JP2006342451A - Dry-wet spinning method and apparatus therefor - Google Patents

Dry-wet spinning method and apparatus therefor Download PDF

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JP2006342451A
JP2006342451A JP2005168139A JP2005168139A JP2006342451A JP 2006342451 A JP2006342451 A JP 2006342451A JP 2005168139 A JP2005168139 A JP 2005168139A JP 2005168139 A JP2005168139 A JP 2005168139A JP 2006342451 A JP2006342451 A JP 2006342451A
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Yasushi Kitagishi
泰 北岸
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a dry-wet spinning method by which a spinning speed is heightened to improve the productivity, and a fiber having little dispersion of quality among single fibers constituting a yarn, and stable properties is obtained while suppressing the occurrence of single fiber breakage; and to provide an apparatus therefor. <P>SOLUTION: The dry-wet spinning method comprises spinning a spinning dope (D) from a spinning cap (1) having many spinning holes bored therein into a gaseous body, introducing the spun dope (D) into a coagulation liquid (La) flowing down in a flow tube (3) to coagulate the dope and to form the fiber, and taking up the fiberized yarn (Y), wherein a coagulation liquid (Lb) having a different solvent concentration contained in the coagulation liquid is injected to the midway of the flow tube (3), and the speed, the flow rate, the concentration and/or the temperature of the coagulation liquid flowing down in the flow tube (3) are regulated. <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、紡出した紡糸ドープを凝固液が流下する流管中へ導入して繊維化する乾湿式紡糸方法及びその装置に関する。   The present invention relates to dry-wet spinning in which a spinning dope is once spun into the air from a spinneret having a large number of spinning holes, and the spun dope is introduced into a flow tube through which a coagulating liquid flows to be fiberized. The present invention relates to a method and an apparatus thereof.

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、従来より多数の紡糸孔が穿設された紡糸口金から全芳香族ポリアミド重合体を含む溶液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により脱溶媒して凝固させ繊維化することは周知である。なお、本発明において、紡糸口金に穿設された紡糸孔から紡出された紡糸原液から溶剤が抽出されて繊維化されるまでの間の状態を「ドープ」と総称するものとする。   As a conventional technique for spinning a wholly aromatic polyamide fiber having both high strength and high modulus, a solution dope containing a wholly aromatic polyamide polymer is once in the air from a spinneret having a larger number of spinning holes. It is well known that the dope stream is spun and then solidified by removing the solvent with a coagulating liquid and coagulating it. In the present invention, the state until the solvent is extracted from the spinning stock solution spun from the spinning hole formed in the spinneret and made into a fiber is collectively referred to as “dope”.

しかしながら、静止した凝固液を貯えた凝固浴へドープを導入して凝固させると、ドープの導入速度がある速度以上になると、凝固液から受ける抵抗により、単繊維切れが起こる。このため、ドープの凝固液中への導入速度を上げることができず、それ故に、紡糸速度を低速にせざるを得なかった。それに加えて、紡糸速度を高速にすると、速度上昇に伴い凝固液中での凝固に要する時間を確保するために、浸漬時間(浸漬長)を大きくとる必要が生じ、必然的に装置サイズが大きくなるという問題があった。   However, when the dope is introduced into the coagulation bath storing the stationary coagulation liquid and coagulated, when the dope introduction speed exceeds a certain speed, the single fiber breakage occurs due to the resistance received from the coagulation liquid. For this reason, the introduction speed of the dope into the coagulation liquid cannot be increased, and therefore the spinning speed has to be reduced. In addition, when the spinning speed is increased, it is necessary to increase the immersion time (immersion length) in order to secure the time required for coagulation in the coagulation liquid as the speed increases, and the size of the apparatus is inevitably increased. There was a problem of becoming.

そこで、紡糸速度を高速化するために、静止した凝固液中へドープを導入するのではなく、走行するドープと共に凝固液を流動させて凝固液から受ける抵抗を減らしつつ、ドープを凝固させて繊維化する流管式紡糸方法とその装置が、例えば特開昭60−52610号公報に提案されている。   Therefore, in order to increase the spinning speed, the dope is not introduced into the stationary coagulating liquid, but the dope is coagulated while reducing the resistance received from the coagulating liquid by flowing the coagulating liquid together with the running dope. Japanese Patent Application Laid-Open No. 60-52610 proposes a flow tube spinning method and an apparatus therefor.

確かに、この従来技術によれば、流管内を流下する凝固液の流速を上げることによって、紡糸速度を上げることができる。しかしながら、この従来技術では、流管内のドープの速度を流管内を流下する凝固流の流速と一致させることが難しく、単繊維切れを起こしてしまい安定した紡糸を行うことができない。更に、この従来技術では、流管内を流下する凝固液は新たに追加又は置換されない。   Certainly, according to this prior art, the spinning speed can be increased by increasing the flow rate of the coagulating liquid flowing down in the flow tube. However, in this prior art, it is difficult to match the dope speed in the flow tube with the flow rate of the solidified flow flowing down in the flow tube, and the single fiber breakage occurs, and stable spinning cannot be performed. Furthermore, in this prior art, the coagulating liquid flowing down in the flow tube is not newly added or replaced.

このため、脱溶媒により凝固させる系においては、流管を通過するに従い凝固液中にドープ由来の溶媒が抽出されるために、凝固液の溶媒濃度が上昇し、品質の安定性が損なわれる。特に、生産性を確保するため糸条を構成する単繊維数を増やした場合に、ドープから凝固液に抽出される溶媒濃度の増加が撚り顕著になる。したがって、前記問題がより深刻となり、単繊維切れの発生がより大きくクローズアップされてくる。   For this reason, in a system that solidifies by desolvation, the solvent derived from the dope is extracted into the coagulating liquid as it passes through the flow tube, so that the solvent concentration of the coagulating liquid is increased and quality stability is impaired. In particular, when the number of single fibers constituting the yarn is increased in order to ensure productivity, the increase in the concentration of the solvent extracted from the dope into the coagulation liquid becomes more noticeable. Therefore, the problem becomes more serious, and the occurrence of single fiber breakage is more closely highlighted.

