JPS61291684A - Production of spinning pitch for carbon fiber - Google Patents

Production of spinning pitch for carbon fiber

Info

Publication number
JPS61291684A
JPS61291684A JP13355185A JP13355185A JPS61291684A JP S61291684 A JPS61291684 A JP S61291684A JP 13355185 A JP13355185 A JP 13355185A JP 13355185 A JP13355185 A JP 13355185A JP S61291684 A JPS61291684 A JP S61291684A
Authority
JP
Japan
Prior art keywords
inert gas
pitch
raw material
reactor
carbonaceous raw
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
Application number
JP13355185A
Other languages
Japanese (ja)
Other versions
JPH0635586B2 (en
Inventor
Kenzou Ban
伴 釼三
Toshio Irie
敏夫 入江
Hideo Takakura
高倉 秀男
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.)
Mitsubishi Kasei Corp
Original Assignee
Mitsubishi Kasei Corp
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 Mitsubishi Kasei Corp filed Critical Mitsubishi Kasei Corp
Priority to JP13355185A priority Critical patent/JPH0635586B2/en
Publication of JPS61291684A publication Critical patent/JPS61291684A/en
Publication of JPH0635586B2 publication Critical patent/JPH0635586B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Working-Up Tar And Pitch (AREA)
  • Inorganic Fibers (AREA)

Abstract

PURPOSE:To obtain the titled pitch capable of giving pitch based carbon fibers having a high strength and high elastic modulus, by heat-treating a carbonaceous raw material while blowing an inert gas from a feed pipe having a specific caliber at a specific gas linear velocity thereinto and removing volatile low molecular materials. CONSTITUTION:A carbonaceout raw material is filled ina reactor 1 equipped with an agitator 3, and heat-treated while feeding a pregeated inert gas, e.g. nitrogen, from an inert gas feed pipe 2 having <=15mm caliber at >=30m/sec gas linear velocity thereto to afford the aimed spinning pitch. Preferably, the opening part of the inert gas feed pipe 2 is installed at <=150mm distance from the bottom of the reactor 1 containing the carbonaceous raw material and the inert gas is made to collide with the bottom of the reactor 1 and then blown thereinto.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は炭素繊維用紡糸ピッチの製造方法に関するもの
で、より詳しくは、高強度及び高弾性率を有するピッチ
系炭素繊維を与える紡糸ピッチの製造方法に関するもの
である。
Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a method for producing a spinning pitch for carbon fibers, and more specifically, a method for producing a spinning pitch for producing pitch-based carbon fibers having high strength and high modulus. This relates to a manufacturing method.

(従来の技術) 周知のように、重質油、タール、ピッチ等の炭素質原料
を330〜200℃に加熱すると、それら物質中に粒径
が数ミクロンから数百ミクロンの偏光下光学的異方性を
示す小球体が生成する。そして、更に加熱するとこれら
の小球体は成長合体し、ついには全体が光学的異方性を
示す状態となる。この異方性組織は炭素質原料の熱重縮
合反応により生成した高分子芳香族炭化水素が層状に積
み重なり配向したもので、黒鉛結晶構造の前駆体とみな
されている。
(Prior Art) As is well known, when carbonaceous raw materials such as heavy oil, tar, and pitch are heated to 330 to 200°C, optical differences with particle sizes ranging from several microns to several hundred microns occur in these materials under polarized light. Small spheres exhibiting directionality are generated. Then, when heated further, these small spheres grow and coalesce, and finally the whole becomes in a state exhibiting optical anisotropy. This anisotropic structure is composed of polymeric aromatic hydrocarbons produced by a thermal polycondensation reaction of carbonaceous raw materials, stacked and oriented in layers, and is considered to be a precursor of graphite crystal structure.

この様な熱処理物は、紡糸口金を通し、溶融紡糸、不融
化、炭化、更に場合により黒鉛化することによって、高
強度、高弾性率などの特徴をもつピッチ系の高特性炭素
繊維の原料として提案されている。
This heat-treated product is passed through a spinneret, melt-spun, made infusible, carbonized, and optionally graphitized, and then used as a raw material for pitch-based high-performance carbon fibers, which have characteristics such as high strength and high modulus. Proposed.

