JPS62282025A - Production of pitch carbon yarn - Google Patents

Production of pitch carbon yarn

Info

Publication number
JPS62282025A
JPS62282025A JP12082186A JP12082186A JPS62282025A JP S62282025 A JPS62282025 A JP S62282025A JP 12082186 A JP12082186 A JP 12082186A JP 12082186 A JP12082186 A JP 12082186A JP S62282025 A JPS62282025 A JP S62282025A
Authority
JP
Japan
Prior art keywords
pitch
guide
fibers
spinning
guide mechanism
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP12082186A
Other languages
Japanese (ja)
Inventor
Kazutoshi Haraguchi
和敏 原口
Akio Nanto
南都 明男
Eiji Tanigawa
谷川 栄司
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
DIC Corp
Osaka Gas Co Ltd
Original Assignee
Osaka Gas Co Ltd
Dainippon Ink and Chemicals Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Osaka Gas Co Ltd, Dainippon Ink and Chemicals Co Ltd filed Critical Osaka Gas Co Ltd
Priority to JP12082186A priority Critical patent/JPS62282025A/en
Publication of JPS62282025A publication Critical patent/JPS62282025A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To obtain high-quality tow stably without causing end breakage, wrapping, etc., by bundling pitch yarn spun from a great number of nozzles by two or more specific guide mechanisms. CONSTITUTION:In forming tow by bundling a pitch yarn group 3 spun from a great number of nozzles of a spinning head 1, the pitch yarn group after spinning is treated by using two or more guides. A fixed type guide which will not rotate is used as a first guide 7 and a rotary roller having low resistance is used a second guide 9.

Description

【発明の詳細な説明】 発明の詳細な説明 良釆よの五■匁1 本発明は、ピッチ系材料を原見とする炭素繊維の製造方
法に関する。
DETAILED DESCRIPTION OF THE INVENTION Detailed Description of the Invention The present invention relates to a method for producing carbon fiber using a pitch-based material.

旭米反框及堕工辺訓貝荒 ピッチ系材料を紡糸し、不融化し、炭化及び/又は黒鉛
化して得られるピッチ系炭化繊維は、ポリアクリロニト
リル(、PA、N)等の有機合成繊維をプリカーサ−と
する炭素繊維に比して、原料が安価で炭化時の収率が高
いので製造コストが低い、高弾性率の製造が得られやす
い等の理由により、より安価で高性能の素材となり得る
ものと期待されている。しかしながら、ピッチ系、炭素
構維の、製造上の問題点の一つは、ピッチ系材料から得
られるプリカーサ−(ピッチ繊維〉がPA、N等の有機
合成繊維に比して脆弱であるみ、従来の有機合成繊維の
紡糸において用いられている〃法では、ヒ:ツチ繊維を
紡糸・集束する際に毛羽の原因となる糸切れを生じたり
、口、−ラーへの巻きつきが、生じたり、集*性が低か
ったりすることから、欠陥、の少ないピッチ繊維を安定
して連続的に紡糸することか難しい点にある。これらの
問題点を充分に解決することなく得られた炭素繊維は、
当然のことながら、物性、毛羽立ち性などの点からみて
品質安定性に劣り、又紡糸時の歩止まりが悪いので、製
造コストの上臂をもたらす。
Pitch-based carbonized fibers obtained by spinning, infusible, carbonizing, and/or graphitizing pitch-based materials are organic synthetic fibers such as polyacrylonitrile (, PA, N). Compared to carbon fiber that uses carbon fiber as a precursor, it is a cheaper and higher-performance material because the raw material is cheaper and the yield during carbonization is lower, so the manufacturing cost is lower, and it is easier to produce with a high modulus of elasticity. It is expected that this will become possible. However, one of the manufacturing problems with pitch-based and carbon fibers is that the precursor (pitch fiber) obtained from pitch-based materials is weaker than organic synthetic fibers such as PA and N. In the conventional method used for spinning organic synthetic fibers, when spinning and bundling H:Tutsi fibers, thread breakage that causes fuzz occurs, and winding around the ends and ends of the fibers occurs. It is difficult to stably and continuously spin pitch fibers with few defects due to their low aggregation properties.The carbon fibers obtained without fully solving these problems are ,
Naturally, quality stability is poor in terms of physical properties, fluffiness, etc., and the yield during spinning is poor, resulting in higher production costs.

