EP0302084B1 - Apparatus for thermal aftertreatment of carbon fibres from coaltar pitch, in particular from glance- (hard)- coaltar pitch - Google Patents

Apparatus for thermal aftertreatment of carbon fibres from coaltar pitch, in particular from glance- (hard)- coaltar pitch 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
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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
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EP88900817A
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German (de)
French (fr)
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EP0302084A1 (en
Inventor
Rudolf Geier
Rolf Joest
Wilhelm WÜLLSCHEIDT
Horst Mathejka
Heinrich Patalon
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Deutsche Voest Alpine Industrieanlagenbau GmbH
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Deutsche Voest Alpine Industrieanlagenbau GmbH
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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
    • 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.

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  • 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)

Abstract

In a process for producing carbon fibres from coal tar pitch, the coal tar pitch is filtered before being spun and the pitch filtrate is distilled in a thin-film evaporator in order to increase its softening point over 260 C. A pure and homogeneous hard pitch is thus obtained, without the re-formation of infusable, chinolin-insoluble components. The most difficult and cost intensive step of the fibre production process, namely the thermal aftertreatment of the spun pitch fibres, can thus be easily and quickly carried out. The subsequent thermal treatment is carried out in a cyclic treatment installation.

Description

Die Erfindung betrifft eine Vorrichtung zum thermischen Nachbehandeln von Kohlenstoff-Fasern aus Kohlenteerpech, insbesondere Steinkohlenteerpech, mit zumindest einer Faserablage, einem Oxidationsofen und einem Carbonisationsofen.

  • Die Erfindung umfaßt in gleicher Weise die Nachbehandlung von Kohlenstoff-Fäden. Aus den Kohlenstoff-Fasern oder
  • Fäden lassen sich in bekannter Weise auch Graphitfasern oder -fäden herstellen.
The invention relates to a device for the thermal aftertreatment of carbon fibers from coal tar pitch, in particular coal tar pitch, with at least one fiber deposit, an oxidation furnace and a carbonization furnace.
  • In the same way, the invention comprises the aftertreatment of carbon threads. From the carbon fibers or
  • Threads can also be produced in a known manner graphite fibers or threads.

Es ist ein Verfahren zur Herstellung von Kohlenstoff- oder Graphitfasern oder -fäden aus Kohlenteerpech bekannt, wonach man das Kohlenteerpech aus der Schmelze verspinnt und die erhaltenen Pechfasern einer Oxidation, dann einer Carbonisierung und ggf. Graphitierung unterwirft. Die aus der Pechschmelze versponnenen Kohlenstoff-Fasern bzw. -Fäden werden vor der Carbonisierung -mit fein gemahlener Aktivkohle, die mit flüssigen Oxidationshilfsmitteln imprägniert ist, bestäubt und in oxidierender Atmosphäre bis auf 400° C erhitzt Die nachfolgende Carbonisierung der oxidierten Kohlenstoff-Fäden erfolgt bei einer Temperatur von ca. 1000° C (vgl. DE-PS 24 19 659). Auf diese Weise will man Kohlenstoff-Fasern bzw. -Fäden aus Kohlenteerpech herstellen, die in verhältnismäßig kurzer Zeit oxidiert und carbonisiert werden können. Tatsächlich ist die thermische Nachbehandlung - Oxidation und Carbonisierung der ersponnenen Pechfasern - jedoch zeitaufwendig, schon weil die einzelnen Prozeßstufen nacheinander ablaufen.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). In this way, you want to produce carbon fibers or threads from coal tar pitch, which can be oxidized and carbonized in a relatively short time. In fact, 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.

Der Erfindung liegt die Aufgabe zugrunde, eine Vorrichtung der eingangs beschriebenen Art zu schaffen, mit der sich die thermische Nachbehandlung extrem einfach und schnell durchführen läßt, so daß die Herstellung der Kohlenstoff-Fasern bzw. -Fäden im ganzen besonders rationell und wirtschaftlich wird.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.

