EP0302084B1 - Vorrichtung zum thermischen Nachbehandeln von Kohlenstoff-Fasern aus Kohlenteerpech, insbesondere Steinkohlenteerpech - Google Patents

Vorrichtung zum thermischen Nachbehandeln von Kohlenstoff-Fasern aus Kohlenteerpech, insbesondere Steinkohlenteerpech Download PDF

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Publication number
EP0302084B1
EP0302084B1 EP88900817A EP88900817A EP0302084B1 EP 0302084 B1 EP0302084 B1 EP 0302084B1 EP 88900817 A EP88900817 A EP 88900817A EP 88900817 A EP88900817 A EP 88900817A EP 0302084 B1 EP0302084 B1 EP 0302084B1
Authority
EP
European Patent Office
Prior art keywords
retort
treatment
pitch
rotating stage
lid
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 - Lifetime
Application number
EP88900817A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0302084A1 (de
Inventor
Rudolf Geier
Rolf Joest
Wilhelm WÜLLSCHEIDT
Horst Mathejka
Heinrich Patalon
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.)
Deutsche Voest Alpine Industrieanlagenbau GmbH
Original Assignee
Deutsche Voest Alpine Industrieanlagenbau GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Deutsche Voest Alpine Industrieanlagenbau GmbH filed Critical Deutsche Voest Alpine Industrieanlagenbau GmbH
Priority to AT88900817T priority Critical patent/ATE71132T1/de
Publication of EP0302084A1 publication Critical patent/EP0302084A1/de
Application granted granted Critical
Publication of EP0302084B1 publication Critical patent/EP0302084B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • 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
    • D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
    • D01F9/15—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from coal pitch
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C1/00—Working-up tar
    • 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
    • D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues

