EP3114261B1 - Heizvorrichtung zur herstellung von kohlenstofffasern - Google Patents

Heizvorrichtung zur herstellung von kohlenstofffasern Download PDF

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Publication number
EP3114261B1
EP3114261B1 EP15709412.9A EP15709412A EP3114261B1 EP 3114261 B1 EP3114261 B1 EP 3114261B1 EP 15709412 A EP15709412 A EP 15709412A EP 3114261 B1 EP3114261 B1 EP 3114261B1
Authority
EP
European Patent Office
Prior art keywords
heating device
induction heating
inert gas
heating element
starting material
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.)
Active
Application number
EP15709412.9A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP3114261A1 (de
Inventor
Daniel Decker
Michael WÖLKI
Phillip Schwerdt
Horst Linn
Rudolf Linn
Jürgen Kunstmann
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.)
Clariant International Ltd
Linn High Therm GmbH
Original Assignee
Clariant International Ltd
Linn High Therm 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 Clariant International Ltd, Linn High Therm GmbH filed Critical Clariant International Ltd
Publication of EP3114261A1 publication Critical patent/EP3114261A1/de
Application granted granted Critical
Publication of EP3114261B1 publication Critical patent/EP3114261B1/de
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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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
    • D01F9/32—Apparatus therefor
    • D01F9/328—Apparatus therefor for manufacturing filaments from polyaddition, polycondensation, or polymerisation products
    • 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
    • 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
    • D01F9/32—Apparatus therefor
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
    • D02J13/001—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass in a tube or vessel
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
    • D02J13/005—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass by contact with at least one rotating roll
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/02—Induction heating
    • H05B6/10—Induction heating apparatus, other than furnaces, for specific applications
    • H05B6/105—Induction heating apparatus, other than furnaces, for specific applications using a susceptor
    • H05B6/108—Induction heating apparatus, other than furnaces, for specific applications using a susceptor for heating a fluid
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/02—Induction heating
    • H05B6/36—Coil arrangements
    • H05B6/44—Coil arrangements having more than one coil or coil segment

