JPH1112874A - Acrylic fiber yarn, and method and apparatus for steam-drawing of the same, and carbon fiber - Google Patents
Acrylic fiber yarn, and method and apparatus for steam-drawing of the same, and carbon fiberInfo
- Publication number
- JPH1112874A JPH1112874A JP16289697A JP16289697A JPH1112874A JP H1112874 A JPH1112874 A JP H1112874A JP 16289697 A JP16289697 A JP 16289697A JP 16289697 A JP16289697 A JP 16289697A JP H1112874 A JPH1112874 A JP H1112874A
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- JP
- Japan
- Prior art keywords
- yarn
- steam
- acrylic
- stretching
- fluid
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は炭素繊維用前駆体な
どとしても用いられるアクリル系糸条に関し、および４
０００フィラメント以上の太物アクリル系フィラメント
糸条を高倍率で安定に延伸するスチーム延伸方法および
装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an acrylic yarn which is also used as a precursor for carbon fibers and the like.
The present invention relates to a steam drawing method and apparatus for stably drawing a thick acrylic filament yarn of 000 filaments or more at a high magnification.
【０００２】[0002]
【従来の技術】ポリアクリロニトリル系繊維糸条は、炭
素繊維の前駆体（プリカーサ）としても利用されてお
り、性能の優れた炭素繊維を得るために、多くの改善技
術が開示されている。炭素繊維はそのプリカーサである
アクリロニトリル系繊維を紡糸する製糸工程、２００〜
４００℃の空気雰囲気中で該繊維を加熱焼成して酸化繊
維に転換する耐炎化工程、窒素、アルゴン、ヘリウム等
の不活性雰囲気中でさらに３００〜２５００℃に加熱し
て炭化する炭化工程を経ることで得られ、複合材料の強
化繊維として航空宇宙用途やスポーツ用途、一般産業用
途などに幅広く利用されている。2. Description of the Related Art Polyacrylonitrile fiber yarns are also used as precursors of carbon fibers, and many improved techniques have been disclosed in order to obtain carbon fibers having excellent performance. A carbon fiber spinning process for spinning an acrylonitrile-based fiber as a precursor thereof;
Through a flame-proofing step in which the fiber is heated and baked in an air atmosphere at 400 ° C. to convert it into an oxidized fiber, and a carbonization step in which the fiber is further heated to 300 to 2500 ° C. in an inert atmosphere such as nitrogen, argon, helium, and carbonized. It is widely used as a reinforcing fiber of composite materials for aerospace applications, sports applications, general industrial applications, and the like.
【０００３】これらのうち一般産業分野への用途拡大の
要求に応えるためには、第一に製造原価を軽減して、廉
価な炭素繊維を提供することが重要である。従来、炭素
繊維に係わる改善は性能の改善に関するものが多く、製
造原価の低減を目的としたものは少なかった。[0003] Of these, in order to meet the demand for expanding applications in the general industrial field, it is first important to reduce production costs and to provide inexpensive carbon fibers. Hitherto, many improvements relating to carbon fibers have been related to improvement in performance, and few have aimed at reducing manufacturing costs.
【０００４】炭素繊維のプリカーサの製造方法に関し
て、処理する糸条を太く（太糸条化）するとともに、糸
条幅を狭く（高密度化）することによって、限られた設
備の中で生産量を増大させること、すなわち設備生産性
を向上させることがコストダウンを図る上で重要なポイ
ントとなっている。[0004] With regard to the method for producing a precursor of carbon fiber, the yarn to be treated is made thicker (thicker yarn) and the yarn width is made narrower (densified), so that the production amount can be reduced in a limited facility. Increasing, that is, improving equipment productivity is an important point in reducing costs.
【０００５】製糸工程での糸条単位を太糸条化したり、
あるいは高密度化すると、特に延伸工程や水洗工程およ
び工程油剤の付与工程で単糸間接着が発生したり、延伸
での毛羽や断糸、水洗不足、油剤の付着斑が惹起され
て、原糸の製造工程における工程通過性が阻害されるの
みならず、次の焼成工程においても断糸や毛羽が発生し
て工程通過性を阻害すると共に、得られる炭素繊維の物
性をも低下させる原因になるのである。これらの製糸工
程での阻害要因は、糸条への加熱や、浴液の浸透が均一
とならず、処理斑が発生することにあることをつきと
め、これらの要因を排除することによって、工程通過性
を改善することについて鋭意検討した。[0005] The yarn unit in the yarn making process is changed to a thick yarn,
Or, when the density is increased, adhesion between single yarns occurs in the stretching step, the washing step, and the step of applying the process oil agent, and fluff and breakage during stretching, insufficient washing, and uneven adhesion of the oil agent are caused. Not only is the process-passing property of the production process impaired, but also in the next baking step, thread breaks and fluff are generated, which impairs the process-passing property and also reduces the physical properties of the obtained carbon fiber. It is. The factors that hinder the yarn-making process are that the heating of the yarn and the permeation of the bath solution are not uniform, resulting in the occurrence of processing unevenness. We studied diligently to improve the performance.
【０００６】このうちスチーム延伸については、これを
安定に行う手段として、これまでに特開昭５８−２１４
５２０号公報、特開昭６０−１９３６３２号公報、特開
昭６０−２５７２１９号公報、および特開平５−２６３
３１３号公報等が開示されている。[0006] Among them, steam stretching has been disclosed as a means for stably performing the above-described steam stretching.
