JP5037977B2 - Flameproofing furnace and method for producing flameproofed fiber - Google Patents

Flameproofing furnace and method for producing flameproofed fiber Download PDF

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JP5037977B2
JP5037977B2 JP2007068769A JP2007068769A JP5037977B2 JP 5037977 B2 JP5037977 B2 JP 5037977B2 JP 2007068769 A JP2007068769 A JP 2007068769A JP 2007068769 A JP2007068769 A JP 2007068769A JP 5037977 B2 JP5037977 B2 JP 5037977B2
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hot air
flameproofing
wind speed
furnace
heat treatment
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JP2008231589A (en
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斉 友部
篤志 川村
伸之 山本
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Mitsubishi Chemical Corp
Mitsubishi Rayon Co Ltd
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Mitsubishi Rayon Co Ltd
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本発明は、前駆体繊維に耐炎化処理を施すための耐炎化炉及び耐炎化繊維の製造方法に関する。   The present invention relates to a flameproofing furnace for applying flameproofing treatment to a precursor fiber and a method for producing flameproofed fiber.

炭素繊維、特にポリアクリロニトリル系炭素繊維は、その引張強度が500kg/mm以上、伸度2%以上と極めて高い強度を有するため、航空や宇宙用素材を始めとして、多方面で使用されている。
炭素繊維は、例えばポリアクリロニトリル系繊維等の前駆体繊維束(プリカーサ)を、耐炎化炉内を循環する200〜350℃程度の比較的低温の酸化性雰囲気の熱風(以下、単に熱風と略する。)によって焼成(耐炎化処理)して耐炎化繊維束とし、得られた耐炎化繊維束を1,000℃程度以上の高温の不活性雰囲気中で焼成(炭素化処理)することで製造されている。
Carbon fiber, especially polyacrylonitrile-based carbon fiber, has an extremely high strength of tensile strength of 500 kg / mm 2 or more and elongation of 2% or more, so it is used in various fields including aviation and space materials. .
The carbon fiber is, for example, a precursor fiber bundle (precursor) such as polyacrylonitrile-based fiber that circulates in the flameproofing furnace in a relatively low-temperature oxidizing atmosphere of about 200 to 350 ° C. (hereinafter simply referred to as hot air). )) To produce a flame-resistant fiber bundle, and the obtained flame-resistant fiber bundle is fired (carbonization treatment) in an inert atmosphere at a high temperature of about 1,000 ° C. or more. ing.

耐炎化炉に送入された前駆体繊維束は、その熱処理室内を流れる熱風によって徐々に耐炎化処理される。その際、前駆体繊維束自体が耐炎化反応による発熱を生じ、特に初期の走行域において激しく発熱する。従って、初期の走行域の前駆体繊維が熱処理室内で過度の高温に晒されると、耐炎化反応が急激に進行して、発火や糸切れを生じやすい。初期の走行域での発火や糸切れを低減するには、熱処理室内を流れる熱風の温度を低く抑える必要がある。しかしながら、熱風の温度を低くすると、後期の走行域の耐炎化処理の進行が遅くなるため、これが耐炎化繊維束の生産性を低下させる要因の一つとなっていた。   The precursor fiber bundle sent to the flameproofing furnace is gradually flameproofed by the hot air flowing through the heat treatment chamber. At that time, the precursor fiber bundle itself generates heat due to the flameproofing reaction, and generates intense heat particularly in the initial running region. Therefore, when the precursor fiber in the initial traveling region is exposed to an excessively high temperature in the heat treatment chamber, the flameproofing reaction proceeds rapidly, and ignition and yarn breakage are likely to occur. In order to reduce ignition and yarn breakage in the initial running area, it is necessary to keep the temperature of the hot air flowing in the heat treatment chamber low. However, when the temperature of the hot air is lowered, the progress of the flameproofing treatment in the later traveling area is delayed, and this is one of the factors that reduce the productivity of the flameproofed fiber bundle.

これに対し、例えば特許文献1では、耐炎化炉の熱処理室内を複数の熱処理区画に区分し、各熱処理区画の温度を、耐炎化処理の進行に合わせて個別に設定できるようにした耐炎化炉が提案されている。また、例えば特許文献2では、初期の走行域の温度を後期の走行域の温度より低くするために、熱風の熱風吹出口に外気、水、その他の冷媒による冷却手段を備えた耐炎化炉が提案されている。
特開平10−237723号公報 特開2004−197239号公報
On the other hand, for example, in Patent Document 1, the heat treatment chamber of the flameproofing furnace is divided into a plurality of heat treatment sections, and the temperature of each heat treatment section can be set individually according to the progress of the flameproofing process. Has been proposed. Further, for example, in Patent Document 2, there is provided a flameproof furnace provided with a cooling means using hot air, hot water or other refrigerant at the hot air outlet of the hot air in order to make the temperature of the initial traveling region lower than the temperature of the latter traveling region. Proposed.
JP-A-10-237723 JP 2004-197239 A

しかしながら、特許文献1に記載の耐炎化炉は、前駆体繊維が走行する順に各熱処理区画の温度を上昇させているため、熱処理室に出入りを繰り返しながら走行する前駆体繊維にとって、異なる熱処理区画に送入される度に急激な温度上昇が加わることになり、得られる耐炎化繊維束の品質低下を招く恐れがある。
また、特許文献2に記載の耐炎化炉は、冷却手段の周囲温度が低下するために、熱風中に漂うタール成分等の分解生成物が凝集し、冷却手段を始めとした耐炎化炉内の各所に付着してしまう恐れがある。これらの凝集物が冷却手段に付着すると、冷却能力が低下し、安全運転に支障をきたす。また、凝集物が耐炎化処理中の前駆体繊維に付着すると、糸切れ等の品質低下を招きやすい。
本発明は、前記事情に鑑みてなされたものであって、耐炎化繊維の生産性及び品質の向上が可能な耐炎化炉及び耐炎化繊維の製造方法を目的とする。
However, the flameproofing furnace described in Patent Document 1 raises the temperature of each heat treatment section in the order in which the precursor fibers travel, so that the precursor fibers that travel while repeatedly entering and exiting the heat treatment chamber have different heat treatment sections. Each time it is fed, a rapid temperature increase is applied, and there is a risk of degrading the quality of the resulting flameproof fiber bundle.
Further, in the flameproofing furnace described in Patent Document 2, since the ambient temperature of the cooling means is lowered, decomposition products such as tar components floating in the hot air are aggregated, and the inside of the flameproofing furnace including the cooling means is aggregated. There is a risk of sticking to various places. If these agglomerates adhere to the cooling means, the cooling capacity is lowered, which hinders safe driving. Further, when the aggregates adhere to the precursor fiber during the flameproofing treatment, it is easy to cause quality degradation such as yarn breakage.
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a flame resistant furnace and a flame resistant fiber manufacturing method capable of improving the productivity and quality of the flame resistant fiber.

