JPS6189317A publication Critical patent/JPS6189317A/en
Publication of JPH0123571B2 publication Critical patent/JPH0123571B2/ja
Granted legal-status Critical Current

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  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Description

【発明の詳細な説明】[Detailed description of the invention]

産業上の利用分野 本発明は芳香族ポリアミド繊維の製造方法に関
するものである。更に詳しくは、特定のポリマー
繰返し単位からなる実質的にパラ配向の芳香族ポ
リアミドの糸条を高温下で高倍率に延伸して、優
れた品位の高強力高モジユラス芳香族ポリアミド
繊維を良好な工程調子にて製造する方法に関する
ものである。 従来技術 近年、産業用の合成繊維に対する要求が高度化
し、特に高強力高モジユラス化の要請に対し、
種々の新規な繊維素材が開発されつつある。 それらのうち、或る種の芳香族ポリアミド繊
維、殊に英国特許第1501948号明細書に記載のよ
うなポリアミド繰返し単位の一部にエーテル結合
を含む実質的にパラ配向の芳香族コポリアミドの
繊維にあつては、その性能を発現させるため、糸
条を400℃以上の最高延伸温度で6倍以上の全延
伸倍率に1段又は2段以上で延伸する方法が採用
される。この場合、該糸条はネツクを生ずること
なく徐々に延伸され、所謂フロー延伸の形態をと
る。 ところで、芳香族ポリアミドの糸条を400℃以
上のような高温下で延伸を行うと、該糸条を構成
する繊維は延伸時に著しく軟化するため、単繊維
間での融着現象がさけられない。特に、該糸条を
構成する単繊維の数が多くなると融着はますます
増大し、得られる延伸糸は著しく柔軟性の低い低
品位のものとなつてしまう。また、このように糸
条が著しく軟化した状態で延伸する場合、糸条を
均一に加熱することが特に重要であり、もし加熱
が均一に行われないと工程調子が低下する。 発明の目的 本発明の主たる目的は、前述の如き芳香族ポリ
アミドの糸条を高温下で延伸を行う際に生ずる単
繊維間の融着を防止すると共に、延伸時に個々の
単繊維に対して均一に熱を与えることにより、高
品位の高強力高モジユラス芳香族ポリアミド繊維
を優れた工程調子で製造する方法を提供すること
にある。 発明の構成 前述の目的は、本発明に従い、特定の芳香族ポ
リアミドからなる糸条を、最高延伸温度400℃以
上にて、6倍以上の全延伸倍率に1段又は2段以
上で延伸して高強力高モジユラスの芳香族ポリア
ミド繊維を製造する方法において、400℃以上の
温度で延伸を行う際に、延伸される糸条を扁平状
に拡げ、かつ延伸直前の糸条の幅に対する延伸直
後の糸条の幅が1.1〜10倍となるように開繊して
延伸することによつて達成される。 本発明の方法が適用される芳香族ポリアミド
は、ポリマー繰返し単位の80モル%以上が下記の
繰返し単位: ―NH―Ar1―NHCO―Ar2―CO― 〔ここで、Ar1,Ar2は、それぞれ
INDUSTRIAL APPLICATION FIELD The present invention relates to a method for producing aromatic polyamide fibers. More specifically, a substantially para-oriented aromatic polyamide yarn consisting of a specific polymer repeating unit is drawn at a high magnification under high temperature to produce an excellent quality, high tenacity, high modulus aromatic polyamide fiber in a favorable process. The present invention relates to a method for manufacturing the same. Prior Art In recent years, the demands for industrial synthetic fibers have become more sophisticated, especially in response to the demand for high strength and high modulus.
Various new fiber materials are being developed. Among them, certain aromatic polyamide fibers, in particular fibers of substantially para-oriented aromatic copolyamides containing ether linkages in some of the polyamide repeat units, as described in British Patent No. 1501948. In order to achieve this performance, a method is adopted in which the yarn is stretched in one or two or more stages at a maximum stretching temperature of 400° C. or higher and a total stretching ratio of 6 times or higher. In this case, the yarn is drawn gradually without creating a neck, taking the form of so-called flow drawing. By the way, when an aromatic polyamide thread is drawn at a high temperature of 400°C or higher, the fibers constituting the thread soften significantly during drawing, so fusion between single fibers is unavoidable. . In particular, as the number of single fibers constituting the yarn increases, the fusion increases more and more, and the resulting drawn yarn becomes of low quality with extremely low flexibility. Furthermore, when drawing the yarn in such a significantly softened state, it is particularly important to uniformly heat the yarn, and if heating is not performed uniformly, the process performance will deteriorate. Purpose of the Invention The main purpose of the present invention is to prevent the fusion between the single fibers that occurs when drawing the aromatic polyamide yarn at high temperatures as described above, and to uniformly distribute the individual single fibers during drawing. An object of the present invention is to provide a method for producing high-grade, high-strength, high-modulus aromatic polyamide fibers with excellent process conditions by applying heat to the fibers. Structure of the Invention The above-mentioned object, according to the present invention, is to draw a yarn made of a specific aromatic polyamide in one or two or more stages at a maximum drawing temperature of 400° C. or more to a total stretching ratio of 6 times or more. In a method for producing high-strength, high-modulus aromatic polyamide fibers, when drawing is carried out at a temperature of 400°C or higher, the drawn thread is spread out into a flat shape, and the width of the thread immediately before drawing is This is achieved by opening and drawing the yarn so that its width is 1.1 to 10 times larger. In the aromatic polyamide to which the method of the present invention is applied, 80 mol% or more of the polymer repeating units are the following repeating units: -NH-Ar 1 -NHCO-Ar 2 -CO- [Here, Ar 1 and Ar 2 are ,Each

