JP2006336152A - Dry-wet spinning apparatus - Google Patents

Dry-wet spinning apparatus Download PDF

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JP2006336152A
JP2006336152A JP2005162597A JP2005162597A JP2006336152A JP 2006336152 A JP2006336152 A JP 2006336152A JP 2005162597 A JP2005162597 A JP 2005162597A JP 2005162597 A JP2005162597 A JP 2005162597A JP 2006336152 A JP2006336152 A JP 2006336152A
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JP4593370B2 (en
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Yasushi Kitagishi
泰 北岸
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Teijin Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide an apparatus capable of producing a fiber having stabilized performances free from dispersion of quality while raising productivity in dry and wet type spinning. <P>SOLUTION: The dry-wet spinning apparatus comprises a coagulating bath 2a, a spinneret 1 in which many spinning hole groups arranged at a fixed air gap G from a liquid level S in which a coagulating liquid L packed in the coagulating bath 2a is formed are bored, a flow pipe 3 installed in a state immersed in the coagulating liquid L and a take-off means 4 of yarn installed below the flow pipe 3. In the dry-wet spinning apparatus, the flow pipe 3 has a funnel-shaped bent pipe part 3a formed in a state spreading toward the upstream side in which the coagulating liquid L flows and a cylindrical straight pipe part 3b provided in the lower part of the bent pipe part 3a and the flow pipe 3 is equipped with a flow rate regulator 5 for feeding the coagulating liquid from all round directions without reducing inside diameter of pipe of the straight pipe part 3b in succession to the straight pipe part 3b and controls flow rate and flow amount of the coagulating liquid which flows down through the flow pipe 3 by a coagulating liquid fed from the flow rate regulator 5. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、多数の紡糸孔が穿設された紡糸口金より紡糸ドープを一旦空気中に紡出した後に、紡出したドープを凝固浴中へ導入して繊維化する乾湿式紡糸装置に関する。   The present invention relates to a dry-wet spinning apparatus in which a spinning dope is once spun into air from a spinneret having a large number of spinning holes, and then the spun dope is introduced into a coagulation bath to be fiberized.

高強度と高モジュラスを兼ね備えた全芳香族ポリアミド繊維を紡糸するための従来技術として、紡糸口金より全芳香族ポリアミド重合体を含むドープを一旦空気中に紡出し、紡出した前記ドープ流を凝固液中へ導入して凝固させて、繊維化することは周知である。   As a conventional technique for spinning wholly aromatic polyamide fibers having both high strength and high modulus, a dope containing a wholly aromatic polyamide polymer is once spun into the air from a spinneret and the spun dope stream is solidified. It is well known that it is introduced into a liquid and solidified to form a fiber.

しかしながら、紡出ドープをそのまま静止した凝固液中へ導入すると、凝固液から大きな通過抵抗を受けて、紡糸ドープがある速度以上になると単繊維切れを起こす。このため、紡糸ドープの紡出速度を上げることができず、紡糸速度を低速にせざるを得なかった。特に、製造する繊維の繊度が細くなればなるほど、単繊維切れが生じないように安定に紡糸するのが困難となる問題がある。   However, when the spinning dope is introduced into the stationary coagulating liquid as it is, it receives a large passage resistance from the coagulating liquid and causes a single fiber breakage when the spinning dope exceeds a certain speed. For this reason, the spinning speed of the spinning dope could not be increased, and the spinning speed had to be lowered. In particular, there is a problem that as the fineness of the fiber to be manufactured becomes thinner, it becomes more difficult to perform stable spinning so that no single fiber breakage occurs.

そこで、この問題を解決する方法として、凝固液を紡出されるドープと共に流動させて凝固液から受ける抵抗の低減を図るために、凝固液が流れる流管中に紡出ドープを導いて紡糸する技術が、例えば特開昭60−52610号公報に提案されている。確かに、この従来技術によると、流管内を流れる凝固液の流速を上げることができるが、流管内を走行する繊維の速度と流管内を流れる凝固液の流速とを一致させることが難しい。したがって、この従来技術を使用しても、単繊維切れの発生を充分に抑制するに至っていない。   Therefore, as a method for solving this problem, in order to reduce the resistance received from the coagulation liquid by causing the coagulation liquid to flow together with the dope to be spun, a technique of introducing the spinning dope into the flow tube through which the coagulation liquid flows and spinning Is proposed in, for example, Japanese Patent Laid-Open No. 60-52610. Certainly, according to this prior art, the flow velocity of the coagulating liquid flowing in the flow tube can be increased, but it is difficult to match the velocity of the fiber traveling in the flow tube with the flow velocity of the coagulating liquid flowing in the flow tube. Therefore, even if this conventional technique is used, the occurrence of single fiber breakage has not been sufficiently suppressed.

また、特開昭56−128312号公報には、紡糸口金より一旦空気中へ紡出したドープを流管へ導き、その初期段階において複数の小径ノズルあるいはスリットから凝固液を流管中へ糸条の走行方向へ噴出させて、繊維化するドープを流管中で加速して紡糸する乾湿式紡糸方法が提案されている。確かに、このような乾湿式紡糸方法を採用することによって、初期段階で凝固液を流管中へ加速導入した凝固液流の助けを借りて繊維化するドープの流下速度を加速することができ、これによって糸条に働く抵抗を低減しながら、高速紡糸を行うことが可能となる。   Japanese Patent Application Laid-Open No. 56-128312 discloses that a dope once spun into air from a spinneret is introduced into a flow tube, and in the initial stage, a coagulating liquid is fed into the flow tube from a plurality of small diameter nozzles or slits. A dry-wet spinning method has been proposed in which a dope to be fiberized is spun in a flow tube and spun in the running direction. Certainly, by adopting such a dry-wet spinning method, it is possible to accelerate the flow rate of the dope that is fiberized with the help of the coagulation liquid flow that is accelerated and introduced into the flow tube in the initial stage. This makes it possible to perform high speed spinning while reducing the resistance acting on the yarn.