炭素繊維は、比強度、比弾性率が高い材料で、高性能複
合材料のフィラー繊維として最も注目されており、中で
もピッチ系高特性炭素繊維は、炭化工程での歩留が大き
い、繊維の弾性率が高い等、ポリアクリロニトリル系炭
素繊維に比べて様々な利点を持っている。
Carbon fiber is a material with high specific strength and specific modulus, and is attracting the most attention as a filler fiber for high-performance composite materials. Among them, pitch-based high-performance carbon fiber has a high yield in the carbonization process and has a high elasticity of the fiber. It has various advantages over polyacrylonitrile-based carbon fibers, such as a high carbon fiber ratio.

従来、ピッチ系高特性炭素繊維は、通常、所謂メソフェ
ーズを含有したピッチを紡糸原料とし、このメソフェー
ズ含有ピンチから繊維状ピッチを紡糸し、次いで、不融
化し、焼成(炭化、黒鉛化)して製造されている。
Conventionally, pitch-based high-performance carbon fibers have been produced by using so-called mesophase-containing pitch as a spinning raw material, spinning fibrous pitch from this mesophase-containing pinch, then making it infusible and firing it (carbonization, graphitization). Manufactured.

特にメンフェーズを多量に含有する紡糸ピッチを製造す
る際には特開昭57一ダ292ダ号公報、特開昭!;g
−/AtAg7号公報等に開示されているように炭素質
原料を攪拌しながらあるいは更に気体等を吹き込みなが
ら加熱処理して紡糸ピッチを製造することは広く知られ
た技術である。
In particular, when producing spinning pitch containing a large amount of menphase, JP-A-57-1-DA 292-DA, JP-A-Sho! ;g
It is a widely known technique to produce spinning pitch by heat-treating a carbonaceous raw material while stirring or while blowing gas or the like, as disclosed in Publication No. 7 of -/AtAg.

(発明が解決しようとする問題点) しかしながら、従来の方法では、単に攪拌のみであるか
、あるいは攪拌下気体を吹き込む際においても単に気体
の総量を規定しているにすぎず、かかる方法では炭素質
原料を加熱処理して発生する揮発性低分子物を十分に除
去することは困難で、紡糸性に優れ、かつ高特性のピッ
チ系炭素繊維を与えるような紡糸ピッチを安定的に、か
つ均一に製造するのには問題があった。
(Problems to be Solved by the Invention) However, in the conventional methods, only stirring is performed, or even when blowing gas under stirring, the total amount of gas is simply specified, and in such methods, carbon It is difficult to sufficiently remove volatile low-molecular substances generated by heat-treating raw materials, and it is necessary to stably and uniformly create a spinning pitch that yields pitch-based carbon fibers with excellent spinnability and high properties. There were problems in manufacturing it.

(問題点を確決するための手段) そこで、本発明者等は上記問題点を解決するために鋭意
検討した結果、炭素質原料を加熱処理して紡糸ピッチを
製造する際に発生する揮発性低分子物を十分除去するた
めには、十分な気液接触を計ることが重要であると認識
して、特定手段により不活性気体を炭素質原料に微細気
泡として吹き込むことにより、効率的に、かつ十分に揮
発性低分子を除去することができることを見い出し本発
明を完成した。
(Means for Determining the Problem) Therefore, as a result of intensive studies in order to solve the above problem, the present inventors found that Recognizing that sufficient gas-liquid contact is important in order to sufficiently remove molecular substances, we efficiently and The present invention was completed by discovering that volatile low molecules can be sufficiently removed.

すなわち、本発明の目的は特定口径の不活性気体供給管
により特定速度で不活性気体を炭素質原料に炊き込むこ
とにより、高特性のピッチ系炭素繊維を与えるような紡
糸ピッチを安定的かつ均一に製造する方法を提供するも
のである。
That is, the purpose of the present invention is to stably and uniformly create a spinning pitch that provides pitch-based carbon fibers with high properties by injecting an inert gas into a carbonaceous raw material at a specific speed using an inert gas supply pipe with a specific diameter. The present invention provides a method for manufacturing.

そして、かかる目的は炭素質原料に不活性気体を吹き込
みながら加熱処理することにより炭素fII維用紡糸ピ
ッチを製造する際に、不活性気体を口径15馴以下の不
活性気体供給管よりガス線速度、70 m/sec以上
の供給速度で炭素質原料に吹き込むことにより達成され
る。
This purpose is to produce carbon fII textile spinning pitch by heat-treating the carbonaceous raw material while blowing an inert gas into the carbonaceous raw material. This is achieved by blowing into the carbonaceous feedstock at a feed rate of 70 m/sec or more.