【式】【formula】

【式】及び[Formula] and

【式】から選ばれた少くと も1種の芳香族残基を示す。なおAr1,Ar2は互
いに同一でも相異るものでもよい。またこれらの
芳香族残基における水素原子の全部又は一部がハ
ロゲン原子又は低級アルキル基で置換されていて
もよい。〕 で構成される実質的にバラ配向の芳香族ポリアミ
ドであればよいが、なかでも、前記Ar1,Ar2の
合計の80モル%以上が、次のような芳香族残基(A)
及び(B)もしくは(B′)からなり、かつ(B)もしく
は(B′)の比率が10〜40%を占める芳香族コポ
リアミドが好適である。 〔これらの芳香族残基の水素原子は、ハロゲン
原子及び/又は低級アルキル基で置換されていて
もよい。〕 このような芳香族コポリアミドの製造方法の詳
細については、英国特許第1501948号明細書、米
国特許第3738964号明細書、特開昭49−100322号
公報等に記載されている。 好適な芳香族ポリアミドの例としては、次の3
種のモノマー単位より構成されるコポリアミドが
あげられる。 このような芳香族ポリアミドは、その溶液を紡
糸口金から押出して水性凝固浴中で凝固させて糸
条となし、該糸条(未延伸糸)を最高延伸温度
400℃以上、好ましくは420〜550℃の高温で、全
延伸倍率が6倍以上となるように1段又は2段以
上で延伸することによつて、高強力高モジユラス
の繊維となる。 前記芳香族ポリアミドを溶解して紡糸原液を調
製するための溶媒としては、アミド系溶媒が好ま
しく、例えば、N―メチル―2―ピロリドン
(NMP)、N,N′―ジメチルアセトアミド
(DMA)、N,N′―ジメチルホルムアミド
(DMF)、テトラメチル尿素(TMU)が好適で
ある。これらの溶媒中には、周期律表第族又は
第族の金属のハロゲン化物を含有せしめてもよ
い。このようなハロゲン化物としては、例えば、
塩化リチウム、塩化カルシウム等が特に好適であ
る。 一方、紡糸口金から押出された糸条を凝固させ
る水性凝固浴としては、紡糸原液となる芳香族ポ
リアミド溶液中のアミド系溶媒と同種の溶媒を含
む水性凝固浴が好ましく、凝固浴中の溶媒濃度は
芳香族ポリアミドの種類や紡糸条件等によつても
異るが、一般に約5〜50重量%の範囲内が好まし
い。なお、この凝固浴中には前記のハロゲン化物
を含有せしめてもよい。 紡糸に際しては、紡糸口金を凝固浴中に設けて
紡糸原液を直接凝固浴中に押出してもよいが、紡
糸口金を凝固浴上面の数mm〜数cm上方に設けて紡
糸原液を一たん空気中に押出した後、凝固浴中に
導入するのが好ましい。 凝固浴から引上げられた湿潤状態の糸条は、水
洗により溶媒が除去される。この水洗は定長状態
で行われるが、又は湿潤状態で1.05〜2.0倍に予
備延伸するのと併行して行われる。水洗の過程で
このような若干の予備延伸を行うのは、水洗効率
を上げるばかりでなく、個々の単繊維の真円性を
向上させるのに有効である。 水洗された糸条は、通常、定長状態又は若干の
緊張もしくは若干の弛緩状態で乾燥される。乾燥
時の緊張率又は弛緩率は高々10%である。 前述の如く乾燥された芳香族ポリアミドの糸条
は、必要に応じてさらに400℃未満の温度で1.5〜
3倍に予備延伸した後、400℃以上(好ましくは
420〜550℃)の高温下での延伸に供せられるが、
該糸条はこの高温延伸において高い温度のために
軟化し、単繊維が互いに融着して工程調子が悪化
し、さらに得られた延伸糸の品質も低下するとい
う問題がある。 このような問題を解決するために、湿潤状態の
糸条或いは乾燥後の糸条に、予め不活性な無機微
粉末を延伸助剤として付着せしめ、続いて400℃
以上の温度で延伸することにより、前記の融着現
象を抑制する方法が開発された。 前記無機微粉末としては、平均粒径が20ミクロ
ン以下、特に10ミクロン以下の、硅酸アルミニウ
ム、硅酸マグネシウム、グラフアイト、タルク、
シリカ、マイカ等の微粉末が好適であり、これら
の微粉末は単一成分で使用してもよく、2種以上
併用してもよい。これらの微粉末は水性分散浴中
で水和してコロイド状になるものや、単に分散す
るだけのものもあるが、いずれも使用可能であ
る。 前記の微粉末を糸条に均一に付着せしめるに
は、予め微粉末を水等の分散媒に分散させた浴を
用意し、湿潤状態にある水洗された糸条を分散浴
に浸漬させた後乾燥を行う方法を採用するのが好
ましい。なお、微粉末の分散を均一に行うため有
機又は無機の分散を浴中に添加したり、或いは、
糸条の収束性を安定化させるため帯電防止剤を併
用することもできる。 無機微粉末の糸条への付着量は、繊維重量を基
準にして0.1〜3重量%が好適である。付着量が
少な過ぎると効果が減少し、多過ぎると繊維が微
粉末で汚れ後加工工程でのトラブルの原因となり
易い。 このように無機微粉末を芳香族ポリアミド糸条
に付着させて400℃以上の温度で高温延伸を行う
と融着現象がかなり防止され工程調子も良好化す
るものの、未だ十分満足できる水準に達しない。
特に、延伸断糸や単糸切れに基く毛羽発生等を極
力防止するためには、更に飛躍的な改善が必要で
ある。 本発明の方法では、かかる高温延伸において、
延伸される糸条を偏平状に拡げ、かつ、延伸直前
の糸条の幅に対する延伸直後の糸条の幅の比が
1.1〜10、好ましくは1.3〜5になるように開繊し
て延伸するという特殊な拡幅開繊状態での高温フ
ロー延伸を採用することにより、融着がほゞ完全
に防止され、かつ工程調子も大幅に改善される。 従来より一般に知られているポリエステルやナ
イロンの糸条の代表的な延伸方法においては、延
伸調子を向上させるには出来るだけ糸条を収束さ
せる手段が採用されている。これは単繊維が糸条
から遊離すると単繊維切れが発生し易くなるので
糸条は可能な限り密に収束している方が好ましい
からである。そして、糸条の収束性を向上させる
ために、糸条に油剤を付与したり空気の攪乱によ
る交絡(インターレース)を付与した後に該糸条
を延伸するのが常識とされている。また、ステー
プルフアイバー製造用トウのように単繊維数が著
しく多い場合は、均一加熱を目的として糸条即ち
トウを拡げて延伸する方法が採用されているが、
延伸直前のトウ幅に比べて延伸直後のトウ幅は変
化しないか若干狭くなる。これは糸条が延伸され
ると単繊維の直径が小さくなるから糸条が収束力
(単繊維間の油剤による密着力や単繊維間のわず
かの絡みによる拘束力等)をもつ限り延伸後の糸
条幅は小さくなるのが通常である。 これに対し、本発明方法では、延伸される糸条
を偏平状に拡げ、かつ延伸の過程において更に糸
条の幅を増大させるという従来全く考えられなか
つた特殊な延伸方式により良好な延伸が実現され
る。しかも、延伸に供給される前の糸条は実質的
に単繊維間の交絡のないものである。本発明方法
におけるこのような延伸過程での漸進的な開繊に
より単繊維間の圧着状態が軽減され、かつ糸条の
厚みが減少するので糸条の加熱が均一に行われる
ようになり、その結果として融着防止及び工程調
子の著しい改善が達成される。従来の常識ではこ
のような拡幅開繊状態で延伸することは延伸調子
を悪化させる原因とされており、本発明方法の如
き単繊維間の融着防止、工程調子の改善等の効果
が生ずることは全く予測できない所である。 本発明方法において延伸される糸条は、100本
以上の単繊維からなる糸条が好適である。該糸条
を扁平状に拡げる度合は大きい方が良いが、実際
上は、1000本の単繊維からなる糸条の場合は、厚
さ方向に2〜5本の単繊維が積重つており糸条の
幅方向に200〜500本の単繊維が並んでいるような
扁平状にするのが好適である。均一加熱の目的だ
けを考えると、1000本の単繊維がすべて横一列に
並んでいる極限的な形状が有効と考えられるが、
現実には実施が困難であり糸条自体の収束性も不
安定になり易い。 本発明方法において、糸条を扁平状に拡げるに
は、紡糸された糸条をローラーで平行的に搬送し
つつ水洗,乾燥を行うだけでも十分な扁平状の糸
条となるが、必要に応じて、ニツプローラーで糸
条を押圧したり、移動しつつある糸条を曲率を有
する板や棒に押圧して扁平の度合を増加させても
よい。 また、扁平状に拡げた糸条を開繊するには、糸
条の有する静電気による単繊維間の反撥力を利用
する。この静電気による反撥力は小さいものであ
るから、従来のポリエステルやナイロン等のよう
に高張力で延伸する場合は、本発明方法の如き漸
進的な開繊は生じない。 本発明方法では、この漸進的な開繊を適切な程
度に制御して、延伸直前の糸条の幅に対する延伸
直後の糸条の幅の比を1.1〜10(好ましくは1.3〜
5.0)にする必要がある。 ここで、延伸直前直後の糸条の幅は、400℃以
上の温度で延伸する工程において、それぞれ熱板
或いは気体浴等の加熱手段に入る直前の糸条の幅
及び同加熱手段を出た直後の糸条の幅を言う。 延伸の直前と直後における糸条の幅の比が1.1
未満では、延伸過程での開繊が不十分で単繊維間
の融着が生じ易く、工程調子も悪化する。一方、
前記の比が10を超えると糸条の開繊が大き過ぎ
て、単繊維が糸条の束から遊離して単繊維切れが
生じ易く、巻取後の糸条パツケージの端面の毛羽
が増加して製品の品位が悪化する。 このような漸進的な開繊の程度を前記範囲に調
整するには、次のような開繊を助長する手段と開
繊を抑制する手段とを適宜組合せることにより実
現することができる。 まず、漸進的な開繊を助長する手段としては、 1 タルク微粉末,シリカ微粉末,マイカ微粉末
の少くとも1種からなる延伸助剤を糸条に付与
する。 2 乾燥後に糸条の揉みほぐしを行う。 3 延伸張力を下げるような条件に設定する。 等の手段が挙げられる。 一方、漸進的な開繊を抑制する手段としては、 1 硅酸アルミニウム微粉末からなる延伸助剤を
糸条に付与する。 2 静電気を除去する。 等の手段が挙げられる。 本発明方法を実施する場合は、これらの手段の
幾つかを巧みに組合せることにより、延伸直前と
直後の糸条幅の比を1.1〜10の範囲内の適当な値
に保つことができる。 本発明方法において、糸条を400℃以上の温度
で延伸するには、熱板による接触延伸或いは空
気、水蒸気、炭酸ガス、窒素ガス等の不活性ガス
等の雰囲気中で行う非接触延伸のいずれも採用で
きる。 延伸温度は、延伸のうち少くとも1段を400℃
以上(好ましくは420〜550℃)とする必要があ
る。これは、前述の芳香族ポリアミドは、高分子
の分子鎖が剛直なため、最高延伸温度が400℃未
満では、十分な強力が発現しないからである。 本発明方法では、全部の延伸を400℃以上の温
度で行う必要はなく、湿潤状態で1.05〜2倍に予
備延伸したり、更に、400℃未満の温度で1.5〜
3.5倍に追加の予備延伸することも可能であるが、
最終的には、400℃以上の温度で拡幅開繊状態に
て延伸を行う必要がある。 なお、前述の如く400℃以上の温度で延伸する
に当り、熱板を用いて接触式で行う場合、熱板の
一部(例えば両端)が400℃未満となるような温
度分布を有してもよく、また、不活性ガス中で非
接触式で行う場合、雰囲気の一部(例えば入口と
出口近辺)が400℃未満となるような温度分布を
有してもさしつかえない。要は、実質的な延伸を
400℃以上で行えばよい。 延伸倍率は、全延伸倍率にして6倍以上、好ま
しくは8〜12倍となるように設定する。予備延伸
を行う場合は、全延伸倍率が6倍以上となれば
400℃以上の温度で延伸する段階での倍率は6倍
未満でもさしつかえない。 このような本発明方法に従つて延伸された糸条
は、必要に応じ仕上剤処理,脱延伸助剤処理等を
行つた後、ボビンに巻取られる。 発明の作用及び効果 前述の如き本発明方法によれば、芳香族ポリア
ミド繊維を糸条温度400℃以上となるような著し
く軟化した状態で高倍率に延伸して優れた物性を
発現させる際に、延伸に必要な熱が均一に単繊維
にゆきわたると共に、高温での延伸過程における
単繊維間の融着がほゞ完全に防止され、しかも優
れた工程調子で延伸を行うことが可能となる。 そして、得られた芳香族ポリアミド繊維は、強
度及びモジユラスが大きく、柔軟性にすぐれ、か
つ毛羽等も少いため、ゴムや樹脂の補強材をはじ
め種々の用途に広く使用することができる。 特に、好適な条件で製造された繊維は、25g/
deを超える高い強度と560g/de以上の高いモジ
ユラスを示し、従来の芳香族ポリアミド繊維に比
べて格段にすぐれた物性を有する。 実施例 以下、本発明の方法を実施例によつて更に詳し
く説明する。なお、以下の例において用いる主な
特性値は次の如く測定される値である。 (1) ポリマーの固有粘度() オストワルド型粘度管を用い、溶媒のみの流
下時間をto(秒)、ポリマーの希薄溶液の流下時
間をt(秒)、該希薄溶液中のポリマー濃度をc
(g/dl)とすると、 =ln(t/to)/c で表わされる。特に断らない限り、溶媒は97.5
%硫酸,c=0.5g/dlとし、30℃で測定する。 (2) 融着度 延伸された糸条のフイランド総数(N)のう
ち、融着がなく、分離可能なフイラメント(即
ち完全に単繊維として取り出すことのできるフ
イラメント)数(n)を数え、次式で融着度を
表わす。 融着度=N―n/2N×100(%) この測定を5回行つてその平均値をとる。 実施例 1 下記モノマー単位 により構成される..=3.1の芳香族コポリア
ミドを塩化カルシウム(CaCl2)を含有する
NMPに6重量%のポリマー濃度となるよう溶解
せしめた溶液を、孔径0.3mm、孔数250の紡糸口金
から83g/分の吐出速度で押出し、空気中を約10
mm走行させた後、50℃のNMP/水(30/70重量
%)の凝固浴中で凝固させ、11m/分の速度で引
き上げた。続いて、得られた凝固糸を50℃の水浴
中で洗浄しつつ、階段的に1.3倍に予備延伸し、
絞りローラに通して表面付着水を除去し、表1に
示すような組成からなる延伸助剤の浴に約5秒間
ネルソンローラに懸けて浸漬し、次いで絞りロー
ラに通し、延伸助剤分散液の付着した水洗糸を得
た。引続いて該水洗糸を表面温度が120℃の直径
20cmの乾燥ローラと直径3cmのセパレートローラ
の組と250℃の直径15cmの乾燥ローラと直径1.5cm
のセパレートローラの組にそれぞれ10ターンと5
ターン巻きつけて、ほぼ絶乾した糸となし、これ
を表面温度が500℃、長さ1mの熱板に接触させつ
つ、全延伸倍率が11.0倍となるように延伸して巻
取つた。 各条件で1時間ずつ製糸テストを行ない、その
結果を表1に示す。 実験No.1では延伸助剤を付与しないため、延伸