前記の課題を達成するために、本発明は以下の構成を採用した。
[1] 前駆体繊維が送入送出を繰り返して内部を複数回走行する熱処理室と、前駆体繊維が走行するそれぞれの走行域に熱風を吹き込む加熱手段と、初期の走行域の風速を後期の走行域の風速より速くする風速制御手段とを備える耐炎化炉。
[2] 風速制御手段が、加熱手段に備えられている[1]に記載の耐炎化炉。
[3] 初期の走行域と後期の走行域との間に仕切り板が設けられている[1]または[2]に記載の耐炎化炉。
[4] [1]〜[3]のいずれかに記載の耐炎化炉に前駆体繊維を送入する耐炎化繊維の製造方法。
In order to achieve the above object, the present invention adopts the following configuration.
[1] A heat treatment chamber in which the precursor fiber travels in and out a plurality of times by repeatedly sending and delivering, heating means for blowing hot air into each traveling region in which the precursor fiber travels, and the wind speed in the initial traveling region in the latter period A flameproofing furnace comprising wind speed control means for making the wind speed higher than the wind speed in a traveling area.
[2] The flameproof furnace according to [1], wherein the wind speed control means is provided in the heating means.
[3] The flameproofing furnace according to [1] or [2], wherein a partition plate is provided between the initial traveling area and the latter traveling area.
[4] A method for producing a flame resistant fiber, wherein the precursor fiber is fed into the flame resistant furnace according to any one of [1] to [3].

本発明の耐炎化炉及び耐炎化繊維の製造方法を用いれば、耐炎化繊維の生産性及び品質の向上が実現できる。   By using the flameproofing furnace and the flameproofing fiber manufacturing method of the present invention, it is possible to improve the productivity and quality of the flameproofing fiber.

本発明の耐炎化炉について、図1に示す熱風循環方式の耐炎化炉10を用いて説明する。
耐炎化炉10は、前駆体繊維束1が送入送出を繰り返して内部を複数回走行する熱処理室11と、前駆体繊維束1が走行するそれぞれの走行域に熱風を吹き込む加熱手段と、初期の走行域の風速が後期の走行域の風速より速くなる風速制御手段とを備えている。
加熱手段は、熱処理室11内に熱風を吹き込む複数の熱風吹出口13と、熱風を熱処理室11外に排出する複数の熱風排出口14と、各熱風吹出口13と各熱風排出口14とを繋ぐ循環路17と、循環路17の途中に設けられた加熱器15と、送風器16とで構成されている。
各熱風吹出口13から熱処理室11内に吹き込まれた熱風は、熱処理室11内を前駆体繊維束1の走行域に沿いながら熱風排出口14側に向かって流れる。次いで、熱風排出口14から熱処理室11外に排出された熱風は循環路17に導かれ、循環路17に設けられた加熱器15で加温され、さらに送風器16によって風速を制御された後に、再び各熱風吹出口13から前駆体繊維の複数の各走行域に吹き込まれる。吹き込まれた熱風は、熱処理室11内を矢印で示すように前駆体繊維束1の走行域に沿って流れた後、再び熱風排出口14から排出されることで、耐炎化炉10の熱風循環は繰り返されている。このような熱風循環方式の耐炎化炉10は、前駆体繊維束に酸素と熱を適度に供給でき、かつ高温に熱した酸化性雰囲気を繰り返し使うため、熱効率がよい。なお、図示しないが、熱風吹出口13及び熱風排出口14は、紙面に対して垂直な方向、すなわちシート状をなす前駆体繊維束1のシート幅方向に渡って配置されている。
The flameproofing furnace of the present invention will be described using a hot air circulation type flameproofing furnace 10 shown in FIG.
The flameproofing furnace 10 includes a heat treatment chamber 11 in which the precursor fiber bundle 1 travels in and out a plurality of times by repeatedly sending and feeding, heating means for blowing hot air into each traveling region in which the precursor fiber bundle 1 travels, Wind speed control means for speeding up the wind speed in the travel area of the vehicle is higher than the wind speed in the later travel area.
The heating means includes a plurality of hot air outlets 13 for blowing hot air into the heat treatment chamber 11, a plurality of hot air outlets 14 for discharging hot air to the outside of the heat treatment chamber 11, each hot air outlet 13, and each hot air outlet 14. It comprises a circulation path 17 to be connected, a heater 15 provided in the middle of the circulation path 17, and a blower 16.
Hot air blown into the heat treatment chamber 11 from each hot air outlet 13 flows in the heat treatment chamber 11 toward the hot air outlet 14 side along the traveling area of the precursor fiber bundle 1. Next, the hot air discharged from the hot air discharge port 14 to the outside of the heat treatment chamber 11 is guided to the circulation path 17, heated by the heater 15 provided in the circulation path 17, and further, the wind speed is controlled by the blower 16. Then, each hot air blowing port 13 is blown again into each of the plurality of traveling regions of the precursor fiber. The blown hot air flows in the heat treatment chamber 11 along the traveling area of the precursor fiber bundle 1 as indicated by an arrow, and is then discharged from the hot air discharge port 14 again, thereby circulating hot air in the flameproofing furnace 10. Has been repeated. Such a hot air circulation type flameproofing furnace 10 can supply oxygen and heat appropriately to the precursor fiber bundle, and uses an oxidizing atmosphere heated to a high temperature repeatedly, so that the thermal efficiency is good. Although not shown, the hot air outlet 13 and the hot air outlet 14 are arranged in a direction perpendicular to the paper surface, that is, in the sheet width direction of the precursor fiber bundle 1 having a sheet shape.

