JPH11350244A - Production of acrylic fiber - Google Patents

Production of acrylic fiber

Info

Publication number
JPH11350244A
JPH11350244A JP8108399A JP8108399A JPH11350244A JP H11350244 A JPH11350244 A JP H11350244A JP 8108399 A JP8108399 A JP 8108399A JP 8108399 A JP8108399 A JP 8108399A JP H11350244 A JPH11350244 A JP H11350244A
Authority
JP
Japan
Prior art keywords
coagulation bath
liquid level
producing
level fluctuation
acrylic fiber
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.)
Pending
Application number
JP8108399A
Other languages
Japanese (ja)
Inventor
Hidemi Goto
英実 後藤
Fumio Ogawa
文夫 小川
Kazuhisa Narisawa
和久 成澤
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.)
Toray Industries Inc
Original Assignee
Toray Industries Inc
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 Toray Industries Inc filed Critical Toray Industries Inc
Priority to JP8108399A priority Critical patent/JPH11350244A/en
Publication of JPH11350244A publication Critical patent/JPH11350244A/en
Pending legal-status Critical Current

Links

Landscapes

  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

PROBLEM TO BE SOLVED: To stably obtain acrylic fiber with high grade even under increased spinneret hole number and/or travel speed through the coagulation bath by dry/wet spinning of an acrylic polymer while controlling coagulation bath level fluctuation index at a specific value or lower. SOLUTION: This acrylic fiber is obtained by dry/wet spinning of an acrylic polymer at a travel rate of >=10 m/min using a spinneret with the number of holes of >=2,000 while controlling coagulation bath level fluctuation index defined as: coagulation bath level fluctuation width μ coagulation bath level fluctuation frequency [the level fluctuation width (mm) is the maximum fluctuation width over 10 min at a relative position on the liquid level; the level fluctuation frequency (Hz) is the maximum value of liquid level fluctuation over one second] at <=0.05 mm/s through such procedure that, a wire net is disposed around the spinneret, the depth direction and/or interspindle direction of the coagulation bath tank is expanded, or a truncatedly conical rectifying tube is interposed between direction-transformation guides in the coagulation bath.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、乾湿式紡糸法によ
り、安定して高品位のアクリル系繊維を提供することが
できるアクリル系繊維の製造方法及び乾湿式紡糸装置に
関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing acrylic fibers and a dry-wet spinning apparatus capable of stably providing high-quality acrylic fibers by a dry-wet spinning method.

【0002】[0002]

【従来の技術】アクリル系繊維の製造において、生産効
率を高め、製造原価を低減させることは極めて重要であ
る。これに対して、1錘当たりの孔数を増加させた紡糸
口金を使用したり、口金の錘数や紡糸する糸条数を増加
させる、さらには、糸条の走行速度を増大させるなどの
種種の方法が採用されている。
2. Description of the Related Art In the production of acrylic fibers, it is extremely important to increase production efficiency and reduce production costs. On the other hand, there are various kinds of spinnerets with an increased number of holes per spindle, such as increasing the number of spindles and the number of yarns to be spun, and increasing the running speed of the yarn. The method is adopted.

【0003】これら方法の内、口金の錘数や紡糸する糸
条数を増やすに伴っては比較的大きな設備の拡張が必要
となるのに対し、口金1錘当たりの孔数を増加したり、
糸条の走行速度を増大させることは大きな設備の拡張を
伴わずに無理なく実施できる点で大きなメリットがあ
る。
[0003] Among these methods, a relatively large expansion of equipment is required as the number of spindles and the number of yarns to be spun are increased. On the other hand, the number of holes per spindle is increased.
Increasing the running speed of the yarn has a great merit in that it can be carried out without difficulty without a large facility expansion.

【0004】しかし、アクリル系繊維の製造において、
ポリマー溶液を一旦エアギャップを通過させた後、凝固
浴液中に吐出し、脱溶媒及び凝固させることにより凝固
糸条を得、さらに必要に応じて水洗、延伸、乾燥緻密化
等の処理を行う乾湿式紡糸法を採用する場合、1錘当た
りの孔数を増加させた紡糸口金を使用したり、紡糸速度
すなわち凝固浴槽中の糸条の走行速度を大きくすると、
得られる繊維の品位が著しく低下し、ひどい場合は糸切
れなど操業性の悪化を引き起こす問題も有る。この原因
は、紡糸する糸条のフィラメント数が増加したり、糸条
の走行速度が増大すると、凝固浴液の流れに乱れが生
じ、凝固液の液面が擾乱を受けて口金面と凝固浴液面と
の距離が時々刻々変化するためと考えられる。
However, in the production of acrylic fibers,
After the polymer solution is once passed through the air gap, the polymer solution is discharged into a coagulation bath, desolvation and coagulation is performed to obtain a coagulated yarn, and if necessary, washing, stretching, drying and densification are performed. When the dry-wet spinning method is adopted, if a spinneret with an increased number of holes per spindle is used or the spinning speed, that is, the running speed of the yarn in the coagulation bath is increased,
The quality of the obtained fiber is remarkably reduced, and in severe cases, there is a problem that the operability is deteriorated such as yarn breakage. This is because, when the number of filaments of the spun yarn increases or the running speed of the yarn increases, the flow of the coagulation bath liquid is disturbed, and the liquid level of the coagulation liquid is disturbed, and the surface of the die and the coagulation bath are disturbed. It is considered that the distance from the liquid surface changes every moment.

【0005】かかる問題に対し、特公平3−70006
号公報、特開昭60−94617号公報に開示されてい
る、いわゆる流下浴紡糸装置では、凝固浴液中に高分子
溶液を吐出しながら凝固浴液を流下させ、凝固した複数
の糸条と凝固浴液を配管に通じて流出させることによ
り、単糸にかかる凝固液の随伴抵抗を軽減し、また凝固
浴液の流れを強制的にコントロールすることで単糸同士
の擦過を効果的に抑制し、1錘当たりの孔数を増加させ
た紡糸口金の使用を可能としたり、糸条の走行速度を増
大させることを可能とした。
To solve such a problem, Japanese Patent Publication No. 3-70006
In a so-called falling bath spinning apparatus disclosed in Japanese Patent Application Laid-Open No. 60-94617, a coagulation bath solution is caused to flow while discharging a polymer solution into the coagulation bath solution, and a plurality of coagulated yarns are formed. The coagulation bath liquid flows out through the piping to reduce the associated resistance of the coagulation liquid applied to the single yarn, and effectively controls the flow of the coagulation bath liquid to effectively prevent abrasion between the single yarns. In addition, it is possible to use a spinneret having an increased number of holes per spindle, or to increase the running speed of a yarn.

【0006】しかしながら、かかる流下浴紡糸装置では
糸条を流管部に通し始める際、すなわち糸出し時に、糸
条からなる塊状物がノズル部に詰まって紡糸を妨げるこ
とが問題となっていた。
However, in such a falling bath spinning apparatus, when the yarn is started to pass through the flow tube portion, that is, at the time of yarn drawing out, there is a problem that a lump of the yarn is clogged in the nozzle portion to hinder spinning.

【0007】また、実開昭59−21670号公報で提
案されているノズル径可変型の流管式紡糸装置は、糸出
し時はノズル径を大きくし、操業時はノズル径を小さく
することで上記したような問題点を解決することができ
るが、生産設備の複雑化、糸出しの操作の煩雑化を招
き、口金を10錘を越える数備えた規模の大きな生産機
の場合は適用するのが困難であった。
[0007] The variable-diameter flow tube type spinning apparatus proposed in Japanese Utility Model Laid-Open Publication No. 59-21670 is designed to increase the nozzle diameter at the time of yarn feeding and to reduce the nozzle diameter at the time of operation. Although the above-mentioned problems can be solved, the production equipment becomes complicated, and the operation of the yarn feeding becomes complicated. In the case of a large-scale production machine having more than 10 spindles, this method is applied. Was difficult.