520, JP-A-60-193632, JP-A-60-257219, and JP-A-5-263.
No. 313 is disclosed.
【０００７】特開昭５８−２１４５２０号公報には、延
伸チューブの両端にラビリンスシールを配し、ラビリン
ス径と延伸張力を適正化して、糸条を一段で延伸しよう
とする技術が開示されている。しかしながら、本発明の
目的である太い糸条の延伸においては、ラビリンス径の
大きさおよび延伸張力を適正化しても、太糸条の束内を
均一加熱することができず、延伸切れが発生するという
問題があった。Japanese Patent Application Laid-Open No. 58-214520 discloses a technique in which labyrinth seals are provided at both ends of a drawing tube to optimize the labyrinth diameter and the drawing tension to draw the yarn in one step. . However, in the drawing of a thick yarn, which is the object of the present invention, even when the labyrinth diameter and the drawing tension are adjusted appropriately, the inside of the bundle of the thick yarn cannot be heated uniformly, and drawing breakage occurs. There was a problem.
【０００８】特開昭６０−１９３６３２号公報および特
開昭６０−２５７２１９号公報には、いずれも加圧延伸
機に関する技術が開示されており、延伸装置の両端に加
圧流体のシール構造を有し、前者においてはスチーム等
の加圧流体の吹き込み口を糸条の導入側に、後者におい
ては糸条の出側に設けて一段延伸を行うものである。特
に後者においては、加圧流体の吹き込み位置を糸条の出
側に配し、糸条と加圧流体の流れを向流とし、熱効率を
高める構造としたものであるが、これをもってしても太
糸条を均一加熱することはできない。Japanese Patent Application Laid-Open Nos. 60-193632 and 60-257219 both disclose techniques relating to a pressure stretching machine, and have a sealing structure for a pressurized fluid at both ends of the stretching apparatus. In the former case, a blowing port for pressurized fluid such as steam is provided on the introduction side of the yarn, and in the latter case, it is provided on the exit side of the yarn to perform one-stage drawing. In particular, in the latter case, the blowing position of the pressurized fluid is arranged on the outlet side of the yarn, and the flow of the yarn and the pressurized fluid is made to flow countercurrently to increase the thermal efficiency. The thick yarn cannot be heated uniformly.
【０００９】さらに、特開平５−２６３３１３号公報に
は、前述の欠点を補うため、加圧スチーム延伸機の中を
ラビリンスシールで２つに区切り、予熱ゾーンを設ける
ことで太糸条のスチーム延伸を安定して行う技術が開示
されている。本技術は太物糸条のスチーム延伸には効果
的な技術であるが、より高速で処理しようとすると、毛
羽が多発する問題点があった。これはスチーム延伸工程
に先立って処理される、給油工程・乾燥緻密化工程にお
いて、糸条の単糸同士が軽い程度で融着する、単糸間接
着が生じることにより、予熱ゾーンでの熱伝達が不十分
になり、延伸能が低下するものと考えられる。Japanese Patent Application Laid-Open No. 5-263313 discloses that in order to compensate for the above-mentioned drawbacks, the inside of a pressurized steam stretching machine is divided into two sections by a labyrinth seal and a preheating zone is provided to steam stretch a thick yarn. Is disclosed in the art. This technique is an effective technique for steam drawing of thick yarn, but there is a problem that fluff is frequently generated when processing at a higher speed. This is the heat transfer in the preheating zone, where the single yarns of the yarns are fused to a light degree in the lubrication and drying densification processes, which are processed prior to the steam drawing process, and the adhesion between the single yarns occurs. Is considered to be insufficient, and the stretching ability is considered to be reduced.
【００１０】このため、太物糸条を効率良く延伸する手
段として、前述に様な単糸間接着が発生していても十分
な延伸性能を有する技術を検討し、本発明に到達した。[0010] For this reason, as a means for efficiently drawing a thick yarn, a technique having a sufficient drawing performance even when the adhesion between single yarns has occurred as described above has been studied, and the present invention has been reached.
【００１１】[0011]
【発明が解決しようとする課題】本発明の課題は、太物
アクリル系糸条に対して、工程通過性に優れたアクリル
系糸条およびアクリル系糸条のスチーム延伸方法および
装置および炭素繊維を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide an acrylic yarn excellent in processability, a method and an apparatus for steam-drawing an acrylic yarn, and a carbon fiber with respect to a thick acrylic yarn. To provide.
【００１２】[0012]
【課題を解決するための手段】本発明のアクリル系糸
条、スチーム延伸方法、スチーム延伸装置、炭素繊維は
上記課題を解決するために次の構成を有する。The acrylic yarn, the steam drawing method, the steam drawing apparatus, and the carbon fiber of the present invention have the following constitutions to solve the above problems.
【００１３】（１）アクリル系フィラメント糸条であっ
て、下記に示す走行糸幅指数Ｋが９５未満であることを
特徴とするアクリル系糸条。(1) An acrylic filament yarn, wherein a running yarn width index K shown below is less than 95.
