JP7234634B2 - 繊維の製造方法および炭素繊維の製造方法 - Google Patents
繊維の製造方法および炭素繊維の製造方法 Download PDFInfo
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
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- 239000011550 stock solution Substances 0.000 claims description 8
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- 239000007789 gas Substances 0.000 description 31
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- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 238000002166 wet spinning Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 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
- 230000002411 adverse Effects 0.000 description 1
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- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
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- 230000002000 scavenging effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
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- 235000005074 zinc chloride Nutrition 0.000 description 1
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/38—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated nitriles as the major constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/18—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
- D01F9/225—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles from stabilised polyacrylonitriles
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Inorganic Fibers (AREA)
Description
繊維形成性重合体がジメチルスルホキシド、ジメチルホルムアミドまたはジメチルアセトアミドである溶媒に溶解されてなる紡糸原液を紡糸口金から吐出し、一旦空気中にて走行させた後、凝固浴液中に導き凝固させる繊維の製造方法において、紡糸口金の吐出面から鉛直下向きに凝固浴液面との間に形成される気相部の単位時間当たりの風量(Af)が気相部容積(Vh)中の単位時間当たりの紡糸原液中の溶媒量(As)に対して0.0008m3≦Af/(As/Vh)≦0.0015m3の関係式を満たし、気相部における口金外周部4点での絶対湿度の1時間平均値がそれぞれ20g/m3以下で、紡糸口金の孔数が2,000以上、50,000以下であり、繊維形成性重合体がアクリロニトリル系重合体であり、紡糸原液に用いた前記溶媒と同じ溶媒の水溶液を凝固浴として用いる繊維の製造方法、である。
前記の繊維の製造方法で繊維を製造後、200~300℃の酸化性雰囲気中で耐炎化処理し、次いで1,000℃以上の不活性雰囲気中で加熱する炭素繊維の製造方法、である。
e=6.11×10(7.5T/(T+237.3))
AH=217×e/(T+273.15)×RH/100
ここで、口金外周部4点での絶対湿度の1時間平均値は、上記のとおり風速、温度、相対湿度を5分間隔で12回測定し、上記計算式を用いて絶対湿度を算出したものの各測定点の平均値である。
AH=217×e/(t+273.15)×RH/100
ここで、口金外周部4点での絶対湿度の1時間平均値は、上記のとおり風速、温度、相対湿度を5分間隔で12回測定し、上記計算式を用いて絶対湿度を算出したものの各測定点それぞれの平均値とした。
1週間連続して紡糸を続けたときの紡糸口金面の、結露の大きさ、個数を測定し、次の規準で点数換算した。
結露の直径2mm以上5mm未満:5点/個
結露の直径5mm以上:10点/個。
アクリロニトリル系繊維を巻き取る手前で1,000m分のアクリロニトリル系繊維の毛羽の数を数え、品位を5段階で評価した。評価基準は以下の通りである。
2:1<(毛羽本数/1繊維・1,000m)≦2
3:2<(毛羽本数/1繊維・1,000m)≦5
4:5<(毛羽本数/1繊維・1,000m)<60
5:60≦(毛羽本数/1繊維・1,000m)。
アクリロニトリル系繊維10t製造時の糸切れ回数から5段階で評価した。評価基準は以下の通りである。
2:1<(糸切れ回数/アクリロニトリル系繊維10t製造)≦2
3:2<(糸切れ回数/アクリロニトリル系繊維10t製造)≦3
4:3<(糸切れ回数/アクリロニトリル系繊維10t製造)<5
5:5≦(糸切れ回数/アクリロニトリル系繊維10t製造)。
アクリロニトリル99質量%、イタコン酸1質量%からなるアクリロニトリル系重合体のDMSO溶液を溶液重合により調製した。
Af/(As/Vh)を表1の通り変更し、除湿の程度を強めた以外は実施例1~4と同様にしてアクリロニトリル系前駆体繊維を得た。
Af/(As/Vh)を表1の通り変更し、9,000ホールの口金を用いた以外は実施例1~4と同様にしてアクリロニトリル系前駆体繊維を得た。
Af/(As/Vh)を表1の通り変更し、2,000ホールの口金を用いた以外は実施例1~4と同様にしてアクリロニトリル系前駆体繊維を得た。
Af/(As/Vh)を表1の通り変更し、給排気ノズルを稼働させなかった以外は、実施例1~4と同様にしてアクリロニトリル系前駆体繊維を得た。
Af/(As/Vh)を表1の通り変更した以外は、実施例1~4と同様にしてアクリロニトリル系前駆体繊維を得た。
Af/(As/Vh)を表1の通り変更し、除湿の程度を弱めた以外は、実施例1~4と同様にしてアクリロニトリル系前駆体繊維を得た。
Af/(As/Vh)を表1の通り変更し、除湿の程度をさらに弱めた以外は、実施例1~4と同様にしてアクリロニトリル系前駆体繊維を得た。
Af/(As/Vh)を表1の通り変更し供給空気は除湿しなかった以外は、実施例1~4と同様にしてアクリロニトリル系前駆体繊維を得た。
2:給気ノズル又は排気ノズル
3:凝固浴
4:風速・気流測定点A
5:風速・気流測定点B
6:風速・気流測定点C
7:風速・気流測定点D
Claims (3)
