JPH0133570B2 - - Google Patents

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Publication number
JPH0133570B2
JPH0133570B2 JP59028787A JP2878784A JPH0133570B2 JP H0133570 B2 JPH0133570 B2 JP H0133570B2 JP 59028787 A JP59028787 A JP 59028787A JP 2878784 A JP2878784 A JP 2878784A JP H0133570 B2 JPH0133570 B2 JP H0133570B2
Authority
JP
Japan
Prior art keywords
pitch
fibers
temperature
treatment
infusible
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.)
Expired
Application number
JP59028787A
Other languages
Japanese (ja)
Other versions
JPS60181320A (en
Inventor
Masakatsu Oota
Hiroshi Nishitani
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.)
Idemitsu Kosan Co Ltd
Original Assignee
Idemitsu Kosan 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 Idemitsu Kosan Co Ltd filed Critical Idemitsu Kosan Co Ltd
Priority to JP2878784A priority Critical patent/JPS60181320A/en
Publication of JPS60181320A publication Critical patent/JPS60181320A/en
Publication of JPH0133570B2 publication Critical patent/JPH0133570B2/ja
Granted legal-status Critical Current

Links

Description

【発明の詳細な説明】 本発明は炭素繊維の製造方法に関し、詳しくは
ピツチ繊維の不融化処理の時間を短縮することが
でき、しかも強度的にもすぐれた炭素繊維を製造
する方法に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing carbon fibers, and more particularly to a method for producing carbon fibers that can shorten the time required for infusibility treatment of pitch fibers and have excellent strength.

炭素繊維はプラスチツクや金属の複合材料とし
て知られており、近年は炭化収率の良い炭素質ピ
ツチを原料とし、この炭素質ピツチを紡糸したピ
ツチ繊維を不融化処理したのち、炭化あるいは黒
鉛化することにより、強度の高い炭素繊維を製造
する方法が種々提案されている。
Carbon fiber is known as a composite material of plastic and metal, and in recent years, it has been developed to use carbon pitch as a raw material, which has a good carbonization yield, and to process the pitch fibers spun from this carbon pitch to make them infusible and then carbonize or graphitize them. Accordingly, various methods have been proposed for producing carbon fibers with high strength.

例えば、特開昭51−119835号公報によれば、メ
ソ相ピツチ含有量が40〜90重量%のピツチ繊維を
酸素含有雰囲気中で250〜500℃に加熱し、ピツチ
繊維中の酸素含有量が17〜30重量%となるように
酸化し、次いで不活性ガス雰囲気中において高温
で焼成することにより炭素繊維を得る方法が提案
されている。
For example, according to JP-A-51-119835, pitch fibers having a mesophase pitch content of 40 to 90% by weight are heated to 250 to 500°C in an oxygen-containing atmosphere, and the oxygen content in the pitch fibers is reduced. A method has been proposed in which carbon fibers are obtained by oxidizing the carbon fibers to a concentration of 17 to 30% by weight and then firing at high temperatures in an inert gas atmosphere.

しかしながら、この方法ではピツチ繊維を不融
化処理することによつて、ピツチ繊維の機械的強
度が大きくなるため、不融化ピツチ繊維の取扱い
が容易になるという利点を有するものの、多量の
酸素含有量となるまで酸化するためピツチ繊維の
不融化処理に時間がかかり、しかも多大の熱量を
必要とするほか、焼成時に酸素を含む多量の廃ガ
スを発生するため、その廃ガス処理が必要とな
り、また焼成後の炭素繊維の強度の低下を招くと
いう欠点がある。
However, this method has the advantage that the mechanical strength of the pitch fiber is increased by infusible treatment of the pitch fiber, making it easier to handle. It takes a long time to make the pitch fiber infusible because it oxidizes until it becomes oxidized, and it requires a large amount of heat.In addition, a large amount of waste gas containing oxygen is generated during firing, so it is necessary to treat the waste gas. This has the disadvantage of causing a decrease in the strength of the subsequent carbon fiber.

本発明は上記従来の欠点を解消し、ピツチ繊維
の不融化処理の時間を短縮することができ、しか
も強度的にもすぐれた炭素繊維を製造する方法を
提供することを目的とするものである。
The object of the present invention is to eliminate the above-mentioned conventional drawbacks, to provide a method for producing carbon fibers that can shorten the time for infusibility treatment of pitch fibers and also have excellent strength. .