Definitions

  • a process for the production of carbon or graphite fibers or filaments from coal tar pitch is known, after which the coal tar pitch is spun from the melt and the pitch fibers obtained are subjected to oxidation, then carbonization and optionally graphitization.
  • the carbon fibers or threads spun from the pitch melt are dusted with fine ground activated carbon, which is impregnated with liquid oxidation aids, and heated in an oxidizing atmosphere to 400 ° C before carbonization.
  • the subsequent carbonization of the oxidized carbon threads takes place at a temperature of about 1000 ° C (see. DE-PS 24 19 659).
  • you want to produce carbon fibers or threads from coal tar pitch which can be oxidized and carbonized in a relatively short time.
  • the thermal aftertreatment - oxidation and carbonization of the spun pitch fibers - is time-consuming, if only because the individual process steps take place one after the other.
  • the invention has for its object to provide a device of the type described above, with which the thermal aftertreatment can be carried out extremely easily and quickly, so that the manufacture of the carbon fibers or threads is particularly efficient and economical.
  • the invention further provides that the treatment devices on the lower rotating platform are offset by 90 ° to one another and arranged on a rotating circle that projects in vertical projection Exceeds the outer circumference of the upper rotating platform for lateral passage of the treatment devices to be raised and for connecting the raised treatment devices to the respective retort cover below the retort cover receptacles, which are offset by 90 ° to one another, each treatment device being assigned its own lifting device.
  • the fiber tray is designed as a collapsible scissor gate for fiber loops hanging freely on horizontal bars and can be inserted into a treatment retort when pushed together.
  • a scissors creel enables the storage of a strand consisting of a large number of individual pitch fibers or pitch threads, in such a way that no fiber or thread sticking occurs during the thermal aftertreatment and free shrinkage is made possible.
  • coal tar pitch is freed of infusible or quinoline-insoluble components by filtration before spinning.
  • the pitch filtrate is then subjected to distillation to remove volatile or low molecular weight constituents.
  • the pitch fibers 2 spun from the pitch melt or hard pitch melt are oxidized using an oxidation aid such as activated carbon at a predetermined oxidation temperature to make them infusible.
  • the oxidized pitch fibers 2 are carbonized using an inert gas at a predetermined carbonization temperature to drive off volatile by-products.
  • Pitch filtrate is continuously introduced into a thin-film evaporator in the course of the distillation and is evenly distributed over the inner circumference by a rotating distributor ring.
  • the rotor wiper blades moving along the evaporator zone capture the pitch filtrate and spread a thin film over the heating wall.
  • the volatile product portion evaporates under the influence of an applied vacuum and is deposited on a condenser.
  • the non-evaporated part of the product, namely hard pitch leaves the thin film evaporator.
  • a vacuum pump requests the hard pitch to granulate. None of this is shown.
  • the pitch granules are melted in an extruder 3.
  • the pitch melt runs through a filter 4 and is fed to a centrifugal spinning head 6 by means of a metering pump 5.
  • the spinning centrifuge which is provided with nozzle holes on its lower part, pushes the pitch melt through the nozzle holes. Endless filaments are created, which are placed on a slowly rotating catch ring.
  • the catch ring is provided with a cutting device that cuts the continuous filaments to the desired fiber length. Since one would like to have a fuse for the subsequent thermal aftertreatment, a corresponding number of individual fibers, which result in the desired fuse cross section, are placed one above the other on the catch ring.
  • the sliver is deposited in a coiler 7.
  • the fiber sliver is deposited over deflection rollers 8 in free-hanging loops on an extended scissor gate 9.
  • the scissors gate 9 is pushed together in order to ensure a high space utilization of the oxidation furnace 10 or carbonization furnace 11 and placed in a treatment retort 12.
  • the treatment retort 12 is heated to 350 ° C.
  • the carbonization furnace 11 is lowered and heated to 1000 ° C., while the vacuum retort 13 is lifted from the basement under the treatment retort 12.
  • a vacuum unit 17 is then put into operation. After a few minutes, the vacuum retort 13 or treatment retort 12 can be released to normal pressure with nitrogen. For safety reasons, it is flushed again with nitrogen.
  • the vacuum retort 13 is then lowered back into the basement and replaced with the carbonization furnace 11, which has meanwhile been heated to 1000.degree.
  • the carbonization takes ten minutes to dwell, wherein volatile compounds are transported through preheated nitrogen via the treatment retort 12 for condensation or combustion of exhaust air.
  • the carbonization furnace 11 is shut down, the heat exchanger 15 is decommissioned and the interior of the treatment retort 12 is cooled to temperatures below 600 ° C. using cold nitrogen.