【0008】[0008]

【発明が解決しようとする課題】本発明は、上記したよ
うな従来技術の問題点に鑑み、アクリル系繊維を乾湿式
紡糸法により製造する際に、口金1錘当たりの孔数を増
加したり、凝固浴槽中の糸条走行速度を増大した際に特
に顕在化し易い繊維の品位の低下、操業性の悪化を効果
的に防止できるアクリル系繊維の製造方法を提供せんと
するものである。
SUMMARY OF THE INVENTION In view of the above-mentioned problems of the prior art, the present invention is intended to increase the number of holes per spinneret when producing acrylic fibers by a dry-wet spinning method. It is another object of the present invention to provide a method for producing acrylic fibers that can effectively prevent a decrease in fiber quality and a decrease in operability, which are likely to be particularly noticeable when the yarn traveling speed in the coagulation bath is increased.

【0009】[0009]

【課題を解決するための手段】本発明は、かかる課題を
解決するために、次のような構成を採用する。すなわ
ち、口金面から吐出されたポリマー溶液を一旦エアギャ
ップを通過させて凝固浴槽に導く乾湿式紡糸法におい
て、下記に示す凝固浴液面変動指数を0.05mm/sec
以下に保ちながら紡糸することを特徴とするアクリル系
繊維の製造方法である。
The present invention employs the following configuration in order to solve such a problem. That is, in a dry-wet spinning method in which a polymer solution discharged from a die surface is once passed through an air gap and introduced into a coagulation bath, a coagulation bath liquid surface fluctuation index shown below is 0.05 mm / sec.
A method for producing an acrylic fiber, comprising spinning while maintaining the following.

【0010】凝固浴液面変動指数=凝固浴液面変動幅×
凝固浴液面変動振動数 式中:凝固浴液面変動指数(単位;mm/sec ) 凝固浴液面変動幅(単位;mm):10分間の凝固浴液面
の相対位置の最大変動幅 凝固浴液面振動数(単位;Hz):1秒間の凝固浴液面
変動の極大値のの数
Coagulation bath liquid level fluctuation index = coagulation bath liquid level fluctuation width ×
Coagulation bath liquid level fluctuation frequency Formula: Coagulation bath liquid level fluctuation index (unit: mm / sec) Coagulation bath liquid level fluctuation width (unit: mm): Maximum fluctuation width of relative position of coagulation bath liquid level for 10 minutes Bath surface frequency (unit: Hz): number of local maximum values of coagulation bath surface fluctuation for one second

【0011】[0011]

【発明の実施の形態】本発明は、アクリル系繊維を乾湿
式紡糸法により製造する際に、口金1錘当たりの孔数を
増加したり、凝固浴槽中の糸条走行速度を増大した場合
に問題となる繊維の品位の低下、操業性の悪化を効果的
に防止できる技術について、鋭意検討した結果、かかる
場合には凝固浴槽中で糸条に架かる張力が変動すること
により単糸に欠陥が生じて得られる繊維の品位が低下す
ることを見出したものである。さらに、凝固浴槽におい
て、後述する凝固浴液面変動指数を0.05mm/sec 以
下に保ちながら紡糸することにより、かかる課題を一挙
に解決することを究明したものである。
BEST MODE FOR CARRYING OUT THE INVENTION The present invention relates to a method for producing acrylic fibers by a dry-wet spinning method, in which the number of holes per spinneret is increased or the yarn traveling speed in a coagulation bath is increased. As a result of intensive studies on technologies that can effectively prevent the problem of fiber quality deterioration and operability deterioration, in such cases, single yarn defects are caused by fluctuations in the tension applied to the yarn in the coagulation bath. It has been found that the quality of the resulting fiber is reduced. Further, the present inventors have sought to solve such a problem at once by spinning in a coagulation bath tank while maintaining a coagulation bath liquid surface fluctuation index described below at 0.05 mm / sec or less.

【0012】本発明において、アクリル系繊維は、乾湿
式紡糸法により紡糸して得られるものであれば特に限定
されない。本発明は、毛羽など欠陥の少ない高品位のア
クリル系繊維が要求される炭素繊維用プリカーサーの製
造において特に有効に採用し得るものである。
In the present invention, the acrylic fiber is not particularly limited as long as it is obtained by spinning by a dry-wet spinning method. INDUSTRIAL APPLICATION This invention can be employ | adopted especially effectively in manufacture of the precursor for carbon fibers which require high quality acrylic fiber with few defects, such as a fluff.

【0013】本発明において、アクリル系繊維を構成す
るアクリル系重合体には、アクリロニトリル90重量%
以上からなる重合体が好ましく使用される。なお、アク
リロニトリル(以下、ANと略記)に共重合させるモノ
マーとしては、アクリル酸、メタクリル酸、イタコン
酸、又はこれらのメチルエステル、エチルエステルなど
が採用できる。
In the present invention, the acrylic polymer constituting the acrylic fiber contains 90% by weight of acrylonitrile.
A polymer composed of the above is preferably used. In addition, as a monomer copolymerized with acrylonitrile (hereinafter, abbreviated as AN), acrylic acid, methacrylic acid, itaconic acid, or a methyl ester or an ethyl ester thereof can be used.

【0014】かかるアクリル系重合体からなるポリマー
を溶存させる溶液には、ジメチルアセトアミド、ジメチ
ルスルホキシド(以下、DMSOと略記)、ジメチルホ
ルムアミドなどを溶媒として用いることができる。かか
る溶液のポリマー濃度は、10重量%以上50重量%以
下であることが好ましい。
In the solution in which the polymer comprising the acrylic polymer is dissolved, dimethylacetamide, dimethylsulfoxide (hereinafter abbreviated as DMSO), dimethylformamide, or the like can be used as a solvent. The polymer concentration of such a solution is preferably from 10% by weight to 50% by weight.

【0015】かかるポリマー溶液を使用して、1mm以上
50mm以下のエアギャップを設けた乾湿式紡糸装置によ
り、凝固糸条を得た後、水洗、一次延伸、油剤付与、乾
燥緻密化、必要に応じて二次延伸などの工程を経てアク
リル系繊維を製造する。ここで、凝固浴液には、ポリマ
ー溶液に使用される溶媒と同種の溶媒及び水からなるも
のが使用できる。
Using such a polymer solution, a coagulated yarn is obtained by a dry-wet spinning apparatus provided with an air gap of 1 mm or more and 50 mm or less, followed by washing with water, primary drawing, application of an oil agent, drying and densification, if necessary. To produce an acrylic fiber through a process such as secondary stretching. Here, as the coagulation bath solution, a solution containing the same kind of solvent and water as the solvent used for the polymer solution can be used.

【0016】かかるアクリル系繊維の製造方法におい
て、口金1錘当たりの孔数2000以上、3000以
上、さらには4000以上の多数の孔を備えた口金を使
用して、アクリル系繊維を紡糸するような場合に、本発
明の効果が顕著に発現されるのである。さらに、凝固紡
糸速度、すなわち凝固浴槽中での糸条の走行速度が、1
0m/分以上、さらには20m/分以上の高速紡糸の場
合においても、効果を顕著に高めることができる。すな
わち、このような、孔を多数備えた口金を使用して、高
速で紡糸する場合は、凝固浴液の流れの乱れが特に大き
くなり易く、それに伴い凝固浴液面変動も大きくなり、
得られる繊維の品位が著しく低下することが多いことか
ら、本発明によるアクリル系繊維の製造方法は、特に好
適である。
In such a method for producing an acrylic fiber, the spinning of the acrylic fiber is performed by using a die having a large number of holes of 2000 or more, 3000 or more, and even 4000 or more per one spinneret. In such a case, the effect of the present invention is remarkably exhibited. Furthermore, the coagulation spinning speed, that is, the running speed of the yarn in the coagulation bath, is 1
Even in the case of high-speed spinning of 0 m / min or more, and even 20 m / min or more, the effect can be significantly improved. That is, when spinning at a high speed using such a die having a large number of holes, the turbulence of the flow of the coagulation bath liquid is particularly likely to increase, and the fluctuation in the coagulation bath liquid level also increases.
The method for producing acrylic fibers according to the present invention is particularly suitable, since the quality of the obtained fibers is often significantly reduced.

