JPH06108317A - Production of graphitized fiber and apparatus for production - Google Patents
Production of graphitized fiber and apparatus for productionInfo
- Publication number
- JPH06108317A JPH06108317A JP4274823A JP27482392A JPH06108317A JP H06108317 A JPH06108317 A JP H06108317A JP 4274823 A JP4274823 A JP 4274823A JP 27482392 A JP27482392 A JP 27482392A JP H06108317 A JPH06108317 A JP H06108317A
- Authority
- JP
- Japan
- Prior art keywords
- heating element
- temperature
- tubular
- tubular heating
- 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.)
- Pending
Links
- 239000000835 fiber Substances 0.000 title claims description 39
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 143
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011261 inert gas Substances 0.000 claims abstract description 23
- 230000005855 radiation Effects 0.000 claims abstract description 16
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 15
- 239000010439 graphite Substances 0.000 claims abstract description 15
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 13
- 239000004917 carbon fiber Substances 0.000 claims abstract description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000002093 peripheral effect Effects 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 17
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 238000009529 body temperature measurement Methods 0.000 claims description 7
- 230000000149 penetrating effect Effects 0.000 claims description 7
- 125000006850 spacer group Chemical group 0.000 abstract description 7
- 239000011810 insulating material Substances 0.000 abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 230000020169 heat generation Effects 0.000 description 3
- 238000004904 shortening Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
- Tunnel Furnaces (AREA)
- Inorganic Fibers (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、黒鉛化繊維の製造方法
および製造装置の改良に関し、詳しくは、炭素繊維を安
定した温度で焼成し均質な黒鉛化繊維を製造する方法及
び装置に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an improved method and apparatus for producing graphitized fiber, and more particularly to a method and apparatus for producing uniform graphitized fiber by firing carbon fiber at a stable temperature. is there.
【０００２】[0002]
【従来の技術】黒鉛化繊維の製造方法は、通常、次ぎの
方法によって製造される。まず、ポリアクリロニトリル
繊維、再生セルローズ繊維、フェノール系繊維、ピッチ
系繊維等の有機重合体を空気または他の酸化性ガス雰囲
気中にて２００〜３００度（以下、温度は、全て摂氏で
表示する。）の温度で耐炎化する。次いで、これを窒
素、アルゴン等の不活性ガス雰囲気中にて８００〜２０
００度の温度で炭化し、炭素繊維とする。次に、この炭
素繊維を２０００度以上の温度で焼成し黒鉛化を行うこ
とにより、ヤング率が一段と高い黒鉛化繊維を得る。2. Description of the Related Art Generally, a graphitized fiber is manufactured by the following method. First, an organic polymer such as polyacrylonitrile fiber, regenerated cellulose fiber, phenol fiber, pitch fiber or the like is heated to 200 to 300 degrees Celsius in air or another oxidizing gas atmosphere (all temperatures are expressed in degrees Celsius below. ) Flameproof at temperature. Then, this is placed in an inert gas atmosphere such as nitrogen or argon at 800 to 20.
Carbonized at a temperature of 00 degrees to obtain carbon fiber. Next, this carbon fiber is fired at a temperature of 2000 ° C. or higher to graphitize, thereby obtaining a graphitized fiber having a higher Young's modulus.
【０００３】このような黒鉛化繊維の製造方法に用いら
れる従来の装置としては、タンマン型や高周波誘導方式
による発熱体自体を加熱する型の装置が知られている。
この従来の装置の一例を図面に基づいて説明する。As a conventional apparatus used in such a method for producing graphitized fibers, a Tamman type apparatus or a high frequency induction type apparatus for heating a heating element itself is known.
An example of this conventional device will be described with reference to the drawings.
【０００４】第３図は、そのタンマン型の装置（炉）の
概略断面図、第４図は第３図のＣ−Ｃ´断面を示す概略
断面図で、黒鉛または炭素からなり内側を繊維糸条の処
理域とする筒状発熱体２と、前記筒状発熱体の両側に設
けられた電極４と、前記筒状発熱体および前記電極を囲
むと共に前記筒状発熱体の内部に不活性ガスを供給する
ためのガス注入口１２と繊維の入口および出口とを有す
る炉殻１と、前記繊維の入口および出口に接続され前記
不活性ガスをシールするシール部７と、前記筒状発熱体
の外周面温度を炉殻に形成された覗窓９１を通して測定
する測温手段１０１と、前記測温手段からの信号に基づ
き前記電極を経て前記筒状発熱体に流れる電流を制御し
発熱体の温度を調節する温度制御手段２０１とを備えた
ものである。なお、測温手段１０２、温度指示記録計２
０２は、温度管理用である。FIG. 3 is a schematic cross-sectional view of the Tammann type apparatus (furnace), and FIG. 4 is a schematic cross-sectional view showing the CC ′ cross section of FIG. A cylindrical heating element 2 serving as a strip processing region, electrodes 4 provided on both sides of the cylindrical heating element, an inert gas inside the cylindrical heating element while surrounding the cylindrical heating element and the electrodes. Of the tubular heating element, a furnace shell 1 having a gas inlet 12 for supplying the gas, an inlet and an outlet of the fiber, a seal portion 7 connected to the inlet and the outlet of the fiber to seal the inert gas, Temperature measuring means 101 for measuring the temperature of the outer peripheral surface through a viewing window 91 formed in the furnace shell, and the temperature of the heating element by controlling the current flowing through the electrode to the cylindrical heating element based on a signal from the temperature measuring means. And a temperature control means 201 for adjusting the temperature. The temperature measuring means 102 and the temperature instruction recorder 2
02 is for temperature management.