すなわち本発明は、メソ相ピツチの含有量が実
質的に100%であり、かつ軟化点250〜380℃のピ
ツチを紡糸して得られるピツチ繊維を不融化処理
したのち焼成処理して炭素繊維を製造するにあた
り、ピツチ繊維の不融化処理を、該不融化処理後
のピツチ繊維中の酸素含有量が9〜12重量%とな
るように酸素含有雰囲気中で150〜250℃から毎分
5〜40℃の昇温速度で270〜300℃まで昇温し、次
いで毎分20〜100℃の昇温速度で350〜450℃まで
昇温して加熱処理することにより行ない、しかる
後、不活性ガス雰囲気中において1000℃以上の温
度で焼成処理することを特徴とする炭素繊維の製
造方法を提供するものである。
That is, in the present invention, pitch fibers obtained by spinning pitch fibers having a mesophase pitch content of substantially 100% and a softening point of 250 to 380°C are subjected to an infusible treatment and then fired to produce carbon fibers. During production, the pitch fibers are infusible at 5 to 40 degrees per minute from 150 to 250°C in an oxygen-containing atmosphere so that the oxygen content in the pitch fibers after the infusibility treatment is 9 to 12% by weight. Heat treatment is performed by raising the temperature to 270 to 300 °C at a rate of 100 °C, then to 350 to 450 °C at a rate of 20 to 100 °C per minute, and then heating it in an inert gas atmosphere. The purpose of the present invention is to provide a method for producing carbon fiber, which is characterized by performing a firing treatment at a temperature of 1000°C or higher.

本発明の方法において用いるピツチは石油系重
質油を常圧あるいは減圧下に400〜500℃で熱処理
することにより得られるものである。ここで石油
系重質油としては様々なものが挙げられるが、特
に石油留分の接触分解残油、ナフサ等の熱分解残
油など芳香族炭化水素に富む重質油が好適であ
る。
The pitch used in the method of the present invention is obtained by heat treating petroleum heavy oil at 400 to 500°C under normal pressure or reduced pressure. Here, various types of petroleum-based heavy oils can be mentioned, but heavy oils rich in aromatic hydrocarbons, such as catalytic cracking residues of petroleum fractions and thermal cracking residues such as naphtha, are particularly suitable.

本発明の方法においては、このような重質油を
減圧蒸留して、予め沸点約400℃以下の軽質油分
を留去した残油を原料ピツチとして用いることが
好ましい。なお、この際、重質油はフイルター等
により灰分を除いておくことが好ましい。このよ
うな原料ピツチを上記の如く熱処理する。すなわ
ち、この熱処理は400〜500℃の温度において、窒
素ガスなど不活性ガスの流通下に常圧下で行なう
か、或いは減圧下で行なう。
In the method of the present invention, it is preferable to distill such heavy oil under reduced pressure and use residual oil from which light oil components with a boiling point of about 400° C. or less have been distilled off as the raw material pitch. At this time, it is preferable to remove ash from the heavy oil using a filter or the like. Such a raw material pitch is heat treated as described above. That is, this heat treatment is carried out at a temperature of 400 to 500° C. under normal pressure or under reduced pressure while flowing an inert gas such as nitrogen gas.

本発明の方法においては、このようにして生成
したメソ相含有ピツチより炭素繊維を製造する。
In the method of the present invention, carbon fibers are produced from the mesophase-containing pitch thus produced.

なお、ここでメソ相含有ピツチとしてはメソ相
ピツチの含有量が実質的に100%のものであつて、
かつ軟化点250〜380℃のものが用いられ、さらに
分子量分布の狭いものが好ましい。
In addition, here, the mesophase-containing pitch is one in which the content of mesophase pitch is substantially 100%,
A material having a softening point of 250 to 380° C. is used, and a material having a narrow molecular weight distribution is preferable.