【００１４】Ｋ＝Ｗmin ×１００／Ｗmax （ここで、Ｋとは、接触角４πのローラ群に糸条を２分
間走行させたときの、該ローラ上の最大糸幅Ｗmax （ｍ
ｍ）、最小糸幅Ｗmin （ｍｍ）に対し、上式で定義され
る走行糸幅指数である。） （２）アクリル系フィラメント糸条が単糸数４０００本
以上からなるものであることを特徴とする前記（１）に
記載のアクリル系糸条。K = Wmin × 100 / Wmax (where K is the maximum yarn width Wmax (m) when the yarn is run for 2 minutes on a roller group having a contact angle of 4π.
m) is the running yarn width index defined by the above equation with respect to the minimum yarn width Wmin (mm). (2) The acrylic yarn according to the above (1), wherein the acrylic filament yarn comprises 4000 or more single yarns.
【００１５】（３）前記（１）または（２）に記載の糸
条をスチーム延伸して得られるアクリル系糸条。(3) An acrylic yarn obtained by steam-drawing the yarn according to (1) or (2).
【００１６】（４）アクリル系糸条をスチーム中で延伸
するに際し、スチーム延伸する前の糸条に対して流体処
理を施して糸条を開繊したのち延伸することを特徴とす
るアクリル系糸条のスチーム延伸方法。(4) When the acrylic yarn is stretched in steam, the yarn before steam stretching is subjected to a fluid treatment to open the yarn and then stretched. Article steam stretching method.
【００１７】（５）アクリル系フィラメント糸条が単糸
数４０００本以上からなるものであることを特徴とする
前記（４）に記載のアクリル系糸条のスチーム延伸方
法。(5) The method of (4), wherein the acrylic filament yarn comprises 4000 or more single yarns.
【００１８】（６）前記（４）または（５）に記載のス
チーム延伸方法において、開繊処理を施す流体が空気で
あることを特徴とするアクリル系糸条のスチーム延伸方
法。 （７）前記（４）または（５）に記載のスチーム延伸方
法において、開繊処理を施す流体がスチームであること
を特徴とするアクリル系糸条のスチーム延伸方法。(6) The steam drawing method for acrylic yarn according to the above (4) or (5), wherein the fluid to be spread is air. (7) In the steam stretching method according to the above (4) or (5), the fluid subjected to the fiber opening treatment is steam.
【００１９】（８）アクリル系糸条のスチーム延伸装置
において、スチーム延伸機のフィードロールの途中ある
いはフィードロールの上流側に流体処理ノズルを備えた
ことを特徴とするアクリル系糸条のスチーム延伸装置。(8) Acrylic yarn steam stretching apparatus, characterized in that a fluid processing nozzle is provided in the middle of the feed roll of the steam stretching machine or upstream of the feed roll. .
【００２０】（９）前記（３）に記載のアクリル系糸条
を焼成して得られる炭素繊維。(9) Carbon fibers obtained by firing the acrylic yarn described in (3).
【００２１】[0021]
【発明の実施の形態】以下、本発明の詳細と好ましい態
様を説明する。DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, details and preferred embodiments of the present invention will be described.
【００２２】本発明の糸条、方法および装置に適用する
アクリル系糸条の素材としてのアクリル系重合体は、ア
クリロニトリル９０重量％以上からなる重合体とするも
のであることが好ましい。従って、１０重量％以内で他
のモノマーを共重合成分として含んでいてもよい。コモ
ノマーとしてはアクリル酸、メタアクリル酸、イタコン
酸、もしくはこれらのメチルエステル、エチルエステ
ル、プロピルエステル、ブチルエステル、アルカリ金属
塩、アンモニウム塩、またはアリルスルホン酸、メタリ
ルスルホン酸、スチレンスルホン酸、もしくはこれらの
アルカリ金属塩等のうち一種または二種以上を用いるこ
とができる。The acrylic polymer used as the material for the acrylic yarn applied to the yarn, the method and the apparatus of the present invention is preferably a polymer composed of 90% by weight or more of acrylonitrile. Therefore, other monomers may be contained as copolymer components within 10% by weight. As the comonomer, acrylic acid, methacrylic acid, itaconic acid, or methyl ester, ethyl ester, propyl ester, butyl ester, alkali metal salt, ammonium salt thereof, or allyl sulfonic acid, methallyl sulfonic acid, styrene sulfonic acid, or One or more of these alkali metal salts can be used.
【００２３】本発明のアクリル系重合体は、たとえば公
知の乳化重合、塊状重合、溶液重合等の重合法を用いて
重合され、さらにこれらの重合体からアクリル系繊維を
製造するに際しては、ジメチルアセトアミド、ジメチル
スルホキシド（以下、ＤＭＳＯ）、ジメチルホルムアミ
ド、硝酸、ロダンソーダ水溶液等を溶媒とするポリマー
溶液を紡糸原液として、通常の湿式紡糸法、乾湿式紡糸
法によって紡糸し、その後、浴中延伸を行う。浴中延伸
は紡出糸を直接行っても良いし、一度水洗し溶媒を除去
した後に行ってもよい。浴中延伸は通常５０〜９８℃の
延伸浴中で約２〜６倍に延伸される。浴中延伸後は、通
常、油剤を付与し、ホットローラ等で乾燥緻密化した
後、スチーム延伸に供される。The acrylic polymer of the present invention is polymerized by a known polymerization method such as emulsion polymerization, bulk polymerization, solution polymerization and the like. Further, when producing acrylic fibers from these polymers, dimethylacetamide is used. A polymer solution using dimethyl sulfoxide (hereinafter, DMSO), dimethylformamide, nitric acid, an aqueous solution of rhodan soda or the like as a spinning solution is spun by a usual wet spinning method or dry-wet spinning method, and then drawn in a bath. Stretching in the bath may be performed directly on the spun yarn, or may be performed after once washing with water to remove the solvent. Stretching in a bath is usually stretched about 2 to 6 times in a stretching bath at 50 to 98 ° C. After stretching in a bath, usually, an oil agent is applied, dried and densified with a hot roller or the like, and then subjected to steam stretching.