【０００５】そして、この装置を用い、ニップローラ２
１側から炭素繊維１４を供給して筒状発熱体２内で２０
００度以上で焼成し、ニップローラ２２で引き取り、黒
鉛化繊維を製造していた。Using this device, the nip roller 2
The carbon fiber 14 is supplied from the 1 side and 20
It was fired at a temperature of 00 degrees or more and taken up by the nip roller 22 to produce graphitized fiber.
【０００６】[0006]
【発明が解決しょうとする課題】しかし、上記従来の黒
鉛または炭素からなる筒状発熱体は、外周面に発熱体の
熱分解物が付着し、それが経時的に堆積するため、放射
温度計で測定する外周面の温度は、筒状発熱体の内周面
の温度に対して経時的に低下していた。一方、筒状発熱
体の温度は、その発熱体の外周面の温度測定信号に基づ
いて制御されているため、上記のように経時的に低下す
ると、その低下した分だけ外周面の温度を上昇させるよ
うに制御されるので、筒状発熱体の内周面の温度は、外
周面の低下した温度に相当する分だけ逆に上昇する。す
なわち、従来の筒状発熱体は、外周面に発熱体の熱分解
物が経時的に付着堆積するため、その堆積による外周面
と内周面との温度差に対応する分だけ内周面の温度が経
時的に上昇し、発熱体の内側である繊維の処理域の温度
が経時的に変化するという欠点を有していた。However, in the conventional cylindrical heating element made of graphite or carbon, the thermal decomposition product of the heating element adheres to the outer peripheral surface and is deposited over time, so that the radiation thermometer is used. The temperature of the outer peripheral surface measured in 1. was lower than the temperature of the inner peripheral surface of the tubular heating element with time. On the other hand, since the temperature of the cylindrical heating element is controlled based on the temperature measurement signal of the outer peripheral surface of the heating element, if the temperature decreases over time as described above, the temperature of the outer peripheral surface rises by the reduced amount. Therefore, the temperature of the inner peripheral surface of the cylindrical heating element rises conversely by an amount corresponding to the lowered temperature of the outer peripheral surface. That is, in the conventional cylindrical heating element, since the thermal decomposition product of the heating element adheres and deposits on the outer peripheral surface over time, the inner peripheral surface of the inner peripheral surface corresponds to the temperature difference between the outer peripheral surface and the inner peripheral surface due to the deposition. It has a drawback that the temperature rises with time and the temperature of the treated area of the fiber inside the heating element changes with time.
【０００７】また、筒状発熱体は、使用温度が２０００
度以上と非常に高いため、炭素質の蒸発（昇華）が起こ
り、短時間で減耗、劣化し、頻繁な発熱体の交換を余儀
なくされることになる。炭素質の蒸発は、発熱体温度が
２５００度を超えると急速に激しくなり、３０００度レ
ベルの超高温度では、数十乃至数百時間の寿命でしかな
く、上記の如く、経時的に温度が上昇することは、それ
だけ、寿命が短くなるという欠点を生ずる。The operating temperature of the cylindrical heating element is 2000
Since the temperature is extremely high, the carbonaceous material is evaporated (sublimated), is worn and deteriorated in a short time, and the heat generating element is frequently replaced. The carbonaceous material vaporizes rapidly when the temperature of the heating element exceeds 2500 degrees Celsius, and at an extremely high temperature of 3000 degrees Celsius, it has a life of several tens to several hundreds of hours. Rising raises the drawback of shortening the life accordingly.
【０００８】また、一度発熱体の交換の必要が生ずる
と、先ず、炉の温度を下げなければならず、２０００度
或いは２５００度といった状態から、作業できる状態ま
でおよそ１週間が必要である。交換に数日を要したとし
て、交換完了から徐々に温度を上げてゆき、定常状態に
達するまでに約一週間が必要である。従って、交換の都
度約半ヶ月間は生産は行われない。使用時間が数時間或
いは数十時間ということになると、装置はほとんど発熱
体の交換に時間を取られ、使用時間は極めて少なくなる
ので、装置の稼働率が極めて低く、上記の如き経時的温
度上昇による寿命低下の改善が強く望まれていた。Further, once it becomes necessary to replace the heating element, the temperature of the furnace must first be lowered, and it takes about one week from the state of 2000 ° C. or 2500 ° C. to the working state. Even if it takes several days for replacement, it takes about one week from the completion of replacement to gradually raising the temperature and reaching a steady state. Therefore, there is no production for about half a month for each replacement. When the usage time is several hours or tens of hours, most of the equipment takes time to replace the heating element, and the usage time is extremely short, so the operation rate of the equipment is extremely low and the temperature rise with time as described above. There has been a strong demand for improvement in life reduction due to
【０００９】本発明は、このような従来の状態に鑑み、
これを改善して正確な温度制御による加熱を可能にする
ことにより、発熱体の適正な寿命を確保し、被処理物の
製品品質を向上し、処理装置全体の稼働率を上げること
を可能にする高温加熱装置を提供しようとするものであ
る。The present invention has been made in view of such a conventional state.
By improving this and enabling heating by accurate temperature control, it is possible to ensure the proper life of the heating element, improve the product quality of the object to be processed, and increase the operating rate of the entire processing equipment. The present invention is intended to provide a high temperature heating device.
