EP2135961B1 - Procédé et dispositif destinés au traitement à chaud de matières métalliques sous atmosphère protectrice - Google Patents

Procédé et dispositif destinés au traitement à chaud de matières métalliques sous atmosphère protectrice Download PDF

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Publication number
EP2135961B1
EP2135961B1 EP20090007348 EP09007348A EP2135961B1 EP 2135961 B1 EP2135961 B1 EP 2135961B1 EP 20090007348 EP20090007348 EP 20090007348 EP 09007348 A EP09007348 A EP 09007348A EP 2135961 B1 EP2135961 B1 EP 2135961B1
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Prior art keywords
gas
treatment
protective gas
heating chamber
area
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EP20090007348
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German (de)
English (en)
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EP2135961A3 (fr
EP2135961A2 (fr
Inventor
Bernd Dr. Edenhofer
Hendrik Grobler
Peter Haase
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Ipsen International GmbH
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Ipsen International GmbH
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Priority to PL09007348T priority Critical patent/PL2135961T3/pl
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/20—Carburising
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/76—Adjusting the composition of the atmosphere
    • C21D1/763—Adjusting the composition of the atmosphere using a catalyst
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D11/00—Process control or regulation for heat treatments

Definitions

  • the invention relates to a method and a device for heat treatment of metallic materials in an industrial furnace comprising a heating chamber with a treatment chamber and a quenching chamber using protective gas and reaction gas.
  • U. a. are in the DE 36 32 577 Catalyst beds, in the DE 38 88 814 Catalyst-like linings with net-like structures of furnaces, in the DE 40 05 710 Ni, Mn, Cr. Fe-containing full metallic oxidation catalysts and in the DE 44 16 469 a two-stage nitrocarburizing by Ni o. Cu catalyst described.
  • FR 2181 597 A1 Endogas should be used as a carrier gas plus additional gas in a continuous furnace for the gas fumigation and process gas to be saved, with an exhaust gas recirculation is provided.
  • the treatment of the kiln exhaust gas takes place by adding and passing air.
  • As the catalyst type an oxidizing catalyst with nickel oxide is used, which is mounted in the furnace housing.
  • the exhaust gases are cooled with a cooler.
  • a CP control is carried out by adding hydrocarbon (HC) in the space of the furnace housing.
  • HC hydrocarbon
  • This teaching discloses only technologically a carburizing, in which by directly in or in the furnace by reaction of the furnace supplied with oxygen KW, possibly. Supported by a catalyst device located in or in the furnace, as a peculiarity of the KW gaseous alkenes, preferably propylene and ethylene , be used.
  • the practice of the heat treatment of metallic materials under inert gas as in the gas carburizing arranges so that the heat treatment furnace is fumigated with a reducing inert gas.
  • This shielding gas usually consists of carbon monoxide, hydrogen, water vapor, carbon dioxide and nitrogen.
  • the fumigation introduction takes place in the heating chamber.
  • a cold treatment chamber is connected to this heating chamber as a so-called quenching chamber. Separately, both chambers are usually through a gas-permeable door.
  • the gas fed into the heating chamber thus also enters the cold treatment chamber. From this, the protective gas is then discharged at a burn-off point, safely ignited by a pilot burner and burned.
  • the catalyst used on the catalyst bed should advantageously have nickel, platinum, palladium or rhodium.
  • Natural gas is used as reaction gas.
  • gas enrichment takes place at the catalyst bed according to the reactions 2CH 4 + O 2 ⁇ 2CO + 4H 2 CH 4 + CO 2 ⁇ 2CO + 2H 2 CH 4 + H 2 O ⁇ CO + 3H 2 instead, where the C-level increases and Vol.% CO 2 , H 2 O and O 2 fall off.
  • the C potential (carbon potential) is controlled by gas analysis, whereby a temperature measurement is possible.
  • air and hydrocarbon gas are used so that an amount of air is supplied when the C level is to decrease; when the C-level is increased, hydrocarbon gas is supplied.
  • the C potential present in the treatment chamber of the heating chamber is regulated after the feed of the hydrocarbon at the catalyst bed.
  • the C potential present in the treatment chamber of the heating chamber is regulated by feeding the hydrocarbon into the treatment space, the hydrocarbon reacting in a recirculating manner on the catalyst bed.
  • the shielding gas is then conducted to a burn-off point, ignited and burned off when there is an impermissible pressure rise, thus regulating the operating pressure, or when a brief flushing process requires it.
  • the working pressure is preferably 1 to 10 mbar.
  • reaction gas and air or inert gas can be supplied accordingly. Any resulting excess of H 2 is separated.
  • the method provides that a forced circulating gas guide is carried out, which is largely isothermal to avoid undesirable reactions such as soot formation.
  • the forcibly recirculated gas guide can be carried out by means of recirculating gas removal from the region of the heating chamber without gas cooling or alternatively by means of recirculating gas removal from the region of the quenching chamber.
