JP2001288622A - Method for producing carbon fiber precursor fiber bundle and method for producing carbon fiber bundle - Google Patents
Method for producing carbon fiber precursor fiber bundle and method for producing carbon fiber bundleInfo
- Publication number
- JP2001288622A JP2001288622A JP2000094766A JP2000094766A JP2001288622A JP 2001288622 A JP2001288622 A JP 2001288622A JP 2000094766 A JP2000094766 A JP 2000094766A JP 2000094766 A JP2000094766 A JP 2000094766A JP 2001288622 A JP2001288622 A JP 2001288622A
- Authority
- JP
- Japan
- Prior art keywords
- fiber bundle
- carbon fiber
- fluid
- entanglement
- fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 227
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 101
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 101
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000002243 precursor Substances 0.000 title claims abstract description 53
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 44
- 239000012530 fluid Substances 0.000 claims abstract description 106
- 238000000034 method Methods 0.000 claims description 39
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims 1
- 238000002347 injection Methods 0.000 abstract description 19
- 239000007924 injection Substances 0.000 abstract description 19
- 238000011282 treatment Methods 0.000 description 21
- 238000007380 fibre production Methods 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 9
- 238000004804 winding Methods 0.000 description 7
- 238000003763 carbonization Methods 0.000 description 6
- 230000000704 physical effect Effects 0.000 description 6
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 229920000297 Rayon Polymers 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003780 insertion Methods 0.000 description 3
- 230000037431 insertion Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000010409 ironing Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000009191 jumping Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Landscapes
- Artificial Filaments (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
- Inorganic Fibers (AREA)
Abstract
(57)【要約】
【課題】炭素繊維前駆体繊維束に長手方向及び径方向に
均一で適度な交絡を付与できる炭素繊維前駆体繊維束の
製造方法と、操業安定性が良好で後の開繊が容易な炭素
繊維束の製造方法とを提供する。
【解決手段】流体噴射室(3) とその前後に前記流体噴射
室(3) の複数段の渦流が発生するシール室(4,5) と、後
方のシール室(5) の出口にエゼクター(6) とを備えた交
絡付与装置(1) を用いて炭素繊維前駆体繊維束に交絡を
付与する。流体噴射室(3) の内径D(mm) は繊維束の総繊
度T/800 <D<T/80、同噴射室(3) の長さL(mm) は0.3
<L/D <30、1の繊維束当たりの流体の流量Q(m3/分)
を、0.5t<Q<4.3t、走行する前記繊維束の張力G(g/テ
ックス)を、0.2 <G<1.5 の範囲に設定する。得られ
た交絡の付与された炭素繊維前駆体繊維束を耐炎化及び
炭素化して炭素繊維束を製造する。
(57) [Problem] To provide a method for producing a carbon fiber precursor fiber bundle capable of imparting uniform and appropriate entanglement to the carbon fiber precursor fiber bundle in the longitudinal direction and the radial direction, and a method for producing a carbon fiber precursor fiber bundle having good operation stability and subsequent opening. Provided is a method for producing a carbon fiber bundle that is easy to produce. A fluid injection chamber (3), a seal chamber (4, 5) in which a plurality of stages of vortex flow of the fluid injection chamber (3) are generated before and after the fluid injection chamber, and an ejector ( 6) The entanglement is imparted to the carbon fiber precursor fiber bundle using the entanglement imparting device (1) provided with The inner diameter D (mm) of the fluid injection chamber (3) is the total fineness of the fiber bundle T / 800 <D <T / 80, and the length L (mm) of the injection chamber (3) is 0.3
<L / D <30, flow rate Q of fluid per fiber bundle (m 3 / min)
Is set in the range of 0.5t <Q <4.3t, and the tension G (g / tex) of the running fiber bundle is in the range of 0.2 <G <1.5. The obtained entangled carbon fiber precursor fiber bundle is flame-resistant and carbonized to produce a carbon fiber bundle.
Description
本発明は、炭素繊維前駆体繊維束の製造方法及び炭素繊
維束の製造方法に関し、特に、前記繊維束を長手方向及
び径方向に均一に交絡して適度な集束性を付与して、後
の炭素繊維束製造工程での工程通過安定性を向上できる
炭素繊維前駆体繊維束の製造方法と、高品質で毛羽並び
に単糸切れが少なく、開繊性及び機械的特性に優れた炭
素繊維束の製造方法とに関する。The present invention relates to a method for producing a carbon fiber precursor fiber bundle and a method for producing a carbon fiber bundle, and in particular, imparts an appropriate convergence by uniformly entangled the fiber bundle in the longitudinal direction and the radial direction, and A method for producing a carbon fiber precursor fiber bundle that can improve the process passage stability in the carbon fiber bundle production process, and a method for producing a carbon fiber bundle having high quality, less fluff and single yarn breakage, and excellent fiber opening properties and mechanical properties. A manufacturing method.
【0001】[0001]
【従来の技術】炭素繊維は他の繊維と比較して優れた比
強度や比弾性率を有し、金属と比較しても優れた比抵抗
や高い耐薬品性をもつなどの多くの優れた特性を有し、
その優れた各種特性を利用して樹脂との複合材料用の補
強繊維や、その他工業用途に、またスポーツ、航空宇宙
分野などにも幅広く利用されている。2. Description of the Related Art Carbon fibers have excellent specific strength and specific elastic modulus as compared with other fibers, and have many excellent properties such as excellent specific resistance and high chemical resistance as compared with metals. Has characteristics,
Utilizing its excellent various properties, it is widely used in reinforcing fibers for composite materials with resins, other industrial uses, and also in the sports and aerospace fields.
【0002】一般に、炭素繊維はアクリロニトリル系繊
維などの原料繊維を200℃以上の酸化性雰囲気中で耐
炎化し、次いで300℃以上の不活性雰囲気中で炭化す
ることによって得られる。Generally, carbon fibers are obtained by oxidizing raw material fibers such as acrylonitrile-based fibers in an oxidizing atmosphere at 200 ° C. or higher and then carbonizing them in an inert atmosphere at 300 ° C. or higher.
【0003】前記耐炎化工程では処理効率を向上させる
ため、また、装置の省スペース化を図るために、複数の
炭素繊維前駆体繊維束を所定の間隔を空けて平行にシー
ト状に並べて耐炎化炉内を走行させると共に、走行する
前記繊維束を複数のロールに掛け回して同繊維束の走行
方向を変更し、前記耐炎化炉内を複数段で通過させてい
る。In the above-mentioned flame-proofing step, in order to improve the processing efficiency and to save the space of the apparatus, a plurality of carbon fiber precursor fiber bundles are arranged in parallel at predetermined intervals in a sheet form, and the flame-proofing is performed. While traveling in the furnace, the traveling fiber bundle is wrapped around a plurality of rolls to change the traveling direction of the fiber bundle, and is passed through the flameproofing furnace in a plurality of stages.
【0004】この走行する炭素繊維前駆体繊維束は前記
ロールへの巻き付きや隣を走行する繊維束との干渉など
により、炭素繊維の物性や品質に低下を来すため、かか
るロールへの巻き付きや繊維束同士の干渉を防止すべ
く、各繊維束にそれぞれ集束性を付与することが必要で
ある。そこで、特に炭素繊維の製造においても、各繊維
束の集束性を改善するための様々な検討がこれまでなさ
れてきた。The running carbon fiber precursor fiber bundle deteriorates the physical properties and quality of the carbon fiber due to winding around the roll or interference with the fiber bundle running next to the running roll. In order to prevent interference between the fiber bundles, it is necessary to impart convergence to each fiber bundle. Therefore, various studies have been made to improve the convergence of each fiber bundle, especially in the production of carbon fibers.
【0005】繊維束に集束性を付与する方法としては、
例えば油剤を付与する油剤処理や、繊維束を構成する単
繊維同士を同繊維束内で絡み合わせる交絡処理を施すこ
とが一般的であり、これら処理のいづれか、もしくはこ
れら処理の組み合わせによって繊維束に集束性を付与し
ている。[0005] As a method of imparting a bundle property to a fiber bundle,
For example, it is common to apply an oil agent treatment for applying an oil agent, or to perform a entanglement treatment in which single fibers constituting a fiber bundle are entangled in the same fiber bundle, and any of these treatments or a combination of these treatments is applied to the fiber bundle. Provides convergence.
