JP2014025167A5 - - Google Patents
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- JP2014025167A5 JP2014025167A5 JP2012166593A JP2012166593A JP2014025167A5 JP 2014025167 A5 JP2014025167 A5 JP 2014025167A5 JP 2012166593 A JP2012166593 A JP 2012166593A JP 2012166593 A JP2012166593 A JP 2012166593A JP 2014025167 A5 JP2014025167 A5 JP 2014025167A5
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- fiber bundle
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- 239000000835 fiber Substances 0.000 claims description 57
- 239000002245 particle Substances 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 15
- 239000004917 carbon fiber Substances 0.000 claims description 15
- 239000010419 fine particle Substances 0.000 claims description 9
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 8
- 230000001590 oxidative Effects 0.000 claims description 7
- 229920002456 HOTAIR Polymers 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910052803 cobalt Inorganic materials 0.000 claims description 4
- 238000010924 continuous production Methods 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- 230000003746 surface roughness Effects 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 239000003063 flame retardant Substances 0.000 description 2
Description
但し、（式１）において、
Ｄ：前記熱処理炉内に存在する粒径０．３μｍ以上の微粒子の濃度［個／リットル］
Ｗ：以下に定義される繊維束の幅［ｃｍ／ストランド］
Ｖ：繊維束を通過する循環熱風の風速［ｍ／秒］
Ｌ：繊維束が通過する炉長をＬ［ｍ］
Ｓ：繊維束の炉内通過速度［ｍ／分］である。
（２）熱処理炉内を循環する酸化性気体に含まれる粒径０．３μｍ以上の微粒子の濃度を、集塵装置を用いて３００〜６００個／リットルに保つ、（１）に記載の耐炎化繊維束の製造方法。
（３）（１）または（２）に記載の方法で得られた耐炎化繊維束を、不活性雰囲気下、１２００℃以上で加熱処理することを特徴とする炭素繊維束の製造方法。
（４）（１）または（２）に記載の方法で得られた耐炎化繊維束であって、単糸繊度が１．０ｄｔｅｘ以下の耐炎化繊維束を、不活性雰囲気下、１３００℃以上で加熱処理することを特徴とする炭素繊維束の製造方法。
（５）ポリアクリロニトリル系繊維束を、酸化性気体を循環する熱処理炉で２００〜３００℃で加熱して得られる、単糸直径が６〜１３μｍ、単糸の算術平均表面粗さＲａが１〜２０ｎｍ、単糸繊度が０．４〜１．７ｄｔｅｘ、以下に定義される繊維束の糸幅が１糸条あたり０．５〜１．０ｃｍ、密度が１．３４〜１．４０ｇ／ｃｍ３の耐炎化繊維束であって、以下に定義される単糸表面に観察されるＳｉ、Ｃ、Ｎａ、Ｍｇ、Ａｌ、Ｋ、Ｃａ、Ｍｎ、Ｆｅ、Ｃｏ、Ｎｉ、Ｚｎのいずれかを主成分とし、かつ粒径が０．３μｍ以上である微粒子の個数と、以下に定義される０．３μｍ以上の単糸表面の傷の個数の合計が、観察面積０．１ｍｍ２あたり１５個以下であることを特徴とする耐炎化繊維束。
（６）粒径０．３μｍ以上の微粒子の個数が３００〜２５００個／リットルである酸化性気体を、アミノ変性シリコーンを含むシリコーン系油剤が付与されたポリアクリロニトリル系繊維束の走行方向と垂直に循環させる熱処理炉で、該ポリアクリロニトリル系繊維束を２００〜３００℃で加熱処理をするに際し、
［Ｄ×（Ｗ×Ｖ×Ｌ）］／［（Ｓ／６０）×１０５］ （式１）
の値が５〜４０である条件下で加熱処理することによって、単糸直径が６〜１３μｍ、以下に定義される繊維束の糸幅が１糸条あたり０．５〜１．０ｃｍ、密度が１．３４〜１．４０ｇ／ｃｍ３の耐炎化繊維束を得る方法であって、該耐炎化繊維束は、以下に定義される単糸表面に観察されるＳｉ、Ｃ、Ｎａ、Ｍｇ、Ａｌ、Ｋ、Ｃａ、Ｍｎ、Ｆｅ、Ｃｏ、Ｎｉ、Ｚｎのいずれかを主成分とし、かつ粒径が０．３μｍ以上である微粒子の個数と、以下に定義される０．３μｍ以上の単糸表面の傷の個数の合計が観察面積０．１ｍｍ２あたり１５個以下であることを特徴とする耐炎化繊維束の製造方法。
但し、（式１）において、
Ｄ：前記熱処理炉内に存在する粒径０．３μｍ以上の微粒子の濃度［個／リットル］
Ｗ：以下に定義される繊維束の幅［ｃｍ／ストランド］
Ｖ：繊維束を通過する循環熱風の風速［ｍ／秒］
Ｌ：繊維束が通過する炉長をＬ［ｍ］
Ｓ：繊維束の炉内通過速度［ｍ／分］である。
（７）前記耐炎化繊維束の単糸の算術平均表面粗さＲａが１〜２０ｎｍ、単糸繊度が０．４〜１．７ｄｔｅｘである（６）に記載の耐炎化繊維束の製造方法。
（８）（６）または（７）に記載の方法で得られた耐炎化繊維束を、不活性雰囲気下、１２００℃以上で加熱処理する炭素繊維束の製造方法であって、該炭素繊維束は、耐炎化炉を清掃せずに連続生産する全期間において引張強度が４．７ＧＰａ以上、引張弾性率が２００ＧＰａ以上であることを特徴とする炭素繊維束の製造方法。
（９）（６）または（７）に記載の方法で得られた耐炎化繊維束であって、単糸繊度が１．０ｄｔｅｘ以下の耐炎化繊維束を、不活性雰囲気下、１３００℃以上で加熱処理する炭素繊維束の製造方法であって、該炭素繊維束は、耐炎化炉を清掃せずに連続生産する全期間において引張強度が５．５ＧＰａ以上、引張弾性率が２８０ＧＰａ以上であることを特徴とする炭素繊維束の製造方法。
However, in (Formula 1):
D: Concentration of particles having a particle size of 0.3 μm or more existing in the heat treatment furnace [piece / liter]