前駆体繊維束1は、耐炎化炉10の熱処理室11側壁に設けたスリットから熱処理室11内に送入され、熱処理室11内を直線的に走行した後、対面の側壁のスリットから熱処理室11外に一旦送出され、熱処理室11外の側壁に設けられたガイドロール12によって折り返され、再び熱処理室11内に送入される。このように、前駆体繊維束1は複数のガイドロール12によって走行方向を複数回折り返すことで、熱処理室11内への送入送出を複数回繰り返しながら、熱処理室11内を全体として図1の下から上に向けて移動する。
前駆体繊維束1は、熱処理室11内を走行している間に、熱風吹出口13から吹き出される200〜350℃程度の熱風によって耐炎化処理されて耐炎化繊維束となる。なお、図示しないが、前駆体繊維束1は紙面に対して垂直な方向に複数本並行するように引き揃えられた前駆体繊維束の繊維束群を形成しており、幅広のシート状の形態、もしくは一定間隔で前駆体繊維束が配列した形態を有している。
The precursor fiber bundle 1 is fed into the heat treatment chamber 11 from the slit provided on the side wall of the heat treatment chamber 11 of the flameproofing furnace 10, travels linearly in the heat treatment chamber 11, and then passes through the slit on the opposite side wall. 11 is once sent out, is turned back by a guide roll 12 provided on the side wall outside the heat treatment chamber 11, and is again fed into the heat treatment chamber 11. As described above, the precursor fiber bundle 1 is bent in a plurality of directions by a plurality of guide rolls 12 so that the inside of the heat treatment chamber 11 as a whole is repeated as shown in FIG. Move from bottom to top.
The precursor fiber bundle 1 is flameproofed by hot air of about 200 to 350 ° C. blown from the hot air outlet 13 while traveling in the heat treatment chamber 11 to become a flameproof fiber bundle. Although not shown, the precursor fiber bundle 1 forms a fiber bundle group of precursor fiber bundles aligned so as to be parallel to each other in a direction perpendicular to the paper surface, and has a wide sheet-like form. Alternatively, the precursor fiber bundles are arranged at regular intervals.

熱風吹出口13には、その吹き出し面に多孔板等の抵抗体及びハニカム等の整流部材を配して圧力損失を持たせ、熱処理室11内に吹き込む熱風の整流を行うことが好ましい。
熱風排出口14は、熱風吹出口13と同様に、その排出面に多孔板等の抵抗体を配して圧力損失を持たせてもよいが、持たせなくてもよく、必要に応じて適宜決定される。なお、各熱風吹出口13は、耐炎化炉10の設備費を低減するために、加熱器15及び送風器16を共通とすることもできるが、共通としていなくてもよい。
加熱器15は、熱風を所望の温度に加熱できる性能を有していれば特に限定されないが、例えば電気ヒーター等が用いられる。
送風器16は、所望の性能を有していれば特に限定されないが、例えば軸流ファン等が用いられる。
循環路17には、必要に応じて、熱風中のタール等の異物を漉し取る異物除去手段(不図示)を設けていてもよい。異物除去手段としては特に制限されないが、例えば金網やパンチングプレート等の多孔板が挙げられる。また、熱風中の一部を排気する排気ライン(不図示)もしくは清浄な空気を供給する供給ライン(不図示)を設けて、熱処理室11内のガスの交換を促進させてもよい。
The hot air outlet 13 is preferably provided with a resistor such as a perforated plate and a rectifying member such as a honeycomb on the blowing surface to give a pressure loss to rectify the hot air blown into the heat treatment chamber 11.
Similarly to the hot air outlet 13, the hot air outlet 14 may be provided with a pressure loss by arranging a resistor such as a perforated plate on the discharge surface, but it may not be provided and may be appropriately changed according to need. It is determined. In addition, in order to reduce the installation cost of the flameproofing furnace 10, each hot air blower outlet 13 can make the heater 15 and the air blower 16 common, but it does not need to be made common.
Although the heater 15 will not be specifically limited if it has the performance which can heat a hot air to desired temperature, For example, an electric heater etc. are used.
The blower 16 is not particularly limited as long as it has a desired performance. For example, an axial fan or the like is used.
The circulation path 17 may be provided with foreign matter removing means (not shown) for scrubbing foreign matters such as tar in the hot air as necessary. Although it does not restrict | limit especially as a foreign material removal means, For example, perforated plates, such as a wire net and a punching plate, are mentioned. Further, an exhaust line (not shown) for exhausting a part of the hot air or a supply line (not shown) for supplying clean air may be provided to promote the exchange of the gas in the heat treatment chamber 11.

耐炎化処理が進行した後期の走行域の前駆体繊維束1は、発熱量が少ないので発火や糸切れを起こしにくいが、初期の走行域の前駆体繊維束1は、耐炎化反応に伴う発熱量が多い。従って、前駆体繊維束1が蓄熱して発火や糸切れを生じないように、初期の走行域の前駆体繊維束1から発せられる熱は、速やかに除熱される必要がある。
ここで初期の走行域とは、前駆体繊維束1の耐炎化初期の走行域を表す。初期の走行域は、熱処理室の大きさ、両端のガイドロール12の間隔、熱風の温度、前駆体繊維の耐炎化の進行度合いによって左右されるが、例えば図1の耐炎化炉10においては、およそ熱処理室11内の下側1/3程度の走行域(前駆体繊維束1の1往復分の走行域)が初期の走行域の目安である。後期の走行域は、前駆体繊維束1の耐炎化が進行した耐炎化後期の走行域のことを表し、熱処理室11内における初期の走行域以外の走行域が後期の走行域に該当する。
The precursor fiber bundle 1 in the later traveling region where the flameproofing process has progressed has a small amount of heat generation, and thus is unlikely to ignite or break the yarn, but the precursor fiber bundle 1 in the initial traveling region generates heat due to the flameproofing reaction. Large amount. Therefore, heat generated from the precursor fiber bundle 1 in the initial travel region needs to be quickly removed so that the precursor fiber bundle 1 does not accumulate heat and cause ignition or yarn breakage.
Here, the initial traveling region represents the traveling region in the initial stage of flame resistance of the precursor fiber bundle 1. The initial traveling area depends on the size of the heat treatment chamber, the distance between the guide rolls 12 at both ends, the temperature of the hot air, and the progress of the flame resistance of the precursor fiber. For example, in the flame resistance furnace 10 of FIG. A traveling range of about 1/3 of the lower side in the heat treatment chamber 11 (a traveling region for one reciprocation of the precursor fiber bundle 1) is an indication of the initial traveling region. The latter traveling region represents a traveling region in the later flame-proofing in which the precursor fiber bundle 1 has been flame-resistant, and a traveling region other than the initial traveling region in the heat treatment chamber 11 corresponds to the latter traveling region.