【0006】特開昭58−214516号公報に開示さ
れている炭素繊維前駆体糸条パッケージの製造方法にあ
っては、炭素繊維製造工程において、集束性の不足によ
るローラへの巻き付きを防止すると共に、過度な集束に
よる擬似融着や耐炎化のムラを改善すべくなされたもの
である。同方法では、アクリル系重合体の溶液を紡糸、
延伸、乾燥緻密化後に、前記糸条に0.1〜0.3g/
d(0.11〜0.33g/テックス)の張力を付与し
ながら空気処理することにより単糸を開繊させ、且つ交
絡程度を示すCF値が20〜60となるまで絡合させた
後に巻き上げている。前記空気処理には、3〜10個の
吹出し孔を有するリング状エアノズルを用いている。In the method of manufacturing a carbon fiber precursor yarn package disclosed in Japanese Patent Application Laid-Open No. 58-215516, it is possible to prevent winding around a roller due to insufficient convergence in a carbon fiber manufacturing process. The purpose of the present invention is to improve unevenness of pseudo fusion and flame resistance due to excessive focusing. In the same method, spinning a solution of an acrylic polymer,
After stretching and drying and densifying, 0.1-0.3 g /
Air treatment is performed while applying a tension of d (0.11 to 0.33 g / tex) to open the single yarn, and the yarn is entangled until the CF value indicating the degree of entanglement becomes 20 to 60, and then wound up. ing. For the air treatment, a ring-shaped air nozzle having 3 to 10 blowing holes is used.
【0007】また、例えば特開昭58−214530号
公報に開示されている耐炎化繊維の製造方法にあって
は、従来の耐炎化処理に先だって繊維束にシリコン系化
合物を含浸させた場合における前記シリコン系化合物に
起因する静電気による障害や、集束性の欠如による耐炎
化処理時の毛羽や単糸切れの発生を防止することを目的
としている。そして同公報の製造方法では、繊維束を耐
炎化炉へと導入する前に、繊維束にシリコン系化合物を
含浸させることなく前記繊維束に流体噴射法による交絡
処理を施してから更に10回/m以下の低仮撚処理を施
している。[0007] Further, for example, in the method for producing oxidized fiber disclosed in Japanese Patent Application Laid-Open No. 58-214530, the above-described method is used in a case where a fiber bundle is impregnated with a silicon compound prior to the conventional oxidization treatment. An object of the present invention is to prevent a failure due to static electricity caused by a silicon-based compound and a generation of fluff or breakage of single yarn during a flame-proof treatment due to lack of convergence. In the manufacturing method of the publication, before the fiber bundle is introduced into the flameproofing furnace, the fiber bundle is subjected to the entanglement treatment by the fluid jetting method without impregnating the fiber bundle with the silicon-based compound, and then 10 times / m or less.
【0008】ところで、炭素繊維製造工程以前或いは製
造工程途中でその製造工程通過安定性を確保するために
交絡を付与し、その後、炭素繊維製造工程を通過して製
造された炭素繊維束は、その交絡が付与された状態で利
用される場合と、製織時どの開繊が必要な場合とがあ
る。By the way, before or during the carbon fiber production process, confounding is applied to ensure the stability of the production process, and then the carbon fiber bundle produced through the carbon fiber production process is There is a case where the fiber is used in a state of being entangled, and a case where fiber opening is required during weaving.
【0009】例えば交絡が付与された状態で利用される
場合には、炭素繊維製造工程以前或いはその工程途中で
付与された交絡が不均一であると、炭素繊維束としての
物性や品質も不均一なものとなり、好ましくない。一
方、交絡を開繊して使用する場合には、交絡を開繊ロー
ルなどによって開繊するが、交絡が不均一であると、開
繊の程度も不均一となる。更には、交絡が強い場合、或
いは局部的に過剰な交絡がある場合には開繊のために強
いしごき操作が必要になり、物性の低下や毛羽等の発生
による品質の低下を招くといった問題をも同時に含むも
のである。For example, in the case where the carbon fiber bundle is used in a state of being entangled, if the entanglement imparted before or during the carbon fiber manufacturing process is not uniform, the physical properties and quality of the carbon fiber bundle are also uneven. And is not preferred. On the other hand, in the case where the confounding is used after being opened, the confounding is performed by using a spreading roll or the like. Furthermore, when the confounding is strong, or when there is an excessive confounding locally, a strong ironing operation is required for opening the fiber, which causes a problem that the physical properties are deteriorated and the quality is deteriorated due to generation of fluff. At the same time.
【0010】ここで、特開昭58−214516号公報
では、空気処理には3〜10個の吹出し孔を有するリン
グ状エアノズルを用いている。一方、特開昭58−21
4530号公報では流体噴射法による交絡付与に用いら
れる交絡付与装置について具体的な記載はない。Here, in Japanese Patent Application Laid-Open No. 58-214516, a ring-shaped air nozzle having 3 to 10 blowout holes is used for air treatment. On the other hand, JP-A-58-21
Japanese Patent No. 4530 does not specifically describe a confounding device used for confounding by a fluid ejection method.
【0011】一般に繊維束への交絡付与は、所要の張力
下にある繊維束を、高圧で流体が噴射されている流体噴
射域へ導入し、乱流により交絡させるものである。一般
的な繊維束の交絡付与装置として、例えば実公昭50−
46005号公報にマルチフィラメント糸の集束装置が
開示されている。同装置は長手方向に同一径の円形断面
をもつ糸条の走行路を有しており、前記走行路には長手
方向の中央部分において互いに180°変位した2つの
流体噴射孔が形成され、同噴射孔から糸条に流体が噴射
されて糸条が集束される。また、前記走行路への糸条の
挿通を容易にするために、同走行路には全長にわたって
糸条挿通用スリットが形成されており、更に、同スリッ
トからの糸条の飛び出しを紡糸するために、前記糸条挿
通用スリットへの流体供給孔が形成され、同スリットへ
も流体が供給される。Generally, the entanglement of the fiber bundle is such that a fiber bundle under a required tension is introduced into a fluid ejection area where a fluid is ejected at a high pressure, and is entangled by turbulence. As a general fiber bundle entanglement giving device, for example,
Japanese Patent No. 46005 discloses a multifilament yarn bundling device. The apparatus has a running path of a yarn having a circular cross section of the same diameter in the longitudinal direction, and two fluid injection holes which are displaced by 180 ° from each other at a central portion in the longitudinal direction are formed in the running path. The fluid is ejected from the injection holes to the yarn, and the yarn is focused. Further, in order to facilitate the insertion of the yarn into the traveling path, the traveling path is formed with a slit for thread insertion over the entire length, and further for spinning out the yarn from the slit. In addition, a fluid supply hole is formed to the thread insertion slit, and the fluid is also supplied to the slit.
【0012】[0012]
【発明が解決しようとする課題】前記実公昭50−46
005号公報に開示された一般的な繊維束への交絡付与
装置では、均一な集束性が付与できるとしているもの
の、繊維束が糸条走行路からスリットへと飛び出すのを
防止することに重点を置いたものであり、炭素繊維束と
して必要な高度な均一性は得られなかった。しかも、一
般の繊維束では当然に後に交絡を解除する開繊性につい
ては全く考慮していないため、開繊性も悪い。Problems to be Solved by the Invention
In the general apparatus for imparting confounding to a fiber bundle disclosed in Japanese Patent Publication No. 005, it is stated that uniform convergence can be imparted, but emphasis is placed on preventing the fiber bundle from jumping out of the yarn running path to the slit. It did not provide the high degree of uniformity required for the carbon fiber bundle. Moreover, in general fiber bundles, since the fiber-opening property for releasing the entanglement later is not considered at all, the fiber-opening property is also poor.
【0013】また、炭素繊維の製造方法に関する前記特
開昭58−214516号公報では、炭素繊維の製造工
程において均一な耐炎化を図るためにある程度の開繊性
は確保されるものの、炭素繊維として高度に開繊が必要
な用途に用いることについては考慮しておらず、開繊性
は不充分である。更に、特開昭58−214530号公
報は、炭素繊維製造工程での耐炎化の均一性を特に上記
公報は繊維束の集束性を向上させて炭素繊維製造工程で
の工程通過性の向上を図ることにのみ重点を置いたもの
であり、炭素繊維の用途や炭素繊維を開繊させることに
ついては全く考慮されていない。そのため、集束性は高
くて工程安定性には優れているが、反面、開繊しにくい
ものであり、開繊が必要な場合には、しごきなど強制的
な力を加えなければならず、炭素繊維の製造工程中ない
しは後の高次加工において物性や品質の低下を来す惧れ
がある。In Japanese Patent Application Laid-Open No. 58-214516 concerning the method for producing carbon fibers, although a certain degree of opening property is ensured in order to achieve uniform flame resistance in the carbon fiber production process, the carbon fiber is used as a carbon fiber. No consideration is given to use in applications that require a high degree of fiber opening, and the fiber opening properties are insufficient. Furthermore, Japanese Patent Application Laid-Open No. 58-214530 discloses a method for improving the uniformity of flame resistance in the carbon fiber production process, and in particular, the aforementioned publication aims to improve the convergence of the fiber bundle to improve the processability in the carbon fiber production process. No particular consideration is given to the use of carbon fibers or the opening of carbon fibers. For this reason, although the convergence is high and the process stability is excellent, it is difficult to spread, and when opening is required, forced force such as ironing must be applied. There is a concern that physical properties and quality may be deteriorated during or after the fiber manufacturing process.
