JPWO2016114385A1 - Acrylic fiber bundle manufacturing method and pressurized steam drawing apparatus - Google Patents

Acrylic fiber bundle manufacturing method and pressurized steam drawing apparatus Download PDF

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JPWO2016114385A1
JPWO2016114385A1 JP2016504231A JP2016504231A JPWO2016114385A1 JP WO2016114385 A1 JPWO2016114385 A1 JP WO2016114385A1 JP 2016504231 A JP2016504231 A JP 2016504231A JP 2016504231 A JP2016504231 A JP 2016504231A JP WO2016114385 A1 JPWO2016114385 A1 JP WO2016114385A1
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steam
fiber bundle
filtration
pressurized
acrylic fiber
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旭成 多田
旭成 多田
由貴廣 水鳥
由貴廣 水鳥
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Mitsubishi Chemical Corp
Mitsubishi Rayon Co Ltd
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Mitsubishi Rayon Co Ltd
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    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02JFINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/22Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B23/00Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
    • D06B23/14Containers, e.g. vats
    • D06B23/16Containers, e.g. vats with means for introducing or removing textile materials without modifying container pressure

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Artificial Filaments (AREA)
  • Treatment Of Fiber Materials (AREA)

Abstract

加圧スチームを濾過し、濾過後の前記加圧スチームを加圧スチーム延伸装置の蒸気室に供給しながら、前記蒸気室内にアクリル繊維束を走行させて延伸処理をする、アクリル繊維束の製造方法、及び、蒸気室に供給する加圧スチームを濾過して異物を除去する濾過装置を備えたスチーム延伸装置。A method for producing an acrylic fiber bundle, in which the pressurized steam is filtered, and the filtered steam is supplied to the steam chamber of a pressurized steam stretching apparatus, and the acrylic fiber bundle is run in the steam chamber for stretching. And a steam stretching device provided with a filtration device for filtering the pressurized steam supplied to the steam chamber to remove foreign substances.

Description

本発明は、加圧スチーム延伸工程を有するアクリル繊維束の製造方法ならび加圧スチーム延伸装置に関する。さらに詳しくはアクリル繊維束を高速、高倍率で安定に延伸する加圧スチーム延伸工程を有するアクリル繊維束の製造方法に関するものである。
本願は、2015年1月16日に、日本に出願された特願2015−006470号に基づき優先権を主張し、その内容をここに援用する。
The present invention relates to a method for producing an acrylic fiber bundle having a pressurized steam stretching process and a pressurized steam stretching apparatus. More specifically, the present invention relates to a method for producing an acrylic fiber bundle having a pressurized steam stretching process for stably stretching an acrylic fiber bundle at a high speed and a high magnification.
This application claims priority on January 16, 2015 based on Japanese Patent Application No. 2015-006470 for which it applied to Japan, and uses the content here.

アクリル繊維束を延伸する方法として、加圧スチーム中でアクリル繊維束を延伸する技術が、従来から用いられてきた。加圧スチームを用いれば、大気圧下の熱水より高温が得られ、さらに水分がアクリル繊維束に対して可塑剤として作用するため、アクリル繊維束を高倍率に延伸することが可能となる。特に、炭素繊維の前駆体として使用されるアクリル繊維束は、主成分であるアクリロニトリル系重合体が明確な融点をもたないため、アクリル繊維束を単に高温下で延伸するだけでは、延伸が不均一になる場合や、繊維が破断する場合があり、加圧スチーム下でアクリル繊維束を可塑化しながら延伸する方法(以下、「スチーム延伸」と略する)が提案されてきた。   As a method of stretching the acrylic fiber bundle, a technique of stretching the acrylic fiber bundle in pressurized steam has been used conventionally. If pressurized steam is used, a higher temperature than hot water under atmospheric pressure is obtained, and moisture acts as a plasticizer on the acrylic fiber bundle, so that the acrylic fiber bundle can be stretched at a high magnification. In particular, an acrylic fiber bundle used as a carbon fiber precursor does not have a clear melting point because an acrylonitrile-based polymer as a main component does not have a clear melting point. In some cases, the fiber may break or the fiber may break, and a method of stretching an acrylic fiber bundle while plasticizing under pressure steam (hereinafter, abbreviated as “steam stretching”) has been proposed.

しかしながら、アクリル繊維束をスチーム延伸で高倍率に延伸すると、スチーム延伸中に単繊維が切断したり、アクリル繊維束が切断したりしてしまう場合があった。また、高倍率でスチーム延伸したアクリル繊維束を焼成して得られた炭素繊維束においては、焼成処理中に単繊維が切断して生じた毛羽が加わる場合があった。特に、細繊度の炭素繊維を製造する場合や、より高速でスチーム延伸を行う場合は、その問題が更に顕著に発生した。   However, when the acrylic fiber bundle is drawn at a high magnification by steam drawing, the single fiber may be cut or the acrylic fiber bundle may be cut during the steam drawing. Further, in the carbon fiber bundle obtained by firing the acrylic fiber bundle that has been steam-stretched at a high magnification, fluff generated by cutting the single fiber during the firing treatment may be added. In particular, when producing fine carbon fibers or when performing steam drawing at a higher speed, the problem occurred more remarkably.

加圧スチームを使用する延伸装置において、安定にスチーム延伸を行うために、これまでに糸条を予熱するスチームボックスを通した後に、スチーム延伸機に導入する方法(特許文献1)やスチーム延伸する前の糸条に対して流体処理を施して糸条を開繊したのち延伸する方法(特許文献2)が開示されている。   In a stretching apparatus using pressurized steam, in order to perform stable steam stretching, after passing through a steam box that preheats the yarn so far, a method of introducing into a steam stretching machine (Patent Document 1) or steam stretching. A method (Patent Document 2) is disclosed in which a fluid treatment is applied to a previous yarn to open the yarn and then stretch the yarn.

特開平8−246284号公報JP-A-8-246284 特開平11−12874号公報Japanese Patent Laid-Open No. 11-12874

特許文献1は、シリコーン系の油剤が付与されその撥水作用により、スチームの伝熱が得られ難くなるアクリル繊維束でも、スチームボックスで予熱されるので、伝熱不足による毛羽の発生を防ぐ効果があり、特許文献2は、スチーム延伸工程に先立って処理される、油剤付着工程、乾燥緻密化工程で生じる、糸条の単糸間接着により、スチームの伝熱が得られ難くなるアクリル繊維束でも、高い倍率で延伸することが可能になる効果はある。しかしながら、これらの方法を用いても、毛羽の発生は十分に防止されてはいなかった。   Patent Document 1 has an effect of preventing the occurrence of fluff due to insufficient heat transfer because an acrylic fiber bundle, to which a silicone-based oil agent is applied and the water repellent action makes it difficult to obtain heat transfer of steam, is preheated in a steam box. Patent Document 2 describes an acrylic fiber bundle that is processed prior to the steam drawing step, and that makes it difficult to obtain heat transfer of steam due to the inter-single yarn adhesion that occurs in the oil agent attaching step and the drying densification step. However, there is an effect that the film can be stretched at a high magnification. However, even if these methods were used, the generation of fluff was not sufficiently prevented.

本願発明の発明者らは、上記課題を解決すべく鋭意検討した結果、加圧スチーム延伸装置に供給するスチームには、多くの異物が含まれていることを見出すとともに、濾過装置を用いて、スチーム中の当該異物を除去した後のスチームを用いて、アクリル繊維束のスチーム延伸を行うことにより、炭素繊維束の毛羽の発生が顕著に低減することを見出し、本発明に至った。   The inventors of the present invention have intensively studied to solve the above problems, and as a result, the steam supplied to the pressurized steam stretching apparatus has been found to contain many foreign substances, and using a filtration device, It has been found that the occurrence of fluff in the carbon fiber bundle is significantly reduced by performing steam stretching of the acrylic fiber bundle using the steam after removing the foreign matters in the steam, and the present invention has been achieved.