Zur Lösung dieser Aufgabe ist die gattungsgemäße Vorrichtung gekennzeichnet durch

  • eine untere Drehbühne mit dem Oxidationsofen, einer Vakuumretorte, dem Carbonisationsofen und einer Kühlretorte, sämtliche Behandlungseinrichtungen in oben offener Behälterbauweise,
  • eine unabhängig von der unteren Drehbühne drehbare obere Drehbühne mit einer Changiereinrichtung für Behandlungsretorten zur vorübergehenden Aufnahme der Faserablage bzw. Faserablagen mit den zu behandelnden Pechfasern,
  • eine Beschickungsebene oberhalb der oberen Drehbühne mit zumindest einer Beschickungsöffnung und zumindest einer Retortendeckelaufnahme für Retortendeckel mit Anschluß für Luft- und Inertgaszufuhr, Vakuum und Abluft,
wobei die Changiereinrichtung die Behandlungsretorten zum Abschluß an den jeweiligen Retortendeckel von der oberen Drehbühne unter dem betreffenden Retortendeckel überführt und umgekehrt, und wobei die untere Drehbühne zumindest eine Hubvorrichtung für jeweils den Oxidationsofen, die Vakuum, retorte, den Carbonisationsofen und die Kühlretorte aufweist und diese Behandlungseinrichtungen zur Aufnahme der Behandlungsretorten unter die Retortendeckelaufnahme bzw. den betreffenden Retortendeckel verfahrbar und hochfahrbar sind sowie umgekehrt. - Im Zuge der thermischen Nachbehandlung der Pechfasern zu Kohlenstoff-Fasern werden sehr kurze Verweilzeiten sowie ein äußerst geringer Inertgas- und Energieverbrauch erreicht. Tatsächlich läßt sich die thermische Nachbehandlungszeit und insbesondere Oxidationszeit sowie Carbonisationszeit erheblich verkürzen, schon weil die verschiedenen Prozeßstufen in der erfindungsgemäßen Vorrichtung gleichzeitig ablaufen können. Im Ergebnis entstehen in wirtschaftlicher Hinsicht rationell gefertigte Kohlenstoff-Fasern bzw. -Fäden von hoher Qualität und insbesondere Zugfestigeit.To solve this problem, the generic device is characterized by
  • a lower revolving stage with the oxidation furnace, a vacuum retort, the carbonization furnace and a cooling retort, all treatment facilities in an open container design,
  • an upper revolving stage that can be rotated independently of the lower revolving stage with a traversing device for treatment retorts for the temporary reception of the fiber deposition or fiber depositions with the pitch fibers to be treated,
  • a loading level above the upper revolving platform with at least one loading opening and at least one retort lid receptacle for retort lid with connection for air and inert gas supply, vacuum and exhaust air,
wherein the traversing device transfers the treatment retorts to the respective retort lid from the upper revolving platform under the relevant retort lid and vice versa, and wherein the lower revolving stage has at least one lifting device for each of the oxidation furnace, the vacuum, retort, the carbonization furnace and the cooling retort and these treatment devices for receiving the treatment retorts can be moved and raised under the retort lid receptacle or the relevant retort lid and vice versa. - In the course of the thermal aftertreatment of the pitch fibers to carbon fibers, very short residence times and extremely low inert gas and energy consumption are achieved. In fact, the thermal aftertreatment time and in particular the oxidation time and carbonization time can be shortened considerably, if only because the different process stages in the device according to the invention can take place simultaneously. As a result, economically produced carbon fibers or threads of high quality and especially tensile strength are produced.