そこで、例えば特開昭61−19805号公報に開示された技術では、流管の下流側に流体噴射装置及び気体噴射装置を設けて紡糸する高速度湿式紡糸方法が提案されている。確かに、この装置によると、流体噴射装置によって吹出される流体の推進力を借りて、流管内の流速を上げることができ、且つ噴射装置から濃度の異なる凝固液を供給することができるため、紡出されたドープが凝固して繊維化される過程において凝固液の濃度制御を行うことができる高速紡糸が可能となる。   Therefore, for example, in the technique disclosed in Japanese Patent Application Laid-Open No. 61-19805, a high-speed wet spinning method is proposed in which a fluid ejecting device and a gas ejecting device are provided on the downstream side of the flow tube for spinning. Certainly, according to this device, it is possible to increase the flow velocity in the flow tube by using the propulsive force of the fluid blown out by the fluid ejecting device, and it is possible to supply coagulating liquids having different concentrations from the ejecting device. High-speed spinning is possible in which the concentration of the coagulating liquid can be controlled in the process in which the spun dope is solidified and made into a fiber.

しかしながら、例えば特開昭61−19805号公報に提案されているようなこの種の従来技術では、流管と流体噴射装置との間が自由落下ゾーンとなっているため、ドープ又は糸条が流体噴射装置入った時に急激な流体の速度変化が生じてしまい、凝固過程の途上にある半凝固状態の糸条を構成する単繊維が切れてしまうという問題が生じる。   However, in this type of prior art proposed in Japanese Patent Laid-Open No. 61-19805, for example, a free fall zone is formed between the flow tube and the fluid ejecting device, so that the dope or the yarn is fluid. When entering the injection device, a rapid change in the speed of the fluid occurs, and there arises a problem that the single fibers constituting the semi-solidified yarn in the course of the solidification process are broken.

特開昭60−52610号公報JP 60-52610 A 特開昭61−19805号公報Japanese Patent Laid-Open No. 61-19805

以上に述べた従来技術が有する諸問題に鑑み、本発明が解決しようとする課題は、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、凝固液中へ紡出したドープを導いて繊維化する乾湿式紡糸において、紡糸速度を高速化して生産性を向上させることができると共に、糸条を構成する単繊維群間に品質バラツキが無く、しかも、単繊維切れの発生を抑制でき安定した性能を有する繊維を得ることができる方法と装置を提供することにある。   In view of the problems of the prior art described above, the problem to be solved by the present invention is that a spinning dope is once spun into the air from a spinneret having a large number of spinning holes and spun into a coagulation liquid. In dry-wet spinning, in which the dope is introduced into fibers, the spinning speed can be increased to improve productivity, and there is no quality variation among the single fibers constituting the yarn, and the single fibers are broken. It is an object of the present invention to provide a method and an apparatus capable of obtaining a fiber having a stable performance and capable of suppressing the occurrence of the above.

ここに、上記課題を解決する本発明に係わる湿式紡糸方法として、
(1) 多数の紡糸孔群が穿設された紡糸口金から紡糸原液を気体中へ紡出した後、引き続いて流管中を流下する凝固液中に前記紡糸原液を導入して凝固させて繊維化し、繊維化した糸条を引き取る乾湿式紡糸方法において、前記流管の途中から凝固液に含まれる溶剤濃度の異なる凝固液を注入し、流管内を流下する凝固液の濃度を調整することを特徴とする湿式紡糸方法、
(2) 流管を流下する前記凝固液の温度と異なる温度に維持された凝固液を前記流管の途中から流管内に注入し、流管内を流下する凝固液の温度を調整することを特徴とする (1)記載の湿式紡糸方法、
(3) 前記流管の途中から供給する凝固液の流量によって、凝固液の注入位置まで流下する凝固液の流速及び/又は流量を制御することを特徴とする(1)又は(2)に記載の湿式紡糸方法、そして、
(4) 全芳香族ポリアミド繊維を乾湿式紡糸することを特徴とする請求項1〜3の何れかに記載の湿式紡糸方法が提供される。
Here, as a wet spinning method according to the present invention for solving the above problems,
(1) After spinning a spinning solution into a gas from a spinneret having a number of spinning hole groups, the spinning solution is introduced into a coagulating solution that flows down in a flow tube, and then coagulated. In the dry-wet spinning method for taking up the fiberized yarn, the coagulating liquid having a different solvent concentration contained in the coagulating liquid is injected from the middle of the flow pipe, and the concentration of the coagulating liquid flowing down in the flow pipe is adjusted. Wet spinning method,
(2) The coagulating liquid maintained at a temperature different from the temperature of the coagulating liquid flowing down the flow pipe is injected into the flow pipe from the middle of the flow pipe, and the temperature of the coagulating liquid flowing down the flow pipe is adjusted. And the wet spinning method according to (1),
(3) The flow rate and / or flow rate of the coagulation liquid flowing down to the coagulation liquid injection position is controlled by the flow rate of the coagulation liquid supplied from the middle of the flow tube. (1) or (2) A wet spinning method, and
(4) The wet spinning method according to any one of claims 1 to 3, wherein the wholly aromatic polyamide fiber is dry-wet spun.

