EP0778354B1 - Procédé d'alimentation de gaz protecteur dans un four de traitement thermique et installation de traitement thermique - Google Patents

Procédé d'alimentation de gaz protecteur dans un four de traitement thermique et installation de traitement thermique Download PDF

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Publication number
EP0778354B1
EP0778354B1 EP96119651A EP96119651A EP0778354B1 EP 0778354 B1 EP0778354 B1 EP 0778354B1 EP 96119651 A EP96119651 A EP 96119651A EP 96119651 A EP96119651 A EP 96119651A EP 0778354 B1 EP0778354 B1 EP 0778354B1
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EP
European Patent Office
Prior art keywords
gas
zone
oxygen
furnace
protective
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
EP96119651A
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German (de)
English (en)
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EP0778354A1 (fr
Inventor
Reinhard Dipl.-Ing. Strigl
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.)
Linde Gas AG
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Linde Gas AG
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    • 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
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04527—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general
    • F25J3/04539—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the H2/CO synthesis by partial oxidation or oxygen consuming reforming processes of fuels
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04563—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating

Definitions

  • the invention relates to a method for supplying protective gas to a heat treatment furnace with several zones, in particular an entry and exit zone and a heating zone in which the protective gas is obtained using source gas is generated with an air separation plant working on site.
  • the invention relates to a corresponding heat treatment plant.
  • This reaction is usually carried out with one next to the one or more heat treatment furnaces arranged, in the core of a gas generator consisting of a catalyst accomplished, and the so-called endogas formed in the generator is in Usually supplied to the associated heat treatment system without further treatment. It is also known to use the same starting gas mixture in an oven arranged and in this way already set to a higher temperature level Implement catalyst retort and the product gas either directly into the furnace allow to flow in or also to subtract and distribute (see e.g. DE 39 42 810 A1.
  • EP-A-0 261 461 discloses a method for the heat treatment of metallic workpieces by means of a continuous furnace.
  • the treatment atmosphere in the area of the heating zone is supplied in the form of a gas mixture which is generated by a catalytic reaction of a hydrocarbon and air-containing gas.
  • the areas at the oven inlet and outlet are supplied with nitrogen.
  • the oxygen-contaminated nitrogen obtained from the dismantling plant directly that is to say without post-purification, as a protective gas, specifically in furnace zones in which the oxygen content of the protective gas is less critical.
  • these are generally the colder supply and removal tunnels in front of the heating chamber (prechamber) or, in the case of continuous systems, the inlet area in front of the heating zone or treatment chamber (inlet chamber with subsequent zone) and the cooling zone or cooling chamber of the system on the outlet side.
  • the nitrogen shielding gas not warmed up according to the invention also acts as a particularly effective cooling gas.
  • the proportion of oxygen to be converted in this gas fraction is very high - namely at least about 25% - so that an effective conversion reaction between the oxygen of the said product gas and a correspondingly admixed KW gas is appropriate 1.5 O 2 + 3.5 N 2 + 3 CH 4 ⁇ 3 CO + 6 H 2 + 3.5 N 2 can take place. Since the starting gas used here has a relatively low nitrogen content, the unnecessarily heated gas content is relatively low compared to the above-mentioned post-purification of impure nitrogen, and the formation of protective gas is therefore comparatively energy-efficient.
  • the predominantly Nitrogen-containing fraction with a purity of at least 98.5% and the oxygen-rich starting gas fraction is produced with 25 to 35% oxygen.
  • a particularly favorable embodiment of the procedure according to the invention is thereby characterized in that the oxygen-rich starting gas with one in the heat treatment furnace arranged catalyst retort is implemented, the retort and the reactants to a temperature above 500 ° C, preferably above 800 ° C, are heated, for which purpose the retort may be additionally heated.
  • the figure shows an elongated continuous furnace D with an inlet zone 3, a central heating and treatment zone 5 and a cooling zone 7.
  • a catalyst retort 2 inside the furnace, that is to say an aggregate containing a catalyst material and having gas outlet openings at its head end , arranged, which is connected via gas lines 6 and 8 on the one hand to a membrane-based, ie permeate air separation plant 1 and its oxygen outlet O 2+ and on the other hand is connected via lines 6 and 10 to a hydrocarbon source CnHm, eg natural gas.
  • a hydrocarbon source CnHm eg natural gas.
  • the second product gas outlet N 2 of the air separator 1 i.e.
  • the one which supplies a nitrogen-rich gas is finally connected directly to the heat treatment furnace via lines 11, 12 and 14, the gas supply line, however, specifically into the furnace inlet zone 3 - line 12 - and into the furnace outlet zone 7 - Line 14 - done.
  • the middle part of the heat treatment plant is not supplied with any gas which does not come from the nitrogen outlet of the air separation plant and is not further treated.
  • the shielding gas requirement of the continuous furnace shown can be, for example, 150 m 3 / h.
  • the permeation air separation plant 1 shown is now set so that approximately 110 m 3 of nitrogen gas with 99% purity are made available per hour.
  • This nitrogen gas, the so-called retentate is fed to the inlet zone 3 and the outlet zone 7 of the furnace shown in a quantity of 55 m 3 / h in each case, without removing further oxygen therefrom.
  • the still necessary for the heating zone 5, 40 m 3 / h of very low-oxygen protective gas are obtained according to the invention from the oxygen-rich gas, the so-called permeate, which also occurs in larger quantities in the operation of the air separation plant 1 described.
  • this is done by mixing 15.6 m 3 of this permeate, which contains about 31% oxygen and 69% nitrogen, in mixer 9 with 7 m 3 / h of natural gas (methane) and catalytically gas mixture obtained in catalyst retort 2 is converted to a protective gas containing about 24% CO, 48% H 2 and 28% N 2 and is released as such into the heating zone 5 of the furnace.
  • the catalyst 2 which is preferably a nickel catalyst, must be set to temperatures above 800 ° C., preferably 900 to 1050 ° C.
  • a large part of the heat supply for maintaining this temperature level is already guaranteed by the heating in the heating zone 5 of the continuous furnace D, which is heated to, for example, 800 to 900 ° C.
  • the protective gas quantity of 40 m 3 / h required for the heating zone is obtained.
  • Excess oxygen-rich permeate is released to the environment via an outlet A installed in the gas line 8 or advantageously supplied as O 2 -enriched air to the other jet pipes instead of air as an oxygen carrier for heating the jet pipes.
  • the shielding gas supplied in the middle part of the furnace represents a shielding gas consisting essentially of CO, H 2 and N 2 , while the shielding gas supplied on the inlet and outlet sides consists of almost pure nitrogen, the nitrogen purity for the complete avoidance of metallurgically disadvantageous effects at least about 99 % should be.
  • the supply of differently composed protective gases according to the invention also results in a protective gas composition that varies somewhat over the length of the furnace, which leads to an equally locally varying gas reactivity, which has its peak in particular in the heating zone of the furnace and which decreases towards the furnace ends.
  • an atmosphere with about 12% CO, 24% H 2 and 64% N 2 is usually established in the heating zone at the described conditions, which gives an atmosphere which is particularly advantageous for many annealing treatments, which is somewhat reducing and in terms of the carburizing effect has almost neutral properties for many materials.
  • the supply of the cold nitrogen shielding gas in the outlet area of the continuous furnace achieves an improved cooling performance compared to other annealing processes.
  • the method according to the invention thus has advantages such as the improved economy and the increased cooling capacity compared to methods in which only the nitrogen product of an on-site air separator is used for protective gas production, and thus represents an advantageous alternative to these methods.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Furnace Details (AREA)
  • Control Of Heat Treatment Processes (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)