なお、ここで異物とは、スチームが加圧スチーム延伸装置に供給されるまでに経由する各種配管や工程設備に由来する金属及び/又は金属酸化物をさす。   In addition, a foreign material means the metal and / or metal oxide which originate in the various piping and process equipment which go through until steam is supplied to a pressurized steam extending | stretching apparatus here.

本発明の課題は、従来技術の欠点を改善し、毛羽の発生を大幅に改善した炭素繊維を得るための、アクリル繊維束の製造方法と加圧スチーム延伸装置を提供することにある。   An object of the present invention is to provide a method for producing an acrylic fiber bundle and a pressure steam drawing apparatus for obtaining carbon fibers that improve the disadvantages of the prior art and greatly improve the generation of fluff.

[1] 加圧スチームを濾過し、濾過後の前記加圧スチームを加圧スチーム延伸装置の蒸気室に供給しながら、前記蒸気室内にアクリル繊維束を走行させて延伸処理をする、アクリル繊維束の製造方法。
[2] 加圧スチームの濾過を、大きさ7μm以上の異物の異物捕捉率が90%以上である濾過材を備えた濾過装置を用いて行う、[1]に記載のアクリル繊維束の製造方法。
[3] 前記濾過後の加圧スチームは、大きさ50μm以上の異物の個数が0個/10mLである、[1]または[2]に記載のアクリル繊維束の製造方法。
[4] 前記濾過後の加圧スチームは、大きさ1μm以上の異物の個数が、3000個/10mL以下である、[1]〜[3]のいずれか一つに記載のアクリル繊維束の製造方法。
[5] 前記濾過後の加圧スチームは、大きさ4μm以上の異物の個数が、500個/10mL以下である、[1]〜[4]のいずれか一つに記載のアクリル繊維束の製造方法。
[6] 前記蒸気室は、ラビリンスシールを通じて蒸気室内部の加圧スチームを排出するものである、[1]〜[5]のいずれか一つに記載のアクリル繊維束の製造方法。
[7] 前記濾過後の加圧スチームを、前記加圧スチーム延伸装置内を走行するアクリル繊維束に直接吹きつける、[1]〜[6]のいずれか一つに記載のアクリル繊維束の製造方法。
[8] 繊維の送入口、蒸気室、及び、延伸処理された繊維の送出口を有し、加圧スチームを前記蒸気室に供給しながら、前記蒸気室内に繊維を走行させて延伸処理をする加圧スチーム延伸装置であって、濾過装置を有し、前記濾過装置を用いて濾過した加圧スチームを前記蒸気室内に供給する加圧スチーム延伸装置。
[9] 濾過装置として、大きさ7μm以上の異物の異物捕捉率が90%以上である濾過材を備えた濾過装置を有する、[8]に記載の加圧スチーム延伸装置。
[10] 濾過装置として、前記濾過後の加圧スチームが、大きさ50μm以上の異物の個数が0個/10mLとなる濾過装置を有する、[8]または[9]に記載の加圧スチーム延伸装置。
[11] 濾過装置として、前記濾過後の加圧スチームが、大きさ1μm以上の異物の個数が、3000個/10mL以下となる濾過装置を有する、[8]〜[10]のいずれか一つに記載の加圧スチーム延伸装置。
[12] 濾過装置として、前記濾過後の加圧スチームが、大きさ4μm以上の異物の個数が、500個/10mL以下となる濾過装置を有する、[8]〜[11]のいずれか一つに記載の加圧スチーム延伸装置。
[13] 前記送入口と前記蒸気室の間と、前記送出口と前記蒸気室の間のそれぞれに前記蒸気室内部の加圧スチームを排出するラビリンスシールを有する、[8]〜[12]のいずれか一つに記載の加圧スチーム延伸装置。
[14] 前記濾過後の加圧スチームを、前記蒸気室内を走行するアクリル繊維束に直接吹きつける、[8]〜[13]のいずれか一つに記載の加圧スチーム延伸装置。
[1] Acrylic fiber bundle that is subjected to a stretching treatment by running the acrylic fiber bundle in the steam chamber while filtering the pressurized steam and supplying the filtered pressurized steam to the steam chamber of the pressurized steam stretching apparatus. Manufacturing method.
[2] The method for producing an acrylic fiber bundle according to [1], wherein the filtration of the pressurized steam is performed using a filtration apparatus including a filtering material having a foreign matter capturing rate of 90% or more of foreign matters having a size of 7 μm or more. .
[3] The method for producing an acrylic fiber bundle according to [1] or [2], wherein the pressure steam after the filtration is 0/10 mL of foreign matters having a size of 50 μm or more.
[4] The production of the acrylic fiber bundle according to any one of [1] to [3], wherein the pressure steam after the filtration has a number of foreign matters having a size of 1 μm or more of 3000 pieces / 10 mL or less. Method.
[5] The production of the acrylic fiber bundle according to any one of [1] to [4], wherein the pressure steam after the filtration has a number of foreign matters having a size of 4 μm or more of 500 pieces / 10 mL or less. Method.
[6] The method for manufacturing an acrylic fiber bundle according to any one of [1] to [5], wherein the steam chamber discharges pressurized steam in the steam chamber through a labyrinth seal.
[7] Production of acrylic fiber bundle according to any one of [1] to [6], wherein the pressurized steam after filtration is directly sprayed onto the acrylic fiber bundle running in the pressurized steam stretching apparatus. Method.
[8] It has a fiber inlet / outlet, a steam chamber, and an outlet / outlet of a stretched fiber, and while the pressurized steam is supplied to the steam chamber, the fiber travels in the steam chamber to perform the stretching process. A pressurized steam stretching apparatus, comprising a filtration device, for supplying pressurized steam filtered using the filtration device into the steam chamber.
[9] The pressurized steam stretching apparatus according to [8], including a filtering device including a filtering material having a foreign matter capturing rate of 90% or more as a filtering device.
[10] Pressurized steam stretching according to [8] or [9], wherein the filtered steam has a filtering device in which the number of foreign matters having a size of 50 μm or more is 0/10 mL. apparatus.
[11] Any one of [8] to [10], wherein the pressure steam after filtration has a filtration device in which the number of foreign matters having a size of 1 μm or more is 3000 pieces / 10 ml or less. The pressurized steam stretching apparatus according to 1.
[12] As the filtration device, any one of [8] to [11], wherein the pressurized steam after the filtration has a filtration device in which the number of foreign matters having a size of 4 μm or more is 500 pieces / 10 mL or less. The pressurized steam stretching apparatus according to 1.
[13] The labyrinth seal for discharging pressurized steam in the steam chamber is provided between the inlet and the steam chamber and between the outlet and the steam chamber, respectively, according to [8] to [12] The pressurized steam stretching apparatus according to any one of the above.
[14] The pressurized steam stretching apparatus according to any one of [8] to [13], wherein the filtered pressurized steam is directly blown onto an acrylic fiber bundle traveling in the steam chamber.

本発明の要旨は、アクリル繊維束を、蒸気室内を走行させながら、連続的に延伸処理するアクリル繊維束の製造方法であって、下記(1)〜(3)を満たすことを特徴とする。
(1)前記蒸気室は、加圧スチームが導入される蒸気導入口を有する。
(2)前記蒸気導入口に連結する濾過装置を有する。
(3)スチームを前記濾過装置を用いて濾過した後、蒸気導入口から前記蒸気室に、前記濾過後の加圧スチームを供給する。
The gist of the present invention is an acrylic fiber bundle manufacturing method in which an acrylic fiber bundle is continuously stretched while running in a steam chamber, and is characterized by satisfying the following (1) to (3).
(1) The steam chamber has a steam inlet through which pressurized steam is introduced.
(2) It has a filtration device connected to the steam inlet.
(3) After filtering the steam using the filtration device, the pressurized steam after the filtration is supplied from the steam inlet to the steam chamber.