【0017】かかる凝固浴液の流れの乱れや、凝固浴液
面変動を適切に制御すれば、得られる繊維の品位を著し
く改善することができる。すなわち、本発明では、下式
に示す凝固浴液面変動指数を0.05mm/sec 以下に制
御することによって、かかる凝固浴液の流れの乱れや、
凝固浴液面変動を効果的に抑制することに成功したもの
である。
If the turbulence of the flow of the coagulation bath liquid and the fluctuation of the liquid level of the coagulation bath liquid are appropriately controlled, the quality of the obtained fiber can be remarkably improved. That is, in the present invention, by controlling the coagulation bath liquid surface fluctuation index shown below to 0.05 mm / sec or less, the flow of the coagulation bath liquid is disturbed,
It has succeeded in effectively suppressing the fluctuation of the liquid level of the coagulation bath.

【0018】図1に,凝固浴液面変動の測定結果の一例
を示す。ここで凝固浴液面変動指数は、次式に示すよう
に10分間の凝固浴液面の相対位置の最大変動幅(ここ
では、図1のように、10分間の凝固浴液面変動を示す
グラフにおいて、変動幅の最大値Hmaxを指す)と一定
時間の凝固浴液面変動の極大値の数を1秒間当たりに換
算して得られる凝固浴液面変動振動数を掛け合わせた数
であり、1秒間当たりに凝固浴液面が変動する程度の指
標となるものである。
FIG. 1 shows an example of the measurement result of the liquid level fluctuation of the coagulation bath. Here, the coagulation bath liquid level fluctuation index is the maximum fluctuation width of the relative position of the coagulation bath liquid surface for 10 minutes as shown by the following equation (here, the coagulation bath liquid surface fluctuation for 10 minutes as shown in FIG. 1). In the graph, the maximum value of the fluctuation range Hmax) is multiplied by the coagulation bath liquid level fluctuation frequency obtained by converting the number of the maximum values of the coagulation bath liquid level fluctuation for a certain period of time into one second. It is an index of the degree to which the liquid level of the coagulation bath changes per second.

【0019】凝固浴液面変動指数=凝固浴液面変動幅×
凝固浴液面変動振動数 なお、後で掲げる図表においては、凝固浴液面変動指数
については略称としてMを、凝固浴液面変動幅について
は略称としてHmaxを、凝固浴液面振動数については略
称としてfをそれぞれ使用する。
Coagulation bath liquid level fluctuation index = Coagulation bath liquid level fluctuation width x
In the charts given below, M is an abbreviation for the coagulation bath liquid surface fluctuation index, Hmax is an abbreviation for the coagulation bath liquid surface fluctuation width, and the coagulation bath liquid surface frequency is F is used as an abbreviation.

【0020】かかる凝固浴液面変動指数が0.05mm/
sec 以下であれば、安定して、高品位の繊維を得ること
ができる。毛羽などが僅少な品位の高いアクリル系繊維
が要求されることの多い炭素繊維用プリカーサーの製造
においては、かかる凝固浴液面変動指数を0.03mm/
sec 以下に制御するのが好ましい。なお、かかる凝固浴
液面変動指数は0.01mm/sec 程度で有れば、本発明
の効果を奏するに当たって、十分であることが多い。
The solidification bath liquid level fluctuation index is 0.05 mm /
If it is less than sec, high-quality fibers can be stably obtained. In the production of a precursor for carbon fiber, which often requires high-quality acrylic fiber with little fluff, etc., such a coagulation bath liquid surface fluctuation index is 0.03 mm /
It is preferable to control the time to sec or less. If the solidification bath liquid level fluctuation index is about 0.01 mm / sec, it is often sufficient to achieve the effects of the present invention.

【0021】この凝固浴液面変動指数が0.05mm/se
c 以下になるように、凝固浴液面変動を抑制する方法と
しては様々な方法があるが、例えば、図2のように凝固
浴液面において口金の周囲を取り囲むようにして金網を
設置する方法が挙げられる。しかし、この方法では、凝
固浴液面変動幅を低く抑える効果はあるものの、凝固浴
液面変動振動数を低減する効果は小さく、結果的に凝固
浴液面変動を抑制する効果は弱いものとなる。また、凝
固浴槽を深さ方向又は錘間方向に拡張することにより、
凝固浴の液面変動は、その幅、振動数ともに抑制される
が、1錘当たりの凝固浴槽が過大となり、例えば錘数が
10を越えるような規模の大きな生産機の場合には適用
が困難となることがある。
The solidification bath liquid level fluctuation index is 0.05 mm / se.
c There are various methods for suppressing the fluctuation of the liquid level of the coagulation bath as described below. For example, a method of installing a wire mesh so as to surround the periphery of the die on the liquid surface of the coagulation bath as shown in FIG. Is mentioned. However, in this method, although the effect of suppressing the coagulation bath liquid surface fluctuation width is low, the effect of reducing the coagulation bath liquid surface fluctuation frequency is small, and as a result, the effect of suppressing the coagulation bath liquid surface fluctuation is weak. Become. Also, by expanding the coagulation bath in the depth direction or the direction between the weights,
Fluctuations in the liquid level of the coagulation bath are suppressed in both width and frequency, but the coagulation bath per spindle becomes excessively large, making it difficult to apply in the case of a large-scale production machine having, for example, more than 10 spindles. It may be.

【0022】生産設備の大規模な変更を必要としないこ
とから、凝固浴槽中に円錐台状の整流筒を設置する方法
が、本発明において凝固浴液面変動の抑制に当たり、最
適である。図3は、整流筒を使用した本発明の実施態様
の一例を示す概略斜視図であるが、このように整流筒
は、口金と凝固浴槽中の方向転換ガイドの間に、流下す
る糸条を適度な距離を置いて取り囲むようにして設置す
るのが好ましい。
Since a large-scale change of the production equipment is not required, a method of installing a truncated conical rectifying cylinder in the coagulation bath is the most suitable method for suppressing the fluctuation of the liquid level of the coagulation bath in the present invention. FIG. 3 is a schematic perspective view showing an example of an embodiment of the present invention using a flow straightening tube. In this way, the flow straightening tube has a thread flowing down between a die and a direction changing guide in a coagulation bath. It is preferable to install it so as to surround it at an appropriate distance.

【0023】かかる整流筒の材質としては、凝固浴液に
対して耐腐食性があり、溶解したり膨潤したりせず、そ
の形状を長期間維持できるものが好ましい。具体的に
は、室温での水との接触角が75度以下であるものが良
く、好ましくは50度以下、より好ましくは20度以下
であるものが良い。かかる接触角が75度を越えると凝
固浴液中に存在する微小気泡が整流筒の表面に付着し易
くなり、数mm大に成長後、凝固浴液面に浮上すること
により、凝固浴液面変動の原因となることがある。ま
た、整流筒の材質が、前記接触角において75度を越え
るものであっても、その表面を接触角が75度以下にな
るように、一般的に使用されているコーティング法など
により、適宜処理すれば良い。材質は前記要件を満たす
ようなものであれば、ステンレスに代表される金属、ポ
リ塩化ビニル、ポリカボーネートに代表されるプラスチ
ックなどその材質は限定されない。なお、かかる接触角
は5度程度であれば、本発明の効果を奏するに当たり十
分である。
The material of the flow regulating tube is preferably a material which has corrosion resistance to the coagulation bath solution, does not dissolve or swell, and can maintain its shape for a long period of time. Specifically, those having a contact angle with water at room temperature of 75 degrees or less are preferable, preferably 50 degrees or less, and more preferably 20 degrees or less. When the contact angle exceeds 75 degrees, the microbubbles present in the coagulation bath liquid tend to adhere to the surface of the rectifying cylinder, grow to a size of several mm, and then float on the coagulation bath liquid surface, thereby increasing the coagulation bath liquid surface. It may cause fluctuation. Further, even if the material of the rectifying cylinder has a contact angle exceeding 75 degrees, the surface thereof is appropriately treated by a commonly used coating method or the like so that the contact angle is 75 degrees or less. Just do it. As long as the material satisfies the above requirements, the material is not limited, such as metal typified by stainless steel, plastic typified by polyvinyl chloride and polycarbonate. It is to be noted that the contact angle of about 5 degrees is sufficient for achieving the effects of the present invention.

