JP2001278353A - Carbon fiber packing body - Google Patents

Carbon fiber packing body

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Publication number
JP2001278353A
JP2001278353A JP2000090832A JP2000090832A JP2001278353A JP 2001278353 A JP2001278353 A JP 2001278353A JP 2000090832 A JP2000090832 A JP 2000090832A JP 2000090832 A JP2000090832 A JP 2000090832A JP 2001278353 A JP2001278353 A JP 2001278353A
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JP
Japan
Prior art keywords
fiber
weight
carbonaceous
carbon
fibers
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP2000090832A
Other languages
Japanese (ja)
Other versions
JP4318833B2 (en
Inventor
Hiroshi Tsunekawa
浩 恒川
Kenji Shimazaki
賢司 島崎
Toshimitsu Watanabe
俊充 渡辺
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Teijin Ltd
Original Assignee
Toho Tenax Co Ltd
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Filing date
Publication date
Application filed by Toho Tenax Co Ltd filed Critical Toho Tenax Co Ltd
Priority to JP2000090832A priority Critical patent/JP4318833B2/en
Publication of JP2001278353A publication Critical patent/JP2001278353A/en
Application granted granted Critical
Publication of JP4318833B2 publication Critical patent/JP4318833B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To provide a carbon fiber packing body which prevents any natural ignition caused by the heat accumulation while storing a carbon fiber, stores the fiber in a safe condition, and is convenient for the use when it is used in a following step, and free from generation of any migration. SOLUTION: In this carbon fiber packing body, the carbon fibers having the composition consisting of, by weight, 65-85% carbon with the mean fiber length of 0.1-150 mm are sealed maintaining the filling density of 0.1-0.5 g/cm3 and the water content of 3-8%.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、炭素質繊維の蓄熱
による自然発火を防止した炭素質繊維梱包体に関するも
のである。更に詳しくは、炭素含有率65〜85重量%
からなり、他に水素、酸素を含む炭素質繊維の蓄熱によ
る自然発火を防止した炭素質繊維梱包体に関するもので
ある。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a carbonaceous fiber package which prevents spontaneous ignition due to heat storage of carbonaceous fiber. More specifically, the carbon content is 65 to 85% by weight.
In addition, the present invention relates to a carbonaceous fiber package which prevents spontaneous ignition due to heat storage of carbonaceous fibers containing hydrogen and oxygen.

【0002】[0002]

【従来の技術】従来、炭素繊維は、高強度且つ高弾性を
有する補強材用繊維として優れた素材であり、合成樹脂
との複合材料として広く使用されている。この炭素繊維
は、アクリロニトリル系繊維、ピッチ系繊維等の有機繊
維より誘導されて製造されているが、特にアクリロニト
リル系繊維を原料として誘導された、所謂アクリル系炭
素繊維は、高強度且つ高弾性の繊維として有用されてい
る。
2. Description of the Related Art Hitherto, carbon fiber has been an excellent material as a reinforcing fiber having high strength and high elasticity, and has been widely used as a composite material with a synthetic resin. This carbon fiber is produced by being derived from organic fibers such as acrylonitrile-based fibers and pitch-based fibers. In particular, so-called acrylic carbon fibers derived from acrylonitrile-based fibers as raw materials have high strength and high elasticity. It is useful as a fiber.

【0003】アクリル系炭素繊維の製造は、アクリロニ
トリル系繊維を200〜400℃の酸化性雰囲気で酸化
処理(耐炎化処理)して所謂耐炎繊維とし、更に炭素の
昇華温度までの不活性雰囲気中にて焼成することによっ
て、狭義の意味での炭素繊維及び黒鉛繊維としている。
[0003] Acrylic carbon fibers are produced by so-called oxidizing treatment (flaming-resistant treatment) of acrylonitrile-based fibers in an oxidizing atmosphere at 200 to 400 ° C to form so-called flame-resistant fibers. By firing, carbon fibers and graphite fibers in a narrow sense are obtained.

【0004】このような不活性雰囲気中での焼成は、目
的とする炭素繊維の性能に応じ条件設定がされ、この焼
成過程において、繊維中の炭素含有率は、アクリロニト
リル系繊維段階で55重量%程度であったものが次第に
高くなり、最終的には殆ど炭素のみの繊維となる。通
常、汎用されている炭素繊維の炭素含有率は、90重量
%以上であり、その焼成温度は1000℃以上で、一般
的には1200℃以上のものが普通である。
[0004] Conditions for firing in such an inert atmosphere are set according to the performance of the target carbon fiber. In this firing process, the carbon content in the fiber is 55% by weight in the acrylonitrile-based fiber stage. What has been gradually increased, and eventually becomes almost carbon-only fibers. Usually, the carbon content of widely used carbon fibers is 90% by weight or more, and the sintering temperature is 1000 ° C or more, and generally 1200 ° C or more.

【0005】このような炭素繊維に対して、アクリロニ
トリル系繊維を200〜400℃の酸化性雰囲気で酸化
処理した繊維(耐炎繊維)を焼成温度が500〜100
0℃、特に一般的には600〜800℃の炭素繊維の場
合に比べて、低い焼成温度で不活性雰囲気中で焼成した
繊維は炭素質繊維と呼ばれ、炭素含有率は65〜85重
量%程度である。炭素質繊維は、炭素繊維に比べて親水
性、電気抵抗が高く、一般的に樹脂との親和性も高いと
いう特性を有する。また炭素繊維とは異なる摺動特性を
有する。
An acrylonitrile fiber obtained by subjecting such acrylonitrile fiber to oxidation treatment in an oxidizing atmosphere at 200 to 400 ° C. is fired at a firing temperature of 500 to 100.
Fibers fired in an inert atmosphere at a lower firing temperature than carbon fibers at 0 ° C., particularly generally 600-800 ° C., are called carbonaceous fibers and have a carbon content of 65-85% by weight. It is about. Carbonaceous fibers have characteristics of being higher in hydrophilicity and electric resistance than carbon fibers, and generally higher in affinity with resin. It also has sliding characteristics different from carbon fibers.

