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EP3049543A1 - Production of high-grade manganese from ferromanganese by means of vaporization in a vacuum induction plant - Google Patents

Production of high-grade manganese from ferromanganese by means of vaporization in a vacuum induction plant

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Publication number
EP3049543A1
EP3049543A1 EP14789775.5A EP14789775A EP3049543A1 EP 3049543 A1 EP3049543 A1 EP 3049543A1 EP 14789775 A EP14789775 A EP 14789775A EP 3049543 A1 EP3049543 A1 EP 3049543A1
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EP
European Patent Office
Prior art keywords
manganese
water cooling
condensation chamber
range
evaporator
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.)
Granted
Application number
EP14789775.5A
Other languages
German (de)
French (fr)
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EP3049543B1 (en
Inventor
Johann Reichel
Lutz Rose
Jan Bader
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.)
SMS Group GmbH
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SMS Group GmbH
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Publication of EP3049543A1 publication Critical patent/EP3049543A1/en
Application granted granted Critical
Publication of EP3049543B1 publication Critical patent/EP3049543B1/en
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/04—Refining by applying a vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B47/00—Obtaining manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/04—Alloys based on copper with zinc as the next major constituent

Definitions

  • the present invention relates to a process for the production of technically pure manganese by evaporation of carbonaceous ferromanganese in an induction vacuum vessel.
  • Manganese is one of the most important alloying elements in steelmaking. It is characterized by high strength and elongation. The production of steel grades with manganese takes place by adding manganese-containing alloying agents during the steelmaking process. These include Mn alloys produced in blast furnaces or high carbon reduction furnaces such as FeMnHC (HCFeMn) and FeMnLC (LCFeMn) alloys with medium FeMnMC (MCFeMn) and low carbon content. produced in secondary metallurgical plants.
  • the manganese alloys are loaded in addition to the carbon contents mentioned also with other elements such as phosphorus and sulfur, so that the application of materials can not be used indefinitely.
  • Typical composition of manganese alloys in% by weight are:
  • a pure manganese sulfate solution is used, which is electrolysed with stainless steel electrodes at 5 -7 V. Pure manganese is produced at the cathode and oxygen at the anode, which reacts with manganese ions to form brownstone.
  • Another way of Mangan strung is to heat the above manganese compounds so far, so that the manganese evaporates.
  • An object of the present invention is to provide a process for continuous manganese production by evaporation of the raw raw materials available, which is inexpensive and therefore economical.
  • the plant presented in the invention and the process represents an innovative technique not only in terms of continuous manganese production but also their potting.
  • the two-component system Mn-Fe represents various phases of the manganese-iron solution. As shown in the diagram below, the liquidus temperature of pure manganese is 1246 ° C.
  • the liquidus temperature is in the range 1246-1280 ° C. It defines the lowest temperature at which the liquid material starts to evaporate.
  • the vapor pressure as a function of the temperature has an exponentially increasing course.
  • Mn-vapor pressure In order to illustrate the physical conditions of the process according to the invention, the evaporation kinetics of manganese will be described below.
  • the evaporation kinetics of manganese is a function of pressure, temperature and inert gas rate.
  • the evaporation process itself is carried out by phase transformation - liquid / gas (steam) at a given temperature and pressure according to the law of the first order, as represented in equation (1), dMn
  • NMn Mn - volume flow in a vacuum vessel in Nm3 / min, directly proportional to the evaporation rate expressed by k (-dMn / dt),
  • Equations (4) and (5) in conjunction with equation (1) give the following relation:
  • Equation (6) represents the control principle based on the following quantities:
  • the method provides that the liquefaction of the Mn vapors takes place continuously by means of the secondary cooler, which is arranged in the vapor stream within a vapor line and is formed in a conical shape for the purpose of improving the drop outflow.
  • the vacuum pump system is additionally equipped with a secondary water cooling system, a condenser and a filter.
  • the evaporation process is additionally supported with argon as the inert gas and forms a kind of protective gas atmosphere.
  • the technically pure manganese is continuously cooled with water, tapped and placed under the Argon protective gas atmosphere in a casting machine, where it can be poured into the desired formats.
  • the evaporation material to be evaporated may consist of various Mn concentrations, which in turn may then influence the rate of evaporation, temperature and inert gas flow rate.
