EP1525342B1 - Verfahren und anlage zur thermischen behandlung von natrium-enthaltenden kohlenstoffprodukten - Google Patents

Verfahren und anlage zur thermischen behandlung von natrium-enthaltenden kohlenstoffprodukten Download PDF

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Publication number
EP1525342B1
EP1525342B1 EP03748208A EP03748208A EP1525342B1 EP 1525342 B1 EP1525342 B1 EP 1525342B1 EP 03748208 A EP03748208 A EP 03748208A EP 03748208 A EP03748208 A EP 03748208A EP 1525342 B1 EP1525342 B1 EP 1525342B1
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EP
European Patent Office
Prior art keywords
sodium
oven
exhaust pipe
neutralizing agent
pipe
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
EP03748208A
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English (en)
French (fr)
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EP1525342A2 (de
Inventor
Etienne 12 Rue Du Bussac LONCLE
Jacky Domaine de la Forêt MINET
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.)
Safran Ceramics SA
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SNECMA Propulsion Solide SA
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Publication of EP1525342A2 publication Critical patent/EP1525342A2/de
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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
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • 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

Definitions

  • the invention relates to the high temperature heat treatment of carbon products containing sodium, and more particularly to the treatment of gaseous effluents produced during the heat treatment.
  • a particular field of application of the invention is the production of textures or preforms made of carbon fibers intended to constitute fibrous reinforcements for parts made of composite material such as carbon / resin composite, for example C / epoxy or C / phenolic composite, or thermostructural composite, for example carbon / carbon composite (C / C) or ceramic matrix composite and carbon reinforcement.
  • composite material such as carbon / resin composite, for example C / epoxy or C / phenolic composite, or thermostructural composite, for example carbon / carbon composite (C / C) or ceramic matrix composite and carbon reinforcement.
  • Such fibrous textures are usually obtained from carbon precursor fibers that are better able to undergo the textile operations required for shaping these textures.
  • carbon precursor fibers are preoxidized polyacrylonitrile (PAN) fibers, pitch fibers, phenolic fibers, and rayon fibers.
  • PAN polyacrylonitrile
  • the second step is generally carried out under reduced pressure and under a purge of neutral gas such as nitrogen.
  • the second step is usually carried out before densification of the fibrous texture by the resin, carbon or ceramic matrix of the composite material.
  • the densification can be carried out by a liquid route, that is to say impregnation with a liquid compound, such as a resin, precursor of the material of the matrix, and transforming this precursor by heat treatment.
  • the densification can also be carried out by gaseous means, that is to say by chemical vapor infiltration, the two processes, the liquid route and the gaseous route being well known and possibly associable.
  • the object of the invention is to provide a method which avoids the aforementioned drawback by preventing the formation on the walls of gaseous effluent extraction pipes of potentially dangerous deposits at the stage of cleaning these pipes.
  • This object is achieved by a process of the type in which the carbon products are heated in an oven, under a purge of neutral gas and under reduced pressure, with continuous extraction out of the effluent furnace.
  • gas containing in particular sublimed sodium by an effluent discharge pipe, in which process, in accordance with the invention, at least one sodium neutralization product is injected into the effluent discharge pipe, immediately downstream of the effluent gas outlet out of the oven.
  • sodium neutralization product is meant a product to obtain a stable sodium compound and fairly easily removed.
  • a relatively easy handling product for example water vapor or preferably carbon dioxide, optionally mixed with water vapor, is preferably chosen.
  • the neutralization product may be injected at or downstream of a bend formed by the effluent gas discharge pipe out of the oven.
  • the injected neutralization product may further be diluted in a neutral gas such as nitrogen.
  • the neutralization product can be continuously injected into the gaseous effluent stream extracted from the furnace during the heat treatment, so as to form a stable and easily removable sodium compound and avoid the deposition of sodium on the pipe wall of the furnace. evacuation.
  • the neutralization product is injected into the evacuation pipe after the end of the heat treatment in order to neutralize the sodium deposited on the wall of the evacuation pipe, before cleaning it.
  • the invention also aims to provide an installation for implementing the method.
  • a heat treatment plant for carbon products containing sodium of the type comprising an oven, means for supplying the oven with neutral gas for scavenging, and a line for extracting gaseous effluent out of the oven, installation which further comprises, according to the invention means for injecting a sodium neutralization product in the extraction pipe immediately after the exit of the furnace.