このようなメソ相ピツチの含有量が大きく、か
つ軟化点の高いピツチを用いることにより不融化
を短時間で行なうことができる。しかもピツチ繊
維の機械的強度を低下させることなく、最終製品
として強度の大きい炭素繊維を製造することがで
きる。
By using such a pitch having a large content of mesophase pitch and a high softening point, infusibility can be achieved in a short time. Furthermore, carbon fibers with high strength can be produced as final products without reducing the mechanical strength of pitch fibers.

本発明の方法においては、まず上記のようにし
て得られるメソ相含有ピツチを紡糸してピツチ繊
維を得る。ここでピツチ繊維としては、メソ相含
有ピツチを5〜15μ径の繊維に紡糸したものが適
している。なお、通常紡糸温度は260〜410℃、好
ましくは270〜400℃であり、また紡糸速度は50〜
2000m/分、好ましくは100〜1000m/分である。
In the method of the present invention, first, the mesophase-containing pitch obtained as described above is spun to obtain pitch fiber. Suitable pitch fibers are those obtained by spinning mesophase-containing pitch into fibers having a diameter of 5 to 15 μm. Note that the spinning temperature is usually 260 to 410°C, preferably 270 to 400°C, and the spinning speed is 50 to 410°C.
2000 m/min, preferably 100-1000 m/min.

次に、上記の如く得られたピツチ繊維を不融化
処理する。本発明はこの不融化処理工程に最大の
特色を有するものである。すなわち、ピツチ繊維
の不融化処理を、該不融化処理後のピツチ繊維中
の酸素含有量が9乃至12重量%となるように酸素
含有雰囲気中で加熱処理することにより行なう。
ここで、この不融化処理後のピツチ繊維中の酸素
含有量が9重量%以下未満であると、不融化が不
十分となり、続いて行なわれる炭化、黒鉛化工程
(焼成処理工程)においてピツチ繊維が溶融し、
ピツチ繊維の移動や加工など扱いに支障をきたす
ので好ましくない。一方、12重量%を超えると、
不融化のための加熱処理時間が長くなつて不経済
であり、かつ最終製品である炭素繊維の機械的強
度の低下を招くので好ましくない。このような不
融化処理は様々な方法により行なうことができる
が、通常酸素含有雰囲気、好ましくは空気中にお
いて、150〜250℃から350〜450℃までの間の昇温
速度を毎分5〜100℃で昇温する方法が好ましい。
より好ましくは150〜250℃から毎分5〜40℃の昇
温速度で270〜300℃まで昇温し、次いで毎分20〜
100℃の昇温速度で350〜450℃まで昇温して行な
う。
Next, the pitch fibers obtained as described above are treated to be infusible. The greatest feature of the present invention is this infusibility treatment step. That is, the pitch fibers are made infusible by heat treatment in an oxygen-containing atmosphere so that the oxygen content in the pitch fibers after the infusibility treatment becomes 9 to 12% by weight.
Here, if the oxygen content in the pitch fiber after this infusibility treatment is less than 9% by weight, the infusibility will be insufficient, and the pitch fiber will be melts,
This is undesirable because it interferes with the movement and processing of pitch fibers. On the other hand, if it exceeds 12% by weight,
This is not preferable because the heat treatment time for infusibility becomes long, which is uneconomical, and also causes a decrease in the mechanical strength of the final product, the carbon fiber. Such infusibility treatment can be carried out by various methods, but it is usually carried out in an oxygen-containing atmosphere, preferably in air, at a heating rate of 5 to 100 degrees per minute from 150 to 250°C to 350 to 450°C. A method of raising the temperature at °C is preferred.
More preferably, the temperature is raised from 150 to 250°C to 270 to 300°C at a rate of 5 to 40°C per minute, and then at a rate of 20 to 300°C per minute.
The temperature is raised to 350-450°C at a heating rate of 100°C.

すなわち、270〜300℃以下では昇温速度を毎分
40℃を超えたものとする融着のおそれがあり、
270〜300℃を超えると表面付近は既に不融化され
ているので、昇温速度を上げ、酸素の拡散速度を
増大させることにより、不融化が促進され、不融
化時間を一層短縮することができるからである。
In other words, below 270-300℃, the heating rate should be reduced per minute.
If the temperature exceeds 40℃, there is a risk of fusion.
When the temperature exceeds 270 to 300°C, the area near the surface is already infusible, so by increasing the heating rate and oxygen diffusion rate, infusibility is promoted and the infusibility time can be further shortened. It is from.