Claims (6)

  1. Procédé pour l'alimentation en un gaz de protection d'un four de traitement thermique présentant plusieurs zones, en particulier une zone d'entrée et une zone de chauffage ainsi que, le cas échéant, une zone de sortie, dans lequel on alimente en différents gaz de protection les différentes zones, caractérisé en ce que chaque gaz de protection est obtenu avec utilisation d'un gaz de départ, qui est produit avec une installation de séparation d'air fonctionnant sur place, la fraction de gaz de départ obtenue avec l'installation de séparation, contenant essentiellement de l'azote, étant produite avec une pureté d'au moins 98,5% et introduite sans autre élimination d'oxygène dans la zone d'entrée et, le cas échéant, dans la zone de sortie du four en tant que gaz de protection, et un gaz de protection convenant pour la zone de chauffage ou de traitement étant obtenu par le fait qu'au moins une partie de la fraction riche en oxygène, également produite par l'installation de séparation, cette fraction étant produite avec une proportion d'oxygène d'au moins 25%, est mélangée avec un gaz hydrocarbure, par le fait que ce mélange est transformé catalytiquement, avec apport de chaleur, en un mélange gazeux contenant essentiellement, outre de l'azote, du monoxyde de carbone et de l'hydrogène, et par le fait que ce mélange gazeux est amené à la zone de chauffage (zone chaude) du four en tant que gaz de protection.
  2. Procédé selon la revendication 1, caractérisé en ce que la séparation d'air sur place est réalisée par perméation ou adsorption.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce qu'on produit une fraction de gaz de départ riche en oxygène, contenant 25 à 35% d'oxygène.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que le gaz de départ riche en oxygène est transformé avec un gaz hydrocarbure et avec une cornue de catalyseur disposée dans le four de traitement thermique, la cornue et les partenaires de réaction étant chauffés à une température supérieure à 500°C, de préférence supérieure à 800°C, la cornue étant à cette fin le cas échéant chauffée en supplément.
  5. Procédé selon la revendication 1, caractérisé en ce que le gaz hydrocarbure est du gaz naturel ou du propane.
  6. Four de traitement thermique avec une alimentation en gaz de protection, la zone d'entrée et, le cas échéant, la zone de sortie (3, 7) du four étant équipées de conduites d'alimentation en gaz (12, 14) et un aggrégat de transformation (2) pour l'oxygène avec un gaz hydrocarbure étant présent, qui délivre son gaz produit à la zone de chauffage (5) du four ou selon le cas le transporte, et qui est d'autre part raccordé à des sources de gaz (CnHm) correspondantes, caractérisé en ce que l'alimentation en gaz de protection comporte en outre une installation de séparation d'air (1), la sortie de gaz produit (N2) de l'installation de séparation d'air (1), qui fournit la fraction de gaz contenant essentiellement de l'azote (N2), étant d'une part raccordée aux conduites d'alimentation en gaz (12, 14) pour la zone d'entrée et, le cas échéant, la zone de sortie (3, 7) du four, et la sortie de gaz produit (O2+) de l'installation de séparation d'air (1), qui fournit la fraction riche en oxygène, étant d'autre part en liaison avec l'aggrégat de transformation (2) via des conduites (8, 6).
EP96119651A 1995-12-07 1996-12-06 Procédé d'alimentation de gaz protecteur dans un four de traitement thermique et installation de traitement thermique Expired - Lifetime EP0778354B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19545764 1995-12-07
DE19545764A DE19545764C2 (de) 1995-12-07 1995-12-07 Verfahren zur Schutzgaserzeugung für einen Wärmebehandlungsofen und Wärmebehandlungsanlage