【００２４】本発明に適用する糸条は、前述したアクリ
ル系糸条で加圧スチーム延伸処理するものであれば特に
限定されないが、炭素繊維プリカーサを製造する場合
に、本発明の効果が後段の焼成工程で重要性を増すので
好適である。The yarn to be applied to the present invention is not particularly limited as long as it is subjected to the above-mentioned acrylic yarn under pressure and steam stretching. However, in the case of producing a carbon fiber precursor, the effect of the present invention will be described later. This is preferable because the importance is increased in the firing step.
【００２５】本発明に適用する糸条は、糸条を構成する
単糸の数が４０００フィラメント以上、さらには６００
０フィラメント以上である場合に効果が著しく、また、
最終的に得られるアクリル系糸条の総繊度が４０００デ
ニール以上、さらには６０００デニール以上である場合
に特に効果が著しく発現するので好ましい。このような
太糸条のフィラメントをスチーム延伸する場合、糸束内
部にまでスチームや熱が均一に伝わりにくく、十分な延
伸性能が得られない場合が多い。特にスチーム延伸に先
立って行われる乾燥緻密化工程で、油剤に起因する疑似
接着が生じる場合はその延伸能低下が顕著となる。In the yarn applied to the present invention, the number of single yarns constituting the yarn is 4000 filament or more, and furthermore,
The effect is remarkable when it is 0 filament or more.
When the total fineness of the acrylic yarn finally obtained is 4000 denier or more, and more preferably 6000 denier or more, the effect is particularly remarkably exhibited, so that it is preferable. When such a thick yarn filament is subjected to steam drawing, steam and heat are difficult to be uniformly transmitted to the inside of the yarn bundle, and sufficient drawing performance is often not obtained. In particular, when pseudo-adhesion caused by the oil agent occurs in the dry densification step performed prior to the steam stretching, the stretching ability is significantly reduced.
【００２６】このため、本発明の延伸方法では、下記式
に示す走行糸幅指数Ｋが９５未満である糸条を延伸する
ことが重要である。ここで、Ｋとは、接触角４πのロー
ラ群に糸条を２分間走行させたときの、該ローラ上の最
大糸幅Ｗmax （ｍｍ）、最小糸幅Ｗmin （ｍｍ）に対
し、次式で定義される走行糸幅指数である。Therefore, in the drawing method of the present invention, it is important to draw a yarn having a running yarn width index K represented by the following formula of less than 95. Here, K is defined by the following formula with respect to the maximum yarn width Wmax (mm) and the minimum yarn width Wmin (mm) on the rollers when the yarn is run for 2 minutes on a roller group having a contact angle of 4π. It is a running yarn width index defined.
【００２７】Ｋ＝Ｗmin ×１００／Ｗmax 接触角４πのローラ群に糸条を走行させたときの上記Ｋ
値が９５未満、より好ましくは９０未満のアクリル糸条
であればスチーム延伸機に供給するローラ本、接触角は
特に限定されない。K = Wmin × 100 / Wmax The above K when the yarn is run on a group of rollers having a contact angle of 4π.
As long as the value is less than 95, more preferably less than 90, the number of rollers and the contact angle to be supplied to the steam stretching machine are not particularly limited.
【００２８】Ｋが９５未満、より好ましくは９０未満で
あれば太糸条のスチーム延伸は良好に行われるが、さら
にはスチーム延伸機に供給する糸条を流体処理して糸条
に十分開繊させることにより、糸条の疑似接着をはがす
とともに糸束内部へスチームを浸透させる作用が高まる
のでスチーム延伸をさらに好ましく行うことができる。If K is less than 95, and more preferably less than 90, steam drawing of the thick yarn is performed well, but furthermore, the yarn supplied to the steam drawing machine is subjected to fluid treatment to sufficiently open the yarn. By doing so, the pseudo-adhesion of the yarn is removed, and the action of permeating steam into the inside of the yarn bundle is increased, so that steam drawing can be performed more preferably.
【００２９】通常、これらの開繊処理は、スチーム延伸
機のフィードロールに導く糸条に対して行ない、この開
繊処理によってフィードロール上の糸幅が変化するほど
糸条の各単糸を動きやすくして、単糸間の疑似接着を容
易にひきはがすことが可能となる。Normally, these opening processes are performed on the yarn guided to the feed roll of the steam drawing machine, and the single yarn of the yarn moves as the yarn width on the feed roll changes by the opening process. This makes it possible to easily peel off the pseudo adhesion between the single yarns.
【００３０】開繊のための流体処理に使用する流体は空
気、スチーム、水、有機溶媒、無機物あるいは有機物を
含んだ溶液など、アクリル系糸条に化学変化を生じさせ
ず、かつ開繊効果を与えるものであればいずれでもよい
が、生産時の作業性等を考慮すると空気、スチームなど
が好ましい。The fluid used in the fluid treatment for fiber opening is air, steam, water, an organic solvent, a solution containing an inorganic substance or an organic substance, or the like, which does not cause a chemical change to the acrylic yarn and has an opening effect. Any one may be used as long as it gives the air, but air, steam, and the like are preferable in consideration of workability during production and the like.