本発明の耐炎化炉10は、初期の走行域の風速が後期の走行域の風速より速くなる風速制御手段を備えている。初期の走行域の風速を後期の走行域の風速より速めることで、初期の走行域の前駆体繊維束1の発熱を速やかに除熱することができる。従って、本発明の熱処理炉10は、熱処理室11内が一様に同じ温度であったとしても、初期の走行域の除熱効果を高めることができる。ゆえに、本発明の耐炎化炉10は、熱処理室11全体をより高い温度に設定して、前駆体繊維束1の耐炎化反応を早めることができる。これにより、耐炎化処理の時間を短縮でき、生産性の向上を図ることができる。初期の走行域の風速を後期の走行域の風速に比べてどの程度速めるかは、前駆体繊維束の種類、太さ、走行速度、走行域の段数、熱処理室11内の温度等によっても異なるが、後期の走行域の風速より、少なくとも1.2倍に風速を速めるのが好ましく、1.5倍〜2.5倍がより好ましい。   The flameproofing furnace 10 of the present invention is provided with a wind speed control means that makes the wind speed in the initial travel area faster than the wind speed in the later travel area. By making the wind speed in the initial travel area faster than the wind speed in the later travel area, the heat generation of the precursor fiber bundle 1 in the initial travel area can be quickly removed. Therefore, the heat treatment furnace 10 of the present invention can enhance the heat removal effect in the initial traveling region even if the heat treatment chamber 11 is uniformly at the same temperature. Therefore, the flameproofing furnace 10 of the present invention can accelerate the flameproofing reaction of the precursor fiber bundle 1 by setting the entire heat treatment chamber 11 to a higher temperature. Thereby, the time of a flameproofing process can be shortened and productivity can be improved. The extent to which the wind speed in the initial travel area is increased compared with the wind speed in the later travel area depends on the type of precursor fiber bundle, the thickness, the travel speed, the number of stages in the travel area, the temperature in the heat treatment chamber 11, and the like. However, it is preferable to increase the wind speed at least 1.2 times, and more preferably 1.5 times to 2.5 times the wind speed in the late driving region.

本発明の耐炎化炉10は、風速制御手段が加熱手段に備えられていることが好ましい。例えば初期の走行域に熱風を吹き込む熱風吹出口13aの吹き出し面に配した多孔板の開孔率を、熱風吹出口13bのそれより大きくしてやれば、熱風吹出口13aの圧力損失を、熱風吹出口13bのそれより低減することができる。圧力損失が低減されると、熱風吹出口13aからの熱風の吹き込み量が増えるため、初期の走行域の風速を後期の走行域のそれより速めることができる。多孔板の開孔率の変更による風速制御は、多孔板の交換のみで済むため、すでに設置済みの耐炎化炉にも大掛かりな改造無しに適用可能である。   In the flameproofing furnace 10 of the present invention, the wind speed control means is preferably provided in the heating means. For example, if the aperture ratio of the perforated plate arranged on the blowing surface of the hot air outlet 13a that blows hot air into the initial traveling area is made larger than that of the hot air outlet 13b, the pressure loss of the hot air outlet 13a is reduced to the hot air outlet. It can be reduced from that of 13b. When the pressure loss is reduced, the amount of hot air blown from the hot air outlet 13a increases, so that the wind speed in the initial travel area can be made faster than that in the later travel area. Since the wind speed control by changing the aperture ratio of the perforated plate can be performed only by replacing the perforated plate, it can be applied to an already installed flameproof furnace without any major modification.

熱風排出口14の排出面にも、熱風吹出口13と同様に、熱風排出口14a及び熱風排出口14bの排出面に開孔率を変えた多孔板等の抵抗体を配して、吸い込み速度に変化を持たせるのが好ましい。熱風吹出口13aの吹き込み風速と熱風排出口14aの排出速度を速く、また、熱風吹出口13b吹き込み速度と熱風排出口14bの排出速度を遅くすることで、初期の走行域及び後期の走行域の熱風の流れを、よりスムーズにすることができる。   Similarly to the hot air outlet 13, the discharge surface of the hot air outlet 14 is provided with a resistor such as a perforated plate having a different opening ratio on the discharge surfaces of the hot air outlet 14a and the hot air outlet 14b. It is preferable to have a change in. By increasing the blowing air speed of the hot air outlet 13a and the discharging speed of the hot air outlet 14a, and by reducing the blowing speed of the hot air outlet 13b and the discharging speed of the hot air outlet 14b, the initial traveling area and the latter traveling area The flow of hot air can be made smoother.

加熱手段に好ましく設置される風速制御手段としては、前述の例示の他にも、例えば風速制御用ダンパー(不図示)を熱風吹出口13a及び、または熱風吹出口13bに設置することが挙げられる。熱風吹出口13aに設置された風速制御用ダンパーの開閉度合いを、熱風吹出口13bに設置されたそれよりも大きくすることで、初期の走行域の風速を後期の走行域のそれよりも速くすることができる。なお、風速制御用ダンパーは、予め、所望の風速が得られるようにその開閉度合いを固定していてもよいが、熱処理室11外に設けた開閉制御器(不図示)等によって、その開閉度合いを耐炎化炉の稼働中でも可変できるようにしてもよい。なお、風速制御用ダンパーは、熱風吹出口13a及び、または熱風吹出口13bの吹き出し面の外側に設けてもよく、熱風吹出口13a及び、または熱風吹出口13bの内部に設けてもよく、必要に応じて適宜決定される。   As a wind speed control means preferably installed in the heating means, in addition to the above-described examples, for example, a wind speed control damper (not shown) may be installed in the hot air outlet 13a and / or the hot air outlet 13b. By making the opening / closing degree of the wind speed control damper installed in the hot air outlet 13a larger than that installed in the hot air outlet 13b, the wind speed in the initial traveling area is made faster than that in the latter traveling area. be able to. The damper for wind speed control may be fixed in advance so that a desired wind speed can be obtained, but the degree of opening / closing is controlled by an opening / closing controller (not shown) provided outside the heat treatment chamber 11. May be variable while the flameproofing furnace is in operation. The wind speed control damper may be provided outside the blowing surface of the hot air outlet 13a and / or the hot air outlet 13b, or may be provided inside the hot air outlet 13a and / or the hot air outlet 13b. It is determined appropriately according to

