JPH0635586B2 - Method for producing spinning pitch for carbon fiber - Google Patents
Method for producing spinning pitch for carbon fiberInfo
- Publication number
- JPH0635586B2 JPH0635586B2 JP13355185A JP13355185A JPH0635586B2 JP H0635586 B2 JPH0635586 B2 JP H0635586B2 JP 13355185 A JP13355185 A JP 13355185A JP 13355185 A JP13355185 A JP 13355185A JP H0635586 B2 JPH0635586 B2 JP H0635586B2
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- JP
- Japan
- Prior art keywords
- inert gas
- pitch
- raw material
- spinning
- 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.)
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- Working-Up Tar And Pitch (AREA)
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ツ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ツチ
系炭素繊維を与える紡糸ピツチの製造方法に関するもの
である。Description: TECHNICAL FIELD The present invention relates to a method for producing a spinning pitch for carbon fiber, and more specifically, to a spinning pitch which gives a pitch-based carbon fiber having high strength and high elastic modulus. The present invention relates to a manufacturing method.
（従来の技術） 周知のように、重質油、タール、ピツチ等の炭素質原料
を３５０〜５００℃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 a carbonaceous raw material such as heavy oil, tar, and pitch is heated to 350 to 500 ° C., an optically polarized substance having a particle diameter of several microns to several hundreds of microns is included in these substances. Small spheres that show direction are generated. Then, upon further heating, these small spheres grow and coalesce, and finally the whole becomes a state exhibiting optical anisotropy. This anisotropic structure is formed by stacking and orienting high molecular weight aromatic hydrocarbons produced by a thermal polycondensation reaction of a carbonaceous raw material in layers, and is regarded as a precursor of a 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つて、高
強度、高弾性率などの特徴をもつピツチ系の高特性炭素
繊維の原料として提案されている。Such a heat-treated product is melt-spun, infusibilized, carbonized, and optionally graphitized through a spinneret to obtain a Pitch-based high-performance carbon fiber having characteristics such as high strength and high elastic modulus. Proposed as a raw material.
炭素繊維は、比強度、比弾性率が高い材料で、高性能複
合材料のフイラー繊維として最も注目されており、中で
もピツ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つている。Carbon fiber is a material with a high specific strength and a high specific elastic modulus, and has been the focus of attention as a filler fiber for high-performance composite materials. Among them, Pitch-based high-performance carbon fiber has a large yield in the carbonization process, It has various advantages over polyacrylonitrile-based carbon fiber such as high rate.
従来、ピツチ系高特性炭素繊維は、通常、所謂メソフエ
ーズを含有したピツチを紡糸原料とし、このメソフエー
ズ含有ピツチから繊維状ピツチを紡糸し、次いで、不融
化し、焼成（炭化、黒鉛化）して製造されている。Conventionally, the Pitch-based high-performance carbon fiber is usually prepared by using a so-called mesophase-containing pitch as a spinning raw material, spinning a fibrous pitch from the mesophase-containing pitch, then infusibilizing and firing (carbonization, graphitization). Being manufactured.
特にメソフエーズを多量に含有する紡糸ピツチを製造す
る際には特開昭57-42924号公報、特開昭58-168687号公
報等に開示されているように炭素質原料を撹拌しながら
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
ピツチを製造することは広く知られた技術である。In particular, when producing a spinning pitch containing a large amount of mesophases, as disclosed in JP-A-57-42924, JP-A-58-168687 or the like, while stirring the carbonaceous raw material or further gas. It is a well-known technique to produce a spinning pitch by heat-treating while blowing air.
（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、単に撹拌のみである
か、あるいは撹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
ツチ系炭素繊維を与えるような紡糸ピツチを安定的に、
かつ均一に製造するのには問題があつた。(Problems to be Solved by the Invention) However, in the conventional method, only the stirring is performed, or even when the gas is blown under the stirring, only the total amount of the gas is regulated. It is difficult to sufficiently remove volatile low-molecular substances generated by heat-treating a high-quality raw material, excellent spinnability, and stable spinning pitch that gives high-performance pitch-based carbon fibers,
In addition, there was a problem in manufacturing uniformly.