【００３１】本開繊処理は、通常開繊ノズルを使用して
行うが、走行糸条を開繊できるものであればその形状は
特に限定されないが、走行糸条の直角方向から流体を吹
き付けることのできるノズルが好ましく用いることがで
きる。また、流体が空気あるいはスチームの場合は、そ
の圧力が１〜５ｋｇｆ／ｃｍ2 程度であるのが好まし
い。The opening process is usually performed using a spreading nozzle. The shape of the running yarn is not particularly limited as long as the running yarn can be spread, but a fluid is sprayed from a direction perpendicular to the running yarn. Nozzles that can be used are preferably used. When the fluid is air or steam, the pressure is preferably about 1 to 5 kgf / cm 2 .
【００３２】開繊ノズルの位置や、開繊処理時の糸条張
力は、糸条を開繊させるために適宜選ぶことができる
が、好ましくはローラ間の距離が３００ｍｍ以上あるロ
ーラ間に開繊ノズルを設置し、できるだけ小さい張力で
処理すると開繊効果が高まって延伸性が向上する。The position of the opening nozzle and the yarn tension during the opening operation can be appropriately selected in order to open the yarn. Preferably, the opening between the rollers having a distance between the rollers of 300 mm or more is used. When a nozzle is installed and the treatment is performed with a tension as small as possible, the opening effect is enhanced and the stretchability is improved.
【００３３】本発明の延伸方法は、延伸チューブにスチ
ームを吹き込むことにより延伸するのが好ましいが、延
伸チューブ内を糸条通過口を有するシール部材によって
予熱状態の延伸工程とそれに続く加熱状態の延伸工程の
２工程に分割し、それぞれの領域を圧力制御して延伸す
ると、延伸安定性がより向上して好ましい。糸条通過口
を有するシール部材を２領域間に設けることにより、同
一チューブ内の２領域の圧力を設定することができる。
この場合、加熱状態の延伸工程における圧力を予熱状態
の延伸工程における圧力より０．２〜５．０ｋｇ／ｃｍ
2 高くするのが好ましい。この圧力差が０．２ｋｇ／ｃ
ｍ2 未満では、従来の一段延伸と同様、前段の予熱部で
糸条内の延伸張力斑が生じやすくなり、毛羽が発生する
という問題があり、一方、圧力差が５．０ｋｇ／ｃｍ2
を越えると予熱部の温度が低すぎて、十分な予熱が行わ
れないか、または、予熱が十分であったとしても後段の
圧力が高すぎて、延伸ゾーンで糸条の溶断が生じるとい
う問題がある。In the stretching method of the present invention, the stretching is preferably performed by blowing steam into the stretching tube. However, the stretching step in the preheated state and the subsequent stretching in the heated state are performed in the stretching tube by a sealing member having a yarn passage. It is preferable to divide the process into two processes, and to stretch each of the regions under pressure control, since the stretching stability is further improved. By providing a seal member having a yarn passage between two regions, it is possible to set the pressure in two regions in the same tube.
In this case, the pressure in the stretching step in the heated state is 0.2 to 5.0 kg / cm higher than the pressure in the stretching step in the preheated state.
It is preferable to make it higher. This pressure difference is 0.2kg / c
If it is less than m 2, as in the conventional single-stage drawing, there is a problem that unevenness in the drawing tension in the yarn is apt to occur in the pre-heating section in the former stage and fuzz is generated, while the pressure difference is 5.0 kg / cm 2.
If the temperature exceeds the limit, the temperature of the preheating section is too low, and sufficient preheating is not performed, or even if the preheating is sufficient, the pressure in the subsequent stage is too high, and the yarn is melted in the drawing zone. There is.
【００３４】また、本発明の延伸方法は、延伸時の糸条
張力を０．１〜１．０ｇ／ｄ、好ましくは０．２〜０．
８ｇ／ｄの範囲に保持するのが好ましい。延伸張力が
０．１ｇ／ｄ未満では、スチーム圧力が高すぎて（温度
が高すぎて）溶断による延伸切れが発生するという問題
があり、一方、延伸張力が１．０ｇ／ｄを越えるとスチ
ーム圧力が低すぎて（温度が低すぎて）延伸切れが起こ
るという問題がある。In the stretching method of the present invention, the yarn tension at the time of stretching is 0.1 to 1.0 g / d, preferably 0.2 to 0.1 g / d.
It is preferable to keep it in the range of 8 g / d. When the stretching tension is less than 0.1 g / d, there is a problem that the steam pressure is too high (the temperature is too high) to cause stretching breakage due to fusing. On the other hand, when the stretching tension exceeds 1.0 g / d, the steam pressure is too high. There is a problem that the stretching is broken due to too low pressure (too low temperature).
