JPS6314093B2 - - Google Patents
Info
- Publication number
- JPS6314093B2 JPS6314093B2 JP5520981A JP5520981A JPS6314093B2 JP S6314093 B2 JPS6314093 B2 JP S6314093B2 JP 5520981 A JP5520981 A JP 5520981A JP 5520981 A JP5520981 A JP 5520981A JP S6314093 B2 JPS6314093 B2 JP S6314093B2
- Authority
- JP
- Japan
- Prior art keywords
- treatment
- fibers
- acrylonitrile
- heat
- temperature
- 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.)
- Expired
Links
- 239000000835 fiber Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 12
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000002657 fibrous material Substances 0.000 claims 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 16
- 239000004917 carbon fiber Substances 0.000 description 16
- 230000003647 oxidation Effects 0.000 description 15
- 238000007254 oxidation reaction Methods 0.000 description 15
- 238000000034 method Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 238000003763 carbonization Methods 0.000 description 5
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229920002239 polyacrylonitrile Polymers 0.000 description 4
- 230000009257 reactivity Effects 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BXALRZFQYDYTGH-UHFFFAOYSA-N 1-oxoprop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)C(=O)C=C BXALRZFQYDYTGH-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 1
- FGHSTPNOXKDLKU-UHFFFAOYSA-N nitric acid;hydrate Chemical compound O.O[N+]([O-])=O FGHSTPNOXKDLKU-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
Landscapes
- Artificial Filaments (AREA)
- Inorganic Fibers (AREA)
Description
本発明はアクリロニトリル系重合体から炭素繊
維を製造する方法に関するものであり、すでによ
く知られているアクリロニトリル系繊維から炭素
繊維を製造する工程中の熱酸化工程を、まつたく
省略できるかあるいはその処理を著しく短縮する
ことのできる方法を提供するものである。
炭素繊維は比強度、比弾性率が高い特性を活用
して樹脂等の強化材として使用したりあるいは耐
熱性、耐薬品性、電気伝導性を利用した分野への
用途が展開されている。しかしながら、今日炭素
繊維の用途開発において最も大きな障害の１つは
高価格であり、高品質で低コストの炭素繊維の開
発が望まれているところである。
アクリロニトリル系合成繊維を前駆体とする炭
素繊維は高品質のものが得られるが、その製造は
熱酸化工程と炭素化工程の２つの工程からなり、
しかも特に熱酸化工程は長時間を要することが大
きな問題である。したがつて、この熱酸化工程を
短縮あるいは省略することの意義は大きく、かか
る観点から炭素繊維の製造方法に関して検討した
ところ、繊維化前の重合体粉体を不活性雰囲気中
で加熱処理した後溶剤に溶解せしめて繊維化する
ことで、従来必要であつて熱酸化工程なしにある
いは熱酸化工程に要する時間を著しく短縮するこ
とのできる本発明を完成するに至つた。
アクリロニトリル系合成繊維はアクリロニトリ
ルモノマーを溶液重合あるいは懸濁重合等により
高分子化したあと賦形して繊維化する。この時繊
維重合の場合等では重合体を一たん粉体化し、こ
れを溶剤に溶解せしめて紡糸液とし、その後凝固
浴に吐出して繊維化する。この重合体の粉体を溶
剤に溶解するに際しては水分量をコントロールし
なければならないため乾燥工程を必要とする。本
発明はこの乾燥後に粉体の状態で効率よく加熱処
理して適度な不融性を付与することが特徴であ
る。
本発明に用いられるアクリロニトリル重合体と
してはアクリロニトリルが80重量％以上からなる
ものであればよく、アクリロニトリルと共重合可
能な単量体との共重合体あるいはアクリロニトリ
ルのみからなる重合体であつてもよい。共重合可
能な単量体としてはとくに制限されるものはな
く、一般に汎用されているアクリル酸メチル、ア
クリル酸エチル等のアクリル酸エステル類あるい
はメタクリル酸、アクリル酸、イタコン酸等の不
飽和カルボン酸、さらに塩化ビニル、酢酸ビニ
ル、スチレン、アクリルアミド、ジアセトンアク
リルアミド、アクリスルホン酸等の一種あるいは
二種以上を用いることができる。
つぎにアクリロニトリル系重合体粉体の加熱処
理であるが、重合体粉体の乾燥工程後にとくに不
活性雰囲気に維持した乾燥機あるいは釜で行な