以下、本発明の詳細な説明する。The present invention will be explained in detail below.

本発明で紡糸ピッチを得るために炭素質原料としては、
例えば石炭系のコールタール、コールタールピンチ、石
炭液化物、石油系の重質油、タール、ピンチ等で、ベン
ゼン不溶分60重量%以下、好ましくは、50重量%以
下、更に好ましくは、5〜75重量%、キノリンネ溶分
:10重t%以下、好ましくは73重量%以下、更に好
ましくは、5重量%以下のものが挙げられる。
The carbonaceous raw materials for obtaining the spinning pitch in the present invention include:
For example, coal-based coal tar, coal-tar pinch, coal liquefaction, petroleum-based heavy oil, tar, pinch, etc., and the benzene-insoluble content is 60% by weight or less, preferably 50% by weight or less, more preferably 5 to 5% by weight. 75% by weight, quinoline solubility: 10% by weight or less, preferably 73% by weight or less, more preferably 5% by weight or less.

この炭素質原料のベンゼン不溶分、キノリンネ溶分が上
記範囲を超えると得られる紡糸ピッチの溶融粘度が高く
なり、従って、高温にて紡糸しなければならなくなる。
If the benzene-insoluble and quinoline-soluble components of this carbonaceous raw material exceed the above ranges, the resulting spinning pitch will have a high melt viscosity, and therefore, it will be necessary to spin at a high temperature.

その為、紡糸中に紡糸ピッチの熱変質を生じゃすくなり
、好ましくない。
Therefore, thermal alteration of the spinning pitch is likely to occur during spinning, which is undesirable.

予備処理としては、前記炭素質原料を35θ〜SOO℃
、常圧〜lO9/crI−Gでθ、5〜u O時間程度
加熱処理して光学的異方性部分を少なくとも30%以上
、好ましくは、50%以上、特に好ましくは、70%以
上含むような熱処理物を得、次いで、この熱処理物/重
量部に対して約0.7〜3重量部の沸点又は初留点が7
30℃以上の芳香族油と接触させ、その可溶分を得るも
のである。芳香族油としては、ナフタリン油、吸収油、
クレオソート油又はアントラセン油が好ましい。
As a preliminary treatment, the carbonaceous raw material is heated to 35θ~SOO℃.
, normal pressure to lO9/crI-G for about θ, 5 to uO hours so that the optically anisotropic portion is at least 30% or more, preferably 50% or more, particularly preferably 70% or more. A heat-treated product is obtained, and then about 0.7 to 3 parts by weight of the heat-treated product/part by weight has a boiling point or an initial boiling point of 7.
It is brought into contact with an aromatic oil at a temperature of 30°C or higher to obtain its soluble content. Aromatic oils include naphthalene oil, absorption oil,
Creosote oil or anthracene oil is preferred.

この予備処理の意味については、完全に明らかではない
が、以後の処理でば再び適当物質に復原し得ない比較的
高分子量部分を予じめ削除することにあると本発明者等
によって推測される。なお、かかる意味を充足する手段
として炭素質原料あるいは、上記芳香族油可溶分をテト
ラリン、デカリン、テトラヒドロキノリン、水添した芳
香族油の水素供与性溶剤と共に、あるいは、水素供与性
溶剤に容易に転換しうるキノリン、ナフタリン油、アン
トラセン油等の溶剤と触媒として鉄系化合物、MOを含
む担持又は非担持触媒を触媒に添加して、水素ガス加圧
下、yt、o−zoo℃にて水添処理後必要に応じ濾過
等で固形分を除去し、更に必要に応じて蒸留等によって
、溶媒を除いて残渣物を得る方法も考えられる。
The meaning of this pretreatment is not completely clear, but the inventors speculate that it is to remove in advance a relatively high molecular weight portion that cannot be restored to a suitable substance in subsequent treatments. Ru. In addition, as a means to satisfy this meaning, carbonaceous raw materials or the above-mentioned aromatic oil soluble components may be used together with a hydrogen-donating solvent such as tetralin, decalin, tetrahydroquinoline, or hydrogenated aromatic oil, or easily into a hydrogen-donating solvent. A solvent such as quinoline, naphthalene oil, anthracene oil, etc., which can be converted into It is also conceivable that after the addition treatment, the solid content is removed by filtration or the like if necessary, and then the solvent is removed by distillation or the like if necessary to obtain a residue.