の直前に対する直後の糸条幅の比(直後/直前)
が1.1未満となり、単繊維間の融着が激しく、工
程調子も悪く、毛羽やループの発生も多かつた。
実験No.2〜4ではフイラメント間のタルクによる
滑りとセパレートローラ上でのほぐし作用によ
り、糸間膠着が解除され、前記糸条幅の比が1.1
よりも大きくなり、単繊維間融着が激減する。し
かし、実験No.2では糸条幅の比が10倍を超えてあ
まりに大きく、工程は不安定となり、断糸の発
生、毛羽、ループの増大を生じた。
Indicates at least one aromatic residue selected from [Formula]. Note that Ar 1 and Ar 2 may be the same or different. Further, all or part of the hydrogen atoms in these aromatic residues may be substituted with a halogen atom or a lower alkyl group. ] Any aromatic polyamide with a substantially uneven orientation composed of the following may be used, but in particular, 80 mol% or more of the total of Ar 1 and Ar 2 is the following aromatic residue (A)
and (B) or (B'), and the proportion of (B) or (B') is 10 to 40%. [The hydrogen atoms of these aromatic residues may be substituted with a halogen atom and/or a lower alkyl group. ] Details of the method for producing such an aromatic copolyamide are described in British Patent No. 1,501,948, US Pat. Examples of suitable aromatic polyamides include the following three:
Mention may be made of copolyamides composed of various monomer units. Such aromatic polyamides are made into yarn by extruding the solution from a spinneret and coagulating in an aqueous coagulation bath, and the yarn (undrawn yarn) is heated to a maximum drawing temperature.
High strength and high modulus fibers are obtained by stretching in one or more stages at a high temperature of 400° C. or higher, preferably 420 to 550° C., so that the total stretching ratio is 6 times or higher. The solvent for preparing the spinning dope by dissolving the aromatic polyamide is preferably an amide solvent, such as N-methyl-2-pyrrolidone (NMP), N,N'-dimethylacetamide (DMA), N , N'-dimethylformamide (DMF), and tetramethylurea (TMU) are preferred. These solvents may contain halides of metals belonging to Group 1 or Group 3 of the periodic table. Examples of such halides include,
Particularly suitable are lithium chloride, calcium chloride, and the like. On the other hand, as the aqueous coagulation bath for coagulating the yarn extruded from the spinneret, it is preferable to use an aqueous coagulation bath containing the same kind of solvent as the amide solvent in the aromatic polyamide solution serving as the spinning stock solution, and the solvent concentration in the coagulation bath is Although it varies depending on the type of aromatic polyamide, spinning conditions, etc., it is generally preferably within the range of about 5 to 50% by weight. Incidentally, the above-mentioned halide may be contained in this coagulation bath. During spinning, a spinneret may be placed in a coagulation bath to extrude the spinning dope directly into the coagulation bath, but the spinneret may be placed several mm to several centimeters above the top surface of the coagulation bath and the spinning dope may be extruded once into the air. After extrusion, it is preferably introduced into a coagulation bath. The wet yarn pulled up from the coagulation bath is washed with water to remove the solvent. This water washing is carried out in a constant length state, or in parallel with pre-stretching to 1.05 to 2.0 times in a wet state. Performing such a slight preliminary stretching during the water washing process is effective not only for increasing the water washing efficiency but also for improving the roundness of each single fiber. The washed yarn is usually dried in a constant length state or in a slightly tensioned or slightly relaxed state. The tension or relaxation rate during drying is at most 10%. The aromatic polyamide yarn dried as described above may be further heated at a temperature of less than 400°C for 1.5~
After pre-stretching to 3 times, the temperature is 400°C or higher (preferably
It is subjected to stretching at high temperatures (420-550℃),
In this high-temperature drawing, the yarn is softened due to the high temperature, and the single fibers are fused to each other, resulting in poor process quality and furthermore, the quality of the obtained drawn yarn is also reduced. In order to solve this problem, inert inorganic fine powder is applied as a drawing aid to the wet yarn or dry yarn, and then the yarn is stretched at 400°C.
A method has been developed for suppressing the above-mentioned fusion phenomenon by stretching at a temperature above. Examples of the inorganic fine powder include aluminum silicate, magnesium silicate, graphite, talc, and the like, each having an average particle size of 20 microns or less, particularly 10 microns or less.
Fine powders of silica, mica, etc. are suitable, and these fine powders may be used as a single component, or two or more types may be used in combination. Some of these fine powders become colloidal when hydrated in an aqueous dispersion bath, while others are simply dispersed, and any of these can be used. In order to uniformly adhere the fine powder to the yarn, a bath in which the fine powder is dispersed in a dispersion medium such as water is prepared in advance, and the wet, washed yarn is immersed in the dispersion bath. It is preferable to adopt a method that involves drying. In addition, in order to uniformly disperse the fine powder, an organic or inorganic dispersion may be added to the bath, or
An antistatic agent can also be used in combination to stabilize the convergence of the yarn. The amount of the inorganic fine powder attached to the yarn is preferably 0.1 to 3% by weight based on the weight of the fiber. If the amount of adhesion is too small, the effect will be reduced, and if it is too large, the fibers will become fine powder and will likely cause trouble in the post-processing process. In this way, when inorganic fine powder is attached to aromatic polyamide yarn and high-temperature stretching is performed at a temperature of 400°C or higher, the fusion phenomenon is considerably prevented and the process condition is improved, but it still does not reach a fully satisfactory level. .
In particular, further dramatic improvements are required in order to prevent as much as possible the occurrence of fluff due to stretch yarn breakage or single yarn breakage. In the method of the present invention, in such high temperature stretching,