次に、上記課題を解決する本発明に係わる湿式紡糸装置として、
(5) 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、前記液面より下方に浸漬させて前記凝固浴中に設けられた前記凝固液が流下する流管と、前記流管の途中から新鮮な凝固液を流管中へ注入する凝固液注入器と、前記流管の下方に設けられた糸条の引取手段とを少なくとも備えた乾湿式紡糸装置、
(6) 流管の途中で注入する前記凝固液の温度を一定に制御する温度制御装置を備えたことを特徴とする(5)に記載の湿式紡糸装置、
(7) 流管内へ凝固液を注入する前記凝固液注入器の液注入部に、前記液注入部に凝固液の注入圧力を均圧化する均圧化部材を設けた(5)又は(6)に記載の湿式紡糸装置、
(8) 流管内へ凝固液を注入する前記凝固液注入器の液注入部に、前記液注入部に凝固液を整流する整流部材を設けた(5)〜(7)の何れかに記載の湿式紡糸装置、そして
(9) 流管内へ凝固液を注入する前記凝固液注入器の液注入部の形状を下流方向に沿って錐状に末広がりとした(5)〜(8)の何れかに記載の湿式紡糸装置が提供される。
Next, as a wet spinning device according to the present invention that solves the above problems,
(5) A coagulation bath filled with a coagulation liquid, and a spinneret in which a number of spinning hole groups provided with a certain air gap from the liquid surface formed by the coagulation liquid filled in the coagulation bath are formed. And a flow tube that is immersed below the liquid surface and flows in the coagulation bath, and a coagulating liquid injector that injects fresh coagulated liquid into the flow tube from the middle of the flow tube And a dry-wet spinning device comprising at least thread take-up means provided below the flow tube,
(6) The wet spinning device according to (5), characterized by comprising a temperature control device that controls the temperature of the coagulation liquid injected in the middle of the flow tube to a constant level,
(7) The liquid injection part of the coagulation liquid injector that injects the coagulation liquid into the flow tube is provided with a pressure equalizing member that equalizes the injection pressure of the coagulation liquid in the liquid injection part (5) or (6 ) Wet spinning apparatus according to
(8) The liquid injection part of the coagulation liquid injector for injecting the coagulation liquid into the flow tube is provided with a rectifying member for rectifying the coagulation liquid in the liquid injection part, according to any one of (5) to (7) Wet spinning equipment, and
(9) The wet spinning device according to any one of (5) to (8), wherein the shape of the liquid injecting portion of the coagulating liquid injector that injects the coagulating liquid into the flow tube extends conically in the downstream direction. Is provided.

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、紡糸速度を上げることができ、かつ、流管内の濃度および温度を任意に設定できることにより、流管内でドープを凝固して繊維化することを効率的に行うことができる。このため、得られる糸条は、単繊維切れが少なく、かつ品質のバラツキのない安定したものを得ることができるといる極めて顕著な効果を奏する。   As described above, according to the dry and wet spinning method and apparatus of the present invention, the spinning speed can be increased and the concentration and temperature in the flow tube can be arbitrarily set, so that the dope is solidified in the flow tube. Thus, fiberization can be performed efficiently. For this reason, the obtained yarn has an extremely remarkable effect that it can obtain a stable one with few single fiber breaks and no quality variation.

本発明がその対象とするのは、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などを製造するために好適な乾湿式紡糸方法とそのための装置である。   The object of the present invention is a dry and wet spinning method suitable for producing a fully aromatic polyamide fiber having both high strength and high modulus, and an apparatus therefor.

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り、図2は図1の要部を拡大して模式的に示した要部拡大断面図である。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はドープが繊維化された糸条を引き取る回転体をそれぞれ示す。
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 an embodiment of a dry / wet spinning apparatus according to the present invention, and FIG. 2 is an enlarged cross-sectional view schematically showing an essential part of FIG. It is. 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 that takes up a yarn in which the dope is made into fibers.

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。   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.

以下、この本発明に係わる乾湿式紡糸装置を用いて、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の実施形態について詳細に説明する。   Hereinafter, an embodiment of a process in which a dope D containing a polymer made of wholly aromatic polyamide is fiberized to form a yarn Y using the dry and wet spinning apparatus according to the present invention will be described in detail.

先ず、本発明では、紡糸原液として「ドープ」を使用するが、この「ドープ」は、例えば次に述べるようにして調整することができる。すなわち、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。   First, in the present invention, “dope” is used as the spinning dope. This “dope” can be adjusted, for example, as described below. That is, 112.9 parts of N-methyl-2-pyrrolidone (hereinafter referred to as NMP) having a moisture content of 100 ppm or less, 1.506 parts of paraphenylenediamine, and 2.789 parts of 3,4'-diaminodiphenyl ether at a room temperature. And after dissolving in nitrogen, 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”.

前述のようにして、調整したドープ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、このスピンブロックに装着された紡糸口金1からドープを紡出する。ただし、前記紡糸口金1は、例えば、外径100mmの円板に孔直径が0.5mmの紡糸孔を1000個穿設したものであって、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である。その際、図1に例示したように、凝固液Lが形成する液面Sと紡糸口金1のドープ吐出面との間はエアギャップGが形成されている。   As described above, when the adjusted dope is made into fiber, first, using a metering means such as a gear pump, the dope is continuously metered and distributed to a spin block (not shown). The dope is spun from the spinneret 1 attached to the spin block. However, the spinneret 1 is, for example, a disc having an outer diameter of 100 mm with 1,000 spinning holes having a hole diameter of 0.5 mm, and the dope D is made into a fibrous form from these many spinning hole groups. It is to be spun. At that time, as illustrated in FIG. 1, an air gap G is formed between the liquid surface S formed by the coagulation liquid L and the dope discharge surface of the spinneret 1.