本発明において、前記の予備処理を行なった炭素質原料
を300〜SOO℃、好ましくは3gθ〜lI!rθ℃
、減圧〜/ OKl/ cj ” G %好ましくは1
0wtmHg〜常圧でコO分〜10時間、好ましくは7
〜6時間程度加熱処理することにより紡糸ピッチを得る
が、その際、不活性気体を口径15mm以下の不活性気
体供給管よりガス線速度30 m/sec以上の供給速
度で前記炭素質原料に吹き込みながら、上記の様な条件
で加熱処理を行なうことが重要である。好ましくは口径
7〜11m以下、更に好ましくは/ = g m以下の
供給管を用い、ガス線速度JOm/秒以上、好ましくは
SO〜!! 00 m1秒で不活性気体を吹き込むのが
よい。かかる方法により不活性気体を炭素質原料中に、
例えば/ = !r m程度の微細気泡として分散させ
ることができる。
In the present invention, the carbonaceous raw material subjected to the above pretreatment is heated to a temperature of 300°C to SOO°C, preferably 3gθ to lI! rθ℃
, reduced pressure ~/OKl/cj ”G % preferably 1
0wtmHg to normal pressure for 10 minutes, preferably 7 hours
A spinning pitch is obtained by heat treatment for about ~6 hours, at which time an inert gas is blown into the carbonaceous raw material at a gas linear velocity of 30 m/sec or more through an inert gas supply pipe with a diameter of 15 mm or less. However, it is important to perform the heat treatment under the conditions described above. Preferably, a supply pipe with a diameter of 7 to 11 m or less, more preferably / = g m or less is used, and the gas linear velocity is JOm/sec or more, preferably SO~! ! It is best to blow inert gas at 00 ml/sec. By this method, an inert gas is introduced into the carbonaceous raw material,
For example / =! It can be dispersed as fine bubbles of about rm.

供給管の口径が上記範囲より小さいものであると、炭素
質原料中に含有された微小の固体物質等により供給管口
が閉塞する問題があり、また、大きすぎると適切なガス
線速度が得られ難いので好ましくない。
If the diameter of the supply pipe is smaller than the above range, there is a problem that the supply pipe port will be blocked by minute solid substances contained in the carbonaceous raw material, and if it is too large, it may be difficult to obtain an appropriate gas linear velocity. This is not desirable because it is difficult to get caught.

なお、攪拌は炭素質原料の加熱処理装置の壁面付近での
局部加熱によるコーキング防止には効果があるものの、
発生する揮発性低分子物を除去するには十分ではなく、
たとえ、不活性気体を吹き込んでも不活性気体の気泡を
小さくする効果は小さい。
Although stirring is effective in preventing coking caused by local heating near the wall of the heat treatment equipment for carbonaceous raw materials,
It is not sufficient to remove volatile low molecular weight substances that are generated.
Even if an inert gas is blown into the air, the effect of the inert gas in reducing the size of the bubbles is small.

したがって、十分に気液接触を行なって揮発性低分子物
を不活性気体に同伴させて除去するには本発明の吹き込
み条件が重要である。
Therefore, the blowing conditions of the present invention are important in order to effect sufficient gas-liquid contact and remove the volatile low-molecular substances along with the inert gas.

また、不活性気体の気泡を十分小さくするには、不活性
気体供給管の設置位置も重要であって、該供給管の開口
部を炭素質原料を収容する反応器底面から通常200−
2!rOm、好ましくは/!rOwr以内とするのがよ
く、更に該開口部は不活性気体が反応器底面に衝突する
ように該底面に対向させて設置するのが好ま゛しい。
Furthermore, in order to make the inert gas bubbles sufficiently small, the installation position of the inert gas supply pipe is also important.
2! rOm, preferably /! The opening is preferably within rOwr, and the opening is preferably placed opposite the bottom of the reactor so that the inert gas collides with the bottom of the reactor.

更に、揮発性低分子物の除去をより効果的に行なうため
には、不活性気体供給管を複数個、例えば−〜、200
個に分割して設けるのが好ましい。
Furthermore, in order to more effectively remove volatile low-molecular substances, a plurality of inert gas supply pipes, for example, 200
It is preferable to provide it separately.