しかしながら、この従来技術では、初期段階で紡出されたドープに沿って凝固液を強制推進流として流す必要があるため、未凝固のドープに対し急激な速度変化を与えてしまうことになる。そうすると、その速度変化による液抵抗の変化により単繊維切れが発生するという問題が生じる。   However, in this prior art, since it is necessary to flow the coagulation liquid as a forced propulsion flow along the dope spun in the initial stage, an abrupt speed change is given to the unsolidified dope. If it does so, the problem that a single fiber piece will generate | occur | produce by the change of the liquid resistance by the speed change will arise.

また、この従来技術には、凝固浴から流管の上部に導入される凝固液流が乱されるという問題があり、凝固液流に乱れが生じると、それによって凝固浴の液面も乱されてしまう。このように、急激な凝固液流の流速変化と凝固浴の液面の乱れが生じると、得られる繊維品質のバラツキが大きくなり、流管への導入部で単繊維切れが発生し易くなるという問題が生じる。特に、単繊維繊度が細くなればなるほど、この単繊維切れの問題はより顕著に現れる。   In addition, this conventional technique has a problem that the flow of coagulation liquid introduced from the coagulation bath to the upper part of the flow tube is disturbed, and when the coagulation liquid flow is disturbed, the liquid level of the coagulation bath is also disturbed thereby. End up. In this way, when the flow rate of the coagulation liquid flow rate changes suddenly and the liquid level of the coagulation bath is disturbed, the resulting fiber quality varies greatly, and single fiber breakage is likely to occur at the inlet to the flow tube. Problems arise. In particular, as the single fiber fineness becomes thinner, the problem of single fiber breakage becomes more prominent.

そこで、この問題を解消するために、特開昭57−106707号公報において、流管中に絞りを設け、絞りの面積を調節することにより流管内を流れる凝固液の流量(速度)を調整する方法が提案されている。確かに、この従来技術を採用すると、凝固浴の乱れが生じ難く液面も乱れ難い条件を作り出し易くなる。   In order to solve this problem, in Japanese Patent Application Laid-Open No. 57-106707, the flow rate (speed) of the coagulating liquid flowing in the flow tube is adjusted by providing a throttle in the flow tube and adjusting the area of the throttle. A method has been proposed. Certainly, when this conventional technique is adopted, it is easy to create conditions in which the coagulation bath is less likely to be disturbed and the liquid level is less likely to be disturbed.

しかしながら、流管途中に絞り部が存在すると、絞り部において急激に凝固液の流速が変化してしまい、流管内に流速差が発生して凝固途中の繊維が延伸されて物性が低下したり、単繊維切れを生じてしまうことが生じる。更に、繊維が絞り部を通過する時に、絞り部の壁面に接触するために、繊維がダメージを受ける。   However, if there is a constriction part in the middle of the flow tube, the flow rate of the coagulation liquid suddenly changes in the constriction part, a flow rate difference occurs in the flow tube, the fibers in the middle of solidification are stretched, and the physical properties decrease, A single fiber breakage may occur. Furthermore, when the fiber passes through the drawn portion, the fiber is damaged because it contacts the wall surface of the drawn portion.

特開昭60−52610号公報JP 60-52610 A 特開昭56−128312号公報JP-A-56-128312 特開昭57−106707号公報JP-A-57-106707

以上に述べた従来技術が有する諸問題に鑑み、本発明の目的は、「多数の紡糸孔が穿設された紡糸口金より紡糸ドープを一旦空気中に紡出し、凝固液を貯えた凝固浴へドープを導いて繊維化する乾湿式紡糸において、糸条を構成する単繊維及び単繊維群間の品質のバラツキの無い安定した性能を有する繊維を生産性を上げながら製造することができる装置を提供する」ことにある。   In view of the above-described problems of the prior art, the object of the present invention is to “spin the spinning dope into the air from the spinneret having a large number of spinning holes and store the coagulating liquid. In dry-wet spinning that guides the dope into fibers, we provide a device that can produce a single fiber that forms a yarn and a fiber that has stable performance without variations in quality between single fiber groups while increasing productivity. To do.

ここに、上記課題を解決する本発明として、
(1)凝固液を充填する凝固浴と、前記凝固浴に充填される前記凝固液が形成する液面と一定のエアギャップをおいて設けられた多数の紡糸孔群が穿設された紡糸口金と、前記凝固液中に浸漬させて設けられた流管と、前記流管の下方に設けられた糸条の引取手段を含む乾湿式紡糸装置において、前記流管は、その上部内壁面は凝固液が流入する上流側に向って末広がりに形成された漏斗状の曲管部を有し、その下部内壁面は筒状の直管部を有すると共に、前記直管部に引き続いて前記直管部の管内径を縮小することなく全周方向から凝固液を供給する流速調節器を備え、前記流速調節器から供給する凝固液によって流管内を流下する凝固液の流速及び流量を制御することを特徴とする乾湿式紡糸装置、
(2)前記流管の曲管部と直管部とが段差を生じずになだらかに接続されている(1)に記載の乾湿式紡糸装置、
(3)前記流速調節器が貯液部と、該貯液部から流管中に凝固液を注入供給する液注入部を備え、該液注入部が貯液部に供給された凝固液を均圧化する均圧化部材及び/又は整流した凝固液を流管を流下した凝固液に注入する整流部材を兼ねる(1)に記載の乾湿式紡糸装置、
(4)前記流速調節器の液注入部内径が下流側に向かって末広がりに錐状に形成された(3)に記載の乾湿式紡糸装置、
(5)前記液面から前記流管の上端部までの距離が2〜100mmである(1)に記載の乾湿式紡糸装置、
(6)前記流管の直管部の内径が2〜30mmである(1)に記載の乾湿式紡糸装置、そして、
(7)前記方法により得られる繊維の引取り速度が10〜300m/minである(1)に記載の乾湿式紡糸装置が提供される。
Here, as the present invention for solving the above problems,
(1) A coagulation bath filled with a coagulation liquid, and a spinneret having a plurality of spinning hole groups provided with a certain air gap from the liquid surface formed by the coagulation liquid filled in the coagulation bath And a wet and wet spinning apparatus comprising a flow tube immersed in the coagulation liquid and a yarn take-up means provided below the flow tube, wherein the flow tube has a solidified upper inner wall surface. It has a funnel-shaped curved pipe portion formed so as to widen toward the upstream side into which the liquid flows, and its lower inner wall surface has a cylindrical straight pipe portion, and the straight pipe portion following the straight pipe portion. A flow rate regulator for supplying the coagulating liquid from all around without reducing the inner diameter of the pipe, and controlling the flow rate and flow rate of the coagulating liquid flowing down in the flow tube by the coagulating liquid supplied from the flow rate regulator. Dry-wet spinning equipment,
(2) The dry and wet spinning device according to (1), wherein the curved pipe portion and the straight pipe portion of the flow pipe are gently connected without causing a step.
(3) The flow rate regulator includes a liquid storage part and a liquid injection part for injecting and supplying the coagulating liquid from the liquid storage part into the flow tube, and the liquid injection part equalizes the coagulated liquid supplied to the liquid storage part. The dry-wet spinning apparatus according to (1), which also serves as a pressure equalizing member to be compressed and / or a rectifying member that injects the rectified coagulating liquid into the coagulating liquid flowing down the flow tube,
(4) The dry and wet spinning device according to (3), wherein the liquid injection portion inner diameter of the flow rate regulator is formed in a conical shape spreading toward the downstream side,
(5) The dry and wet spinning apparatus according to (1), wherein the distance from the liquid level to the upper end of the flow tube is 2 to 100 mm,
(6) The dry and wet spinning device according to (1), wherein the inner diameter of the straight pipe portion of the flow pipe is 2 to 30 mm, and
(7) The dry / wet spinning apparatus according to (1), wherein a fiber take-up speed obtained by the above method is 10 to 300 m / min.