Damit gleichzeitig unter jedem Retortendeckel jeweils einer der vier Prozesse Oxidation, Evakuierung, Carbonisation und Kühlung ablaufen kann, sieht die Erfindung weiter vor, daß die Behandlungseinrichtungen auf der unteren Drehbühne um 90° zueinander versetzt und auf einem Drehkreis angeordnet sind, der in vertikaler Projektion den Außenumfang der oberen Drehbühne zum seitlichen Passieren der hochzufahrenden Behandlungseinrichtungen übersteigt und zum Anschluß der hochgefahrenen Behandlungseinrichtungen an den jeweiligen Retortendeckel unterhalb der in gleicher Weise um 90° zueinander versetzten Retortendeckelaufnahmen verläuft, wobei jeder Behandlungseinrichtung eine eigene Hubvorrichtung zugeordnet ist. Auf die obere Drehbühne sind zumindest zwei um 180° zueinander versetzte Behandlungsretorten gleich- zeitig aufsetzbar, damit dem Behandlungssystem wechselweise eine Behandlungsretorte mit zu behandelnden Pechfasern zugeführt und einer Behandlungsretorte mit fertig behandelten Kohlenstoff-Fasern abgeführt werden kann. Nach einer bevor- zugten Ausführungsform der Erfindung ist vorgesehen, daß die Faserablage als zusammenschiebbares Scherengatter für an waagerechten Stäben freihängende Faserschlaufen ausgebildet und in zusammengeschobenem Zustand in eine Behandlungsretorte einsetzbar ist. Ein derartiges Scherengatter ermöglicht die Ablage eines aus einer Vielzahl einzelner Pechfasern oder Pechfäden bestehenden Stranges, und zwar derart, daß während der thermischen Nachbehandlung keine Faser- bzw. Fadenverklebungen auftreten und ein freier Schrumpf ermöglicht wird. Durch das Zusammenschieben des Scherengatters wird eine hohe Dichte ≧ 0,03 g/cm³ erreicht.So that one of the four processes of oxidation, evacuation, carbonization and cooling can take place simultaneously under each retort lid, 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. At least two treatment retorts offset by 180 ° to each other can be placed on the upper rotating platform at the same time, so that the treatment system alternates a treatment retort with pitch fibers to be treated and a treatment retort with finished carbon fibers can be removed. According to a preferred embodiment of the invention, it is provided that 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. Such 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. By pushing the scissors gate together, a high density ≧ 0.03 g / cm³ is achieved.

Im folgenden wird die Erfindung anhand einer lediglich ein Ausführungsbeispiel darstellenden Zeichnung näher erläutert. Es zeigen

  • Fig. 1 ein schematisches Verfahrensfließbild zur Herstellung von Kohlenstoff-Fasern,
  • Fig. 2 die Vorrichtung zur thermischen Nachbehandlung in schematischer Aufsicht unterhalb der Beschickebene und
    Fig. 3 bis 17 einen Behandlungszyklus mit dem Gegenstand nach Fig. 2 in Seitenansicht.
The invention is explained in more detail below with reference to a drawing which represents only one exemplary embodiment. Show it
  • 1 is a schematic process flow diagram for the production of carbon fibers,
  • Fig. 2 shows the device for thermal aftertreatment in a schematic plan view below the loading level and
    3 to 17 a treatment cycle with the object of FIG. 2 in side view.

Im Zuge der Herstellung von Kohlenstoff-Fasern 1 aus Kohlenteerpech und insbesondere Steinkohlenteerpech wird das Kohlenteerpech vor dem Verspinnen durch Filtration von unschmelzbaren bzw. chinolinunlöslichen Bestandteilen befreit. Anschließend wird das Pechfiltrat einer Destillation zum Entfernen flüchtiger bzw. niedermolekularer Bestandteile unterzogen. Dann werden die aus der gewonnenen Pechschmelze bzw. Hartpechschmelze versponnenen Pechfasern 2 unter Verwendung eines Oxidationshilfsmittels wie Aktivkohle bei vorgegebener Oxidationstemperatur zum Unschmelzbarmachen oxidiert. Schließlich werden die oxidierten Pechfasern 2 unter Verwendung eines Inertgases bei vorgegebener Carbonisationstemperatur zum Austreiben flüchtiger Nebenprodukte carbonisiert. Pechfiltrat wird im Zuge der Destillation kontinuierlich in einen Dünnschichtverdampfer eingetragen und durch einen rotierenden Verteilerring gleichmäßig auf dem inneren Umfang verteilt. Die sich entlang der Verdampferzone bewegenden Rotor-Wischblätter erfassen das Pechfiltrat Lind breiten einen dünnen Film über der Heizwand aus. Dabei verdampft unter dem Einfluß eines angelegten Vakuums der flüchtige Produktanteil und wird auf einem Kondensator niedergeschlagen. Der nichtverdampfte Produktanteil, nämlich Hartpech, verläßt den Dünnschichtverdampfer. Eine Vakuumpumpe fordert das Hartpech zum Granulieren ab. Das alles ist nicht gezeigt.In the course of the production of carbon fibers 1 from coal tar pitch and in particular coal tar pitch, the 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. Then 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. Finally, 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. Here 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.