また、本発明においても、不活性気体を吹き込むと同時
に攪拌を行ないながら、炭素質原料を加熱処理を行なっ
てもよい。
Also in the present invention, the carbonaceous raw material may be heat-treated while stirring and simultaneously blowing inert gas.

次に不活性気体としては、加熱処理の際に炭素質原料を
酸化して重質化させる様な気体でないのであれば、特に
限定されるものではなく、具体的には窒素、アルゴン、
二酸化炭素、ヘリウム、水蒸気、水素あるいは炭素数が
6個以下の炭化水素等が挙げられ、特に好ましくは窒素
、アルゴン、水素等を用いるのが好ましい。
Next, the inert gas is not particularly limited as long as it does not oxidize and make the carbonaceous raw material heavy during heat treatment, and specific examples include nitrogen, argon,
Examples include carbon dioxide, helium, water vapor, hydrogen, and hydrocarbons having 6 or less carbon atoms, and it is particularly preferable to use nitrogen, argon, hydrogen, and the like.

また、これらの不活性気体は単独で用いてもよく、必要
があれば一種以上の不活性気体を混合して用いてもよい
Moreover, these inert gases may be used alone, or if necessary, one or more types of inert gases may be used in combination.

本発明においては、光学的異方性相を170%以上、好
ましくは、70〜100チ、特に好ましくは、90−1
00%含み、しかも、キノリンネ溶分がaO重量%以下
、好ましくは、30重量%以下、特に好ましくは、−5
重量%以下の紡糸ピッチを得るように上記加熱処理条件
を選ぶ必要がある。
In the present invention, the optically anisotropic phase is 170% or more, preferably 70-100%, particularly preferably 90-1
00%, and the quinoline soluble content is less than or equal to aO weight %, preferably less than 30 weight %, particularly preferably -5
It is necessary to select the above heat treatment conditions so as to obtain a spinning pitch of less than % by weight.

尚、本発明でいう紡糸ピッチの光学的異方性相の含量は
、常温上偏光顕微鏡での熱処理物試料中の光学的異方性
を示す部分の面積割合として求めた値である。
Incidentally, the content of the optically anisotropic phase in the spinning pitch as used in the present invention is a value determined as the area ratio of a portion exhibiting optical anisotropy in a heat-treated sample under a polarizing microscope at room temperature.

具体的には、例えば、熱処理物試料を数■角に粉砕した
ものを常法に従って約2CM直径の樹脂の表面のほぼ全
面に試料片を埋込み、表面を研磨後、表面全体をくまな
く偏光顕微鏡(100倍率)下で観察し、試料の全表面
積に占める光学的異方性相の面積の割合を測定すること
によって求める。
Specifically, for example, a sample piece of a heat-treated product is crushed into several square pieces, embedded into almost the entire surface of a resin with a diameter of approximately 2 cm using a conventional method, and after polishing the surface, the entire surface is thoroughly inspected using a polarizing microscope. (100x magnification) and determine the ratio of the area of the optically anisotropic phase to the total surface area of the sample.

この様にして得られた紡糸ピッチを公知の方法に従い、
溶融紡糸し、得られた繊維状ピッチを不融化、炭化し、
場合によっては更に黒鉛化する事により、強度が向上し
、かつ強度分布のバラツキが小さい高特性ピッチ系炭素
繊維を得る事ができる。
The spinning pitch obtained in this way is processed according to a known method.
The fibrous pitch obtained by melt spinning is infusible and carbonized.
In some cases, by further graphitizing, it is possible to obtain high-performance pitch-based carbon fibers with improved strength and small variations in strength distribution.

(効果) 本発明によれば、特定の条件で炭素質原料に不活性気体
を吹き込みながら加熱処理することにより、発生する揮
発性低分子物を効率よく、かつ十分に除去することがで
きるので、均質化した物性を有する紡糸ピッチが安定的
に得られ、そしてかかる紡糸ピッチにより高特性のピッ
チ系炭素繊維を製造することができる。
(Effects) According to the present invention, volatile low-molecular substances generated can be efficiently and sufficiently removed by heating the carbonaceous raw material while blowing an inert gas under specific conditions. A spinning pitch having homogenized physical properties can be stably obtained, and pitch-based carbon fibers with high properties can be produced using this spinning pitch.