本発明の要旨は、アクリル繊維束を、蒸気室内を走行させながら、連続的に延伸処理する加圧スチーム延伸装置であって、下記(6)〜(8)を満たすことを特徴とする。
(6)前記蒸気室は、加圧スチームが導入される蒸気導入口を有する。
(7)前記蒸気導入口に連結する濾過装置を有する。
(8)スチームを前記濾過装置を用いて濾過した後、蒸気導入口から前記蒸気室に、前記濾過後の加圧スチームを供給する。
The gist of the present invention is a pressurized steam stretching apparatus that continuously stretches an acrylic fiber bundle while traveling in a steam chamber, and is characterized by satisfying the following (6) to (8).
(6) The steam chamber has a steam inlet through which pressurized steam is introduced.
(7) It has a filtration device connected to the steam inlet.
(8) After filtering the steam using the filtration device, the pressurized steam after the filtration is supplied from the steam inlet to the steam chamber.

本発明により、毛羽の発生が大幅に改善された高品質の炭素繊維を得ることができる。   According to the present invention, it is possible to obtain a high-quality carbon fiber in which the generation of fluff is greatly improved.

本発明の加圧スチーム延伸装置の一例を示す概略図。Schematic which shows an example of the pressurized steam extending | stretching apparatus of this invention. 本発明の加圧スチーム延伸装置の一例を示す概略図。Schematic which shows an example of the pressurized steam extending | stretching apparatus of this invention. 図2の加圧スチーム延伸装置の内部を示す図。The figure which shows the inside of the pressurized steam extending | stretching apparatus of FIG. 図2の加圧スチーム延伸装置の内部を示す図。The figure which shows the inside of the pressurized steam extending | stretching apparatus of FIG.

以下、本発明を詳細に説明する。   Hereinafter, the present invention will be described in detail.

本発明のアクリル繊維束の製造方法及び加圧スチーム延伸装置においては、加圧スチーム延伸(加圧スチーム延伸処理ともいう)を行うことができる。
加圧スチーム延伸とは、大気圧超の圧力を有するスチームを利用して対象物を延伸することをいう。
加圧スチームとは、加圧スチーム延伸工程に用いるスチームのことをいい、単にスチームともいう。
In the method for producing an acrylic fiber bundle and the pressure steam stretching apparatus of the present invention, pressure steam stretching (also referred to as pressure steam stretching treatment) can be performed.
Pressurized steam stretching refers to stretching an object using steam having a pressure exceeding atmospheric pressure.
Pressurized steam refers to steam used in the pressurized steam stretching process, and is also simply referred to as steam.

本発明の製造方法を適用できる範囲は、繊維の種類、製造工程等により特に限定されない。本発明の製造方法は、高い紡糸速度を要求される場合に有効であり、特にアクリル繊維束や炭素繊維前駆体束等の繊維束の細繊度化延伸の高倍率化及び高速化に適する。さらに、複数の繊維束を一括で延伸処理する場合に好適である。   The range to which the production method of the present invention can be applied is not particularly limited by the type of fiber, the production process, and the like. The production method of the present invention is effective when a high spinning speed is required, and is particularly suitable for increasing the magnification and increasing the speed of finer drawing of fiber bundles such as acrylic fiber bundles and carbon fiber precursor bundles. Furthermore, it is suitable when a plurality of fiber bundles are stretched together.

本発明の製造方法において、加圧スチーム延伸処理を行う工程(加圧スチーム延伸工程)の前後には、繊維を製造する技術分野において公知の処理工程を適宜設置できる。例えば、アクリル繊維を溶液紡糸する場合は、アクリロニトリル系(共)重合体を公知の有機溶剤又は無機溶剤に溶解した重合体溶液を、紡糸して凝固糸とする紡糸工程の後、凝固糸を延伸する工程において本発明の加圧スチーム延伸工程を配置することができる。この場合、紡糸工程は、いわゆる湿式法、乾湿式法、乾式法のいずれの紡糸方法を用いることができる。また、紡糸工程の後に、脱溶剤処理、浴中延伸処理、油剤付着処理、乾燥処理を行う工程を配置することができる。   In the production method of the present invention, before and after the step of performing the pressurized steam stretching process (pressurized steam stretching process), a processing process known in the technical field of producing fibers can be appropriately installed. For example, in the case of solution spinning of acrylic fiber, after the spinning process in which a polymer solution in which acrylonitrile (co) polymer is dissolved in a known organic solvent or inorganic solvent is spun into a coagulated yarn, the coagulated yarn is drawn. In the step of performing, the pressurized steam stretching step of the present invention can be arranged. In this case, the spinning process can use any of the so-called wet method, dry wet method, and dry method. In addition, after the spinning process, a process of performing a solvent removal process, a stretching process in a bath, an oil agent attaching process, and a drying process can be arranged.

本発明の加圧スチーム延伸処理は、繊維製造のいかなる段階で実施してもよく、溶液紡糸を行う場合は、繊維束中に含まれる溶剤を目的に応じた溶剤含有量となるまで除去した後に行うことが好ましい。具体的には、洗浄処理後、浴中延伸処理後又は乾燥処理後に加圧スチーム延伸処理を行うことが好ましく、高配向の繊維を得る観点からは、乾燥処理後に行うことがより好ましい。   The pressurized steam drawing treatment of the present invention may be carried out at any stage of fiber production. When solution spinning is performed, the solvent contained in the fiber bundle is removed until the solvent content according to the purpose is reached. Preferably it is done. Specifically, it is preferable to perform a pressurized steam stretching process after the washing process, after the stretching process in the bath or after the drying process, and more preferably after the drying process from the viewpoint of obtaining highly oriented fibers.

本発明のアクリル繊維束の製造方法は、加圧スチームを濾過し、前記加圧スチームを加圧スチーム延伸装置の蒸気室に供給しながら、前記蒸気室内にアクリル繊維束を走行させて延伸処理をする、アクリル繊維束の製造方法である。
本発明のアクリル繊維束の製造方法の一つの態様は、アクリル繊維束を、加圧スチーム延伸装置の蒸気室内を走行させながら、連続的に延伸処理するアクリル繊維束の製造方法であって、下記(1)〜(3)を満たすことを特徴とする。
(1)前記蒸気室は、加圧スチームが導入される蒸気導入口を有する。
(2)前記蒸気導入口の前または後に連結する濾過装置を有する。
(3)前記濾過装置を用いて濾過した後の加圧スチームを前記蒸気室に供給する。
また、本発明の加圧スチーム延伸装置は、蒸気室及び濾過装置を有する。本発明の加圧スチーム延伸装置は、濾過後の加圧スチームを蒸気室に供給しながら、前記蒸気室内にアクリル繊維束を走行させて延伸処理をするものである。
In the method for producing an acrylic fiber bundle of the present invention, the pressurized steam is filtered, and while the pressurized steam is supplied to the steam chamber of the pressurized steam stretching apparatus, the acrylic fiber bundle is allowed to travel in the steam chamber to perform the stretching treatment. This is a method for producing an acrylic fiber bundle.
One aspect of the method for producing an acrylic fiber bundle according to the present invention is a method for producing an acrylic fiber bundle in which an acrylic fiber bundle is continuously stretched while being run in a steam chamber of a pressurized steam stretching apparatus. (1) to (3) are satisfied.
(1) The steam chamber has a steam inlet through which pressurized steam is introduced.
(2) It has a filtration device connected before or after the steam inlet.
(3) Supply pressurized steam after filtration using the filtration device to the vapor chamber.
The pressurized steam stretching apparatus of the present invention has a steam chamber and a filtration device. The pressurized steam stretching apparatus of the present invention performs stretching by running an acrylic fiber bundle in the steam chamber while supplying the pressurized steam after filtration to the steam chamber.