（問題点を解決するための手段） 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ツチを
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 Solving Problems) Then, as a result of intensive studies by the present inventors in order to solve the above-mentioned problems, as a result, low volatility generated when a carbonaceous raw material is heat-treated to produce a spinning pitch. Recognizing that it is important to measure sufficient gas-liquid contact in order to sufficiently remove the molecular substances, and by blowing an inert gas into the carbonaceous raw material as fine bubbles by a specific means, efficiently and The present inventors have completed the present invention by discovering that volatile small 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吹き込むこ
とにより、高特性のピツチ系炭素繊維を与えるような紡
糸ピツ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 object of the present invention is to blow a inert gas into a carbonaceous raw material at a specific rate through an inert gas supply pipe having a specific diameter, thereby stably and uniformly producing a spinning pitch such as a pitch-based carbon fiber having high characteristics. A method of manufacturing is provided.
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繊維用紡糸ピツチ
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により達成される。The purpose is to produce a spinning pitch for carbon fiber by heat-treating an inert gas while blowing an inert gas into the carbonaceous raw material. The inert gas is supplied from an inert gas supply pipe having a diameter of 15 mm or less at a gas linear velocity of 30 m / It is achieved by blowing carbonaceous material at a supply rate of sec or more.
以下、本発明を詳細に説明する。Hereinafter, the present invention will be described in detail.
本発明で紡糸ピツ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、コールタールピツチ、石
炭液化物、石油系の重質油、タール、ピツチ等で、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、５〜４５重量％、キノリン不溶分
２０重量％以下、好ましくは１５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。As the carbonaceous raw material for obtaining the spinning pitch in the present invention,
For example, coal-based coal tar, coal tar pitch, coal liquefaction, petroleum heavy oil, tar, pitch, etc., the benzene-insoluble content is 60 wt% or less, preferably 50 wt% or less, more preferably 5 to 45% by weight, quinoline insoluble content is 20% by weight or less, preferably 15% by weight or less, and more preferably 5% by weight or less.
この炭素質原料のベンゼン不溶分、キノリン不溶分が上
記範囲を超えると得られる紡糸ピツチの溶融粘度が高く
なり、従つて、高温にて紡糸しなければならなくなる。
その為、紡糸中に紡糸ピツチの熱変質を生じやすくな
り、好ましくない。If the benzene-insoluble matter and the quinoline-insoluble matter of the carbonaceous raw material exceed the above-mentioned ranges, the melt viscosity of the obtained spinning pitch becomes high, and accordingly, spinning must be performed at a high temperature.
Therefore, thermal deterioration of the spinning pitch is likely to occur during spinning, which is not preferable.
予備処理としては、前記炭素質原料を３５０〜５００
℃、常圧〜１０Kg/cm2・Ｇで０．５〜２０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１重量部
に対して約０．１〜３重量部の沸点又は初留点が１５０
℃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 pretreatment, the carbonaceous raw material is 350 to 500
At least 30% or more, preferably 50% or more, and particularly preferably 70% or more of the optically anisotropic portion is obtained by heat treatment at 0 ° C and normal pressure to 10 kg / cm 2 · G for 0.5 to 20 hours. Such a heat-treated product is obtained, and then the boiling point or initial boiling point of about 0.1 to 3 parts by weight is 150 with respect to 1 part by weight of this heat-treated product.
The soluble component is obtained by contacting with an aromatic oil at a temperature of ℃ or higher. As the aromatic oil, naphthalene oil, absorbing oil, creosote oil or anthracene oil is preferable.