  • High temperature heat treatment means a treatment at a temperature usually greater than that encountered by the textures during carbonization, that is to say a temperature greater than 1000 ° C., typically between 1400 ° C. and 2000 ° C. ° C at 2200 ° C or 2500 ° C.
  • the heat treatment is carried out under reduced pressure, below atmospheric pressure, preferably below 50 kPa, typically between 0.1 kPa and 50 kPa, preferably below 5 kPa, and under a purge of neutral gas such as nitrogen or argon.
  • the process according to the invention is applicable to the removal of sodium present at low levels in fibers, for example less than 80 ppm, or at a much higher content, greater than 3500 ppm.
  • the figure 1 shows very schematically an oven 10 comprising a susceptor 12 of cylindrical shape and vertical axis which laterally delimits a volume or enclosure 11 for loading products (not shown) of carbon.
  • the susceptor 12 for example graphite, is surmounted by a cover 14, is heated by inductive coupling with an inductor 16 which surrounds the susceptor with the interposition of a thermal insulator 18.
  • the inductor is powered by a circuit 20 which delivers a current depending on the need for heating the oven.
  • the inductor can be divided into several sections on the height of the oven. Each section is powered separately with electric power to define different heating zones in the oven in which the temperature can be regulated independently.
  • the bottom of the furnace is formed of a thermal insulator 22 covered with a furnace hearth 24, for example made of graphite, on which the susceptor 12 rests.
  • the assembly is housed in an envelope 26, for example metal, sealed by a removable cover 28.
  • a pipe 30 provided with a valve 31 is connected to a source (not shown) of inert gas, for example nitrogen N 2 .
  • the pipe 30 supplies the oven 10 with inert scanning gas to the upper part thereof, possibly through several inlets 32 opening at different locations around the casing 26 of the oven.
  • An extraction device 40 is connected to an outlet duct 42 of the furnace passing through the bottom thereof, to extract the gaseous effluent produced during the heat treatment of the carbon products, in order to remove residual sodium in particular.
  • the device 40 is connected to the outlet duct 42 by an evacuation pipe 44 provided with a carbon dioxide injection inlet 46 CO 2 .
  • the pipe 44 forms a bend 44 has at its extremity connected by a flange 45 to the outlet duct 42 of the furnace.
  • the injection inlet 46 is connected to a pipe 48 connected to a source (not shown) of CO 2 gas and provided with a valve 49.
  • the pipe 48 is extended by a nozzle 50 which penetrates into the pipe 44 in order to inject the CO 2 gas in this pipe towards the downstream end of the elbow 44a and to avoid an accidental injection of the CO 2 gas inside the furnace by the exit pipe 42.
  • Several points of injection of CO 2 gas spaced apart from each other along the pipe 44 may be provided.
  • the CO 2 injection is carried out as close as possible to the outlet of the furnace, at a level where the sodium contained in the effluent is always in sublimated form.
  • the injection at a bend of the pipe 44 promotes a mixture by turbulence between the gaseous effluent and CO 2 .
  • Two columns 52, 54 provided with trays 53, 55 imposing a tortuous path to the gases are connected in series between the pipe 44 and a pipe 56 provided with a valve 57.
  • a pump 58 is mounted on the pipe 56, between the valve 57 and a valve 59 in order to be able to switch on or isolate the pump 58.
  • the pump 58 makes it possible to establish the desired reduced pressure level in the furnace. Although only one pump is shown, the presence of two pumps can be considered for the sake of redundancy.
  • the gaseous effluent extracted by the pump 58 is fed to a burner 60 which supplies a stack 62.
  • the oven 10 is equipped with temperature sensors connected to the control circuit 20 in order to set the heating temperature to the desired value.
  • Two sensors 64 for example, is used, 64 b consist of pyrometers optical sighting, which are fitted in the lid 28 under 28a 28b windows made therein openings 14a and 14b formed in the cover 14 of the susceptor .
  • the use of several pyrometric sensors is not a necessity, but makes it possible to measure at different levels and to eliminate any aberrant measurements by comparison. Preference is given to using bichromatic type pyrometers producing a continuously exploitable continuous signal.
  • the temperature measured by the sensors 64a 64b is transmitted to the control circuit 20 to supply the inductor to change this temperature according to a preset temperature rise profile.
  • the sodium contained in the fibrous textures is released and is discharged with the gaseous effluent in a sublimated form, in the elemental state and optionally in the combined state, for example in the state of sodium oxide NaO 2 .
  • CO 2 is injected into the pipe 44 with a controlled flow rate by opening the valve 49 in order to carry out a neutralization of Na (or NaO 2 ) as soon as it leaves the furnace and to avoid its deposition on the walls of the pipe 44.
  • CO 2 injection can be started at a temperature below 900 ° C. This injection is also preferably continued at least until the end of the process.