W: width of the fiber bundle defined below (cm / strand)
V: Wind speed of circulating hot air passing through the fiber bundle [m / sec]
L: The furnace length through which the fiber bundle passes is L [m]
S: The passing speed of the fiber bundle in the furnace [m / min].
(2) The flame resistance according to (1), wherein the concentration of fine particles having a particle size of 0.3 μm or more contained in the oxidizing gas circulating in the heat treatment furnace is maintained at 300 to 600 particles / liter using a dust collector. A method of manufacturing a fiber bundle.
(3) A method for producing a carbon fiber bundle, comprising heat-treating the flame-resistant fiber bundle obtained by the method according to (1) or (2) at 1200 ° C. or higher in an inert atmosphere.
(4) A flame-resistant fiber bundle obtained by the method according to (1) or (2), wherein the flame-resistant fiber bundle having a single yarn fineness of 1.0 dtex or less is 1300 ° C. or higher in an inert atmosphere. A method for producing a carbon fiber bundle, characterized by heat treatment.
(5) A polyacrylonitrile fiber bundle is obtained by heating at 200 to 300 ° C. in a heat treatment furnace in which an oxidizing gas is circulated. The single yarn diameter is 6 to 13 μm, and the arithmetic average surface roughness Ra of the single yarn is 1 to 1. 20 nm, single yarn fineness is 0.4 to 1.7 dtex, the fiber width of the fiber bundle defined below is 0.5 to 1.0 cm per yarn, and the density is 1.34 to 1.40 g / cm 3 . Flame retardant fiber bundle, which is mainly composed of any one of Si, C, Na, Mg, Al, K, Ca, Mn, Fe, Co, Ni, and Zn observed on the surface of the single yarn defined below. The total number of fine particles having a particle size of 0.3 μm or more and the number of scratches on the surface of a single yarn of 0.3 μm or more defined below is 15 or less per observation area of 0.1 mm 2. Flame retardant fiber bundle characterized by .
(6) An oxidizing gas in which the number of fine particles having a particle size of 0.3 μm or more is 300 to 2500 / liter is perpendicular to the running direction of the polyacrylonitrile fiber bundle to which the silicone oil containing amino-modified silicone is applied. When the polyacrylonitrile fiber bundle is heat-treated at 200 to 300 ° C. in a circulating heat treatment furnace,
[D × (W × V × L)] / [(S / 60) × 10 5 ] (Formula 1)
By performing heat treatment under the condition of a value of 5 to 40, the single yarn diameter is 6 to 13 μm, the yarn width of the fiber bundle defined below is 0.5 to 1.0 cm per yarn, and the density is 1. A method of obtaining a flame-resistant fiber bundle of 1.34 to 1.40 g / cm 3, wherein the flame-resistant fiber bundle is observed on the surface of a single yarn defined below, Si, C, Na, Mg, Al , K, Ca, Mn, Fe, Co, Ni, Zn, and the number of fine particles having a particle size of 0.3 μm or more and the surface of a single yarn of 0.3 μm or more as defined below The total number of scratches is 15 or less per observation area of 0.1 mm 2 .