さらに本発明の方法においては、このようにし
て不融化処理したのち焼成処理する。この焼成処
理は窒素ガス、アルゴンガスなど不活性ガス雰囲
気中において1000℃以上の温度に加熱することに
より行なう。なお、ここで焼成処理の温度は通
常、炭化処理の場合、1000〜2500℃であり、黒鉛
化処理の場合、2500〜3000℃である。
Further, in the method of the present invention, after the infusibility treatment is performed in this manner, the calcination treatment is performed. This firing treatment is performed by heating to a temperature of 1000° C. or higher in an inert gas atmosphere such as nitrogen gas or argon gas. Note that the temperature of the firing treatment here is usually 1000 to 2500°C in the case of carbonization treatment, and 2500 to 3000°C in the case of graphitization treatment.

叙上の如くして炭素繊維を製造することができ
る。
Carbon fibers can be produced as described above.

本発明の方法によれば、従来の方法に比しピツ
チ繊維の不融化処理の時間を短縮することがで
き、省エネルギーとなる。しかも本発明の方法に
より得られる炭素繊維は引張強度、弾性率など機
械的強度にもすぐれている。
According to the method of the present invention, compared to conventional methods, the time required for infusibility treatment of pitch fibers can be shortened and energy can be saved. Moreover, the carbon fiber obtained by the method of the present invention has excellent mechanical strength such as tensile strength and elastic modulus.

したがつて、本発明の方法は炭素繊維の製造、
とりわけ高強度の要求される製品の製造に有効に
用いることができる。
Therefore, the method of the present invention can be used for producing carbon fibers,
In particular, it can be effectively used for manufacturing products that require high strength.

次に本発明を実施例により詳細に説明する。 Next, the present invention will be explained in detail with reference to examples.

実施例 1 重質軽油の接触分解装置から得られた接触分解
残油をフイルターにより灰分を除去したのち、減
圧蒸留して得た沸点430℃(常圧換算)以上の残
油を、温度420℃、圧力10mmHgにおいて2時間熱
処理することによりピツチを得た。ここで得られ
たピツチを溶融状態で静置分離することにより、
比重の大なるメソ相ピツチのみを抜き取つた。こ
の実質的にメソ相の含量が100%であり、軟化点
290℃のピツチを、340℃において紡糸速度1000
m/分にて糸径10μのピツチ繊維に紡糸した。
Example 1 After removing the ash content from the catalytic cracking residual oil obtained from the catalytic cracking equipment for heavy gas oil using a filter, the residual oil with a boiling point of 430°C or higher (converted to normal pressure) obtained by distilling it under reduced pressure was heated to a temperature of 420°C. Pitch was obtained by heat treatment for 2 hours at a pressure of 10 mmHg. By statically separating the pitch obtained here in a molten state,
Only the mesophase pitch with high specific gravity was extracted. This practically has a mesophase content of 100% and a softening point of
Pitch at 290℃, spinning speed 1000 at 340℃
It was spun into pitch fibers with a diameter of 10 μm at a speed of m/min.

ここで得られたピツチ繊維を、まず200℃の空
気恒温槽に入れると同時に、昇温速度10℃/分で
280℃まで、次いで昇温速度40℃/分で360℃まで
昇温し、さらに360℃で30秒間保持することによ
り不融化処理した。不融化の所定時間は10分間で
あつた。不融化処理したピツチ繊維について、そ
の酸素含有量を測定したところ10.2重量%であつ
た。次に、この不融化処理したピツチ繊維をアル
ゴン雰囲気下、1500℃において10分間焼成処理し
て炭素繊維を得た。
The Pituchi fibers obtained here were first placed in an air constant temperature bath at 200°C, and at the same time the temperature was increased at a rate of 10°C/min.
The temperature was increased to 280°C, then to 360°C at a heating rate of 40°C/min, and further held at 360°C for 30 seconds to perform infusibility treatment. The predetermined time for infusibility was 10 minutes. The oxygen content of the infusible pitch fiber was measured and found to be 10.2% by weight. Next, the infusible pitch fibers were fired at 1500° C. for 10 minutes in an argon atmosphere to obtain carbon fibers.