う。この場合、雰囲気としては酸素を含まない不
活性ガスが望ましい。温度は通常200〜400℃の範
囲で行なうが、処理時間を短縮する点からはでき
るだけ温度を高くすることが有利であるる。
処理時間は処理温度と処理の程度によつて決め
られるべきものであるが、最低数分で充分に目的
を達成することが可能である。
次にここでの処理の程度は、その後の熱処理条
件あるいは溶剤への溶解性と繊維化に影響をおよ
ぼす重要な因子であり、通常密度で1.20ｇ/cm3以
上となるように処理せしめることが望ましい。こ
の程度に反応を進めると有機溶剤には不溶となる
が、硝酸、硫酸あるいはギ酸には可溶であり、こ
れらの酸に溶解して繊維化することができる。
繊維化は密度で1.20ｇ/cm3以上に反応せしめた
粉体を、濃度が約15〜30％となるよう前記の酸の
いずれかに溶解せしめ、その後凝固さらに適度な
延伸操作を行なうことによつてなし得る。
延伸条件等は得られる炭素繊維の物性に敏感に
反映されるため、適切な配向を賦与することが望
ましい。
このようにして得られた繊維は、反応の程度に
よつて着色の程度は異なるが、反応度が低い場合
の黄色から、反応の進行とともに茶色→茶褐色→
黒色という特有の色相をもつて得られる。この繊
維をついで酸化処理なしであるいは酸化処理した
後熱処理して炭素繊維とする。
すなわち熱処理は、窒素中での反応度が1.20
ｇ／cm3以上であれば酸化処理なしにいきなり不活
性雰囲気中で約1000℃以上まで昇温して炭素繊維
を得ることができる。しかし、反応度が1.20ｇ/
cm3に近いか又はそれよりも低いときには処理温度
が500〜600℃にいたるまでの昇温速度はできれば
ゆるやかにする方が炭素繊維物性の面からは好ま
しい。したがつて、場合によつては反応度が約
1.20〜1.25ｇ/cm3と低い繊維については、酸化性
雰囲気中でごく短時間処理して後の急激な炭素化
熱処理が可能となるような方法をとることもでき
る。
反応度が1.25ｇ/cm3以上であれば、現在通常に
実施されている条件と同等で、しかも酸化処理を
除いた炭素化処理のみで十分高品質の炭素繊維を
得ることができる。
現在一般的に実施されている酸化処理は熱風循
環炉を用いることが多いが、酸化処理に長時間を
要することと熱効率向上のため炉内を何往復かさ
せており、処理が煩雑となりトラブルも多く発生
する。また酸化処理は発熱を伴なうため、処理す
るトウの巾出しと温度の制御は厳しいものが要求
される等装置的な設備費も大きくなる。
一方、本発明ではそれに代る処理として不活性
雰囲気中で加熱処理を行なうが、この場合たとえ
ば密閉式の釜型装置とすれば、熱風循環炉等とは
格段に熱効率は向上し、かつ使用する不活性雰囲
気の使用もごく少量でよい。特に安価な窒素ガス
等を使用すれば不活性ガスを使用することのコス
ト的な面への影響は極めて小さくなる。加熱処理
温度も高くできることから処理時間も通常の酸化
処理の数分の１以下にすることができる。したが
つて、製造時間の短縮化と製造工程の簡略化に伴
なう炭素繊維の製造コストは現在市販されている
炭素繊維より大巾に低減できる。
以下実施によつて本発明を更に詳細に説明す
る。
実施例 １
アクリロニトリル／メチルアクリレート／メタ
クリレート酸＝95／４／１なる共重合体の粉体
を、窒素置換した乾燥機中280℃で５分、10分又
は30分間撹拌しながら加熱処理し３種の熱処理重
合体粉体を作成した。
処理後の粉体は黄色から黒褐色となつていた
が、密度はそれぞれ1.211ｇ/cm3、1.252ｇ/cm3、
1.306ｇ/cm3であつた。
この粉体を61％硝酸に溶解せしめて紡糸液を調
製した後、25％硝酸水浴中に吐出して凝固し、そ
の後沸水中で延伸して繊維を得た。
この繊維を熱酸化処理することなく、窒素中で
300℃から1300℃までの平均的昇温速度が100℃／
分となるよう昇温して炭素化した。
得られた炭素繊維は、試長25mmで単繊維引張試
験を行ない力学特性を評価したが、その結果は表
−１のごとくであつた。
The present invention relates to a method for producing carbon fibers from acrylonitrile polymers, and it is possible to omit the thermal oxidation step in the already well-known process of producing carbon fibers from acrylonitrile fibers, or to improve the process thereof. The present invention provides a method that can significantly shorten the time period. Carbon fiber is being used as a reinforcing material for resins and the like by taking advantage of its high specific strength and specific modulus, and is being used in fields that utilize its heat resistance, chemical resistance, and electrical conductivity. However, one of the biggest obstacles in the development of carbon fiber applications today is the high price, and there is a desire to develop high quality, low cost carbon fibers. High quality carbon fibers can be obtained using acrylonitrile synthetic fibers as precursors, but their production consists of two steps: a thermal oxidation process and a carbonization process.