加熱手段に設置される風速制御手段としては、前述の例示の他にも、例えば分岐路17aの内寸の断面積を、熱風吹出口13aに繋がれる分岐路17aと、熱風吹出口13bのそれとで差を持たせることによってもよい。具体的には、熱風吹出口13aに繋がる分岐路17a内の断面積を、熱風吹出口13bに繋がるそれよりも広くすることで、熱風吹出口13aに対して、より多くの熱風が流すことができる。これにより、初期の走行域の風速を後期の走行域の風速より速めることができる。熱風吹出口13a及び熱風吹出口13bに繋がる分岐路17a内の断面積に、どの程度の断面積差を付けるかは、耐炎化炉の規模や熱風流量などによって適宜決定される。
本発明の耐炎化炉10は、これら風速制御手段を組み合わせて用いてもよい。また、これら風速制御手段は、熱風排出口14側にも同様に設けられていてもよい。
本発明の耐炎化炉10は、前述のような加熱手段に設けた風速制御手段以外にも、例えば熱処理室11内の初期の走行域に、送風器(不図示)等の風速制御手段を備えていてもよい。また、加熱手段に設置した風速制御手段と、それ以外の風速制御手段を組み合わせて用いることもできる。
As the wind speed control means installed in the heating means, in addition to the above-described examples, for example, the internal cross-sectional area of the branch path 17a is divided into the branch path 17a connected to the hot air outlet 13a, and that of the hot air outlet 13b. It is also possible to make a difference in. Specifically, by making the cross-sectional area in the branch passage 17a connected to the hot air outlet 13a wider than that connected to the hot air outlet 13b, more hot air can flow to the hot air outlet 13a. it can. Thereby, the wind speed of the initial travel area can be made faster than the wind speed of the latter travel area. How much cross-sectional area difference is added to the cross-sectional area in the branch passage 17a connected to the hot air outlet 13a and the hot air outlet 13b is appropriately determined according to the scale of the flameproofing furnace, the hot air flow rate, and the like.
The flameproofing furnace 10 of the present invention may be used in combination with these wind speed control means. Moreover, these wind speed control means may be similarly provided in the hot air discharge port 14 side.
In addition to the wind speed control means provided in the heating means as described above, the flameproofing furnace 10 of the present invention includes wind speed control means such as a blower (not shown) in the initial traveling region in the heat treatment chamber 11, for example. It may be. Further, the wind speed control means installed in the heating means and other wind speed control means may be used in combination.

図2に示すように、本発明の耐炎化炉20は、初期の走行域と後期の走行域との間に仕切り板18を設けるのが好ましい。なお、仕切り板18は走行域に対して平行に設置される。
仕切り板18を設けることで、熱処理室11内を初期の走行域に該当する熱処理区画11aと後期の走行域に該当する熱処理区画11bとに区分けでき、初期の走行域及び後期の走行域を流れる熱風が適切な風速を維持することができる。これにより、双方を走行する前駆体繊維束1に対してより的確な熱風を吹き付けることができる。なお、仕切り板18は、熱処理区画11aと熱処理区画11bとの間を完全に仕切っていてもよいが、部分的に仕切るだけでもよい。また、図2の耐炎化炉20では、仕切り板18を1枚のみ設置しているが、必要に応じて、各走行域の間の任意の位置に仕切り板18を複数配置してもよい。なお、図2の耐炎化炉20の符号について、図1の耐炎化炉10の各構成と同様の構成物に関しては、便宜上、図1と同じ符号を使用して、説明を省略する。
As shown in FIG. 2, it is preferable that the flameproofing furnace 20 of the present invention is provided with a partition plate 18 between an initial traveling region and a later traveling region. In addition, the partition plate 18 is installed in parallel with the traveling area.
By providing the partition plate 18, the inside of the heat treatment chamber 11 can be divided into a heat treatment section 11 a corresponding to the initial traveling area and a heat treatment section 11 b corresponding to the latter traveling area, and flows through the initial traveling area and the latter traveling area. Hot air can maintain an appropriate wind speed. Thereby, more accurate hot air can be sprayed with respect to the precursor fiber bundle 1 which travels both. Note that the partition plate 18 may completely partition between the heat treatment section 11a and the heat treatment section 11b, or may partition only partly. Moreover, in the flameproofing furnace 20 of FIG. 2, although only one partition plate 18 is installed, a plurality of partition plates 18 may be disposed at arbitrary positions between the traveling areas as necessary. For the reference numerals of the flameproofing furnace 20 in FIG. 2, the same reference numerals as those in FIG.

さらに本発明は、図3に示すように複数の加熱器15、送風器16、及び循環路17を備えた耐炎化炉30であってもよい。耐炎化炉30は仕切り板18で仕切られた熱処理区画11a及び11bに対して、それぞれ個別の加熱手段を設けている。これにより、耐炎化炉30は熱処理区画11aと熱処理区画11bそれぞれに配される送風器16によって個別に風速制御することができる。すなわち、耐炎化炉30は、前述の加熱手段に風速制御手段を設けた一例でもある。また、耐炎化炉30は、熱処理室毎に加熱手段を備えているので、加熱手段毎に温度設定を違えることで、熱処理区画11aと熱処理区画11bを異なった温度設定とすることができる。なお、図3の耐炎化炉30の符号について、図1の耐炎化炉10の各構成と同様の構成物に関しては、便宜上、図1と同じ符号を使用して、説明を省略する。   Further, the present invention may be a flameproof furnace 30 including a plurality of heaters 15, a blower 16, and a circulation path 17 as shown in FIG. 3. The flameproofing furnace 30 is provided with individual heating means for the heat treatment sections 11 a and 11 b partitioned by the partition plate 18. Thereby, the flame-resistant furnace 30 can individually control the wind speed by the blower 16 disposed in each of the heat treatment section 11a and the heat treatment section 11b. That is, the flameproofing furnace 30 is also an example in which wind speed control means is provided in the above-described heating means. Moreover, since the flameproofing furnace 30 is provided with a heating means for each heat treatment chamber, the heat treatment section 11a and the heat treatment section 11b can be set to different temperature settings by changing the temperature setting for each heating means. For the reference numerals of the flameproofing furnace 30 in FIG. 3, the same reference numerals as those in FIG.