加圧スチーム延伸装置の蒸気室内のスチーム圧は、加圧状態すなわち大気圧より高い圧力となるように、目的に応じて適宜設定できる。すなわち延伸する繊維の種類、加圧スチーム延伸工程での処理状態、あるいは目的とする繊維特性等により適宜設定される。   The steam pressure in the steam chamber of the pressurized steam stretching apparatus can be appropriately set according to the purpose so as to be a pressurized state, that is, a pressure higher than the atmospheric pressure. That is, it is set as appropriate depending on the type of fiber to be stretched, the state of treatment in the pressurized steam stretching step, or the desired fiber characteristics.

蒸気室内の温度は、炭素繊維前駆体アクリル繊維を構成する高分子を可塑化し、延伸しやすくするために、120〜170℃とすることができる。120℃以上であれば可塑化の効果が得られる。蒸気室内の蒸気が飽和状態であれば、より可塑化の効果が得られる。   The temperature in the steam chamber can be set to 120 to 170 ° C. in order to plasticize the polymer constituting the carbon fiber precursor acrylic fiber and facilitate stretching. If it is 120 degreeC or more, the effect of plasticization will be acquired. If the steam in the steam chamber is saturated, a plasticizing effect can be obtained.

加圧スチーム延伸装置の蒸気室は、加圧スチームが導入される蒸気導入口を有し、蒸気導入口の前または後には濾過装置が連結している。本発明においては、前記濾過装置を用いて濾過した後の加圧スチームを、前記蒸気室に供給することが重要である。   The steam chamber of the pressurized steam stretching apparatus has a steam inlet through which pressurized steam is introduced, and a filtration device is connected before or after the steam inlet. In the present invention, it is important to supply pressurized steam after filtration using the filtration device to the steam chamber.

アクリル繊維束が、加圧スチーム延伸装置の蒸気室内を走行する場合、同繊維束を水平方向に走行させても良いし、垂直方向に走行させても良い。同繊維束を水平方向に走行させて、加圧スチームを同繊維束の走行方向に対して、略直交するように供給すれば、繊維束の延伸斑を低減できるので好ましい。   When the acrylic fiber bundle travels in the steam chamber of the pressurized steam stretching apparatus, the fiber bundle may travel in the horizontal direction or in the vertical direction. It is preferable to cause the fiber bundle to travel in the horizontal direction and supply pressurized steam so as to be substantially orthogonal to the traveling direction of the fiber bundle because stretch spots of the fiber bundle can be reduced.

また、本発明の製造方法および装置においては、濾過後の加圧スチームを蒸気室に供給するにあたり、前記濾過後のスチームを、加圧スチーム延伸装置中を走行するアクリル繊維束に直接吹きつける形式としてもよいし、直接吹き付けない形式としてもよい。加圧スチームをアクリル繊維束に直接吹きつける形式とする場合に、本発明の効果がより顕著なものとなる。   In addition, in the production method and apparatus of the present invention, when supplying the filtered pressurized steam to the steam chamber, the filtered steam is directly blown onto the acrylic fiber bundle running in the pressurized steam stretching apparatus. It is good also as a form which does not spray directly. The effect of the present invention becomes more remarkable when the pressurized steam is directly sprayed onto the acrylic fiber bundle.

さらに、本発明のアクリル繊維束の製造方法及び加圧スチーム延伸装置において、下記(4)及び(5)を満たすこともできる。
(4)前記蒸気室は、アクリル繊維束の送入口側と送出口側に連接したシール室を有し、該シール室により前記蒸気室内部を加圧状態に維持する。
(5)濾過後の加圧スチームを、前記シール室に供給する。
シール室を有することにより、蒸気室内の加圧スチームを徐々に排出することができ、前記蒸気室内部は加圧状態に維持される。前記濾過後の加圧スチームを、該シール室に供給することもできる。
シール室として、ラビリンスシールを用いることが好ましい。
Furthermore, the following (4) and (5) can be satisfied in the method for producing an acrylic fiber bundle and the pressurized steam stretching apparatus of the present invention.
(4) The steam chamber has a seal chamber connected to the inlet side and the outlet side of the acrylic fiber bundle, and the inside of the steam chamber is maintained in a pressurized state by the seal chamber.
(5) Supply pressurized steam after filtration to the seal chamber.
By providing the seal chamber, the pressurized steam in the steam chamber can be gradually discharged, and the inside of the steam chamber is maintained in a pressurized state. The pressurized steam after the filtration can be supplied to the seal chamber.
A labyrinth seal is preferably used as the seal chamber.

濾過装置を用いて異物が除去されたスチームを用いることで、スチーム中に含まれている異物がアクリル繊維束に衝突して、同繊維束中の単繊維が切断したり同繊維束に毛羽が発生すること等を避けることができ、アクリル繊維束のダメージを軽減する効果が得られる。   By using steam from which foreign matter has been removed using a filtration device, the foreign matter contained in the steam collides with the acrylic fiber bundle, and single fibers in the fiber bundle are cut or fluff is formed in the fiber bundle. Generation | occurrence | production etc. can be avoided and the effect which reduces the damage of an acrylic fiber bundle is acquired.

前記濾過装置に用いられる濾過材としては、大きさ7μm以上の異物の補足率が90%以上である濾過材を用いることが好ましく、大きさ2μm以上の異物の補足率が90%以上である濾過材を用いることがより好ましく、大きさ0.5μm以上の異物の補足率が90%以上である濾過材を用いることが更に好ましい。   As the filtering material used in the filtering device, it is preferable to use a filtering material having a capture rate of foreign matter having a size of 7 μm or more of 90% or more, and a filtration material having a capture rate of foreign matter having a size of 2 μm or more of 90% or more. It is more preferable to use a filter material, and it is even more preferable to use a filter medium in which the capture rate of foreign matters having a size of 0.5 μm or more is 90% or more.

より優れた効果を得るために、前記濾過装置に用いられる濾過材には、大きさ0.5μm以上の異物の異物捕捉率が95.0%以上の濾過材を用いることが好ましい。異物捕捉率が95.0%以上であれば、アクリル繊維束中の単繊維の切断や、同繊維束の毛羽の発生を、最終的に得られる炭素繊維束の品質や生産性を損なわないレベルにまで抑制できる。濾過材の異物捕捉率は97.0%以上がより好ましく、99.0%が特に好ましい。   In order to obtain a more excellent effect, it is preferable to use a filter medium having a foreign matter trapping rate of 95.0% or more for a foreign substance having a size of 0.5 μm or more as the filter medium used in the filtration device. If the foreign matter catching rate is 95.0% or higher, the level of the carbon fiber bundle that is finally obtained is not damaged by the single fiber cutting in the acrylic fiber bundle or the generation of fluff of the fiber bundle. It can be suppressed to. The foreign matter trapping rate of the filter medium is more preferably 97.0% or more, and particularly preferably 99.0%.

前記濾過装置で濾過処理された後のスチームに含まれる、大きさ50μm以上の異物個数が、0個/10mLであることが好ましい。スチーム中の大きさ50μm以上の異物個数が0個/10mLであれば、アクリル繊維束中の単繊維の切断や、同繊維束の毛羽の発生を、最終的に得られる炭素繊維束の品質や生産性を損なわないレベルにまで抑制できる。   It is preferable that the number of foreign matters having a size of 50 μm or more contained in the steam after being filtered by the filtering device is 0/10 mL. If the number of foreign matters having a size of 50 μm or more in steam is 0/10 mL, the quality of the carbon fiber bundle finally obtained can be determined by cutting single fibers in the acrylic fiber bundle or generating fluff in the fiber bundle. It can be suppressed to a level that does not impair productivity.