【００１０】[0010]
【課題を解決するための手段】本発明は、 １．黒鉛または炭素からなり内側を繊維の処理域とする
筒状発熱体と、前記筒状発熱体の両側に設けられた電極
と、前記筒状発熱体および前記電極を囲むと共に前記筒
状発熱体の内部に不活性ガスを供給するためのガス注入
口と繊維の入口および出口とを有する炉殻と、前記繊維
の入口および出口に接続され前記不活性ガスをシールす
るシール部と、前記筒状発熱体の温度を炉殻に形成され
た窓を通して測定する測温手段と、前記測温手段からの
信号に基づき前記電極を経て前記筒状発熱体に流れる電
流を制御し発熱体の温度を調節する温度制御手段とを備
えた加熱装置を用い、炭素繊維を、前記筒状発熱体内へ
連続的に通過せしめながら加圧不活性ガス雰囲気中、２
０００℃以上の温度で焼成する黒鉛化繊維の製造方法に
おいて、前記筒状発熱体には筒体の外側から内側へ貫通
する測温孔を設け、前記測温手段で前記筒状発熱体の測
温孔を通して筒状発熱体の内周面の温度を測定し、前記
温度測定信号に基づいて前記筒状発熱体の温度を前記温
度制御手段で制御しながら前記焼成をすることを特徴と
する黒鉛化繊維の製造方法。The present invention includes: A tubular heating element made of graphite or carbon and having a fiber treatment area on the inside, electrodes provided on both sides of the tubular heating element, the tubular heating element and the tubular heating element surrounding the electrode. Furnace shell having a gas inlet for supplying an inert gas, an inlet and an outlet for the fiber, a seal portion connected to the inlet and the outlet for the fiber to seal the inert gas, and the tubular heat generation A temperature measuring means for measuring the temperature of the body through a window formed in the furnace shell, and a current flowing through the tubular heating element via the electrode based on a signal from the temperature measuring means to control the temperature of the heating element. Using a heating device provided with a temperature control means, while continuously passing carbon fibers into the tubular heating element, in a pressurized inert gas atmosphere, 2
In the method for producing graphitized fiber that is fired at a temperature of 000 ° C. or higher, the tubular heating element is provided with a temperature measuring hole penetrating from the outside to the inside of the tubular body, and the temperature measuring means measures Graphite characterized in that the temperature of the inner peripheral surface of the cylindrical heating element is measured through a warm hole, and the firing is performed while controlling the temperature of the cylindrical heating element by the temperature control means based on the temperature measurement signal. Method for producing synthetic fiber.
【００１１】２．黒鉛または炭素からなり内側を繊維の
処理域とする筒状発熱体と、前記筒状発熱体の両側に設
けられた電極と、前記筒状発熱体および前記電極を囲む
と共に前記筒状発熱体の内部に不活性ガスを供給するた
めのガス注入口と繊維の入口および出口とを有する炉殻
と、前記繊維の入口および出口に接続され前記不活性ガ
スをシールするシール部と、前記筒状発熱体の温度を炉
殻に形成された窓を通して測定する測温手段と、前記測
温手段からの信号に基づき前記電極を経て前記筒状発熱
体に流れる電流を制御し発熱体の温度を調節する温度制
御手段とを備えた黒鉛化繊維の製造装置において、前記
筒状発熱体は、筒体の外側から内側へ貫通する測温孔が
設けられ、かつ、前記測温手段は、前記測温孔を通して
前記筒状発熱体の内周面の温度を測定する放射温度計で
あることを特徴とする黒鉛化繊維の製造装置。2. A tubular heating element made of graphite or carbon and having a fiber treatment area on the inside, electrodes provided on both sides of the tubular heating element, the tubular heating element and the tubular heating element surrounding the electrode. Furnace shell having a gas inlet for supplying an inert gas, an inlet and an outlet for the fiber, a seal portion connected to the inlet and the outlet for the fiber to seal the inert gas, and the tubular heat generation A temperature measuring means for measuring the temperature of the body through a window formed in the furnace shell, and a current flowing through the tubular heating element via the electrode based on a signal from the temperature measuring means to control the temperature of the heating element. In the apparatus for producing graphitized fiber having temperature control means, the tubular heating element is provided with a temperature measuring hole penetrating from the outside to the inside of the cylindrical body, and the temperature measuring means is the temperature measuring hole. To measure the temperature of the inner peripheral surface of the cylindrical heating element. Graphitized fiber manufacturing apparatus which is a radiation thermometer to be.
【００１２】３．黒鉛または炭素からなる筒状発熱体で
あって、前記発熱体は筒体の外側から内側へ貫通する孔
が形成されていることを特徴とする筒状発熱体。によっ
て目的を達成するものである。3. A tubular heating element made of graphite or carbon, wherein the heating element has a hole penetrating from the outside to the inside of the tubular body. To achieve the purpose.
【００１３】本発明者らは目的を達成するにあたり次ぎ
の点に着目した。すなわち、一般の物質の蒸発速度は蒸
気の外周雰囲気中への拡散係数に比例する。そして、拡
散係数は、発熱体の温度の１．５乗に比例し、発熱体に
加わる圧力に反比例するので、発熱体の寿命を向上する
ためには雰囲気圧力を上げると共に発熱体の温度を経時
的に上昇させないようにすることが有効となる。よっ
て、本発明は、発熱体に、内壁を覗ける窓を設けて内部
温度を直接測定し、その測定信号で温度制御することに
より、発熱体の加熱温度の経時的変化による寿命低下の
防止と、糸に対する処理温度の安定化を図るものであ
る。The present inventors have paid attention to the following points in achieving the object. That is, the evaporation rate of a general substance is proportional to the diffusion coefficient of vapor into the outer atmosphere. The diffusion coefficient is proportional to the power of 1.5 of the temperature of the heating element and inversely proportional to the pressure applied to the heating element. Therefore, in order to improve the life of the heating element, increase the atmospheric pressure and increase the temperature of the heating element over time. It is effective not to raise it. Therefore, the present invention, the heating element, by providing a window through the inner wall to directly measure the internal temperature, by controlling the temperature by the measurement signal, prevention of life shortening due to the change over time of the heating temperature of the heating element, It is intended to stabilize the processing temperature for the yarn.