前記においては、いわゆる横型耐炎化炉について説明したが、本発明はそれに限定されず、熱処理室が上下方向に延びる縦型耐炎化炉も全く同様に構成することができる。
また、前記の説明では、熱風循環方式の耐炎化炉10、20、30を例示したが、本発明は、例えば図5に示すように、熱風の循環系を有しない非循環方式の耐炎化炉50であってもよい。非循環方式の耐炎化炉50は、外気を供給路51で導き、その供給路51の途中に設けた加熱器15及び送風器16によって所望の温度に加熱された熱風とした上で、熱処理室11内に吹き込む。吹き込まれた熱風は、熱処理室11内を通過して前駆体繊維束1を加熱した後、熱風排出口14によって熱処理室11外に排出される。排出された熱風は、熱処理室11内に再び戻されることなく、排出路52を通り、耐炎化炉50外に排出される。このような非循環方式の耐炎化炉50は、循環方式に比べて熱風の加熱に要するエネルギーコストが掛かるが、常に新鮮な熱風を送り込めるという利点がある。なお、図5の耐炎化炉50の符号について、図1の耐炎化炉10の各構成と同様の構成物に関しては、便宜上、図1と同じ符号を使用して、説明を省略する。
In the above description, a so-called horizontal flameproofing furnace has been described. However, the present invention is not limited thereto, and a vertical flameproofing furnace in which the heat treatment chamber extends in the vertical direction can be configured in exactly the same manner.
In the above description, the hot air circulation type flameproofing furnaces 10, 20, and 30 have been exemplified. However, as shown in FIG. 5, for example, the present invention is a non-circulation type flameproofing furnace having no hot air circulation system. 50 may be sufficient. The non-circulating flameproofing furnace 50 guides the outside air through a supply path 51, forms hot air heated to a desired temperature by a heater 15 and a blower 16 provided in the middle of the supply path 51, and then forms a heat treatment chamber. 11 is blown into. The blown hot air passes through the inside of the heat treatment chamber 11 to heat the precursor fiber bundle 1, and is then discharged out of the heat treatment chamber 11 through the hot air discharge port 14. The discharged hot air passes through the discharge path 52 and is discharged out of the flameproofing furnace 50 without being returned to the heat treatment chamber 11 again. Such non-circulation type flameproofing furnace 50 has the advantage that fresh hot air can always be sent, although it costs more energy to heat the hot air than the circulation type. 5, the same reference numerals as those in FIG. 1 are used for the sake of convenience and the description of the components similar to the respective components of the flameproofing furnace 10 in FIG. 1 is omitted.

さらに本発明は、前駆体繊維束1の走行方向に沿って熱処理室11内に熱風を吹き込む方式の耐炎化炉であればよいので、前記の例示以外にも、例えば、熱処理室11の中央部付近の各走行域間に熱風吹出口13を設けて、そこから熱処理室11の両端に設けた熱風排出口14に向けて熱風を吹き出す公知の耐炎化炉(不図示)でもその効果が得られる。   Furthermore, since the present invention only needs to be a flameproofing furnace of a type in which hot air is blown into the heat treatment chamber 11 along the traveling direction of the precursor fiber bundle 1, in addition to the above examples, for example, the central portion of the heat treatment chamber 11 The effect can be obtained also in a known flameproofing furnace (not shown) in which a hot air outlet 13 is provided between each of the nearby traveling areas, and hot air is blown out toward the hot air outlets 14 provided at both ends of the heat treatment chamber 11. .

本発明の耐炎化炉10、20、30、50を用いた耐炎化繊維の製造方法においては、これらの耐炎化炉を複数使用してもよく、さらに、例えば図4に示すような従来の耐炎化炉40と組み合わせて用いてもよい。なお、図4の従来の耐炎化炉40の符号について、図1の耐炎化炉10の各構成と同様の構成物に関しては、便宜上、図1と同じ符号を使用して、説明を省略する。
本発明の耐炎化炉10、20、30、50に送入される前駆体繊維束1を構成する繊維としては、公知の前駆体繊維を挙げる事ができ、例えば炭素繊維の前駆体繊維であるポリアクリロニトリル系繊維、ピッチ系繊維、フェノール系繊維等が挙げられる。また、本発明は他にも、例えば糸やフィルム、シート等といった各種の熱処理にも適用が可能である。
In the method for producing flame-resistant fibers using the flame-resistant furnaces 10, 20, 30, and 50 of the present invention, a plurality of these flame-resistant furnaces may be used. Further, for example, a conventional flame-resistant furnace as shown in FIG. It may be used in combination with the conversion furnace 40. In addition, about the code | symbol of the conventional flameproofing furnace 40 of FIG. 4, about the structure similar to each structure of the flameproofing furnace 10 of FIG. 1, the same code | symbol as FIG. 1 is used for convenience and description is abbreviate | omitted.
As a fiber which comprises the precursor fiber bundle 1 sent into the flameproofing furnace 10, 20, 30, 50 of this invention, a well-known precursor fiber can be mentioned, for example, it is a precursor fiber of carbon fiber. Examples thereof include polyacrylonitrile fiber, pitch fiber, and phenol fiber. In addition, the present invention can be applied to various heat treatments such as yarns, films, and sheets.

本発明の耐炎化繊維の製造方法によって製造された耐炎化繊維束は、次いで炭素化炉に送入され、窒素ガスやアルゴンガス等の不活性熱風中にて1,000〜3,000℃程度の温度で焼成、炭化処理することによって炭素繊維束とすることができる。また、耐炎化繊維束は、炭素繊維束に加工される以外にも、難燃性織布の素材としても広く用いられている。  The flame-resistant fiber bundle produced by the method for producing flame-resistant fibers of the present invention is then fed into a carbonization furnace and is about 1,000 to 3,000 ° C. in an inert hot air such as nitrogen gas or argon gas. A carbon fiber bundle can be obtained by firing and carbonizing at a temperature of. In addition to being processed into a carbon fiber bundle, the flame-resistant fiber bundle is widely used as a material for a flame-retardant woven fabric.