【００３５】また、本発明では、加熱域に吹き込む加圧
スチームに適度の湿り度を与えることは、アクリル系糸
条を適度に濡らして可塑化効果を与え、延伸性を高める
ことからも好ましいことである。この湿りスチームを吹
き込むことによる糸条の水分率は、糸条に含まれる水分
が低すぎると十分な可塑化効果が得られずに延伸性が低
下し単糸切れによる毛羽が発生し、また、その後の乾燥
工程における糸条の水分蒸発負荷が増大することを防ぐ
観点から、高すぎても好ましくなく、延伸後の糸条水分
率の範囲は概ね２〜３０％の範囲であるのが好ましい。In the present invention, it is preferable that the pressurized steam blown into the heating zone be given an appropriate degree of wetness in order to appropriately wet the acrylic yarn to give a plasticizing effect and enhance the drawability. It is. The moisture content of the yarn by blowing this wet steam, if the moisture contained in the yarn is too low, a sufficient plasticizing effect is not obtained, the stretchability is reduced, and fluff due to single yarn breakage occurs, From the viewpoint of preventing an increase in the moisture evaporation load of the yarn in the subsequent drying step, it is not preferable that the yarn moisture content is too high, and the range of the yarn moisture content after stretching is generally in the range of 2 to 30%.
【００３６】延伸チューブ内の加圧スチームのシール部
材は、通常ラビリンスノズルと称する糸条の通過とスチ
ームの流出を同時に行う小口径を有するパイプを一個あ
るいは複数個連ねて用いるが、これに限定されるもので
はない。なおラビリンスノズルを使用する場合は、該小
口径の形状、寸法および使用個数はチューブ内の圧力を
糸条通過口の大小により所定の圧力範囲に調節できるも
のであればよい。As the sealing member for the pressurized steam in the drawn tube, one or a plurality of pipes each having a small diameter, usually referred to as a labyrinth nozzle, for simultaneously passing the yarn and flowing out the steam are used, but the present invention is not limited to this. Not something. In the case of using a labyrinth nozzle, the shape, size and number of the small bore may be any as long as the pressure in the tube can be adjusted to a predetermined pressure range depending on the size of the yarn passage opening.
【００３７】スチーム延伸倍率は、スチーム延伸に先立
って行われる浴中での延伸倍率によって決定すべきであ
るが、通常、２〜６倍の延伸を行い、全延伸倍率を７〜
１６倍の範囲にするのが好ましい。この時のスチーム圧
力は、延伸倍率と延伸温度によって左右されるが、本発
明における糸条の張力は、前記した延伸倍率のもとで、
先に述べたように０．１〜１．０ｇ／ｄに保持するもの
であることが好ましい。The steam stretching ratio should be determined by the stretching ratio in a bath performed prior to the steam stretching. Usually, the stretching ratio is 2 to 6 times, and the total stretching ratio is 7 to 7.
It is preferable to set the range to 16 times. The steam pressure at this time depends on the draw ratio and the draw temperature, but the tension of the yarn in the present invention is determined under the above draw ratio.
As described above, it is preferable to maintain the pressure at 0.1 to 1.0 g / d.
【００３８】次に、図面に示す実施例にしたがって本発
明の実施態様をさらに詳細に説明する。Next, embodiments of the present invention will be described in more detail with reference to the embodiments shown in the drawings.
【００３９】図１は本発明に係るスチーム延伸装置の一
例を示すものであり、延伸チューブの両端および中央部
にスチームのシール構造を有した二段延伸機構を有する
延伸機と糸条開繊のためのノズルを有する断面図であ
る。FIG. 1 shows an example of a steam drawing apparatus according to the present invention. The drawing machine has a two-stage drawing mechanism having a steam sealing structure at both ends and a center of a drawing tube, and a yarn opening device. FIG. 2 is a cross-sectional view having a nozzle.
【００４０】糸条Ａはフィードローラ群８を径て、スチ
ーム加圧装置Ｂへ供給される。このスチーム加圧装置Ｂ
は、糸条の供給口１を有するシール部材４と、糸条取り
出し口２を有するシール部材５を両端に備えた円筒状容
器（延伸チューブ）１０から構成されている。延伸チュ
ーブ１０はシール部材１１により予熱域と加熱域に分け
られ、加熱域に加圧スチーム供給口３を有している。加
圧スチームは加湿器７およびスチーム導入管６を径て延
伸チューブ１０に導入される。糸条Ａは、フィードロー
ラ群８に入る前、あるいはフィードローラ群の途中で、
開繊ノズル１３により開繊処理を受けた後、スチーム加
圧装置Ｂに導かれ、スチーム加圧装置Ｂ中を通過する間
にスチームにより加圧加温され、ドローローラ９により
延伸される。The yarn A has a diameter of the feed roller group 8 and is supplied to a steam pressurizing device B. This steam pressurizer B
Is composed of a cylindrical container (stretched tube) 10 provided at both ends with a seal member 4 having a thread supply port 1 and a seal member 5 having a thread take-out port 2. The stretching tube 10 is divided into a preheating region and a heating region by a seal member 11, and has a pressurized steam supply port 3 in the heating region. The pressurized steam is introduced into the stretching tube 10 through the humidifier 7 and the steam introduction tube 6. Before the yarn A enters the feed roller group 8 or in the middle of the feed roller group,
After being subjected to the fiber opening process by the fiber opening nozzle 13, it is guided to the steam pressurizing device B, heated and heated by steam while passing through the steam pressurizing device B, and stretched by the draw roller 9.
【００４１】この延伸ゾーンの圧力制御は、供給スチー
ムの圧力制御器１２ならびにシール部材４、５および１
１の開口径を調節することにより行われる。この際、糸
条Ａが円滑に通過し、かつチューブ内の圧力バランスが
適正に保たれるように開口径を調整することが好まし
い。このシール部材の形状、寸法は上記条件が満たされ
るなら特に限定されるものではない。スチームの供給口
３の位置は、糸条の予熱と延伸が十分に行われることを
考慮すれば、シール部材１１に隣接した位置に設けるこ
とが好ましい。The pressure control of this stretching zone is performed by controlling the pressure controller 12 of the supply steam and the sealing members 4, 5 and 1.