- 繊維形成性重合体がジメチルスルホキシド、ジメチルホルムアミドまたはジメチルアセトアミドである溶媒に溶解されてなる紡糸原液を紡糸口金から吐出し、一旦空気中にて走行させた後、凝固浴液中に導き凝固させる繊維の製造方法において、紡糸口金の吐出面から鉛直下向きに凝固浴液面との間に形成される気相部の単位時間当たりの風量(Af)が気相部容積(Vh)中の単位時間当たりの紡糸原液中の溶媒量(As)に対して0.0008m3≦Af/(As/Vh)≦0.0015m3の関係式を満たし、気相部における口金外周部4点での絶対湿度の1時間平均値がそれぞれ20g/m3以下で、紡糸口金の孔数が2,000以上、50,000以下であり、繊維形成性重合体がアクリロニトリル系重合体であり、紡糸原液に用いた前記溶媒と同じ溶媒の水溶液を凝固浴として用いる繊維の製造方法。
- 気相部における口金外周部4点の風速の相対標準偏差が40%以下である請求項1に記載の繊維の製造方法。
- 請求項1または2に記載の繊維の製造方法で繊維を製造後、200~300℃の酸化性雰囲気中で耐炎化処理し、次いで1,000℃以上の不活性雰囲気中で加熱する炭素繊維の製造方法。
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JP2018032781 | 2018-02-27 | ||
JP2018032781 | 2018-02-27 | ||
PCT/JP2018/040807 WO2019167344A1 (ja) | 2018-02-27 | 2018-11-02 | 繊維の製造方法および炭素繊維の製造方法 |
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US (1) | US20200407885A1 (ja) |
EP (1) | EP3760768A4 (ja) |
JP (1) | JP7234634B2 (ja) |
KR (1) | KR20200123776A (ja) |
CN (1) | CN111684114B (ja) |
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Citations (4)
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JP2007119973A (ja) | 2005-10-31 | 2007-05-17 | Teijin Techno Products Ltd | 乾湿式紡糸装置及び乾湿式紡糸方法 |
JP2010236139A (ja) | 2009-03-31 | 2010-10-21 | Toray Ind Inc | アクリル系繊維の製造方法 |
WO2018180188A1 (ja) | 2017-03-27 | 2018-10-04 | 東レ株式会社 | 繊維の製造方法および炭素繊維の製造方法 |
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JPH0544104A (ja) | 1991-08-01 | 1993-02-23 | Unitika Ltd | 乾・湿式紡糸方法 |
MY115308A (en) * | 1993-05-24 | 2003-05-31 | Tencel Ltd | Spinning cell |
JPH07292520A (ja) * | 1994-04-15 | 1995-11-07 | Toray Ind Inc | アクリル系繊維の製造方法 |
JP3808643B2 (ja) * | 1998-11-09 | 2006-08-16 | 三菱レイヨン株式会社 | アクリロニトリル系繊維束及びその製造方法 |
WO2006001324A1 (ja) * | 2004-06-25 | 2006-01-05 | Toray Industries, Inc. | 乾湿式紡糸用スピニングパック、繊維束の方向転換ガイド、ならびに、繊維束の製造装置および製造方法 |
EP1961847B1 (en) * | 2005-12-13 | 2018-02-07 | Toray Industries, Inc. | Carbon fiber, process for production of polyacrylonitrile-base precursor fiber for carbon fiber production, and process for production of carbon fiber |
JP4983261B2 (ja) * | 2006-02-07 | 2012-07-25 | 東レ株式会社 | 繊維の製造方法 |
JP5673809B2 (ja) * | 2012-03-14 | 2015-02-18 | 三菱レイヨン株式会社 | 中空状多孔質膜の製造装置および中空状多孔質膜の製造方法 |
JP6295890B2 (ja) * | 2014-08-27 | 2018-03-20 | 三菱ケミカル株式会社 | 炭素繊維束 |
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2018
- 2018-11-02 WO PCT/JP2018/040807 patent/WO2019167344A1/ja active Application Filing
- 2018-11-02 KR KR1020207019124A patent/KR20200123776A/ko not_active Application Discontinuation
- 2018-11-02 RU RU2020126570A patent/RU2020126570A/ru unknown
- 2018-11-02 JP JP2018560240A patent/JP7234634B2/ja active Active
- 2018-11-02 CN CN201880088422.5A patent/CN111684114B/zh active Active
- 2018-11-02 EP EP18908160.7A patent/EP3760768A4/en active Pending
- 2018-11-02 US US16/970,428 patent/US20200407885A1/en not_active Abandoned
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003014436A1 (en) | 2001-08-11 | 2003-02-20 | Tencel Limited | Process for the preparation of cellulosic shaped bodies |
JP2007119973A (ja) | 2005-10-31 | 2007-05-17 | Teijin Techno Products Ltd | 乾湿式紡糸装置及び乾湿式紡糸方法 |
JP2010236139A (ja) | 2009-03-31 | 2010-10-21 | Toray Ind Inc | アクリル系繊維の製造方法 |
WO2018180188A1 (ja) | 2017-03-27 | 2018-10-04 | 東レ株式会社 | 繊維の製造方法および炭素繊維の製造方法 |
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US20200407885A1 (en) | 2020-12-31 |
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CN111684114A (zh) | 2020-09-18 |
EP3760768A4 (en) | 2021-11-17 |
RU2020126570A (ru) | 2022-03-28 |
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WO2019167344A1 (ja) | 2019-09-06 |
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