  • the evaporation material is charged continuously or discontinuously in the induction evaporator.
  • Another object of the present invention is to provide an apparatus for carrying out the method according to the invention.
  • a device in particular by an evaporator in which the manganese alloy is used, the metal under vacuum, and generated by a vacuum pump and filter system in the range of 10-900 mbar and a temperature In the range of> 1248 ° C stirring with argon is inert as a protective gas and is cooled by a primary water cooling and a secondary water cooling, the Mn vapors are collected in a mobile condensation chamber at temperatures in the range 1350-1400 ° C in the liquid state and is continuously abstechbar by a siphon-like heated tap hole in a Verg screensschieb.
  • the evaporator is an induction evaporator, which is arranged on a hydraulic platform and designed to be vertically movable over it.
  • the mobile condensation chamber is designed to be horizontally movable.
  • the induction evaporator and the condensation chamber are gas-tightly connected to one another via a steam line operatively connected to the primary water cooling and the secondary water cooling.
  • the secondary water cooling within the steam line is arranged in the vapor stream above the condensation chamber.
  • the steam line is connected to a supply line for the protective gas (inert gas) and the protective gas (inert gas) is circulated in the steam line and the supply line, wherein manganese manganese can be separated by a secondary condenser assigned to the feed line and the protective gas (inert gas) via the feed line to the induction evaporator and thus the steam flow is fed back.
  • additional inert gas can be supplied via the feed to the circuit in order to compensate for the process-related losses and so to be able to regulate the concentration in the circulatory system.
  • additional protective gas can be introduced via a feed into the supply line, where it can be flushed back into the induction evaporator via a secondary filter.
  • Fig. 1 is a schematic view of the apparatus for performing the method as a process flow model.
  • the device 18 consists essentially of an induction evaporator 1, in which the FeMn introduced is kept at a temperature of 1600 - 1700 ° C in the liquid state.
  • the induction evaporator 1 is arranged in this embodiment on a hydraulic platform 9, which allows it to raise and lower.
  • At least one flushing pipe connection 19 is provided, which is connected to a supply line 15 and via which a protective gas, in this case argon, is introduced into the induction evaporator 1.
  • a protective gas in this case argon
  • the protective gas rises through the FeMn melt, where it collects with the vaporized portion of manganese at a pressure of 100 to 200 mbar in a vapor line 14 and is discharged in a vapor stream 17, shown here as arrows.
  • the steam line 14 is connected in a gas-tight manner to the induction evaporator 1.
  • the steam flow 17 located in the steam line 14 is conducted past a primary water cooling 4, which surrounds the steam line from the outside, and is cooled down at the same time.
  • a secondary water cooling 5 the steam flow 17 is cooled down to the extent that an aggregate state change of the manganese from gaseous to liquid occurs. In order to do this as efficiently and quickly as possible, it is provided to arrange the secondary water cooling 5 within the steam line 14 and in the steam flow 17.
  • the secondary water cooling 5 is conical and lies with the tapered side in the direction of the incoming vapor stream 17. In the figure, this is shown as an isosceles triangle.
  • a horizontally movable condensation chamber 2 is arranged below the secondary water cooling 5, below the secondary water cooling 5, a horizontally movable condensation chamber 2 is arranged.
  • the condensation chamber 2 can be connected in a gastight manner to the steam line 14.
  • the liquefied high-purity manganese collects and is maintained at a temperature of 1350 to 1400 ° C in the liquid state.
  • the movable condensation chamber 2 is associated with a siphon-like tap hole 13.
  • the tap hole 13 the manganese is tapped and placed in a casting machine 8.
  • the casting machine 8 is chambered and is also under a protective gas atmosphere 7 (argon) and is equipped with appropriate device means for applying and maintaining the protective gas atmosphere.
  • the manganese is poured into a final product 11 in the appropriate desired formats.
  • the final product 11 has a purity of 99.9% manganese.
  • the protective gas atmosphere is drawn off via a connection 20 by means of a vacuum pump 3 and fed back into the supply line 15.
  • the vaporized manganese still present in the protective gas is cooled down in a secondary condenser 12 and separated from the protective gas atmosphere.
  • the secondary capacitor 12 is for this purpose a vacuum pump with water cooling 6 available.
  • the inert gas purified by the manganese vapor is circulated in the supply line 15 and fed back into the induction evaporator via a feed 16 and a secondary filter 10. Via the feed 16, the circulation process returns lost protective gas to the cycle, so that a stable argon protective gas atmosphere is ensured at all times.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Description