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が紡糸口金1の直下で凝固を起こし、単繊維切れを生じる。また、大き過ぎると紡糸口金1内の隣接する糸同士が密着を起し、独立した繊維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 discharged from the spinneret 1 will solidify immediately below the spinneret 1, Causes fiber breakage. If it is too large, adjacent yarns in the spinneret 1 are brought into close contact with each other, and independent fibers 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群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へと浸漬され、ついで、流管3へと導かれる。なお、凝固浴2aの内部には紡糸口金1に対応させて流管3が挿入固定されており、この流管3は、凝固液Lが形成する液面Sよりも低い位置に設定されている。   As described above, the dope D discharged from the numerous spinning hole groups drilled in the spinneret 1 is once spun into the air, and then into the coagulation liquid L filled in the coagulation bath 2a. And then led to the flow tube 3. A flow tube 3 is inserted and fixed in the coagulation bath 2a in correspondence with the spinneret 1. The flow tube 3 is set at a position lower than the liquid level S formed by the coagulation liquid L. .

このように、流管3の上端は凝固浴2aの液面Sより低い位置に設けられているために、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の上方の凝固液流に乱れが生じ、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凝固液Lの流れの安定化効果が無くなる。したがって、凝固浴2aの液面Sを安定させるためには、液面Sから流管3の上端部までの距離を2mm以上、100mm以下、好ましくは、5mm以上、50mm以下にすることが必要である。   Thus, since the upper end of the flow tube 3 is provided at a position lower than the liquid surface S of the coagulation bath 2a, if the distance from the liquid surface S of the coagulation bath 2a to the upper end portion of the flow tube 3 is small, the flow tube 3 Disturbance occurs in the coagulating liquid flow above the tube 3, and this is propagated to the liquid surface S, and the liquid surface S is disturbed. On the other hand, when this distance increases, the effect of stabilizing the flow of the coagulating liquid L due to the installation of the flow tube 3 is lost. Therefore, in order to stabilize the liquid level S of the coagulation bath 2a, the distance from the liquid level S to the upper end of the flow tube 3 needs to be 2 mm or more and 100 mm or less, preferably 5 mm or more and 50 mm or less. is there.

次に、本発明の流管3に適した形状について述べると、紡糸口金1から紡出されたドープDを繊維化するための凝固にはある程度の時間が必要であるから、流管3の長さはある程度以上の長さが必要となる。しかし、他方で、流管3の下部の直円筒長が長くなると、流管3の内壁面と走行糸条Yとの間に過大な摩擦抵抗が作用して、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、流管下部3bの直円筒長Lが100mm以上、5000mm以下とすることが好ましい。   Next, the shape suitable for the flow tube 3 of the present invention will be described. Since a certain amount of time is required for solidification to make the dope D spun from the spinneret 1 into a fiber, the length of the flow tube 3 is long. The length of a certain length is required. On the other hand, however, if the length of the straight cylinder at the bottom of the flow tube 3 is increased, an excessive frictional resistance acts between the inner wall surface of the flow tube 3 and the running yarn Y, and the yarn Y is rubbed strongly. I want to shorten it because it leads to single fiber breakage and thread breakage. Therefore, if these conditions are satisfied, it is preferable that the straight cylinder length L of the flow tube lower part 3b is 100 mm or more and 5000 mm or less.

また、流管3の内径に関しては、例えば引取手段4による糸条Yの引取速度が10m/min以上、300m/min以下の範囲であれば、糸条Yを構成する単繊維群の数(フィラメント数)として、効率的な生産を考慮すると、10〜5000本が必要とされる。この点を考慮に入れると、糸条の相当直径が1mm以上、20mm以下となることから、これに対応して、流管3の最小内径dは、2mm以上、30mm以下とすることが好ましい。   Regarding the inner diameter of the flow tube 3, for example, if the take-up speed of the yarn Y by the take-up means 4 is in the range of 10 m / min to 300 m / min, the number of single fiber groups constituting the yarn Y (filament As for the number), considering efficient production, 10 to 5000 pieces are required. Considering this point, the equivalent diameter of the yarn is 1 mm or more and 20 mm or less, and accordingly, the minimum inner diameter d of the flow tube 3 is preferably 2 mm or more and 30 mm or less.

ただし、その最終形状は、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Laの液量、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。   However, the final shape of the dope D discharged from the spinneret 1 is the amount of coagulating liquid La brought into the flow tube 3, the amount of dope D itself flowing into the flow tube 3, or the fiberized yarn Y Therefore, it is necessary to finally perform an experiment to meet these conditions and determine an optimum shape.

なお、図1では図示を省略したが、凝固浴2a内に必要に応じて整流部材(図示せず)を設置して、供給配管2bから供給された凝固液Lの流れが擾乱されないように安定な流れを形成させながら流管3へ供給することは、本発明においては、好ましい実施態様である。ここで、前記整流部材を例示するならば、多孔板、ハニカム板、織編物などの流体通過性に優れたスクリーンなどを挙げることができ、これらを特に流管3に流入する凝固液の導入部近辺に設けることが望ましい。   Although not shown in FIG. 1, a rectifying member (not shown) is installed in the coagulation bath 2a as necessary to stabilize the flow of the coagulation liquid L supplied from the supply pipe 2b. It is a preferred embodiment in the present invention to supply the flow tube 3 while forming a simple flow. Examples of the rectifying member include a screen having excellent fluid passage properties such as a perforated plate, a honeycomb plate, and a woven or knitted fabric. It is desirable to provide in the vicinity.

以上に述べたようにして、凝固浴2aと流管3とに存在する凝固液とドープDとが接触することによって、ドープDに含有される有機溶剤が凝固液中へ抽出されて繊維化され、全芳香族ポリアミドからなる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が形成されることは周知の通りである。   As described above, when the coagulation liquid present in the coagulation bath 2a and the flow tube 3 and the dope D come into contact with each other, the organic solvent contained in the dope D is extracted into the coagulation liquid and fiberized. As is well known, a yarn Y composed of a number of single fiber groups (multifilaments) made of a polymer made of wholly aromatic polyamide is formed.