  • the scissors gate 9 can be removed, pulled apart and transported to the cooling stand, where the cooling of the carbon fibers 1 is carried out to room temperature.
  • the device for the thermal aftertreatment of the pitch fibers 2 has a lower rotating stage 18 with the oxidation furnace 10, the vacuum retort 13, the carbonization furnace 11 and a cooling retort 19. All treatment devices 10, 11, 13, 19 are designed in an open container construction for receiving treatment retorts 12. Furthermore, an upper rotating stage 20, which can be rotated independently of the lower rotating platform 18, is provided with a traversing device for treatment retorts 12 for temporarily receiving the fiber trays 9 with the pitch fibers 2 to be treated.
  • the traversing device transfers the treatment retorts 12 for connection to the respective retort cover 24 from the upper turntable 20 below the respective one Retort lid 24 and vice versa.
  • the lower turntable 18 has at least one lifting device 25 for each of the oxidation furnace 10, the vacuum retort 13, the carbonization furnace 11 and the cooling retort 19.
  • treatment devices can be moved to accommodate the treatment retorts 12 under the retort lid receptacle 23 or the relevant retort lid 24 and can be raised or vice versa.
  • the treatment devices 10, 11, 13, 19 can be displaced by 90 ° to one another on the lower rotating platform 18 and are arranged on a rotating circle which, in vertical projection, the outer periphery of the upper rotating platform 20 for passing the upper rotating platform 20 to be raised for laterally passing the treatment devices to be raised 10, 11, 13, 19 and for connecting the raised treatment facilities to the respective retort cover 24 extends below the retort cover receptacles 23, which are offset by 90 ° to one another.
  • Each treatment device 10, 11, 13, 19 is assigned its own lifting device 25, so that one of the four processes of oxidation, evacuation, carbonization and cooling can take place simultaneously under each retort lid 24.
  • At least two treatment retorts 12 offset from one another by 180 ° C. can be placed simultaneously on the upper rotating stage 20.
  • the fiber tray is designed as a collapsible scissors gate 9 for fiber loops hanging freely on horizontal bars and can be used in a retracted condition in a treatment retort 12.
  • the device operates as follows if one of the four processes of oxidation, evacuation, carbonization and cooling takes place simultaneously under each retort lid 24:
  • the upper rotating stage 20 rotates by 180 ° C. While a scissor gate 9 with finished carbon fibers 1 is removed from the other treatment retort 12, the lower rotating stage 18 rotates by 90 °, so that the cooling retort 19 against the oxidation furnace 10 is exchanged.
  • the lifting device 25 moves the oxidation furnace 10 - a low-temperature furnace - from below over the treatment retort 12.
  • hot oxidation air is passed through the treatment retort 12 and the oxidation furnace 10 is heated up in accordance with the optimized temperature profile.
  • the hot process gases are fed to the exhaust air cleaning system.
  • the vacuum retort 13 is lifted from below over the treatment retort 12 via the lifting device 25.
  • the vacuum applied evacuates the oxidation furnace 10.
  • the treatment retort 12 is still flushed with nitrogen while relieving pressure.
  • the vacuum retort 13 is moved down to the lower rotating platform 18.
  • Fig. 12 The carbonization furnace 11 is moved from below via the treatment retort 12 by means of the lifting device 25. During the subsequent carbonization process, preheated nitrogen is passed through treatment retort 12 and transports the volatile compounds to the exhaust system.
  • the lower rotating stage 18 rotates by 90 °, so that the cooling retort 19 comes to rest under the treatment retort 12.
  • the pitch fibers 2 are cooled to temperatures below 600 ° C. by supplying cold nitrogen.
  • the further cooling can take place in the cooling station 19 with cold air.
  • the pitch fibers obtained were heated in an oxidation oven 10 in 16 minutes to an oxidation temperature of 340 ° C.
  • a critical oxidation range (softening point ⁇ 25 ° C) was run through with a maximum heating rate of 20 ° C / min.
  • the air flow rate was 2000 to 3000 1 / h.
  • the pitch fibers 2 did not fuse during the oxidation and also showed no external damage.
  • the infusibility achieved allowed subsequent rapid carbonization using the usual method.
  • activated carbon (without H2SO4) was used as an oxidation aid.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Fibers (AREA)
  • Working-Up Tar And Pitch (AREA)
  • Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
  • Peptides Or Proteins (AREA)
EP88900817A 1987-02-07 1988-01-05 Vorrichtung zum thermischen Nachbehandeln von Kohlenstoff-Fasern aus Kohlenteerpech, insbesondere Steinkohlenteerpech Expired - Lifetime EP0302084B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88900817T ATE71132T1 (de) 1987-02-07 1988-01-05 Vorrichtung zum thermischen nachbehandeln von kohlenstoff-fasern aus kohlenteerpech, insbesondere steinkohlenteerpech.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3703825 1987-02-07
DE19873703825 DE3703825A1 (de) 1987-02-07 1987-02-07 Verfahren und vorrichtung zum herstellen von kohlenstoff-fasern