【0014】そこで本発明にあっては、炭素繊維前駆体
繊維束に適度な集束性を与えると共に前記繊維束の長手
方向及び径方向に均一な交絡を付与し、炭素繊維製造工
程での操業安定性を向上させることができ、且つ、後に
開繊が必要な場合には、過度な強制開繊操作を行うこと
なく均一に開繊しやすい交絡を付与することができる、
炭素繊維前駆体繊維束の製造方法と、高品質で毛羽並び
に単糸切れが少なく、開繊性及び機械的特性に優れた炭
素繊維束の製造方法とを提供することを目的としてい
る。Therefore, in the present invention, the carbon fiber precursor fiber bundle is provided with appropriate bunching properties and uniform entanglement is provided in the longitudinal and radial directions of the fiber bundle, thereby stabilizing the operation in the carbon fiber production process. Can be improved, and, if later opening is necessary, it is possible to impart a confounding that can be uniformly opened without performing an excessive forced opening operation,
It is an object of the present invention to provide a method for producing a carbon fiber precursor fiber bundle and a method for producing a carbon fiber bundle having high quality, less fluff and single yarn breakage, and excellent in fiber opening properties and mechanical properties.
【0015】[0015]
【課題を解決するための手段】かかる課題を解決するた
めに、本発明は、次の構成を有する。即ち、実質的に無
撚りの炭素繊維前駆体繊維束に流体を噴射して交絡を付
与する方法であって、前記繊維束を交絡付与装置の出口
に配されたエゼクターを用いて前記交絡付与装置の入口
から出口へと挿通させること、前記繊維束が前記交絡付
与装置の入口から出口へと走行する間に、前記繊維束に
前記流体噴射室において流体を噴射した後、同流体噴射
室に続くシール室を通過させること、及び少なくとも前
記流体噴射室において、前記繊維束は同繊維束の走行方
向と直交する断面が円形又は楕円形である走行路を走行
させることを特徴としている。In order to solve such a problem, the present invention has the following configuration. That is, a method of injecting a fluid into a substantially untwisted carbon fiber precursor fiber bundle to impart entanglement, wherein the fiber bundle is entangled using an ejector arranged at an outlet of the entanglement device. After the fiber bundle travels from the entrance to the exit of the entanglement imparting device, the fluid is ejected to the fiber bundle in the fluid ejection chamber, and then continues to the fluid ejection chamber. The method is characterized in that the fiber bundle is caused to pass through a running path having a circular or elliptical cross section perpendicular to the running direction of the fiber bundle, at least in the fluid ejection chamber.
【0016】本発明にあっては、先ず、前記エゼクター
を作動させることにより交絡付与装置内部が減圧され、
前記繊維束を交絡付与装置内に容易に通糸することが可
能となる。更に、本発明では繊維束に流体噴射室で交絡
を付与した後に続けて、同繊維束にはシール室を通過さ
せている。即ち、繊維束は流体が噴射され高圧な状態に
ある流体噴射室から大気圧の装置外部へと直接に導出さ
れるのではなく、前記流体噴射室と装置外部との間には
シール室が介在している。そのため、流体噴射室の内部
流体は繊維束が同流体噴射室から導出される際にその導
出口から多量に流出することがなく、流体噴射室内での
圧力が均一に維持されると共に、その噴射流体の噴射量
を制御することにより同流体噴射室の内圧が容易に且つ
高精度に制御される。そのため、繊維束には長手方向及
び径方向に均一な交絡が付与される。In the present invention, first, the inside of the confounding device is depressurized by operating the ejector,
The fiber bundle can be easily passed through the entanglement imparting device. Further, in the present invention, the fiber bundle is passed through the seal chamber after the fiber bundle is entangled in the fluid ejection chamber. That is, the fiber bundle is not directly discharged from the fluid ejection chamber in which the fluid is ejected and in a high pressure state to the outside of the apparatus at atmospheric pressure, but a seal chamber is interposed between the fluid ejection chamber and the outside of the apparatus. are doing. Therefore, when the fiber bundle is discharged from the fluid ejection chamber, a large amount of the internal fluid of the fluid ejection chamber does not flow out from the outlet, so that the pressure in the fluid ejection chamber is maintained uniformly, and By controlling the fluid injection amount, the internal pressure of the fluid ejection chamber is easily and accurately controlled. Therefore, uniform entanglement is imparted to the fiber bundle in the longitudinal direction and the radial direction.
【0017】また、前記流体噴射室の内圧が安定化でき
るため、交絡の程度は流体の供給量によって容易に且つ
正確に調整することができ、本発明の交絡付与装置の流
体供給側の流体圧力によってモニタリングできる。な
お、前記シール室は前記流体噴射室の入口側にも設ける
ことができる。Further, since the internal pressure of the fluid ejection chamber can be stabilized, the degree of entanglement can be easily and accurately adjusted by the supply amount of the fluid, and the fluid pressure on the fluid supply side of the entanglement imparting device of the present invention can be adjusted. Can be monitored by The seal chamber can be provided on the inlet side of the fluid ejection chamber.
【0018】このように長手方向及び径方向で均一な交
絡が付与された繊維束は、炭素繊維製造工程での工程通
過安定性が確保され、炭素繊維束の物性並びに品質に優
れた炭素繊維を提供することができる。しかも工程通過
安定性が確保されることにより、工程監視点を省略でき
るなど、炭素繊維製造工程及び高次加工工程の生産性を
著しく向上させることができる。The fiber bundles imparted with uniform entanglement in the longitudinal direction and the radial direction as described above ensure the process passage stability in the carbon fiber production process, and provide carbon fibers excellent in physical properties and quality of the carbon fiber bundles. Can be provided. Moreover, by ensuring the process passage stability, the process monitoring point can be omitted, and the productivity in the carbon fiber manufacturing process and the high-order processing process can be significantly improved.
【0019】また、上述のように繊維束の長手方向及び
径方向に均一な交絡を付与することができ、前記繊維束
が不必要に高度に交絡されたり、局部的に過剰に交絡さ
れたりすることはないため、製造された炭素繊維を後に
開繊する場合にもその開繊が容易であり、開繊時の繊維
への損傷も防止され品質を維持できると共に開繊用の設
備負担を軽減できる。Further, as described above, uniform entanglement can be provided in the longitudinal direction and the radial direction of the fiber bundle, and the fiber bundle is unnecessarily highly entangled or locally excessively entangled. Therefore, even if the manufactured carbon fiber is opened later, it is easy to open the fiber, preventing damage to the fiber at the time of opening, maintaining the quality and reducing the load on the equipment for opening. it can.
【0020】なお、前記流体噴射室だけでなく、前記前
方及び後方のシール室においても、あっても、前記繊維
束は同繊維束の走行方向と直交する断面が、前記流体噴
射室と同一又は相似形の円形又は楕円形である走行路を
走行させることが好ましい。In addition, not only in the fluid ejection chamber, but also in the front and rear seal chambers, the fiber bundle has the same cross section perpendicular to the running direction of the fiber bundle as the fluid ejection chamber. It is preferable to travel on a similar circular or elliptical travel path.
【0021】更に、本件請求項2に係る発明にあって
は、前記炭素繊維前駆体繊維束として、単繊維繊度が
0.04テックス以上、0.4テックス以下であり、構
成する単繊維の数が1000本以上、80000本以下
である繊維束を採用することを特徴としている。Further, in the invention according to the second aspect of the present invention, the carbon fiber precursor fiber bundle has a single fiber fineness of not less than 0.04 tex and not more than 0.4 tex, and Is a fiber bundle of 1,000 or more and 80,000 or less.
【0022】上述のように、本発明の炭素繊維前駆体繊
維束の製造方法では均一な交絡で且つ任意の適度な集束
を付与することができるため、後に開繊が必要な場合で
あっても容易に開繊できる。そのため、単繊維繊度が
0.04テックス以上、0.4テックス以下と細い炭素
繊維前駆体繊維束であっても単糸切れや毛羽が発生する
ことはない。As described above, in the method for producing a carbon fiber precursor fiber bundle of the present invention, uniform entanglement and any appropriate convergence can be imparted, so that even when fiber opening is required later. Easy opening. Therefore, even if the carbon fiber precursor fiber bundle has a fineness of single fiber fineness of not less than 0.04 tex and not more than 0.4 tex, no single yarn breakage or fluff occurs.
【0023】本件請求項3に係る発明は、前記繊維束を
前記シール室内において走行方向に直交する断面積が異
なる複数の領域を通過させることを特徴としている。繊
維束を走行方向に直交する断面積が異なる複数の領域を
通過させるためには、即ち、シール室における繊維束の
走行路が走行方向に直交する断面積の異なる複数の領域
を有している。特に、炭素繊維前駆体繊維束に対して非
接触でシールができ、且つ装置内圧をより効果的に保持
することを可能とするために、前記シール部はラビリン
シール構造を有していることが好ましい。The invention according to a third aspect of the present invention is characterized in that the fiber bundle passes through a plurality of regions having different cross-sectional areas perpendicular to the running direction in the seal chamber. In order to allow the fiber bundle to pass through a plurality of regions having different cross-sectional areas perpendicular to the traveling direction, that is, the traveling path of the fiber bundle in the seal chamber has a plurality of regions having different cross-sectional areas perpendicular to the traveling direction. . In particular, in order to be able to seal the carbon fiber precursor fiber bundle in a non-contact manner and to be able to more effectively maintain the internal pressure of the device, the seal portion has a labyrinth seal structure. preferable.