【0006】このような性質を持つ炭素質繊維は、例え
ば、摩擦材の補強繊維や、建築材等の補強繊維に使用さ
れる。炭素質繊維は炭素繊維に比較して安価であり、特
に摩擦材に使用された場合には、安定した高摩擦係数を
与えることが知られている(例えば、特公平6−847
72号公報)。
[0006] The carbonaceous fibers having such properties are used, for example, as reinforcing fibers for friction materials and reinforcing fibers for building materials. It is known that carbonaceous fiber is inexpensive as compared with carbon fiber, and particularly when used as a friction material, provides a stable high coefficient of friction (for example, Japanese Patent Publication No. 6-847).
No. 72).

【0007】このような摩擦材、建築材等に使用される
炭素質繊維は、所定長に切断されて保管、輸送され、使
用される。炭素質繊維の切断は、湿潤状態で行われるこ
とが多い。これは、乾燥状態で切断すると、収束性が悪
く、毛羽立ちが生じ、その後の取り扱い性が著しく困難
となるからである。したがって、水分率10〜50%程
度の高水分状態で保管、輸送されることが多かった。し
かしながら、このような高水分状態の炭素質繊維を、乾
燥状態で使用する場合には、一旦乾燥する必要がある
が、高水分状態から徐々に乾燥すると、炭素質繊維に付
着されているサイズ剤、油脂等の移動、付着ムラが生
じ、マイグレーションの原因となる。
[0007] The carbonaceous fibers used for such friction materials and building materials are cut into predetermined lengths, stored, transported, and used. Cutting of carbonaceous fibers is often performed in a wet state. This is because cutting in a dry state results in poor convergence, fuzzing, and extremely difficult handling thereafter. Therefore, they are often stored and transported in a high moisture state with a moisture content of about 10 to 50%. However, when such a high-moisture state carbonaceous fiber is used in a dry state, it is necessary to dry the carbonaceous fiber once. Movement and adhesion unevenness of oils and fats occur, which causes migration.

【0008】[0008]

【発明が解決しようとする課題】乾燥状態の炭素質繊維
を使用する場合には、乾燥状態で保管された炭素質繊維
がそのままの乾燥状態で使用できるので便利である。し
かしながら、本発明者らの知見によると、炭素含有率の
低い炭素質繊維の一つの問題点として、乾燥状態で10
0℃程度の温度条件下で保管すると、酸化が徐々に進行
して内部に蓄熱し、最終的に自然発火するという問題が
あることを見いだしている。このような現象は、炭素繊
維及び耐炎繊維には見られない、炭素質繊維固有の現象
である。
When dry carbonaceous fibers are used, it is convenient because the carbonaceous fibers stored in a dry state can be used as they are in a dry state. However, according to the findings of the present inventors, one of the problems of the carbonaceous fiber having a low carbon content is that the carbonaceous fiber has
It has been found that when stored under a temperature condition of about 0 ° C., there is a problem that oxidation gradually progresses, heat is stored inside, and eventually spontaneous ignition occurs. Such a phenomenon is a phenomenon peculiar to carbonaceous fiber which is not found in carbon fiber and flame resistant fiber.

【0009】炭素質繊維を保管する場合、保管スペース
の関係から、或いはストランド、不織布、織物といった
長尺物の場合巻かれた状態や積み重ねられた状態で保管
される。このように、ある程度の充填密度でこのような
蓄熱による自然発火を防止するために、保管温度を厳密
に管理し、80℃を超えない温度に維持し、或いは積み
重ねた炭素質繊維の間に温度センサを挿入し内部温度を
常時チェックするという方法が必要とされていた。
[0009] When carbonaceous fibers are stored, they are stored in a wound state or a stacked state in the case of a long object such as a strand, a nonwoven fabric, or a woven fabric due to a storage space. Thus, in order to prevent spontaneous ignition due to such heat storage at a certain packing density, the storage temperature is strictly controlled, maintained at a temperature not exceeding 80 ° C., or the temperature between the stacked carbonaceous fibers is reduced. There was a need for a method of inserting a sensor and constantly checking the internal temperature.

【0010】しかしながら、不慮の温度管理状態におい
て自然発火することは避けなければならない。
However, spontaneous ignition must be avoided in an accidental temperature control state.

【0011】したがって、本発明の目的は、炭素質繊維
の保管中における蓄熱による自然発火を防止し、安全に
保管するとともに、次工程で使用する場合にも使用勝手
がよく、マイグレーションの発生が無い炭素質繊維の梱
包体を提供することにある。
Therefore, an object of the present invention is to prevent spontaneous ignition due to heat storage during storage of carbonaceous fiber, to store it safely, and to use it easily in the next step without causing migration. An object of the present invention is to provide a carbonaceous fiber package.

【0012】[0012]

【課題を解決するための手段】前記した目的を達成する
ための本発明の炭素質繊維梱包体は、炭素含有率65〜
85重量%、平均繊維長0.1〜150mmの炭素質繊
維が、不透湿フィルムにより、充填密度0.1〜0.5
g/cm3 、好ましくは0.15〜0.3g/cm
3 で、水分率3〜8重量%を維持した状態で密閉されて
いることを特徴とする。
Means for Solving the Problems The carbonaceous fiber package of the present invention for achieving the above object has a carbon content of 65 to 65.
85% by weight, a carbonaceous fiber having an average fiber length of 0.1 to 150 mm is filled with a packing density of 0.1 to 0.5 by an impermeable film.
g / cm 3 , preferably 0.15 to 0.3 g / cm
3 , characterized by being sealed while maintaining a moisture content of 3 to 8% by weight.