Herstellung von hochwertigem Mangan aus Ferromangan mittels Verdampfung in einer Vakuuminduktionsanlage  Production of high quality manganese from ferromanganese by evaporation in a vacuum induction plant

Beschreibung description

Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung von technisch reinem Mangan durch Verdampfung von kohlenstoffhaltigem Ferromangan in einem Induktionsvakuumgefäß. The present invention relates to a process for the production of technically pure manganese by evaporation of carbonaceous ferromanganese in an induction vacuum vessel.

Mangan ist eins von den wichtigsten Legierungselementen bei der Stahlherstellung. Es zeichnet sich mit hoher Festigkeit und Dehnung aus. Die Erzeugung von Stahlsorten mit Mangan erfolgt durch Zugabe von manganhaltigen Legierungsmitteln während des Stahlherstellungsprozesses. Zu denen gehören Mn-Legierungen erzeugt in Hochöfen bzw. Reduktionsöfen mit hohem Kohlenstoffgehalt wie FeMnHC (HCFeMn) und Legierungen mit mittlerem FeMnMC (MCFeMn) und niedrigem Kohlestoffgehalt FeMnLC (LCFeMn). erzeugt in sekundärmetallurgischen Anlagen. Manganese is one of the most important alloying elements in steelmaking. It is characterized by high strength and elongation. The production of steel grades with manganese takes place by adding manganese-containing alloying agents during the steelmaking process. These include Mn alloys produced in blast furnaces or high carbon reduction furnaces such as FeMnHC (HCFeMn) and FeMnLC (LCFeMn) alloys with medium FeMnMC (MCFeMn) and low carbon content. produced in secondary metallurgical plants.

Die Mangan-Legierungen sind außer mit den genannten Kohlenstoffgehalten auch mit weiteren Elementen wie Phosphor und Schwefel belastet, so dass die Anwendung der Materialien nicht unbegrenzt in Einsatz kommen kann. Typische Zusammensetzung von Mangan-Legierungen in Gew. % sind: The manganese alloys are loaded in addition to the carbon contents mentioned also with other elements such as phosphorus and sulfur, so that the application of materials can not be used indefinitely. Typical composition of manganese alloys in% by weight are:

C Si P S Mn  C Si P S Mn

FeMnHC 7-8 1.5-4.5 0.2-0.4 0.03 65-82  FeMnHC 7-8 1.5-4.5 0.2-0.4 0.03 65-82

FeMnMC 1.0 1.5-2.5 0.2-0.4 0.02 75-85  FeMnMC 1.0 1.5-2.5 0.2-0.4 0.02 75-85

FeMnLC 0.2-0.7 1-2 0.1-0.3 0.02 78-92  FeMnLC 0.2-0.7 1-2 0.1-0.3 0.02 78-92

Es wird allerdings immer öfter nach technisch reinem Mangan gefragt, um dem ständig wachsenden Ansprüchen der hochqualitativen Stahlherstellung nachzugehen. Derzeit wird technisch reines Mangan nur auf elektrolytischer Weise hergestellt, da reines Mangan technisch nicht durch die Reduktion mit Kohlenstoff gewonnen werden kann, da sich hierbei neben Mangan auch stabile Carbide, insbesondere Mn7C3, bilden. However, there is an increasing demand for technically pure manganese in order to meet the constantly growing demands of high-quality steel production. At present, technically pure manganese is only produced in an electrolytic manner, since pure manganese can not be obtained technically by reduction with carbon, since in addition to manganese there are also stable carbides, in particular Mn 7 C 3 .

Hierzu wird eine möglichst reine Mangansulfat-Lösung verwendet, die mit Edelstahl-Elektroden bei 5 -7 V elektrolysiert wird. An der Kathode entsteht dabei reines Mangan, an der Anode Sauerstoff, der mit Manganionen weiter zu Braunstein reagiert. For this purpose, a pure manganese sulfate solution is used, which is electrolysed with stainless steel electrodes at 5 -7 V. Pure manganese is produced at the cathode and oxygen at the anode, which reacts with manganese ions to form brownstone.