以上説明したように、本発明の乾湿式紡糸方法とその装置によれば、所望量の凝固液を流管内を流下する凝固液流を擾乱することなく円滑に供給することができ、流管内を流れる凝固液の流量及び流速を極めて良好に制御することができる。しかも、本発明では、流管内を流下する凝固液の流量と流速を制御するために、従来技術のように絞り部を設けないため、通過する凝固液の流路断面積が急激に変わることがなく、流管内で凝固液の速度差が発生することもない。その上、ノズルによって凝固液を直接流管内に強制的に噴出することもないため、流管内で凝固液の流速が急激に変化することもなくなる。   As described above, according to the dry and wet spinning method and apparatus of the present invention, a desired amount of coagulating liquid can be smoothly supplied without disturbing the coagulating liquid flow flowing down the flow pipe, The flow rate and flow rate of the flowing coagulating liquid can be controlled very well. In addition, in the present invention, in order to control the flow rate and flow velocity of the coagulating liquid flowing down in the flow tube, the throttle section is not provided as in the prior art, so that the flow passage cross-sectional area of the coagulating liquid passing therethrough changes suddenly. In addition, the speed difference of the coagulation liquid does not occur in the flow tube. In addition, since the coagulating liquid is not forcibly ejected directly into the flow tube by the nozzle, the flow rate of the coagulating liquid does not change abruptly in the flow tube.

したがって、紡糸口金から吐出されたドープは、凝固浴液によって繊維化される過程において、流管内を流れる凝固液の流速変化を小さくできる。このため、流管内で紡出したドープを安定的に単繊維切れの発生を極力抑制しながら繊維化することができ、繊維化することによって得られた糸条は、品質のバラツキが少なく安定した品質を有するという極めて顕著な効果を奏する。   Therefore, the dope discharged from the spinneret can reduce the change in the flow rate of the coagulating liquid flowing in the flow tube in the process of fiberizing with the coagulating bath liquid. For this reason, the dope spun in the flow tube can be made into fiber while stably suppressing the occurrence of single fiber breakage as much as possible, and the yarn obtained by making into fiber is stable with little variation in quality. There is an extremely remarkable effect of having quality.

以下、本発明の実施の形態について図面を参照しながら詳細に説明する。
図1は、本発明に係る乾湿式紡糸装置の一実施形態を模式的に例示した概略構成図である。この図1において、Dは全芳香族ポリアミドからなるポリマーを含むドープ、そして、Yはこのようなドープから溶媒が抽出されて繊維化された糸条をそれぞれ示す。また、1は多数の紡糸孔が穿設された紡糸口金、2は凝固装置、3は流管、そして、4は糸条を引き取るための回転体をそれぞれ示す。なお、前記凝固装置2は、凝固浴2a、凝固液の供給配管2b、凝固液の排出配管2c、凝固液の回収手段2d及び堰2eを含んで構成され、更に、符号Lは凝固液、そして符号Sは前記凝固液Lによって凝固浴2aに形成された液面をそれぞれ表す。
Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
FIG. 1 is a schematic configuration diagram schematically illustrating one embodiment of a dry / wet spinning apparatus according to the present invention. In FIG. 1, D represents a dope containing a polymer made of wholly aromatic polyamide, and Y represents a yarn obtained by extracting a solvent from such a dope and fiberized. Reference numeral 1 denotes a spinneret having a large number of spinning holes, 2 denotes a coagulating device, 3 denotes a flow tube, and 4 denotes a rotating body for taking up the yarn. The coagulation apparatus 2 includes a coagulation bath 2a, a coagulation liquid supply pipe 2b, a coagulation liquid discharge pipe 2c, a coagulation liquid recovery means 2d, and a weir 2e. Symbol S represents the liquid level formed in the coagulation bath 2a by the coagulation liquid L, respectively.

以上のように構成される本発明に係る乾湿式紡糸装置の実施形態例において、凝固液Lは、一定の流量に制御されながら凝固液Lの供給配管2bから凝固浴2aへ供給される。ついで、このようにして凝固浴2aへ供給された凝固液Lは、一方では、過剰に供給された凝固液Lが凝固浴2aに設けられた堰2eからオーバーフローして流出する。このようにして、前記堰2eは、凝固浴2aに貯えられる凝固液の液面Sの高さを、常に一定レベルに維持する役割を果たす。なお、前記オーバーフローした過剰の凝固液Lは回収手段2dによって回収され、この回収手段2dに接続する排出配管2cから排出される。   In the embodiment of the dry / wet spinning apparatus according to the present invention configured as described above, the coagulation liquid L is supplied from the supply pipe 2b of the coagulation liquid L to the coagulation bath 2a while being controlled at a constant flow rate. Next, the coagulating liquid L supplied to the coagulation bath 2a in this way overflows and flows out from the weir 2e provided in the coagulation bath 2a. In this way, the weir 2e serves to maintain the level of the liquid surface S of the coagulating liquid stored in the coagulating bath 2a at a constant level. The excessive coagulating liquid L overflowed is recovered by the recovery means 2d and discharged from the discharge pipe 2c connected to the recovery means 2d.