【0013】本発明の炭素質繊維梱包体はこのような状
態で密閉されることにより、保管中における蓄熱による
自然発火を防止し、安全に保管するとともに、次工程で
使用する場合にも、使用勝手のよいものとなる。
[0013] The carbonaceous fiber package of the present invention is sealed in such a state to prevent spontaneous ignition due to heat storage during storage, to store safely, and to be used in the next step. It becomes selfish.

【0014】本発明は、炭素含有率65〜85重量%、
平均繊維長が0.1〜150mmの炭素質繊維を梱包の
対象としている。炭素有量が65重量%未満であると、
耐熱性が低くなり、耐熱用途に適さなくなる。また炭素
含有量が85重量%を超えると炭素繊維に近似乃至炭素
繊維となるが、製造コストが高くなり、しかも摩擦係数
が低下してくるので、摩擦材用途には適さなくなる。平
均繊維長が0.1mm未満であると、摩擦材や建築材の
補強等における補強効果が少なくなり、150mmを超
えると補強繊維として混合し分散させて使用する時に分
散が困難となる。
According to the present invention, a carbon content of 65 to 85% by weight is provided.
The carbon fiber having an average fiber length of 0.1 to 150 mm is to be packed. If the carbon content is less than 65% by weight,
The heat resistance is low, making it unsuitable for heat-resistant applications. On the other hand, if the carbon content exceeds 85% by weight, the carbon fiber becomes similar to the carbon fiber or becomes a carbon fiber. However, the production cost increases and the friction coefficient decreases, so that the carbon fiber is not suitable for use as a friction material. If the average fiber length is less than 0.1 mm, the reinforcing effect in reinforcing a friction material or a building material is reduced, and if it exceeds 150 mm, dispersion becomes difficult when mixed and dispersed as reinforcing fibers for use.

【0015】本発明の炭素質繊維梱包体は、不透湿フィ
ルム内に上記の水分範囲を維持した状態で密閉されてい
ることが必要である。水分率が3重量%未満であれば、
炭素質繊維の収束性が低下し、ばらけ易くなり炭素質繊
維の使用時の混合工程における分散性が悪く作業性が悪
くなると共に、高温保管時に発火の恐れが生じる。水分
率が8重量%を超えれば、そのままの状態では水分が多
すぎて使用できず乾燥を必要とし、さらに水分率が多す
ぎると乾燥時にマイグレーションの発生が起こりやすく
なる。また、不慮の温度管理状態、或いは、赤道直下の
船積みで100℃を超えるような状態となった場合に
は、通常の包装形態では、水分率3〜8重量%を維持す
ることは困難で、高温のため水分率が低下して絶乾状態
となり、発火に至るようになる。したがって、不透湿フ
ィルムにより密閉して水分率を上記範囲に保つことは発
火防止のため、且つ良好な作業性を得るために必要であ
る。
[0015] The carbonaceous fiber package of the present invention must be hermetically sealed in the moisture-impermeable film while maintaining the above moisture range. If the moisture content is less than 3% by weight,
The convergence of the carbonaceous fiber is reduced, and the carbonaceous fiber is easily disintegrated, the dispersibility in the mixing step at the time of using the carbonaceous fiber is poor, the workability is deteriorated, and there is a risk of ignition during high-temperature storage. If the water content exceeds 8% by weight, the water cannot be used as it is and cannot be used as it is, and drying is required. If the water content is too high, migration is likely to occur during drying. In addition, in the case of an unexpected temperature control state or a state where the temperature exceeds 100 ° C. due to shipping just below the equator, it is difficult to maintain a moisture content of 3 to 8% by weight in a normal packaging form. Due to the high temperature, the moisture content is reduced to become a completely dry state, leading to ignition. Therefore, it is necessary to keep the moisture content in the above range by sealing with an impermeable film in order to prevent ignition and to obtain good workability.

【0016】本発明で使用する不透湿フィルムには、水
蒸気透過量が50g/m2 ・24hr以下(JIS K
7129による、40℃、90RHの条件下)であるこ
とが望ましい。不透湿フィルムの材質には、水分が透過
しないものであれば何でもよいが、例えば、ポリエチレ
ン、ポリプロピレン等のポリオレフィン、ナイロン、ポ
リエステル、ポリ塩化ビニリデン等或いはこれらの材質
と他の材質を組み合わせたもの、例えば、不透湿加工し
た布帛、積層フィルム等が使用できる。不透湿フィルム
厚みは好ましくは30〜200μm、さらに好ましくは
50〜100μmである。不透湿フィルムが薄いと破損
の危険があり、水蒸気透過量が多くなり、一方、厚いと
堅くなり、取り扱い性が悪く、コスト高となる。梱包体
の形態はどのようなものでもよく、開孔部をシールして
密閉とする。
The moisture-impermeable film used in the present invention has a water vapor transmission rate of 50 g / m 2 · 24 hr or less (JIS K
7129 under the conditions of 40 ° C. and 90 RH). As the material of the moisture-impermeable film, any material may be used as long as it does not allow moisture to permeate. For example, polyethylene, polypropylene, and other polyolefins, nylon, polyester, polyvinylidene chloride, or a combination of these materials and other materials For example, an impermeable fabric, a laminated film, or the like can be used. The thickness of the moisture-impermeable film is preferably 30 to 200 µm, more preferably 50 to 100 µm. If the moisture-impermeable film is thin, there is a risk of breakage, and the amount of water vapor transmission increases. On the other hand, if the film is thick, the film becomes hard, poor in handleability, and costs high. The form of the package may be any, and the opening is sealed and sealed.