2MnS04 + 2 H20 -» 2Mn + 2 H2S04 + 02 2MnS0 4 + 2 H 2 0 - »2Mn + 2 H 2 S0 4 + 0 2

Daneben sind auch die Gewinnung von Mangan durch die Reduktion von Manganoxiden mit Aluminium (Aluminothermie) oder Silicium bekannt. In addition, the extraction of manganese by the reduction of manganese oxides with aluminum (aluminothermy) or silicon are known.

Eine weitere Möglichkeit der Mangangewinnung besteht darin, die oben genannten Manganverbindungen soweit zu erhitzen, so dass das Mangan verdampf. Another way of Mangangewinnung is to heat the above manganese compounds so far, so that the manganese evaporates.

Allerdings entsteht reines Mangan erst bei Temperaturen über 1600° C, da erst bei dieser Temperatur ein Teil des Mangans zu verdampfen beginnt, so dass dieser Herstellungsweg bisher nicht wirtschaftlich anwendbar war. However, pure manganese is formed only at temperatures above 1600 ° C, since only at this temperature, a portion of the manganese begins to evaporate, so that this production route has not been economically applicable.

Eine Aufgabe der vorliegen Erfindung ist es, ein Verfahren zur kontinuierlichen Mangan-Herstellung durch Verdampfung der Ausgang roh Stoffe zur Verfügung zu stellen, die kostengünstig und damit wirtschaftlich ist. An object of the present invention is to provide a process for continuous manganese production by evaporation of the raw raw materials available, which is inexpensive and therefore economical.

Diese Aufgabe wird durch die im Anspruch 1 angegebenen Merkmale gelöst, insbesondere dadurch, dass das Verfahren unter Vakuum und Temperaturen oberhalb der Liquidus-Temperatur des Mangans ausgeführt wird, wobei eine Pfanne mit flüssigem kohlenstoffhaltigem Ferromangan in einen Induktionsverdampfer eingesetzt wird, das Metall unter Vakuum, erzeugt und durch ein Vakuumpumpen- und Filtersystem im Bereich von 10-900 mbar und einer Temperatur im Bereich von > 1248°C rührend mit einem Inertgas verdampft und im weiteren Verlauf der Anlage mit Wasser gekühlt wird, wobei die Mn-Dämpfe in einer mobilen Kondensationskammer bei Temperaturen im Bereich 1350-1400°C verflüssigt und durch ein siphonartiges beheiztes Abstichloch kontinuierlich in eine Vergießmaschine abgestochen werden. This object is achieved by the features specified in claim 1, in particular, by carrying out the process under vacuum and temperatures above the liquidus temperature of the manganese using a ladle of liquid carbonaceous ferromanganese in an induction evaporator producing metal under vacuum and by a vacuum pumping and filtering system in the range of 10 -900 mbar and a temperature in the range of> 1248 ° C is vigorously evaporated with an inert gas and cooled in the further course of the plant with water, the Mn vapors liquefied in a mobile condensation chamber at temperatures in the range 1350-1400 ° C and by a siphon-type heated taphole are continuously tapped into a caster.

Die in der Erfindung präsentierte Anlage und das Verfahren stellt eine innovative Technik nicht nur im Sinne der kontinuierlichen Mangan-Herstellung aber auch ihres Vergießens dar. The plant presented in the invention and the process represents an innovative technique not only in terms of continuous manganese production but also their potting.

Im Folgenden sollen die metallurgischen Eigenschaften des Mangans beschrieben werden. In the following, the metallurgical properties of manganese are described.

Das Zweikomponentensystem Mn-Fe, stellt verschiedene Wandlungsphasen der Lösung Mangan-Eisen dar. Wie dem untenstehenden Diagramm zu entnehmen ist, liegt die Liquidustemperatur des reinen Mangans bei 1246°C. The two-component system Mn-Fe represents various phases of the manganese-iron solution. As shown in the diagram below, the liquidus temperature of pure manganese is 1246 ° C.

Phasengleichgewichtsystem Mn-Fe  Phase equilibrium system Mn-Fe

Beim Mangangehalt von 65-92%, typischem Gehalt der Ferrolegierungen, liegt die Liquidustemperatur im Bereich 1246-1280°C. Sie definiert die niedrigste Temperatur bei der das Flüssigmaterial zu verdampfen beginnt. Der Dampfdruck in Abhängigkeit der Temperatur hat einen exponentiell wachsenden Verlauf. At the manganese content of 65-92%, typical content of the ferroalloys, the liquidus temperature is in the range 1246-1280 ° C. It defines the lowest temperature at which the liquid material starts to evaporate. The vapor pressure as a function of the temperature has an exponentially increasing course.