そして、このようにして形成された糸条Yは、その後、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、熱延伸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得ることも周知の通りである。   The yarn Y thus formed is then taken up by the rotating body 4 such as a take-up roller, and the water adhering in the water washing step and water washing step for removing the coagulating liquid L adhering to the yarn Y is dried. A series of yarn making processes including a drying step and a heat drawing step is performed. It is also well known that fibers having high performance and / or high function are obtained by this series of spinning processes.

その際、紡出されたドープを凝固させて繊維化するための凝固液Lは、先ず、一定の流量に制御されながら供給配管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。   At that time, the coagulation liquid L for coagulating the spun dope into fibers is first supplied from the supply pipe 2b 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の一部は、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。なお、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Laの流速と流量を調節するための凝固液注入器5が設けられている。   On the other hand, a part of the coagulation liquid L supplied to the coagulation bath 2a flows into the flow tube 3 provided below the level of the liquid surface S of the coagulation liquid, and the dope D spun from the spinneret 1 At the same time, it flows down in the flow tube 3. The flow tube 3 includes 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 pipe 3 is provided with a coagulating liquid injector 5 for adjusting the flow rate and flow rate of the coagulating liquid La flowing down the flow pipe 3 as shown in the figure.

ここで、前記凝固液注入器5は、凝固液Lbを供給するための液入口部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Laと、貯液部5bを介して液注入部5cから流管3へ供給された凝固液Lbとが注入される。そして、前記凝固液Laと凝固液Lbとが混合された状態で流管3の下方に形成された直管部3cを流下する。   Here, the coagulating liquid injector 5 includes a liquid inlet part 5a for supplying the coagulating liquid Lb, a liquid storing part 5b for storing the supplied coagulating liquid L, and the stored coagulating liquid directly in the flow tube 3. It is comprised at least from the liquid injection | pouring part 5c injected and supplied in the pipe part 3b. Therefore, the coagulating liquid La supplied from the upper curved pipe portion 3a via the coagulation bath 2a and the coagulating liquid supplied from the liquid injection portion 5c to the flow tube 3 via the liquid storage portion 5b are supplied to the flow tube 3. Lb is injected. And the straight pipe part 3c formed under the flow pipe 3 flows down in the state which the said coagulating liquid La and the coagulating liquid Lb were mixed.

このように、本例においては、流管3中を流下する凝固液Laに対して、凝固液注入器5から供給される凝固液Lbを液注入部5cから注入する。そうすると、流管3の上方部3a及び3b中を流下する凝固液Laに通過抵抗を負荷することができ、凝固液Laの速度及び流量を制御することができる。なお、凝固液Laの速度及び流量は、注入する凝固液Lbの量を調整することで所望の値に制御される。すなわち、凝固液Lbの流量と凝固液Laの流量との混合比と、注入する凝固液Lbの温度と濃度とを適切に調整することによって、凝固液La及び凝固液Lbの混合凝固液の温度と濃度を適正に調節することができる。   As described above, in this example, the coagulating liquid Lb supplied from the coagulating liquid injector 5 is injected from the liquid injecting unit 5 c into the coagulating liquid La flowing down in the flow tube 3. Then, passage resistance can be applied to the coagulating liquid La flowing down in the upper portions 3a and 3b of the flow tube 3, and the speed and flow rate of the coagulating liquid La can be controlled. The speed and flow rate of the coagulating liquid La are controlled to desired values by adjusting the amount of the coagulating liquid Lb to be injected. That is, by appropriately adjusting the mixing ratio between the flow rate of the coagulation liquid Lb and the flow rate of the coagulation liquid La and the temperature and concentration of the coagulation liquid Lb to be injected, the temperature of the coagulation liquid La and the coagulation liquid Lb is adjusted. And the concentration can be adjusted appropriately.

このように、本発明においては、流管3内を流下する凝固液Laの流速と流量を流管の全長に渡って所望の値に調整できる。このため、紡糸口金1から紡出したドープDを流管3内を流下する制御された流速、流量、温度、溶媒濃度を持った凝固液と共に走行させることができ、これによって、ドープDに余分な付加張力を作用させること無く、ドープDの繊維化速度を適切に制御することができる。したがって、凝固液中で生じる単繊維切れを抑制しながら、ドープDを円滑に繊維化することができるという極めて顕著な効果を奏する。   Thus, in the present invention, the flow velocity and flow rate of the coagulating liquid La flowing down in the flow tube 3 can be adjusted to desired values over the entire length of the flow tube. For this reason, the dope D spun from the spinneret 1 can be run together with a coagulating liquid having a controlled flow velocity, flow rate, temperature, and solvent concentration flowing down in the flow tube 3, thereby allowing the dope D to be extraneous. Thus, the fiberization rate of the dope D can be appropriately controlled without applying any additional tension. Therefore, there is an extremely remarkable effect that the dope D can be made into a fiber smoothly while suppressing the single fiber breakage that occurs in the coagulation liquid.

ここで、本発明に好適に使用できる凝固液としては、特公昭47−50219号公報、特開平7−309958号公報などに記載されている周知のもの、例えば塩化カルシウム、塩化リチウム、塩化ナトリウム、塩化マグネシウム、塩化亜鉛、塩化ストロンチウム、塩化アルミニウム、塩化第2スズ、塩化ニッケル、臭化カルシウム、硝酸亜鉛及び硝酸アルミニウムよりなる群から選ばれた無機塩類の少なくとも1種を含有し、水1リットルに対する上記塩類の全含有量が少なくとも2モル(無水塩換算濃度)である水性凝固液を例示することができる。しかしながら、これらに制限されるものではなく、これら以外のものであっても、本発明の要旨を満足される限り利用することができることは言うまでもない。   Here, as the coagulating liquid that can be suitably used in the present invention, known ones described in JP-B-47-50219, JP-A-7-309958, etc., such as calcium chloride, lithium chloride, sodium chloride, Contains at least one inorganic salt selected from the group consisting of magnesium chloride, zinc chloride, strontium chloride, aluminum chloride, stannic chloride, nickel chloride, calcium bromide, zinc nitrate, and aluminum nitrate, per liter of water Examples thereof include an aqueous coagulation liquid in which the total content of the salts is at least 2 mol (anhydrous salt equivalent concentration). However, it is not limited thereto, and it goes without saying that other than these can be used as long as the gist of the present invention is satisfied.