【００１４】以下図面を用いて詳細説明する。図１は、
本発明に係る高温加熱装置の全体構成を示すための、正
面断面図である。図２は、図１におけるＡ−Ａ´部で切
断した側面断面図である。なお、図１は図２のＢ−Ｂ´
部で切断した断面図である。A detailed description will be given below with reference to the drawings. Figure 1
It is a front sectional view for showing the whole high temperature heating equipment composition concerning the present invention. 2 is a side sectional view taken along the line AA ′ in FIG. In addition, FIG. 1 is BB ′ of FIG.
It is sectional drawing cut | disconnected by the part.
【００１５】図１は符号１４で示した被処理物と装置各
部の関わりあいが示されている。図面では被処理物は炭
化工程を経た炭化糸（炭素繊維）が示されており、図面
に示された加熱炉で加熱されて黒鉛化処理を受けるもの
が示されている。なお、本発明に適用される炭素繊維
は、公知の炭素繊維であれば何れであってもよく特に限
定されない。糸１４は矢印の方向に進行する。FIG. 1 shows the relationship between the object to be processed indicated by reference numeral 14 and each part of the apparatus. In the drawings, the object to be treated is a carbonized yarn (carbon fiber) which has undergone a carbonization process, and is shown to be heated in a heating furnace shown in the drawing and subjected to graphitization treatment. The carbon fiber applied to the present invention may be any known carbon fiber and is not particularly limited. The thread 14 advances in the direction of the arrow.
【００１６】加熱装置は全体が炉殻１の中に収容されて
いる。２は筒状の黒鉛製又は炭素製の発熱体である。筒
状発熱体２の外側にはスペーサーリング３１を介して外
筒３が嵌合している。外筒３は発熱体の支持と保護のた
めに設けられるものである。外筒３の外側には例えば黒
鉛粉末と電気絶縁材からなる黒鉛成形フェルトの如き断
熱材５が外筒と一体に設けられており炉殻内部を埋めて
いる。The entire heating device is housed in the furnace shell 1. Reference numeral 2 is a cylindrical graphite or carbon heating element. The outer cylinder 3 is fitted to the outside of the cylindrical heating element 2 via a spacer ring 31. The outer cylinder 3 is provided for supporting and protecting the heating element. A heat insulating material 5 such as a graphite molding felt made of graphite powder and an electric insulating material is provided integrally with the outer cylinder on the outer side of the outer cylinder 3 to fill the inside of the furnace shell.
【００１７】筒状発熱体２の両端部に電極４が接続され
ている。電極４は発熱体への通電のために設けられてお
り、高温度下での通電を確保するため水冷電極が使用さ
れ、外部の低電圧大電流の温度制御機２０１に接続して
いる。通電により筒状発熱体２はジュール熱により発熱
する。なお、水冷電極４は発熱体の発熱に伴う膨張に対
応するため一方を炉内に固定し、他方は炉内を移動でき
る構造となっている。Electrodes 4 are connected to both ends of the cylindrical heating element 2. The electrode 4 is provided to energize the heating element, and a water-cooled electrode is used to ensure energization under high temperature, and is connected to an external low-voltage large-current temperature controller 201. By energizing, the cylindrical heating element 2 generates Joule heat. The water-cooled electrode 4 has a structure in which one is fixed in the furnace and the other is movable in the furnace in order to cope with expansion due to heat generation of the heating element.
【００１８】炉殻１にはガス注入口１２が設けられてい
る。またこれに対応して炉殻１には圧力検出器１５、圧
力調節弁１６が設けられている。ガス注入口１２からは
例えば窒素、アルゴン等の不活性ガスが注入される。炉
内は発熱体の蒸発を抑制するため加圧状態にしておく必
要がある。このため炉殻内の雰囲気は少なくとも１Ｋｇ
／ｃｍ2Ｇの圧力に加圧することが好ましく、２〜１０
Ｋｇ／ｃｍ2Ｇの範囲がより好ましい。圧力検出器１
５、圧力調節弁１６は炉殻内の圧力を所定の値に保持す
るためのもので、自動的に圧力調節弁を作用させて炉殻
１内の圧力を所定の設定範囲に維持するよう作用する。
炉殻１は内部の圧力が加圧状態に保たれるので当然これ
に耐える耐圧構造となっている。The furnace shell 1 is provided with a gas inlet 12. Correspondingly, the furnace shell 1 is provided with a pressure detector 15 and a pressure control valve 16. An inert gas such as nitrogen or argon is injected from the gas injection port 12. The inside of the furnace needs to be in a pressurized state in order to suppress evaporation of the heating element. Therefore, the atmosphere in the furnace shell is at least 1 kg.
Pressure is preferably pressurized to a pressure of / cm 2 G, 2~10
The range of Kg / cm 2 G is more preferable. Pressure detector 1
5. The pressure control valve 16 is for keeping the pressure in the furnace shell at a predetermined value, and automatically acts to maintain the pressure in the furnace shell 1 within a predetermined setting range. To do.
Since the internal pressure of the furnace shell 1 is maintained in a pressurized state, the furnace shell 1 naturally has a pressure resistant structure that can withstand this.