However, in (Formula 1):
D: Concentration of particles having a particle size of 0.3 μm or more existing in the heat treatment furnace [piece / liter]
W: width of the fiber bundle defined below (cm / strand)
V: Wind speed of circulating hot air passing through the fiber bundle [m / sec]
L: The furnace length through which the fiber bundle passes is L [m]
S: The passing speed of the fiber bundle in the furnace [m / min].
(7) The method for producing a flame-resistant fiber bundle according to (6) , wherein the arithmetic average surface roughness Ra of the single yarn of the flame-resistant fiber bundle is 1 to 20 nm and the single yarn fineness is 0.4 to 1.7 dtex.
(8) A method for producing a carbon fiber bundle, wherein the flame-resistant fiber bundle obtained by the method according to (6) or (7) is heat-treated at 1200 ° C. or higher in an inert atmosphere, the carbon fiber bundle Is a method for producing a carbon fiber bundle, wherein the tensile strength is 4.7 GPa or more and the tensile elastic modulus is 200 GPa or more over the entire period of continuous production without cleaning the flameproofing furnace.
(9) A flame-resistant fiber bundle obtained by the method according to (6) or (7) , wherein the flame-resistant fiber bundle having a single yarn fineness of 1.0 dtex or less is 1300 ° C. or higher in an inert atmosphere. A method for producing a carbon fiber bundle to be heat-treated, wherein the carbon fiber bundle has a tensile strength of 5.5 GPa or more and a tensile elastic modulus of 280 GPa or more over the entire period of continuous production without cleaning the flameproofing furnace. A method for producing a carbon fiber bundle characterized by the above.
Claims (9)
［Ｄ×（Ｗ×Ｖ×Ｌ）］／［（Ｓ／６０）×１０５］ （式１）
の値が５〜４０である条件下で加熱処理することを特徴とする耐炎化繊維束の製造方法。
但し、（式１）において、
Ｄ：前記熱処理炉内に存在する粒径０．３μｍ以上の微粒子の濃度［個／リットル］
Ｗ：明細書中に定義される繊維束の幅［ｃｍ／ストランド］
Ｖ：繊維束を通過する循環熱風の風速［ｍ／秒］
Ｌ：繊維束が通過する炉長をＬ［ｍ］
Ｓ：繊維束の炉内通過速度［ｍ／分］ A single yarn fineness of 0.4 to 1.6 dtex, a filament number of 1000, to which an oxidizing gas having a concentration of fine particles having a particle size of 0.3 μm or more of 300 to 2500 / liter, a silicone-based oil containing amino-modified silicone is applied. When heat-treating the polyacrylonitrile fiber bundle at 200 to 300 ° C. in a heat treatment furnace that circulates in a direction perpendicular to the traveling direction of -80000 polyacrylonitrile fiber bundles,
[D × (W × V × L)] / [(S / 60) × 10 5 ] (Formula 1)
A method for producing a flame-resistant fiber bundle, wherein the heat treatment is carried out under the condition of a value of 5 to 40.
