JP4658194B2 - 全芳香族ポリアミドフィラメントの製造方法 - Google Patents
全芳香族ポリアミドフィラメントの製造方法 Download PDFInfo
- Publication number
- JP4658194B2 JP4658194B2 JP2008520180A JP2008520180A JP4658194B2 JP 4658194 B2 JP4658194 B2 JP 4658194B2 JP 2008520180 A JP2008520180 A JP 2008520180A JP 2008520180 A JP2008520180 A JP 2008520180A JP 4658194 B2 JP4658194 B2 JP 4658194B2
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- JP
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- Prior art keywords
- sulfuric acid
- aromatic polyamide
- wholly aromatic
- coagulating liquid
- spun
- 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 - Fee Related
Links
- 239000004760 aramid Substances 0.000 title claims description 43
- 229920003235 aromatic polyamide Polymers 0.000 title claims description 43
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000007788 liquid Substances 0.000 claims description 95
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 87
- 230000001112 coagulating effect Effects 0.000 claims description 76
- 238000009987 spinning Methods 0.000 claims description 36
- 238000002347 injection Methods 0.000 claims description 33
- 239000007924 injection Substances 0.000 claims description 33
- 238000005345 coagulation Methods 0.000 claims description 25
- 230000015271 coagulation Effects 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229920000642 polymer Polymers 0.000 claims description 22
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 8
- 238000004804 winding Methods 0.000 claims description 6
- 239000013078 crystal Substances 0.000 description 25
- 239000000047 product Substances 0.000 description 25
- 238000010438 heat treatment Methods 0.000 description 21
- 239000000523 sample Substances 0.000 description 21
- 238000005259 measurement Methods 0.000 description 16
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 12
- 238000006116 polymerization reaction Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 10
- 150000004984 aromatic diamines Chemical class 0.000 description 7
- 230000000704 physical effect Effects 0.000 description 7
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical group NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- LXEJRKJRKIFVNY-UHFFFAOYSA-N terephthaloyl chloride Chemical group ClC(=O)C1=CC=C(C(Cl)=O)C=C1 LXEJRKJRKIFVNY-UHFFFAOYSA-N 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 4
- 229910001628 calcium chloride Inorganic materials 0.000 description 4
- 239000001110 calcium chloride Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000012488 sample solution Substances 0.000 description 4
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 238000001891 gel spinning Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000006355 external stress Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- XTHPWXDJESJLNJ-UHFFFAOYSA-N sulfurochloridic acid Chemical compound OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical class ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000578 dry spinning Methods 0.000 description 1
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Images
Classifications
-
- 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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
- D01F6/605—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
-
- 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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
-
- 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
- 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
- D01D5/08—Melt spinning methods
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
-
- 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
- D01D5/08—Melt spinning methods
- D01D5/10—Melt spinning methods using organic materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
- Y10T428/2964—Artificial fiber or filament
- Y10T428/2967—Synthetic resin or polymer
- Y10T428/2969—Polyamide, polyimide or polyester
Description
紡糸した紡糸物を図1に示すように、凝固浴槽50内に通過させたことを除いては、実施例1と同一条件で処理して熱処理前及び熱処理後のポリ(パラ−フェニレンテレフタルアミド)フィラメントを製造した。
・弾性率(g/d)
・固有粘度
・結晶化度(X)
(i)サンプリング(Sampling)
(ii)測定手順
角度計(Goniometer)、連続スキャンモード(Continuous scan mode)、スキャン角度範囲(Scan angle range):10〜40°、スキャンスピード(Scan speed):2.
・見かけ上の結晶サイズ(ACS)
(i)サンプリング
(ii)測定手順
・パラ結晶パラメーター(g II )
(i)サンプリング
(ii)測定手順
20 第2凝固液噴射浴槽
30 第3凝固液噴射浴槽
11,21,31 凝固液噴射ノズル
32 水供給管
L1、L2 凝固液移送管
40 紡糸口金
50 凝固浴槽
51 凝固液受容器
60 水洗装置
70 乾燥装置
80 熱処理装置
90 巻取機
Claims (7)