【００１９】６は筒状発熱体の両端に設けられたスペー
サーで、発熱体である筒の内部の熱の逃げるのを抑える
機能を果たしている。７はシールで炉殻の糸の出入口に
設けられ、糸の通過に伴う不活性ガスの漏出を抑制する
ために設けられている。図１において被処理物である糸
１４は図の左側からシール７を経て炉殻内に入る。炉殻
内は不活性ガスにより加圧状態となっているので筒状発
熱体の蒸発は抑制された条件下にある。糸１４はこの雰
囲気の中でスペーサー６を経て筒状の発熱体の筒の中に
送られ所定の加熱を受ける。次いで加熱による処理が終
わるとスペーサー６シール７を経て炉殻１の外へ移動す
る。Numeral 6 is a spacer provided at both ends of the cylindrical heating element, and has a function of suppressing the escape of heat inside the tube which is the heating element. A seal 7 is provided at the inlet / outlet of the yarn of the furnace shell, and is provided to suppress the leakage of the inert gas accompanying the passage of the yarn. In FIG. 1, the thread 14 as the object to be processed enters the furnace shell through the seal 7 from the left side of the drawing. Since the furnace shell is pressurized by the inert gas, the evaporation of the cylindrical heating element is suppressed. In this atmosphere, the thread 14 is sent through the spacer 6 into the tube of the tubular heating element and is subjected to predetermined heating. Next, when the treatment by heating is completed, the spacer 6 is moved to the outside of the furnace shell 1 through the seal 7.
【００２０】図２には図１のＡ−Ａ´断面で切断した側
面が示されている。外筒３に孔をあけ、ここに測温パイ
プ８１、８２、８３が嵌合されている。測温パイプ８
１、８２、８３はグラファイトで作られており、一方の
端を外筒３の中に開口し、断熱材５の中を通り他方の端
を炉殻１に設けた取付部１７、１８、１９に開口してい
る。取付部１７、１８、１９の端は覗き窓９１、９２、
９３に接続している。１３は取付部の覗き窓付近に設け
られたガス注入口である。FIG. 2 shows a side surface taken along the line AA 'in FIG. A hole is formed in the outer cylinder 3, and temperature measuring pipes 81, 82, 83 are fitted therein. Temperature measuring pipe 8
1, 82, and 83 are made of graphite, one end of which is opened in the outer cylinder 3 and which passes through the heat insulating material 5 and the other end of which is provided in the furnace shell 1, 18, 19 It is open to. The ends of the mounting portions 17, 18 and 19 are viewing windows 91 and 92,
It is connected to 93. Reference numeral 13 is a gas injection port provided near the viewing window of the mounting portion.
【００２１】筒状発熱体２の一部に測温孔１１１、１１
２を設けている。測温パイプ８１、８３の一端は測温孔
１１１、１１２にそれぞれ対峙し筒状発熱体の内壁に向
いている。測温パイプ８１に対応している覗窓９１には
放射温度計１０１が設けられている。測温パイプ８２対
応している覗窓９２には放射温度計１０２が設けられ、
さらに、測温パイプ８３に対応している覗窓９３には放
射温度計１０３が設けられている。 測温孔１１１、１
１２の大きさは、筒状発熱体の熱膨張を考慮して定めら
れるが５〜３０ｍｍ、なかんずく５〜１５ｍｍの範囲が
好ましい。また、孔の形は同じ理由から丸孔よりも長孔
が好ましい。Temperature measuring holes 111, 11 are formed in a part of the cylindrical heating element 2.
2 is provided. One ends of the temperature measuring pipes 81 and 83 face the temperature measuring holes 111 and 112, respectively, and face the inner wall of the tubular heating element. A radiation thermometer 101 is provided on the viewing window 91 corresponding to the temperature measuring pipe 81. A radiation thermometer 102 is provided in the viewing window 92 corresponding to the temperature measuring pipe 82,
Further, a radiation thermometer 103 is provided on the viewing window 93 corresponding to the temperature measuring pipe 83. Temperature measuring holes 111, 1
The size of 12 is determined in consideration of the thermal expansion of the tubular heating element, but is preferably in the range of 5 to 30 mm, especially 5 to 15 mm. Also, the shape of the holes is preferably long holes rather than round holes for the same reason.
【００２２】測温パイプ８１、８３は筒状発熱体２の内
壁を炉殻１の外から見えるようになっている。従って覗
窓９１、９３に設けられた放射温度計１０１、１０３に
より筒状発熱体２の内壁の温度を測定することが出来
る。また、測温パイプ８２に対応している覗窓９２に設
けられた放射温度計１０２は、筒状発熱体２の外壁の温
度を測定することが出来る。なお、放射温度計１０２と
１０３は、筒状発熱体２の内壁と外壁の温度が経時的に
どのように変化するかを見るために設けたものである。
筒状発熱体２の内壁温度を直接測定している放射温度計
１０１の信号は、図１に示すように、加熱を制御する機
構を持つ加熱制御器２０１に伝達されるので、加熱体の
内壁温度は、その制御器２０１により一定値に保持され
る。The temperature measuring pipes 81 and 83 are arranged so that the inner wall of the cylindrical heating element 2 can be seen from the outside of the furnace shell 1. Therefore, the temperature of the inner wall of the tubular heating element 2 can be measured by the radiation thermometers 101 and 103 provided in the viewing windows 91 and 93. Further, the radiation thermometer 102 provided in the viewing window 92 corresponding to the temperature measuring pipe 82 can measure the temperature of the outer wall of the tubular heating element 2. The radiation thermometers 102 and 103 are provided to see how the temperatures of the inner wall and the outer wall of the tubular heating element 2 change with time.
Since the signal of the radiation thermometer 101 that directly measures the inner wall temperature of the tubular heating element 2 is transmitted to the heating controller 201 having a mechanism for controlling heating as shown in FIG. The temperature is kept constant by the controller 201.