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、以後の処理では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
によつて推測される。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接触として鉄系化合物、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
３６０〜５００℃にて水添処理後必要に応じ過等で固
形分を除去し、更に必要に応じて蒸留等によつて、溶媒
を除いた残渣物を得る方法も考えられる。Although the meaning of this pretreatment is not completely clear, it is assumed by the present inventors that the relatively high molecular weight portion that cannot be restored to an appropriate substance again in the subsequent treatment is to be removed in advance. To be done. As a means for satisfying such a meaning, a carbonaceous raw material or the above-mentioned aromatic oil-soluble component is easily combined with a hydrogen-donating solvent of tetralin, decalin, tetrahydroquinoline, hydrogenated aromatic oil, or a hydrogen-donating solvent. Quinoline, naphthalene oil, anthracene oil, etc., which can be converted into hydrogen, are added to the catalyst in contact with a supported or unsupported catalyst containing an iron-based compound and Mo, and hydrogenated at 360 to 500 ° C. under hydrogen gas pressure. A method is also conceivable in which the solid content is removed excessively if necessary, and if necessary, the residue is obtained by removing the solvent by distillation or the like.
本発明において、前記の予備処理を行なつた炭素質原料
を３００〜５００℃、好ましくは３８０〜４５０℃、減
圧〜１０Kg/cm2・Ｇ、好ましくは１０mmHg〜常圧で２０
分〜１０時間、好ましくは１〜６時間程度加熱すること
により紡糸ピツチを得るが、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３０m/se
c 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１〜１５mm以下、更に好ましくは１〜８
mm以下の供給管を用い、ガス線速度３０m/秒以上、好ま
しくは５０〜５００m/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１〜５mm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-mentioned pretreatment is 300 to 500 ° C., preferably 380 to 450 ° C., reduced pressure to 10 Kg / cm 2 · G, preferably 10 mmHg to atmospheric pressure.
The spinning pitch is obtained by heating for about 10 minutes, preferably about 1 to 6 hours. At that time, the inert gas is fed with an inert gas supply pipe having a diameter of 15 mm or less at a gas linear velocity of 30 m / se.
While blowing into the carbonaceous raw material at a supply rate of c or more,
It is important to perform the heat treatment under the above conditions.
The diameter is preferably 1 to 15 mm or less, more preferably 1 to 8
It is advisable to use a supply pipe of mm or less and blow an inert gas at a gas linear velocity of 30 m / sec or more, preferably 50 to 500 m / sec. By such a method, the inert gas can be dispersed in the carbonaceous raw material as fine bubbles of, for example, about 1 to 5 mm.
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 is blocked by a minute solid substance contained in the carbonaceous raw material, and if it is too large, an appropriate gas linear velocity can be obtained. This is not preferable because it is difficult to be done.
なお、撹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 due to local heating near the wall surface of the carbonaceous raw material heat treatment device,
Not enough to remove the volatile low-molecular substances that are generated,
Even if an inert gas is blown in, the effect of reducing the bubbles of the inert gas is small.
したがつて、十分に気液接触を行なつて揮発性低分子物
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 carry out sufficient gas-liquid contact and to remove the volatile low-molecular substances by entraining them in 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つて、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〜
２５０mm、好ましくは１５０mm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。Further, in order to sufficiently reduce the bubbles of the inert gas, the installation position of the inert gas supply pipe is important, and the opening of the supply pipe is usually 200 to 200 mm from the bottom of the reactor containing the carbonaceous raw material.
It is preferably 250 mm or less, preferably 150 mm or less, and it is preferable that the opening is installed so as to face the bottom surface of the reactor so that the inert gas collides with the bottom surface.
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２〜２００個
に分割して設けるのが好ましい。Further, in order to more effectively remove the volatile low-molecular-weight substances, it is preferable to provide the inert gas supply pipe by dividing it into a plurality of, for example, 2 to 200 pieces.
また、本発明においても、不活性気体を吹き込むと同時
に撹拌を行ないながら、炭素質原料を加熱処理を行なつ
てもよい。Further, also in the present invention, the carbonaceous raw material may be subjected to the heat treatment while the inert gas is blown and stirring is performed at the same time.