Publications (2)

Publication Number Publication Date
EP0302084A1 EP0302084A1 (de) 1989-02-08
EP0302084B1 true EP0302084B1 (de) 1992-01-02

Family

ID=6320505

Family Applications (1)

Application Number Title Priority Date Filing Date
EP88900817A Expired - Lifetime EP0302084B1 (de) 1987-02-07 1988-01-05 Vorrichtung zum thermischen Nachbehandeln von Kohlenstoff-Fasern aus Kohlenteerpech, insbesondere Steinkohlenteerpech

Country Status (10)

Country Link
EP (1) EP0302084B1 (enrdf_load_stackoverflow)
CN (1) CN88100656A (enrdf_load_stackoverflow)
AT (1) ATE71132T1 (enrdf_load_stackoverflow)
AU (1) AU1103888A (enrdf_load_stackoverflow)
DD (1) DD279907A5 (enrdf_load_stackoverflow)
DE (2) DE3703825A1 (enrdf_load_stackoverflow)
ES (1) ES2006553A6 (enrdf_load_stackoverflow)
GR (1) GR1000124B (enrdf_load_stackoverflow)
IN (1) IN168504B (enrdf_load_stackoverflow)
WO (1) WO1988005805A1 (enrdf_load_stackoverflow)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GR1000326B (el) * 1988-02-05 1992-06-25 Didier Eng Μηχανικη διαταξη για την παραγωγη ινων ανθρακα.
DE3829986A1 (de) * 1988-09-03 1990-03-15 Enka Ag Verfahren zur erhoehung des mesophasenanteils in pech
US5427908A (en) * 1990-05-01 1995-06-27 Affymax Technologies N.V. Recombinant library screening methods
ES2099256T3 (es) * 1990-11-01 1997-05-16 Ashland Inc Procedimientos de fabricacion mejorados de fibras de carbono y brea enriquecida.
CN100402419C (zh) * 2006-08-02 2008-07-16 太原理工大学 一种以煤焦油沥青为原料制备纳米碳纤维的方法
CN103361096B (zh) * 2012-04-10 2014-12-03 上海宝钢化工有限公司 一种生产通用级碳纤维的高软化点沥青的制备方法
CN102912477B (zh) * 2012-11-13 2016-09-28 重庆科燃科技有限公司 一种聚丙烯腈基碳纤维生产设备
DE102013208426A1 (de) 2013-05-07 2014-11-13 Bayerische Motoren Werke Aktiengesellschaft Verfahren und Vorrichtung zur Verarbeitung von Carbonfasersträngen
CN105839213B (zh) * 2016-06-13 2019-05-17 天津工业大学 一种沥青炭纤维原丝熔融纺丝机
CN111849530B (zh) * 2020-07-30 2021-12-03 贵州省煤炭产品质量监督检验院 煤焦油深度处理加工系统

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB850880A (en) * 1957-10-16 1960-10-12 Gelsenkirchener Bergwerks Ag Process and apparatus for the continuous production of pitch
US3718493A (en) * 1968-06-04 1973-02-27 Great Lakes Carbon Corp Process for the production of carbon filaments from coal tar pitch
BE759139A (fr) * 1970-02-20 1971-04-30 Mitsubishi Oil Co Procede de fabrication d'une fibre au carbone
US3895447A (en) * 1973-05-10 1975-07-22 Vaportech Corp Apparatus for treating cellulosic-containing articles to render them crease resistant
JPS6057478B2 (ja) * 1978-06-28 1985-12-14 呉羽化学工業株式会社 炭素繊維用ピツチの製造法
IT1137958B (it) * 1981-06-26 1986-09-10 Manifattura Tintoria & Trasfor Procedimento per la tintura di fascio di fibre strappato,apparecchiatura per la sua realizzazione e prodotto cosi'ottenuto
US4497789A (en) * 1981-12-14 1985-02-05 Ashland Oil, Inc. Process for the manufacture of carbon fibers
JPS58220805A (ja) * 1982-06-15 1983-12-22 Nippon Oil Co Ltd 炭素繊維用前駆体ピツチの製造方法
DE3509861C2 (de) * 1984-03-26 1986-03-06 Idemitsu Kosan Co. Ltd., Tokio/Tokyo Pechmaterial für einen kohlenstoffhaltigen Formkörper und Verfahren zu seiner Herstellung
US4550579A (en) * 1984-04-13 1985-11-05 Frank Clifford G Apparatus for the dyeing of shaped articles

Also Published As

Publication number Publication date
EP0302084A1 (de) 1989-02-08
CN88100656A (zh) 1988-08-17
GR880100060A (en) 1988-12-16
DE3703825C2 (enrdf_load_stackoverflow) 1991-11-21
GR1000124B (el) 1991-07-31
AU1103888A (en) 1988-08-24
WO1988005805A1 (en) 1988-08-11
DE3703825A1 (de) 1988-08-18
DE3867365D1 (de) 1992-02-13
ATE71132T1 (de) 1992-01-15
IN168504B (enrdf_load_stackoverflow) 1991-04-13
DD279907A5 (de) 1990-06-20
ES2006553A6 (es) 1989-05-01

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