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、凝固液注入器5を備えて、これにより流管3中に流管内の凝固液Lの濃度及び温度を途中で変えることができることである。そこで、以下に、この凝固液注入器5によって流管3を流下する凝固液の濃度及び温度を変える方法と装置について詳細に説明する。   In the dry-wet spinning process in the series of yarn making processes as described above, the present invention is characterized in that, as already described, the coagulating liquid injector 5 is provided, thereby the flow tube 3. The concentration and temperature of the coagulating liquid L in the flow tube can be changed in the middle. Therefore, a method and apparatus for changing the concentration and temperature of the coagulating liquid flowing down the flow tube 3 by the coagulating liquid injector 5 will be described in detail below.

前述のように、流管3には、その内部を流れる凝固液の速度、流量、濃度および温度を調節するための凝固液注入器5を設ける。この凝固液注入器5には、流管3内に新たに追加するための凝固液Lbを供給する液入口部5aを有している。なお、この液入口部5aには、その濃度が予め調整された凝固液Lbが、温度制御装置6を介して供給される。   As described above, the flow tube 3 is provided with the coagulating liquid injector 5 for adjusting the speed, flow rate, concentration and temperature of the coagulating liquid flowing in the flow tube 3. The coagulating liquid injector 5 has a liquid inlet portion 5 a for supplying a coagulating liquid Lb to be newly added to the flow tube 3. The liquid inlet portion 5a is supplied with a coagulating liquid Lb whose concentration is adjusted in advance via the temperature control device 6.

ただし、この温度制御装置6は、凝固液注入器5へ供給する凝固液Lbを加熱及び/又は冷却する周知の加熱冷却手段を備えており、この加熱冷却手段によって凝固液Lbを所定の一定温度に制御して維持する。したがって、凝固液注入器5の液入口部5aに供給される凝固液Lbは、貯液部5bを介して液注入部5cから流管3の周りを取り囲んだ状態で、予め設定された温度と濃度を維持して全周方向から流管3内へ安定的に一定流量に計量された状態で注入される。   However, the temperature control device 6 includes a known heating / cooling means for heating and / or cooling the coagulating liquid Lb supplied to the coagulating liquid injector 5, and the coagulating liquid Lb is heated to a predetermined constant temperature by the heating / cooling means. Control and maintain. Accordingly, the coagulating liquid Lb supplied to the liquid inlet portion 5a of the coagulating liquid injector 5 has a preset temperature in a state of surrounding the flow tube 3 from the liquid injecting portion 5c via the liquid storage portion 5b. The liquid is injected in a state of being stably metered at a constant flow rate from the entire circumference direction into the flow tube 3 while maintaining the concentration.

このとき、流管3内をドープDと共に凝固液注入器5の設置位置まで流下する凝固液Laは、流管3内を流下する間にドープDに含まれた有機溶剤が凝固液La中へ抽出されてその濃度は当初濃度よりも上昇している。また、この凝固液Laの温度が、ドープDの温度よりも低いと、ドープDから凝固液Laに伝達された熱によって凝固液Laの温度が上昇する。   At this time, the coagulating liquid La flowing down to the installation position of the coagulating liquid injector 5 together with the dope D in the flow tube 3, the organic solvent contained in the dope D into the coagulating liquid La while flowing in the flow pipe 3. The extracted concentration is higher than the initial concentration. When the temperature of the coagulating liquid La is lower than the temperature of the dope D, the temperature of the coagulating liquid La rises due to the heat transferred from the dope D to the coagulating liquid La.

そうすると、このまま状態で流管3内の凝固液Lbを流下させると、ドープDから溶剤を凝固液Lb中に抽出する効率が低下し、ドープDに含まれる有機溶剤濃度が目標濃度まで到達させるのに時間を要してしまう。そのため、有機溶剤濃度を短時間でその品質を維持しながらドープDに含まれる溶剤濃度を目標濃度まで低下させることが困難となる。特に、繊維化する糸条を構成する単繊維の本数(フィラメント数)が多くなればなるほど、流管3内の濃度および温度上昇は著しくなるため、得られる繊維の物性の低下を招く。   Then, if the coagulation liquid Lb in the flow tube 3 is caused to flow down in this state, the efficiency of extracting the solvent from the dope D into the coagulation liquid Lb is reduced, and the concentration of the organic solvent contained in the dope D reaches the target concentration. It takes time. Therefore, it is difficult to reduce the solvent concentration contained in the dope D to the target concentration while maintaining the organic solvent concentration in a short time. In particular, as the number of single fibers (the number of filaments) constituting the yarn to be fiberized increases, the concentration and temperature rise in the flow tube 3 become more significant, leading to a decrease in the physical properties of the resulting fiber.

そこで、凝固液注入器5の液注入部5cから濃度および温度の異なる追加凝固液Lbを供給して、流管3内を流れてきた凝固液Laに混合注入することによって、凝固液の濃度および温度を調節する。なお、凝固液注入器5から注入される凝固液Lbの条件は、一般的に凝固液Laの到達濃度に追加凝固液Lbの溶液を混ぜ合わせたときの混合液の濃度が凝固液Lの濃度と同等またはそれ以下であることが望ましい。   Therefore, by supplying additional coagulating liquid Lb having different concentrations and temperatures from the liquid injection part 5c of the coagulating liquid injector 5, and mixing and injecting the coagulating liquid La flowing in the flow tube 3, the concentration of the coagulating liquid and Adjust the temperature. The condition of the coagulating liquid Lb injected from the coagulating liquid injector 5 is generally that the concentration of the mixed liquid when the solution of the additional coagulating liquid Lb is mixed with the concentration of the coagulating liquid La is the concentration of the coagulating liquid L. It is desirable to be equal to or less than.