【0017】本発明の炭素質繊維梱包体における、炭素
質繊維の充填密度は0.1〜0.5g/cm3 とする。
充填密度が0.1g/cm3 未満であると輸送コストが
高くなり、輸送時に片寄り等が生じ不安定となる。一
方、0.5g/cm3 を超えると解舒困難となり、例え
ば、繊維の絡みが生じるため混合工程で均一分散が困難
となり、さらに、蓄熱性が高まることから発火の危険が
高まるので好ましくない。
The packing density of the carbonaceous fiber in the carbonaceous fiber package of the present invention is 0.1 to 0.5 g / cm 3 .
When the packing density is less than 0.1 g / cm 3 , the transportation cost is increased, and the transportation becomes unbalanced and unstable during transportation. On the other hand, if it exceeds 0.5 g / cm 3 , unwinding becomes difficult, and, for example, it becomes difficult to uniformly disperse in the mixing step due to entanglement of the fibers, and further, the heat storage property is increased, and the risk of ignition is increased, which is not preferable.

【0018】特公昭48−34538号公報には、アク
リル系重合体よりなる繊維を10〜50%の水分を含有
した状態で採取する炭素繊維用アクリル系連続繊維束の
製造方法について示されているが、これは無撚り、無
捲、油剤無しの繊維束の収束性向上を目的としたもので
あり、本発明のような炭素質繊維が特定の条件で密閉さ
れた梱包体の保管中における蓄熱による自然発火を防止
し、安全に保管するとともに、次工程で使用する場合に
も使用勝手がよく、マイグレーションの発生が無い炭素
質繊維の梱包体とは無縁のものである。
Japanese Patent Publication No. 48-34538 discloses a method for producing an acrylic continuous fiber bundle for carbon fiber, in which fibers made of an acrylic polymer are collected in a state containing 10 to 50% of water. However, this is intended to improve the convergence of a fiber bundle without twist, no winding, and no oil agent, and heat storage during storage of a package in which carbonaceous fibers are sealed under specific conditions as in the present invention. In addition to preventing spontaneous ignition caused by the carbon fiber, it is safe to store, and is easy to use when used in the next step, and is free from a carbon fiber package without migration.

【0019】特開平1−272864号公報には、サイ
ジング剤無しの炭素繊維を0.1重量%以上の水を付着
した状態で巻き取ることが示されているが、これは炭素
繊維の収束性の向上、毛羽発生のトラブルを防止するも
のであり、上記と同様に本発明の炭素質繊維梱包体とは
目的、構成、効果の異なるものである。
Japanese Unexamined Patent Publication (Kokai) No. 1-272864 discloses that a carbon fiber without a sizing agent is wound with 0.1% by weight or more of water adhered thereto. The purpose of the present invention is to improve the quality and prevent the occurrence of fluff, and has a different purpose, structure and effect from the carbonaceous fiber package of the present invention as described above.

【0020】本発明の炭素質繊維梱包体における炭素質
繊維の燐含有量は、50〜300ppmであることが望
ましい。燐含有量が50ppm未満であると耐酸化性が
悪くなり、300ppmを超えると繊維強度が劣化す
る。また、ナトリウム含有量は200ppm以下が好ま
しく、さらに好ましくは100ppm以下であり、ナト
リウム含有量が多いと酸化性が悪くなる。
The carbonaceous fiber in the carbonaceous fiber package of the present invention preferably has a phosphorus content of 50 to 300 ppm. If the phosphorus content is less than 50 ppm, the oxidation resistance will be poor, and if it exceeds 300 ppm, the fiber strength will be degraded. Further, the sodium content is preferably 200 ppm or less, more preferably 100 ppm or less. When the sodium content is large, the oxidizing property is deteriorated.

【0021】炭素質繊維のうち、ポリアクリロニトリル
系炭素質繊維は、他の材料を起源とする炭素質繊維より
も強度が高く、補強繊維として優れている。
Among the carbonaceous fibers, polyacrylonitrile-based carbonaceous fibers have higher strength than carbonaceous fibers derived from other materials, and are excellent as reinforcing fibers.

【0022】[0022]

【実施例】〔実施例1〕アクリロニトリル96重量%、
アクリル酸メチル4重量%からなる共重合体塩化亜鉛水
溶液(塩化亜鉛濃度45重量%)を紡糸し、1.9dt
exで12,000フィラメントのアクリル系糸条を得
た。次に該糸条をポリエチレングリコール0.2重量%
の水溶液に含浸した後、空気中245℃で1時間、さら
に255℃で1時間酸化処理して繊維密度1.4g/c
3 の耐炎化糸を得た。
EXAMPLES Example 1 96% by weight of acrylonitrile,
A copolymer aqueous zinc chloride solution containing 4% by weight of methyl acrylate (zinc chloride concentration: 45% by weight) was spun and 1.9 dt.
ex, 12,000 filament acrylic yarn was obtained. Next, the yarn was subjected to polyethylene glycol 0.2% by weight.
And then oxidized in air at 245 ° C. for 1 hour and further at 255 ° C. for 1 hour to obtain a fiber density of 1.4 g / c.
m 3 of the flame-resistant yarn was obtained.

【0023】該耐炎化糸を窒素ガス中800℃で加熱
し、繊維密度1.7g/cm3 、炭素含有率74重量
%、酸素含有率6重量%の炭素質繊維を得た。
The oxidized yarn was heated at 800 ° C. in nitrogen gas to obtain a carbonaceous fiber having a fiber density of 1.7 g / cm 3 , a carbon content of 74% by weight, and an oxygen content of 6% by weight.