他方で、凝固浴2aへ供給された凝固液Lは、凝固液の液面Sの高さよりも下方に設けられた流管3へ流入し、紡糸口金1から紡出されたドープDと共に流管3内を流下する。また、この流管3は、上方の漏斗状を呈する曲管部3aと下方の筒状を呈する直管部3bとで構成されている。このとき、前記流管3の直管部3bには、図示したように流管3を流下する凝固液Lの流速と流量を調節するための流速調節器5が設けられている。ここで、本発明は前記流速調節器5を有することを一大特徴とするものであって、以下にこの流速調節器5について詳細に説明する。   On the other hand, the coagulation liquid L supplied to the coagulation bath 2 a flows into the flow tube 3 provided below the level of the liquid surface S of the coagulation liquid, and flows along with the dope D spun from the spinneret 1. Flow down in 3. The flow tube 3 is composed of a bent tube portion 3a having an upper funnel shape and a straight tube portion 3b having a lower tubular shape. At this time, the straight pipe portion 3b of the flow tube 3 is provided with a flow rate adjuster 5 for adjusting the flow rate and flow rate of the coagulating liquid L flowing down the flow tube 3 as shown in the figure. Here, the present invention is characterized by having the flow rate regulator 5, and the flow rate regulator 5 will be described in detail below.

以上に述べた本発明の流速調節器5は、凝固液Lを供給するための供給配管5aと、供給された凝固液Lを貯える貯液部5bと、貯えられた凝固液を流管3の直管部3b中へ注入供給する液注入部5cとから少なくとも構成されている。したがって、流管3へは、凝固浴2aを介して上方の曲管部3aから供給される凝固液Lと、貯液部5bを介して液注入部5cへ供給される凝固液Lとが注入される。   The flow rate regulator 5 of the present invention described above includes a supply pipe 5a for supplying the coagulating liquid L, a liquid storage part 5b for storing the supplied coagulating liquid L, and the stored coagulating liquid in the flow tube 3. It is at least comprised from the liquid injection | pouring part 5c injected and supplied in the straight pipe | tube part 3b. Therefore, the coagulating liquid L supplied from the upper curved pipe part 3a through the coagulation bath 2a and the coagulating liquid L supplied to the liquid injection part 5c through the liquid storage part 5b are injected into the flow tube 3. Is done.

このように、本例においては、流管3中を流下する凝固液Lに対して、流速調節器5から供給される凝固液Lを液注入部5cから注入することにより流下する凝固液に抵抗を与えることができる。したがって、流速調節器5からの凝固液Lの流量によって直管部3b内を流下する凝固液の流速と流量とを所望の値に調節することができる。   As described above, in this example, the coagulating liquid L flowing down in the flow pipe 3 is resisted against the coagulating liquid flowing down by injecting the coagulating liquid L supplied from the flow rate regulator 5 from the liquid injection unit 5c. Can be given. Therefore, the flow rate and flow rate of the coagulating liquid flowing down in the straight pipe portion 3b can be adjusted to desired values by the flow rate of the coagulating liquid L from the flow rate adjuster 5.

本発明においては、前述のように、流管3内を流下する凝固液Lの流速と流量を所望の値に調整できる。このため、紡糸口金1から紡出した紡糸原液(紡糸ドープD)を流管3内を流れる凝固液Lと共に走行させることで、ドープDの繊維化速度を所望の値に制御することができる。   In the present invention, as described above, the flow velocity and flow rate of the coagulating liquid L flowing down in the flow tube 3 can be adjusted to desired values. For this reason, the spinning speed of the dope D can be controlled to a desired value by running the spinning stock solution (spun dope D) spun from the spinneret 1 together with the coagulating liquid L flowing in the flow tube 3.

なお、調整したドープDを繊維化するにあたって、先ずギアポンプなどの計量供給手段を使用して、ドープの供給量を連続的に計量しながらスピンブロック(図示せず)へ分配供給し、スピンブロックに備えられた紡糸口金1からドープDとして紡出する。ただし、前記紡糸口金1の実施態様については、例えば、外径100mmの円板に孔径が0.5mmである紡糸孔群を1000個穿設して、これら多数の紡糸孔群からドープDを繊維状に紡出するものを挙げることができる。   In order to fiberize the adjusted dope D, first, a metering means such as a gear pump is used to distribute and supply the dope to the spin block (not shown) while continuously metering the dope supply amount. Spinning as a dope D from the spinneret 1 provided. However, with respect to the embodiment of the spinneret 1, for example, 1000 spinning hole groups having a hole diameter of 0.5 mm are drilled in a disk having an outer diameter of 100 mm, and the dope D is produced from these many spinning hole groups. Can be mentioned.

本発明においては、前述のような紡糸口金1から紡出したドープDは、図1に例示したように、紡糸口金1のドープ吐出面と凝固液の液面Sとの間に形成されたエアギャップG中へ一旦紡出され、ついで凝固液L中へ導入される。   In the present invention, the dope D spun from the spinneret 1 as described above is air formed between the dope discharge surface of the spinneret 1 and the liquid surface S of the coagulating liquid, as illustrated in FIG. Once spun into the gap G, it is then introduced into the coagulation liquid L.