Moreover, a particularly serious problem is that the thermal oxidation step requires a long time. Therefore, it is of great significance to shorten or omit this thermal oxidation step, and from this point of view, we investigated the manufacturing method of carbon fibers and found that after heating the polymer powder before fiberization in an inert atmosphere, By dissolving it in a solvent and making it into fibers, we have completed the present invention, which can eliminate the conventionally necessary thermal oxidation process or significantly shorten the time required for the thermal oxidation process. Acrylonitrile-based synthetic fibers are produced by polymerizing acrylonitrile monomers by solution polymerization or suspension polymerization, and then shaping them into fibers. At this time, in the case of fiber polymerization, the polymer is once pulverized, dissolved in a solvent to form a spinning solution, and then discharged into a coagulation bath to form fibers. When dissolving this polymer powder in a solvent, a drying step is required because the amount of water must be controlled. The present invention is characterized in that after this drying, the powder is efficiently heat-treated to impart appropriate infusibility. The acrylonitrile polymer used in the present invention may be one containing 80% by weight or more of acrylonitrile, and may be a copolymer of acrylonitrile and a copolymerizable monomer or a polymer consisting only of acrylonitrile. . There are no particular restrictions on the monomers that can be copolymerized, and commonly used acrylic esters such as methyl acrylate and ethyl acrylate, or unsaturated carboxylic acids such as methacrylic acid, acrylic acid, and itaconic acid. Furthermore, one or more of vinyl chloride, vinyl acetate, styrene, acrylamide, diacetone acrylamide, acrylsulfonic acid, etc. can be used. Next, heat treatment of the acrylonitrile polymer powder is carried out after the drying step of the polymer powder, particularly in a dryer or a pot maintained in an inert atmosphere. In this case, the atmosphere is preferably an inert gas that does not contain oxygen. The temperature is usually in the range of 200 to 400°C, but it is advantageous to raise the temperature as high as possible in order to shorten the processing time. Although the treatment time should be determined depending on the treatment temperature and degree of treatment, it is possible to sufficiently achieve the purpose with a minimum of several minutes. Next, the degree of treatment here is an important factor that affects the subsequent heat treatment conditions, solubility in solvents, and fiber formation, and it is usually treated to have a density of 1.20 g/cm 3 or more. desirable. When the reaction proceeds to this extent, it becomes insoluble in organic solvents, but it is soluble in nitric acid, sulfuric acid, or formic acid, and can be dissolved in these acids to form fibers. Fiberization is accomplished by dissolving the reacted powder with a density of 1.20 g/cm 3 or higher in one of the acids mentioned above to a concentration of approximately 15 to 30%, followed by solidification and appropriate stretching. It can be done. Since the stretching conditions etc. are sensitively reflected in the physical properties of the obtained carbon fiber, it is desirable to impart appropriate orientation. The degree of coloration of the fibers obtained in this way varies depending on the degree of reaction, but from yellow when the degree of reaction is low, to brown, brown, and brown as the reaction progresses.