The yarn to be drawn is expanded into a flat shape, and the ratio of the width of the yarn immediately after stretching to the width of the yarn immediately before stretching is
By employing high-temperature flow stretching in a special widening state in which the fibers are opened and drawn to a width of 1.1 to 10, preferably 1.3 to 5, fusion is almost completely prevented and the process condition is controlled. is also significantly improved. In typical methods of drawing polyester and nylon threads that have been generally known, means are employed to converge the threads as much as possible in order to improve the drawing condition. This is because if single fibers are separated from the yarn, single fiber breakage is likely to occur, so it is preferable that the yarns are converged as closely as possible. In order to improve the convergence of the yarn, it is common knowledge that the yarn is drawn after being coated with an oil agent or interlaced by air turbulence. In addition, when the number of single fibers is extremely large, such as tow for producing staple fibers, a method is adopted in which the yarn, or tow, is expanded and drawn for the purpose of uniform heating.
The tow width immediately after stretching does not change or becomes slightly narrower than the tow width immediately before stretching. This is because the diameter of the single fibers becomes smaller when the yarn is drawn, so as long as the yarn has convergence force (adhesion force due to oil between single fibers, restraining force due to slight entanglement between single fibers, etc.), the diameter of the single fibers becomes smaller. The yarn width is usually small. On the other hand, the method of the present invention achieves good drawing using a special drawing method that was completely unthinkable in the past, in which the thread to be drawn is spread out into a flat shape and the width of the thread is further increased during the drawing process. be done. Moreover, the yarn before being supplied for drawing is substantially free from entanglement between single fibers. In the method of the present invention, the gradual opening during the drawing process reduces the pressure bond between single fibers and reduces the thickness of the yarn, so that the heating of the yarn is uniformly performed. As a result, significant improvements in prevention of fusion and process conditions are achieved. According to conventional wisdom, drawing in such a wide spread state causes deterioration of the drawing condition, but the method of the present invention has the effect of preventing fusion between single fibers and improving the process condition. is completely unpredictable. The yarn to be drawn in the method of the present invention is preferably a yarn consisting of 100 or more single fibers. The degree to which the yarn is expanded into a flat shape is better, but in reality, in the case of a yarn consisting of 1000 single fibers, 2 to 5 single fibers are stacked in the thickness direction. It is preferable to form the strip into a flat shape in which 200 to 500 single fibers are lined up in the width direction. Considering only the purpose of uniform heating, an extreme shape in which all 1000 single fibers are lined up horizontally in a row is considered to be effective.
In reality, it is difficult to implement, and the convergence of the yarn itself tends to become unstable. In the method of the present invention, in order to spread the yarn into a flat shape, simply washing and drying the spun yarn while conveying it in parallel with rollers is enough to make the yarn into a flat shape. Then, the degree of flatness may be increased by pressing the yarn with a nip roller or by pressing the moving yarn against a plate or rod having a curvature. Furthermore, in order to open the filament spread into a flat shape, the repulsive force between single fibers due to the static electricity possessed by the filament is utilized. Since this repulsive force due to static electricity is small, when conventional polyester, nylon, etc. are stretched with high tension, gradual opening as in the method of the present invention does not occur. In the method of the present invention, this gradual opening is controlled to an appropriate degree, and the ratio of the width of the yarn immediately after drawing to the width of the yarn immediately before drawing is 1.1 to 10 (preferably 1.3 to 10).
5.0). Here, the width of the yarn immediately before and after drawing refers to the width of the yarn immediately before entering a heating means such as a hot plate or gas bath, and the width immediately after leaving the heating means, respectively, in the drawing process at a temperature of 400°C or higher. refers to the width of the yarn. The ratio of the yarn widths immediately before and after drawing is 1.1.
If it is less than that, the opening during the drawing process will be insufficient and fusion between single fibers will easily occur, resulting in poor process performance. on the other hand,
If the above ratio exceeds 10, the opening of the yarn is too large, and single fibers are likely to separate from the yarn bundle, resulting in single fiber breakage, and the fuzz on the end face of the yarn package after winding increases. The quality of the product deteriorates. Adjustment of the degree of such gradual fiber opening within the above range can be achieved by appropriately combining the following means for promoting fiber opening and means for suppressing fiber opening. First, as means for promoting gradual opening, 1. A drawing aid consisting of at least one of fine talc powder, fine silica powder, and fine mica powder is applied to the yarn. 2 After drying, massage the threads to loosen them. 3. Set the conditions to lower the stretching tension. Examples of such methods include: On the other hand, as a means for suppressing gradual opening, 1. A drawing aid made of fine aluminum silicate powder is applied to the yarn. 2 Remove static electricity. Examples of such methods include: When carrying out the method of the present invention, by skillfully combining some of these means, the ratio of the yarn widths immediately before and after drawing can be maintained at an appropriate value within the range of 1.1 to 10. In the method of the present invention, to draw the yarn at a temperature of 400°C or higher, either contact drawing using a hot plate or non-contact drawing carried out in an atmosphere of air, water vapor, inert gas such as carbon dioxide gas, nitrogen gas, etc. can also be adopted. The stretching temperature is 400℃ for at least one stage of stretching.