  • a heating chamber for the quenching chamber gas-tight final interior door is arranged.
  • the treatment room has several feed points for the feed of the recovered protective gas and / or the feed of the hydrocarbon, the z. B. as the first and second feed points for the feed of the hydrocarbon can be formed.
  • the treatment room with catalyst bed can be locally separated from the treatment room.
  • the C-potential controller comprises an O 2 probe, a CO analyzer and a temperature gauge.
  • the invention thus aims at a novel inert gas recirculation system for gas carburizing in which the components carbon dioxide, oxygen and water vapor are reacted with a hydrocarbon feed, e.g. Natural gas again catalytically react to carbon monoxide and hydrogen.
  • a hydrocarbon feed e.g. Natural gas again catalytically react to carbon monoxide and hydrogen.
  • the alternatively shown C-potential control can be carried out advantageously by means of atmospheric analysis.
  • the "treated" inert gas can then be fed back to the feed points, so that sets a real cycle and gas carburizing is continued.
  • the device-side requirements for this recirculation system can be met depending on the process variant by a gas-tight inner door or a gas-tight outer door.
  • the burn-off by means of a gas-tight valve must still open in case of impermissible pressure increases in the furnace in order to regulate the operating pressure.
  • the working pressure should be between 10 and 100 mmWS or 1 to 10 mbar.
  • Natural gas and air or inert gas are supplied in an appropriate amount.
  • Another advantage is the control of the C potential according to the disclosed variants. Carburization of components due to immediate hydrocarbon dissociation is therefore excluded.
  • the gas routing may be largely isothermal to avoid undesirable reactions such as e.g. To avoid soot.
  • C-potential regulated in situ catalytic gas generation in combination with flow recirculation in a heat treatment furnace functionally fuses to a surprisingly novel effect with the illustrated beneficial effects.
  • the method is typical that in detail the process steps of the heat treatment are associated with the stages of inert gas recovery.
  • the drawing shows a simplified representation of an industrial furnace with schematic superimposition of the reaction sequences of the method and features of the invention essential to a construction variant of the device.
  • the drawing outlines, in a simplified representation, an industrial furnace 1 which is used in practice and which comprises a heating chamber 2 with a treatment space 2.1 and a treatment space 3 with a catalyst bed 3.1 and an associated quenching chamber 8.
  • the treatment room 3 with catalyst bed 3.1 is in this example structurally connected to the treatment room 2.1, but it may be locally separated and functionally assigned, which construction is not shown here.
  • the materials and constructions known from the known state of the art can be used, such as the systems of catalysts known from the automotive industry.
  • Said components form a functional control loop R, which is essential to the invention.
  • a gas-tight inner door 7 between the heating chamber and the subsequent quenching chamber 8 for a recirculating gas removal from the area of the heating chamber 2 without gas cooling, a gas-tight inner door 7 between the heating chamber and the subsequent quenching chamber 8.
  • the gas is taken from the area of the quenching chamber 8, the inner door 7 gas-tight closing arranged between the heating chamber 2 and quenching chamber 8, but provided the quenching chamber 8 with a gas-tight closing outer door 9.
  • Both construction variants are also essential to the invention compared with the so-called open systems described in the prior art, such as with gas-permeable doors, and also support the system of the control loop R in its function according to the method.
  • the C-potential is required, by means of the C-potential controller 5 with O 2 probe 5.1, CO analyzer 5.2 and 5.3 temperature meter regulated so that the treated inert gas recirculating the treatment room 2.1 at first feed points 2.2 can be fed again.
  • the regulation of the C potential present in the treatment space 2.1 is also present after the feed of the hydrocarbon via the second feed points 3.2 on the catalyst bed 3.1 provided to adjust the demand-level C level.
  • a temperature measurement can be made.
  • the regulation of the present in the treatment chamber 2.1 C potential can alternatively be done after feeding of the hydrocarbon via the first feed points 2.2 in the treatment chamber 2.1 and thereby react the hydrocarbon at the catalyst bed 3.1 recirculating.
  • the protective gas can then be conducted, ignited and burned off to a burn-off point 6 if the burn-off must take place in the event of impermissible pressure increases in order to regulate the operating pressure or if a brief rinsing process requires this.
  • the treatment chamber must be rinsed to remove process-damaging foreign matter or to perform a gas exchange in the process, when e.g. the C-potetial should be lowered rapidly from 1.3% C to 0.6% C
  • the working pressure may preferably be 1 to 10 mbar, whereby higher pressures are possible.
  • reaction gas e.g. Natural gas 10 and 11 air or inert gas are supplied accordingly.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Furnace Details (AREA)
  • Waste-Gas Treatment And Other Accessory Devices For Furnaces (AREA)
  • Catalysts (AREA)