【0024】該炭素質繊維を加湿条件下、ギロチンカッ
ターにて平均繊維長3mmにるようにカットし、低密度
ポリエチレン、厚さ80μmの不透湿袋(水蒸気透過量
15g/m2 /24時間)に入れ、充填密度0.2g/
cm3 、水分率5重量%になるように密封し70℃で保
管したところ、蓄熱による梱包体の温度上昇はなく、6
ヶ月安定に保管できた。本実施例1の炭素質繊維梱包体
の製造条件、保管条件及びその結果を下記の表1に示
す。
The carbonaceous fibers humidified conditions, and cut to resemble average fiber length 3mm at guillotine cutter, low density polyethylene, impermeability Shimefukuro thickness 80 [mu] m (water vapor permeability of 15g / m 2/24 hours ) And a packing density of 0.2 g /
When sealed and stored at 70 ° C. so as to have a water content of 5 cm 3 and a water content of 5% by weight, there was no increase in the temperature of the package due to heat storage.
It was stable for months. The manufacturing conditions, storage conditions and results of the carbonaceous fiber package of Example 1 are shown in Table 1 below.

【0025】〔実施例2〕アクリロニトリル96重量
%、アクリル酸メチル4重量%からなる共重合体塩化亜
鉛水溶液(塩化亜鉛濃度45重量%)を紡糸し、12,
000フィラメントのプリカーサー(1.9dtex)
とした。このプリカーサーをポリエチレングリコールを
0.2重量%含む水溶液からなる油剤処理浴で処理し
た。次にこの処理済プリカーサーを、245℃で1時
間、次いで255℃で1時間空気中で酸化処理し、密度
1.4g/cm3 の耐炎化糸を得た。これを窒素ガス中
900℃で炭素質化処理することにより、密度1.8g
/cm3 の炭素質繊維を得た。この炭素質繊維は、炭素
含有率が80重量%、酸素含有率が4重量%であった。
Example 2 A copolymer zinc chloride aqueous solution consisting of 96% by weight of acrylonitrile and 4% by weight of methyl acrylate (zinc chloride concentration: 45% by weight) was spun.
2,000 filament precursor (1.9 dtex)
And The precursor was treated in an oil treatment bath consisting of an aqueous solution containing 0.2% by weight of polyethylene glycol. Next, the treated precursor was oxidized in air at 245 ° C. for 1 hour and then at 255 ° C. for 1 hour to obtain an oxidized yarn having a density of 1.4 g / cm 3 . This is carbonized at 900 ° C. in nitrogen gas to obtain a density of 1.8 g.
/ Cm 3 of carbonaceous fiber was obtained. This carbonaceous fiber had a carbon content of 80% by weight and an oxygen content of 4% by weight.

【0026】この炭素質繊維を加湿条件下、ギロチンカ
ッターにて平均繊維長3mmになるようにカットし、嵩
密度が0.2g/cm3 のチョップドフィバーを得た。
このチョップドフィバー15kgをポリエチレン製不透
湿袋に入れ、充填密度0.2g/cm3 、水分率5重量
%になるように密封し70℃で保管したところ、蓄熱に
よる梱包体の温度上昇はなく、6ヶ月安定に保管でき
た。本実施例2の炭素質繊維梱包体の製造条件、保管条
件及びその結果を下記の表1に示す。
The carbonaceous fiber was cut with a guillotine cutter under humidifying conditions so as to have an average fiber length of 3 mm to obtain a chopped fiber having a bulk density of 0.2 g / cm 3 .
When 15 kg of the chopped fiber was put into a polyethylene impermeable bag, it was sealed at a packing density of 0.2 g / cm 3 and a water content of 5% by weight and stored at 70 ° C., and there was no temperature rise of the package due to heat storage. For 6 months. The manufacturing conditions, storage conditions, and results of the carbonaceous fiber package of Example 2 are shown in Table 1 below.

【0027】〔実施例3〕アクリロニトリル96重量
%、アクリル酸メチル4重量%からなる共重合体塩化亜
鉛水溶液(塩化亜鉛濃度45重量%)を紡糸し、12,
000フィラメントのプリカーサー(1.9dtex)
とした。このプリカーサーをポリエチレングリコールを
0.2重量%の水溶液に含浸した後、空気中245℃で
1時間処理した。この炭素繊維は繊維密度1.7g/c
3 、炭素含有率が74重量%、酸素含有率が6重量%
であった。この炭素質繊維を水添化条件下、ギロチンカ
ッターにて平均繊維長6mmになるようにカットし、嵩
密度が0.6g/cm3 のチョップドフィバーを得た。
この時の水分率は20重量%であった。このチョップド
フィバーを減圧下70℃で乾燥し、40℃まで降温した
後、常圧に戻してポリエチレン製不透湿袋で20kgを
密封し、充填密度0.5g/cm3 、水分率4重量%に
なるよう密封し70℃で保管したところ、蓄熱による梱
包体の温度上昇はなく、6ヶ月安定に保管できた。本実
施例3の炭素質繊維梱包体の製造条件、保管条件及びそ
の結果を下記の表1に示す。
Example 3 A copolymer zinc chloride aqueous solution (zinc chloride concentration: 45% by weight) consisting of 96% by weight of acrylonitrile and 4% by weight of methyl acrylate was spun.
2,000 filament precursor (1.9 dtex)
And The precursor was impregnated with a 0.2% by weight aqueous solution of polyethylene glycol, and then treated in air at 245 ° C. for 1 hour. This carbon fiber has a fiber density of 1.7 g / c.
m 3 , carbon content 74% by weight, oxygen content 6% by weight
Met. This carbonaceous fiber was cut with a guillotine cutter under hydrogenation conditions so as to have an average fiber length of 6 mm, and a chopped fiber having a bulk density of 0.6 g / cm 3 was obtained.
The water content at this time was 20% by weight. The chopped fiber was dried at 70 ° C. under reduced pressure, cooled to 40 ° C., returned to normal pressure, sealed with 20 kg of polyethylene impermeable bag, filled density 0.5 g / cm 3 , moisture content 4% by weight. When sealed and stored at 70 ° C., there was no increase in the temperature of the package due to heat storage, and the package could be stored stably for 6 months. The manufacturing conditions, storage conditions and results of the carbonaceous fiber package of Example 3 are shown in Table 1 below.