さらに、前記濾過装置で濾過処理された後のスチームに含まれる、大きさ1μm以上の異物個数が、3000個/10mL以下であることがより好ましく、500個/10mL以下であることがより好ましい。スチーム中の大きさ1μm以上の異物個数が3000個/10mL以下であれば、アクリル繊維束中の単繊維の切断や、同繊維束の毛羽の発生を、最終的に得られる炭素繊維束の品質や生産性を損なわないレベルにまで抑制できる。   Furthermore, the number of foreign matters having a size of 1 μm or more contained in the steam after being filtered by the filtration device is more preferably 3000 pieces / 10 mL or less, and more preferably 500 pieces / 10 mL or less. If the number of foreign matters having a size of 1 μm or more in the steam is 3000/10 mL or less, the quality of the carbon fiber bundle finally obtained by cutting the single fiber in the acrylic fiber bundle or generating the fluff of the fiber bundle And can be suppressed to a level that does not impair productivity.

前記濾過装置で濾過処理された後のスチームに含まれる、大きさ4μm以上の異物個数が、500個/10mL以下であることがより好ましく、350個/mL以下であることがより好ましい。スチーム中の大きさ4μm以上の異物個数が500個/10mL以下であれば、アクリル繊維束中の単繊維の切断や、同繊維束の毛羽の発生を、最終的に得られる炭素繊維束の品質や生産性を損なわないレベルにまで抑制できる。   The number of foreign matters having a size of 4 μm or more contained in the steam after being filtered by the filtration device is more preferably 500 pieces / mL or less, and more preferably 350 pieces / mL or less. If the number of foreign matters with a size of 4 μm or more in the steam is 500 pieces / 10 mL or less, the quality of the carbon fiber bundle finally obtained by cutting the single fiber in the acrylic fiber bundle or generating the fluff of the fiber bundle And can be suppressed to a level that does not impair productivity.

なお、本願において異物の大きさとは、レーザー光散乱・遮蔽(light obscuration)法で測定される異物の粒径を意味する。
大きさ1μm以上100μm未満の異物個数を大きさ1μm以上の異物個数とし、大きさ4μm以上100μm未満の異物個数を大きさ4μm以上の異物個数とし、大きさ50μm以上100μm未満の異物個数を大きさ50μm以上の異物個数とした。
In the present application, the size of the foreign matter means a particle size of the foreign matter measured by a laser light scattering / light obstruction method.
The number of foreign matters having a size of 1 μm or more and less than 100 μm is defined as the number of foreign matters having a size of 1 μm or more, the number of foreign matters having a size of 4 μm or more and less than 100 μm is defined as the number of foreign matters having a size of 4 μm or more. The number of foreign matters was 50 μm or more.

なお、スチームに含まれる異物個数は、下記の測定方法により測定する。凝縮水に含まれる異物とは、例えば金属、金属酸化物である。
<スチームに含まれる異物個数>
スチームを凝縮器に導入して、凝縮させた凝縮水を液中微粒子計測用のサンプルとする。液中微粒子計測器を用いて、前記凝縮水サンプル10mLに含まれる、特定の異物径の範囲内にある異物個数をレーザー光散乱・遮蔽(light obscuration)法で測定する。
The number of foreign matters contained in steam is measured by the following measuring method. The foreign substances contained in the condensed water are, for example, metals and metal oxides.
<Number of foreign substances contained in steam>
Steam is introduced into a condenser, and condensed condensed water is used as a sample for measuring fine particles in liquid. Using a submerged particle measuring instrument, the number of foreign matters within a specific foreign matter diameter contained in the 10 mL of the condensed water sample is measured by a laser light scattering / shielding method.

上記の方法で得られたアクリル繊維束を、200〜300℃の酸性化雰囲気中で耐炎化処理した後、400〜900℃の不活性雰囲気中で前炭素化処理し、次いで、1200〜2500℃の不活性雰囲気中で炭素化処理を行い炭素繊維束を得ることができる。   The acrylic fiber bundle obtained by the above method is flameproofed in an acidified atmosphere at 200 to 300 ° C, then pre-carbonized in an inert atmosphere at 400 to 900 ° C, and then 1200 to 2500 ° C. A carbon fiber bundle can be obtained by performing carbonization treatment in an inert atmosphere.

本発明の製造方法及び加圧スチーム延伸装置を用いて製造された炭素繊維束は、スチーム延伸工程においてスチームを濾過せずに製造された炭素繊維束と比較すると、毛羽発生数が大幅に低減する。   The carbon fiber bundle produced by using the production method and the pressure steam drawing apparatus of the present invention significantly reduces the number of fluff generation compared to the carbon fiber bundle produced without filtering the steam in the steam drawing step. .

<加圧スチーム延伸装置>
本願発明の加圧スチーム延伸装置の一態様を図1に示す。図1の加圧スチーム延伸装置10において、蒸気室4には、蒸気導入口11が設けられ、蒸気導入口11の前には濾過装置7が連結している。蒸気減圧弁9から供給されたスチームは、濾過装置7で濾過された後、蒸気導入口11から蒸気室4に供給される。
加圧スチーム延伸装置10において、アクリル繊維束1の送入口部2及び送出口部と蒸気室4との間には、それぞれシール室3、5が設けられている。シール室3、5を有することにより、蒸気室内の加圧スチームを徐々に排出することができ、加圧スチーム延伸装置10の蒸気室4内の圧力は大気圧超で維持されている。蒸気室4内の圧力は、100〜500KPaであることが好ましい。
<Pressurized steam stretching device>
One embodiment of the pressurized steam stretching apparatus of the present invention is shown in FIG. In the pressurized steam stretching apparatus 10 of FIG. 1, a steam inlet 11 is provided in the steam chamber 4, and a filtration device 7 is connected in front of the steam inlet 11. The steam supplied from the steam pressure reducing valve 9 is filtered by the filtration device 7 and then supplied from the steam inlet 11 to the steam chamber 4.
In the pressurized steam stretching apparatus 10, seal chambers 3 and 5 are provided between the inlet / outlet portion 2 and the outlet / outlet portion of the acrylic fiber bundle 1 and the steam chamber 4, respectively. By having the seal chambers 3 and 5, the pressurized steam in the steam chamber can be gradually discharged, and the pressure in the steam chamber 4 of the pressurized steam stretching apparatus 10 is maintained above atmospheric pressure. The pressure in the steam chamber 4 is preferably 100 to 500 KPa.

また、本願発明の加圧スチーム延伸装置の別の態様を図2に示す。図2の加圧スチーム延伸装置20においては、加圧スチーム延伸装置10と異なり濾過装置が蒸気室内部に設けられている。図3、4はそれぞれ、濾過装置が蒸気導入口より後に設けられている加圧スチーム延伸装置20の一態様を表す。図3は、加圧スチームが蒸気導入口に接続した蒸気分配管により蒸気室の下面に分配されて噴出する態様を表すが、その蒸気分配管よりも蒸気室内側に濾過装置が設けられている。図4も同じく、蒸気分配管により蒸気室の下面に分配されて噴出する態様を表すが、その蒸気分配管に濾過装置が設けられている。また、図3から蒸気分配管を除いた態様も可能である。   Another embodiment of the pressurized steam stretching apparatus of the present invention is shown in FIG. In the pressurized steam stretching apparatus 20 of FIG. 2, unlike the pressurized steam stretching apparatus 10, a filtration device is provided in the steam chamber. 3 and 4 each show one mode of the pressurized steam stretching device 20 in which the filtration device is provided after the steam inlet. FIG. 3 shows a mode in which pressurized steam is distributed to the lower surface of the steam chamber by a steam distribution pipe connected to the steam inlet, and a filtration device is provided on the steam chamber side of the steam distribution pipe. . FIG. 4 also shows a mode in which the steam is distributed to the lower surface of the steam chamber by the steam distribution pipe and ejected, and a filtration device is provided in the steam distribution pipe. Moreover, the aspect remove | excluding the steam distribution piping from FIG. 3 is also possible.