or higher (preferably 420 to 550°C). This is because the above-mentioned aromatic polyamide has a rigid polymer chain, and therefore does not exhibit sufficient strength if the maximum stretching temperature is less than 400°C. In the method of the present invention, it is not necessary to carry out all the stretching at a temperature of 400°C or higher, but pre-stretching may be carried out by 1.05 to 2 times in a wet state, and further stretching may be carried out at a temperature of 1.5 to 2 times at a temperature below 400°C.
Additional pre-stretching to 3.5 times is also possible;
Ultimately, it is necessary to draw the fibers in an expanded state at a temperature of 400°C or higher. In addition, as mentioned above, when stretching at a temperature of 400°C or higher, if a contact method is used using a hot plate, the temperature distribution may be such that a part of the hot plate (for example, both ends) is less than 400°C. In addition, when conducting in a non-contact manner in an inert gas, it is acceptable to have a temperature distribution such that a part of the atmosphere (for example, near the inlet and outlet) is less than 400°C. In short, substantial stretching
It can be carried out at a temperature of 400℃ or higher. The stretching ratio is set so that the total stretching ratio is 6 times or more, preferably 8 to 12 times. When performing preliminary stretching, if the total stretching ratio is 6 times or more
The magnification at the stage of stretching at a temperature of 400° C. or higher may be less than 6 times. The yarn drawn according to the method of the present invention is treated with a finishing agent, a de-drawing aid, etc., if necessary, and then wound onto a bobbin. Functions and Effects of the Invention According to the method of the present invention as described above, when aromatic polyamide fibers are stretched at a high magnification in a significantly softened state with a yarn temperature of 400°C or higher to exhibit excellent physical properties, The heat necessary for drawing is uniformly distributed over the single fibers, and fusion between the single fibers during the drawing process at high temperatures is almost completely prevented, and drawing can be carried out under excellent process conditions. The obtained aromatic polyamide fiber has high strength and modulus, excellent flexibility, and has little fuzz, so it can be widely used in various applications including reinforcing materials for rubber and resin. In particular, the fibers produced under suitable conditions are 25g/
It exhibits high strength exceeding de and high modulus of over 560 g/de, and has significantly superior physical properties compared to conventional aromatic polyamide fibers. Examples Hereinafter, the method of the present invention will be explained in more detail with reference to Examples. Note that the main characteristic values used in the following examples are values measured as follows. (1) Intrinsic viscosity of the polymer () Using an Ostwald viscosity tube, the flow time of the solvent alone is to (seconds), the flow time of the dilute polymer solution is t (seconds), and the polymer concentration in the dilute solution is c
(g/dl), it is expressed as =ln(t/to)/c. Unless otherwise specified, solvents are 97.5
% sulfuric acid, c = 0.5 g/dl, and measured at 30°C. (2) Fusing degree Count the number (n) of filaments that are not fused and can be separated (i.e., filaments that can be completely taken out as single fibers) out of the total number of filaments (N) of the drawn yarn, and then The degree of fusion is expressed by the formula. Degree of fusion=N-n/2N×100 (%) Perform this measurement five times and take the average value. Example 1 The following monomer units It is composed of .. = 3.1 aromatic copolyamide containing calcium chloride (CaCl 2 )
A solution prepared by dissolving the polymer in NMP to a polymer concentration of 6% by weight was extruded through a spinneret with a pore diameter of 0.3 mm and a number of holes of 250 at a discharge rate of 83 g/min.
After traveling mm, it was coagulated in a coagulation bath of NMP/water (30/70 wt%) at 50°C and pulled up at a speed of 11 m/min. Subsequently, the obtained coagulated thread was pre-stretched stepwise to 1.3 times while being washed in a water bath at 50°C.
It is passed through a squeeze roller to remove water adhering to the surface, immersed in a drawing aid bath having the composition shown in Table 1 for about 5 seconds by passing it through a Nelson roller, and then passed through a squeeze roller to remove the drawing aid dispersion. A washed thread with attached water was obtained. Subsequently, the washed thread was heated to a diameter of 120℃ at a surface temperature of 120℃.
A set of a 20cm drying roller and a 3cm diameter separate roller, a 15cm diameter drying roller at 250℃, and a 1.5cm diameter drying roller.
10 turns and 5 turns on each set of separate rollers.
The yarn was wound in turns to form an almost completely dry yarn, which was stretched and wound at a total stretching ratio of 11.0 times while contacting a hot plate with a surface temperature of 500°C and a length of 1 m. A yarn spinning test was conducted for 1 hour under each condition, and the results are shown in Table 1. In Experiment No. 1, no drawing aid was applied, so the ratio of yarn width immediately after drawing to that immediately after drawing (immediately/immediately before)
was less than 1.1, the fusion between single fibers was severe, the process was poor, and fuzz and loops were often generated.
In Experiments Nos. 2 to 4, the stiction between the yarns was released due to the sliding of the talc between the filaments and the loosening action on the separation roller, and the yarn width ratio was 1.1.
, and the fusion between single fibers is drastically reduced. However, in Experiment No. 2, the yarn width ratio was too large, exceeding 10 times, and the process became unstable, resulting in yarn breakage, fluff, and increased loops.