【0024】また、整流筒は、形状を維持するために適
度な厚みを有することが好ましい。具体的には厚みは、
8mm以下のものが良い。すなわち、厚みが8mmを越える
と、凝固浴液の流れが乱れて、凝固浴液面変動を抑制す
る効果が大きく低下する場合がある。
It is preferable that the flow regulating cylinder has an appropriate thickness in order to maintain the shape. Specifically, the thickness is
8mm or less is good. That is, when the thickness exceeds 8 mm, the flow of the coagulation bath liquid is disturbed, and the effect of suppressing the fluctuation of the coagulation bath liquid level may be greatly reduced.

【0025】かかる整流筒は、その上端部が凝固浴液面
から、好ましくは10mm以上200mm以下、より好まし
くは50mm以上150mm以下の距離を置いて配置されて
いるのが良い。整流筒の上端部と凝固浴液面との距離が
10mmより小さくなると、整流筒上部からの浴液の供給
が不十分となり易く、得られる凝固糸に凝固斑が発生す
ることがあり、整流筒の上端部と凝固浴液面との距離が
200mmより大きくなると凝固浴液面変動を抑制する効
果が著しく低下することがある。
[0025] The straightening cylinder is preferably arranged such that its upper end is spaced from the liquid surface of the coagulation bath by preferably 10 mm or more and 200 mm or less, more preferably 50 mm or more and 150 mm or less. If the distance between the upper end of the flow control cylinder and the surface of the coagulation bath liquid is smaller than 10 mm, the supply of the bath liquid from the upper part of the flow control cylinder is likely to be insufficient, and the obtained coagulated yarn may have coagulation spots. When the distance between the upper end of the liquid and the liquid level of the coagulation bath is larger than 200 mm, the effect of suppressing the fluctuation of the liquid level of the coagulation bath may be remarkably reduced.

【0026】また、整流筒の下端部と浴中に設置される
方向転換ガイドとの距離は100mm以上離すのが好まし
い。100mm未満であると、整流筒を通して排出された
凝固浴液が、方向転換ガイドにより糸道が変更された糸
条に糸道に対して有る角度を持って衝突し、単糸同士が
擦過されて、得られる繊維の品位の低下を引き起こすこ
とがある。
It is preferable that the distance between the lower end of the rectifying cylinder and the direction changing guide installed in the bath is 100 mm or more. If it is less than 100 mm, the coagulating bath liquid discharged through the straightening cylinder collides with the yarn whose yarn path has been changed by the direction change guide at an angle with respect to the yarn path, and the single yarns are rubbed against each other. In some cases, the quality of the obtained fiber may be degraded.

【0027】かかる整流筒は、その断面の形状は、円
形、楕円形、矩形、多角形などいずれでも良いが、流下
する糸条の断面形状に近似する円形、又は楕円形である
と凝固浴液面変動を抑制する効果が高まるため好まし
い。
The straightening cylinder may have a cross-sectional shape of any of a circle, an ellipse, a rectangle, a polygon, and the like. This is preferable because the effect of suppressing surface fluctuation increases.

【0028】また、整流筒において、糸条の流下方向に
おける断面形状としては、流下する糸条の流下方向にお
ける断面形状に近似させて、整流筒の側面と流下する糸
条との最短距離が2mm以上50mm以下になるよう、円錐
台状、又は楕円錐台状にすることが好ましい。整流筒の
側面と流下する糸条との最短距離が2mm未満であると、
単糸が整流筒で擦過されて得られる繊維の品位の低下を
引き起こすことがあり、50mmを越えると凝固浴液面変
動を抑制する効果が著しく低下することがある。ここ
で、整流筒は、その上端部の断面形状と下端部の断面形
状が異なる変則的な円錘台状であっても良い。
Further, in the straightening cylinder, the shortest distance between the side surface of the straightening cylinder and the flowing yarn is 2 mm by approximating the cross-sectional shape of the flowing yarn in the flowing direction in the flow direction. It is preferable to make the shape of a truncated cone or an elliptical truncated cone so as to be at least 50 mm or less. If the shortest distance between the side surface of the straightening cylinder and the flowing yarn is less than 2 mm,
When the single yarn is rubbed with the rectifying cylinder, the quality of the obtained fiber may be deteriorated, and when it exceeds 50 mm, the effect of suppressing the fluctuation in the liquid level of the coagulation bath may be significantly reduced. Here, the flow regulating cylinder may have an irregular truncated cone shape in which the cross-sectional shape of the upper end portion and the cross-sectional shape of the lower end portion are different.

【0029】整流筒には、図4に示すように、開孔率が
0.02以上0.50以下になるように孔を穿孔して、
随伴液流がその側面から外部に逃散させるようにしたも
のが好ましい。ここでいう開孔率とは、整流筒の側面に
穿孔された孔の面積の総和を該側面の全表面積で除した
値を指す。孔を穿孔しなかったり、開孔率が0.01と
いうような、開孔率が不充分な場合は、随伴液流が凝固
浴液面に湧き上がり、凝固浴液面変動が大きくなること
がある。一方、開孔率が0.50より大きいと、凝固浴
液面の変動を抑制する効果が著しく低下することがあ
る。また、かかる孔の形状としては、円形、楕円形、矩
形などいずれの形状でも良く、また、形状や面積は均一
でも不均一であっても良いが、単糸が孔のエッジ部で擦
過されて品位の低下を引き起こさないように、孔のエッ
ジ部は十分角落ちされ、有る程度丸みを有した形状のも
のが良い。
As shown in FIG. 4, holes are drilled in the flow regulating cylinder so that the opening ratio is 0.02 or more and 0.50 or less.
It is preferable that the accompanying liquid flow is allowed to escape from the side surface to the outside. The aperture ratio here refers to a value obtained by dividing the total area of the holes formed in the side surface of the flow regulating cylinder by the total surface area of the side surface. If holes are not drilled or the porosity is insufficient, such as 0.01, the accompanying liquid flow may spring up to the liquid surface of the coagulation bath, and the fluctuation in the liquid surface of the coagulation bath may increase. is there. On the other hand, if the porosity is larger than 0.50, the effect of suppressing fluctuations in the liquid level of the coagulation bath may be significantly reduced. The shape of the hole may be any shape such as a circle, an ellipse, and a rectangle.The shape and area may be uniform or non-uniform, but the single yarn is rubbed at the edge of the hole. The edge portion of the hole is desirably cut off at a sufficient angle so that the quality is not deteriorated, and a shape having a roundness to some extent is preferable.

【0030】[0030]

【実施例】以下、本発明を実施例によりさらに詳細に説
明する。
The present invention will be described in more detail with reference to the following examples.

【0031】実施例中の凝固浴液面変動は、レーザー法
により10分間測定し、凝固浴液面変動幅と凝固浴液面
変動振動数を求めた。また、得られる繊維の品位の目安
として、二次延伸時に走行する糸条の毛羽の個数を目視
により10分間観察し、1000mあたりの値に換算し
たものを利用した。
The liquid level fluctuation of the coagulating bath in the examples was measured for 10 minutes by a laser method, and the fluctuation width of the liquid level of the coagulating bath and the frequency of the liquid level fluctuation of the coagulating bath were obtained. Further, as a standard of the quality of the obtained fiber, the number of fluffs of the yarn running at the time of secondary drawing was visually observed for 10 minutes, and the value converted to a value per 1000 m was used.