得られた炭素繊維の引張強度は214Kg/mm2、弾
性率は24.3t/mm2であつた。
The obtained carbon fiber had a tensile strength of 214 Kg/mm 2 and an elastic modulus of 24.3 t/mm 2 .

実施例 2 実施例1において、実施例1で得られたピツチ
繊維の不融化処理を、まず200℃の空気恒温槽に
入れると同時に、昇温速度10℃/分で280℃まで、
次いで昇温速度40℃/分で360℃まで昇温し、さ
らに360℃で5分間保持することにより行なつた。
不融化の所要時間は15分間であつた。不融化処理
したピツチ繊維の酸素含有量は11.4重量%であつ
た。次に、この不融化処理したピツチ繊維を実施
例1と同様に焼成処理して炭素繊維を得た。
Example 2 In Example 1, the pitch fiber obtained in Example 1 was first put into an air constant temperature bath at 200°C, and at the same time, the temperature was raised to 280°C at a temperature increase rate of 10°C/min.
Next, the temperature was raised to 360°C at a heating rate of 40°C/min, and the temperature was further maintained at 360°C for 5 minutes.
The time required for infusibility was 15 minutes. The oxygen content of the infusible pitch fiber was 11.4% by weight. Next, the infusible pitch fibers were fired in the same manner as in Example 1 to obtain carbon fibers.

得られた炭素繊維の引張強度は166Kg/mm2、弾
性率は23.8t/mm2であつた。
The obtained carbon fiber had a tensile strength of 166 Kg/mm 2 and an elastic modulus of 23.8 t/mm 2 .

比較例 1 実施例1において、実施例1で得られたピツチ
繊維の不融化処理を、まず200℃の空気恒温槽に
入れると同時に昇温速度10℃/分で280℃まで昇
温し、次いで昇温速度40℃/分で360℃まで昇温
し、さらに360℃で10分間保持することにより行
なつた。不融化の所要時間は20分間であつた。不
融化処理したピツチ繊維の酸素含有量は13.3重量
%であつた。次に、この不融化処理したピツチ繊
維を実施例1と同様に焼成処理して炭素繊維を得
た。
Comparative Example 1 In Example 1, the pitch fiber obtained in Example 1 was first placed in an air constant temperature bath at 200°C, and at the same time the temperature was raised to 280°C at a rate of 10°C/min. The temperature was raised to 360°C at a heating rate of 40°C/min, and the temperature was further maintained at 360°C for 10 minutes. The time required for infusibility was 20 minutes. The oxygen content of the infusible pitch fiber was 13.3% by weight. Next, the infusible pitch fibers were fired in the same manner as in Example 1 to obtain carbon fibers.

得られた炭素繊維の引張強度は116Kg/mm2に低
下し、また弾性率も19.1t/mm2に低下した。
The tensile strength of the obtained carbon fiber decreased to 116 Kg/mm 2 and the elastic modulus also decreased to 19.1 t/mm 2 .

比較例 2 実施例1において、実施例1で得られたピツチ
繊維の不融化処理を、室温から昇温速度10℃/分
で300まで昇温し、さらに300℃において1時間保
持することにより行なつた。不融化の所要時間は
1時間30分であつた。不融化処理したピツチ繊維
の酸素含有量は15.0重量%であつた。次に、この
不融化処理したピツチ繊維を実施例1と同様に焼
成処理して炭素繊維を得た。
Comparative Example 2 In Example 1, the pitch fiber obtained in Example 1 was infusible by increasing the temperature from room temperature to 300°C at a heating rate of 10°C/min, and then holding it at 300°C for 1 hour. Summer. The time required for infusibility was 1 hour and 30 minutes. The oxygen content of the infusible pitch fiber was 15.0% by weight. Next, the infusible pitch fibers were fired in the same manner as in Example 1 to obtain carbon fibers.

得られた炭素繊維の引張強度は136Kg/mm2であ
り、弾性率は19.6t/mm2であつた。
The obtained carbon fiber had a tensile strength of 136 Kg/mm 2 and an elastic modulus of 19.6 t/mm 2 .