【0024】このように、走行路が断面積が異なる複数
の領域を有しているため、前記流体噴射部からシール部
へと入り込んだ流体は、前記走行路を装置外部へと流れ
る間に複数段の渦流が発生する。従って、流体噴射室に
おいて交絡付与された繊維束は前記シール室を通過する
間に、前記渦流によって交絡がより均一化及び安定化す
る。また、シール室の内圧は複数段の前記渦流によって
前記流体噴射室から装置外部へ向けて徐々に低くなる。
そのため装置への繊維束の出入口では圧力が十分に低減
されており、流体が強い勢いで噴出することがなく、繊
維束の走行に乱れが生じたり、或いは損傷を受けること
がない。As described above, since the traveling path has a plurality of regions having different cross-sectional areas, the fluid that has entered the seal portion from the fluid ejecting section is not removed while flowing through the traveling path to the outside of the apparatus. A step vortex is generated. Therefore, the entanglement of the fiber bundle imparted in the fluid ejection chamber is more uniform and stabilized by the vortex while passing through the seal chamber. Further, the internal pressure of the seal chamber gradually decreases from the fluid ejection chamber to the outside of the apparatus due to the plurality of stages of the vortex.
Therefore, the pressure at the entrance and exit of the fiber bundle to the apparatus is sufficiently reduced, and the fluid does not erupt with a strong force, and the running of the fiber bundle is not disturbed or damaged.
【0025】本件請求項4に係る発明は、炭素繊維前駆
体繊維束として総繊度T (テックス)の繊維束を採用
し、前記流体噴射室の繊維束の走行路の内径D(mm)
をT/800<D<T/80の範囲に設定すると共に、
同流体噴射室の長さL(mm)と前記内径D(mm)と
の比の値を0.3<L/D<30の範囲に設定すること
を特徴とする。The invention according to claim 4 employs a fiber bundle having a total fineness T (tex) as the carbon fiber precursor fiber bundle, and has an inner diameter D (mm) of a traveling path of the fiber bundle in the fluid ejection chamber.
Is set in the range of T / 800 <D <T / 80, and
The ratio of the length L (mm) of the fluid ejection chamber to the inner diameter D (mm) is set in a range of 0.3 <L / D <30.
【0026】なお、繊維束走行路の内径とは、前記走行
路が円形断面であるときにはその円の直径であり、前記
走行路が楕円形断面であるときには、同楕円の面積と同
一面積の円における直径である。この楕円形の長径と短
径との比は前駆体繊維束が交絡付与装置へ供給されると
きの繊維束の断面形状に応じて適宜決定すればよい。The inner diameter of the fiber bundle traveling path is the diameter of the circle when the traveling path has a circular cross section, and the circle having the same area as the area of the ellipse when the traveling path has an elliptical cross section. Is the diameter at The ratio between the major axis and the minor axis of the elliptical shape may be appropriately determined according to the cross-sectional shape of the fiber bundle when the precursor fiber bundle is supplied to the entanglement imparting device.
【0027】前記流体噴射室の走行路の内径Dは、炭素
繊維前駆体繊維束の総繊度T(テックス)に応じて適宜
決定され、前記内径DがT/800以下であると前駆体
繊維束の乱れが拘束されて交絡が不十分となり、逆に前
記内径DがT/80以上である場合は、交絡付与装置自
体が必要以上に大きくなり動力や流体の供給量が多くな
るため製造コストがかさみ、また、前記装置の設置スペ
ースも大きくなるため、 好ましくない。更に検討を進め
た結果、前記内径DはT/500より大きく、T/10
0より小さい場合に、本発明の効果をより好ましく享受
することができる。The inner diameter D of the traveling path of the fluid injection chamber is appropriately determined according to the total fineness T (tex) of the carbon fiber precursor fiber bundle. When the internal diameter D is T / 80 or more, the confounding device itself becomes unnecessarily large and the supply amount of power and fluid increases, so that the manufacturing cost is reduced. It is not preferable because it is bulky and requires a large installation space for the device. As a result of further study, the inner diameter D was larger than T / 500 and T / 10
When it is smaller than 0, the effects of the present invention can be more preferably enjoyed.
【0028】また、シール室を除いた前記流体噴射室の
長さLと前記内径Dとの比の値は、0.3<L/D<3
0の範囲であり、L/D≦0.3であると前駆体繊維束
の乱れが拘束され交絡が不十分となり、30≦L/Dで
あると交絡付与装置自体が必要以上に大きくなり経済的
に好ましくない。The ratio of the length L of the fluid ejection chamber excluding the seal chamber to the inner diameter D is 0.3 <L / D <3.
If L / D ≦ 0.3, turbulence of the precursor fiber bundle is restrained and entanglement becomes insufficient. If 30 ≦ L / D, the entanglement imparting device itself becomes unnecessarily large, and the economy is reduced. Is not preferred.
【0029】本件請求項5に係る発明は、単一の繊維束
当たりの前記流体の流量Q(m3 /分)と単繊維の繊度
t(テックス )との比の値を、0.5<Q/t<4.
3の範囲に設定することを特徴とする。前記流量Qと繊
度tとの比の値がQ/t≦0.5以下であると流体の乱
れ、すなわち前駆体繊維束の乱されの効果が希薄にな
り、逆に4.3≦Q/tであると前駆体繊維束が過度に
乱されることによって繊維束自体の機械的物性を損なう
と同時に、毛羽を生じやすくなる。According to a fifth aspect of the present invention, the value of the ratio of the flow rate Q (m 3 / min) of the fluid per single fiber bundle to the fineness t (tex) of the single fiber is set to 0.5 < Q / t <4.
3 is set. If the value of the ratio between the flow rate Q and the fineness t is Q / t ≦ 0.5 or less, the turbulence of the fluid, that is, the effect of the turbulence of the precursor fiber bundle is diminished, and conversely 4.3 ≦ Q / At t, the precursor fiber bundle is excessively disturbed, thereby impairing the mechanical properties of the fiber bundle itself and, at the same time, easily causing fluff.
【0030】また、本件請求項6に係る発明は、走行す
る前記繊維束の張力G(g/テックス)を、0.2<G
<1.5の範囲に設定することを特徴とする。前記繊維
束の張力GがG≦0.2であると交絡装置内で弛みを生
じて交絡の斑がかりの要因になり、逆に1.5≦Gであ
ると過大な張力によって単繊維切れの原因ともなる。よ
り好ましい張力Gの範囲は、0.25g/テックス<G
<1.15g/テックスの範囲であって、前記張力Gは
交絡付与装置の前後に配置される繊維束駆動装置の速度
比によって制御することができる。Further, according to the present invention, the tension G (g / tex) of the running fiber bundle is set to 0.2 <G
It is characterized in that it is set in the range of <1.5. If the tension G of the fiber bundle is G ≦ 0.2, slack occurs in the confounding device, causing confounding spots. Conversely, if 1.5 ≦ G, excessive tension causes breakage of the single fiber. It also causes. A more preferable range of the tension G is 0.25 g / tex <G
In the range of <1.15 g / tex, the tension G can be controlled by the speed ratio of the fiber bundle driving device disposed before and after the entanglement device.
【0031】また、本発明に適用される炭素繊維前駆体
繊維束は、アクリロニトリル系繊維が好ましく、更に少
なくともアクリロニトリルを90モル%以上含有するも
のがより好ましい。The carbon fiber precursor fiber bundle applied to the present invention is preferably an acrylonitrile fiber, and more preferably contains at least 90 mol% of acrylonitrile.
【0032】更に本件請求項7に係る発明は、炭素繊維
束の製造方法であって、上述した炭素繊維前駆体繊維束
の製造方法により製造されたポリアクリロニトリル系繊
維束を耐炎化し、次いで炭素化することを特徴とする。
なお、本発明に適用される無撚の炭素繊維前駆体繊維束
は、アクリロニトリル90モル%以上のポリアクリロニ
トリル系繊維束であることが好ましい。The invention according to claim 7 is a method for producing a carbon fiber bundle, wherein the polyacrylonitrile-based fiber bundle produced by the above-mentioned method for producing a carbon fiber precursor fiber bundle is made flame-resistant, and then carbonized. It is characterized by doing.
The non-twisted carbon fiber precursor fiber bundle applied to the present invention is preferably a polyacrylonitrile fiber bundle of 90 mol% or more of acrylonitrile.