【００２３】覗窓９１、９２、９３は測温パイプ８１、
８２、８３で外筒３に連なっているので筒状発熱体２が
加熱され蒸発をすると、蒸発物がその測温パイプを通っ
て覗窓に至り覗窓の中側を曇らせてしまう。そこでガス
注入口１３から、不活性ガスを測温パイプ内に送り込み
覗窓の曇りを防ぎ温度測定の正確さを確保するものであ
る。この場合、ガス注入量があまり多いことは炉殻内の
各部分に悪影響があるので、毎分１〜１０リットル、な
かんずく１〜５リットル程度が好ましい。The viewing windows 91, 92, 93 are temperature measuring pipes 81,
When the cylindrical heating element 2 is heated and evaporated because it is connected to the outer cylinder 3 by 82 and 83, the evaporate passes through the temperature measuring pipe to reach the peephole and cloud the inside of the peephole. Therefore, an inert gas is sent from the gas inlet 13 into the temperature measuring pipe to prevent the peephole from fogging and to ensure the accuracy of temperature measurement. In this case, an excessively large amount of gas injection adversely affects each portion in the furnace shell, so 1 to 10 liters per minute, preferably 1 to 5 liters per minute is preferable.
【００２４】かくして筒状発熱体の内壁の温度が正確に
制御されるので、被処理物を正確な所定の温度で熱処理
することができる。なお、直接円筒状発熱体の内壁の温
度を測定し、この測定信号に基づいて温度制御すること
は如何に重大な意味があるかを示すために行った実験結
果を表１に示している。Thus, since the temperature of the inner wall of the cylindrical heating element is accurately controlled, the object to be processed can be heat-treated at an accurate predetermined temperature. Table 1 shows the results of an experiment conducted to show how significant it is to directly measure the temperature of the inner wall of the cylindrical heating element and control the temperature based on this measurement signal.
【００２５】表１は不活性ガスとしてアルゴンガスを使
用し、雰囲気圧力を平方センチメートルあたり３Ｋｇに
設定した後、円筒内部の温度を３０００度になるように
加熱し、筒状発熱体の内壁と外壁の温度を経時的に測定
したものである。使用した発熱体は、外形５０ｍｍ、内
径３０ｍｍ、長さ６５０ｍｍの円筒状のグラファイト製
のものを用い図２の放射温度計１０２、１０３で測定し
たものである。Table 1 shows that argon gas was used as an inert gas, the atmospheric pressure was set to 3 kg per square centimeter, and then the temperature inside the cylinder was heated to 3000 ° C., and the inner wall and the outer wall of the cylindrical heating element were heated. The temperature is measured over time. The heating element used was one made of cylindrical graphite having an outer diameter of 50 mm, an inner diameter of 30 mm, and a length of 650 mm, which was measured by the radiation thermometers 102 and 103 in FIG.
【００２６】[0026]
【表１】 [Table 1]
【００２７】表１によれば、発熱体内壁の温度は一定に
た持たれている。しかしながら、加熱当初から発熱体外
壁温度は発熱体内壁温度より若干低いが、時間の経過と
ともにその温度差は拡大しており、３５０時間経過した
状態では１７０度にも達している。したがって筒状発熱
体の外壁の温度を測定し、この測定信号に基づいて筒状
発熱体の温度が一定となるように制御する場合、筒状発
熱体の内壁の温度は経時的に表１の値だけ高い値に制御
され、筒状発熱体が過加熱されて寿命が短くなるだけで
なく、糸に対する処理温度も経時的に変化するという欠
点を有する。これに対し、本発明は、筒状発熱体の内壁
の温度を測定し、この測定信号に基づいて筒状発熱体の
温度が一定となるように制御するので、筒状発熱体の手
内壁の温度は経時的に変化するということがなく一定と
なり、筒状発熱体の寿命を短くすることもなく、また、
糸に対する処理温度も経時的に安定化する。According to Table 1, the temperature of the inner wall of the heat generating body is kept constant. However, the temperature of the outer wall of the heating element is slightly lower than the temperature of the inner wall of the heating element from the beginning of heating, but the temperature difference increases with the passage of time, reaching 170 degrees after 350 hours. Therefore, when the temperature of the outer wall of the tubular heating element is measured and the temperature of the tubular heating element is controlled to be constant based on this measurement signal, the temperature of the inner wall of the tubular heating element of Table 1 changes with time. It has a drawback that not only is it controlled to a value higher than that value, the tubular heating element is overheated and the life is shortened, but also the processing temperature for the yarn changes with time. On the other hand, the present invention measures the temperature of the inner wall of the tubular heating element and controls the temperature of the tubular heating element to be constant based on this measurement signal. The temperature does not change over time and remains constant, without shortening the life of the cylindrical heating element.
The processing temperature for the yarn also stabilizes over time.
【００２８】[0028]
（１）本発明は、炭素繊維を、筒状発熱体内へ連続的に
通過せしめながら加圧不活性ガス雰囲気中、２０００度
以上の温度で焼成する黒鉛化繊維の製造方法において、
前記筒状発熱体には筒体の外側から内側へ貫通する測温
孔を設け、前記測温手段で前記筒状発熱体の測温孔を通
して筒状発熱体の内周面の温度を測定し、前記温度測定
信号に基づいて前記筒状発熱体の温度を前記温度制御手
段で制御しながら焼成をする黒鉛化繊維の製造方法とし
たので、焼成温度が経時的に安定し、均質な炭素繊維を
得ることができるという優れた効果を奏する。(1) The present invention provides a method for producing graphitized fiber, wherein carbon fiber is fired at a temperature of 2000 ° C. or higher in a pressurized inert gas atmosphere while continuously passing carbon fiber into a tubular heating element,
The cylindrical heating element is provided with a temperature measuring hole penetrating from the outside to the inside of the cylindrical heating element, and the temperature measuring means measures the temperature of the inner peripheral surface of the cylindrical heating element through the temperature measuring hole of the cylindrical heating element. Since the method for producing the graphitized fiber is carried out while controlling the temperature of the tubular heating element on the basis of the temperature measurement signal while controlling the temperature by the temperature control means, the firing temperature is stable over time, and the carbon fiber is homogeneous. There is an excellent effect that can be obtained.