Claims (14)

  1. Procédé pour le traitement thermique de matériaux métalliques par carburation dans un four de traitement thermique, qui en tant que four industriel (1) comprend une chambre de chauffe et une chambre de trempe (8), à l'aide d'un gaz protecteur, dans lequel, pour la récupération du gaz protecteur,
    a) dans un espace de préparation (3), comportant un lit de catalyseur, de la chambre de chauffe du four industriel (1), les composants du gaz protecteur, comprenant du dioxyde de carbone, de l'oxygène et de la vapeur d'eau, subissent une réaction catalytique avec un hydrocarbure amené, servant de gaz de réaction, pour donner du monoxyde de carbone et de l'hydrogène, et
    b) après cette réaction, le gaz protecteur présente un potentiel carbone régulé,
    c) la réaction étant accélérée par utilisation d'un catalyseur au niveau du lit de catalyseur, et
    d) le gaz protecteur ainsi préparé étant renvoyé en recirculation dans un espace de traitement (2) de la chambre de chauffe.
  2. Procédé selon la revendication 1, caractérisé en ce que le catalyseur utilisé comprend du nickel, du platine, du palladium ou du rhodium.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que, dans chaque phase active de transfert de carbone du processus de carburation, on n'injecte que la quantité de carbone, sous forme d'un gaz de réaction, tel que le gaz naturel, qui est nécessaire à la carburation du gaz.
  4. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que, lors d'une carburation dans l'espace de traitement (2), les réactions suivantes se déroulent :

            2CO → C + CO2

            O + H2 → C + H2O

            CO → C + 0,502,

    puis le niveau de C diminue, et le pourcentage en volume de CO2, de H2O et de O2 augmente, et, dans l'espace de préparation (3), un enrichissement selon les réactions