- 全芳香族ポリアミド重合体を濃硫酸溶媒に溶解させて製造した紡糸原液を紡糸口金で紡糸し、紡糸した紡糸物を非凝固性流体層を通じて凝固液噴射浴槽内に通過させて全芳香族ポリアミドフィラメントを製造する方法において、
前記凝固液噴射浴槽を通過する紡糸物に、後段階に行くほど硫酸濃度が低くなる凝固液を多段階に噴射することを特徴とする全芳香族ポリアミドフィラメントの製造方法。 - 紡糸物に凝固液は2ないし5段階に噴射することを特徴とする請求項1に記載の全芳香族ポリアミドフィラメントの製造方法。
- 凝固液は硫酸水溶液及び水の中から選択された1種であることを特徴とする請求項1に記載の全芳香族ポリアミドフィラメントの製造方法。
- 紡糸物に1段階で硫酸濃度が10〜20%である硫酸水溶液を1〜10m/秒の速度で噴射し、続いて2段階で硫酸濃度が3〜10%である硫酸水溶液を13〜20m/秒の速度で噴射し、続いて3段階に水を20〜25m/秒の速度で噴射することを特徴とする請求項1に記載の全芳香族ポリアミドフィラメントの製造方法。
- 第3段階で紡糸物に噴射させた水を回収し、これを第2段階で紡糸物に噴射する硫酸水溶液として再使用することを特徴とする請求項4に記載の全芳香族ポリアミドフィラメントの製造方法。
- 第2段階で紡糸物に噴射させた硫酸水溶液を回収し、これを第1段階で紡糸物に噴射する硫酸水溶液として再使用することを特徴とする請求項4に記載の全芳香族ポリアミドフィラメントの製造方法。
- 紡糸巻取速度が1,000〜1,500m/分であることを特徴とする請求項1に記載の全芳香族ポリアミドフィラメントの製造方法。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR20050060502 | 2005-07-06 | ||
PCT/KR2006/002624 WO2007004848A1 (en) | 2005-07-06 | 2006-07-05 | Aromatic polyamide filament and method of manufacturing the same |
Related Child Applications (1)
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JP2010240405A Division JP5340246B2 (ja) | 2005-07-06 | 2010-10-27 | 全芳香族ポリアミドフィラメント |
Publications (2)
Publication Number | Publication Date |
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JP2009500534A JP2009500534A (ja) | 2009-01-08 |
JP4658194B2 true JP4658194B2 (ja) | 2011-03-23 |
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Family Applications (2)
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JP2008520180A Expired - Fee Related JP4658194B2 (ja) | 2005-07-06 | 2006-07-05 | 全芳香族ポリアミドフィラメントの製造方法 |
JP2010240405A Expired - Fee Related JP5340246B2 (ja) | 2005-07-06 | 2010-10-27 | 全芳香族ポリアミドフィラメント |
Family Applications After (1)
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JP2010240405A Expired - Fee Related JP5340246B2 (ja) | 2005-07-06 | 2010-10-27 | 全芳香族ポリアミドフィラメント |
Country Status (9)
Country | Link |
---|---|
US (2) | US7851061B2 (ja) |
EP (1) | EP1899511B1 (ja) |
JP (2) | JP4658194B2 (ja) |
KR (1) | KR100749962B1 (ja) |
CN (2) | CN101914817A (ja) |
IL (1) | IL188564A (ja) |
RU (2) | RU2382125C2 (ja) |
WO (1) | WO2007004848A1 (ja) |
ZA (1) | ZA200800097B (ja) |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
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KR100749962B1 (ko) * | 2005-07-06 | 2007-08-16 | 주식회사 코오롱 | 전방향족 폴리아미드 필라멘트 및 그의 제조방법 |
EP1899513B1 (en) * | 2005-07-06 | 2011-12-21 | Kolon Industries, Inc. | Aromatic polyamide filament |
EP2053147A1 (en) * | 2007-10-23 | 2009-04-29 | Teijin Aramid B.V. | Method for spinning and washing aramid fiber and recovering sulfuric acid |
KR100924905B1 (ko) | 2008-03-31 | 2009-11-03 | 주식회사 코오롱 | 파라 아라미드 섬유의 제조방법 |
JP5148745B2 (ja) | 2008-03-31 | 2013-02-20 | コーロン インダストリーズ インク | パラアラミド繊維及びその製造方法 |
KR101277157B1 (ko) * | 2008-04-30 | 2013-06-20 | 코오롱인더스트리 주식회사 | 아라미드 합연사의 제조방법 |
WO2010023037A1 (en) * | 2008-08-29 | 2010-03-04 | Teijin Aramid B.V. | Process for producing a plurality of high-strength, high modulus aromatic polyamide filaments |
KR101488534B1 (ko) * | 2009-01-08 | 2015-01-30 | 코오롱인더스트리 주식회사 | 폐도프 재용해장치 및 이를 이용하여 제조한 파라계 방향족폴리아미드 섬유 |
CN101988219A (zh) * | 2009-08-04 | 2011-03-23 | 上海太平洋纺织机械成套设备有限公司 | Lyocell纤维纺丝凝固成型设备 |
CN103911002A (zh) * | 2014-03-14 | 2014-07-09 | 江苏华洋尼龙有限公司 | 新型纳米聚酰胺66树脂 |
CN108728918A (zh) * | 2018-07-09 | 2018-11-02 | 睢宁县同佳化纤厂 | 一种化纤生产专用的自动喷涂化纤油导丝机 |
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KR102454479B1 (ko) * | 2021-06-17 | 2022-10-12 | 코오롱인더스트리 주식회사 | 파라계 아라미드 섬유 및 이의 제조 방법 |
CN114717745B (zh) * | 2022-03-30 | 2023-02-28 | 南通纺织丝绸产业技术研究院 | 一种混合纤网及其制备方法和应用 |
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Also Published As
Publication number | Publication date |
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ZA200800097B (en) | 2008-12-31 |
RU2008104406A (ru) | 2009-08-20 |
EP1899511A4 (en) | 2009-11-25 |
EP1899511A1 (en) | 2008-03-19 |
JP5340246B2 (ja) | 2013-11-13 |
US20100301516A1 (en) | 2010-12-02 |
EP1899511B1 (en) | 2012-10-10 |
JP2011042921A (ja) | 2011-03-03 |
CN101218381A (zh) | 2008-07-09 |
CN101218381B (zh) | 2011-05-11 |
US8834755B2 (en) | 2014-09-16 |
RU2009134171A (ru) | 2011-03-20 |
IL188564A (en) | 2012-12-31 |
WO2007004848A1 (en) | 2007-01-11 |
RU2505628C2 (ru) | 2014-01-27 |
US7851061B2 (en) | 2010-12-14 |
US20080200640A1 (en) | 2008-08-21 |
JP2009500534A (ja) | 2009-01-08 |
KR100749962B1 (ko) | 2007-08-16 |
CN101914817A (zh) | 2010-12-15 |
RU2382125C2 (ru) | 2010-02-20 |
IL188564A0 (en) | 2008-04-13 |
KR20070005504A (ko) | 2007-01-10 |
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