It has a unique hue of black. This fiber is then heat treated without oxidation treatment or after oxidation treatment to obtain carbon fiber. In other words, the heat treatment reduces the reactivity in nitrogen to 1.20.
g/cm 3 or more, carbon fibers can be obtained by suddenly raising the temperature to about 1000° C. or more in an inert atmosphere without oxidation treatment. However, the reactivity is 1.20g/
When the temperature is close to or lower than cm 3 , it is preferable from the viewpoint of carbon fiber physical properties that the temperature increase rate until the treatment temperature reaches 500 to 600° C. be slow if possible. Therefore, in some cases the reactivity is approximately
For fibers with a low weight of 1.20 to 1.25 g/cm 3 , it is also possible to use a method that allows rapid carbonization heat treatment after treatment in an oxidizing atmosphere for a very short time. If the degree of reactivity is 1.25 g/cm 3 or more, carbon fibers of sufficiently high quality can be obtained under the same conditions as currently commonly used, and only by carbonization treatment excluding oxidation treatment. The oxidation treatment commonly carried out today often uses a hot air circulation furnace, but the oxidation treatment takes a long time and the furnace must be moved back and forth several times in order to improve thermal efficiency, making the treatment complicated and causing problems. Occurs often. Furthermore, since the oxidation treatment is accompanied by heat generation, strict control of the width and temperature of the tow to be treated is required, which increases equipment costs. On the other hand, in the present invention, heat treatment is performed in an inert atmosphere as an alternative treatment, but in this case, for example, if a closed pot-type device is used, the thermal efficiency is significantly improved compared to a hot air circulation furnace, etc. Only a small amount of inert atmosphere is required. In particular, if inexpensive nitrogen gas or the like is used, the cost impact of using an inert gas will be extremely small. Since the heat treatment temperature can also be increased, the treatment time can also be reduced to a fraction of that of ordinary oxidation treatment. Therefore, the manufacturing cost of carbon fiber due to shortening of manufacturing time and simplification of the manufacturing process can be significantly reduced compared to carbon fibers currently available on the market. The present invention will be explained in more detail by the following examples. Example 1 Powder of a copolymer of acrylonitrile/methyl acrylate/methacrylate acid = 95/4/1 was heat-treated at 280°C for 5 minutes, 10 minutes, or 30 minutes with stirring in a nitrogen-substituted dryer to produce three types. A heat-treated polymer powder was prepared. After treatment, the powder was yellow to blackish brown in color, with densities of 1.211g/cm 3 , 1.252g/cm 3 , and 1.252g/cm 3 , respectively.
It was 1.306g/ cm3 . This powder was dissolved in 61% nitric acid to prepare a spinning solution, then discharged into a 25% nitric acid water bath to solidify, and then stretched in boiling water to obtain fibers. This fiber is heated in nitrogen without being subjected to thermal oxidation treatment.
The average temperature increase rate from 300℃ to 1300℃ is 100℃/
Carbonization was carried out by raising the temperature to a temperature of 100 min. The obtained carbon fibers were subjected to a single fiber tensile test with a sample length of 25 mm to evaluate their mechanical properties, and the results were as shown in Table 1.
【表】
実施例 ２
実施例１で用いたアクリロニトリル系重合体粉
体を窒素中で280℃で５分処理した重合体を紡糸
して得た繊維を、炭素化に先だち、空気中270℃
で５分定長下に酸化処理を行ない、その後実施例
１と同条件で炭素化処理して炭素繊維を得た。実
施例１と同様に評価した結果は次のとおりであつ
た。
引張強度 240Kg/mm2
引張弾性率 20.2ton/mm2 [Table] Example 2 A fiber obtained by spinning the acrylonitrile polymer powder used in Example 1 at 280°C in nitrogen for 5 minutes was heated at 270°C in air prior to carbonization.