【表】【table】

【表】 実施例 2 実施例1と同じ芳香族ポリアミド溶液を、孔径
0.25mm、孔数1000の紡糸口金から1111g/分の吐
出速度で押し出し空気中を7mm走行させた後、温
度50℃、濃度30重量%のNMP水溶液の凝固浴中
で凝固させ、38.5m/分の速度で引き上げた。続
いて得られた凝固糸を50℃の水浴中で洗浄しつつ
階段的に1.3倍に延伸し、絞りローラーに通して
表面付着水を除去し、表2に示すような組成から
なる濃度2重量%の延伸助剤の水系分散浴に約1
秒間浸漬し、絞りローラーに通し延伸助剤の付着
した水洗糸を得た。 表2 延伸助剤の組成 タルク 85部 硅酸アルミニウム 15部 ポリエチレングリコール 7部 ヘキサメタリン酸ソーダ 3部 次いで、この水洗糸を120℃の乾燥ローラーに
30回巻きつけて乾燥した後、三角歯を有する一対
のギヤーロールの間で乾燥した糸条のもみほぐし
を行つた。なお、各ギヤーロールは直径84mmで円
周上に40個の三角歯を有しており、三角歯の先端
は曲率半径1mmの丸みになるように仕上げてあ
る。ギヤーロールはお互にある深さに噛み合つて
いるが、この噛合の深さによつて揉みほぐしの程
度を変化させる。噛み合いの深さは0mm(噛合な
し)から1.5mmまで変化させた。噛合が深くなる
と糸条の揉みほぐしが強くなつて、後述するよう
に400℃以上での延伸に於いて開繊し易くなる。 揉みほぐし後、乾燥された糸条を温度360℃、
長さ2mの熱板上で2倍に延伸し、最後に温度500
℃、長さ3mの熱板上で4倍に延伸した。(したが
つて、全延伸倍率は10.4倍である。) かくして延伸された糸条に仕上オイルを付与し
て400m/minで巻き取つた。得られた糸条の繊
度は1550デニールであつた。 この延伸に於いて、500℃の熱板に入る延伸直
前の糸条の幅と熱板を出た延伸直後の糸条の幅を
測定し、糸質、品位、工程調子と併せてその結果
を表3に示す。
[Table] Example 2 The same aromatic polyamide solution as in Example 1 was
It was extruded from a spinneret with a size of 0.25 mm and 1000 holes at a discharge rate of 1111 g/min, traveled 7 mm in air, and then coagulated in a coagulation bath of an aqueous NMP solution at a temperature of 50°C and a concentration of 30% by weight at 38.5 m/min. pulled up at a speed of Subsequently, the obtained coagulated thread was washed in a water bath at 50°C and stretched stepwise to 1.3 times, passed through a squeezing roller to remove water adhering to the surface, and a concentration of 2 weight containing the composition shown in Table 2 was obtained. % of a drawing aid in an aqueous dispersion bath of about 1%
The yarn was immersed for a second and passed through a squeezing roller to obtain a water-washed yarn to which the drawing aid was attached. Table 2 Composition of drawing aid Talc 85 parts Aluminum silicate 15 parts Polyethylene glycol 7 parts Sodium hexametaphosphate 3 parts Next, this water-washed yarn was placed on a drying roller at 120°C.
After winding the yarn 30 times and drying it, the dried yarn was loosened between a pair of gear rolls with triangular teeth. Each gear roll has a diameter of 84 mm and has 40 triangular teeth on its circumference, and the tips of the triangular teeth are rounded with a radius of curvature of 1 mm. The gear rolls are engaged with each other to a certain depth, and the degree of kneading changes depending on the depth of this engagement. The depth of engagement was varied from 0 mm (no engagement) to 1.5 mm. The deeper the interlocking, the stronger the loosening of the threads, which makes it easier to open the fibers during drawing at 400°C or higher, as described below. After kneading and loosening, the dried yarn is heated at a temperature of 360℃.
Stretch it twice on a 2m long hot plate and finally heat it to 500℃.
℃ and stretched 4 times on a 3 m long hot plate. (Thus, the total drawing ratio is 10.4 times.) Finishing oil was applied to the thus drawn yarn and it was wound at 400 m/min. The fineness of the obtained yarn was 1550 denier. During this drawing, we measured the width of the yarn just before it entered the hot plate at 500°C and the width of the yarn just after it left the hot plate, and reported the results along with the yarn quality, quality, and process condition. It is shown in Table 3.