Definitions

  • the invention relates to a heating device for producing carbon fibers from a filamentary fiber starting material, the heating device having a central tubular induction heating element through which the fiber starting material is moved, the tubular induction heating element is surrounded by thermal insulation, an induction coil is provided outside the thermal insulation as a heating source, and an inert gas flows through the central induction heating element, in particular for carbonization and / or graphitization of the fiber starting material.
  • the US 4,469,925 discloses a heating device for workpieces made of carbon with a first heat insulation layer made of carbon powder and a second heat insulation layer made of a mixture of carbon and silicon powder.
  • a carbonization furnace with heat insulation which is composed of a carbon fiber felt and a ceramic fiber felt.
  • the carbon fiber felt and the ceramic fiber felt are spaced apart.
  • a heating device for producing carbon fibers in which the heating source is formed by a high-frequency induction coil.
  • the heat insulation consists of carbon particles with an average grain diameter of 0.5 to 1.5 mm and an angle of repose of ⁇ 35 °.
  • the carbon particles are obtained by granulating carbon black powder, which has an average grain diameter of about 50 to 300 ⁇ m, with a binder and by carbonizing the binder.
  • the heat insulation in this known heating device can consist of a relatively thin layer of carbon fiber felt and a layer of carbon particles provided around this felt layer.
  • the carbon fiber felt layer there is, for example, 10 to 15 mm, because it is easily subject to induction due to the high frequency generated by the high-frequency coil, as stated in column 8, lines 45 to 51.
  • the Thermal insulation of this known heating device is provided in a tube made of a heat-resistant material immediately adjacent to this.
  • the tube made of the heat-resistant material is hermetically sealed at its two axially facing ends by cover elements.
  • One of the two cover elements is designed with a gas inlet and a gas outlet for the inert gas.
  • the inert gas is, for example, nitrogen, argon, helium or the like.
  • This vertically oriented heating device has deficiencies in terms of its energy balance, although it should not be overlooked that its energy balance is better than the energy balance of a generic heating device which uses an electrical resistance heater instead of a high-frequency induction coil.
  • GB 808 442 A and US 3,883,718 A also disclose heaters for making carbon fibers from a filamentary fiber stock, the heaters having a central tubular induction heater.
  • the invention has for its object to provide a heating device of the type mentioned, in which the energy balance is significantly improved with structurally simple means.
  • the heating source is formed by at least one medium to high frequency induction coil, and that on the outside of the heat insulation a first and a second tubular element made of material transparent to the induction field of the medium to high frequency induction coil are provided, which are separated from one another by are spaced an annular gap through which the inert gas flows, the inert gas is passed through the annular gap between the first and the second tubular element and through the central tubular induction heating element in countercurrent, at the two axially facing ends of the central tubular induction heating element and the first and a second tubular element, a cover element is provided, the one cover element for deflecting the inert gas from the annular gap between the first and the second tubular element to the central tubular induction heating element and the other cover element for introducing the inert gas it is provided in the annular gap between the first and the second tubular element and for discharging the inert gas from the central tubular induction heating element.
  • the heating device uses a medium to high-frequency induction coil as the heating source. This is in the frequency range of the induction coil Heat insulation used according to the invention is transparent, ie an undesired dissipation of the induction field into the heat insulation is negligible.
  • the inert gas not only the central tubular induction heating element but upstream beforehand Through the annular gap between the first and the second tubular element on the outside of the thermal insulation, an energy saving is advantageously achieved because cold inert gas is heated in the said annular gap so that it enters the central tubular induction heating element at an elevated temperature and here the desired high Temperature reached in particular for carbonization and / or graphitization of the filamentary fiber starting material with an overall reduced use of energy.
  • gas guide elements are provided in the said annular gap.
  • the gas guide elements can be guide ribs, knobs, or the like. act. With the help of the gas guide elements, the dwell time of the inert gas in the annular gap is increased in a defined manner. The preheating or heating of the inert gas at the point of exit from the annular gap is proportional to this increase in the residence time.
  • the inert gas is passed through the annular gap between the first and the second tubular element and through the central tubular induction heating element in countercurrent, i.e. when the inert gas is passed through the annular gap in one axial direction and in the central tubular induction heating element in the axially opposite direction.
  • This counterflow control of the inert gas can be implemented in a structurally simple manner.
  • Optimal carbonization and / or graphitization of the filamentary fiber starting material can be achieved according to the invention by passing the inert gas through the central induction heating element in one axial direction and at the same time moving the filamentary fiber starting material in the opposite direction through the induction heating element.
  • the heating device according to the invention can be used to move at least one fiber starting material thread through the central tubular induction heating element. From a productivity point of view, it is advantageous if the heating device according to the invention is provided for a number of fiber starting material threads to be moved simultaneously through the central induction heating element, the fiber starting material threads being spaced apart from one another in one or more planes.
  • the induction heating element can have a circular or an oval ring cross section.
  • the thermal insulation surrounding the central tubular induction heating element can have a circular outer surface or an oval outer surface adapted to the oval ring cross section.
  • the heat insulation consists of a carbon fiber felt.
  • the thermal insulation it is possible for the thermal insulation to have an inner layer made of a carbon fiber felt and an outer layer made, for example, of Al 2 O 3 fibers or of Al 2 O 3 / SiO 2 fibers.
  • the efficiency of the heating device according to the invention can advantageously be further improved, i.e. can be increased if the thermal insulation is spaced from the central tubular induction heating element by an annular gap through which a portion of the inert gas flows.
  • the flow of the inert gas in the last-mentioned annular gap and the flow of the inert gas in the central tubular induction heating element expediently run in the same direction, i.e. in parallel directions.
  • a cover element is provided on each of the two axially facing ends of the central tubular induction heating element and the first and second tubular elements of the heating device according to the invention.
  • the two cover elements are hermetically sealed on the outside tubular element.
  • a lock device for the thread-like fiber starting material to be carbonized and / or graphitized is preferably provided on the outside.
  • the cover elements are expediently each equipped with a cooling device.
  • Water for example, can be used as the cooling medium.
  • a radiation screen perforated disk is expediently provided in the central tubular induction heating element at the two axially facing end sections in order to minimize possible heat losses in the central tubular induction heating element and consequently to optimize the efficiency of the heating device.
  • the same purpose can be useful if at least one radiation shield ring disk is adjacent to the two axially facing end faces of the thermal insulation.
  • the cover elements of the heating device according to the invention can be made, for example, of aluminum, an aluminum alloy, stainless steel or the like. consist.
  • the cooling of the cover elements can be, for example, water cooling, as has already been explained.
  • At least the first tubular element adjacent for thermal insulation is provided on the inside and / or outside with an infrared reflection coating.
  • the infrared reflective coating can be a full-surface or a partial coating. In the case of a partial coating, this can be strip-like, grid-like, punctiform or the like. be trained.
  • Figure 1 shows schematically an embodiment of the heating device 10 for the production of carbon fibers from a thread-like fiber starting material 12.
  • filamentary fiber starting material is oxidized in a known manner in a first process step at temperatures up to 400 ° C., then carbonized at 400 ° C. to approx. 1600 ° C. and then graphitized at 1600 ° C. to 2800 ° C.