【0033】上述した炭素繊維前駆体繊維束の製造方法
により得られた前駆体繊維束は、長手方向及び径方向に
均一な交絡が付与されており、しかも開繊性にも優れて
いる。そのため、耐炎化処理時及び炭素化処理時にはロ
ールへの巻き付きや隣り合う繊維束との干渉によってダ
メージが生じることなく、長手方向及び径方向に均一に
耐炎化及び炭素化がなされ、物性に優れ、毛羽の発生も
ない高品質な炭素繊維束を得ることができる。また、炭
素繊維束の開繊が必要な場合にも、開繊ロールによって
過度にしごくことなく容易に開繊できるため、炭素繊維
束の品質を維持できる。The precursor fiber bundle obtained by the above-described method for producing a carbon fiber precursor fiber bundle has uniform entanglement in the longitudinal direction and the radial direction, and also has excellent openability. Therefore, at the time of the oxidation treatment and the carbonization treatment, no damage is caused by winding around the roll or interference with the adjacent fiber bundle, the oxidation and the carbonization are uniformly performed in the longitudinal direction and the radial direction, and the physical properties are excellent. A high-quality carbon fiber bundle free of fluff can be obtained. Further, even when the carbon fiber bundle needs to be opened, the fiber can be easily opened without excessively squeezing by the opening roll, so that the quality of the carbon fiber bundle can be maintained.
【0034】[0034]
【発明の実施の形態】以下、本発明の炭素繊維前駆体繊
維束の製造方法に好適に使用できる交絡付与装置につい
て、図面を参照して具体的に説明する。図1は、本発明
に係る炭素繊維前駆体繊維束の製造方法に好適に使用で
きる交絡付与装置の概略断面図であり、図2は図1のA
−A線から見た矢視図、図3は図1のB−B線に沿った
断面図である。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, an entanglement imparting apparatus which can be suitably used in the method for producing a carbon fiber precursor fiber bundle of the present invention will be specifically described with reference to the drawings. FIG. 1 is a schematic cross-sectional view of an entanglement imparting device that can be suitably used in the method for producing a carbon fiber precursor fiber bundle according to the present invention, and FIG.
FIG. 3 is a sectional view taken along the line BB of FIG.
【0035】交絡付与装置1は、その長手方向中央に繊
維束Fの走行路2が貫通しており、その走行路2内を繊
維束Fが連続して走行している。前記装置1の長手方向
中央に流体噴射室3が配されており、同流体噴射室3の
前後にそれぞれシール室4,5が配されている。更に、
後方のシール室5の出口にエゼクター6が配されてい
る。The running path 2 for the fiber bundle F penetrates the center of the longitudinal direction of the entanglement imparting device 1, and the fiber bundle F runs continuously in the running path 2. A fluid ejection chamber 3 is arranged at the center in the longitudinal direction of the device 1, and seal chambers 4 and 5 are arranged before and after the fluid ejection chamber 3, respectively. Furthermore,
An ejector 6 is arranged at an outlet of the rear seal chamber 5.
【0036】前記流体噴射室3は繊維束Fの走行方向に
直交する断面が円形の内壁面3aを有しており、同内壁
面3aの内部が繊維束Fの前記走行路2を構成してい
る。更に前記内壁面3aには互いに180°変位して2
つの流体噴射孔3bが開口している。前記流体噴射孔3
bは中心軸線が前記走行路2の中心線と直交して(90
°)形成されている。The fluid ejection chamber 3 has an inner wall surface 3a having a circular cross section orthogonal to the running direction of the fiber bundle F, and the inside of the inner wall surface 3a constitutes the running path 2 of the fiber bundle F. I have. Further, the inner wall surface 3a is displaced by 180 ° with respect to each other.
Three fluid injection holes 3b are open. The fluid injection hole 3
b, the center axis is perpendicular to the center line of the traveling path 2 (90
°) is formed.
【0037】前記内壁面3aの直径D(mm)は、炭素
繊維前駆体繊維束Fの総繊度をTとしたときに、T/8
00<D<T/80の範囲内に設定することが好まし
い。また、前記流体噴射室3の長さL(mm)は、0.
3<L/D<30の範囲に設定することが好ましい。The diameter D (mm) of the inner wall surface 3a is T / 8, where T is the total fineness of the carbon fiber precursor fiber bundle F.
It is preferable to set in the range of 00 <D <T / 80. Further, the length L (mm) of the fluid ejection chamber 3 is set to 0.1.
It is preferable to set the range of 3 <L / D <30.
【0038】また、図1に示す交絡付与装置1では、2
つの流体噴射孔3bを互いに180°変位させ、且つ前
記流体噴射孔3bの中心軸線を糸条の走行路2の中心線
に対して90°となるように形成しているが、前記流体
噴射孔の数及び角度は上述に限定されるものではなく、
交絡処理後の繊維束に求められる要素を十分吟味して適
宜選択し使用すればよい。In the confounding device 1 shown in FIG.
The two fluid injection holes 3b are displaced by 180 ° from each other, and the central axis of the fluid injection holes 3b is formed to be 90 ° with respect to the center line of the yarn traveling path 2. The number and angle of are not limited to those described above,
The elements required for the fiber bundle after the entanglement treatment are sufficiently examined and appropriately selected and used.
【0039】例えば、複数の流体噴射孔を同一周面内に
等間隔で形成することもでき、或いは、1以上の流体噴
射孔からなる流体噴射面を繊維束の走行方向に沿って複
数段に形成することもできる。For example, a plurality of fluid ejection holes can be formed at equal intervals in the same peripheral surface, or a fluid ejection surface composed of one or more fluid ejection holes can be formed in a plurality of steps along the running direction of the fiber bundle. It can also be formed.
【0040】また、図3に示すように、前記交絡付与装
置1には1本の炭素繊維前駆体繊維束Fを供給して交絡
処理を施しているが、本発明の範囲内であれば、前記繊
維束を多数本供給して同時に交絡処理を施すこともでき
る。但し、隣接して走行する繊維束との混繊防止や繊維
束ごとの交絡度の斑を低減するなどの観点から、単一の
交絡付与装置1に供給する繊維束の数は1本であること
が好ましい。Further, as shown in FIG. 3, one carbon fiber precursor fiber bundle F is supplied to the entanglement imparting device 1 to perform the entanglement treatment. It is also possible to supply a large number of the fiber bundles and simultaneously perform the entanglement treatment. However, the number of fiber bundles supplied to a single entanglement imparting device 1 is one from the viewpoint of preventing fiber mixing with the fiber bundle running adjacently and reducing unevenness of the degree of entanglement for each fiber bundle. Is preferred.
【0041】前記シール室4,5は、繊維束の走行方向
に直交する断面積が異なる複数の領域を形成するために
ラビリンスシール構造を採用し、ハウジング4a,5a
の内側に円筒形の複合直通型のラビリンスシール構造体
4b,5bが挿入され、且つセットボルト等により規定
の位置に固定されている。前記ラビリンスシール構造体
4b,5bの内部に形成されている繊維束Fの走行路2
は、その走行方向に直交する断面が、前記流体噴射室3
よりも径の小さな円形である。本実施形態では流体噴射
室3の前後両方の側にシール室4,5を配しているた
め、前記流体噴射室3を効果的にシールできる。The seal chambers 4 and 5 employ a labyrinth seal structure to form a plurality of regions having different cross-sectional areas perpendicular to the running direction of the fiber bundle, and the housings 4a and 5a.
A cylindrical composite through-type labyrinth seal structure 4b, 5b is inserted into the inside, and is fixed at a predetermined position by a set bolt or the like. The traveling path 2 of the fiber bundle F formed inside the labyrinth seal structures 4b, 5b
Has a cross section perpendicular to the running direction of the fluid injection chamber 3
It has a smaller diameter than a circle. In the present embodiment, since the seal chambers 4 and 5 are disposed on both front and rear sides of the fluid ejection chamber 3, the fluid ejection chamber 3 can be effectively sealed.
【0042】即ち、流体が噴射され高圧な状態にある流
体噴射室3と大気圧の装置外部との間にシール室4,5
が介在しているため、流体噴射室3内での圧力が均一に
維持される。また、前記シール室4,5により前記流体
噴射室3の内圧を容易に制御することができるため、繊
維束Fには長手方向及び径方向に均一な交絡を付与する
ことができ、必要に応じて交絡の程度を自由に調節でき
る。That is, the seal chambers 4, 5 are provided between the fluid injection chamber 3 in which the fluid is injected and in a high pressure state and the outside of the apparatus at atmospheric pressure.
, The pressure in the fluid ejection chamber 3 is maintained uniformly. In addition, since the internal pressure of the fluid ejection chamber 3 can be easily controlled by the seal chambers 4 and 5, uniform entanglement can be imparted to the fiber bundle F in the longitudinal direction and the radial direction. The degree of confounding can be adjusted freely.
【0043】また、上記実施形態にあっては特に、シー
ル室4,5がラビリンスシール構造を有しており複数段
の渦流が形成されるため、シール室4,5内の圧力は前
記流体噴射室3から装置外部へ向けて徐々に低くなって
おり、前記流体噴射室3において交絡が付与された繊維
束Fは、この複数段の渦流を通過することにより交絡が
より均一化及び安定化される。Further, in the above-described embodiment, in particular, since the seal chambers 4 and 5 have a labyrinth seal structure and a plurality of vortices are formed, the pressure in the seal chambers 4 and 5 is reduced by the fluid injection. The fiber bundle F, which is gradually lowered from the chamber 3 toward the outside of the apparatus, and is entangled in the fluid ejection chamber 3, passes through the plurality of vortices, whereby the entanglement is made more uniform and stabilized. You.