Das Pechgranulat wird in einem Extruder 3 aufgeschmolzen. Die Pechschmelze läuft über ein Filter 4 und wird mittels einer Dosierpumpe 5 einem Zentrifugalspinnkopf 6 zugeführt. Die Spinnzentrifuge, die an ihrem unteren Teil mit Düsenbohrungen versehen ist, drückt die Pechschmelze durch die Düsenbohrungen. Es entstehen zunächst endlose Filamente, die auf einem langsam rotierenden Fangring abgelegt werden. Der Fangring ist mit einer Schneidvorrichtung versehen, welche die Endlosfilamente auf die gewünschte Faserlänge schneidet. Da man für die nachfolgende thermische Nachbehandlung eine Lunte haben möchte, wird eine entsprechende Anzahl von Einzelfasern, die den gewünschten Luntenquerschnitt ergeben, am Fangring übereinander abgelegt. Die Luntenablage erfolgt in einem Coiler 7. Die Faserlunte wird über Umlenkrollen 8 in freihängenden Schlaufen auf einem auseinandergezogenen Scherengatter 9 abgelegt. Nach beendeter Ablage wird das Scherengatter 9, um eine hohe Raumausnutzung des Oxidationsofens 10 bzw. Carbonisationsofens 11 zu gewährleisten, zusammengeschoben und in eine Behandlüngsretorte 12 gegeben. Während des sich anschließenden Oxidationsprozesses befindet sich eine Vakuumretorte 13 im Untergeschoß und der Oxidationsofen 10 wird von unten über die Behandlungsretorte 12 gefahren. Nach einem abgestuften Temperaturprogramm wird die Behandlungsretorte 12 auf 350° C aufgeheizt. Während dieses Oxidationsprozesses zur Unschmelzbarmachung der Pechfasern 2 wird über ein Filter durch eine Pumpe 14 Luft über einen elektrischen Wärmetauscher 15 geleitet und durchströmt als heiße Oxidationsluft die Behandlungsretorte 12 von unten nach oben. Da während des Oxidationsprozesses flüchtige Pechbestandteile entweichen, wird die Abluft zunächst einem Wärmetauscher 16 zugeführt. Nichtkondensierbare Schadstoffe werden anschließend in einer fremdflammengeschützten Abluftverbrennungsanlage verbrannt. - Der nachfolgende Carbonisationsprozeß muß, um ein Verbrennen der Pechfasern 2 zu vermeiden, unter Inertgas ausgeführt werden. Um den Sauerstoff möglichst quantitativ aus der Faserlunte zu entfernen wird die Behandlungsretorte 12 zunächst evakuiert. Da die Behandlungsretorte 12 zwecks gutem Wärmedurchgangsmassearm aus nichtvakuumfestem Dünnblech hergestellt ist, wird der Carbonisationsofen 11 hinabgefahren und auf 1000° C aufgeheizt, während die Vakuumretorte 13 aus dem Untergeschoß unter die Behandlungsretorte 12 gehoben wird. Anschließend wird ein Vakuumaggregat 17 in Betrieb gesetzt. Nach einigen Minuten kann die Vakuumretorte 13 bzw. Behandlungsretorte 12 mit Stickstoff auf Normaldruck entspannt werden. Zur Sicherheit wird noch einmal mit Stickstoff gespült. Anschließend wird die Vakuumretorte 13 wieder in das Untergeschoß herabgelassen und gegen den mittlerweile auf 1000° C aufgeheizten Carbonisationsofen 11 ausgetauscht. Die Carbonisation erfordert zehn Minuten Verweilzeit, wobei flüchtige Verbindungen durch vorgeheizten Stickstoff über die Behandlungsretorte 12 zur Kondensation bzw. Abluftverbrennung transportiert werden. Nach beendeter Carbonisation wird der Carbonisationsofen 11 hinabgefahren, der Wärmetauscher 15 außer Betrieb genommen und der Innenraum der Behandlungsretorte 12 mit kaltem Stickstoff auf Temperaturen unter 600° C gekühlt. Nun kann das Scherengatter 9 entnommen, auseinandergezogen und zum Kühlstand transportiert werden, wo die Abkühlung der Kohlenstoff-Fasern 1 bis auf Raumtemperatur vollzogen wird.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. After the storage has been completed, 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. During the subsequent oxidation process there is a vacuum retort 13 in the basement and the oxidation furnace 10 is from below drove over the treatment retort 12. After a graduated temperature program, the treatment retort 12 is heated to 350 ° C. During this oxidation process to make the pitch fibers 2 infusible, air is passed through a filter 14 through a pump 14 through an electrical heat exchanger 15 and flows through the treatment retort 12 as hot oxidation air from bottom to top. Since volatile pitch components escape during the oxidation process, the exhaust air is first fed to a heat exchanger 16. Non-condensable pollutants are then burned in a flame-protected exhaust air combustion system. - The subsequent carbonization process must be carried out under inert gas in order to avoid burning the pitch fibers 2. In order to remove the oxygen as quantitatively as possible from the fiber sliver, the treatment retort 12 is first evacuated. Since the treatment retort 12 is made of non-vacuum-proof thin sheet for the purpose of good heat transfer mass arm, 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. After the carbonization has ended, 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. Now 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.