【００２９】（２）また、本発明は、黒鉛または炭素か
らなり内側を繊維の処理域とする筒状発熱体と、前記筒
状発熱体の両側に設けられた電極と、前記筒状発熱体お
よび前記電極を囲むと共に前記筒状発熱体の内部に不活
性ガスを供給するためのガス注入口と繊維の入口および
出口とを有する炉殻と、前記繊維の入口および出口に接
続され前記不活性ガスをシールするシール部と、前記筒
状発熱体の温度を炉殻に形成された窓を通して測定する
測温手段と、前記測温手段からの信号に基づき前記電極
を経て前記筒状発熱体に流れる電流を制御し発熱体の温
度を調節する温度制御手段とを備えた黒鉛化繊維の製造
装置において、前記筒状発熱体は、筒体の外側から内側
へ貫通する測温孔が設けられ、かつ、前記測温手段は、
前記測温孔を通して前記筒状発熱体の内周面の温度を測
定する放射温度計である黒鉛化繊維の製造装置としたの
で、発熱体が過加熱されることがなく、その結果発熱体
の寿命の延長を図ることができ、また、発熱体の交換周
期の延長により装置の稼働率を高めることができるとい
う優れた効果を奏する。(2) Further, according to the present invention, a tubular heating element made of graphite or carbon and having a fiber processing region inside thereof, electrodes provided on both sides of the tubular heating element, and the tubular heating element. And a furnace shell having a gas inlet for supplying an inert gas to the inside of the tubular heating element and an inlet and an outlet for fibers, and the inert gas connected to the inlet and the outlet for the fibers. A sealing portion for sealing gas, a temperature measuring means for measuring the temperature of the tubular heating element through a window formed in the furnace shell, and a tubular heating element via the electrode based on a signal from the temperature measuring means. In the manufacturing apparatus of the graphitized fiber having a temperature control means for controlling the flowing current and adjusting the temperature of the heating element, the tubular heating element is provided with a temperature measuring hole penetrating from the outer side to the inner side of the tubular body, And the temperature measuring means,
Since the apparatus for producing graphitized fiber is a radiation thermometer that measures the temperature of the inner peripheral surface of the cylindrical heating element through the temperature measuring hole, the heating element is not overheated, and as a result, This has an excellent effect that the life can be extended and the operating rate of the device can be increased by extending the replacement period of the heating element.
【００３０】[0030]
【図１】は本発明に係る黒鉛化装置の中心部分における
正面断面図である。FIG. 1 is a front sectional view of a central portion of a graphitizing apparatus according to the present invention.
【図２】は図１のＡ−Ａ´断面の断面図である。FIG. 2 is a cross-sectional view taken along the line AA ′ of FIG.
【図３】は在来の黒鉛化装置の中心部分における正面断
面図である。FIG. 3 is a front sectional view of a central portion of a conventional graphitizer.
【図４】は図３のＣ−Ｃ´断面の断面図である。4 is a cross-sectional view taken along the line CC ′ of FIG.
【００３１】[0031]
１：炉殻 ２：発熱体 ３：外筒 ４：電極 ５：断熱材 ６：スペーサー ７：シール ８１：測温パイプ ８２：測温パイプ ８３：測温パイプ ９１：覗窓 ９２：覗窓 ９３：覗窓 １０１：放射温度計 １０２：放射温度計 １０３：放射温度計 １１１：測温孔 １１２：測温孔 １２：ガス注入口 １３：ガス注入口 １４：糸 １５：圧力検出器 １６：圧力調節弁 １７：取付部 １８：取付部 １９：取付部 ２０１：温度制御器 ２０２：温度指示記録計 ２０３：温度指示記録計 ２１：ニップローラ ２２：ニップローラ ３１：スペーサリング 1: Furnace shell 2: Heating element 3: Outer cylinder 4: Electrode 5: Heat insulating material 6: Spacer 7: Seal 81: Temperature measuring pipe 82: Temperature measuring pipe 83: Temperature measuring pipe 91: Viewing window 92: Looking window 93: Viewing window 101: Radiation thermometer 102: Radiation thermometer 103: Radiation thermometer 111: Temperature measurement hole 112: Temperature measurement hole 12: Gas injection port 13: Gas injection port 14: Thread 15: Pressure detector 16: Pressure control valve 17: Mounting part 18: Mounting part 19: Mounting part 201: Temperature controller 202: Temperature indicator recorder 203: Temperature indicator recorder 21: Nip roller 22: Nip roller 31: Spacer ring
Claims (3)
域とする筒状発熱体と、前記筒状発熱体の両側に設けら
れた電極と、前記筒状発熱体および前記電極を囲むと共
に前記筒状発熱体の内部に不活性ガスを供給するための
ガス注入口と繊維の入口および出口とを有する炉殻と、
前記繊維の入口および出口に接続され前記不活性ガスを
シールするシール部と、前記筒状発熱体の温度を炉殻に
形成された窓を通して測定する測温手段と、前記測温手
段からの信号に基づき前記電極を経て前記筒状発熱体に
流れる電流を制御し発熱体の温度を調節する温度制御手
段とを備えた加熱装置を用い、炭素繊維を、前記筒状発
熱体内へ連続的に通過せしめながら加圧不活性ガス雰囲
気中、２０００℃以上の温度で焼成する黒鉛化繊維の製
造方法において、前記筒状発熱体には筒体の外側から内
側へ貫通する測温孔を設け、前記測温手段で前記筒状発
熱体の測温孔を通して筒状発熱体の内周面の温度を測定
し、前記温度測定信号に基づいて前記筒状発熱体の温度
を前記温度制御手段で制御しながら前記焼成をすること
を特徴とする黒鉛化繊維の製造方法。1. A tubular heating element made of graphite or carbon, the inside of which is a treatment area for fibers, electrodes provided on both sides of the tubular heating element, and surrounding the tubular heating element and the electrode. A furnace shell having a gas inlet for supplying an inert gas to the inside of the tubular heating element, and an inlet and an outlet for fibers,
A seal portion connected to the inlet and the outlet of the fiber to seal the inert gas, a temperature measuring means for measuring the temperature of the tubular heating element through a window formed in the furnace shell, and a signal from the temperature measuring means. Based on the above, using a heating device equipped with a temperature control means for controlling the current flowing through the tubular heating element through the electrode and adjusting the temperature of the heating element, the carbon fiber is continuously passed into the tubular heating element. In the method for producing graphitized fiber, which is calcined at a temperature of 2000 ° C. or higher in a pressurized inert gas atmosphere, the tubular heating element is provided with a temperature measuring hole penetrating from the outer side to the inner side of the tubular body. While measuring the temperature of the inner peripheral surface of the tubular heating element through the temperature measuring hole of the tubular heating element by the temperature means, while controlling the temperature of the tubular heating element by the temperature control means based on the temperature measurement signal. Graphite characterized by being fired Method for producing a fiber.