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 is not a gas that oxidizes the carbonaceous raw material to make it heavy during heat treatment, and specifically, nitrogen, argon,
Examples thereof 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 or 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２種以上の不活性気体を混合して用いてもよ
い。Further, these inert gases may be used alone, or if necessary, two or more kinds of inert gases may be mixed and used.
本発明においては、光学的異方性相を４０％以上、好ま
しくは、７０〜１００％、特に好ましくは、９０〜１０
０％含み、しかも、キノリン不溶分が４０重量％以下、
好ましくは、３０重量％以下、特に好ましくは、２５重
量％以下の紡糸ピツ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 40% or more, preferably 70 to 100%, particularly preferably 90 to 10%.
0% and quinoline insoluble content is 40% by weight or less,
It is necessary to select the above heat treatment conditions so as to obtain a spinning pitch of preferably 30% by weight or less, particularly preferably 25% by weight or less.
尚、本発明でいう紡糸ピツチの光学的異方性相の含量
は、常温下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。The content of the optically anisotropic phase of the spinning pitch in the present invention is a value obtained as the area ratio of the portion showing the optical anisotropy in the heat-treated product sample under a polarization microscope at room temperature.
具体的には、例えば、熱処理物試料を数mm角に粉砕した
ものを常法に従つて約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
よつて求める。Specifically, for example, a heat-treated sample crushed into a few mm square is embedded with a sample piece on almost the entire surface of a resin having a diameter of about 2 cm according to a conventional method, the surface is polished, and then the entire surface is covered. It is determined by observing under a polarizing microscope (100 magnification) and measuring 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ツチを公知の方法に従い、
溶融紡糸し、得られた繊維状ピツチを不融化、炭化し、
場合によつては更に黒煙化する事により、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ツチ系炭
素繊維を得る事ができる。According to a known method, the spinning pitch thus obtained is
Melt spinning, infusibilize and carbonize the resulting fibrous pitch,
In some cases, by further producing black smoke, it is possible to obtain a high-performance pitch-based carbon fiber having improved strength and a small variation 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ツチが安定的
に得られ、そしてかかる紡糸ピツチにより高特性のピツ
チ系炭素繊維を製造することができる。(Effect) According to the present invention, the heat treatment while blowing an inert gas into the carbonaceous raw material under specific conditions makes it possible to efficiently and sufficiently remove the volatile low-molecular substances generated. A spinning pitch having homogenized physical properties can be stably obtained, and a high-characteristic pitch-based carbon fiber can be produced by the spinning pitch.
本発明の紡糸ピツ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 a gelled substance and the like, it is excellent in spinnability, and the industrial properties of the present invention are great together with the high characteristics of the obtained fiber.
（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 described with reference to Examples, but the present invention is not limited to the Examples described below as long as the gist of the present invention is not exceeded.
実施例１〜４ 撹拌機付オートクレーブにコールタールピツチ１００
部、クレオソート油１００部、酸化鉄５部および硫黄
２．４部の混合物を連続的に供給し、水素圧１５０Kg/c
m2・Ｇ、温度４７０℃、平均滞留時間２時間で水添処理
した。この処理物を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ツチを得た。Examples 1 to 4 Coal tar pitch 100 in an autoclave equipped with a stirrer
Parts, 100 parts of creosote oil, 5 parts of iron oxide and 2.4 parts of sulfur are continuously supplied, and the hydrogen pressure is 150 Kg / c.
Hydrogenation was carried out at m 2 · G, temperature of 470 ° C. and average residence time of 2 hours. After passing through this treated product to remove the iron catalyst and the like, the solvent was distilled off by vacuum distillation to obtain a hydrogenated pitch.
第１図に示す容積１００（内径３５０mm、長さ１１０
０mm）の撹拌機付反応器１に所定の口径を有する不活性
気体供給管２を、該供給管２の開口部が反応器１底面か
ら１００mmとなる位置に下向きに設置した。Volume 100 shown in Fig. 1 (internal diameter 350 mm, length 110
An inert gas supply pipe 2 having a predetermined diameter was installed in a reactor 1 with a stirrer of 0 mm) at a position where the opening of the supply pipe 2 was 100 mm from the bottom surface of the reactor 1 downward.