以上の説明から理解できるように、本発明は特許請求の範囲を逸脱しない範囲において、多様な変更が可能である。   As can be understood from the above description, the present invention can be variously modified without departing from the scope of the claims.

以下、実施例を用いて本発明をより具体的に説明する。
<スチームに含まれる異物個数>
スチームを凝縮器に導入して、凝縮させた凝縮水を液中微粒子計測用のサンプルとした。液中微粒子計測器(HIAC/ROYCO社製:型番M−8000A)を用いて、前記凝縮水サンプル10mLに含まれる、特定の異物の大きさの範囲内(1μm以上2μm未満、2μm以上4μm未満、4μm以上7μm未満、7μm以上13μm未満、13μm以上25μm未満、25μm以上50μm未満、50μm以上100μm未満)にあるそれぞれの異物個数を測定した。
Hereinafter, the present invention will be described more specifically with reference to examples.
<Number of foreign substances contained in steam>
Steam was introduced into the condenser, and condensed condensed water was used as a sample for measuring fine particles in liquid. Using an in-liquid particle measuring instrument (manufactured by HIAC / ROYCO: Model number M-8000A), within a range of the size of a specific foreign substance contained in the 10 mL of the condensed water sample (1 μm or more and less than 2 μm, 2 μm or more and less than 4 μm, 4 μm or more and less than 7 μm, 7 μm or more and less than 13 μm, 13 μm or more and less than 25 μm, 25 μm or more and less than 50 μm, or 50 μm or more and less than 100 μm).

<炭素繊維束の毛羽発生数>
炭素化処理直後の走行状態にある炭素繊維束5本を肉眼で10分間観察し、炭素繊維束表面の毛羽の数を計測した。
<Number of fluff generated from carbon fiber bundles>
Five carbon fiber bundles in the running state immediately after the carbonization treatment were observed with the naked eye for 10 minutes, and the number of fluff on the carbon fiber bundle surface was measured.

<単繊維繊度>
乾燥したアクリル繊維束の1mの質量の測定値を、アクリル繊維束中のフィラメント数で割った値から単繊維繊度を算出した。ここでアクリル繊維束中のフィラメント数はアクリル繊維束の紡糸に用いた口金の孔数に等しいものとして扱った。
<Single fiber fineness>
The single fiber fineness was calculated from the value obtained by dividing the measured value of 1 m of the dried acrylic fiber bundle by the number of filaments in the acrylic fiber bundle. Here, the number of filaments in the acrylic fiber bundle was treated as being equal to the number of holes in the die used for spinning the acrylic fiber bundle.

[実施例1]
アクリロニトリル単位98モル%、メタクリル酸単位2モル%からなるアクリル系共重合体を、ジメチルホルムアミドに溶解して重合体濃度23質量%の紡糸原液を調整した。この紡糸原液を、紡糸ノズルを用いて、温度10℃、ジメチルホルムアミドの濃度80質量%からなる凝固浴中に吐出しアクリル系凝固糸束を得た。このアクリル系凝固糸束に、冷延伸および熱水中延伸を実施し、シリコ―ン系油剤を付与し、乾燥緻密化処理を行った。乾燥緻密化処理後の繊維束を、図1に示す加圧スチーム延伸装置10に通し、400KPaに加圧した蒸気室4(工程長100cm)内を、公称ろ過精度0.5μmの濾過材(エイコーフィルター株式会社製、スティームフィルターSPFT)を装着した濾過装置7で濾過したスチームを吹き付けつつ4.0倍の長さとなるよう延伸を行った。
蒸気室4を走行するアクリル繊維束1に対するスチームの吹き付けは、同繊維束の走行方向に対して略直交方向に行った。
その結果、単繊維繊度1.2dtex、フィラメント数12000本のアクリル繊維束を得た。
得られたアクリル繊維束を、200〜300℃の酸性化雰囲気中で耐炎化処理した後、400〜900℃の不活性雰囲気中で前炭素化処理した。次いで、1200〜2500℃の不活性雰囲気中で炭素化処理を行い、炭素繊維束を得た。
蒸気室に供給されるスチームに含まれる異物個数を表1に記載した。得られた炭素繊維束の毛羽発生数は90個/10minであった。
なお、表1において「A〜B」は「A以上B以下」を表す。
[Example 1]
An acrylic copolymer composed of 98 mol% acrylonitrile units and 2 mol% methacrylic acid units was dissolved in dimethylformamide to prepare a spinning dope having a polymer concentration of 23% by mass. This spinning dope was discharged using a spinning nozzle into a coagulation bath having a temperature of 10 ° C. and a dimethylformamide concentration of 80% by mass to obtain an acrylic coagulated yarn bundle. The acrylic coagulated yarn bundle was subjected to cold drawing and hot water drawing to give a silicone oil agent, followed by dry densification treatment. The fiber bundle after the drying densification treatment is passed through the pressurized steam drawing apparatus 10 shown in FIG. 1 and the inside of the vapor chamber 4 (process length 100 cm) pressurized to 400 KPa is filtered with a nominal filtration accuracy of 0.5 μm (Eiko). Stretching was performed so that the length was 4.0 times while spraying steam filtered by a filtration device 7 equipped with a filter manufactured by Filter Co., Ltd. (Steam filter SPFT).
Steam was sprayed onto the acrylic fiber bundle 1 traveling in the steam chamber 4 in a direction substantially orthogonal to the traveling direction of the fiber bundle.
As a result, an acrylic fiber bundle having a single fiber fineness of 1.2 dtex and a filament number of 12,000 was obtained.
The obtained acrylic fiber bundle was flameproofed in an acidified atmosphere at 200 to 300 ° C., and then pre-carbonized in an inert atmosphere at 400 to 900 ° C. Subsequently, the carbonization process was performed in 1200-2500 degreeC inert atmosphere, and the carbon fiber bundle was obtained.
Table 1 shows the number of foreign substances contained in the steam supplied to the steam chamber. The number of fluff generations in the obtained carbon fiber bundle was 90/10 min.
In Table 1, “A to B” represents “A or more and B or less”.

Figure 2016114385
Figure 2016114385

[実施例2〜4]
表1に示すようにアクリル繊維束の単繊維繊度、フィラメント数、紡糸速度を変更した以外は、実施例1と同様にして炭素繊維束を得た。蒸気室に供給されるスチームに含まれる異物個数と、得られた炭素繊維束の毛羽発生数を表1に示した。
[Examples 2 to 4]
As shown in Table 1, a carbon fiber bundle was obtained in the same manner as in Example 1 except that the single fiber fineness, the number of filaments, and the spinning speed of the acrylic fiber bundle were changed. Table 1 shows the number of foreign substances contained in the steam supplied to the steam chamber and the number of fluffs generated in the obtained carbon fiber bundle.

[比較例1]
加圧スチーム延伸装置の濾過装置を使用しない(より具体的には、濾過装置に濾過材を装着せずに加圧スチームを通過させる)以外は、実施例1と同様にして炭素繊維束を得た。蒸気室に供給されるスチームに含まれる異物個数と、得られた炭素繊維束の毛羽発生数を表1に示した。実施例1と比較して、得られた炭素繊維束の毛羽発生数は3倍以上であった。
[Comparative Example 1]
A carbon fiber bundle is obtained in the same manner as in Example 1 except that the filtration device of the pressurized steam stretching device is not used (more specifically, the pressurized steam is passed without attaching the filtering material to the filtration device). It was. Table 1 shows the number of foreign substances contained in the steam supplied to the steam chamber and the number of fluffs generated in the obtained carbon fiber bundle. Compared with Example 1, the number of fluff generation of the obtained carbon fiber bundle was 3 times or more.