  • the sodium carbonate product is collected in particular in the tray columns 52, 54.
  • the purified gaseous effluent of sodium is fed to the burner 60.
  • the extraction device 40 or at least a part thereof comprising the tray columns 52, 54 and optionally the pipe 44 is cleaned periodically to eliminate in particular the deposited sodium carbonate.
  • the cleaning can be carried out by rinsing with water in situ or by washing with water in a washing container after at least partial disassembly of the extraction device.
  • the neutralization of sodium is carried out by hydration.
  • the pipe 44 is provided with one or more injection devices 70 for example in the form of hollow rings 72 surrounding the pipe 44.
  • the injection device 70 is placed immediately downstream of the bend 44a, with interposition an isolation valve 71 between the outlet 42 of the oven and the injection device 70.
  • two rings are provided spaced apart from each other along the pipe 44.
  • the rings injection 72 are fed in parallel through a pipe 74 connected on the one hand to a source of neutralizing agent, for example a source of water vapor via a pipe 76 provided with a valve 75 and, secondly, a source of neutral gas such as nitrogen or argon, via a pipe 78 provided with a valve 57.
  • the pipe 44 Downstream of the injection device 70, in the flow direction of gaseous effluent, the pipe 44 has a purge port connected to a purge pipe 80 provided with a valve 81. Downstream of the connection with the pipe of purge, the pipe 44 can be connected directly to the pump 58 through the valve 57, the use of tray columns is not necessary here. The rest of the installation is identical to what was described above.
  • Each injection ring 72 forms an O-ring surrounding the pipe 44 and communicating with it through holes 74 formed in the wall of the pipe.
  • the holes 74 may be inclined relative to the normal to the wall of the pipe 44 to direct the flow of neutralization agent downstream.
  • the injection of the mixture H 2 O + N 2 can be carried out during the heat treatment process, as described above with regard to the CO 2 injection, or after the end of the heat treatment process to hydrate the sodium deposited on the wall of the pipe 44.
  • the pipe 44 may be insulated along its portion connecting the pipe. output 42 to this injection device. Insulation 43 prevents premature sodium condensation on the wall of pipe 44 by too rapid cooling of the gaseous effluent.
  • the insulation 43 may be replaced or supplemented by heating means for example by electrical resistors.
  • valves 75 and 81 are open, the valves 71, 57 and 77 are closed and water in liquid form is admitted into the pipe 76 and thence into the injection device 70.
  • Several rinses consecutive lines of the line 44 can be carried out to remove the soda produced by neutralization of sodium.
  • drying of the pipe 44 can be achieved by simply opening the valve 57 and turning on the pump 58, the valves 75 and 81 being closed.
  • the dilution with nitrogen is preferred to avoid a too violent reaction with sodium, the amount of sodium to be neutralized being low.
  • the injected CO 2 can also be diluted by mixing with nitrogen.
  • the method and the installation which have just been described are particularly suitable for carbon products obtained from pre-oxidized PAN precursor, in particular for fibrous carbon textures intended for the manufacture of parts made of carbon / resin composite material C / C or C / ceramic, for example silicon carbide matrix (C / SiC) or ternary matrix silicon-boron-carbon (C / Si-BC).
  • C / SiC silicon carbide matrix
  • C / Si-BC ternary matrix silicon-boron-carbon
  • the textures are made of fibers in the precursor state of carbon more capable of undergoing textile operations than carbon fibers.
  • These textures may be one-dimensional such as wires or cables, or two-dimensional, such as fabrics or webs formed of parallel son or cables, or three-dimensional, such as preforms obtained by filament winding, or by stacking, winding or draping fabrics or plies in superimposed layers and possibly linked together by needling or stitching, for example.
  • fibrous preforms are nozzle preforms or divergent nozzles or brake disc preforms.
  • the invention also applies to carbon products, obtained from carbon precursor materials other than preoxidized PAN, also containing sodium and optionally one or more other metals or metal impurities to be removed.
  • carbon precursor materials other than preoxidized PAN, also containing sodium and optionally one or more other metals or metal impurities to be removed.
  • Examples of such precursors are pitches, phenolic materials, or rayon.
  • the process according to the invention is advantageous in that it makes it possible to eliminate sodium which is present at a very low content in the fibers, for example less than 80 ppm, which sodium would be impossible to remove by another method such as rinsing with water. 'water. It also makes it possible to eliminate sodium present in larger amounts in the fibers, for example at more than 3500 ppm.
  • calcium and / or magnesium can be removed by sublimation.
  • metals such as Fe, Ni and Cr may also have to be eliminated in addition to sodium. It is then necessary to perform the heat treatment to a temperature sufficient to ensure the sublimation of these metals, for example a temperature up to 2000 ° C or 2200 ° C, or 2500 ° C.