なお、前記エアギャップGは、小さ過ぎると紡糸口金1のドープ吐出面に凝固液Lが接触する事態が発生し、紡糸口金1から吐出されたドープDが紡糸口金1の直下で凝固を起こしてしまい、単繊維切れを生じるため好ましくない。また、大き過ぎると紡糸孔群から紡出された隣接する糸同士が密着を起し、独立した単繊維群を得ることができない。このような理由から、前記エアギャップGは、例えば、上記紡糸口金1では1mm以上、50mm以下が適している。   If the air gap G is too small, the coagulation liquid L may come into contact with the dope discharge surface of the spinneret 1, and the dope D discharged from the spinneret 1 is solidified immediately below the spinneret 1. Therefore, it is not preferable because a single fiber breakage occurs. On the other hand, if the size is too large, adjacent yarns spun from the spinning hole group are brought into close contact with each other, and an independent single fiber group cannot be obtained. For this reason, the air gap G is suitably 1 mm or more and 50 mm or less in the spinneret 1, for example.

以上に述べたようにして、紡糸口金1に穿設された多数の紡糸孔から吐出されたドープDは、一旦空気中に紡出され、ついで、凝固浴2aに充填された凝固液Lへ導かれて流管3の曲管部3aへと導入される。   As described above, the dope D discharged from the numerous spinning holes drilled in the spinneret 1 is once spun into the air and then introduced into the coagulation liquid L filled in the coagulation bath 2a. Then, it is introduced into the curved pipe portion 3a of the flow pipe 3.

ここで、凝固浴2aの液面Sから流管3の上端部までの距離が小さいと、流管3の上部曲管部3aへ流入する凝固液Lの流れに乱れを生じ、これが液面Sまで伝播して液面Sが乱される。また、反対にこの距離が大きくなると、流管3を設置したことによる液面S近傍における凝固液Lの速度が所定の速度になるまでの立ち上がりを早くするという効果が無くなり、糸Y(ドープD)の走行速度と凝固液Lとの間の流速差が大きくなって単繊維切れが発生する。したがって、凝固浴2aの液面Sを安定させ、かつ単繊維切れの発生を抑制するには、液面Sから流管3の上端部までの距離を2mm以上、100mm以下の長さ、好ましくは、5mm以上、50mm以下にすることが必要である。   Here, if the distance from the liquid level S of the coagulation bath 2a to the upper end of the flow tube 3 is small, the flow of the coagulated liquid L flowing into the upper curved pipe portion 3a of the flow tube 3 is disturbed, and this is caused by the liquid surface S. And the liquid level S is disturbed. On the other hand, when this distance is increased, the effect of increasing the speed until the speed of the coagulating liquid L in the vicinity of the liquid surface S due to the installation of the flow tube 3 reaches a predetermined speed is lost. ) And the flow velocity difference between the coagulating liquid L and the single fiber breakage occurs. Therefore, in order to stabilize the liquid surface S of the coagulation bath 2a and suppress the occurrence of single fiber breakage, the distance from the liquid surface S to the upper end of the flow tube 3 is a length of 2 mm or more and 100 mm or less, preferably It is necessary to make it 5 mm or more and 50 mm or less.

このとき、図1では図示省略したが、凝固浴2a内に凝固液Lの流れを整流するための整流部材を設置して、凝固液Lの流れが擾乱されないように安定な流れを形成させることは、本発明においては、好ましい実施態様である。ここで、このような好ましい整流部材を例示するならば、多孔板、ハニカム板、織編物などの凝固液Lの通過性に優れたスクリーンなどを挙げることができる。なお、これらの整流部材の設置位置に関しては、特に流管3へ流入する凝固液Lの導入部近辺に設けることが望ましい。   At this time, although not shown in FIG. 1, a rectifying member for rectifying the flow of the coagulating liquid L is installed in the coagulating bath 2a to form a stable flow so that the flow of the coagulating liquid L is not disturbed. Is a preferred embodiment in the present invention. Here, examples of such a preferable rectifying member include a screen excellent in the passage of the coagulating liquid L such as a perforated plate, a honeycomb plate, and a woven or knitted fabric. In addition, regarding the installation position of these rectification members, it is desirable to provide especially in the vicinity of the introduction part of the coagulating liquid L which flows into the flow tube 3.

次に、本発明に用いる流管3の好ましい形状について述べると、その形状は紡糸口金1から吐出されるドープDが流管3内へ持ち込む凝固液Lの持込液量、ドープD自体の流管3への流入量、あるいは繊維化された糸条Yの引取速度などの多様な条件により決定される。このため、最終的には、これらの条件に適合するように実験を行って、最適な形状を決定する必要がある。しかしながら、凝固液Lの流管3内での速度上昇を滑らかにするためには、流管3上方の曲管部3aは、凝固液Lが流下する上流側に向ってなだらかな末広がり形状を有する曲面であることが必要である。   Next, the preferable shape of the flow tube 3 used in the present invention will be described. The shape is the amount of the solidified liquid L brought into the flow tube 3 by the dope D discharged from the spinneret 1 and the flow of the dope D itself. It is determined by various conditions such as the amount of inflow into the pipe 3 or the take-up speed of the fiberized yarn Y. For this reason, ultimately, it is necessary to determine an optimum shape by performing experiments so as to meet these conditions. However, in order to smooth the speed increase of the coagulating liquid L in the flow tube 3, the curved pipe portion 3a above the flow tube 3 has a gently divergent shape toward the upstream side where the coagulating liquid L flows down. It must be a curved surface.

このとき、ドープDが流管3内で凝固して繊維化されるプロセスとして、凝固浴2aと流管の曲管部3aと直管部3bとに存在する凝固液Lと紡出したドープDとを接触させ、ドープDに含有される有機溶剤を凝固液L中へ抽出し、例えばパラ系全芳香族ポリアミドポリマーからなる多数の単繊維群(マルチフィラメント)で構成される糸条Yを形成することは周知の通りである。   At this time, as a process in which the dope D is solidified in the flow tube 3 to be fiberized, the dope D spun with the coagulation liquid L existing in the coagulation bath 2a, the curved pipe portion 3a and the straight pipe portion 3b of the flow tube. And the organic solvent contained in the dope D is extracted into the coagulation liquid L to form a yarn Y composed of a number of single fiber groups (multifilaments) made of, for example, a para-type wholly aromatic polyamide polymer. It is well known to do.