問題点を解決するための手段 本発明者は、上記の如き従来技術の現状に鑑みて鋭意研
究を重ねた結果、ピッチ繊維を集束し、トウを作る工程
において、少なくとも2個のカイト機構を使用し、第一
のガイド機構を回転しない固定型カイト又はエアサッカ
ーにより構成し、第二のカイト機構を回転抵抗の小さい
回転ローラーにより構成する場合には、従来技術の問題
点を大巾に軽減し得ることを見出した。更に又は、第一
のカイト機構にいたる前にピンチ繊維に集束剤を付与す
る場合には、より一層良好な結果が得られることも判明
した。即ち、本発明は、以下の方法を提供するものであ
る: ■ ピンチ系材料を多ホールノズルを用いて紡糸し、不
融化し、炭化及び/又は黒鉛化して炭素繊維を製造する
方法において、紡糸したピッチ繊維を集束してトウを形
成させるに際し、2個以上のカイト機構を使用し、第一
のカイト機構を回転しない固定型カイト又はエアサッカ
ーにより構成し、第二のガイド機構を回転抵抗の小さい
回転ローラーにより構成することを特徴とするピッチ系
炭素繊維の製造方法。
Means for Solving the Problems As a result of extensive research in view of the current state of the prior art as described above, the present inventor has developed a method that uses at least two kite mechanisms in the process of converging pitch fibers and making tows. However, if the first guide mechanism is configured with a fixed kite or air sucker that does not rotate, and the second kite mechanism is configured with a rotating roller with low rotational resistance, the problems of the prior art can be greatly alleviated. I found out what I got. Furthermore, it has also been found that even better results are obtained if the pinched fibers are provided with a sizing agent before reaching the first kite mechanism. That is, the present invention provides the following method: ■ A method for producing carbon fiber by spinning a pinch material using a multi-hole nozzle, making it infusible, and carbonizing and/or graphitizing it. When converging pitch fibers to form a tow, two or more kite mechanisms are used, the first kite mechanism being a fixed kite or air sucker that does not rotate, and the second guide mechanism being configured with a rotational resistance. A method for producing pitch-based carbon fiber, characterized by comprising using small rotating rollers.

■ ノズル面と第一のカイト機構との間でピンチ繊維に
集束剤を付与する上記■に記載のピッチ系炭素繊維の製
造方法。
(2) The method for producing pitch-based carbon fibers according to (2) above, wherein a sizing agent is applied to the pinched fibers between the nozzle surface and the first kite mechanism.

本発明で使用する紡糸用ピッチ系vJiFlは、ピッチ
状物質を不活性カス流通下に熱重縮合させることにより
得ることが好ましい。ピッチ状物質としては、石油系ピ
ッチ、石炭系ピンチ及び有機化合物からの熱分解残渣ピ
ッチのいずれてあっても良い。
The spinning pitch system vJiFl used in the present invention is preferably obtained by thermal polycondensation of a pitch-like substance while flowing an inert gas. The pitch-like substance may be any of petroleum-based pitch, coal-based pinch, and pyrolysis residue pitch from organic compounds.

本発明方法で使用するガイド機構は、ボビン巻き又はケ
ンス取りする場合のトラバースカイト又はエアサッカー
を除いて2個以上必要であり、1個ではピッチ繊維の集
束が良好に行なわれない。
Two or more guide mechanisms are required for use in the method of the present invention, except for traverse skies or air suckers for bobbin winding or can picking, and pitch fibers cannot be focused well with one guide mechanism.

ピッチ繊維を集束する2個以上のガイド機構のうちの第
一のものは、回転しない固定型のガイド又はエアサッカ
ーであることを要する。第一のガイド機構が回転型のカ
イト、例えば、回転抵抗の小さいフリーローラーである
場合には、ピンチ繊維の単糸切れが多発して切れた糸が
回転するローラーに巻き付いて、紡糸の続行が不可能と
なる。固定型ガイドの材質及び形状は、表面が硬くかつ
滑らかで、電気抵抗及び接触抵抗の小さいものであれば
良く、特に制限されない。その材質としては、硬質クロ
ムメッキを施したアルミニウム、導電性を付与し剛性樹
脂等が例示される。エアサッカーに付いても、均等な空
気の送り込みが可能で、内面が滑らかな曲面であれば良
く、固定型ガイドと同様な材質を使用することができる
。第二のガイド機構は、回転抵抗の小さい回転ローラー
により構成することを必須とする。第二のガイド機構を
固定型カイトとする場合には、毛羽の原因となる糸切れ
が多発する。回転ローラーの材質は、第一のガイド機構
のそれと同様で良い。
The first of the two or more guide mechanisms for focusing the pitch fibers must be a fixed, non-rotating guide or air sucker. If the first guide mechanism is a rotating kite, such as a free roller with low rotational resistance, the pinched fibers will often break, causing the broken threads to wrap around the rotating rollers, making it difficult to continue spinning. It becomes impossible. The material and shape of the fixed guide are not particularly limited as long as they have a hard and smooth surface and low electrical resistance and contact resistance. Examples of the material include aluminum plated with hard chrome, and rigid resin that provides conductivity. As for the air sucker, it only needs to be able to send air evenly and have a smooth curved inner surface, and can be made of the same material as the fixed guide. The second guide mechanism must be constructed of a rotating roller with low rotational resistance. When the second guide mechanism is a fixed kite, thread breakage that causes fluff occurs frequently. The material of the rotating roller may be the same as that of the first guide mechanism.