この反応器１に上記水添ピツチ６０Kgを装入し、不活性
気体供給管２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４２０℃で４時間
加熱処理して紡糸ピツチを得た。This reactor 1 was charged with 60 kg of the above hydrogenated pitch, and nitrogen gas preheated from the inert gas supply pipe 2 was supplied under the conditions shown in Table 1 while heating under atmospheric pressure or reduced pressure at 420 ° C. for 4 hours. This was processed to obtain a spinning pitch.
各紡糸ピツチ（光学的異方性割合はいずれも９０％以
上）を、ノズル口径０．３mm、ノズル長０．６mmの紡糸
ノズルを用いて液温３４０℃、吐出速度０．０６g/min
で溶融紡糸し、紡糸時の巻取速度を変えることによつて
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。Using a spinning nozzle having a nozzle diameter of 0.3 mm and a nozzle length of 0.6 mm, each spinning pitch (optical anisotropy ratio of 90% or more) was supplied at a liquid temperature of 340 ° C. and a discharge rate of 0.06 g / min.
Was melt-spun, and the yarn diameter was changed by changing the winding speed at the time of spinning, and the duration at each yarn diameter was measured to evaluate the spinnability. The results are shown in Table 1.
比較例−１〜２ 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−１と同様に実施した。結果は第１表に示す。Comparative Examples-1 and 2 The procedure of Example-1 was repeated 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−１〜５では１０μ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ツチが得られたが、比較例
−１および２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１２μ糸でも安定紡糸で
きなかつた。In Examples 1 to 5, spinning pitches capable of stable spinning of fine fibers of 10 μm or less were obtained, and industrially sufficiently useful spinning pitches were obtained, but in Comparative Examples 1 and 2, removal of light components represented by toluene-soluble components. Stable spinning was not possible even with 12μ yarn due to bubble breakage due to lack.
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１８
０mmとした以外は実施例−１と同様に実施した。その結
果を第１表に示す。Example-5 The position of the opening of the inert gas supply pipe was set to 18 from the bottom of the reactor.
Example 1 was repeated except that the thickness was 0 mm. The results are shown in Table 1.
第１図は本発明の紡糸ピツ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。 １；反応器、２；不活性気体供給管 ３；撹拌翼、４；不活性気体導入管 ５；排気管FIG. 1 is a schematic sectional view of an example of a manufacturing apparatus for manufacturing the spinning pitch of the present invention. 1; Reactor, 2; Inert gas supply pipe 3; Stirrer, 4; Inert gas introduction pipe 5; Exhaust pipe
Claims (5)
加熱処理することにより炭素繊維用紡糸ピツチを製造す
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ツチの
製造方法。1. When producing a spinning pitch for carbon fiber by heat-treating a carbonaceous raw material while blowing an inert gas, the inert gas is supplied from an inert gas supply pipe having a diameter of 15 mm or less at a gas linear velocity of 30 m / A method for producing a spinning pitch for carbon fiber, which comprises blowing the carbonaceous raw material at a supply rate of sec or more.
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. 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 according to claim 1.
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, wherein the opening of the inert gas supply pipe is installed within 150 mm from the bottom of the reactor containing the carbonaceous raw material.
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. An opening of an inert gas supply pipe is installed so as to face a bottom surface of a reactor containing a carbonaceous raw material, and an inert gas is blown into the bottom surface of the reactor while colliding with the bottom surface of the reactor. The method according to claim 1.
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, wherein an inert gas is blown through a plurality of supply pipes.
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 JPS61291684A (en) | 1986-12-22 |
| JPH0635586B2 true 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) |
-
1985
- 1985-06-19 JP JP13355185A patent/JPH0635586B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61291684A (en) | 1986-12-22 |
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