次に、このようにして形成された糸条Yは、図1に例示したように、引取ローラなどの回転体4によって引き取られ、糸条Yに付着した凝固液Lを取り除く水洗工程、水洗工程で付着した水分を乾燥させる乾燥工程、乾湿式紡糸をした糸条を熱延伸する工程などからなる一連の製糸プロセスが行われる。そして、この一連の製糸プロセスによって高性能及び/又は高機能を有する繊維を最終的に得ることも周知の通りである。   Next, as illustrated in FIG. 1, the yarn Y formed in this way is taken up by a rotating body 4 such as a take-up roller, and a water washing step and a water washing step for removing the coagulating liquid L attached to the yarn Y. A series of yarn-making processes including a drying step of drying the moisture adhering to the above and a step of hot-drawing the yarn subjected to dry and wet spinning are performed. It is also well known that a fiber having high performance and / or high function is finally obtained by this series of yarn forming processes.

以上に述べたような一連の製糸プロセス中の乾湿式紡糸工程において、本発明が一大特徴とするところは、既に述べてきたように、流管3内の凝固液Lの流速を調節できる機構を要することである。そこで、本発明の流速調節器5について、図2を用いて以下に更に詳細に説明する。   In the dry-wet spinning process in the series of yarn forming processes as described above, the present invention is characterized by a mechanism capable of adjusting the flow rate of the coagulating liquid L in the flow tube 3 as described above. Is required. Therefore, the flow rate regulator 5 of the present invention will be described in more detail below with reference to FIG.

前記流速調節器5では、流管3内を流れる凝固液Lの流速と流量とを急激に変えないようにするため、流管3と流量調節器5の上部の接続部は絞り部などの急激な径変化がないことが望ましく、径変化が生じないように接続されることが好ましい。   In the flow rate adjuster 5, in order not to change the flow rate and flow rate of the coagulating liquid L flowing in the flow tube 3 abruptly, a connection portion at the upper part of the flow tube 3 and the flow rate adjuster 5 is a sudden portion such as a throttle portion. It is desirable that there is no change in diameter, and it is preferable that the connection is made so that no change in diameter occurs.

その際、前記流速調節器5の内部には流管3の直管部3bの一部を囲繞し、その全周方向から凝固液Lを安定して供給することができる整流部材あるいは均圧化部材をそれぞれ設置して、直管部3b内を流れる凝固液Lを大きく擾乱することなく、供給することが好ましい。なお、図1及び図2の例では、前記液注入部5cを構成する部材自体を多孔質性の焼結金属で構成して整流部材及び/又は均圧化部材の機能を兼ね備えさせている。   At that time, a part of the straight pipe portion 3b of the flow pipe 3 is surrounded inside the flow rate adjuster 5, and a rectifying member or pressure equalization capable of stably supplying the coagulating liquid L from the entire circumferential direction thereof. It is preferable to install each member and supply the coagulating liquid L flowing in the straight pipe portion 3b without greatly disturbing. In the example shown in FIGS. 1 and 2, the member constituting the liquid injection part 5c itself is made of a porous sintered metal so as to function as a rectifying member and / or a pressure equalizing member.

なお、この液注入部5cを構成する部材の他の例としては、凝固液Lの流れが擾乱されないように安定な流れを形成させることが好ましく、したがって、前記整流部材及び/又は均圧化部材の好ましい例を挙げるならば、多孔質焼結金属などの多孔板、ハニカム板、織編物などの流体通過性に優れたスクリーンなどの濾過媒体を挙げることができる。   As another example of the member constituting the liquid injection portion 5c, it is preferable to form a stable flow so that the flow of the coagulating liquid L is not disturbed. Therefore, the rectifying member and / or the pressure equalizing member As a preferable example, a filtration medium such as a porous plate such as a porous sintered metal, a screen having excellent fluid passage properties such as a honeycomb plate and a woven or knitted fabric can be used.

更に、液注入部5cから安定且つ均一に凝固液Lを供給するためには、凝固液Lの通過抵抗がある程度以上必要である。例えば、金属細線からなる織編物を材料として使用した場合には、20メッシュから2000メッシュの目開きの織編物を1枚または複数枚組み合わせて用いるとよい。もちろん、本発明においては、織編物に限定されること無く、類似の効果が得られるものであれば良いことは言うまでもない。   Furthermore, in order to supply the coagulation liquid L stably and uniformly from the liquid injection part 5c, the passage resistance of the coagulation liquid L is required to some extent. For example, when a woven or knitted fabric made of fine metal wires is used as a material, one or a plurality of woven or knitted fabrics having a mesh size of 20 to 2000 mesh may be used. Of course, in the present invention, it is needless to say that the present invention is not limited to the woven or knitted fabric, and any similar effect can be obtained.

ここで、前記液注入部5cの形状としては、流管3を流下する凝固液Lをできるだけ擾乱しないように流管3の直管部3bに対して径変化や段差が生じずになだらかに接続して急激な形状変化のないものが良いことは言うまでもない。更に、液注入部5cを流下する凝固液Lの平均流速が一定となるように、絞り部を設けずに、その内径が末広がりに錐状に拡がる形状が好ましい。   Here, the shape of the liquid injecting portion 5c is such that the solidified liquid L flowing down the flow tube 3 is gently connected to the straight tube portion 3b of the flow tube 3 without causing a diameter change or a step so as not to be disturbed as much as possible. Needless to say, it is good to have no sudden shape change. Furthermore, it is preferable that the inner diameter of the coagulating liquid L flowing down the liquid injecting portion 5c is constant without expanding the inner diameter of the coagulating liquid L.

以上に述べた流量調節器5は、流管3の直管部3bの下部に接続して設けられ、ここで、凝固液Lが流管3の直管部3bへと円滑に注入供給される。したがって、凝固浴2aから流管3を介して流速調節器5へ流下する凝固液Lは急激な速度変化を起さない。しかも、流管3内を流れる凝固液Lの流速と流量は、流量調節器5から供給する凝固液L流量を変化させることにより任意に調節することができる。   The flow rate regulator 5 described above is provided connected to the lower portion of the straight pipe portion 3b of the flow tube 3, and here, the coagulating liquid L is smoothly injected and supplied to the straight pipe portion 3b of the flow pipe 3. . Therefore, the coagulation liquid L flowing down from the coagulation bath 2a to the flow rate regulator 5 through the flow pipe 3 does not cause a rapid change in speed. In addition, the flow rate and flow rate of the coagulating liquid L flowing in the flow tube 3 can be arbitrarily adjusted by changing the flow rate of the coagulating liquid L supplied from the flow rate regulator 5.