【0028】〔実施例4〕アクリロニトリル96重量
%、アクリル酸メチル4重量%からなる共重合体塩化亜
鉛水溶液(塩化亜鉛濃度45重量%)を紡糸し、12,
000フィラメントのプリカーサー(1.9dtex)
とした。このプリカーサーをポリエチレングリコールを
0.2重量%含む水溶液からなる油剤処理浴で処理し
た。
Example 4 A copolymer zinc chloride aqueous solution (zinc chloride concentration 45% by weight) consisting of acrylonitrile 96% by weight and methyl acrylate 4% by weight was spun.
2,000 filament precursor (1.9 dtex)
And This precursor was treated in an oil treatment bath consisting of an aqueous solution containing 0.2% by weight of polyethylene glycol.

【0029】この処理済プリカーサーを、245℃で1
時間、次いで255℃で1時間空気中で酸化処理し、密
度1.4g/cm3 の耐炎糸を得た。これを窒素ガス中
600℃で炭素質化処理することにより、密度1.6g
/cm3 の炭素質繊維を得た。この炭素質繊維は、炭素
含有率が79重量%、酸素含有率が7重量%であった。
The treated precursor was heated at 245 ° C. for 1 hour.
After that, oxidation treatment was performed in the air at 255 ° C. for 1 hour to obtain a flame resistant yarn having a density of 1.4 g / cm 3 . This was carbonized at 600 ° C. in nitrogen gas to give a density of 1.6 g.
/ Cm 3 of carbonaceous fiber was obtained. This carbonaceous fiber had a carbon content of 79% by weight and an oxygen content of 7% by weight.

【0030】この炭素質繊維を加湿条件下、ギロチンカ
ッターにて平均繊維長10mmになるようカットし、嵩
密度が0.3g/cm3 のチョップドファイバーを得
た。このチョップドファイバー20kgをポリエチレン
製不透湿袋で、充填密度0.3g/cm3 、水分率が5
重量%となるように密封し、70℃で保管したが、蓄熱
による梱包体の温度上昇はなく、6ヶ月安定に保管でき
た。本実施例4の炭素質繊維梱包体の製造条件、保管条
件及びその結果を下記の表1に示す。
The carbonaceous fiber was cut with a guillotine cutter to an average fiber length of 10 mm under humidified conditions to obtain a chopped fiber having a bulk density of 0.3 g / cm 3 . 20 kg of the chopped fiber is packed in a polyethylene impermeable bag with a packing density of 0.3 g / cm 3 and a moisture content of 5 kg.
The package was sealed at 70% by weight and stored at 70 ° C., but there was no increase in the temperature of the package due to heat storage, and storage was stable for 6 months. The manufacturing conditions, storage conditions and results of the carbonaceous fiber package of Example 4 are shown in Table 1 below.

【0031】[0031]

【表1】 〔比較例1〕アクリロニトリル96重量%、アクリル酸
メチル4重量%からなる共重合体塩化亜鉛水溶液(塩化
亜鉛濃度45重量%)を紡糸し、12,000フィラメ
ントのプリカーサー(1.9dtex)とした。このプ
リカーサーをポリエチレングリコールを0.2重量%含
む水溶液からなる油剤処理浴で処理した。
[Table 1] Comparative Example 1 A copolymer zinc chloride aqueous solution (zinc chloride concentration: 45% by weight) composed of 96% by weight of acrylonitrile and 4% by weight of methyl acrylate was spun into a precursor of 12,000 filaments (1.9 dtex). This precursor was treated in an oil treatment bath consisting of an aqueous solution containing 0.2% by weight of polyethylene glycol.

【0032】この処理済プリカーサーを、245℃で1
時間、次いで255℃で1時間空気中で酸化処理し、密
度1.4g/cm3 の耐炎糸を得た。これを窒素ガス中
800℃で炭素質化処理することにより、密度1.7g
/cm3 の炭素質繊維を得た。この炭素質繊維は、炭素
含有率が74重量%、酸素含有率が6重量%であった。
The treated precursor was heated at 245 ° C. for 1 hour.
After that, oxidation treatment was performed in the air at 255 ° C. for 1 hour to obtain a flame resistant yarn having a density of 1.4 g / cm 3 . This was carbonized at 800 ° C. in nitrogen gas to obtain a density of 1.7 g.
/ Cm 3 of carbonaceous fiber was obtained. This carbonaceous fiber had a carbon content of 74% by weight and an oxygen content of 6% by weight.

【0033】この炭素質繊維を乾燥条件下、ギロチンカ
ッターにて平均繊維長3mmになるようカットし、嵩密
度が0.2g/cm3 のチョップドファイバーを得た。
このチョップドファイバー15kgをポリエチレン製不
透湿袋で、充填密度0.2g/cm3 、水分率が1重量
%となるように密封し、70℃で保管したところ、3日
後の測定で蓄熱により梱包体の温度上昇(80℃)が見
られた。比較例1の炭素質繊維梱包体の製造条件、保管
条件及びその結果を下記の表2に示す。
This carbonaceous fiber was cut under a dry condition with a guillotine cutter so as to have an average fiber length of 3 mm to obtain a chopped fiber having a bulk density of 0.2 g / cm 3 .
15 kg of the chopped fiber was sealed in a polyethylene impermeable bag so as to have a packing density of 0.2 g / cm 3 and a water content of 1% by weight, and was stored at 70 ° C. A rise in body temperature (80 ° C.) was observed. The production conditions, storage conditions and results of the carbonaceous fiber package of Comparative Example 1 are shown in Table 2 below.