ピッチ繊維は、一般の有機合成繊維に比して、伸び及び
強度が小さく、脆弱である為、紡糸及び集束時にも、ピ
ッチ繊維は他の機構等と出来るだけ接触しない方が良い
。従って、可能ならば、上記第−及び第二のガイド機構
とボビン巻き又はダンス取り用のトラバースガイド又は
エアサッカーとで構成される紡糸・集束機構が好ましい
Pitch fibers have lower elongation and strength than general organic synthetic fibers and are brittle, so it is better that pitch fibers do not come into contact with other mechanisms as much as possible during spinning and convergence. Therefore, if possible, it is preferable to use a spinning/focusing mechanism that is composed of the above-mentioned first and second guide mechanisms and a traverse guide or air sucker for bobbin winding or dancing.

集束剤を使用する場合には、ノズル面と第一のガイド機
構との間でその少なくとも一部をピンチ繊維に付与する
ことが必要である。ピッチm、*が第一のガイド機構を
通過した後にはじめて集束剤が付与される場合には、集
束剤使用による効果の改善は、はとんど認められない。
If a sizing agent is used, it is necessary to apply at least a portion of it to the pinched fibers between the nozzle face and the first guide mechanism. If the sizing agent is applied only after the pitch m,* has passed through the first guide mechanism, no improvement in the effect of using the sizing agent can be observed.

ノズル面と第一のガイド機構との間で集束剤の一部のみ
を付与する場合には、集束剤の残余は、第一のガイド機
構と第二のガイド機構との間、第二のガイド機構とボビ
ン巻き又はダンス取り用のトラバースガイド又はエアサ
ッカーとの間等の任意の位置で付与することができる。
When only a portion of the sizing agent is applied between the nozzle surface and the first guide mechanism, the remainder of the sizing agent is applied between the first and second guide mechanisms and between the second guide mechanism. It can be applied at any position, such as between the mechanism and the traverse guide or air sucker for bobbin winding or dancing.

集束剤としては、公知のものを使用することができ、例
えば、水、シリコーン油、高級アルコールのエチレンオ
キサイド付加物などやシリコーン油、高級アルコールの
エチレンオキサイド付加物などの水系分散液が挙げられ
る。
As the sizing agent, known ones can be used, such as water, silicone oil, ethylene oxide adducts of higher alcohols, and aqueous dispersions of silicone oils, ethylene oxide adducts of higher alcohols, and the like.

第1図に本発明方法の一実施態様の大要を示す。FIG. 1 shows an outline of one embodiment of the method of the present invention.

多ホールノズルを備えた紡糸装置(1)により得られた
ピッチ繊維(3)は、紡糸筒(5)を通り、第一のガイ
ド機構としての固定カイト(7)と接触した後、第二の
ガイド機構としてのフリーローラー(9)と接触する。
The pitch fiber (3) obtained by the spinning device (1) equipped with a multi-hole nozzle passes through the spinning tube (5) and comes into contact with the fixed kite (7) as a first guide mechanism, and then passes through the second It comes into contact with a free roller (9) as a guide mechanism.

次いで、ピッチ繊維は、フリーローラー(11)により
方向を変えられ、トラバースガイド(13)をへて駆動
されたボビン(15)に巻きとられるか、もしくはボビ
ン(15)の代りにゴデツトローラーを用いてダンス取
りされる。集束剤を使用する場合には、その少なくとも
一部を紡糸装置(1)と固定ガイド(7)との間で、好
ましくは紡糸装置(1)と紡糸筒(5〉内でピンチ繊維
(3)に噴霧する。
The pitch fibers are then redirected by a free roller (11) and wound onto a driven bobbin (15) through a traverse guide (13) or by using a godet roller instead of the bobbin (15). Dance is taken. If a sizing agent is used, at least a portion of it is distributed between the spinning device (1) and the fixed guide (7), preferably between the spinning device (1) and the spinning tube (5) to pinch the fibers (3). Spray on.