Im einzelnen weist die Vorrichtung zur thermischen Nachbehandlung der Pechfasern 2 eine untere Drehbühne 18 mit dem Oxidationsofen 10, der Vakuumretorte 13, dem Carbonisationsofen 11 und einer Kühlretorte 19 auf. Sämtliche Behandlungseinrichtungen 10, 11, 13, 19 sind in oben offener Behälterbauweise zur Aufnahme von Behandlungsretorten 12 ausgeführt. Ferner ist eine unabhängig von der unteren Drehbühne 18 drehbare obere Drehbühne 20 mit einer Changiereinrichtung für Behandlungsretorten 12 zur vorübergehenden Aufnahme der Faserablagen 9 mit den zu behandelnden Pechfasern 2 vorgesehen. Oberhalb der oberen Drehbühne 20 befindet sich eine Beschickebene 21 mit zumindest einer Beschicköffnung 22 und zumindest einer Retortendeckelaufnahme 23 für Retortendeckel 24 mit Anschluß für Luft- und Inertaszufuhr, Vakuum und Abluft. Die Changiereinrichtung überführt die Behandlungsretorten 12 zum Anschluß an den jeweiligen Retortendeckel 24 von der oberen Drehscheibe 20 unter den betreffenden Retortendeckel 24 und umgekehrt. Die untere Drehscheibe 18 weist zumindest eine Hubvorrichtung 25 für jeweils den Oxidationsofen 10, die Vakuumretorte 13, den Carbonisationsofen 11 und die Kühlretorte 19 auf. Diese Behandlungseinrichtungen sind zur Aufnahme der Behandlungsretorten 12 unter die Retortendeckelaufnahme 23 bzw. den betreffenden Retortendeckel 24 verfahrbar und hochfahrbar bzw. umgekehrt. Die Behandlungseinrichtungen 10, 11, 13, 19 sind auf der unteren Drehbühne 18 um 90° zueinander versetzbar und auf einem Drehkreis angeordnet, der in vertikaler Projektion den Außenumfang der oberen Drehbühne 20 zum seitlichen Passieren der hochzufahrenden oberen Drehbühne 20 zum seitlichen Passieren der hochzufahrenden Behandlungseinrichtungen 10, 11, 13, 19 übersteigt und zum Anschluß der hochgefahrenen Behandlungseinrichtungen an den jeweiligen Retortendeckel 24 unterhalb der in gleicher Weise um 90° zueinander versetzten Retortendeckelaufnahmen 23 verläuft. Jeder Behandlungseinrichtung 10, 11, 13, 19 ist eine eigene Hubvorrichtung 25 zugeordnet, so daß jeweils gleichzeitig unter jedem Retortendeckel 24 einer der vier Prozesse Oxidation, Evakuierung, Carbonisation und Kühlung ablaufen kann. Auf die oberer Drehbühne 20 sind zumindest zwei um 180° C zueinander versetzte Behandlungsretorten 12 gleichzeitig aufsetzbar. Die Faserablage ist als zusammeschiebbarens Scherengatter 9 für an waagerechten Stäben freihängende Faserschlaufen ausgebildet und in zusammengeschobenem Zustand in jeweils eine Behandlungsretorte 12 einsetzbar.In particular, 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. Above the upper rotating platform 20 there is a loading level 21 with at least one loading opening 22 and at least one retort lid receptacle 23 for retort lid 24 with a connection for air and inert gas supply, vacuum and exhaust air. 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. These 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.