その際、背景技術欄で説明した理由から、流管3内を流下してきた凝固液Laの流速を急激に変えることがないようにする必要がある。そのため、流管3と凝固液注入器5の上部の接続部は急激な径変化がないことが望ましい。   At that time, for the reason described in the background art column, it is necessary to prevent the flow rate of the coagulating liquid La flowing down in the flow tube 3 from changing abruptly. Therefore, it is desirable that the connecting portion at the upper part of the flow tube 3 and the coagulating liquid injector 5 does not have a sudden diameter change.

また、凝固液Lbを供給する液注入部5cに関しては、この液注入部5cから流管3を取り囲んでその全周方向から凝固液Lbの供給を行う役割を果たすが、その際、凝固液Lbは、流下してきた凝固液Laの流れを擾乱することなく、流管3中へ均一に供給されることが望ましい。したがって、これを具現化するために、液注入部5cは濾過媒体として使用される周知の金属細線からなる織編物あるいは多孔質焼結金属のような均圧化効果と整流効果を併せ持つ部材で形成しておくことが望ましい。   Further, regarding the liquid injection part 5c for supplying the coagulation liquid Lb, the liquid injection part 5c surrounds the flow tube 3 and plays a role of supplying the coagulation liquid Lb from the entire circumferential direction. Is preferably supplied uniformly into the flow tube 3 without disturbing the flow of the coagulating liquid La flowing down. Therefore, in order to realize this, the liquid injection part 5c is formed of a member having both a pressure equalizing effect and a rectifying effect, such as a woven or knitted fabric made of a well-known fine metal wire used as a filtration medium or a porous sintered metal. It is desirable to keep it.

特に、液注入部5cから安定的に且つ均一に凝固液Lbを供給するためには、前記整流部材での流体による抵抗がある程度以上必要で、織編物で例示するなら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。但し、本発明においては前記織編物あるいは多孔質焼結金属に限定する理由はなく、本発明の要旨を満足する限りにおいて、均圧化及び/又は整流化効果が得られるもの、例えば不織布、穴開きプレート等を用いることもできる。   In particular, in order to supply the coagulation liquid Lb stably and uniformly from the liquid injection part 5c, the resistance by the fluid in the rectifying member is required to some extent. One or more open woven or knitted fabrics may be used in combination. However, in the present invention, there is no reason to limit to the woven or knitted fabric or the porous sintered metal, and as long as the gist of the present invention is satisfied, a material capable of obtaining a pressure equalizing and / or rectifying effect, such as a nonwoven fabric, a hole, etc. An opening plate or the like can also be used.

なお、前記液注入部5cは、供給する凝固液Lbの均圧化と整流を兼用する部材とする必要は必ずしも無く、これらの機能を別々に果たすことができるような構成としてもよい。例えば、整流効果を奏する整流部材として、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を設け、更に均圧化部材としてその空隙率が適切に制御されたセラミックスあるいは金属からなる微粒子粉末を焼結した焼結体を別々に設けるようにしてもよい。   The liquid injection part 5c does not necessarily have to be a member for both equalizing and rectifying the coagulating liquid Lb to be supplied, and may be configured to perform these functions separately. For example, as a rectifying member having a rectifying effect, a screen having excellent fluid permeability such as a perforated plate, a honeycomb plate, a woven or knitted fabric is provided, and further, a ceramic or metal whose porosity is appropriately controlled as a pressure equalizing member. You may make it provide separately the sintered compact which sintered the fine particle powder which becomes.

また、前記液注入部5cの形状に関しては、流管3を流下してきた凝固液Laの流速を急激に変化させないようにすることが好ましく、このために流管3内に注入された凝固液Lbの流量増加分を考慮して、流管3内の平均流速が一定となるよう下流側に向かって錐状に末広がりとなる形状とすることが望ましい。   As for the shape of the liquid injection part 5c, it is preferable not to change the flow rate of the coagulating liquid La flowing down the flow tube 3 rapidly. For this purpose, the coagulated liquid Lb injected into the flow tube 3 is used. In consideration of the increase in the flow rate, it is desirable to have a shape that expands in a conical shape toward the downstream side so that the average flow velocity in the flow tube 3 is constant.

この発明によって、本発明者等は、図1及び図2に例示したような濃度および凝固液注入器5を有することを特徴とした流管の装置を用いることにより、流管3内を通過するドープDの有機溶剤濃度を効率的かつ物性に影響をおよぼさない装置を着想するに至ったものである。このため、紡糸口金1から吐出され凝固浴の液面Sから着水した糸条Yは、凝固液注入器5で供給する凝固液Lbにより適正な濃度および温度プロファイルを持つ流管3内の凝固液を得ることによって、最終的に得られる糸条Yの単繊維の切れや品質のバラツキも小さくできる。   By this invention, the inventors pass through the flow tube 3 by using a flow tube device characterized by having a concentration and coagulation liquid injector 5 as illustrated in FIGS. The present inventors have come up with an apparatus that efficiently controls the organic solvent concentration of the dope D and does not affect the physical properties. For this reason, the yarn Y discharged from the spinneret 1 and landed from the liquid surface S of the coagulation bath is coagulated in the flow tube 3 having an appropriate concentration and temperature profile by the coagulation liquid Lb supplied by the coagulation liquid injector 5. By obtaining the liquid, it is possible to reduce the breakage of single fibers of the yarn Y finally obtained and the variation in quality.