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Treatment Of Fiber Materials (AREA)
  • Treating Waste Gases (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Waste-Gas Treatment And Other Accessory Devices For Furnaces (AREA)
  • Muffle Furnaces And Rotary Kilns (AREA)
  • Furnace Details (AREA)
  • Inorganic Fibers (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)

Claims (12)

  1. Verfahren zur Wärmebehandlung von natriumhaltigen Kohlenstoffprodukten, wonach die Produkte in einem Ofen unter vermindertem Druck sowie unter Spülen mit Neutralgas erhitzt werden und Abgase, die Natrium in sublimierter Form enthalten, über eine Rohrleitung zum Abführen der Abgase kontinuierlich aus dem Ofen abgezogen werden, dadurch gekennzeichnet, daß wenigstens ein Produkt zur Neutralisierung des Natriums in die Rohrleitung zum Abführen der Abgase, direkt nach dem Austritt der Abgase aus dem Ofen eingespritzt wird.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Produkt zur Neutralisierung des Natriums aus Kohlendioxid und Wasserdampf ausgewählt ist.
  3. Verfahren nach einem der Ansprüche 1 und 2, dadurch gekennzeichnet, daß das Neutralisierungsprodukt im Bereich eines oder nach einem durch die Rohrleitung zum Abführen der Abgase aus dem Ofen gebildeten Krümmer(s) eingespritzt wird.
  4. Verfahren nach einem der Ansprüche 2 und 3, dadurch gekennzeichnet, daß das eingespritzte Neutralisierungsprodukt in einem Neutralgas verdünnt wird.
  5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß das Neutralgas Stickstoff oder Argon ist.
  6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß das Neutralisierungsprodukt in den während der Wärmebehandlung aus dem Ofen abgezogenen Abgasstrom kontinuierlich eingespritzt wird.
  7. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß das Neutralisierungsprodukt nach dem Ende der Wärmebehandlung in die Abführrohrleitung eingespritzt wird, um Natrium, das sich an der Wand der Abführrohrleitung abgesetzt hat, vor deren Reinigung zu neutralisieren.
  8. Anlage zur Wärmebehandlung von natriumhaltigen Kohlenstoffprodukten, umfassend einen Ofen (10), Mittel (30) zum Beaufschlagen des Ofens mit Spülneutralgas sowie eine Rohrleitung (44) zum Abführen der Abgase aus dem Ofen, dadurch gekennzeichnet, daß sie ferner Mittel (50; 72) zum Einspritzen eines Produkts zum Neutralisieren des Natriums in die Abführrohrleitung (44), direkt nach dem Ausgang des Ofens umfaßt.
  9. Anlage nach Anspruch 8, dadurch gekennzeichnet, daß sie wenigstens eine in die Abführrohrleitung (44) eindringende Düse (50) zum Einspritzen eines Neutralisierungsprodukts umfaßt.
  10. Anlage nach Anspruch 9, dadurch gekennzeichnet, daß die Düse (50) in einen Krümmer (44a) der Abführrohrleitung (44) eindringt.
  11. Anlage nach einem der Ansprüche 8 bis 10, dadurch gekennzeichnet, daß sie mehrere, entlang der Abführrohrleitung beabstandete Punkte zum Einspritzen eines Neutralisierungsmittels aufweist.
  12. Anlage nach einem der Ansprüche 8 bis 10, dadurch gekennzeichnet, daß die Abführrohrleitung (44) mit einer Entlüftungsvorrichtung (80, 81) ausgestattet ist.
EP03748208A 2002-07-12 2003-07-11 Verfahren und anlage zur thermischen behandlung von natrium-enthaltenden kohlenstoffprodukten Expired - Lifetime EP1525342B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0208818 2002-07-12
FR0208818A FR2842191B1 (fr) 2002-07-12 2002-07-12 Procede et installation de traitement thermique de produits en carbonne contenant du sodium
PCT/FR2003/002204 WO2004007819A2 (fr) 2002-07-12 2003-07-11 Procede et installation de traitement thermique de produits en carbone contenant du sodium