Mn-Dampfdruck Um die physikalischen Bedingungen des erfindungsgemäßen Verfahrens zu veranschaulichen, wird nachstehend die Verdampfungskinetik des Mangans beschrieben. Mn-vapor pressure In order to illustrate the physical conditions of the process according to the invention, the evaporation kinetics of manganese will be described below.

Die Verdampfungskinetik des Mangans ist eine Funktion des Druckes, der Temperatur und der Inertgasrate. Der Verdampfungsprozess selbst erfolgt durch Phasenumwandlung - Flüssigkeit / Gas (Dampf) bei gegebener Temperatur und dem Druck nach dem Gesetz der ersten Ordnung, wie in Gleichung (1 ) darstellt ist, dMn The evaporation kinetics of manganese is a function of pressure, temperature and inert gas rate. The evaporation process itself is carried out by phase transformation - liquid / gas (steam) at a given temperature and pressure according to the law of the first order, as represented in equation (1), dMn

-[[Mn] - [ «*]) - [[Mn] - [« * ])

dt (1 ) worin  dt (1) where

(-dMn/dt) : Verdampfungsrate in % / min (-dMn / dt): evaporation rate in% / min

1 : Phasenumwandlungskonstante in Minuten 1 : Phase conversion constant in minutes

[Mn]: aktuelle Mangan-Konzentration [Mn]: current manganese concentration

[Mn*]:Mn-Gleichgewichtskonzentration bei aktuellem Prozesszustand (p,T, Inertgas) ist. [Mn *]: Mn equilibrium concentration at current process state (p, T, inert gas).

Bei einem Phasengleichgewicht (Flüssigkeit - Gas) At a phase equilibrium (liquid - gas)

[Mn*] = {Mn*} (2) ausgedrückt durch eine temperaturabhängige Konstante K(T) den Verdampfungsdruck pMn als auch durch den Aktivitätskoeefizient fMn als Funktion der Metallzusammensetzung wird das Mangangleichgewicht [Mn*] folgend dargestellt: worin [Mn * ] = {Mn * } (2) expressed by a temperature-dependent constant K (T) the vaporization pressure pMn as well as the activity coefficient fMn as a function of the metal composition, the manganese balance [Mn *] is represented as follows: wherein

(5) (5)

Dabei gilt It applies

1. NMn: Mn - Volumenstrom im Vakuumgefäß in Nm3/min, direkt proportional zur Verdampfungsrate ausgedrückt durch k(-dMn/dt), 1. NMn: Mn - volume flow in a vacuum vessel in Nm3 / min, directly proportional to the evaporation rate expressed by k (-dMn / dt),

2. uAr: eingeblasener Ar-Volumenstrom in das Vakuumgefäß in Nm3/min, 2. uAr: blown Ar volumetric flow into the vacuum vessel in Nm3 / min,

3. p: Druck innerhalb des Verdampfungsgefässes 3. p: pressure inside the evaporation vessel

Gleichungen (4) und (5) in Verbindung mit der Gleichung (1 ) ergeben den folgenden Zusammenhang: Equations (4) and (5) in conjunction with equation (1) give the following relation:

Die Gleichung (6) gibt das Steuerprinzip angelehnt an die folgenden Größen wieder: Equation (6) represents the control principle based on the following quantities:

- Metalltemperatur T, geregelt im Temperaturbereich größer als 1246°C mit einer induktiven Heizung - Metal temperature T, regulated in the temperature range greater than 1246 ° C with an inductive heating

- Gefäßdruck p, geregelt im Bereich 10 bis 900 mbar mittels eines Vakuumpumpensystems - Vessel pressure p, regulated in the range 10 to 900 mbar by means of a vacuum pump system

- Ar-Inertgasdurchflussrate uAr, geregelt im Bereich 0.05 bis 0.5 Nm3 / (tMetall min) mittels eines Einblassystems. - Ar-Inertgasdurchflußrate uAr, regulated in the range 0.05 to 0.5 Nm3 / (tMetall min) by means of an injection system.