[比較例2〜4]
表1に示すように、加圧スチーム延伸装置の濾過装置を使用しない(より具体的には、濾過装置に濾過材を装着せずに加圧スチームを通過させる)以外は、それぞれ実施例2〜4と同様にして炭素繊維束を得た。蒸気室に供給されるスチームに含まれる異物個数と、得られた炭素繊維束の毛羽発生数を表1に示した。単繊維繊度、フィラメント数、紡糸速度が対応する実施例2〜4のそれぞれと比較して、得られた炭素繊維束の毛羽発生数はいずれも3倍以上であった。
[Comparative Examples 2 to 4]
As shown in Table 1, each of Examples 2 to 2 except that the filtration device of the pressurized steam stretching device is not used (more specifically, the pressurized steam is allowed to pass through without attaching the filtering material to the filtration device). In the same manner as in No. 4, a carbon fiber bundle was obtained. Table 1 shows the number of foreign substances contained in the steam supplied to the steam chamber and the number of fluffs generated in the obtained carbon fiber bundle. The number of fluff generations of the obtained carbon fiber bundle was 3 times or more as compared with each of Examples 2 to 4 corresponding to the single fiber fineness, the number of filaments, and the spinning speed.

表1の結果から明らかなように、蒸気室に供給されるスチームに含まれる異物個数を、本発明のように濾過装置を用いて低減することにより、炭素繊維束の毛羽の発生の原因となる欠陥が少ない、高品質のアクリル繊維束を安定的に得ることが出来る。   As is apparent from the results in Table 1, the number of foreign matters contained in the steam supplied to the steam chamber is reduced by using a filtration device as in the present invention, which causes generation of fluff of the carbon fiber bundle. A high-quality acrylic fiber bundle with few defects can be stably obtained.

本発明により、毛羽の発生が大幅に改善された高品質の炭素繊維を得ることができる。したがって、本発明は「アクリル繊維束の製造方法及び加圧スチーム延伸装置」に好適に利用でき、産業上極めて重要である。   According to the present invention, it is possible to obtain a high-quality carbon fiber in which the generation of fluff is greatly improved. Therefore, the present invention can be suitably used for “a method for producing an acrylic fiber bundle and a pressurized steam drawing apparatus” and is extremely important in industry.

1 アクリル繊維束
2 アクリル繊維束の送入口
3 シール室
4 蒸気室
5 シール室
6 アクリル繊維束の送出口
7 濾過装置
8 ドレンセパレーター
9 蒸気減圧弁
10 加圧スチーム延伸装置
11 蒸気導入口
12 蒸気分配管
20 加圧スチーム延伸装置
DESCRIPTION OF SYMBOLS 1 Acrylic fiber bundle 2 Acrylic fiber bundle inlet 3 Seal chamber 4 Vapor chamber 5 Seal chamber 6 Acrylic fiber bundle outlet 7 Filtration device 8 Drain separator 9 Steam pressure reducing valve 10 Pressurized steam stretcher 11 Steam inlet 12 Steam content Piping 20 Pressurized steam stretcher

[1] 加圧スチームを濾過し、濾過後の前記加圧スチームを加圧スチーム延伸装置の蒸気室に供給しながら、前記蒸気室内にアクリル繊維束を走行させて延伸処理をする、アクリル繊維束の製造方法であって、
前記濾過後の加圧スチームは、大きさ50μm以上の異物の個数が0個/10mLであり、大きさ7μm以上の異物の個数が102個/10mL以上であるアクリル繊維束の製造方法
[2] 加圧スチームの濾過を、大きさ7μm以上の異物の異物捕捉率が90%以上であり、大きさ4〜7μmの異物の異物捕捉率が91.6%以下である濾過材を備えた濾過装置を用いて行う、[1]に記載のアクリル繊維束の製造方法。
] 前記濾過後の加圧スチームは、大きさ1μm以上の異物の個数が、3000個/10mL以下である、[1]または[2]に記載のアクリル繊維束の製造方法。
] 前記濾過後の加圧スチームは、大きさ4μm以上の異物の個数が、500個/10mL以下である、[1]〜[]のいずれか一つに記載のアクリル繊維束の製造方法。
] 前記蒸気室は、ラビリンスシールを通じて蒸気室内部の加圧スチームを排出するものである、[1]〜[]のいずれか一つに記載のアクリル繊維束の製造方法。
] 前記濾過後の加圧スチームを、前記加圧スチーム延伸装置内を走行するアクリル繊維束に直接吹きつける、[1]〜[]のいずれか一つに記載のアクリル繊維束の製造方法。
] 繊維の送入口、蒸気室、及び、延伸処理された繊維の送出口を有し、加圧スチームを前記蒸気室に供給しながら、前記蒸気室内に繊維を走行させて延伸処理をする加圧スチーム延伸装置であって、濾過装置を有し、前記濾過装置を用いて濾過した加圧スチームを前記蒸気室内に供給する加圧スチーム延伸装置であって、
前記濾過後の加圧スチームは、大きさ50μm以上の異物の個数が0個/10mLであり、大きさ7μm以上の異物の個数が102個/10mL以上である加圧スチーム延伸装置。
] 濾過装置として、大きさ7μm以上の異物の異物捕捉率が90%以上であり、大きさ4〜7μmの異物の異物捕捉率が91.6%以下である濾過材を備えた濾過装置を有する、[]に記載の加圧スチーム延伸装置。
] 濾過装置として、前記濾過後の加圧スチームが、大きさ1μm以上の異物の個数が、3000個/10mL以下となる濾過装置を有する、[7]又は[8]に記載の加圧スチーム延伸装置。
10] 濾過装置として、前記濾過後の加圧スチームが、大きさ4μm以上の異物の個数が、500個/10mL以下となる濾過装置を有する、[]〜[]のいずれか一つに記載の加圧スチーム延伸装置。
11] 前記送入口と前記蒸気室の間と、前記送出口と前記蒸気室の間のそれぞれに前記蒸気室内部の加圧スチームを排出するラビリンスシールを有する、[]〜[10]のいずれか一つに記載の加圧スチーム延伸装置。
12] 前記濾過後の加圧スチームを、前記蒸気室内を走行するアクリル繊維束に直接吹きつける、[]〜[11]のいずれか一つに記載の加圧スチーム延伸装置。
[1] Acrylic fiber bundle that is subjected to stretching treatment by running the acrylic fiber bundle in the steam chamber while filtering the pressurized steam and supplying the filtered pressurized steam to the steam chamber of the pressurized steam stretching apparatus. A manufacturing method of
The pressure steam after the filtration is a method for producing an acrylic fiber bundle in which the number of foreign matters having a size of 50 μm or more is 0/10 mL and the number of foreign matters having a size of 7 μm or more is 102/10 mL or more .
[2] The filtration of pressurized steam state, and are foreign matter collection efficiency of size 7μm or more foreign matter 90%, foreign body capturing rate of foreign matter sizes 4~7μm is Ru der less 91.6% filtering material The manufacturing method of the acrylic fiber bundle as described in [1] performed using the filtration apparatus provided with.
[ 3 ] The method for producing an acrylic fiber bundle according to [1] or [2] , wherein the pressure steam after the filtration has a number of foreign matters having a size of 1 μm or more of 3000 pieces / 10 mL or less.
[ 4 ] The acrylic steam bundle according to any one of [1] to [ 3 ], wherein the pressure steam after the filtration has a number of foreign matters having a size of 4 μm or more of 500 pieces / 10 mL or less. Method.
[ 5 ] The method for producing an acrylic fiber bundle according to any one of [1] to [ 4 ], wherein the steam chamber discharges pressurized steam in the steam chamber through a labyrinth seal.
[ 6 ] The production of the acrylic fiber bundle according to any one of [1] to [ 5 ], wherein the pressurized steam after the filtration is directly sprayed onto the acrylic fiber bundle traveling in the pressurized steam stretching apparatus. Method.
[ 7 ] It has a fiber inlet / outlet, a steam chamber, and a fiber outlet / outlet that has been subjected to stretching treatment, and while the pressurized steam is supplied to the steam chamber, the fiber travels in the steam chamber to perform the stretching treatment. A pressurized steam stretching device, comprising a filtration device, and supplying the pressurized steam filtered using the filtration device into the steam chamber ,
The pressurized steam stretching apparatus after filtration, wherein the number of foreign matters having a size of 50 μm or more is 0/10 mL, and the number of foreign matters having a size of 7 μm or more is 102/10 mL or more .
[8] as a filtration device state, and are foreign matter collection efficiency of size 7μm or more foreign matter 90%, foreign body capturing rate of foreign body size 4~7μm is equipped with Der Ru filtering material below 91.6% The pressurized steam stretching apparatus according to [ 7 ], including a filtration device.
[ 9 ] The pressurization according to [7] or [8] , wherein the post-filtration pressurizing steam has a filtration device in which the number of foreign matters having a size of 1 μm or more is 3000 pieces / 10 mL or less. Steam stretching device.
[ 10 ] Any one of [ 7 ] to [ 9 ], wherein the pressure steam after filtration has a filtration device in which the number of foreign matters having a size of 4 μm or more is 500 pieces / 10 mL or less. The pressurized steam stretching apparatus according to 1.
[ 11 ] The labyrinth seal for discharging pressurized steam in the steam chamber is provided between the inlet and the steam chamber and between the outlet and the steam chamber, respectively, according to [ 7 ] to [ 10 ] The pressurized steam stretching apparatus according to any one of the above.
[ 12 ] The pressurized steam stretching apparatus according to any one of [ 7 ] to [ 11 ], wherein the filtered pressurized steam is directly blown onto an acrylic fiber bundle traveling in the steam chamber.