【0034】〔比較例2〕コモノマー6重量%を含むP
AN系プリカーサーを200〜300℃で耐炎化処理
し、密度1.4g/cm3 の耐炎糸を得た。これを窒素
ガス雰囲気下600℃で処理する事により、密度1.6
g/cm3 の炭素質繊維を得た。この炭素質繊維は、炭
素含有率が79重量%、酸素含有率が7重量%であっ
た。
Comparative Example 2 P containing 6% by weight of comonomer
The AN-based precursor was subjected to a flame-proof treatment at 200 to 300 ° C. to obtain a flame-resistant yarn having a density of 1.4 g / cm 3 . This is treated at 600 ° C. in a nitrogen gas atmosphere to obtain a density of 1.6.
g / cm 3 of carbonaceous fiber was obtained. This carbonaceous fiber had a carbon content of 79% by weight and an oxygen content of 7% by weight.

【0035】この炭素質繊維を水添条件下、ギロチンカ
ッターにて平均繊維長6mmになるようカットし、嵩密
度が0.6g/cm3 のチョップドファイバーを得た。
この時の水分率は20重量%であった。このチョップド
ファイバーを70℃で真空水分率1重量%以下まで乾燥
し、降温せず、ポリエチレン製不透湿袋で充填密度が
0.2g/cm3 となるように該チョップドファイバー
20kgを密封し、60℃で保管したところ、蓄熱によ
り1日後に、密封体内の温度が360℃まで上昇し発煙
が見られた。比較例2の炭素質繊維梱包体の製造条件、
保管条件及びその結果を下記の表2に示す。
The carbonaceous fiber was cut under a hydrogenation condition with a guillotine cutter to an average fiber length of 6 mm to obtain a chopped fiber having a bulk density of 0.6 g / cm 3 .
The water content at this time was 20% by weight. The chopped fiber was dried at 70 ° C. to a moisture content in a vacuum of 1% by weight or less, and without cooling, 20 kg of the chopped fiber was sealed with a polyethylene impermeable bag so that the packing density was 0.2 g / cm 3 . When stored at 60 ° C., one day later due to heat storage, the temperature inside the sealed body rose to 360 ° C., and smoke was observed. Manufacturing conditions of the carbonaceous fiber package of Comparative Example 2,
The storage conditions and the results are shown in Table 2 below.

【0036】〔比較例3〕コモノマー4重量%を含むP
AN系プリカーサーを200〜300℃で耐炎化処理
し、密度1.4g/cm3 の耐炎糸を得た。これを窒素
ガス雰囲気下800℃で処理する事により、密度1.7
g/cm3 の炭素質繊維を得た。この炭素質繊維は、炭
素含有率が74重量%、酸素含有率が6重量%であっ
た。
Comparative Example 3 P containing 4% by weight of comonomer
The AN-based precursor was subjected to a flame-proof treatment at 200 to 300 ° C. to obtain a flame-resistant yarn having a density of 1.4 g / cm 3 . This is treated at 800 ° C. in a nitrogen gas atmosphere to obtain a density of 1.7.
g / cm 3 of carbonaceous fiber was obtained. This carbonaceous fiber had a carbon content of 74% by weight and an oxygen content of 6% by weight.

【0037】この炭素質繊維を加湿条件下、ギロチンカ
ッターにて平均繊維長6mmになるようカットし、嵩密
度が0.4g/cm3 のチョップドファイバーを得た。
このチョップドファイバー30kgをポリエチレン製不
透湿袋で、充填密度0.5g/cm3 、水分率が10重
量%となるように密封し、70℃で保管したところ、蓄
熱による梱包体の温度上昇はなかったが、6ヶ月後では
水分斑を生じ、後工程の分散処理時に分散斑(水分ム
ラ)を生じた。比較例3の炭素質繊維梱包体の製造条
件、保管条件及びその結果を下記の表2に示す。
This carbonaceous fiber was cut with a guillotine cutter to an average fiber length of 6 mm under humidified conditions to obtain a chopped fiber having a bulk density of 0.4 g / cm 3 .
When 30 kg of the chopped fiber was sealed in a polyethylene impermeable bag with a packing density of 0.5 g / cm 3 and a water content of 10% by weight and stored at 70 ° C., the temperature rise of the package due to heat storage was reduced. However, after 6 months, water spots occurred, and during the subsequent dispersion treatment, water spots (moisture unevenness) occurred. The production conditions, storage conditions and results of the carbonaceous fiber package of Comparative Example 3 are shown in Table 2 below.

【0038】〔比較例4〕アクリロニトリル96重量
%、アクリル酸メチル4重量%からなる共重合体塩化亜
鉛水溶液(塩化亜鉛濃度45重量%)を紡糸し、12,
000フィラメントのプリカーサー(1.9dtex)
とした。このプリカーサーをポリエチレングリコールを
0.2重量%含む水溶液からなる油剤処理浴で処理し
た。
[Comparative Example 4] A copolymer zinc chloride aqueous solution (zinc chloride concentration: 45% by weight) consisting of 96% by weight of acrylonitrile and 4% by weight of methyl acrylate was spun.
2,000 filament precursor (1.9 dtex)
And This precursor was treated in an oil treatment bath consisting of an aqueous solution containing 0.2% by weight of polyethylene glycol.

【0039】この処理済プリカーサーを、245℃で1
時間、次いで255℃で1時間空気中で酸化処理し、密
度1.4g/cm3 の耐炎糸を得た。これを窒素ガス中
800℃で炭素質化処理することにより、密度1.7g
/cm3 の炭素質繊維を得た。この炭素質繊維は、炭素
含有率が74重量%、酸素含有率が6重量%であった。
The treated precursor was heated at 245 ° C. for 1 hour.
After that, oxidation treatment was performed in the air at 255 ° C. for 1 hour to obtain a flame resistant yarn having a density of 1.4 g / cm 3 . This was carbonized at 800 ° C. in nitrogen gas to obtain a density of 1.7 g.
/ Cm 3 of carbonaceous fiber was obtained. This carbonaceous fiber had a carbon content of 74% by weight and an oxygen content of 6% by weight.