1 is adjusted by adjusting the opening diameter. At this time, it is preferable to adjust the opening diameter so that the yarn A passes smoothly and the pressure balance in the tube is properly maintained. The shape and dimensions of the seal member are not particularly limited as long as the above conditions are satisfied. The position of the steam supply port 3 is preferably provided at a position adjacent to the seal member 11 in consideration of sufficient preheating and drawing of the yarn.
【００４２】なお、予熱ゾーンの圧力はシール部材１１
の開口径を調節することにより適宜設定することができ
る。The pressure in the preheating zone is controlled by the sealing member 11.
It can be set appropriately by adjusting the opening diameter of.
【００４３】[0043]
【実施例】以下実施例をあげて本発明をさらに具体的に
説明する。The present invention will be described more specifically with reference to the following examples.
【００４４】実施例１ アクリロニトリル９９．７モル％、イタコン酸０．３モ
ル％からなる固有粘度［η］が１．８０のアクリル系重
合体の２０％ＤＭＳＯ溶液を紡糸原液として、孔径が
０．１ｍｍφの６０００ホールの口金を用いてＤＭＳＯ
３０％、水７０％からなる凝固浴中に３ｍｍの空気層を
介した後に吐出し、凝固糸を得た。該凝固糸を２本合わ
せて１２０００フィラメントとしてから水洗し、熱水中
で２．５倍に延伸した後、シリコーン系油剤を付与して
から乾燥緻密化を行い、引続いて延伸チューブの両端を
ラビリンスノズルでシールし、チューブ中央部のスチー
ム吹き込み口に隣接し、かつ糸条導入側にもう一段ラビ
リンスシールを設けた加圧スチーム延伸装置で延伸し
（５倍延伸）、単繊維繊度が１．０ｄで、総繊度が１２
０００ｄの延伸糸を得た。Example 1 A 20% DMSO solution of an acrylic polymer composed of 99.7 mol% of acrylonitrile and 0.3 mol% of itaconic acid and having an intrinsic viscosity [η] of 1.80 was used as a stock solution for spinning and had a pore size of 0. DMSO using 1mmφ 6000 hole base
After passing through a 3 mm air layer in a coagulation bath consisting of 30% and 70% water, the mixture was discharged to obtain a coagulated yarn. The two coagulated yarns were combined to form 12000 filaments, washed with water, stretched 2.5 times in hot water, then applied with a silicone oil agent, and then dried and densified. It is sealed with a labyrinth nozzle and stretched by a pressurized steam stretching device provided with another labyrinth seal on the yarn introduction side, adjacent to the steam inlet at the center of the tube (5 times stretching), and the single fiber fineness is 1. 0d, total fineness is 12
A 000d drawn yarn was obtained.
【００４５】スチーム延伸にあたって、図１に示すよう
に接触角４πのフィードローラ群に糸条を通しながら開
繊ノズルに圧縮空気を供給し、糸条を開繊しながら延伸
し、延伸糸条の走行毛羽数（１０分間の毛羽数を目測で
カウントし、１分当たりに換算）を測定した。また、こ
のときのフィードロール上の糸幅を２分間測定し、その
間の最大糸幅Ｗmax 、最小糸幅Ｗmin も測定した。結果
を表１に示す。In steam stretching, as shown in FIG. 1, compressed air is supplied to a fiber opening nozzle while passing the yarn through a feed roller group having a contact angle of 4π, and the yarn is stretched while being spread. The number of running fluffs (the number of fluffs for 10 minutes was counted by eye and converted per minute) was measured. At this time, the yarn width on the feed roll was measured for 2 minutes, and the maximum yarn width Wmax and the minimum yarn width Wmin during that time were also measured. Table 1 shows the results.
【００４６】表１の結果から、本発明による開繊処理後
の延伸方法により、毛羽の発生が大幅に改善されること
がわかる。From the results shown in Table 1, it can be seen that generation of fluff is greatly improved by the stretching method after the fiber opening treatment according to the present invention.
【００４７】[0047]
【表１】 [Table 1]
【００４８】[0048]
【発明の効果】本発明によれば、アクリル系太物糸条を
高倍率で延伸することができるスチーム延伸方法を提供
することができる。According to the present invention, it is possible to provide a steam stretching method capable of stretching an acrylic thick yarn at a high magnification.
【図１】本発明の延伸装置の一例の断面図である。FIG. 1 is a cross-sectional view of an example of a stretching device of the present invention.