【0044】また、流体噴射室3の繊維束の出入口近傍
での急激な圧力の変化を抑制でき、前記交絡付与装置1
への繊維束の出入口において流体が強い勢いで噴出する
こともないため、繊維束Fは安定した走行が可能とな
り、糸揺れもなく、装置1の出入口や走行路2の周壁へ
の接触による損傷も発生しない。なお、本実施例のよう
に、前記流体噴射室3の出入口の双方に前記シール室
4,5は設けることが最も望ましいが、装置1の設置ス
ペース等を考慮して前記流体噴射室3の出口側にのみシ
ール室を設けることもできる。Further, it is possible to suppress a rapid change in pressure near the entrance and exit of the fiber bundle in the fluid ejection chamber 3, and the entanglement imparting device 1
Since the fluid does not erupt with a strong force at the entrance of the fiber bundle to the fiber bundle, the fiber bundle F can run stably, there is no yarn sway, and damage due to contact with the entrance and exit of the device 1 and the peripheral wall of the traveling path 2 Also does not occur. It is most preferable to provide the seal chambers 4 and 5 at both the entrance and exit of the fluid ejection chamber 3 as in the present embodiment, but the exit of the fluid ejection chamber 3 is considered in consideration of the installation space of the apparatus 1 and the like. It is also possible to provide a sealing chamber only on the side.
【0045】上述した交絡付与装置1を用いて炭素繊維
前駆体繊維束に交絡を付与する場合には、先ず、前記エ
ゼクター6を用いて繊維束を前記交絡付与装置1の走行
路2内に挿通させる。前記エゼクター6に流体導入口6
aから流体を供給すると共に交絡付与装置1の内部を減
圧下にした状態で、繊維束を交絡装置1の走行路2の入
り側に近づけると繊維束Fが交絡付与装置1の内部に挿
入されるものであり、通糸が容易になる。なお、前記エ
ゼクター6は繊維束Fの挿通作業が終了した後は、前記
流体導入口6aからの流体の導入は停止される。When the entanglement is imparted to the carbon fiber precursor fiber bundle by using the entanglement imparting device 1 described above, first, the fiber bundle is inserted into the traveling path 2 of the entanglement imparting device 1 by using the ejector 6. Let it. The ejector 6 has a fluid inlet 6
When the fiber bundle is brought close to the entrance side of the traveling path 2 of the entanglement device 1 in a state where the fluid is supplied from a and the inside of the entanglement device 1 is reduced in pressure, the fiber bundle F is inserted into the entanglement device 1. This makes threading easier. After the operation of inserting the fiber bundle F into the ejector 6 is completed, the introduction of the fluid from the fluid introduction port 6a is stopped.
【0046】こうして交絡付与装置1に繊維束Fを挿通
させた後、前記繊維束Fを走行させると共に同装置1を
駆動して前記繊維束Fに交絡を付与する。なお、この交
絡付与装置1に挿通された繊維束Fは緊張下にあり、こ
の繊維束Fに付与する張力G(g/テックス)は0.2
<G<1.5の範囲内に設定することが好ましい。After the fiber bundle F is inserted into the entanglement imparting device 1 in this manner, the fiber bundle F is run and the device 1 is driven to impart the entanglement to the fiber bundle F. The fiber bundle F inserted into the entanglement device 1 is under tension, and the tension G (g / tex) applied to the fiber bundle F is 0.2.
It is preferable to set within the range of <G <1.5.
【0047】前方のシール室4から交絡付与装置1へと
導入された前記繊維束Fは、装置の入口において急激な
圧力変動がないため、大きな糸揺れがなく、安定した走
行が維持される。前記前方のシール室4では、前記繊維
束Fは複数段の渦流を通過し、弱い交絡が付与される。
更に、流体噴射室3に導入されて互いに180°変位し
た2つの流体噴射孔3bから繊維束Fに向けて90°の
方向ベクトルで、所定圧力及び所定流量で流体が噴射さ
れる本格的な交絡が付与された後、後方のシール室5へ
と導入される。The fiber bundle F introduced from the front seal chamber 4 to the entanglement imparting device 1 does not have a sudden pressure fluctuation at the entrance of the device, so that there is no large yarn sway and stable running is maintained. In the front seal chamber 4, the fiber bundle F passes through a plurality of vortices, and is weakly entangled.
Further, full-fledged confounding in which fluid is jetted at a predetermined pressure and a predetermined flow rate from the two fluid jet holes 3b introduced into the fluid jet chamber 3 and displaced by 180 ° toward the fiber bundle F from the two fluid jet holes 3b. Is provided to the rear seal chamber 5.
【0048】この後方のシール室5では再び複数段で渦
流が作用し、交絡がより均一化されると共に安定化され
る。その後、エゼクター6から装置外部へと導出される
が、このときも、装置内外では急激な圧力変化はないた
め、繊維束に大きな揺れは生じることなく、安定した走
行が維持される。In the rear seal chamber 5, the vortex acts again in a plurality of stages, and the confounding becomes more uniform and stabilized. Thereafter, the fluid is drawn out of the ejector 6 to the outside of the apparatus. In this case, too, there is no sudden pressure change inside and outside the apparatus, so that the fiber bundle does not largely shake and stable running is maintained.
【0049】なお、交絡に使用される流体としては特別
に限定はないが、価格並びに取扱性の観点から常温空気
を採用することが好ましく、また、単一の繊維束当たり
の前記流体の流量Q(m3 /分)と、単繊維繊度t(テ
ックス)との比の値は、繊維束の構成単繊維のテックス
をtとしたときに、0.5<Q/t<4.3の範囲に設
定することが好ましい。なお、この流量Qは前記交絡付
与装置1の流体供給側の流体圧力によってモニタリング
することができる。The fluid used for the entanglement is not particularly limited, but it is preferable to use room temperature air from the viewpoint of cost and handleability, and the flow rate Q of the fluid per single fiber bundle The value of the ratio between (m 3 / min) and the single fiber fineness t (tex) is in the range of 0.5 <Q / t <4.3, where t is the tex of the single fiber constituting the fiber bundle. It is preferable to set The flow rate Q can be monitored by the fluid pressure on the fluid supply side of the confounding device 1.
【0050】このようにして得られた炭素繊維前駆体繊
維束は、続けて炭素繊維製造工程へと導入することもで
き、又は、一旦、巻き取った後に炭素繊維製造工程へと
導入することもできる。或いは、必要に応じて炭素繊維
製造工程中のいづれかの場所に上述した交絡付与装置を
配置して交絡を付与することも可能である。The carbon fiber precursor fiber bundle obtained in this manner can be continuously introduced into a carbon fiber production process, or can be once wound and then introduced into a carbon fiber production process. it can. Alternatively, it is also possible to arrange the above-described entanglement imparting device at any place during the carbon fiber manufacturing process to impart the entanglement as needed.
【0051】炭素繊維製造工程では、交絡が付与された
前記炭素繊維前駆体繊維束を酸化性雰囲気中で200℃
以上に加熱して耐炎化処理を施し、次いで不活性雰囲気
中で300℃以上に加熱して炭素化処理を施すことによ
り、を製造することができる。更に、この後、より高温
域での黒鉛化処理を施すこともできる。In the carbon fiber production step, the entangled carbon fiber precursor fiber bundle is heated at 200 ° C. in an oxidizing atmosphere.
By performing the above-described heat-resistant treatment, and then performing the carbonization treatment by heating to 300 ° C. or more in an inert atmosphere, the product can be manufactured. Further, thereafter, a graphitization treatment in a higher temperature range can be performed.
【0052】この製造工程において、上述の方法により
交絡が付与された前記炭素繊維前駆体繊維束は適度な集
束性をもつため、耐炎化処理や炭素化処理において複数
の繊維束をシート状に並べ、且つ複数のロールに掛け回
して走行させる場合にも、隣り合う繊維束と接触した
り、ロールに巻き付いたりするなどの不都合が生じるこ
とはなく、毛羽や単糸切れが少ない高品質で且つ機械的
特性にも優れたを製造することができる。更には、炭素
繊維前駆体繊維束は、長手方向及び径方向に均一な交絡
が付与されており、しかもその交絡程度を自由に制御し
て適度な集束性を付与できるため、の用途により後に開
繊が必要となった場合にも、過剰な負荷を加えることな
く容易に開繊でき、品質及び機械的特性を維持できる。In this manufacturing process, since the carbon fiber precursor fiber bundle entangled by the above-described method has an appropriate bunching property, a plurality of fiber bundles are arranged in a sheet in a flame-resistant treatment or a carbonization treatment. Also, even when running while being wound around a plurality of rolls, there is no inconvenience such as contact with adjacent fiber bundles or winding around the rolls, and high quality and machine with less fluff and single yarn breakage With excellent mechanical properties. Further, the carbon fiber precursor fiber bundle is given uniform entanglement in the longitudinal direction and the radial direction, and the degree of the entanglement can be freely controlled to give appropriate convergence. Even when fiber is required, the fiber can be easily opened without applying an excessive load, and quality and mechanical properties can be maintained.