【0032】なお、実施例においては、オムロン株式会
社製、3Z4M-J12レーザ変位計(50μmタイフ゜)を使用し、
凝固浴液面上に白色の平板状の浮遊物(厚み5mm)を
浮かべ、波長780nm、応答速度1msecにて、その
変位量を測定することによって凝固浴液面変動とした。 比較例1 凝固浴液として20℃に温調された20重量%DMSO
水溶液を用い、紡糸原液としてAN99モル%、イタコ
ン酸1モル%からなるAN共重合体を20重量%含むジ
メチルスルホキシド溶液を用い、1錘当たりの孔数10
00、2000、3000、4000ホールの口金を用
い、図5に示すような、凝固浴槽の横壁面間の距離が6
00mm、浴中の方向転換ガイドと凝固浴槽底面との距
離が300mmの乾湿式紡糸装置でエアギャップ5mmと
して、凝固紡糸速度10m/分、20m/分でそれぞれ
紡糸し、次いで、常法どおり、水洗、一次延伸、油剤付
与、乾燥緻密化、二次延伸を行った。この際の凝固浴液
面変動と繊維の品位すなわち二次延伸時に測定した、走
行する糸条の毛羽数を表1に示す。 実施例1 図2に示すように、口金の周囲に50メッシュのステン
レス製の金網を設置した以外は、比較例1と同様にし
て、1錘当たりの孔数1000ホールの口金を用い、凝
固紡糸速度10m/分で紡糸し、凝固浴液面変動と二次
延伸時の走行する糸条の毛羽数を測定した。その結果を
表1に示す。 比較例2 図2に示すような、口金の周囲に50メッシュのステン
レス製の金網を設置した以外は、比較例1と同様にし
て、1錘当たりの孔数1000ホールの口金を用い、凝
固紡糸速度20m/分で紡糸し、凝固浴液面変動と二次
延伸時に走行する糸条の毛羽数を測定した。さらに、1
錘当たりの孔数2000、3000、4000ホールの
口金を用い、凝固紡糸速度10m/分、20m/分でそ
れぞれ紡糸し、凝固浴液面変動と二次延伸時に走行する
糸条の毛羽数を測定した。その結果を表1に示す。 実施例2 凝固浴槽の横壁面間の距離を1000mmとして凝固浴
槽を拡張した以外は、比較例1と同様にして、1錘当た
りの孔数3000ホールの口金を用い、凝固紡糸速度1
0m/分、20m/分でそれぞれ紡糸し、凝固浴液面変
動と二次延伸時に走行する糸条の毛羽数を測定した。そ
の結果を表1に示す。 実施例3 凝固浴槽の横壁面間の距離を600mm、浴中の方向転
換ガイドと凝固浴槽底面との距離を600mmとして凝
固浴槽を拡張した以外は、実施例2と同様にして、凝固
紡糸速度10m/分、20m/分でそれぞれ紡糸し、凝
固浴液面変動と二次延伸時に走行する糸条の毛羽数を測
定した。その結果を表1に示す。 実施例4 整流筒側面の孔の開孔率が0.10で、整流筒の側面と
流下する糸条との最短距離が1、2、25、50mmであ
る、室温での水との接触角が60度のステンレスを材質
とする図4に示すような円錐台状の整流筒を、図3に示
すように、口金と浴中の方向転換ガイドの間に、整流筒
の上端部と凝固浴液面との距離が100mm、整流筒の下
端部と浴中の方向転換ガイドとの距離が200mmになる
ように配置した以外は、比較例1と同様にして、凝固浴
液面変動と二次延伸時に走行する糸条の毛羽数を測定し
た。その結果を表2に示す。 比較例3 整流筒の側面と流下する糸条との最短距離が75mmであ
る、室温での水との接触角が60度のステンレスを材質
とする図4に示すような円錐台状の整流筒を使用した以
外は、実施例4と同様にして、凝固浴液面変動と二次延
伸時に走行する糸条の毛羽数を測定した。その結果を表
2に示す。 実施例5 整流筒側面の孔の開孔率が0.10で、整流筒の側面と
流下する糸条との最短距離が25mmである、室温での水
との接触角が60度のステンレスを材質とする図6に示
すような円柱状の整流筒を、口金と浴中の方向転換ガイ
ドの間に、整流筒の上端部と凝固浴液面との距離が10
0mm、整流筒の下端部と浴中の方向転換ガイドとの距離
が200mmになるように配置した以外は、比較例1と同
様にして、凝固浴液面変動と二次延伸時に走行する糸条
の毛羽数を測定した。その結果を表2に示す。 実施例6 整流筒側面の孔の開孔率が0.10で、整流筒の側面と
流下する糸条との最短距離が25mmである、室温での水
との接触角が60度のステンレスを材質とする図6に示
すような円錐台状の整流筒を、口金と浴中の方向転換ガ
イドの間に、整流筒の上端部と凝固浴液面との距離が5
0、100、200mmになるように配置した以外は、実
施例4と同様にして、凝固浴液面変動と二次延伸時に走
行する糸条の毛羽数を測定した。その結果を表2に示
す。 比較例4 整流筒の上端部と凝固浴液面との距離が5、300mmに
なるように配置した以外は、実施例6と同様にして、凝
固浴液面変動と二次延伸時に走行する糸条の毛羽数を測
定した。その結果を表2に示す。 実施例7 整流筒側面の孔の開孔率が0.02、0.10、0.5
0、整流筒の側面と流下する糸条との最短距離が25mm
である、室温での水との接触角が60度のステンレスを
材質とする図6に示すような円錐台状の整流筒を、口金
と浴中の方向転換ガイドの間に、整流筒の上端部と凝固
浴液面との距離が100mm、整流筒の下端部と浴中の方
向転換ガイドとの距離が200mmになるように配置した
以外は実施例4と同様にして、凝固浴液面変動と二次延
伸時に走行する糸条の毛羽数を測定した。その結果を表
3に示す。 比較例5 整流筒側面の孔の開孔率が0.00、0.01、0.7
5の整流筒を配置した以外は実施例7と同様にして、凝
固浴液面変動と二次延伸時に走行する糸条の毛羽数を測
定した。その結果を表3に示す。 比較例6 整流筒側面の孔の開孔率が0.10で、整流筒の側面と
流下する糸条との最短距離が25mmである、室温での水
との接触角が80度のポリ塩化ビニルを材質とする図6
に示すような円錐台状の整流筒を、口金と浴中の方向転
換ガイドの間に、整流筒の上端部と凝固浴液面との距離
が100mmになるように配置した以外は実施例4と同様
にして、凝固浴液面変動と二次延伸時に走行する糸条の
毛羽数を測定した。その結果を表3に示す。 実施例8 室温での水との接触角が25度のステンレスを材質とす
る図6に示すような円錐台状の整流筒を使用した以外
は、比較例6と同様にして、凝固浴液面変動と二次延伸
時に走行する糸条の毛羽数を測定した。その結果を表3
に示す。 実施例9 室温での水との接触角が80度のポリ塩化ビニルを材質
とする図6に示すような円錐台状の整流筒に、かかる接
触角が15度になるように親水化表面処理を施した以外
は、比較例6と同様にして、凝固浴液面変動と二次延伸
時に走行する糸条の毛羽数を測定した。その結果を表3
に示す。
In the examples, a 3Z4M-J12 laser displacement meter (50 μm type) manufactured by OMRON Corporation was used.
A white, plate-like floating substance (thickness: 5 mm) was floated on the liquid surface of the coagulation bath, and its displacement was measured at a wavelength of 780 nm and a response speed of 1 msec to determine the fluctuation of the coagulation bath liquid surface. Comparative Example 1 20 wt% DMSO temperature-controlled at 20 ° C. as a coagulation bath solution
Using an aqueous solution, a dimethylsulfoxide solution containing 20% by weight of an AN copolymer composed of 99 mol% of AN and 1 mol% of itaconic acid was used as a spinning solution, and the number of holes per spindle was 10
The distance between the lateral wall surfaces of the coagulation bath was 6 as shown in FIG.
Spinning at a coagulation spinning speed of 10 m / min and 20 m / min with an air gap of 5 mm using a dry / wet spinning device with a distance of 300 mm between the direction changing guide in the bath and the bottom of the coagulation bath, and then washing with water as usual. , Primary stretching, oil application, dry densification, and secondary stretching. Table 1 shows the fluctuation of the liquid level of the coagulating bath and the quality of the fibers, that is, the number of fluffs of the running yarn measured at the time of the second drawing. Example 1 As shown in FIG. 2, solidification spinning was performed using a die having 1,000 holes per weight in the same manner as in Comparative Example 1 except that a 50-mesh stainless steel wire mesh was provided around the die. The yarn was spun at a speed of 10 m / min, and the fluctuation in the liquid level of the coagulation bath and the number of fluffs of the running yarn during the secondary stretching were measured. Table 1 shows the results. Comparative Example 2 Coagulation spinning was performed in the same manner as in Comparative Example 1, except that a 50-mesh stainless steel wire mesh was installed around the die as shown in FIG. The yarn was spun at a speed of 20 m / min, and the fluctuation of the liquid level in the coagulation bath and the number of fluffs of the yarn running during the secondary stretching were measured. In addition, 1
Spinning at a coagulation spinning speed of 10 m / min and 20 m / min, respectively, using a spinneret with 2,000, 3,000, and 4,000 holes per weight, and measuring the fluctuation of the coagulation bath liquid level and the number of fluffs of the yarn running during secondary stretching. did. Table 1 shows the results. Example 2 In the same manner as in Comparative Example 1, except that the distance between the horizontal wall surfaces of the coagulation bath was set to 1000 mm and the coagulation bath was expanded, a solidification spinning speed of 1 was used using a die having 3000 holes per weight.