Claims (1)

【特許請求の範囲】 1 メソ相ピツチの含有量が実質的に100%であ
り、かつ軟化点250〜380℃のピツチを紡糸して得
られるピツチ繊維を不融化処理したのち焼成処理
して炭素繊維を製造するにあたり、ピツチ繊維の
不融化処理を、該不融化処理後のピツチ繊維中の
酸素含有量が9〜12重量%となるように酸素含有
雰囲気中で150〜250℃から毎分5〜40℃の昇温速
度で270〜300℃まで昇温し、次いで毎分20〜100
℃の昇温速度で350〜450℃まで昇温して加熱処理
することにより行ない、しかる後、不活性ガス雰
囲気中において1000℃以上の温度で焼成処理する
ことを特徴とする炭素繊維の製造方法。 2 酸素含有雰囲気が、空気である特許請求の範
囲第1項記載の方法。
[Scope of Claims] 1 Pitch fibers obtained by spinning pitches with a mesophase pitch content of substantially 100% and a softening point of 250 to 380°C are subjected to an infusible treatment and then fired to form carbon fibers. In producing the fibers, the pitch fibers are infusible at 5% per minute from 150 to 250°C in an oxygen-containing atmosphere so that the oxygen content in the pitch fibers after the infusibility treatment is 9 to 12% by weight. Raise the temperature to 270-300℃ at a heating rate of ~40℃, then 20-100℃ per minute
A method for producing carbon fiber, which is carried out by heat treatment at a heating rate of 350 to 450 °C, followed by firing treatment at a temperature of 1000 °C or higher in an inert gas atmosphere. . 2. The method according to claim 1, wherein the oxygen-containing atmosphere is air.
JP2878784A 1984-02-20 1984-02-20 Manufacture of carbon fiber Granted JPS60181320A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2878784A JPS60181320A (en) 1984-02-20 1984-02-20 Manufacture of carbon fiber

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2878784A JPS60181320A (en) 1984-02-20 1984-02-20 Manufacture of carbon fiber

Publications (2)

Publication Number Publication Date
JPS60181320A JPS60181320A (en) 1985-09-17
JPH0133570B2 true JPH0133570B2 (en) 1989-07-13

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
JP2878784A Granted JPS60181320A (en) 1984-02-20 1984-02-20 Manufacture of carbon fiber

Country Status (1)

Country Link
JP (1) JPS60181320A (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2533487B2 (en) * 1986-04-18 1996-09-11 三菱化学株式会社 Carbon fiber manufacturing method
JP2678384B2 (en) * 1989-06-09 1997-11-17 出光興産株式会社 Pitch for carbon fiber and method of manufacturing carbon fiber using the same

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4919127A (en) * 1972-03-30 1974-02-20
JPS5455625A (en) * 1977-10-03 1979-05-02 Union Carbide Corp Low molecular weight meso phase pitch
JPS56101916A (en) * 1979-12-26 1981-08-14 Union Carbide Corp Production of carbon fiber
JPS58156021A (en) * 1982-02-04 1983-09-16 Kashima Sekiyu Kk Production of carbon fiber by two-step infusibilization of melt-spun pitch fiber
JPS6088125A (en) * 1983-10-14 1985-05-17 Nippon Oil Co Ltd Production of pitch based graphitized fiber
JPS60155714A (en) * 1984-01-24 1985-08-15 Teijin Ltd Production of pitch based carbon fiber

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4919127A (en) * 1972-03-30 1974-02-20
JPS5455625A (en) * 1977-10-03 1979-05-02 Union Carbide Corp Low molecular weight meso phase pitch
JPS56101916A (en) * 1979-12-26 1981-08-14 Union Carbide Corp Production of carbon fiber
JPS58156021A (en) * 1982-02-04 1983-09-16 Kashima Sekiyu Kk Production of carbon fiber by two-step infusibilization of melt-spun pitch fiber
JPS6088125A (en) * 1983-10-14 1985-05-17 Nippon Oil Co Ltd Production of pitch based graphitized fiber
JPS60155714A (en) * 1984-01-24 1985-08-15 Teijin Ltd Production of pitch based carbon fiber

Also Published As

Publication number Publication date
JPS60181320A (en) 1985-09-17

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