            2CH4 + O2 → 2CO + 4H2

            CH4 + CO2 → 2CO + 2H2

            CH4 + H2O → CO + 3H2

    a lieu sur le lit de catalyseur, le niveau de C augmentant ici, et le pourcentage en volume de CO2, de H2O et de O2 diminuant.
  5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que le potentiel carbone dans l'espace de préparation (3) est, sur le lit de catalyseur, régulé par une analyse des gaz, et qu'une mesure de la température est effectuée.
  6. Procédé selon l'une des revendications 1 à 5, caractérisé en ce que le gaz protecteur est ensuite envoyé à une zone de calcination, enflammé et calciné quand on est en présence d'une augmentation de pression non admissible, ce à l'occasion de quoi on procède ainsi à une régulation de la pression de marche, ou encore quand une opération de rinçage de courte durée l'exige.
  7. Procédé selon l'une des revendications 1 à 6, caractérisé en ce que la pression de travail est de préférence de 1 à 10 mbar.
  8. Procédé selon l'une des revendications 1 à 7, caractérisé en ce que, en présence d'une chute de la pression de marche, on amène d'une manière correspondante le gaz de réaction et de l'air ou le gaz protecteur.
  9. Procédé selon l'une des revendications 1 à 8, caractérisé en ce qu'on sépare du H2 un excès qui se crée éventuellement.
  10. Procédé selon l'une des revendications 1 à 9, caractérisé en ce qu'on procède à une amenée de gaz à circulation forcée, qui a lieu dans des conditions isothermes pour éviter des réactions indésirables telles que la formation de suie.
  11. Dispositif pour la mise en oeuvre du procédé selon l'une des revendications 1 à 10, dans un four de traitement thermique, tel qu'un four industriel (1), qui comprend une chambre de chauffe comportant un espace de traitement (2) et un espace de préparation (3) comportant un lit de catalyseur, et qui présente aussi une chambre de trempe (8), caractérisé par
    a) un régulateur du potentiel carbone (5), qui effectue une analyse des gaz et qui correspond à l'espace de préparation (3),
    b) un recirculateur (4), pour le circuit fermé d'un gaz protecteur de recirculation, avec une amenée régulée de l'air et du gaz de réaction,
    c) une vanne (6.1), étanche aux gaz, allant vers une zone de calcination (6), comportant un régulateur de pression (6.2) et ayant pour fonction une amenée de gaz en cas de chute de pression,
    les composants a) et c) mentionnés ci-dessus étant fonctionnellement intégrés dans un circuit de régulation (R), et
    d) une porte intérieure (7), qui obture d'une matière étanche aux gaz la chambre de chauffe par rapport à la chambre de trempe (8).
  12. Dispositif selon la revendication 10, caractérisé en ce que l'espace de traitement (2) comprend plusieurs points d'injection (2.1) pour injecter le gaz protecteur récupéré.
  13. Dispositif selon la revendication 10 ou 11, caractérisé en ce que l'espace de traitement (3), comportant le lit de catalyseur, est localement séparé de l'espace de traitement (2).
  14. Dispositif selon l'une des revendications 10 à 12, caractérisé en ce que le régulateur (5) du potentiel carbone comprend une sonde à 02 (5.1), un analyseur de 0 (5.2) et un mesureur de température (5.3).
EP20090007348 2008-06-20 2009-06-03 Procédé et dispositif destinés au traitement à chaud de matières métalliques sous atmosphère protectrice Active EP2135961B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL09007348T PL2135961T3 (pl) 2008-06-20 2009-06-03 Sposób i urządzenie do obróbki cieplnej materiałów metalowych w atmosferze gazu ochronnego

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE200810029001 DE102008029001B3 (de) 2008-06-20 2008-06-20 Verfahren und Einrichtung zur Wärmebehandlung von metallischen Werkstoffen

Related Parent Applications (1)

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DE102008029001 Previously-Filed-Application 2008-06-20

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EP2135961A2 EP2135961A2 (fr) 2009-12-23
EP2135961A3 EP2135961A3 (fr) 2013-02-13
EP2135961B1 true EP2135961B1 (fr) 2014-10-01

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Country Link
US (1) US8313586B2 (fr)
EP (1) EP2135961B1 (fr)
JP (1) JP2010001567A (fr)
CN (1) CN101608294B (fr)
DE (1) DE102008029001B3 (fr)
PL (1) PL2135961T3 (fr)
RU (1) RU2009123209A (fr)

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DE102009038598B4 (de) 2009-08-26 2017-06-22 Ipsen International Gmbh Verfahren und Vorrichtung zur Aufbereitung von Prozessgasen für Wärmebehandlungen von metallischen Werkstoffen/Werkstücken in Industrieöfen
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Publication number Publication date
EP2135961A3 (fr) 2013-02-13
EP2135961A2 (fr) 2009-12-23
DE102008029001B3 (de) 2009-09-17
RU2009123209A (ru) 2010-12-27
CN101608294A (zh) 2009-12-23
JP2010001567A (ja) 2010-01-07
US8313586B2 (en) 2012-11-20
PL2135961T3 (pl) 2015-03-31
US20090314388A1 (en) 2009-12-24
CN101608294B (zh) 2013-10-23

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