Claims (14)

加圧スチームを濾過し、濾過後の前記加圧スチームを加圧スチーム延伸装置の蒸気室に供給しながら、前記蒸気室内にアクリル繊維束を走行させて延伸処理をする、アクリル繊維束の製造方法。   A method for producing an acrylic fiber bundle, in which a pressurized steam is filtered, and the filtered steam is supplied to a steam chamber of a pressurized steam stretching apparatus, and the acrylic fiber bundle is caused to travel in the steam chamber for stretching. . 加圧スチームの濾過を、大きさ7μm以上の異物の異物捕捉率が90%以上である濾過材を備えた濾過装置を用いて行う、請求項1に記載のアクリル繊維束の製造方法。   The method for producing an acrylic fiber bundle according to claim 1, wherein the filtration of the pressurized steam is performed using a filtration apparatus including a filtration material having a foreign matter capture rate of a foreign matter having a size of 7 µm or more of 90% or more. 前記濾過後の加圧スチームは、大きさ50μm以上の異物の個数が0個/10mLである、請求項1または2に記載のアクリル繊維束の製造方法。   3. The method for producing an acrylic fiber bundle according to claim 1, wherein the pressure steam after the filtration is 0/10 mL of foreign matters having a size of 50 μm or more. 前記濾過後の加圧スチームは、大きさ1μm以上の異物の個数が、3000個/10mL以下である、請求項1〜3のいずれか一項に記載のアクリル繊維束の製造方法。   The method for producing an acrylic fiber bundle according to any one of claims 1 to 3, wherein the pressurized steam after the filtration has a number of foreign matters having a size of 1 µm or more of 3000 pieces or 10 mL or less. 前記濾過後の加圧スチームは、大きさ4μm以上の異物の個数が、500個/10mL以下である、請求項1〜4のいずれか一項に記載のアクリル繊維束の製造方法。   The method for producing an acrylic fiber bundle according to any one of claims 1 to 4, wherein the pressure steam after filtration has a number of foreign matters having a size of 4 µm or more of 500 pieces / 10 mL or less. 前記蒸気室は、ラビリンスシールを通じて蒸気室内部の加圧スチームを排出するものである、請求項1〜5のいずれか一項に記載のアクリル繊維束の製造方法。   The said steam chamber is a manufacturing method of the acrylic fiber bundle as described in any one of Claims 1-5 which discharges | emits the pressurization steam of a steam chamber inside through a labyrinth seal. 前記濾過後の加圧スチームを、前記加圧スチーム延伸装置内を走行するアクリル繊維束に直接吹きつける、請求項1〜6のいずれか一項に記載のアクリル繊維束の製造方法。   The manufacturing method of the acrylic fiber bundle as described in any one of Claims 1-6 which sprays the pressurized steam after the filtration directly on the acrylic fiber bundle which drive | works the inside of the said pressurized steam extending | stretching apparatus. 繊維の送入口、蒸気室、及び、延伸処理された繊維の送出口を有し、加圧スチームを前記蒸気室に供給しながら、前記蒸気室内に繊維を走行させて延伸処理をする加圧スチーム延伸装置であって、
濾過装置を有し、前記濾過装置を用いて濾過した加圧スチームを前記蒸気室内に供給する加圧スチーム延伸装置。
Pressurized steam that has a fiber inlet / outlet, a steam chamber, and a fiber outlet / outlet that has been subjected to drawing treatment, and that supplies the pressurized steam to the steam chamber and causes the fibers to travel in the steam chamber for drawing treatment. A stretching device,
A pressurized steam stretching apparatus that has a filtration device and supplies pressurized steam that has been filtered using the filtration device into the steam chamber.
濾過装置として、大きさ7μm以上の異物の異物捕捉率が90%以上である濾過材を備えた濾過装置を有する、請求項8に記載の加圧スチーム延伸装置。   The pressurized steam stretching apparatus according to claim 8, comprising a filtering apparatus having a filtering material having a foreign matter capture rate of 90% or more of foreign matters having a size of 7 μm or more as the filtering device. 濾過装置として、前記濾過後の加圧スチームが、大きさ50μm以上の異物の個数が0個/10mLとなる濾過装置を有する、請求項8または9に記載の加圧スチーム延伸装置。   The pressure steam stretching apparatus according to claim 8 or 9, wherein the pressure steam after the filtration has a filtration apparatus in which the number of foreign matters having a size of 50 µm or more is 0 / 10mL. 濾過装置として、前記濾過後の加圧スチームが、大きさ1μm以上の異物の個数が、3000個/10mL以下となる濾過装置を有する、請求項8〜10のいずれか一項に記載の加圧スチーム延伸装置。   The pressurization according to any one of claims 8 to 10, wherein the pressure steam after the filtration has a filtration device in which the number of foreign matters having a size of 1 µm or more is 3000 pieces / 10 mL or less. Steam stretching device. 濾過装置として、前記濾過後の加圧スチームが、大きさ4μm以上の異物の個数が、500個/10mL以下となる濾過装置を有する、請求項8〜11のいずれか一項に記載の加圧スチーム延伸装置。   The pressurization according to any one of claims 8 to 11, wherein the pressure steam after the filtration has a filtration device in which the number of foreign matters having a size of 4 µm or more is 500 pieces / 10 mL or less. Steam stretching device. 前記送入口と前記蒸気室の間と、前記送出口と前記蒸気室の間のそれぞれに前記蒸気室内部の加圧スチームを排出するラビリンスシールを有する、請求項8〜12のいずれか一項に記載の加圧スチーム延伸装置。   It has a labyrinth seal which discharges the pressurization steam of the inside of the above-mentioned steam room between each of the above-mentioned entrance and the above-mentioned steam room, and between the above-mentioned outlet and the above-mentioned steam room, respectively. The pressurized steam stretching apparatus described. 前記濾過後の加圧スチームを、前記蒸気室内を走行するアクリル繊維束に直接吹きつける、請求項8〜13のいずれか一項に記載の加圧スチーム延伸装置。   The pressurized steam stretching apparatus according to any one of claims 8 to 13, wherein the pressurized steam after the filtration is directly blown onto an acrylic fiber bundle traveling in the steam chamber.
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