The fibers were oxidized for 5 minutes at a constant length, and then carbonized under the same conditions as in Example 1 to obtain carbon fibers. The results of evaluation in the same manner as in Example 1 were as follows. Tensile strength 240Kg/mm 2 Tensile modulus 20.2ton/mm 2
Claims (1)
気中で密度が1.20ｇ/cm3以上となるまで加熱処理
した後、溶剤に溶解して繊維化せしめた繊維状物
を熱処理することを特徴とする炭素繊維の製法。1 Carbon characterized by heat-treating acrylonitrile-based polymer powder in an inert atmosphere until the density becomes 1.20 g/cm 3 or more, and then heat-treating the fibrous material obtained by dissolving it in a solvent and making it into fibers. Fiber manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5520981A JPS57171721A (en) | 1981-04-13 | 1981-04-13 | Production of carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5520981A JPS57171721A (en) | 1981-04-13 | 1981-04-13 | Production of carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS57171721A JPS57171721A (en) | 1982-10-22 |
| JPS6314093B2 true JPS6314093B2 (en) | 1988-03-29 |
Family
ID=12992247
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5520981A Granted JPS57171721A (en) | 1981-04-13 | 1981-04-13 | Production of carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS57171721A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007018136A1 (en) | 2005-08-09 | 2007-02-15 | Toray Industries, Inc. | Flame-resistant fiber, carbon fiber, and processes for the production of both |
| WO2009078099A1 (en) | 2007-12-19 | 2009-06-25 | Toray Industries, Inc. | Dispersion containing flame-resistant polymer, flame-resistant fiber, and carbon fiber |
| JP2012522142A (en) * | 2009-03-31 | 2012-09-20 | ドンファ ユニバーシティー | Carbon fiber, its yarn, and preoxidized fiber manufacturing method |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6277933B1 (en) | 1998-04-03 | 2001-08-21 | Solutia Inc. | Polyacrylonitrile particles by surfmer polymerization and sodium removal by chemical exchange |
| US6143835A (en) * | 1998-04-03 | 2000-11-07 | Solutia Inc. | Polyacrylonitrile polymer treatment |
-
1981
- 1981-04-13 JP JP5520981A patent/JPS57171721A/en active Granted
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007018136A1 (en) | 2005-08-09 | 2007-02-15 | Toray Industries, Inc. | Flame-resistant fiber, carbon fiber, and processes for the production of both |
| US7976945B2 (en) | 2005-08-09 | 2011-07-12 | Toray Industires, Inc. | Flame resistant fiber, carbon fiber and production method thereof |
| WO2009078099A1 (en) | 2007-12-19 | 2009-06-25 | Toray Industries, Inc. | Dispersion containing flame-resistant polymer, flame-resistant fiber, and carbon fiber |
| US9006323B2 (en) | 2007-12-19 | 2015-04-14 | Toray Industries, Inc. | Dispersion containing flame-resistant polymer, flame-resistant fiber, and carbon fiber |
| JP2012522142A (en) * | 2009-03-31 | 2012-09-20 | ドンファ ユニバーシティー | Carbon fiber, its yarn, and preoxidized fiber manufacturing method |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS57171721A (en) | 1982-10-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP3933712B2 (en) | Acrylonitrile-based precursor fiber for carbon fiber, method for producing the same, and carbon fiber obtained from the precursor fiber | |
| US10745828B2 (en) | Process of making polyacrylonitrile fibers | |
| CA1040370A (en) | Process for producing carbon fibers having excellent physical properties | |
| CN102953153B (en) | A kind of preparation method of polyacrylonitrile-based carbon fibre | |
| US5804108A (en) | Process for the preparation of carbon fiber | |
| JPS6314093B2 (en) | ||
| US3733386A (en) | Process for producing acrylic synthetic fibers improved in the hydrophilicity | |
| CN102953151A (en) | Preparation method for polyacrylonitrile-based carbon fiber | |
| JP6998923B2 (en) | Flame resistant fiber, its manufacturing method, and carbon fiber manufacturing method | |
| JPS6257723B2 (en) | ||
| US3993719A (en) | Process for producing carbon fibers | |
| CN102953138B (en) | A kind of manufacture method of polyacrylonitrile base carbon fiber precursors | |
| US4154807A (en) | Process for the production of carbon fibers | |
| JP7166524B2 (en) | Carbon material precursor compact, method for producing same, and method for producing carbon material using same | |
| US4079122A (en) | Preparation of carbon fibres | |
| CA1113647A (en) | Organic polymers | |
| JPH11117123A (en) | Acrylic precursor fiber for carbon fiber excellent in resistance to pre-oxidation | |
| JP7168909B2 (en) | Precursor material for producing carbon material and method for producing carbon material using the same | |
| US12006595B2 (en) | Method for producing carbon fiber | |
| CN102953154B (en) | A kind of manufacture method of polyacrylonitrile-based carbon fibre | |
| KR0139851B1 (en) | Process for preparing acryl copolymers | |
| KR970007241B1 (en) | Process of acrylic copolymer for production of carbon fiber | |
| CN102953140B (en) | Polyacrylonitrile base carbon fiber precursors preparation method | |
| CN102953152B (en) | Preparation method for polyacrylonitrile-based carbon fiber | |
| DE3029145A1 (en) | PREPRODUCTS FOR ACRYLIC CARBON OR GRAPHITE FIBERS |