  • the heating device according to the invention is used in particular for carbonizing the filamentary fiber starting material.
  • the heating device according to the invention can also be used for graphitizing the filamentary fiber starting material if the at least one medium to high-frequency induction coil is dimensioned accordingly.
  • a heating device according to the invention for carbonizing can be used in combination with a further heating device according to the invention for graphitizing.
  • the heating device according to the invention in multiple zones, i.e. to form the medium to high frequency induction coil in several parts, at least one medium to high frequency induction coil for carbonizing and at least one further medium to high frequency induction coil being provided for graphitizing the filamentary fiber starting material.
  • the heating device 10 has a central tubular induction heating element 14 through which the filamentary fiber starting material is moved.
  • the direction of movement of the filamentary fiber starting material 12 is indicated by the arrow 16.
  • the central tubular induction heating element 14 is surrounded by thermal insulation 18.
  • the heat insulation 18 consists of a carbon fiber felt 20.
  • an induction coil is provided as the heat source, which is a medium to high-frequency induction coil 22 which is operated, for example, at a frequency of approximately 5 kHz to approximately 40 kHz. it being understood that other frequencies can also be used.
  • the thermal insulation 18 made of carbon fiber felt 20 is transparent to the induction field generated by the induction coil 22, i. H. the coupling of the induction field into the thermal insulation 18 is negligible.
  • An inert gas flows through the central tubular induction heating element 14 for the carbonization and / or graphitization of the filamentary fiber starting material 12. This is indicated by the arrows 24.
  • the inert gas is passed through the central tubular induction heating element 14 in the one axial direction indicated by the arrows 24.
  • the filamentary starting material 12 to be carbonized and / or graphitized is moved through the central tubular induction heating element 14 in the opposite direction indicated by the arrow 16.
  • a first pipe element 26 and a second pipe element 28 radially spaced therefrom are provided on the outside of the heat insulation 18, which consist of a material which is transparent to the induction field of the induction coil 22.
  • This material is, for example Quartz glass.
  • the first tube element 26 to consist, for example, of quartz glass and the two tube element 28 to consist of borosilicate glass.
  • the two tubular elements 26 and 28 are spaced apart from one another by an annular gap 30.
  • the inert gas flows through the annular gap 30.
  • gas guide elements 32 expediently consist of the same material as the first and / or second tubular element 28.
  • the inert gas is heated by the induction field of the medium to high frequency induction coil 22.
  • the heated inert gas is then introduced into the central space 34 of the tubular induction heating element 14. Is in Figure 1 indicated by the curved arrow 36.
  • the inert gas is through the annular gap 30 between the first and second tubular elements 26 and 28 in the direction indicated by the arrow 38 and then by the central tubular induction heating element 14 in the opposite direction indicated by the arrows 24, ie in counterflow, passed through.
  • the heating device 10 is a heating device, for example for a laboratory system or the like. acts, the heating device 10 is provided for a fiber starting material thread 12.
  • the heating device 10 is preferably designed such that a number of fiber starting material threads 12 can be moved simultaneously through the central tubular induction heating element 14, the fiber starting material threads 12 preferably being spaced apart from one another in at least one common plane or in several slightly spaced apart from one another Levels. This level or levels are to the drawing level of the Figure 1 perpendicular.
  • the central tubular induction heating element 14 with the thermal insulation 18, the first and the second tubular elements 26 and 28 and the medium to high frequency induction coil 22 form a self-supporting central body 40 of the heating device 10, at the ends 42, 44 of which axially facing away from each other a cover element 46 , 48 is provided.
  • the cover elements 46 and 48 are in Figure 1 drawn only very schematically and spaced from the central body 40. In the assembled state of the heating device 10, the cover elements 46, 48 are hermetically sealed to the end sections 50, 52 of the outside second tubular element 28. This is indicated, for example, by sealing beads 54, 56 with which the cover elements 46, 48 are provided.
  • the cover element 46 is for deflecting the inert gas from the annular gap 30 between the first and the second tubular element 26, 28 to the central tubular induction heating element 14, i.e. for deflecting in the central space 34, as indicated by the curved arrow 36, is provided.
  • the cover element 46 is preferably formed with a (not shown) deflection cavity for the inert gas.
  • the opposite other cover element 48 is provided for introducing the inert gas into the annular gap 30 between the first and second tubular elements 26, 28 and for discharging the inert gas from the central space 34 of the central tubular induction heating element 14.
  • the cover element 48 which is also shown only very schematically, is provided with an inlet 58 for the inert gas and outlet 60 for discharging the same, the cover element 48 likewise being designed with partial cavities (not shown) to which the inlet 58 and the outlet 60 are assigned are.
  • the introduction of the inert gas into the cover element 48 is indicated by the arrow 62 and the discharge of the inert gas from the cover element 48 is indicated by the arrow 64.
  • each cover element 46, 48 is each formed with a cooling 70, which is, for example, a water cooling.
  • Reference numeral 72 denotes a cooling medium inlet and reference numeral 74 denotes a cooling medium outlet belonging to the respective cooling medium inlet 72.
  • the respective cover element 46, 48 is provided on the inside with slightly frustoconical positioning and centering pins 76 which, when the cover elements 46, 48 are assembled, project with the central body 40 into the annular gap 30 between the first and the second tubular elements 26, 28 with virtually no play.
  • the cover elements 46, 48 are also provided on the inside with positioning and centering pins 78, which interact with the central tubular induction heating element 14 in the assembled state of the heating device 10, as it were, without play.
  • a radiation screen perforated disk 80 is provided at each of the two axially facing end sections in order to localize the heat generated by the induction heating element 14 in the central space 34.
  • At least one radiation shield washer 84 is adjacent to each of the two axially facing end faces 82 of the thermal insulation 18. In Figure 1 two radiation shield washers 84 are shown axially spaced apart from each other.
  • At least the first tubular element 26 adjacent to the heat insulation 18 can be provided on the inside and or on the outside with an infrared reflection coating 86.
  • the reflection coatings can be formed over the entire surface or over part of the surface. In the case of a partial coating, this can be configured, for example, in the form of a strip, a lattice, a chaotic spot or a grid.
  • the reference number 88 designates axially oriented strip elements, by means of which the windings of the medium to high frequency induction coil 22 are connected to one another and spaced apart from one another in a defined manner.
  • FIG 1 an embodiment of the heating device 10 is shown schematically, in which the thermal insulation 18 - as has been mentioned - consists of a carbon fiber felt 20.
  • the Figure 2 A section of the central body 40 is cut longitudinally on one side in sections, the heat insulation 18 having an inner layer 90 and an outer layer 92.
  • the inner layer 90 consists of a carbon fiber felt 20 and the outer layer 92, for example, of Al 2 O 3 fibers.
  • FIG. 3 clarified in one of the Figure 2 Similar half-sided longitudinal sectional view of a portion of the self-supporting central body 40 of the heating device according to the invention.
  • This embodiment differs from that in FIG Figure 2 schematically illustrated embodiment in that the thermal insulation 18 is spaced from the central tubular induction heating element 14 by an annular gap 94 through which the inert gas flows. This is indicated by arrow 96.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Fibers (AREA)
  • Tunnel Furnaces (AREA)
  • Furnace Details (AREA)
  • General Induction Heating (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
EP15709412.9A 2014-03-03 2015-02-27 Heizvorrichtung zur herstellung von kohlenstofffasern Active EP3114261B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102014003126.8A DE102014003126A1 (de) 2014-03-03 2014-03-03 Heizvorrichtung zur Herstellung von Kohlenstofffasern
PCT/EP2015/000457 WO2015131990A1 (de) 2014-03-03 2015-02-27 Heizvorrichtung zur herstellung von kohlenstofffasern