Ａ：延伸に供される糸条 Ｂ：スチーム加圧装置 １：糸条の供給口 ２：延伸糸条の取り出し口 ３：スチーム供給口 ４：糸条導入部のシール部材 ５：延伸糸条取り出し部のシール部材 ６：スチーム導入管 ７：供給スチームの加湿器 ８：糸条のフィードローラ群 ９：延伸糸条のドローローラ群 １０：円筒状容器 １１：予熱域と加熱域の間の糸条通過口を有するシール
部材 １２：スチーム圧力制御装置 １３：開繊ノズルA: Yarn provided for drawing B: Steam pressurizing device 1: Yarn supply port 2: Draw yarn take-out port 3: Steam supply port 4: Seal member at yarn introduction section 5: Draw yarn take-out Seal member 6: steam introduction pipe 7: humidifier for supply steam 8: feed roller group for yarn 9: draw roller group for drawn yarn 10: cylindrical container 11: yarn between preheating area and heating area Seal member having a passage opening 12: Steam pressure control device 13: Spreading nozzle
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ Ｄ０２Ｊ 1/18 Ｄ０２Ｊ 1/18 ──────────────────────────────────────────────────続 き Continued on front page (51) Int.Cl. 6 Identification code FI D02J 1/18 D02J 1/18
Claims (9)
記に示す走行糸幅指数Ｋが９５未満であることを特徴と
するアクリル系糸条。 Ｋ＝Ｗmin ×１００／Ｗmax （ここで、Ｋとは、接触角４πのローラ群に糸条を２分
間走行させたときの、該ローラ上の最大糸幅Ｗmax （ｍ
ｍ）、最小糸幅Ｗmin （ｍｍ）に対し、上式で定義され
る走行糸幅指数である。）1. An acrylic filament yarn, wherein a running yarn width index K shown below is less than 95. K = Wmin × 100 / Wmax (where K is the maximum yarn width Wmax (m) when the yarn is run for 2 minutes on a roller group having a contact angle of 4π.
m) is the running yarn width index defined by the above equation with respect to the minimum yarn width Wmin (mm). )
００本以上からなるものであることを特徴とする請求項
１に記載のアクリル系糸条。2. An acrylic filament yarn comprising 40 single yarns.
The acrylic yarn according to claim 1, wherein the acrylic yarn comprises at least 00 yarns.
延伸して得られるアクリル系糸条。3. An acrylic yarn obtained by steam-drawing the yarn according to claim 1 or 2.
際し、スチーム延伸する前の糸条に対して流体処理を施
して糸条を開繊したのち延伸することを特徴とするアク
リル系糸条のスチーム延伸方法。4. An acrylic yarn, wherein when the acrylic yarn is drawn in steam, the yarn before steam drawing is subjected to a fluid treatment to open the yarn and then drawn. Steam stretching method.
００本以上からなるものであることを特徴とする請求項
４に記載のアクリル系糸条のスチーム延伸方法。5. An acrylic filament yarn comprising 40 single yarns.
The method for steam stretching acrylic yarn according to claim 4, wherein the method comprises at least 00 yarns.
法において、開繊処理を施す流体が空気であることを特
徴とするアクリル系糸条のスチーム延伸方法。6. A method according to claim 4, wherein the fluid to be spread is air.
法において、開繊処理を施す流体がスチームであること
を特徴とするアクリル系糸条のスチーム延伸方法。7. A method according to claim 4, wherein the fluid to be subjected to the fiber opening treatment is steam.
て、スチーム延伸機のフィードロールの途中あるいはフ
ィードロールの上流側に流体処理ノズルを備えたことを
特徴とするアクリル系糸条のスチーム延伸装置。8. A steam stretching apparatus for acrylic yarn, comprising a fluid treatment nozzle in the middle of a feed roll of the steam stretching machine or upstream of the feed roll.
て得られる炭素繊維。9. A carbon fiber obtained by firing the acrylic yarn according to claim 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16289697A JPH1112874A (en) | 1997-06-19 | 1997-06-19 | Acrylic fiber yarn, and method and apparatus for steam-drawing of the same, and carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16289697A JPH1112874A (en) | 1997-06-19 | 1997-06-19 | Acrylic fiber yarn, and method and apparatus for steam-drawing of the same, and carbon fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH1112874A true JPH1112874A (en) | 1999-01-19 |
Family
ID=15763307
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16289697A Pending JPH1112874A (en) | 1997-06-19 | 1997-06-19 | Acrylic fiber yarn, and method and apparatus for steam-drawing of the same, and carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH1112874A (en) |
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| WO2000077282A1 (en) * | 1999-06-15 | 2000-12-21 | Mitsubishi Rayon Co., Ltd. | Acrylic yarn as thick carbon fiber precursor and method for producing the same |
| JP2008075205A (en) * | 2006-09-21 | 2008-04-03 | Mitsubishi Rayon Co Ltd | Method and apparatus for stretching fiber by using pressurized steam, and method for producing acrylic precursor fiber bundle for carbon fiber |
| JP2009174073A (en) * | 2008-01-23 | 2009-08-06 | Toray Ind Inc | Method for producing precursor fiber of carbon fiber |
| JP2009197373A (en) * | 2008-02-25 | 2009-09-03 | Toray Ind Inc | Production method of carbon fiber precursor fiber and carbon fiber |
| CN102277629A (en) * | 2011-06-10 | 2011-12-14 | 金发科技股份有限公司 | Dry-jet wet-spinning method for preparing polyacrylonitrile carbon fiber precursor |
| JP2012207359A (en) * | 2011-03-11 | 2012-10-25 | Mitsubishi Rayon Co Ltd | Method and apparatus for producing acrylic fiber |
| WO2012165574A1 (en) * | 2011-06-03 | 2012-12-06 | 三菱レイヨン株式会社 | Method of manufacturing carbon fiber precursor acrylic fiber bundle |
| CN103451755A (en) * | 2013-08-31 | 2013-12-18 | 连云港鹰游纺机有限责任公司 | Air handling unit used for carbon fiber precursors |
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-
1997
- 1997-06-19 JP JP16289697A patent/JPH1112874A/en active Pending
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