Spinning was performed at 0 m / min and 20 m / min, respectively, and the fluctuation in the liquid level of the coagulation bath and the number of fluffs of the yarn running during the secondary stretching were measured. Table 1 shows the results. Example 3 The coagulation spinning speed was 10 m in the same manner as in Example 2, except that the distance between the lateral wall surfaces of the coagulation bath was 600 mm, and the distance between the direction change guide in the bath and the bottom of the coagulation bath was 600 mm, and the coagulation bath was expanded. / Min and 20 m / min, respectively, and the fluctuation of the liquid level of the coagulation bath and the number of fluffs of the running yarn during the secondary stretching were measured. Table 1 shows the results. Example 4 A contact angle with water at room temperature, in which the opening ratio of the hole on the side of the flow regulating cylinder is 0.10 and the shortest distance between the side surface of the flow regulating cylinder and the flowing yarn is 1, 2, 25, and 50 mm. As shown in FIG. 3, the upper end of the rectifying cylinder and the coagulating bath are interposed between the base and the direction changing guide in the bath as shown in FIG. Except that the distance from the liquid level was 100 mm, and the distance between the lower end of the rectifying cylinder and the direction change guide in the bath was 200 mm, the liquid level fluctuation of the coagulation bath and the secondary The number of fluffs of the running yarn during drawing was measured. Table 2 shows the results. Comparative Example 3 A frustum-shaped conical rectifying cylinder as shown in FIG. 4 made of stainless steel having a shortest distance between the side surface of the rectifying cylinder and the flowing yarn of 75 mm and a contact angle with water at room temperature of 60 degrees. In the same manner as in Example 4, except for using, the fluctuation of the liquid level of the coagulating bath and the number of fluffs of the yarn running during the secondary stretching were measured. Table 2 shows the results. Example 5 Stainless steel having a contact angle with water at room temperature of 60 degrees at room temperature, in which the opening ratio of the hole on the side of the flow regulating cylinder is 0.10, the shortest distance between the side surface of the flow regulating cylinder and the flowing yarn is 25 mm, and As shown in FIG. 6, the distance between the upper end of the flow regulating cylinder and the liquid level of the coagulation bath is 10 mm between the base and the direction changing guide in the bath.
0 mm, the same as in Comparative Example 1, except that the distance between the lower end of the rectifying cylinder and the direction-changing guide in the bath was 200 mm. The number of fluff was measured. Table 2 shows the results. Example 6 A stainless steel having a contact angle with water at room temperature of 60 degrees at room temperature, in which the opening ratio of the hole on the side of the flow regulating cylinder is 0.10, the shortest distance between the side surface of the flow regulating cylinder and the flowing yarn is 25 mm, A straight truncated conical rectifying cylinder as shown in FIG. 6 made of a material is placed between the base and the direction changing guide in the bath, and the distance between the upper end of the rectifying cylinder and the liquid level of the coagulating bath is 5 mm.
Fluctuations in the liquid level of the coagulation bath and the number of fluffs of the yarn running during the secondary stretching were measured in the same manner as in Example 4 except that the yarns were arranged so as to be 0, 100, and 200 mm. Table 2 shows the results. Comparative Example 4 Coagulation bath liquid level fluctuation and yarn running at the time of secondary stretching were carried out in the same manner as in Example 6, except that the distance between the upper end of the rectifying cylinder and the coagulation bath liquid level was arranged to be 5,300 mm. The number of fuzz on the strip was measured. Table 2 shows the results. Example 7 The opening ratio of the hole on the side surface of the flow regulating cylinder was 0.02, 0.10, 0.5.
0, the shortest distance between the side surface of the straightening cylinder and the flowing yarn is 25 mm
A straight truncated conical rectifying cylinder as shown in FIG. 6 made of stainless steel having a contact angle of 60 degrees with water at room temperature is placed between the base and the direction changing guide in the bath. Coagulation bath liquid level fluctuation in the same manner as in Example 4 except that the distance between the portion and the coagulation bath liquid surface was 100 mm, and the distance between the lower end of the flow straightening tube and the direction change guide in the bath was 200 mm. And the number of fluffs of the yarn running during the secondary stretching was measured. Table 3 shows the results. Comparative Example 5 The opening ratio of the hole on the side surface of the flow regulating cylinder was 0.00, 0.01, 0.7
In the same manner as in Example 7 except that the rectifying cylinder No. 5 was arranged, the fluctuation of the liquid level of the coagulation bath and the number of fluffs of the yarn running during the secondary stretching were measured. Table 3 shows the results. Comparative Example 6 Polychlorinated water with a contact angle of 80 degrees at room temperature with water at room temperature in which the opening ratio of the hole on the side of the flow regulating cylinder is 0.10, the shortest distance between the side surface of the flow regulating cylinder and the flowing yarn is 25 mm. Figure 6 made of vinyl
Example 4 except that a truncated conical rectifying cylinder as shown in Fig. 7 was arranged between the base and the direction changing guide in the bath so that the distance between the upper end of the rectifying cylinder and the liquid level of the coagulating bath was 100 mm. In the same manner as in the above, the fluctuation of the liquid level of the coagulation bath and the number of fluffs of the yarn running during the secondary stretching were measured. Table 3 shows the results. Example 8 The liquid level of the coagulation bath was the same as in Comparative Example 6, except that a frustoconical rectifying cylinder as shown in FIG. 6 made of stainless steel having a contact angle of 25 degrees with water at room temperature was used. The fluctuation and the number of fluffs of the running yarn during the secondary drawing were measured. Table 3 shows the results.
Shown in Example 9 Hydrophilic surface treatment was performed on a frusto-conical rectifying cylinder made of polyvinyl chloride having a contact angle with water of 80 degrees at room temperature as shown in FIG. 6 so that the contact angle became 15 degrees. In the same manner as in Comparative Example 6, except that the coating was performed, the fluctuation in the liquid level of the coagulating bath and the number of fluffs of the yarn running during the secondary stretching were measured. Table 3 shows the results.
Shown in