発明の効果 本発明によれば、ピッチ繊維を紡糸・集束するに際し、
最終炭素繊維の毛羽立ちの原因となる糸切れ及びローラ
ーへの巻き付きを生ずることなく、集束性良好なピッチ
繊維トウが得られ、品質安定性に優れた炭素繊維を効率
良く製造することができる。
Effects of the Invention According to the present invention, when spinning and converging pitch fibers,
A pitch fiber tow with good cohesiveness can be obtained without causing thread breakage or winding around a roller, which causes fuzzing of the final carbon fiber, and carbon fiber with excellent quality stability can be efficiently produced.

実施例 以下に実施例及び比較例を示し、本発明の特徴とするこ
とろをより一層明らかにする。
EXAMPLES Below, Examples and Comparative Examples will be shown to further clarify the characteristics of the present invention.

実施例1 軟化点110’C,キノリンネ溶分0.18重量%、ベ
ンゼン不溶分35重量%のコールタールピッチ1重量部
と水素化型アントラセン油2重量部との混合溶液をオー
トクレーブ中で430’Cで60分間撹拌下加熱した後
、加圧式フィルターで熱時才濾過し、更に減圧下300
℃で水素化型アントラセン油を除去して、還元ピッチを
得た。
Example 1 A mixed solution of 1 part by weight of coal tar pitch and 2 parts by weight of hydrogenated anthracene oil having a softening point of 110'C, a quinoline-soluble content of 0.18% by weight, and a benzene-insoluble content of 35% by weight was heated to 430' in an autoclave. After heating with stirring for 60 minutes at
The hydrogenated anthracene oil was removed at °C to obtain reduced pitch.

ガス導入管、熱電対、撹拌機及び留出分除去管を備えた
反応器に上記で得られた還元ピッチ50KFIを入れ、
撹拌上窒素ガスを導入しつつ、410〜480℃で4時
間にわたり、低分子量成分の除去及び熱重縮合を行なっ
た。
Put the reduced pitch 50KFI obtained above into a reactor equipped with a gas introduction pipe, a thermocouple, a stirrer and a distillate removal pipe,
Removal of low molecular weight components and thermal polycondensation were carried out at 410 to 480° C. for 4 hours while stirring and introducing nitrogen gas.

得られたピッチの物性は、軟化点315℃(スイス、メ
トラー社製軟化点測定装置による)、キノリンネ溶分3
3重量%、光学的異方性成分98゜5容量%であった 得られた熱処理ピッチを使用して、300個のノズル孔
を有するノズルヘッドから紡糸温度340℃、紡糸速度
350m/分、フィラメント径11μmの条件下に溶融
紡糸を行なった。第一のガイド機構としての固定ガイド
に到達する前に300本のフィラメントに水を噴霧し、
第一の固定カストにより集束し、第二のガイド機構とし
ての回転ローラー型ガイドを通過させた後、引続きガイ
ドローラーを通過させて巻取り、ピッチ繊維のトウを得
た。なお、第−及び第二のガイド機構上においても、水
を噴霧した。紡糸時のガイド部における糸切れは、皆無
であり、安定した連続紡糸が可能であった。
The physical properties of the obtained pitch were as follows: a softening point of 315°C (according to a softening point measuring device manufactured by Mettler, Switzerland), a quinoline solubility of 3
Using the obtained heat-treated pitch having an optically anisotropic component of 98° and 5% by volume, the filament was spun from a nozzle head with 300 nozzle holes at a spinning temperature of 340°C and a spinning speed of 350 m/min. Melt spinning was performed under conditions of a diameter of 11 μm. 300 filaments are sprayed with water before reaching the fixed guide as the first guide mechanism;
After converging by the first fixed cast and passing through a rotating roller type guide as a second guide mechanism, the fibers were subsequently passed through a guide roller and wound up to obtain a tow of pitch fibers. Note that water was also sprayed onto the first and second guide mechanisms. There was no yarn breakage at the guide portion during spinning, and stable continuous spinning was possible.

上記の様にして得られたピッチ繊維を空気中200〜3
20’Cで30分間不融化処理し、更に窒素ガス中12
00’Cで3分間保持して、炭素繊維を得た。炭素繊維
は引張強度275 K9/#2で、毛羽立ちの無い、安
定した品質の連続繊維であった。
The pitch fiber obtained as described above was heated to 200 to 3
Infusibility treatment was carried out at 20'C for 30 minutes, and further in nitrogen gas for 12 minutes.
Carbon fibers were obtained by holding at 00'C for 3 minutes. The carbon fibers had a tensile strength of 275 K9/#2, and were continuous fibers with no fuzz and stable quality.