In einzelnen arbeitet die Vorrichtung wie folgt, wenn gleichzeitig unter jedem Retortendeckel 24 jeweils einer der vier Prozesse Oxidation, Evakuierung, Carbonisation und Kühlung abläuft:In detail, 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:

Fig. 3) Auf der oberen Drehbühne 20 wird eine leere Behandlungsietorte 12 von oben mit einem zusammengezogenen Scherengatter 9 gefüllt.Fig. 3) On the upper revolving platform 20, an empty treatment area 12 is filled from above with a contracted scissors gate 9.

Fig. 4) Die obere Drehbühne 20 dreht sich um 180° C. Während aus der anderen Behandlungsretorte 12 ein Scherengatter 9 mit fertigen KohlenstoffFasern 1 entnommen wird, dreht sich die untere Drehbühne 18 um 90°, so daß die Kühlretorte 19 gegen den Oxidationsofen 10 ausgetauscht wird.Fig. 4) 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.

Fig. 5) Die Behandlungsretorte 12 mit den unbehandelten Pechfasern 2 wird durch die Changiereinrichtung unter den zugeordneten Retortendeckel 24 transportiert.Fig. 5) The treatment retort 12 with the untreated pitch fibers 2 is transported through the traversing device under the assigned retort lid 24.

Fig. 6) Durch die Hubvorrichtung 25 wird der Oxidationsofen 10 - ein Niedertemperaturofen - von unten über die Behandlungsretorte 12 gefahren. Während des nun folgenden Oxidationsprozesses-wird heiße Oxidationsluft durch die Behandlungsretorte 12 geleitet und der Oxidationsofen 10 entsprechend dem optimierten Temperaturprofil aufgeheizt. Die heißen Prozeßgase werden der Abluftreinigung zugeführt.Fig. 6) The lifting device 25 moves the oxidation furnace 10 - a low-temperature furnace - from below over the treatment retort 12. During the now following oxidation process, 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.

Fig. 7) Nach beendeter Oxidation wird der Oxidationsofen 10 auf die untere Drehbühne 18 herabgefahren.Fig. 7) After the oxidation, the oxidation furnace 10 is lowered onto the lower rotating stage 18.

Fig. 8) Die untere Drehbühne 18 dreht um 90°, so daß die Vakuumretorte 13 unter der Behandlungsretorte 12 zu stehen kommt.Fig. 8) The lower rotating stage 18 rotates by 90 °, so that the vacuum retort 13 comes to rest under the treatment retort 12.

Fig. 9) Die Vakuumretorte 13 wird über die Hubvorrichtung 25 von unten über die Behandlungsretorte 12 gehoben. Das angelegte Vakuum evakuiert den Oxidationsofen 10.Fig. 9) 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.

Fig. 10) Zur Sicherheit wird die Behandlungsretorte 12 noch mit Stickstoff unter gleichzeitiger Druckentspannung gespült. Die Vakuumretorte 13 wird auf die untere Drehbühne 18 hinabgefahren.Fig. 10) For safety, 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. 11) Die untere Drehbühne 18 dreht um 90°, so daß der inzwischen 1000° heiße Carbonisationsofen 11 - ein Hochtemperaturofen - unter der Behandlungsretorte 12 steht.Fig. 11) The lower rotating stage 18 rotates by 90 °, so that the now 1000 ° hot carbonization furnace 11 - a high-temperature furnace - is under the treatment retort 12.