次に、本発明の実施例について説明するが、本発明はこれらに限定されるものではない。なお、本実施例及び比較例では、実際の使用に則すため、前駆体繊維束への耐炎化処理を、2台の耐炎化炉を用い、耐炎化処理を2回に分けて行った。
(実施例1)
100本のポリアクリロニトリル系繊維束を互いに並行するようにシート状に引き揃えて前駆体繊維束群とした。なお、前記ポリアクリロニトリル系繊維の1本当たりの単糸繊度は1.2dtex、単糸数50,000本である。
前記の前駆体繊維束1を1回目の耐炎化処理として、図4に示すような従来の耐炎化炉40に送入し、熱風温度236℃、熱風風速3.0m/sで17分間の耐炎化処理を施した。なお、1回目の耐炎化処理を終えた前駆体繊維束1の耐炎化密度は、1.24g/cmであった。
1回目の耐炎化処理を終えた前駆体繊維束1に対して、次いで図3に示す耐炎化炉30を用いて2回目の耐炎化処理を行い、熱処理室11内の熱風の温度を236℃から次第に上昇させ、前駆体繊維束1に糸切れが発生した温度を測定した。その結果、250℃で糸切れが発生した。なお、2回目の耐炎化処理において、耐炎化炉30の熱処理区画11aの風速、すなわち前駆体繊維束1の初期の走行域の風速は4.5m/sとし、熱処理区画11bの風速、すなわち後期の走行域の風速は3.0m/sに設定した。
次に、前述の1回目の耐炎化処理を行った前駆体繊維束1を、図2の耐炎化炉20に送入し、前述で得られた前駆体繊維束1の糸切れが発生した温度から8℃低い242℃に設定して、13分間の耐炎化処理を行った。このようにして得られた耐炎化繊維束の耐炎化密度、すなわち耐炎化繊維束の密度を測定したところ、1.27g/cmを示した。また、耐炎化繊維束の耐炎化密度は、耐炎化反応の進み具合を判断するための尺度となる。また、前記耐炎化処理の温度は、耐炎化処理工程内で発生する風速、温度、繊維束投入密度等の条件変動による切断温度の変化を考慮に入れて、糸切れが発生した温度から8℃低い温度に設定した。
Next, examples of the present invention will be described, but the present invention is not limited thereto. In this example and comparative example, in order to comply with actual use, the flame resistance treatment for the precursor fiber bundle was performed in two times using two flame resistance furnaces.
Example 1
100 polyacrylonitrile fiber bundles were arranged in a sheet shape so as to be parallel to each other to form a precursor fiber bundle group. The single yarn fineness per one of the polyacrylonitrile fibers is 1.2 dtex and the number of single yarns is 50,000.
As a first flameproofing treatment, the precursor fiber bundle 1 is fed into a conventional flameproofing furnace 40 as shown in FIG. 4, and has a hot air temperature of 236 ° C. and a hot air wind speed of 3.0 m / s for 17 minutes. Was applied. The flame resistance density of the precursor fiber bundle 1 after the first flame resistance treatment was 1.24 g / cm 3 .
The precursor fiber bundle 1 that has completed the first flameproofing treatment is then subjected to a second flameproofing treatment using the flameproofing furnace 30 shown in FIG. 3, and the temperature of the hot air in the heat treatment chamber 11 is 236 ° C. The temperature at which the yarn breakage occurred in the precursor fiber bundle 1 was measured. As a result, thread breakage occurred at 250 ° C. In the second flameproofing treatment, the wind speed of the heat treatment section 11a of the flameproofing furnace 30, that is, the wind speed in the initial traveling region of the precursor fiber bundle 1 is 4.5 m / s, and the wind speed of the heat treatment section 11b, that is, the latter stage. The wind speed in the traveling area was set to 3.0 m / s.
Next, the precursor fiber bundle 1 subjected to the first flameproofing treatment described above is fed into the flameproofing furnace 20 of FIG. 2, and the temperature at which the yarn breakage of the precursor fiber bundle 1 obtained above occurs. Then, the temperature was set to 242 ° C., which was 8 ° C. lower, and a flame resistance treatment for 13 minutes was performed. The flameproof density of the flameproofed fiber bundle thus obtained, that is, the density of the flameproofed fiber bundle, was measured and found to be 1.27 g / cm 3 . In addition, the flameproof density of the flameproofed fiber bundle is a measure for judging the progress of the flameproofing reaction. The temperature of the flameproofing treatment is 8 ° C. from the temperature at which the yarn breakage occurs, taking into account changes in the cutting temperature due to changes in conditions such as wind speed, temperature, fiber bundle input density, etc. generated in the flameproofing treatment process. A low temperature was set.

(比較例1)
2回目の耐炎化処理にも、図4に示す従来の耐炎化炉40を用いた以外は、実施例と同様にして、前駆体繊維束1の糸切れが発生した温度を測定した。その結果、2回目の耐炎化処理において、246℃で糸切れが発生した。
次に、前述の1回目の耐炎化処理を行った前駆体繊維束1を用いて、2回目の耐炎化炉の熱風温度を、糸切れが発生した温度から8℃低い238℃に設定して、耐炎化処理を行った。耐炎化繊維束の密度が実施例1と同じ1.27g/cmに到達するために要する時間を測定したところ、17分を要した。
(Comparative Example 1)
For the second flameproofing treatment, the temperature at which the yarn breakage of the precursor fiber bundle 1 occurred was measured in the same manner as in the example except that the conventional flameproofing furnace 40 shown in FIG. 4 was used. As a result, yarn breakage occurred at 246 ° C. in the second flameproofing treatment.
Next, using the precursor fiber bundle 1 subjected to the first flameproofing treatment, the hot air temperature of the second flameproofing furnace is set to 238 ° C, which is 8 ° C lower than the temperature at which yarn breakage occurs. The flameproofing treatment was performed. When the time required for the density of the flameproof fiber bundle to reach 1.27 g / cm 3 as in Example 1 was measured, it took 17 minutes.