比較例1〜3 第−及び第二のガイド機構をそれぞれ回転ローラー型−
回転ローラー型(比較例1)、回転ローラー型−固定ガ
イド(比較例2)及び固定ガイド−固定カイト(比較例
3)とする以外は、実施例1と同様にしてピッチ繊維の
トウを得た。いずれの場合にも、フィラメントの糸切れ
及びローラーの巻き付きを生じて、安定した連続紡糸は
困難であった。又、実施例1と同様に不融化及び焼成し
て得た炭素繊維は、毛羽立ちが多く、品質安定性に欠け
ていた。
Comparative Examples 1 to 3 The first and second guide mechanisms were each of rotating roller type.
Pitch fiber tows were obtained in the same manner as in Example 1, except for using a rotating roller type (Comparative Example 1), a rotating roller type-fixed guide (Comparative Example 2), and a fixed guide-fixed kite (Comparative Example 3). . In either case, stable continuous spinning was difficult due to filament breakage and roller wrapping. Further, the carbon fiber obtained by infusibility and firing in the same manner as in Example 1 had a lot of fuzz and lacked quality stability.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は、本発明の実施態様の一例を示すものである。 (1)・・・紡糸装置、 (3)・・・ピッチ繊維、 (5)・・・紡糸筒、 (7)・・・固定ガイド、 (9)・・・フリーローラー、 (ココ)・・・フリーローラー、 (13)・・・トラバースカイト、 (15〉・・・駆動ボビン。 (以 上) 第1 一一\〜 上 ゝ\−一 N5 〜3 ・ 7 ・ 9 .11 FIG. 1 shows an example of an embodiment of the present invention. (1) ... spinning device, (3)...Pitch fiber, (5) ... spinning tube, (7)...Fixed guide, (9)...free roller, (here)...free roller, (13)...traverse skite, (15>... Drive bobbin. (that's all) 1st 11\〜 Up ゝ\-1 N5 ~3 ・ 7 ・ 9 .. 11

Claims (2)

【特許請求の範囲】[Claims] (1)ピツチ系材料を多ホールノズルを用いて紡糸し、
不融化し、炭化及び/又は黒鉛化して炭素繊維を製造す
る方法において、紡糸したピッチ繊維を集束してトウを
形成させるに際し、2個以上のガイド機構を使用し、第
一のガイド機構を回転しない固定型ガイド又はエアサッ
カーにより構成し、第二のガイド機構を回転抵抗の小さ
い回転ローラーにより構成することを特徴とするピッチ
系炭素繊維の製造方法。
(1) Spinning pitch-based material using a multi-hole nozzle,
In a method of producing carbon fiber by infusible carbonization and/or graphitization, two or more guide mechanisms are used and the first guide mechanism is rotated when converging spun pitch fibers to form a tow. 1. A method for producing pitch-based carbon fiber, characterized in that the second guide mechanism is a rotating roller with low rotational resistance.
(2)ノズル面と第一のガイド機構との間でピッチ繊維
に集束剤を噴霧する特許請求の範囲第1項に記載のピッ
チ系炭素繊維の製造方法。
(2) The method for producing pitch-based carbon fibers according to claim 1, wherein a sizing agent is sprayed onto the pitch fibers between the nozzle surface and the first guide mechanism.
JP12082186A 1986-05-26 1986-05-26 Production of pitch carbon yarn Pending JPS62282025A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP12082186A JPS62282025A (en) 1986-05-26 1986-05-26 Production of pitch carbon yarn

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP12082186A JPS62282025A (en) 1986-05-26 1986-05-26 Production of pitch carbon yarn

Publications (1)

Publication Number Publication Date
JPS62282025A true JPS62282025A (en) 1987-12-07

Family

ID=14795795

Family Applications (1)

Application Number Title Priority Date Filing Date
JP12082186A Pending JPS62282025A (en) 1986-05-26 1986-05-26 Production of pitch carbon yarn

Country Status (1)

Country Link
JP (1) JPS62282025A (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5976923A (en) * 1982-10-20 1984-05-02 Kanebo Ltd Manufacture of carbon fiber
JPS60252722A (en) * 1984-05-30 1985-12-13 Idemitsu Kosan Co Ltd Production of carbon fiber

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5976923A (en) * 1982-10-20 1984-05-02 Kanebo Ltd Manufacture of carbon fiber
JPS60252722A (en) * 1984-05-30 1985-12-13 Idemitsu Kosan Co Ltd Production of carbon fiber

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