Publications (2)

Publication Number Publication Date
EP0778354A1 EP0778354A1 (fr) 1997-06-11
EP0778354B1 true EP0778354B1 (fr) 2001-04-04

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EP96119651A Expired - Lifetime EP0778354B1 (fr) 1995-12-07 1996-12-06 Procédé d'alimentation de gaz protecteur dans un four de traitement thermique et installation de traitement thermique

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EP (1) EP0778354B1 (fr)
AT (1) ATE200307T1 (fr)
DE (2) DE19545764C2 (fr)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT1291479B1 (it) * 1997-01-29 1999-01-11 Rivoira Spa Procedimento di trattamento termico di pezzi metallici a base ferrosa in un'atmosfera attiva ad elevato potenziale di carbonio.
DE10051203A1 (de) * 2000-10-16 2002-04-25 Linde Ag Verfahren und Vorrichtung zur Erzeugung eines CO- und H2-haltigen Behandlungsgases für die Wärmebehandlung
DE10300141A1 (de) 2003-01-07 2004-07-15 Blue Membranes Gmbh Verfahren und Vorrichtung zur Sauerstoffanreicherung von Luft bei gleichzeitiger Abreicherung von Kohlendioxid
DE10347312B3 (de) * 2003-10-08 2005-04-14 Air Liquide Deutschland Gmbh Verfahren zur Wärmebehandlung von Eisenwerkstoffen
DK1718171T4 (da) 2004-01-28 2020-01-06 Curation Foods Inc Beholdersystem
EP1916915A4 (fr) 2005-07-28 2010-06-02 Apio Inc Combinaisons d'elements de regulation d'atmosphere
DE102005041817A1 (de) * 2005-09-02 2007-03-08 Behr Gmbh & Co. Kg Anlage zum Herstellen von gelöteten Bauteilen
DE102006013428B4 (de) * 2006-03-23 2012-09-13 Behr Gmbh & Co. Kg Anlage und Verfahren zum Herstellen von gelöteten Bauteilen in einer Schutzgasatmosphäre
CN102822612B (zh) * 2010-04-13 2016-01-13 开利公司 受控大气系统和方法
JP2019189942A (ja) * 2018-04-24 2019-10-31 エア・ウォーター株式会社 金属の焼鈍方法

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BR8504616A (pt) * 1985-09-20 1987-04-28 Aichelin Ind E Comercio De For Processo para o enriquecimento da atmosfera de fornos de tratamentos termoquimicos de pecas metalicas
DE3630833A1 (de) * 1986-09-10 1988-03-17 Linde Ag Verfahren und vorrichtung zur waermebehandlung metallischer werkstuecke
DE3942810A1 (de) * 1989-12-23 1991-06-27 Linde Ag Verfahren zur bereitstellung und verteilung von behandlungsgas bei waermebehandlungen
FR2668584B1 (fr) 1990-10-26 1994-03-18 Lair Liquide Procede d'elaboration d'une atmosphere de traitement thermique et installation de traitement thermique.
DE4212307C2 (de) * 1992-04-13 1994-07-28 Messer Griesheim Gmbh Verfahren zur Herstellung eines Schutz- oder Reaktionsgases für die Wärmebehandlung von Metallen
US5364476A (en) * 1993-11-08 1994-11-15 Surface Combustion, Inc. Industrial variable carbon potential gas generator

Also Published As

Publication number Publication date
DE19545764A1 (de) 1997-06-12
EP0778354A1 (fr) 1997-06-11
DE19545764C2 (de) 2000-02-17
DE59606708D1 (de) 2001-05-10
ATE200307T1 (de) 2001-04-15

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