結果、実施例1の耐炎化炉30は、比較例1の従来の熱処理炉40に比べて、高い温度で耐炎化処理が行えることが確認された。
また、実施例1の耐炎化密度を1.27g/cmとするのに、糸切れの可能性のない温度において、実施例1の耐炎化炉30では13分、比較例1の従来の熱処理炉40では17分を要した。よって、本発明によると、従来の耐炎化炉に比べて耐炎化処理の温度を高く設定できることで、耐炎化処理がより短時間で施せることが確認できた。
As a result, it was confirmed that the flameproofing furnace 30 of Example 1 can perform the flameproofing treatment at a higher temperature than the conventional heat treatment furnace 40 of Comparative Example 1.
Further, in order to set the flameproof density of Example 1 to 1.27 g / cm 3 , the conventional heat treatment of Comparative Example 1 is performed for 13 minutes in the flameproof furnace 30 of Example 1 at a temperature at which there is no possibility of yarn breakage. The furnace 40 required 17 minutes. Therefore, according to the present invention, it was confirmed that the flameproofing treatment can be performed in a shorter time by setting the temperature of the flameproofing treatment higher than that of the conventional flameproofing furnace.

本発明の耐炎化炉を用いた耐炎化繊維の製造方法によると、耐炎化初期(初期の走行域)の前駆体繊維の発熱を効率よく除熱できるため、糸切れや発火等を生じにくくなり、耐炎化繊維束の品質を向上できる。
また、本発明の耐炎化炉は、初期の走行域の熱処理室内の温度を一様としながら、初期の走行域の風速を後期の走行域の風速より速くすることにより、初期の走行域の除熱を後期の走行域の除熱より高めることができる。これにより、熱処理室内の温度制限を初期の走行域の温度設定に制約されずに済み、従来の耐炎化炉に比べて高い温度で耐炎化処理を行うことができる。ゆえに、前駆体繊維束の耐炎化処理を早めることができ、耐炎化繊維束の生産性を向上できる。
よって、本発明の耐炎化炉及び耐炎化繊維の製造方法を用いれば、耐炎化繊維の生産性及び品質の向上が実現できる。
According to the method for producing flame-resistant fibers using the flame-proofing furnace of the present invention, it is possible to efficiently remove the heat of the precursor fibers at the initial stage of flame resistance (initial running region), and therefore, yarn breakage and ignition are less likely to occur. The quality of the flame-resistant fiber bundle can be improved.
In addition, the flameproofing furnace of the present invention eliminates the initial travel area by making the wind speed in the initial travel area faster than the wind speed in the later travel area while keeping the temperature in the heat treatment chamber in the initial travel area uniform. The heat can be increased more than the heat removal in the later driving area. Thereby, the temperature limitation in the heat treatment chamber is not limited to the initial temperature setting of the traveling region, and the flameproofing treatment can be performed at a higher temperature than the conventional flameproofing furnace. Therefore, the flameproofing treatment of the precursor fiber bundle can be accelerated, and the productivity of the flameproof fiber bundle can be improved.
Therefore, if the flameproofing furnace and the method for producing flameproofed fibers of the present invention are used, the productivity and quality of the flameproofed fiber can be improved.

本発明の実施形態例を示す耐炎化炉の概略構成図。The schematic block diagram of the flameproofing furnace which shows the embodiment of this invention. 本発明の別の実施形態例を示す耐炎化炉の概略構成図。The schematic block diagram of the flameproofing furnace which shows another example of embodiment of this invention. 本発明の別の実施形態例を示す耐炎化炉の概略構成図。The schematic block diagram of the flameproofing furnace which shows another example of embodiment of this invention. 従来の耐炎化炉の一例を示す概略構成図。The schematic block diagram which shows an example of the conventional flameproofing furnace. 本発明の別の実施形態例を示す耐炎化炉の概略構成図。The schematic block diagram of the flameproofing furnace which shows another example of embodiment of this invention.

符号の説明Explanation of symbols

1 前駆体繊維
10、20、30、50 耐炎化炉
11 熱処理室
11a、11b熱処理区画
12 ガイドロール
13、13a、13b熱風吹出口
14、14a、14b熱風排出口
15 加熱器
16 送風器
17 循環路
17a 分岐路
18 仕切り板
40 従来の耐炎化炉
DESCRIPTION OF SYMBOLS 1 Precursor fiber 10, 20, 30, 50 Flameproofing furnace 11 Heat processing chamber 11a, 11b Heat processing section 12 Guide rolls 13, 13a, 13b Hot air outlet 14, 14a, 14b Hot air outlet 15 Heater 16 Air blower 17 Circulation path 17a Branch 18 Partition 40 Conventional flameproof furnace

Claims (4)

前駆体繊維が送入送出を繰り返して内部を複数回走行する熱処理室と、前駆体繊維が走行するそれぞれの走行域に熱風を吹き込む加熱手段とを備えた耐炎化炉において、前記耐炎化炉内における初期の走行域の風速を前記耐炎化炉内における後期の走行域の風速より速くする風速制御手段を備える耐炎化炉。 In the flameproofing furnace, comprising: a heat treatment chamber in which the precursor fiber is repeatedly fed and delivered and travels a plurality of times in the interior; and heating means for blowing hot air into each traveling region in which the precursor fiber travels . A flameproofing furnace provided with wind speed control means for making the wind speed in the initial traveling region in the flame faster than that in the latter traveling region in the flameproofing furnace. 風速制御手段が、加熱手段に備えられている請求項1に記載の耐炎化炉。   The flameproof furnace according to claim 1, wherein the wind speed control means is provided in the heating means. 初期の走行域と後期の走行域との間に仕切り板が設けられている請求項1または2に記載の耐炎化炉。   The flameproof furnace according to claim 1 or 2, wherein a partition plate is provided between the initial traveling area and the latter traveling area. 請求項1〜3のいずれかに記載の耐炎化炉に前駆体繊維を送入し、前記耐炎化炉内における初期の走行域の風速を前記耐炎化炉内における後期の走行域の風速より速くする耐炎化繊維の製造方法。 The precursor fiber is fed into the flameproofing furnace according to any one of claims 1 to 3, and the wind speed in the initial traveling area in the flameproofing furnace is faster than the wind speed in the latter traveling area in the flameproofing furnace. A method for producing flame resistant fibers.
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