このとき、供給配管2bから凝固浴2aへ供給される凝固液Lの流量と流速調節器5から供給される凝固液Lの流量は、製糸条件に応じて適宜選定すべき事項である。しかしながら、凝固浴2aの液面Sが乱されないこと、そして、流管3内を流れる流速がドープD及び糸条Yが流管3内を走行する速度と近いことが望ましいことは言うまでもない。そこで、例えば、引取手段4による糸条Yの引取り速度を70〜100m/minとするときに、凝固浴2aの供給配管2bから供給される凝固液Lの量は、2〜10l/min(リットル/分)とし、流量調節器5の凝固液の供給配管5aから供給される凝固液Lの量は、3〜5l/min(リットル/分)とすることが望ましい。   At this time, the flow rate of the coagulation liquid L supplied from the supply pipe 2b to the coagulation bath 2a and the flow rate of the coagulation liquid L supplied from the flow rate regulator 5 are matters to be appropriately selected according to the yarn production conditions. However, it goes without saying that the liquid level S of the coagulation bath 2a is not disturbed, and that the flow velocity flowing in the flow tube 3 is preferably close to the speed at which the dope D and yarn Y travel in the flow tube 3. Therefore, for example, when the take-up speed of the yarn Y by the take-up means 4 is 70 to 100 m / min, the amount of the coagulating liquid L supplied from the supply pipe 2b of the coagulation bath 2a is 2 to 10 l / min ( Liter / minute), and the amount of the coagulating liquid L supplied from the coagulating liquid supply pipe 5a of the flow rate regulator 5 is preferably 3 to 5 l / min (liter / min).

その際、前記直管部3bの管内径については、2mm以上、30mm以下とすることが好ましい。何故ならば、糸条Yを効率的に生産するためには糸条Yを構成する単繊維群(マルチフィラメント)の数として、10〜5000本が必要とされるので、この点を考慮に入れると、糸条の相当直径が1mm以上、20mm以下となるからである。したがって、流管3内を走行するドープDもしくは繊維化された糸条Yが流管壁に過度に接触してダメージを受けないように余裕を持って走行させるためには、流管3の下部直管部3bの円筒内径dは2mm以上、30mm以下とすることが好ましいのである。   At that time, the pipe inner diameter of the straight pipe portion 3b is preferably 2 mm or more and 30 mm or less. This is because, in order to efficiently produce the yarn Y, 10 to 5000 fibers are required as the number of single fiber groups (multifilaments) constituting the yarn Y, and this point is taken into consideration. This is because the equivalent diameter of the yarn is 1 mm or more and 20 mm or less. Therefore, in order to allow the dope D or the fiberized yarn Y traveling in the flow tube 3 to travel with sufficient margin so as not to be damaged due to excessive contact with the flow tube wall, the lower portion of the flow tube 3 is used. The cylindrical inner diameter d of the straight pipe portion 3b is preferably 2 mm or more and 30 mm or less.

また、流管3の下部直管部3bの円筒長さLとしては、紡糸速度などの紡糸条件にもよるが、100mm以上、5000mm以下とすることが好ましい。何故ならば、一方では、紡糸口金1から紡出されたドープDを繊維化するためには、凝固に要する時間が必要であるので、流管3の長さはこの凝固に要する時間を稼ぐことができる長さが必要となるからである。   The cylindrical length L of the lower straight pipe portion 3b of the flow tube 3 is preferably 100 mm or more and 5000 mm or less, although it depends on the spinning conditions such as the spinning speed. This is because, on the other hand, in order to make the dope D spun from the spinneret 1 into a fiber, the time required for solidification is required, so the length of the flow tube 3 increases the time required for this solidification. This is because it is necessary to have a length that can be used.

しかし、他方では、流管3下部の直管部3bの長さが長くなると、流管内壁面と走行するドープDあるいは糸条Yとが接触して過大な摩擦抵抗が作用する。そうすると、ドープDあるいは糸条Yが強く擦過されて単繊維切れや糸切れを招くので短くしたい。そこで、これら条件を両立させると、直管部3bの長Lは、100mm以上、5000mm以下とすることが好ましい。   However, on the other hand, when the length of the straight pipe portion 3b at the lower part of the flow tube 3 is increased, the inner wall surface of the flow tube and the running dope D or yarn Y come into contact with each other, and excessive frictional resistance acts. In this case, the dope D or the yarn Y is strongly abraded to cause a single fiber breakage or a thread breakage. Therefore, when these conditions are satisfied, the length L of the straight pipe portion 3b is preferably 100 mm or more and 5000 mm or less.

次に、本発明の乾湿式紡糸装置は、ポリアクリルニトリルなどの紡糸装置として用いることができるが、好ましくは、全芳香族ポリアミドからなるポリマーを含むドープDが繊維化されて糸条Yを形成するプロセスに用いることが好ましい。   Next, the dry / wet spinning device of the present invention can be used as a spinning device for polyacrylonitrile or the like. Preferably, a dope D containing a polymer made of wholly aromatic polyamide is made into a fiber to form a yarn Y. It is preferable to use it in the process.

例えば、この実施態様として、先ず「ドープ」として、水分率が100ppm以下のN−メチル−2−ピロリドン(以下NMPという)112.9部、パラフェニレンジアミン1.506部、3,4’−ジアミノジフェニルエーテル2.789部を常温下で反応容器に入れ、窒素中で溶解した後、攪拌しながらテレフタル酸クロライド5.658部を添加する。そして、最終的に85℃で60分間反応させ、透明の粘稠なポリマー溶液を得る。次いで、22.5重量%の水酸化カルシウムを含有するNMPスラリー9.174部を添加し、中和反応を行って、必要な「ドープ」を得る。   For example, in this embodiment, first, as “dope”, N-methyl-2-pyrrolidone (hereinafter referred to as NMP) having a moisture content of 100 ppm or less 112.9 parts, paraphenylenediamine 1.506 parts, 3,4′-diamino 2.789 parts of diphenyl ether are put in a reaction vessel at room temperature, dissolved in nitrogen, and 5.658 parts of terephthalic acid chloride is added with stirring. And finally, it is made to react at 85 degreeC for 60 minutes, and a transparent viscous polymer solution is obtained. Next, 9.174 parts of NMP slurry containing 22.5% by weight of calcium hydroxide is added and a neutralization reaction is performed to obtain the necessary “dope”.