However, in (Formula 1):
D: Concentration of particles having a particle size of 0.3 μm or more existing in the heat treatment furnace [piece / liter]
W: width of the fiber bundle defined in the specification [cm / strand]
V: Wind speed of circulating hot air passing through the fiber bundle [m / sec]
L: The furnace length through which the fiber bundle passes is L [m]
S: Passing speed of the fiber bundle in the furnace [m / min]
［Ｄ×（Ｗ×Ｖ×Ｌ）］／［（Ｓ／６０）×１０５］ （式１）
の値が５〜４０である条件下で加熱処理することによって、単糸直径が６〜１３μｍ、明細書中に定義される繊維束の糸幅が１糸条あたり０．５〜１．０ｃｍ、密度が１．３４〜１．４０ｇ／ｃｍ３の耐炎化繊維束を得る方法であって、該耐炎化繊維束は、明細書中に定義される単糸表面に観察されるＳｉ、Ｃ、Ｎａ、Ｍｇ、Ａｌ、Ｋ、Ｃａ、Ｍｎ、Ｆｅ、Ｃｏ、Ｎｉ、Ｚｎのいずれかを主成分とし、かつ粒径が０．３μｍ以上である微粒子の個数と、明細書中に定義される０．３μｍ以上の単糸表面の傷の個数の合計が観察面積０．１ｍｍ２あたり１５個以下であることを特徴とする耐炎化繊維束の製造方法。
但し、（式１）において、
Ｄ：前記熱処理炉内に存在する粒径０．３μｍ以上の微粒子の濃度［個／リットル］
Ｗ：明細書中に定義される繊維束の幅［ｃｍ／ストランド］
Ｖ：繊維束を通過する循環熱風の風速［ｍ／秒］
Ｌ：繊維束が通過する炉長をＬ［ｍ］
Ｓ：繊維束の炉内通過速度［ｍ／分］ Heat treatment in which an oxidizing gas having a number of fine particles having a particle size of 0.3 μm or more of 300 to 2500 / liter is circulated in a direction perpendicular to the running direction of the polyacrylonitrile fiber bundle to which the silicone oil containing amino-modified silicone is applied. When the polyacrylonitrile fiber bundle is heat-treated at 200 to 300 ° C. in a furnace,
[D × (W × V × L)] / [(S / 60) × 10 5 ] (Formula 1)
By performing the heat treatment under the condition of a value of 5 to 40, the single yarn diameter is 6 to 13 μm, and the yarn width of the fiber bundle defined in the specification is 0.5 to 1.0 cm per yarn, A method for obtaining a flame-resistant fiber bundle having a density of 1.34 to 1.40 g / cm 3, wherein the flame-resistant fiber bundle is observed on the surface of a single yarn as defined in the specification. , Mg, Al, K, Ca, Mn, Fe, Co, Ni, Zn, and the number of fine particles having a particle size of 0.3 μm or more as defined in the specification. A method for producing a flame-resistant fiber bundle, wherein the total number of scratches on the surface of a single yarn of 3 μm or more is 15 or less per observation area of 0.1 mm 2 .
However, in (Formula 1):
D: Concentration of particles having a particle size of 0.3 μm or more existing in the heat treatment furnace [piece / liter]
W: width of the fiber bundle defined in the specification [cm / strand]
V: Wind speed of circulating hot air passing through the fiber bundle [m / sec]
L: The furnace length through which the fiber bundle passes is L [m]
S: Passing speed of the fiber bundle in the furnace [m / min]
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2012166593A JP6064409B2 (en) | 2012-07-27 | 2012-07-27 | Method for producing flame-resistant fiber bundle and method for producing carbon fiber bundle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2012166593A JP6064409B2 (en) | 2012-07-27 | 2012-07-27 | Method for producing flame-resistant fiber bundle and method for producing carbon fiber bundle |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| JP2014025167A JP2014025167A (en) | 2014-02-06 |
| JP2014025167A5 true JP2014025167A5 (en) | 2015-08-27 |
| JP6064409B2 JP6064409B2 (en) | 2017-01-25 |
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| JP (1) | JP6064409B2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP6852405B2 (en) * | 2017-01-10 | 2021-03-31 | 東レ株式会社 | Manufacturing method of carbon fiber bundle |
| JP7322327B2 (en) * | 2017-12-21 | 2023-08-08 | 東レ株式会社 | Carbon fiber bundle and its manufacturing method |
| JP7354840B2 (en) * | 2018-09-28 | 2023-10-03 | 東レ株式会社 | Method for producing flame-resistant fiber bundles and method for producing carbon fiber bundles |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11241230A (en) * | 1997-12-11 | 1999-09-07 | Toray Ind Inc | Carbon fiber, precursor fiber for carbon fiber, composite material and production of carbon fiber |
| JP2007314901A (en) * | 2006-05-24 | 2007-12-06 | Toray Ind Inc | Method for producing carbon fiber |
| JP4809757B2 (en) * | 2006-12-07 | 2011-11-09 | 三菱レイヨン株式会社 | Flame-resistant heat treatment apparatus and method for producing flame-resistant fiber bundle |
| JP5022073B2 (en) * | 2007-03-20 | 2012-09-12 | 三菱レイヨン株式会社 | Flameproofing furnace and carbon fiber manufacturing method |
| JP2010133059A (en) * | 2008-12-05 | 2010-06-17 | Mitsubishi Rayon Co Ltd | Flameproofing furnace, and method for producing carbon fiber using the same |
| JP2010222723A (en) * | 2009-03-23 | 2010-10-07 | Toray Ind Inc | Flameproof fiber bundle and method for producing carbon fiber |
| JP5667380B2 (en) * | 2010-05-19 | 2015-02-12 | 東邦テナックス株式会社 | Flame-resistant fiber bundle, carbon fiber bundle, and production method thereof |
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