【0053】以下、本発明について具体的な実施例及び
比較例を挙げて説明する。実施例及び各比較例では上述
した図1に示す、繊維束の走行路の断面形状が円形であ
り、流体噴射室3には繊維束の走行方向に対して90°
(直交)の同一平面内に2つの流体噴射孔3bが互いに
180°変位して形成されている交絡付与装置1を用い
て繊維束に交絡付与処理を施している。このとき、各実
施例及び比較例において流体噴射室3における繊維束の
走行路2(内壁面3a)の内径D(mm)、前記流体噴
射室3の長さL(mm)、単一の繊維束当たりの流体の
流量Q(m3 /分)、及び繊維束Fの張力G(g/テッ
クス)を表1に示す数値に設定している。それぞれ処理
後の繊維束について交絡の均一性を評価し、その結果も
表1に示している。なお、交絡の均一性はJIS−L1
013に準じて測定した繊維束の交絡度におけるばらつ
きを示すCV値である。また、炭素繊維製造工程での工
程通過性についても評価した。Hereinafter, the present invention will be described with reference to specific examples and comparative examples. In the embodiment and each comparative example, the cross section of the running path of the fiber bundle is circular as shown in FIG.
The entanglement imparting process is performed on the fiber bundle by using the entanglement imparting device 1 in which the two fluid ejection holes 3b are displaced from each other by 180 ° in the same (orthogonal) plane. At this time, in each of the examples and comparative examples, the inner diameter D (mm) of the fiber bundle traveling path 2 (the inner wall surface 3a) in the fluid ejection chamber 3, the length L (mm) of the fluid ejection chamber 3, the single fiber The flow rate Q (m 3 / min) of the fluid per bundle and the tension G (g / tex) of the fiber bundle F are set to the values shown in Table 1. Each of the treated fiber bundles was evaluated for uniformity of entanglement, and the results are also shown in Table 1. In addition, the uniformity of confounding was determined according to JIS-L1.
It is a CV value indicating a variation in the degree of entanglement of the fiber bundle measured according to No. 013. In addition, the processability in the carbon fiber production process was also evaluated.
【0054】以下の実施例及び比較例において、 繊維束:アクリロニトリル96モル%含有 単繊維繊度:0.14テックス 繊維束を構成する単繊維の数:12000本 繊維束の総繊度:1680テックス 流体:常温空気 繊維束の張力:0.5g/テックス 繊維束の交絡処理装置走行速度:10m/分 であり、これらの条件は全て同一としている。In the following Examples and Comparative Examples: Fiber bundle: 96 mol% of acrylonitrile Single fiber fineness: 0.14 tex Number of single fibers constituting the fiber bundle: 12,000 Total fineness of fiber bundle: 1680 tex Fluid: Room temperature Air Fiber bundle tension: 0.5 g / tex Fiber bundle entanglement treatment device running speed: 10 m / min. These conditions are all the same.
【表1】 [Table 1]
【0055】[実施例1]流体噴射室の内径D、前記流
体噴射室の長さL、1の繊維束当たりの流体の流量Q、
及び繊維束Fの張力Gの全てが好適な範囲内にある実施
例1では、CV値が8%であり、長手方向及び径方向と
もに均一な斑のない交絡が付与されており、適度な集束
性をもつ前駆体繊維束を得ることができた。更に、炭素
繊維製造工程の通過性を観察した結果、ロールへの巻き
付きや隣り合う繊維束との混繊、干渉等のトラブルも無
く工程通過性良好で、かつ炭素繊維束の開繊性も良好で
あった。[Example 1] The inner diameter D of the fluid ejection chamber, the length L of the fluid ejection chamber, the flow rate Q of the fluid per fiber bundle,
In Example 1 in which the tension G of the fiber bundle F is all within a suitable range, the CV value is 8%, uniform entanglement is provided in both the longitudinal direction and the radial direction, and moderate convergence is achieved. The precursor fiber bundle having the property was obtained. Furthermore, as a result of observing the passability of the carbon fiber production process, there is no trouble such as winding around a roll or blending with an adjacent fiber bundle, interference, etc., and the process passability is good, and the carbon fiber bundle openability is good. Met.
【0056】[比較例1]流体噴射室の繊維束走行路の
内径Dが1.8mmと好適な範囲の下限(T/800=
2.1mm)よりも小さいため、繊維束の乱れが拘束さ
れ交絡が不十分であった。また、交絡の均一性について
みても、CV値が17%であり斑が大きい。更に、炭素
繊維製造工程の通過性を観察した結果、集束性が不十分
であったためロールへの捲き付きが多発し、得られたに
は毛羽が多く発生していた。[Comparative Example 1] The inner diameter D of the fiber bundle traveling path of the fluid ejection chamber is 1.8 mm, which is the lower limit of a suitable range (T / 800 =
2.1 mm), the turbulence of the fiber bundle was restricted and confounding was insufficient. Also, regarding the uniformity of confounding, the CV value is 17%, and the spots are large. Furthermore, as a result of observing the passability in the carbon fiber production process, the bundle was insufficiently converged and frequently wound around the roll.
【0057】[比較例2]流体噴射室の長さL(mm)
と内径D(mm)との比の値が2/10=0.2と好適
な範囲の下限(0.3)よりも小さいため、繊維束の乱
れが拘束され交絡が不十分であった。また、交絡の均一
性についてみても、CV値が14%であり斑が認められ
た。更に、炭素繊維製造工程の通過性を観察した結果、
集束性が不十分であったためロールへの捲き付きが多発
し、得られたは開繊斑も大きかった。Comparative Example 2 Length L (mm) of Fluid Injection Chamber
Since the value of the ratio between the diameter and the inner diameter D (mm) was 2/10 = 0.2, which was smaller than the lower limit (0.3) of the preferred range, the turbulence of the fiber bundle was restrained and confounding was insufficient. Also, regarding the uniformity of confounding, the CV value was 14%, and spots were observed. Furthermore, as a result of observing the permeability of the carbon fiber manufacturing process,
Due to insufficient convergence, wrapping around the roll occurred frequently, and the resulting spread was large.
【0058】[比較例3]単一の繊維束当たりの流体の
流量Qが0.04m3 /分であり、前記流量Qと単繊維
繊度tとの比の値が0.04/0.14=0.28と好
適な範囲の下限(0.5)よりも小さいため、流体の乱
れの効果が小さくなり、交絡が不充分であった。また、
交絡の均一性についてみても、CV値は16%であり、
不均一であった。更に炭素繊維製造工程の通過性を観察
した結果、集束性が不十分であったためロールへの捲き
付き、並びに隣接繊維束との混繊が多発し、工程通過性
は低かった。Comparative Example 3 The flow rate Q of the fluid per single fiber bundle was 0.04 m 3 / min, and the ratio of the flow rate Q to the single fiber fineness t was 0.04 / 0.14. = 0.28, which is smaller than the lower limit (0.5) of the preferable range, the effect of fluid turbulence was reduced, and confounding was insufficient. Also,
As for the uniformity of confounding, the CV value is 16%,
It was uneven. Furthermore, as a result of observing the passability in the carbon fiber production process, the bundle was insufficiently bundled, so that winding around a roll and mixing with an adjacent fiber bundle occurred frequently, and the process passability was low.
【0059】[比較例4]1の繊維束当たりの流体の流
量Qが0.65m3 /分であり、前記流量Qと単繊維繊
度tとの比の値が0.65/0.14=4.64と好適
な範囲の上限(4.3)よりも大きいため、繊維束は過
度に乱され、繊維束自体の機械的物性が低下すると共
に、毛羽の発生が認められた。また、交絡の均一性につ
いてみても、CV値が21%と、斑が極めて大きかっ
た。更に炭素繊維製造工程の通過性も低く、得られた炭
素繊維束は毛羽が多く、外観及び機械的特性の悪いもの
であった。Comparative Example 4 The flow rate Q of the fluid per fiber bundle in one fiber bundle was 0.65 m 3 / min, and the value of the ratio between the flow rate Q and the single fiber fineness t was 0.65 / 0.14 = Since it was 4.64, which is larger than the upper limit of the preferred range (4.3), the fiber bundle was excessively disturbed, the mechanical properties of the fiber bundle itself were reduced, and the generation of fluff was observed. In addition, regarding the uniformity of the confounding, the CV value was 21%, and the spots were extremely large. Furthermore, the permeability of the carbon fiber production process was low, and the obtained carbon fiber bundle had many fluffs and was poor in appearance and mechanical properties.