本発明に係る乾湿式紡糸装置の一実施形態を模式的に例示した概略構成図である。It is the schematic block diagram which illustrated typically one Embodiment of the dry-wet spinning apparatus which concerns on this invention. 本発明の要部(流管部)を模式的に拡大表示した拡大断面図である。It is the expanded sectional view which expanded and displayed the principal part (flow pipe part) of this invention typically.

符号の説明Explanation of symbols

1 紡糸口金
2 凝固装置
2a 凝固浴
2b 凝固液の供給配管
2c 凝固液の排出配管
2d 凝固液の回収手段
2e 堰
3 流管
3a 流管の曲管部
3b 流管の直管部
4 糸条の引取手段
5 流速調節器
5b 凝固液の貯部
5a 凝固液の供給配管
5c 液注入部
D ドープ
G エアギャップ
L 凝固液
S 凝固浴液面
Y 糸条
DESCRIPTION OF SYMBOLS 1 Spinneret 2 Coagulation apparatus 2a Coagulation bath 2b Coagulation liquid supply pipe 2c Coagulation liquid discharge pipe 2d Coagulation liquid recovery means 2e Weir 3 Flow pipe 3a Flow pipe curved pipe section 3b Flow pipe straight pipe section 4 Take-up means 5 Flow rate regulator 5b Coagulating liquid storage section 5a Coagulating liquid supply pipe 5c Liquid injection section D Dope G Air gap L Coagulating liquid S Coagulating bath liquid surface Y Yarn

Claims (7)

凝固液を充填する凝固浴と、前記凝固浴に充填される前記凝固液が形成する液面と一定のエアギャップをおいて設けられた多数の紡糸孔群が穿設された紡糸口金と、前記凝固液中に浸漬させて設けられた流管と、前記流管の下方に設けられた糸条の引取手段を含む乾湿式紡糸装置において、
前記流管は、その上部内壁面は凝固液が流入する上流側に向って末広がりに形成された漏斗状の曲管部を有し、その下部内壁面は筒状の直管部を有すると共に、前記直管部に引き続いて前記直管部の管内径を縮小することなく全周方向から凝固液を供給する流速調節器を備え、前記流速調節器から供給する凝固液によって流管内を流下する凝固液の流速及び流量を制御することを特徴とする乾湿式紡糸装置。
A coagulation bath filled with a coagulation liquid, a spinneret in which a plurality of spinning hole groups provided with a constant air gap and a liquid surface formed by the coagulation liquid filled in the coagulation bath are formed; In a dry-wet spinning apparatus including a flow tube immersed in a coagulation liquid and a yarn take-up means provided below the flow tube,
The flow tube has a funnel-shaped curved pipe portion whose upper inner wall surface is formed to expand toward the upstream side where the coagulating liquid flows, and a lower inner wall surface thereof has a cylindrical straight pipe portion, A flow rate regulator that supplies a coagulating liquid from the entire circumference without reducing the pipe inner diameter of the straight pipe part following the straight pipe part, and a coagulation that flows down in the flow pipe by the coagulating liquid supplied from the flow rate regulator A dry-wet spinning apparatus characterized by controlling the flow rate and flow rate of a liquid.
前記流管の曲管部と直管部とが段差を生じずになだらかに接続されている請求項1記載の乾湿式紡糸装置。   The dry-wet spinning apparatus according to claim 1, wherein the bent pipe portion and the straight pipe portion of the flow pipe are smoothly connected without causing a step. 前記流速調節器が貯液部と、該貯液部から流管中に凝固液を注入供給する液注入部を備え、該液注入部が貯液部に供給された凝固液を均圧化する均圧化部材及び/又は整流した凝固液を流管を流下した凝固液に注入する整流部材を兼ねる請求項1記載の乾湿式紡糸装置。   The flow rate regulator includes a liquid storage unit and a liquid injection unit that injects and supplies the coagulating liquid from the liquid storage unit into the flow tube, and the liquid injection unit equalizes the coagulated liquid supplied to the liquid storage unit. The dry-wet spinning apparatus according to claim 1, which also serves as a pressure equalizing member and / or a rectifying member for injecting the rectified coagulating liquid into the coagulating liquid flowing down the flow tube. 前記流速調節器の液注入部内径が下流側に向かって末広がりに錐状に形成された請求項3に記載の乾湿式紡糸装置。   The dry / wet spinning apparatus according to claim 3, wherein an inner diameter of the liquid injection portion of the flow rate regulator is formed in a conical shape so as to widen toward the downstream side. 前記液面から前記流管の上端部までの距離が2〜100mmである請求項1記載の乾湿式紡糸装置。   The dry-wet spinning apparatus according to claim 1, wherein a distance from the liquid level to the upper end of the flow tube is 2 to 100 mm. 前記流管の直管部の内径が2〜30mmである請求項1記載の乾湿式紡糸装置。   The dry-wet spinning apparatus according to claim 1, wherein the straight pipe portion of the flow pipe has an inner diameter of 2 to 30 mm. 前記方法により得られる繊維の引取り速度が10〜300m/minである請求項1記載の乾湿式紡糸装置。   The dry-wet spinning apparatus according to claim 1, wherein a take-up speed of the fiber obtained by the method is 10 to 300 m / min.
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JP2006342451A (en) * 2005-06-08 2006-12-21 Teijin Techno Products Ltd Dry-wet spinning method and apparatus therefor
JP4598607B2 (en) * 2005-06-08 2010-12-15 帝人テクノプロダクツ株式会社 Dry-wet spinning method and apparatus
JP2010508451A (en) * 2006-10-31 2010-03-18 イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー Method and apparatus for the manufacture of yarn
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JP2011517736A (en) * 2008-03-31 2011-06-16 コーロン インダストリーズ インク Para-aramid fiber and method for producing the same
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