【0040】この炭素質繊維を加湿条件下、ギロチンカ
ッターにて平均繊維長3mmになるようカットし、嵩密
度が0.2g/cm3 のチョップドファイバーを得た。
このチョップドファイバー15kgをポリエチレン製不
透湿袋に入れ、充填密度0.3g/cm3 、水分率が5
重量%となるようにし、袋を解放して70℃で保管した
ところ、蓄熱により10日後温度上昇(90℃)が見ら
れた。この時の水分率は1%未満であった。比較例4の
炭素質繊維梱包体の製造条件、保管条件及びその結果を
下記の表2に示す。
This carbonaceous fiber was cut with a guillotine cutter to an average fiber length of 3 mm under humidified conditions to obtain a chopped fiber having a bulk density of 0.2 g / cm 3 .
15 kg of this chopped fiber is put into a polyethylene impermeable bag, and the packing density is 0.3 g / cm 3 and the moisture content is 5%.
When the bag was opened and stored at 70 ° C., the temperature rose (90 ° C.) after 10 days due to heat storage. The water content at this time was less than 1%. The production conditions, storage conditions and results of the carbonaceous fiber package of Comparative Example 4 are shown in Table 2 below.

【0041】[0041]

【表2】 [Table 2]

【0042】[0042]

【発明の効果】本発明の炭素質繊維梱包体によれば、保
管中における蓄熱による自然発火を防止し、安全に保管
できる。本発明の炭素質繊維梱包体は、水分率3〜8重
量%が維持されているため、使用勝手がよい。
According to the carbonaceous fiber package of the present invention, spontaneous ignition due to heat storage during storage can be prevented and safe storage is possible. Since the carbonaceous fiber package of the present invention maintains a moisture content of 3 to 8% by weight, it is easy to use.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 渡辺 俊充 静岡県駿東郡長泉町上土狩234番地 東邦 レーヨン株式会社三島工場内 Fターム(参考) 3E067 AA11 AB99 BA17A BB14A CA05 GA21  ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Toshimitsu Watanabe 234, Kamitsukari, Nagaizumi-cho, Sunto-gun, Shizuoka Prefecture Toho Rayon Co., Ltd. Mishima Plant F-term (reference) 3E067 AA11 AB99 BA17A BB14A CA05 GA21

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 炭素含有率65〜85重量%、平均繊維
長0.1〜150mmの炭素質繊維が、不透湿フィルム
により、充填密度0.1〜0.5g/cm3で、水分率
3〜8重量%を維持した状態で密閉されている炭素質繊
維梱包体。
1. A carbonaceous fiber having a carbon content of 65 to 85% by weight and an average fiber length of 0.1 to 150 mm is formed by a moisture-impermeable film at a packing density of 0.1 to 0.5 g / cm 3 and a water content of A carbonaceous fiber package hermetically sealed while maintaining 3 to 8% by weight.
【請求項2】 前記炭素質繊維がポリアクリロニトリル
系炭素質繊維である請求項1記載の炭素質繊維梱包体。
2. The carbonaceous fiber package according to claim 1, wherein the carbonaceous fiber is a polyacrylonitrile-based carbonaceous fiber.
JP2000090832A 2000-03-29 2000-03-29 CARBON FIBER PACKAGE AND METHOD FOR PRODUCING CARBON FIBER PACKAGE Expired - Fee Related JP4318833B2 (en)

Priority Applications (1)

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Applications Claiming Priority (1)

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Publications (2)

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WO2009011161A1 (en) * 2007-07-13 2009-01-22 Denki Kagaku Kogyo Kabushiki Kaisha Method of packing fiber for artificial hair
JP2014005014A (en) * 2012-06-22 2014-01-16 Toray Ind Inc Package and manufacturing method of the same

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JPH01503246A (en) * 1987-11-18 1989-11-02 ザ ダウ ケミカル カンパニー Anti-sway, anti-static and flame-resistant construction for use in containers holding flammable fluids
JPH0543320A (en) * 1991-08-01 1993-02-23 Osaka Gas Co Ltd Production of carbonaceous form
JPH05294361A (en) * 1992-04-09 1993-11-09 Toppan Printing Co Ltd Gusset package
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JPS61119717A (en) * 1984-11-14 1986-06-06 Toho Rayon Co Ltd Bundle of water-absorbing carbon fiber of high performance
JPH0684772B2 (en) * 1987-05-29 1994-10-26 東邦レーヨン株式会社 Friction material
JPH01503246A (en) * 1987-11-18 1989-11-02 ザ ダウ ケミカル カンパニー Anti-sway, anti-static and flame-resistant construction for use in containers holding flammable fluids
JPH0543320A (en) * 1991-08-01 1993-02-23 Osaka Gas Co Ltd Production of carbonaceous form
JPH05294361A (en) * 1992-04-09 1993-11-09 Toppan Printing Co Ltd Gusset package
JPH10121325A (en) * 1996-10-14 1998-05-12 Toray Ind Inc Precursor fiber bundle for carbon fiber and its production and production of carbon fiber
JPH10167564A (en) * 1996-12-05 1998-06-23 Toray Ind Inc Carbon fiber package and carbon fiber packaged body

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Publication number Priority date Publication date Assignee Title
WO2009011161A1 (en) * 2007-07-13 2009-01-22 Denki Kagaku Kogyo Kabushiki Kaisha Method of packing fiber for artificial hair
JP2009018846A (en) * 2007-07-13 2009-01-29 Denki Kagaku Kogyo Kk Packaging method of fiber for artificial hair
JP2014005014A (en) * 2012-06-22 2014-01-16 Toray Ind Inc Package and manufacturing method of the same

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