域とする筒状発熱体と、前記筒状発熱体の両側に設けら
れた電極と、前記筒状発熱体および前記電極を囲むと共
に前記筒状発熱体の内部に不活性ガスを供給するための
ガス注入口と繊維の入口および出口とを有する炉殻と、
前記繊維の入口および出口に接続され前記不活性ガスを
シールするシール部と、前記筒状発熱体の温度を炉殻に
形成された窓を通して測定する測温手段と、前記測温手
段からの信号に基づき前記電極を経て前記筒状発熱体に
流れる電流を制御し発熱体の温度を調節する温度制御手
段とを備えた黒鉛化繊維の製造装置において、前記筒状
発熱体は、筒体の外側から内側へ貫通する測温孔が設け
られ、かつ、前記測温手段は、前記測温孔を通して前記
筒状発熱体の内周面の温度を測定する放射温度計である
ことを特徴とする黒鉛化繊維の製造装置。2. A cylindrical heating element made of graphite or carbon, the inside of which is a treatment area for fibers, electrodes provided on both sides of the cylindrical heating element, and surrounding the cylindrical heating element and the electrode. A furnace shell having a gas inlet for supplying an inert gas to the inside of the tubular heating element, and an inlet and an outlet for fibers,
A seal portion connected to the inlet and the outlet of the fiber to seal the inert gas, a temperature measuring means for measuring the temperature of the tubular heating element through a window formed in the furnace shell, and a signal from the temperature measuring means. Based on the above, in the apparatus for producing graphitized fiber, which comprises a temperature control means for controlling a current flowing through the tubular heating element through the electrode to adjust the temperature of the heating element, the tubular heating element is outside the tubular body. From the inside, and the temperature measuring means is a radiation thermometer for measuring the temperature of the inner peripheral surface of the cylindrical heating element through the temperature measuring hole. Fiber manufacturing equipment.
て、前記発熱体は筒体の外側から内側へ貫通する孔が形
成されていることを特徴とする筒状発熱体。3. A tubular heating element made of graphite or carbon, wherein the heating element has a hole penetrating from the outside to the inside of the tubular body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4274823A JPH06108317A (en) | 1992-09-21 | 1992-09-21 | Production of graphitized fiber and apparatus for production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4274823A JPH06108317A (en) | 1992-09-21 | 1992-09-21 | Production of graphitized fiber and apparatus for production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06108317A true JPH06108317A (en) | 1994-04-19 |
Family
ID=17547072
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4274823A Pending JPH06108317A (en) | 1992-09-21 | 1992-09-21 | Production of graphitized fiber and apparatus for production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06108317A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100740448B1 (en) * | 2003-07-28 | 2007-07-19 | 모토로라 인코포레이티드 | communication system |
| CN106914498A (en) * | 2017-03-29 | 2017-07-04 | 金堆城钼业股份有限公司 | A kind of heater and heating means for rolling molybdenum alloy pipe |
| WO2019122252A1 (en) * | 2017-12-20 | 2019-06-27 | Drever International Sa | Kiln comprising a control unit associated with the thermal inertia properties of constitutive elements |
| WO2020022724A1 (en) * | 2018-07-23 | 2020-01-30 | 주식회사 엘지화학 | Carbon fiber carbonizing apparatus using microwave |
| US11459673B2 (en) | 2018-07-23 | 2022-10-04 | Lg Chem, Ltd. | Carbon fiber carbonization apparatus using microwave |
-
1992
- 1992-09-21 JP JP4274823A patent/JPH06108317A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100740448B1 (en) * | 2003-07-28 | 2007-07-19 | 모토로라 인코포레이티드 | communication system |
| CN106914498A (en) * | 2017-03-29 | 2017-07-04 | 金堆城钼业股份有限公司 | A kind of heater and heating means for rolling molybdenum alloy pipe |
| CN106914498B (en) * | 2017-03-29 | 2018-12-14 | 金堆城钼业股份有限公司 | A kind of heating device and heating means for rolling molybdenum alloy pipe |
| WO2019122252A1 (en) * | 2017-12-20 | 2019-06-27 | Drever International Sa | Kiln comprising a control unit associated with the thermal inertia properties of constitutive elements |
| US11905572B2 (en) | 2017-12-20 | 2024-02-20 | Drever International Sa | Kiln comprising a control unit associated with the thermal inertia properties of constitutive elements |
| WO2020022724A1 (en) * | 2018-07-23 | 2020-01-30 | 주식회사 엘지화학 | Carbon fiber carbonizing apparatus using microwave |
| US11459673B2 (en) | 2018-07-23 | 2022-10-04 | Lg Chem, Ltd. | Carbon fiber carbonization apparatus using microwave |
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