Publications (2)

Publication Number Publication Date
EP3114261A1 EP3114261A1 (de) 2017-01-11
EP3114261B1 true EP3114261B1 (de) 2020-01-08

Family

ID=52669572

Family Applications (1)

Application Number Title Priority Date Filing Date
EP15709412.9A Active EP3114261B1 (de) 2014-03-03 2015-02-27 Heizvorrichtung zur herstellung von kohlenstofffasern

Country Status (5)

Country Link
US (1) US10337125B2 (ja)
EP (1) EP3114261B1 (ja)
JP (1) JP6562938B2 (ja)
DE (1) DE102014003126A1 (ja)
WO (1) WO2015131990A1 (ja)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10473398B2 (en) 2015-02-09 2019-11-12 Ciariant International Ltd Modular furnace, in particular for the oxidative stabilization of a carbon fiber starting material
DE102018108291A1 (de) * 2018-04-09 2019-10-10 Eisenmann Se Ofen
US12031243B2 (en) * 2019-12-11 2024-07-09 West Virginia University Methods to produce carbon fibers from carbon pitches
DE102021000118B3 (de) * 2021-01-13 2021-12-30 Allgaier Werke Gmbh Siebgewebe mit erhöhter Verschleißfestigkeit und Verfahren zur Erhöhung der Verschleißfestigkeit eines Siebgewebes
KR102578947B1 (ko) * 2021-12-24 2023-09-18 재단법인 한국섬유기계융합연구원 재생탄소섬유 제조장치 및 이를 이용한 재생탄소섬유의 제조방법

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Also Published As

Publication number Publication date
JP6562938B2 (ja) 2019-08-21
EP3114261A1 (de) 2017-01-11
US20170073846A1 (en) 2017-03-16
DE102014003126A1 (de) 2015-09-03
US10337125B2 (en) 2019-07-02
JP2017515002A (ja) 2017-06-08
WO2015131990A1 (de) 2015-09-11

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