【0033】[0033]

【表1】 [Table 1]

【0034】[0034]

【表2】 [Table 2]

【0035】[0035]

【表3】 [Table 3]

【0036】表1〜3に示す結果から、凝固浴液面変動
指数を0.05mm/sec 以下に定量指標化し、凝固浴液
面の状態をかかる範囲とすることにより、得られる繊維
の品位を著しく高めることができる。また、整流筒を凝
固浴槽内に設置することによりかかる凝固浴液面変動指
数を適切に制御できることが分かる。
From the results shown in Tables 1 to 3, the coagulation bath liquid level fluctuation index was quantitatively indexed to 0.05 mm / sec or less, and by setting the coagulation bath liquid surface state to the above range, the quality of the obtained fiber was reduced. Can be significantly increased. In addition, it can be seen that the coagulation bath liquid level fluctuation index can be appropriately controlled by installing the rectification cylinder in the coagulation bath.

【0037】[0037]

【発明の効果】本発明によれば、凝固浴液面変動の状態
を適切に定量指標化することにより、口金1錘当たりの
孔数を増加したり、紡糸する糸条の速度を増大するなど
繊維の品質を低下させる状況においても、品位に優れた
アクリル系繊維を、安定して効率よく製造することがで
きる。
According to the present invention, the number of holes per spinneret can be increased, and the speed of the yarn to be spun can be increased by appropriately quantifying the state of the liquid level fluctuation in the coagulation bath. Even in a situation where the quality of the fiber is deteriorated, it is possible to stably and efficiently produce an acrylic fiber having excellent quality.

【図面の簡単な説明】[Brief description of the drawings]

【図1】凝固浴液面変動の測定結果の一例を示す図であ
る。
FIG. 1 is a diagram showing an example of a measurement result of a coagulation bath liquid level fluctuation.

【図2】本発明による乾湿式紡糸装置を示す概略斜視図
である。
FIG. 2 is a schematic perspective view showing a dry-wet spinning apparatus according to the present invention.

【図3】本発明による乾湿式紡糸装置の別の実施態様を
示す概略斜視図である。
FIG. 3 is a schematic perspective view showing another embodiment of the dry-wet spinning apparatus according to the present invention.

【図4】本発明による整流筒の実施態様を示す概略斜視
図である。
FIG. 4 is a schematic perspective view showing an embodiment of a flow regulating cylinder according to the present invention.

【図5】従来の乾湿式紡糸装置を示す概略斜視図であ
る。
FIG. 5 is a schematic perspective view showing a conventional dry-wet spinning apparatus.

【図6】円柱状の形状を有する整流筒を示す概略斜視図
である。
FIG. 6 is a schematic perspective view showing a rectifying cylinder having a columnar shape.

【符号の説明】[Explanation of symbols]

1:口金 2:液面変位測定器 3:整流金網 4:(糸条の)方向転換ガイド 5:凝固浴液面 6:凝固糸条 7:糸条進行方向 8:凝固浴槽 9:整流筒 10:孔 1: Cap 2: Liquid level displacement measuring device 3: Rectifying wire net 4: Direction change guide (of yarn) 5: Coagulation bath liquid surface 6: Coagulation yarn 7: Yarn traveling direction 8: Coagulation bath tank 9: Rectification cylinder 10 : Hole

Claims (12)

【特許請求の範囲】[Claims] 【請求項1】 口金から吐出されたポリマー溶液を一旦
エアギャップを通過させて凝固浴槽に導く乾湿式紡糸法
において、下記に示す凝固浴液面変動指数を0.05mm
/sec 以下に保ちながら紡糸することを特徴とするアク
リル系繊維の製造方法。 凝固浴液面変動指数=凝固浴液面変動幅×凝固浴液面変
動振動数 式中:凝固浴液面変動指数(単位;mm/sec ) 凝固浴液面変動幅(単位;mm):10分間の凝固浴液面
の相対位置の最大変動幅 凝固浴液面振動数(単位;Hz):1秒間の凝固浴液面
変動の極大値のの数
In a dry-wet spinning method in which a polymer solution discharged from a die is once passed through an air gap and introduced into a coagulation bath, a coagulation bath liquid surface fluctuation index shown below is 0.05 mm.
A method for producing an acrylic fiber, wherein the fiber is spun while keeping the pressure at or below / sec. Coagulation bath liquid level fluctuation index = coagulation bath liquid level fluctuation width x coagulation bath liquid level fluctuation frequency In the formula: coagulation bath liquid level fluctuation index (unit: mm / sec) Coagulation bath liquid level fluctuation width (unit; mm): 10 Maximum fluctuation width of the relative position of the coagulation bath liquid level for one minute Coagulation bath liquid surface frequency (unit: Hz): Number of maximum values of coagulation bath liquid surface fluctuation for one second
【請求項2】 該凝固浴液面変動指数を0.05mm/se
c 以下に抑制する方法が、凝固液表面において、口金の
周囲に金網を設置する方法である請求項1記載のアクリ
ル系繊維の製造方法。
2. The coagulation bath liquid level fluctuation index is 0.05 mm / se.
c The method for producing an acrylic fiber according to claim 1, wherein the method for suppressing the following is a method of installing a wire mesh around the die on the surface of the coagulating liquid.
【請求項3】 該凝固浴液面変動指数を0.05mm/se
c 以下に抑制する方法が、該凝固浴槽を深さ方向又は錘
間方向の少なくとも一方を拡張する方法である請求項1
記載のアクリル系繊維の製造方法。
3. The liquid level variation index of the coagulation bath is 0.05 mm / se.
c The method of controlling the coagulation bath in at least one of the depth direction and the inter-weight direction is a method for suppressing the coagulation bath below.
The method for producing an acrylic fiber according to the above.
【請求項4】 該凝固浴液面変動指数を0.05mm/se
c 以下に抑制する方法が、口金と凝固浴槽中の方向転換
ガイドの間に整流筒を設置する方法である請求項1記載
のアクリル系繊維の製造方法。
4. The liquid level fluctuation index of the coagulation bath is 0.05 mm / se.
c The method for producing acrylic fibers according to claim 1, wherein the method of suppressing the following is a method of installing a flow straightening tube between the mouthpiece and the direction changing guide in the coagulation bath.
【請求項5】 該整流筒の形状が、円錐台状である請求
項4記載のアクリル系繊維の製造方法。
5. The method for producing an acrylic fiber according to claim 4, wherein the shape of the flow regulating cylinder is a truncated cone.
【請求項6】 該整流筒が、該整流筒内を流下する糸条
と該整流筒の側面との最短距離が2mm以上50mm以下と
なる位置に配置されている請求項4又は5記載のアクリ
ル系繊維の製造方法。
6. The acrylic according to claim 4, wherein the straightening tube is arranged at a position where a shortest distance between a yarn flowing down the straightening tube and a side surface of the straightening tube is 2 mm or more and 50 mm or less. Method for producing base fiber.
【請求項7】 該整流筒が、その側面に孔を有するもの
である請求項4〜6のいずれかに記載のアクリル系繊維
の製造方法。
7. The method for producing an acrylic fiber according to claim 4, wherein the flow regulating cylinder has a hole on a side surface thereof.
【請求項8】 該整流筒の側面に穿孔された孔の開孔率
が、0.02以上0.50以下の範囲である請求項7記
載のアクリル系繊維の製造方法。
8. The method for producing an acrylic fiber according to claim 7, wherein the porosity of the holes formed in the side surface of the flow regulating cylinder is in the range of 0.02 to 0.50.
【請求項9】 該整流筒が、その上端部が凝固浴液面か
ら10mm以上200mm以下の位置になるよう配置されて
いる請求項4〜8のいずれかに記載のアクリル系繊維の
製造方法。
9. The method for producing an acrylic fiber according to claim 4, wherein the straightening cylinder is disposed so that an upper end thereof is at a position of 10 mm or more and 200 mm or less from the liquid level of the coagulation bath.
【請求項10】 該整流筒が、その表面における、室温
での水との接触角が75度以下である請求項4〜9のい
ずれかに記載のアクリル系繊維の製造方法。
10. The method for producing acrylic fibers according to claim 4, wherein the surface of the flow regulating cylinder has a contact angle with water at room temperature of 75 degrees or less.
【請求項11】 該口金が、1錘当たりに2000以上
の孔数を有するものである請求項1〜10のいずれかに
記載のアクリル系繊維の製造方法。
11. The method for producing an acrylic fiber according to claim 1, wherein the die has a number of holes of 2000 or more per weight.
【請求項12】 該凝固浴槽中の糸条の走行速度が、1
0m/分以上である請求項1〜11のいずれかに記載の
アクリル系繊維の製造方法。
12. The running speed of the yarn in the coagulation bath is 1
The method for producing an acrylic fiber according to any one of claims 1 to 11, which is at least 0 m / min.
JP8108399A 1998-03-31 1999-03-25 Production of acrylic fiber Pending JPH11350244A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP8108399A JPH11350244A (en) 1998-03-31 1999-03-25 Production of acrylic fiber