【0060】[比較例5]繊維束Fへの張力が0.15
g/テックスと、好適な範囲の下限(0.2g/テック
ス)よりも小さいため、交絡付与装置内で繊維束に弛み
が生じ、CV値が21%と極めて交絡斑の大きい前駆体
繊維束となった。更に、炭素繊維製造工程の通過性を観
察した結果、ロールへの巻き付き、隣り合う繊維束との
混繊や干渉等のトラブルは無かったものの、炭素繊維束
の開繊斑が大きく、均一な耐炎化や炭素化がなされなか
った。また、高次工程での繊維束幅も不均一であった。[Comparative Example 5] The tension on the fiber bundle F was 0.15.
g / tex and smaller than the lower limit of the preferred range (0.2 g / tex), the fiber bundle is slackened in the confounding device, and the CV value is 21%, and the precursor fiber bundle is extremely large in confounding spots. became. Furthermore, as a result of observing the passability of the carbon fiber production process, there was no trouble such as winding around a roll, mixing or interference with an adjacent fiber bundle, but the spread of carbon fiber bundle spread was large and uniform flame resistance was observed. No carbonization or carbonization was done. Further, the fiber bundle width in the higher order process was also non-uniform.
【0061】以上のように、本発明の炭素繊維前駆体繊
維束の製造方法によれば、適度な集束性をもつ均一な交
絡を付与することが可能になり、炭素繊維製造工程にお
ける高い操業安定性を維持できる。更に、上記方法によ
り製造された炭素繊維前駆体繊維束を用いた本発明の炭
素繊維束製造方法によれば、毛羽並びに単糸切れが少な
く、開繊性及び機械的特性に優れており、炭素繊維製造
工程での高い操業安定性、炭素繊維束の高い品質、品
位、及び高次工程での優れた取扱性の全てを同時に確立
することが可能になる。As described above, according to the method for producing a carbon fiber precursor fiber bundle of the present invention, it is possible to impart uniform entanglement with appropriate convergence, and to achieve high operation stability in the carbon fiber production process. Can maintain sex. Furthermore, according to the method for producing a carbon fiber bundle of the present invention using the carbon fiber precursor fiber bundle produced by the above method, there are few fluffs and single yarn breaks, and the fiber opening properties and mechanical properties are excellent. It is possible to simultaneously establish high operation stability in the fiber manufacturing process, high quality and quality of the carbon fiber bundle, and excellent handleability in the high-order process.
【図1】図1は本発明に好適に用いられる交絡付与装置
の概略を示す断面図である。FIG. 1 is a cross-sectional view schematically illustrating a confounding device suitably used in the present invention.
【図2】図2は図1のA−A線から見た矢視図である。FIG. 2 is a view as seen from an arrow AA in FIG. 1;
【図3】図3は図1のB−B線に沿った断面図である。FIG. 3 is a sectional view taken along the line BB of FIG. 1;
1 交絡付与装置 2 繊維束の走行路 3 流体噴射室 3a 内壁面 3b 流体噴射孔 4 シール室 4a ハウジング 4b ラビリンスシール構造体 5 シール室 5a ハウジング 5b ラビリンスシール構造体 6 エゼクター 6a 流体導入口 F 炭素繊維前駆体繊維束 DESCRIPTION OF SYMBOLS 1 Entangling device 2 Fiber bundle traveling path 3 Fluid injection chamber 3a Inner wall surface 3b Fluid injection hole 4 Seal chamber 4a Housing 4b Labyrinth seal structure 5 Seal chamber 5a Housing 5b Labyrinth seal structure 6 Ejector 6a Fluid inlet F Carbon fiber Precursor fiber bundle
───────────────────────────────────────────────────── フロントページの続き (72)発明者 芝橋 正宏 広島県大竹市御幸町20番1号 三菱レイヨ ン株式会社大竹事業所内 (72)発明者 長嶺 定利 広島県大竹市御幸町20番1号 三菱レイヨ ン株式会社大竹事業所内 (72)発明者 下田代 有生 広島県大竹市御幸町20番1号 三菱レイヨ ン株式会社大竹事業所内 Fターム(参考) 4L035 CC11 FF01 MB00 4L036 MA04 MA33 PA41 UA07 UA08 4L037 CS03 FA03 PA53 PC05 PF23 PF57 PF59 PS02 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Masahiro Shibahashi 20-1 Miyukicho, Otake City, Hiroshima Prefecture Inside Mitsubishi Rayon Co., Ltd. Otake Works (72) Inventor Satoshi Nagamine 20-1 Miyukicho, Otake City, Hiroshima Prefecture No. Mitsubishi Rayon Co., Ltd. Otake Works (72) Inventor Yuki Shimodairo 20-1 Miyukicho, Otake City, Hiroshima Prefecture Mitsubishi Rayon Co., Ltd. Otake Works F-term (reference) 4L035 CC11 FF01 MB00 4L036 MA04 MA33 PA41 UA07 UA08 4L037 CS03 FA03 PA53 PC05 PF23 PF57 PF59 PS02
Claims (7)
に流体を噴射して交絡を付与する方法であって、 前記繊維束を交絡付与装置の出口に配されたエゼクター
を用いて前記交絡付与装置の入口から出口へと挿通させ
ること、 前記繊維束が前記交絡付与装置の入口から出口へと走行
する間に、前記繊維束に前記流体噴射室において流体を
噴射した後、同流体噴射室に続くシール室を通過させる
こと、及び少なくとも前記流体噴射室において、前記繊
維束は同繊維束の走行方向と直交する断面が円形又は楕
円形である走行路を走行させること、を特徴とする炭素
繊維前駆体繊維束の製造方法。1. A method of injecting a fluid into a substantially untwisted carbon fiber precursor fiber bundle to impart entanglement, wherein the fiber bundle is entangled using an ejector arranged at an outlet of an entanglement imparting device. After the fiber bundle travels from the inlet to the outlet of the entanglement applying device, the fluid is ejected to the fiber bundle in the fluid ejection chamber while the fiber bundle travels from the entrance to the exit of the entanglement applying device. Passing through a seal chamber following the chamber, and at least in the fluid ejection chamber, the fiber bundle travels along a traveling path having a circular or elliptical cross section orthogonal to the traveling direction of the fiber bundle. A method for producing a carbon fiber precursor fiber bundle.
維繊度が0.04テックス以上、0.4テックス以下で
あり、構成する単繊維の数が1000本以上、8000
0本以下である繊維束を採用することを特徴とする請求
項1記載の炭素繊維前駆体繊維束の製造方法。2. The carbon fiber precursor fiber bundle has a single fiber fineness of 0.04 tex or more and 0.4 tex or less, and the number of constituent single fibers is 1,000 or more and 8000 or more.
The method for producing a carbon fiber precursor fiber bundle according to claim 1, wherein a fiber bundle having 0 or less fibers is employed.
行方向に直交する断面積が異なる複数の領域を通過させ
ることを特徴とする請求項1又は2記載の炭素繊維前駆
体繊維束の製造方法。3. The method for producing a carbon fiber precursor fiber bundle according to claim 1, wherein the fiber bundle is passed through a plurality of regions having different cross-sectional areas perpendicular to a running direction in the seal chamber.
(テックス)の繊維束を採用し、前記流体噴射室の繊維
束の走行路の内径D(mm)をT/800<D<T/8
0の範囲に設定すると共に、同流体噴射室の長さL(m
m)と前記内径D(mm)との比を0.3<L/D<3
0の範囲に設定することを特徴とする請求項1〜3のい
ずれかに記載の炭素繊維前駆体繊維束の製造方法。4. A carbon fiber precursor fiber bundle having a total fineness T
(Tex) fiber bundle, and the inner diameter D (mm) of the running path of the fiber bundle in the fluid ejection chamber is T / 800 <D <T / 8.
0 and the length L (m
m) and the inner diameter D (mm) are set to 0.3 <L / D <3.
The method for producing a carbon fiber precursor fiber bundle according to any one of claims 1 to 3, wherein the value is set to 0.
(m3 /分)と単繊維の繊度t(テックス )との比の値
を、0.5<Q/t<4.3の範囲に設定することを特
徴とする請求項1〜4のいずれかに記載の炭素繊維前駆
体繊維束の製造方法。5. The flow rate Q of said fluid per single fiber bundle
The value of the ratio between (m 3 / min) and the fineness t (tex) of the single fiber is set in the range of 0.5 <Q / t <4.3. A method for producing a carbon fiber precursor fiber bundle according to any one of the above.
クス)を、0.2<G<1.5の範囲に設定することを
特徴とする請求項1〜5のいずれかに記載の炭素繊維前
駆体繊維束の製造方法。6. The method according to claim 1, wherein a tension G (g / tex) of the running fiber bundle is set in a range of 0.2 <G <1.5. A method for producing a carbon fiber precursor fiber bundle.
維前駆体繊維束の製造方法により製造されたポリアクリ
ロニトリル系繊維束を耐炎化し、次いで炭素化すること
を特徴とする炭素繊維束の製造方法。7. A carbon fiber bundle obtained by oxidizing a polyacrylonitrile-based fiber bundle produced by the method for producing a carbon fiber precursor fiber bundle according to claim 1 and then carbonizing it. Manufacturing method.
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