【表】 表3から明らかなようにギヤーロールの噛合の
深さが0.3mm以下では開繊が不十分で、融着防止
が改善されておらず、強度は低目で、断糸率も高
くなつている(実験No.5,6)。実験No.7,8,
9ではギヤーロールの噛合の深さが0.6〜1.0mm迄
変化しているが、高温延伸下での糸条の開繊が本
発明で特定した範囲にあり、融着は殆んどなく、
強度も高く、断糸率も著しく低くなつている。
又、毛羽の数も少い。 しかし、ギヤーロールの噛合が1.5mm迄深くな
ると開繊が大き過ぎて、かえつて単繊維が断糸し
易く、そのために断糸率が若干高くなると共に巻
き取られた繊維の毛羽が増加して好ましくない
(実験10)。 実施例 3 下記モノマー単位 により構成される=4.0の芳香族ポリアミドを
塩化カルシウム(CaCl2)を含有するNMP中に
6重量%溶解せしめた溶液を、孔径0.3mm、孔数
250の紡糸口金から93g/分の吐出速度で押出し
た。空気中を約10mm走行させた後、50℃の
NMP/水(30/70重量%)の凝固浴中で凝固さ
せ15m/分の速度で引き上げ、引き続き50℃の水
浴で洗浄し、表2に示される不活性な無機微粉末
を水に分散させた分散浴に1秒浸漬して引き上
げ、ゴムローラーと金属ローラーとの間で絞りを
かけて後、乾燥した。 次いで、直径30mm、長さ1mのスリツト状中空
パイプにて12倍に延伸した。但し、この場合スチ
ームの雰囲気温度は460℃であり、糸条の温度は
約430℃であつた。 この延伸に於いて、延伸された糸条が中空パイ
プを出た後、約30cm走行した時点で回転ローラー
に摺接せしめて帯電防止剤を付与した。この回転
ローラーは通常オイルを付与するのに使用さるオ
イリングローラーと同じものである。糸条は帯電
防止剤を付与された後、コデツトローラーを介し
て巻き取つた。帯電防止剤はモノソデイウムジオ
クチルスルホサクシネートの2%水溶液を用い
た。回転ローラーの回転数を上げると帯電防止剤
の付着量が増加し、延伸直後の糸条の幅を収束さ
せようとする力が働く。 このような実験を行つた結果を表4に示す。
[Table] As is clear from Table 3, when the meshing depth of gear rolls is less than 0.3 mm, fiber opening is insufficient, fusion prevention is not improved, strength is low, and yarn breakage rate is high. Summer (Experiment No. 5, 6). Experiment No. 7, 8,
In No. 9, the depth of engagement of the gear rolls varied from 0.6 to 1.0 mm, but the opening of the yarn under high-temperature drawing was within the range specified in the present invention, and there was almost no fusion.
It has high strength and a significantly low thread breakage rate.
Also, the number of fuzz is small. However, when the meshing of the gear rolls is as deep as 1.5 mm, the fiber opening becomes too large and the single fibers are more likely to break.As a result, the breakage rate becomes slightly higher and the fuzz of the wound fibers increases. Unfavorable (Experiment 10). Example 3 The following monomer units A solution of 6% by weight of an aromatic polyamide composed of
It was extruded from a 250 spinneret at a rate of 93 g/min. After traveling about 10 mm in the air, the temperature of 50℃
Coagulate in a NMP/water (30/70% by weight) coagulation bath, pull up at a speed of 15 m/min, and then wash in a 50°C water bath to disperse the inert inorganic fine powder shown in Table 2 in water. The sample was immersed in a dispersion bath for 1 second, pulled out, squeezed between a rubber roller and a metal roller, and then dried. Next, it was stretched 12 times using a slit-shaped hollow pipe with a diameter of 30 mm and a length of 1 m. However, in this case, the steam atmosphere temperature was 460°C, and the yarn temperature was about 430°C. In this drawing, after the drawn yarn exited the hollow pipe and traveled approximately 30 cm, it was brought into sliding contact with a rotating roller to be coated with an antistatic agent. This rotating roller is the same as the oiling roller normally used to apply oil. After the yarn was coated with an antistatic agent, it was wound up through a codet roller. As the antistatic agent, a 2% aqueous solution of monosodium dioctyl sulfosuccinate was used. When the rotation speed of the rotating roller is increased, the amount of the antistatic agent attached increases, and a force is exerted to converge the width of the yarn immediately after drawing. Table 4 shows the results of such experiments.

【表】 本実験ではスチームによる非接触延伸を行つた
ために、糸条は著しく開繊し易い。したがつて前
記延伸助剤を付与すると単に延伸するだけで著し
く開繊し、帯電防止剤を使用しない実験No.11では
糸条が開繊しすぎて、ボビン端面の毛羽が多く断
糸率も若干高い。適当に帯電防止剤を付与すると
開繊の状態が適度に調整されて実験No.12,13に示
す如く繊維の品質、品位、工程調子共に満足され
た状態で製糸される。 しかし、過度に帯電防止剤を付与すると実験No.
14の如く、開繊が全く消失し、その結果として融
着が発生する。
[Table] In this experiment, non-contact drawing was performed using steam, so the yarn was extremely easy to open. Therefore, when the above-mentioned drawing aid was applied, the fibers were opened significantly just by drawing, and in Experiment No. 11, in which no antistatic agent was used, the yarns were opened too much, and there was a lot of fuzz on the bobbin end face, and the yarn breakage rate was also low. Slightly expensive. When an appropriate antistatic agent is applied, the opening condition is adjusted appropriately, and as shown in Experiment Nos. 12 and 13, fibers are spun with satisfactory quality, quality, and process conditions. However, if too much antistatic agent is applied, experiment No.
As shown in No. 14, fiber opening completely disappears, and as a result, fusion occurs.