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP10-87180 1998-03-31
JP8718098 1998-03-31
JP8108399A JPH11350244A (en) 1998-03-31 1999-03-25 Production of acrylic fiber

Publications (1)

Publication Number Publication Date
JPH11350244A true JPH11350244A (en) 1999-12-21

Family

ID=26422121

Family Applications (1)

Application Number Title Priority Date Filing Date
JP8108399A Pending JPH11350244A (en) 1998-03-31 1999-03-25 Production of acrylic fiber

Country Status (1)

Country Link
JP (1) JPH11350244A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006001324A1 (en) 2004-06-25 2006-01-05 Toray Industries, Inc. Spinning pack for dry-wet spinning, diverting guide for fiber bundle, and apparatus and method for producing fiber bundle
JP2007239170A (en) * 2006-02-07 2007-09-20 Toray Ind Inc Method for producing fiber
JP2007291594A (en) * 2006-03-27 2007-11-08 Toray Ind Inc Method for producing acrylic fiber bundle
KR101167452B1 (en) 2010-12-30 2012-07-20 주식회사 효성 An Appratus For Making Carbon Fiber Precursor And A Method Using The Same
WO2013047437A1 (en) * 2011-09-26 2013-04-04 三菱レイヨン株式会社 Dry-wet spinning device and method for manufacturing synthetic fiber
KR101401215B1 (en) * 2013-01-28 2014-05-28 주식회사 효성 Apparatus for coagulating doped solution of polyacrylonitrile precursor for a carbon fiber
CN105350091A (en) * 2015-11-25 2016-02-24 山东大学 Dry-jet wet-spinning jetting device and making method thereof

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006001324A1 (en) 2004-06-25 2006-01-05 Toray Industries, Inc. Spinning pack for dry-wet spinning, diverting guide for fiber bundle, and apparatus and method for producing fiber bundle
JPWO2006001324A1 (en) * 2004-06-25 2008-04-17 東レ株式会社 Spinning pack for dry and wet spinning, fiber bundle direction changing guide, and fiber bundle manufacturing apparatus and method
US7887728B2 (en) 2004-06-25 2011-02-15 Toray Industries, Inc. Spinning pack for dry-wet spinning, diverting guide for fiber bundle, and apparatus and method for producing fiber bundle
JP2011063926A (en) * 2004-06-25 2011-03-31 Toray Ind Inc Spinning pack for dry-wet spinning, and apparatus for producing fiber bundle
JP4730306B2 (en) * 2004-06-25 2011-07-20 東レ株式会社 Manufacturing method of fiber bundle
JP2007239170A (en) * 2006-02-07 2007-09-20 Toray Ind Inc Method for producing fiber
JP2007291594A (en) * 2006-03-27 2007-11-08 Toray Ind Inc Method for producing acrylic fiber bundle
KR101167452B1 (en) 2010-12-30 2012-07-20 주식회사 효성 An Appratus For Making Carbon Fiber Precursor And A Method Using The Same
WO2013047437A1 (en) * 2011-09-26 2013-04-04 三菱レイヨン株式会社 Dry-wet spinning device and method for manufacturing synthetic fiber
KR20140052062A (en) * 2011-09-26 2014-05-02 미쯔비시 레이온 가부시끼가이샤 Dry-wet spinning device and method for manufacturing synthetic fiber
CN103827362A (en) * 2011-09-26 2014-05-28 三菱丽阳株式会社 Dry-wet spinning device and method for manufacturing synthetic fiber
EP2762616A4 (en) * 2011-09-26 2015-03-04 Mitsubishi Rayon Co Dry-wet spinning device and method for manufacturing synthetic fiber
JPWO2013047437A1 (en) * 2011-09-26 2015-03-26 三菱レイヨン株式会社 Synthetic fiber manufacturing method and dry-wet spinning apparatus
US9458557B2 (en) 2011-09-26 2016-10-04 Mitsubishi Rayon Co., Ltd. Method for manufacturing synthetic fiber
KR101401215B1 (en) * 2013-01-28 2014-05-28 주식회사 효성 Apparatus for coagulating doped solution of polyacrylonitrile precursor for a carbon fiber
CN105350091A (en) * 2015-11-25 2016-02-24 山东大学 Dry-jet wet-spinning jetting device and making method thereof

Similar Documents

Publication Publication Date Title
JP4968378B2 (en) Spinning pack for dry and wet spinning, and fiber bundle manufacturing equipment
KR101216901B1 (en) Wet spinning apparatus and method for wet spinning
JPH11350244A (en) Production of acrylic fiber
JP4856566B2 (en) Wet spinning apparatus and wet spinning method
JP5001673B2 (en) Wet spinning apparatus and wet spinning method
JP2015040360A (en) Wet spinning apparatus and method of producing fiber
JP2007291594A (en) Method for producing acrylic fiber bundle
JPH0967714A (en) Wet spinning unit
JP2006118087A (en) Dry and wet type spinning device
JPH07207522A (en) Spinning method of acrylonitrile type fiber and its apparatus
JP3704855B2 (en) Horizontal wet coagulation bath and wet spinning method using the coagulation bath
JP2002294518A (en) Carbon fiber precursor acrylonitrile-based yarn and method for producing the same
JPH0823083B2 (en) Acrylic fiber manufacturing method
JPS6065110A (en) Production of poly-p-phenylene terephthalamide fiber
JPH0341561B2 (en)
JP2891115B2 (en) Dry-wet spinning apparatus and dry-wet spinning method
JPH01250406A (en) Production of high-tenacity fiber
JP2005220508A (en) Method for wet spinning and device for the same
JP2016132847A (en) Manufacturing method of fiber bundle, polyacrylonitrile fiber bundle and carbon fiber bundle
JPH0219508A (en) Spinning column of natural suction type of bath solution
JP3358369B2 (en) Dry-wet spinning guide and dry-wet spinning method
JPH08260223A (en) Preparation of fiber
JP2011168895A (en) Method for producing acrylic fiber
JPS62141111A (en) Dry jet-wet spinning
JP2001329426A (en) Method for producing acrylic fiber and apparatus therefor

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20040906

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20060216

A131 Notification of reasons for refusal

Effective date: 20060228

Free format text: JAPANESE INTERMEDIATE CODE: A131

A02 Decision of refusal

Free format text: JAPANESE INTERMEDIATE CODE: A02

Effective date: 20070410