本発明の紡糸ピッチは均質化しており、ゲル化物等を含
まないので紡糸性にも優れており、得られる繊維の高特
性と共に本発明の工業的有用性は大きいものである。
Since the spinning pitch of the present invention is homogenized and does not contain gelled substances, it has excellent spinnability, and the obtained fibers have high properties and the present invention has great industrial utility.

(実施例) 以下、本発明を実施例により具体的に説明するが、本発
明の要旨を超えない限り、本発明は後記の実施例に限定
されるものではない。
(Examples) Hereinafter, the present invention will be specifically explained using Examples, but the present invention is not limited to the Examples described below unless it exceeds the gist of the present invention.

実施例1−弘 攪拌機付オートクレープにコールタールピッチ100部
、クレオソート油100部、酸化鉄3部および硫黄2.
17部の混合物を連続的に供給し、水素圧t s o 
Kg/ct/i・G 、温度ll70℃、平均滞留時間
2時間で水添処理した。この処理物を濾過して鉄触媒等
を除去後、減圧蒸留により溶媒を留去して水添ピッチを
得た。
Example 1 - In an autoclave with a Hiro stirrer, 100 parts of coal tar pitch, 100 parts of creosote oil, 3 parts of iron oxide, and 2.0 parts of sulfur were added.
17 parts of the mixture were continuously fed and the hydrogen pressure t s o
The hydrogenation treatment was carried out at a temperature of 70° C. and an average residence time of 2 hours. The treated product was filtered to remove the iron catalyst and the like, and then the solvent was distilled off under reduced pressure to obtain hydrogenated pitch.

第1図に示す容積1oot(内径3jOI+511長さ
1100m)の攪拌機付反応器lに所定の口径を有する
不活性気体供給管−を、該供給管λの開口部が反応器/
底面から100wmとなる位置に下向きに設置した。
An inert gas supply pipe having a predetermined diameter is connected to a stirrer-equipped reactor l having a volume of 1oot (inner diameter 3jOI + 511 length 1100m) shown in Fig. 1, and the opening of the supply pipe λ is connected to the reactor /
It was installed facing downward at a position 100 wm from the bottom.

この反応器/に上記水添ピッチ60Kfを装入し、不活
性気体供給管コより予熱した窒素ガスを第1表に示す条
件で供給しながら常圧下、又は減圧下でダλO℃で9時
間加熱処理して紡糸ピッチを得た。
The above hydrogenated pitch 60Kf was charged into this reactor, and preheated nitrogen gas was supplied from the inert gas supply pipe under the conditions shown in Table 1 under normal pressure or reduced pressure at λO ℃ for 9 hours. A spinning pitch was obtained by heat treatment.

各紡糸ピンチ(光学的異方性割合はいずれも90%以上
)を、ノズル口径0.3m、ノズル長0、&tmの紡糸
ノズルを用いて液温J410℃、吐出速度0.□ 49
部mで溶融紡糸し、紡糸時の巻取速度を変えることによ
って糸径を変え、各糸径での持続時間を測定して紡糸性
を評価した。結果を第1表に示す。
Each spinning pinch (all optical anisotropy ratios are 90% or more) was processed using a spinning nozzle with a nozzle diameter of 0.3 m, a nozzle length of 0, &tm, and a liquid temperature of 410°C and a discharge speed of 0. □ 49
Melt spinning was carried out in part m, the yarn diameter was varied by changing the winding speed during spinning, and the duration at each yarn diameter was measured to evaluate spinnability. The results are shown in Table 1.

比較例−/〜コ 不活性気体供給管の口径およびガス線速を変更する以外
は実施例−7と同様に実施した。結果は第1表に示す。
Comparative Example -/- The same procedure as Example 7 was carried out except that the diameter of the inert gas supply pipe and the gas linear velocity were changed. The results are shown in Table 1.

実施例−7〜!ではIOμ以下の細径繊維を安定紡糸で
き工業的に十分有用な紡糸ピッチが得られたが、比較例
−7およびコではトルエン可溶分に代表される軽質分の
除去不足による気泡破断により72μ糸でも安定紡糸で
きなかった0 実施例−5 不活性気体供給管の開口部の位置を反応器底面から/l
Omとした以外は実施例−/と同様に実施した。その結
果を第1表に示す。
Example-7~! In Comparative Examples 7 and 7, fibers with a diameter of IOμ or less could be stably spun, and a spinning pitch that was industrially useful was obtained. Stable spinning could not be achieved even with yarn Example-5 The position of the opening of the inert gas supply pipe was adjusted from the bottom of the reactor to /l.
It was carried out in the same manner as in Example -/, except that Om was used. The results are shown in Table 1.