Fig. 12) Der Carbonisationsofen 11 wird mittels der Hubvorrichtung 25 von unten über die Behandlungsretorte 12 gefahren. Während des nun folgenden Carbonisationsprozesses wird vorgeheizter Stickstoff durch die Behandlungsretorte 12 geleitet und transportiert die flüchtigen Verbindungen zum Abluftsystem.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.

Fig. 13) Der Carbonisationsofen 11 wird auf die untere Drehbühne 18 hinabgefahren.Fig. 13) The carbonization furnace 11 is moved down to the lower rotating stage 18.

Fig. 14) Die untere Drehbühne 18 dreht um 90°, so daß die Kühlretorte 19 unter der Behandlungsretorte 12 zu stehen kommt. Die Pechfasern 2 werden durch Zufuhr von kaltem Stickstoff auf Temperaturen unter 600° C gekühlt.Fig. 14) 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.

Fig. 15) Die weitere Abkühlung kann in der Kühlstation 19 mit kalter Luft erfolgen.Fig. 15) The further cooling can take place in the cooling station 19 with cold air.

Fig. 16) Die Kühlstation 19 wird auf die untere Drehbühne 18 hinabgefahren.Fig. 16) The cooling station 19 is moved down to the lower rotating platform 18.

Fig. 17) Durch die Changiervorrichtung wird die Behandlungsretorte 12 auf die obere Drehbühne 20 transportiert. Ein neuer Zyklus beginnt.17) The treatment retort 12 is transported to the upper rotating stage 20 by the traversing device. A new cycle begins.

Beispiel für den OxidationsprozeßExample of the oxidation process

Die charakteristischen Daten eines in einem Dünnschichtverdampfer destillierten Steinkohlenteerpechs sind im folgenden aufgeführt:

Figure imgb0001
The characteristic data of a coal tar pitch distilled in a thin film evaporator are listed below:
Figure imgb0001

Dieses durch Dünnschichtverdampfung gewonnene hochschmelzende Steinkohlenteerpech (EP (KS): 228° C) wurde zu Pechfasern 2 versponnen. Die erhaltenen Pechfasern wurden hängend in einem Oxidationsofen 10 in 16 Minuten auf eine Oxidationstemperatur von 340° C aufgeheizt. Ein kritischer Oxidationsbereich (Erweichungspunkt ± 25° C) wurde dabei mit einer maximalen Aufheizrate von 20° C/min durchfahren. Der Luftdurchsatz betrug dabei 2000 bis 3000 1/h. Die Pechfasern 2 verschmolzen während des Oxidierens nicht, wiesen auch keine äußerlichen Beschädigungen auf. Die erreichte Unschmelzbarkeit erlaubte ein anschließendes rasches Carbonisieren nach der üblichen Methode. Im übrigen wurde Aktivkohle (ohne H₂SO₄) als Oxidationshilfsmittel verwendet.This high-melting coal tar pitch (EP (KS): 228 ° C.) obtained by thin-layer evaporation was spun into pitch fibers 2. 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. In addition, activated carbon (without H₂SO₄) was used as an oxidation aid.

Claims (4)