Publications (2)

Publication Number Publication Date
EP1525342A2 EP1525342A2 (de) 2005-04-27
EP1525342B1 true EP1525342B1 (de) 2009-04-22

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EP03748208A Expired - Lifetime EP1525342B1 (de) 2002-07-12 2003-07-11 Verfahren und anlage zur thermischen behandlung von natrium-enthaltenden kohlenstoffprodukten

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Country Link
US (1) US7351390B2 (de)
EP (1) EP1525342B1 (de)
JP (1) JP4327086B2 (de)
CN (1) CN1329566C (de)
AT (1) ATE429533T1 (de)
AU (1) AU2003267517A1 (de)
CA (1) CA2492218C (de)
DE (1) DE60327321D1 (de)
FR (1) FR2842191B1 (de)
MX (1) MXPA05000569A (de)
WO (1) WO2004007819A2 (de)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8771623B2 (en) * 2009-10-30 2014-07-08 Goodrich Corporation Methods and apparatus for residual material management
FR2953826B1 (fr) * 2009-12-16 2019-10-11 Safran Landing Systems Procede de fabrication d'une piece de friction a base de materiau composite c/c
US11236021B2 (en) 2017-12-22 2022-02-01 Goodrich Corporation Mitigating pyrophoric deposits in exhaust piping during SIC CVI/CVD processes by introducing water vapor into an outlet portion of a reaction chamber

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3179605A (en) * 1962-10-12 1965-04-20 Haveg Industries Inc Manufacture of carbon cloth
US3413094A (en) * 1966-01-24 1968-11-26 Hitco Method of decreasing the metallic impurities of fibrous carbon products
GB1284399A (en) * 1968-11-27 1972-08-09 Courtalds Ltd Filamentary carbon
GB1600640A (en) * 1977-05-26 1981-10-21 Hitco Method of removing alkali and alkaline earth impurities from carbonizable polyacrylonitrile material
US4507272A (en) * 1983-05-09 1985-03-26 Hitco Method of purifying partially carbonized pan material prior to carbonization
GB8703323D0 (en) * 1987-02-13 1987-03-18 British Petroleum Co Plc Separation process
US5154776A (en) * 1989-05-18 1992-10-13 Bloch Christopher J Method for decontamination of vessels and other equipment polluted with metallic sodium and other reactive metals
FR2842193B1 (fr) * 2002-07-12 2004-10-01 Messier Bugatti Procede et installation pour le traitement thermique a haute temperature et la densification par infiltration chimique en phase vapeur de textures en carbone

Also Published As

Publication number Publication date
WO2004007819A2 (fr) 2004-01-22
DE60327321D1 (de) 2009-06-04
JP2005533193A (ja) 2005-11-04
CA2492218A1 (en) 2004-01-22
ATE429533T1 (de) 2009-05-15
CN1668789A (zh) 2005-09-14
AU2003267517A1 (en) 2004-02-02
JP4327086B2 (ja) 2009-09-09
US20040009116A1 (en) 2004-01-15
CN1329566C (zh) 2007-08-01
FR2842191B1 (fr) 2004-10-01
WO2004007819A3 (fr) 2004-04-08
MXPA05000569A (es) 2005-04-28
FR2842191A1 (fr) 2004-01-16
CA2492218C (en) 2010-10-26
US7351390B2 (en) 2008-04-01
EP1525342A2 (de) 2005-04-27

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