チー−哄掃Qi - Sweeping

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

第1図は本発明の紡糸ピッチを製造するための製造装置
の一例の概略断面図である。 /;反応器  ユ:不活性気体供給管 3;攪拌翼り;不活性気体導入管 5;排気管 出 願 人  三菱化成工業株式会社 代理人弁理士  長谷用   − ほか1名 第 1 図
FIG. 1 is a schematic cross-sectional view of an example of a manufacturing apparatus for manufacturing the spinning pitch of the present invention. /; Reactor U: Inert gas supply pipe 3; Stirring blade; Inert gas introduction pipe 5; Exhaust pipe Applicant Mitsubishi Chemical Industries, Ltd. Patent attorney Yo Hase - 1 other person Figure 1

Claims (5)

【特許請求の範囲】[Claims] (1)炭素質原料に不活性気体を吹き込みながら加熱処
理することにより炭素繊維用紡糸ピッチを製造する際に
、不活性気体を口径15mm以下の不活性気体供給管よ
りガス線速度 30m/sec以上の供給速度で炭素質原料に吹き込む
ことを特徴とする炭素繊維用紡糸ピッチの製造方法。
(1) When producing spinning pitch for carbon fibers by heat-treating carbonaceous raw materials while blowing inert gas into them, inert gas is supplied from an inert gas supply pipe with a diameter of 15 mm or less at a gas linear velocity of 30 m/sec or more. A method for producing spinning pitch for carbon fibers, which comprises blowing into a carbonaceous raw material at a supply rate of .
(2)不活性気体が窒素、アルゴン、二酸化炭素、ヘリ
ウム、水蒸気、水素あるいは炭素数が6個以下の炭化水
素からなる群から選ばれる少なくとも1種以上であるこ
とを特徴とする特許請求の範囲第1項記載の方法。
(2) Claims characterized in that the inert gas is at least one selected from the group consisting of nitrogen, argon, carbon dioxide, helium, water vapor, hydrogen, and hydrocarbons having 6 or less carbon atoms. The method described in paragraph 1.
(3)不活性気体供給管の開口部を炭素質原料を収容す
る反応器底面から150mm以内に設置することを特徴
とする特許請求の範囲第1項記載の方法。
(3) The method according to claim 1, characterized in that the opening of the inert gas supply pipe is installed within 150 mm from the bottom of the reactor containing the carbonaceous raw material.
(4)不活性気体供給管の開口部を炭素質原料を収容す
る反応器底面に対向するよう設置し、不活性気体を該反
応器底面に衝突させて吹き込むことを特徴とする特許請
求の範囲第1項記載の方法。
(4) Claims characterized in that the opening of the inert gas supply pipe is installed to face the bottom of the reactor containing the carbonaceous raw material, and the inert gas is blown into the reactor by colliding with the bottom of the reactor. The method described in paragraph 1.
(5)不活性気体を複数個の供給管より吹き込むことを
特徴とする特許請求の範囲第1項記載の方法。
(5) The method according to claim 1, characterized in that the inert gas is blown through a plurality of supply pipes.
JP13355185A 1985-06-19 1985-06-19 Method for producing spinning pitch for carbon fiber Expired - Lifetime JPH0635586B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13355185A JPH0635586B2 (en) 1985-06-19 1985-06-19 Method for producing spinning pitch for carbon fiber

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13355185A JPH0635586B2 (en) 1985-06-19 1985-06-19 Method for producing spinning pitch for carbon fiber

Publications (2)

Publication Number Publication Date
JPS61291684A true JPS61291684A (en) 1986-12-22
JPH0635586B2 JPH0635586B2 (en) 1994-05-11

Family

ID=15107457

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13355185A Expired - Lifetime JPH0635586B2 (en) 1985-06-19 1985-06-19 Method for producing spinning pitch for carbon fiber

Country Status (1)

Country Link
JP (1) JPH0635586B2 (en)

Also Published As

Publication number Publication date
JPH0635586B2 (en) 1994-05-11

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