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. 本発明の流管の一実施形態例を模式的に示した断面図である。It is sectional drawing which showed typically the example of 1 embodiment of the flow tube of this invention.

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
4 糸条の引取手段
5 凝固液注入器
5a 凝固液の供給部
5b 凝固液の貯液部
5c 凝固液の注入部
D ドープ
L 凝固浴へ供給される凝固液
La 凝固浴から流管中へ供給される凝固液
Lb 凝固液注入器から供給される凝固液
G エアギャップ
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 collection means 2e Weir 3 Flow pipe 4 Yarn take-up means 5 Coagulation liquid injector 5a Coagulation liquid supply part 5b Coagulating liquid storage section 5c Coagulating liquid injection section D Dope L Coagulating liquid supplied to coagulating bath La Coagulating liquid supplied from coagulating bath into flow tube Lb Coagulating liquid supplied from coagulating liquid injector G Air gap S Coagulation bath surface Y Yarn

Claims (9)

多数の紡糸孔群が穿設された紡糸口金から紡糸原液を気体中へ紡出した後、引き続いて流管中を流下する凝固液中に前記紡糸原液を導入して凝固させて繊維化し、繊維化した糸条を引き取る乾湿式紡糸方法において、前記流管の途中から凝固液に含まれる溶剤濃度の異なる凝固液を注入し、流管内を流下する凝固液の濃度を調整することを特徴とする湿式紡糸方法。   After spinning the spinning stock solution into a gas from a spinneret having a large number of spinning hole groups, the spinning solution is introduced into the coagulating solution flowing down in the flow tube and then coagulated to form fibers. In the dry-wet spinning method for pulling out the converted yarn, the coagulating liquid having a different solvent concentration contained in the coagulating liquid is injected from the middle of the flow pipe, and the concentration of the coagulating liquid flowing down in the flow pipe is adjusted. Wet spinning method. 流管を流下する前記凝固液の温度と異なる温度に維持された凝固液を前記流管の途中から流管内に注入し、流管内を流下する凝固液の温度を調整することを特徴とする請求項1記載の湿式紡糸方法。   The coagulating liquid maintained at a temperature different from the temperature of the coagulating liquid flowing down the flow tube is injected into the flow tube from the middle of the flow tube, and the temperature of the coagulating liquid flowing down in the flow tube is adjusted. Item 2. The wet spinning method according to Item 1. 前記流管の途中から供給する凝固液の流量によって、凝固液の注入位置まで流下する凝固液の流速及び/又は流量を制御することを特徴とする請求項1又は2に記載の湿式紡糸方法。   The wet spinning method according to claim 1 or 2, wherein the flow rate and / or flow rate of the coagulating liquid flowing down to the coagulating liquid injection position is controlled by the flow rate of the coagulating liquid supplied from the middle of the flow tube. 全芳香族ポリアミド繊維を乾湿式紡糸することを特徴とする請求項1〜3の何れかに記載の湿式紡糸方法。   The wet spinning method according to any one of claims 1 to 3, wherein the wholly aromatic polyamide fiber is dry-wet spun. 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、前記液面より下方に浸漬させて前記凝固浴中に設けられた前記凝固液が流下する流管と、前記流管の途中から新鮮な凝固液を流管中へ注入する凝固液注入器と、前記流管の下方に設けられた糸条の引取手段とを少なくとも備えた乾湿式紡糸装置。   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; A flow tube in which the coagulating liquid is immersed below the liquid surface and flows down in the coagulating bath; a coagulating liquid injector for injecting fresh coagulating liquid into the flow tube from the middle of the flow tube; A dry-wet spinning apparatus comprising at least a yarn take-up means provided below the flow tube. 流管の途中で注入する前記凝固液の温度を一定に制御する温度制御装置を備えたことを特徴とする請求項5に記載の湿式紡糸装置。   6. The wet spinning apparatus according to claim 5, further comprising a temperature control device for controlling the temperature of the coagulating liquid injected in the middle of the flow tube to be constant. 流管内へ凝固液を注入する前記凝固液注入器の液注入部に、前記液注入部に凝固液の注入圧力を均圧化する均圧化部材を設けた請求項5又は6に記載の湿式紡糸装置。   The wet method according to claim 5 or 6, wherein a pressure equalizing member for equalizing an injection pressure of the coagulating liquid is provided in the liquid injecting part of the coagulating liquid injector for injecting the coagulating liquid into the flow tube. Spinning device. 流管内へ凝固液を注入する前記凝固液注入器の液注入部に、前記液注入部に凝固液を整流する整流部材を設けた請求項5〜7の何れかに記載の湿式紡糸装置。   The wet spinning device according to any one of claims 5 to 7, wherein a rectifying member that rectifies the coagulating liquid is provided in the liquid injecting portion of the coagulating liquid injector that injects the coagulating liquid into the flow tube. 流管内へ凝固液を注入する前記凝固液注入器の液注入部の形状を下流方向に沿って錐状に末広がりとした請求項5〜8の何れかに記載の湿式紡糸装置。   The wet spinning device according to any one of claims 5 to 8, wherein the shape of the liquid injection portion of the coagulation liquid injector for injecting the coagulation liquid into the flow tube is conically diverged along the downstream direction.
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JP2008208480A (en) * 2007-02-26 2008-09-11 Teijin Techno Products Ltd Apparatus for producing aromatic copolyamide fiber
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JP2009179924A (en) * 2008-02-01 2009-08-13 Teijin Techno Products Ltd Dry-wet spinning apparatus
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CN110871037A (en) * 2018-08-30 2020-03-10 中国石油化工股份有限公司 Hollow fiber separation membrane and preparation method thereof
CN110871036B (en) * 2018-08-30 2022-10-21 中国石油化工股份有限公司 Hollow fiber membrane solidification equipment and method

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