Claims (1)

【特許請求の範囲】 1 ポリマー繰返し単位の80モル%以上が下記繰
返し単位 ―NH―Ar1―NHCO―Ar2―CO― 〔ここで、Ar,Ar2は、【式】 【式】【式】及び 【式】から選ばれた少くと も1種の芳香族残基を示す。これらの芳香族残基
は、その水素原子の一部又は全部がハロゲン原子
又は低級アルキル基で置換されていてもよい。〕 で構成される芳香族ポリアミドの糸条を、最高延
伸温度400℃以上にて、6倍以上の全延伸倍率に、
1段又は2段以上で延伸して高強力高モジユラス
の芳香族ポリアミド繊維を製造する方法におい
て、400℃以上の温度で延伸を行う際に、延伸さ
れる糸条を扁平状に拡げ、かつ延伸直前の糸条の
幅に対する延伸直後の糸条の幅が1.1〜10になる
ように開繊して延伸することを特徴とする芳香族
ポリアミド繊維の製造方法。 2 Ar1,Ar2の合計の80モル%以上が、下記芳
香族残基(A)及び(B) 〔ここで、芳香族残基(A),(B)は、その水素原子
の全部又は一部がハロゲン原子及び/又は低級ア
ルキル基で置換されていてもよい。〕 であり、かつ芳香族残基(B)の比率が10〜40モル%
である特許請求の範囲第1項記載の芳香族ポリア
ミド繊維の製造方法。 3 Ar1,Ar2の合計の80モル%以上が、下記芳
香族基(A)及び(B′) 〔ここで、芳香族残基(A),(B′)は、その水素
原子の全部又は一部がハロゲン原子及び/又は低
級アルキル基で置換されていてもよい。〕 であり、かつ構成単位(B′)の比率が10〜40モ
ル%である特許請求の範囲第1項記載の芳香族ポ
リアミド繊維の製造方法。 4 400℃以上の延伸を熱板上で行う特許請求の
範囲第1項記載の芳香族ポリアミド繊維の製造方
法。 5 400℃以上の延伸を気体浴中で行う特許請求
の範囲第1項記載の芳香族ポリアミド繊維の製造
方法。 6 糸条を水浴中で1.05〜2倍に予備延伸した
後、乾燥し、次いで400℃以上の温度で延伸を行
う特許請求の範囲第1項記載の芳香族ポリアミド
繊維の製造方法。 7 糸条を水浴中で1.05〜2倍に第1次予備延伸
した後、乾燥し、次いで400℃未満の温度で1.5〜
3倍に第2次予備延伸し、しかる後400℃以上の
温度で延伸を行う特許請求の範囲第1項記載の芳
香族ポリアミド繊維の製造方法。 8 糸条が100本以上の単繊維から構成される特
許請求の範囲第1項記載の芳香族ポリアミド繊維
の製造方法。 9 糸条に延伸助剤を付着させた後、400℃以上
の温度で延伸する特許請求の範囲第1項記載の芳
香族ポリアミド繊維の製造方法。 10 糸条に機械的なもみほぐし作用を与えた
後、400℃以上の温度で延伸する特許請求の範囲
第1項記載の芳香族ポリアミド繊維の製造方法。 11 延伸直前の糸条の幅に対する延伸直後の糸
条の幅が1.3〜5となるように開繊する特許請求
の範囲第1項記載の芳香族ポリアミド繊維の製造
方法。
[Scope of Claims] 1 80 mol% or more of the polymer repeating units are the following repeating units -NH-Ar 1 -NHCO-Ar 2 -CO- [Here, Ar and Ar 2 are [Formula] [Formula] [Formula] ] and [Formula] represents at least one aromatic residue selected from the following. Some or all of the hydrogen atoms in these aromatic residues may be substituted with a halogen atom or a lower alkyl group. ] The aromatic polyamide yarn composed of
In a method for producing high-strength, high-modulus aromatic polyamide fibers by drawing in one or two or more steps, when drawing is carried out at a temperature of 400°C or higher, the thread to be drawn is expanded into a flat shape and stretched. A method for producing aromatic polyamide fibers, which comprises opening and drawing the fibers so that the width of the thread immediately after drawing is 1.1 to 10 times the width of the thread immediately before drawing. 2 80 mol% or more of the total of Ar 1 and Ar 2 is the following aromatic residues (A) and (B) [Here, in the aromatic residues (A) and (B), all or part of the hydrogen atoms may be substituted with a halogen atom and/or a lower alkyl group. ] and the ratio of aromatic residue (B) is 10 to 40 mol%
A method for producing an aromatic polyamide fiber according to claim 1. 3 80 mol% or more of the total of Ar 1 and Ar 2 is the following aromatic group (A) and (B') [Here, in the aromatic residues (A) and (B'), all or part of the hydrogen atoms may be substituted with a halogen atom and/or a lower alkyl group. ] The method for producing an aromatic polyamide fiber according to claim 1, wherein the ratio of the structural unit (B') is 10 to 40 mol%. 4. The method for producing aromatic polyamide fibers according to claim 1, wherein the stretching is carried out on a hot plate at 400°C or higher. 5. The method for producing aromatic polyamide fibers according to claim 1, wherein the stretching is carried out at 400°C or higher in a gas bath. 6. The method for producing aromatic polyamide fibers according to claim 1, wherein the yarn is pre-stretched to 1.05 to 2 times in a water bath, dried, and then stretched at a temperature of 400°C or higher. 7 The yarn is first pre-stretched to 1.05 to 2 times in a water bath, dried, and then stretched to 1.5 to 2 times at a temperature below 400°C.
2. The method for producing an aromatic polyamide fiber according to claim 1, which comprises performing a second preliminary stretching to 3 times, and then stretching at a temperature of 400° C. or higher. 8. The method for producing an aromatic polyamide fiber according to claim 1, wherein the yarn is composed of 100 or more single fibers. 9. The method for producing aromatic polyamide fibers according to claim 1, which comprises adhering a drawing aid to the yarn and then drawing it at a temperature of 400°C or higher. 10. The method for producing an aromatic polyamide fiber according to claim 1, wherein the yarn is subjected to a mechanical loosening action and then stretched at a temperature of 400°C or higher. 11. The method for producing aromatic polyamide fibers according to claim 1, wherein the fibers are opened so that the width of the yarn immediately after stretching is 1.3 to 5 with respect to the width of the yarn immediately before stretching.
JP20962884A 1984-10-08 1984-10-08 Production of aromatic polyamide fiber Granted JPS6189317A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP20962884A JPS6189317A (en) 1984-10-08 1984-10-08 Production of aromatic polyamide fiber

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP20962884A JPS6189317A (en) 1984-10-08 1984-10-08 Production of aromatic polyamide fiber

Publications (2)

Publication Number Publication Date
JPS6189317A JPS6189317A (en) 1986-05-07
JPH0123571B2 true JPH0123571B2 (en) 1989-05-08

Family

ID=16575942

Family Applications (1)

Application Number Title Priority Date Filing Date
JP20962884A Granted JPS6189317A (en) 1984-10-08 1984-10-08 Production of aromatic polyamide fiber

Country Status (1)

Country Link
JP (1) JPS6189317A (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004113600A1 (en) * 2003-06-18 2004-12-29 Denki Kagaku Kogyo Kabushiki Kaisha Drawing method and apparatus
CN112105765B (en) * 2018-05-10 2023-03-14 帝人株式会社 Fully aromatic polyamide fiber

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59137535A (en) * 1983-01-24 1984-08-07 帝人株式会社 Stretching of synthetic fiber
JPS6017113A (en) * 1983-07-07 1985-01-29 Teijin Ltd Preparation of aromatic polyamide yarn

Also Published As

Publication number Publication date
JPS6189317A (en) 1986-05-07

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