1. Apparatus for the thermal curing treatment of carbon fibres of coal tar pitch, particularly of bitumenous coal tar pitch, with at least one fibre storage, an oxidation stove and a carbonization stove, characterized by:
- a lower rotating stage (18) with the oxidation stove (10), a vacuum retort (13), the carbonization stove (11) and a cooling retort (19), all the treatment appliances being constructed as containers open at the top,
- an upper rotating stage (20) rotatable independently of the lower rotating stage (18) with a change-over appliance for treatment retorts (12) for temporary accommodation of the fibre storage (9) with the pitch fibres (2) to be treated,
- a loading surface (21) above the upper rotating stage (20) with at least one loading opening (22) and at least one retort lid receptor (23) for retort lids (24) with connections for supplies of air and inert gas, for vacuum and for exhaust air,
in which the change-over appliance conveys the treatment retorts (12), for connection to the particular retort lid (24), from the upper rotating stage (20) below the retort lid (24) concerned and vice versa, and in which the lower rotating stage (18) has at least one lifting equipment (25) each for the oxidation stove (10), the vacuum retort (13), the carbonization stove (11) and the cooling retort (19), and these treatment appliances (10, 11, 13, 19) are transportable and movable upwards, or vice versa, below the retort lid receptor (23) or the retort lid (24) concerned.
2. Apparatus according to Claim 1, characterized in that the treatment appliances (10, 11, 13, 19) are located on the lower rotating stage (18) at 90° apart from one another in a circle, that in vertical projection exceeds the outer periphery of the upper turntable (20) in order that the treatment appliances (10, 11, 13, 19) when moving upwards pass outside it, and that extends below the retort lid receptors (23) that are similarly spaced at 90° from one another for connection of the lifted treatment appliances to the individual retort lids (24), for which an individual lifting equipment (25) is associated with each treatment appliance (10, 11, 13, 19).
3. Apparatus according to Claim 1 or 2, characterized in that at least two treatment retorts (12) displaced by 180° from one another can be set down simultaneously on the upper turntable (20).
4. Apparatus according to one of Claims 1 to 3, characterized in that the fibre storage is constructed as an extensible crossbar frame (9) for loops of fibre hanging freely from crossbars, and in the contracted state can be inserted into a treatment retort (12).
EP88900817A 1987-02-07 1988-01-05 Apparatus for thermal aftertreatment of carbon fibres from coaltar pitch, in particular from glance- (hard)- coaltar pitch Expired - Lifetime EP0302084B1 (en)

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AT88900817T ATE71132T1 (en) 1987-02-07 1988-01-05 DEVICE FOR THE THERMAL POST-TREATMENT OF CARBON FIBERS FROM COAL TAR PITCH, IN PARTICULAR COAL TAR PITCH.

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DE3703825 1987-02-07
DE19873703825 DE3703825A1 (en) 1987-02-07 1987-02-07 METHOD AND DEVICE FOR PRODUCING CARBON FIBERS

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GR1000326B (en) * 1988-02-05 1992-06-25 Didier Eng Mechanical disposition for producing carbon fibres
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US5427908A (en) * 1990-05-01 1995-06-27 Affymax Technologies N.V. Recombinant library screening methods
DE69029748T2 (en) * 1990-11-01 1997-05-07 Ashland Inc IMPROVED METHOD FOR PRODUCING ENRICHED PECH AND CARBON FIBERS
CN100402419C (en) * 2006-08-02 2008-07-16 太原理工大学 Method of preparing nano-carbon fiber using coal tar asphalt as raw material
CN103361096B (en) * 2012-04-10 2014-12-03 上海宝钢化工有限公司 Preparation method of high-softening-point asphalt for producing general-grade carbon fibers
CN105463630B (en) * 2012-11-13 2018-07-10 宁波高新区零零七工业设计有限公司 Carbon fibre producing facility
DE102013208426A1 (en) 2013-05-07 2014-11-13 Bayerische Motoren Werke Aktiengesellschaft Process and apparatus for processing carbon fiber strands
CN105839213B (en) * 2016-06-13 2019-05-17 天津工业大学 A kind of pitch carbon fiber precursors melt spinning machine
CN111849530B (en) * 2020-07-30 2021-12-03 贵州省煤炭产品质量监督检验院 Coal tar advanced treatment system

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US3718493A (en) * 1968-06-04 1973-02-27 Great Lakes Carbon Corp Process for the production of carbon filaments from coal tar pitch
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IT1137958B (en) * 1981-06-26 1986-09-10 Manifattura Tintoria & Trasfor PROCEDURE FOR DYING OF RIPPED FIBER BAND, EQUIPMENT FOR ITS REALIZATION AND PRODUCT SO OBTAINED
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DE3509861C2 (en) * 1984-03-26 1986-03-06 Idemitsu Kosan Co. Ltd., Tokio/Tokyo Pitch material for a carbon-containing molded body and process for its manufacture
US4550579A (en) * 1984-04-13 1985-11-05 Frank Clifford G Apparatus for the dyeing of shaped articles

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