Hieraus ergeben sich alle relevanten Parameter zur Durchführung des erfindungsgemäßen Verfahrens mit der erfindungsgemäßen Vorrichtung. Das Verfahren sieht vor, dass die Verflüssigung der Mn-Dämpfe kontinuierlich mittels des sekundären Kühlers, der im Dampfstrom innerhalb einer Dampfleitung angeordnet und zwecks der Verbesserung des Tropfenabflusses in konischer Form ausgebildet ist, erfolgt. This results in all relevant parameters for carrying out the method according to the invention with the device according to the invention. The method provides that the liquefaction of the Mn vapors takes place continuously by means of the secondary cooler, which is arranged in the vapor stream within a vapor line and is formed in a conical shape for the purpose of improving the drop outflow.

Das Vakuumpumpensystem ist zusätzlich mit einem sekundären Wasserkühlsystem, einem Kondensator und einem Filter ausgestattet. Der Verdampfungs- prozess wird dabei zusätzlich mit Argon als Inertgas unterstützt und bildet quasi eine Schutzgasatmosphäre aus. The vacuum pump system is additionally equipped with a secondary water cooling system, a condenser and a filter. The evaporation process is additionally supported with argon as the inert gas and forms a kind of protective gas atmosphere.

Das technisch reine Mangan wird kontinuierlich mit Wasser gekühlt, abgestochen und unter der Argonschutzgasatmosphäre in eine Gießmaschine aufgegeben, wo es in entsprechend gewünschte Formate gegossen werden kann. The technically pure manganese is continuously cooled with water, tapped and placed under the Argon protective gas atmosphere in a casting machine, where it can be poured into the desired formats.

Während des Prozesses ist es vorgesehen, die Verdampfungsrate, Temperatur, Vakuumdruck und Inertgasdurchflussrate zu steuern. Das zu verdampfende Verdampfungsmaterial kann aus verschiedenen Mn-Konzentrationen bestehen, die dann wiederum die Verdampfungsrate, Temperatur und Inertgasdurchflussrate beeinflussen können. During the process, it is intended to control the rate of evaporation, temperature, vacuum pressure and inert gas flow rate. The evaporation material to be evaporated may consist of various Mn concentrations, which in turn may then influence the rate of evaporation, temperature and inert gas flow rate.

Auch soll es möglich sein, dass das Verdampfungsmaterial kontinuierlich oder diskontinuierlich in den Induktionsverdampfer chargiert wird. It should also be possible that the evaporation material is charged continuously or discontinuously in the induction evaporator.

Eine weitere Aufgabe der vorliegenden Erfindung ist es, eine Vorrichtung zur Durchführung des erfindungsgemäßen Verfahrens zur Verfügung zu stellen. Another object of the present invention is to provide an apparatus for carrying out the method according to the invention.

Diese weitere Aufgabe wird durch eine Vorrichtung gemäß der im Anspruch 9 angegebenen Merkmale gelöst, insbesondere dadurch einen Verdampfer in dem die Manganlegierung eingesetzt wird, das Metall unter Vakuum, erzeugt und durch ein Vakuumpumpen- und Filtersystem im Bereich von 10-900 mbar und einer Temperatur im Bereich von > 1248°C rührend mit Argon als Schutzgas verdampfbar ist und über eine primäre Wasserkühlung und über eine sekundäre Wasserkühlung gekühlt wird, wobei die Mn-Dämpfe in einer mobilen Kondensationskammer bei Temperaturen im Bereich 1350-1400°C im flüssigen Aggregatzustand gesammelt werden und durch ein siphonartiges beheiztes Abstichloch kontinuierlich in eine Vergießmaschine abstechbar ist. In einer weiteren Ausführungsform ist der Verdampfer ein Induktionsverdampfer, der auf einer Hydraulikplattform angeordnet und über diese vertikal verfahrbar ausgebildet ist. This further object is achieved by a device according to the features specified in claim 9, in particular by an evaporator in which the manganese alloy is used, the metal under vacuum, and generated by a vacuum pump and filter system in the range of 10-900 mbar and a temperature In the range of> 1248 ° C stirring with argon is inert as a protective gas and is cooled by a primary water cooling and a secondary water cooling, the Mn vapors are collected in a mobile condensation chamber at temperatures in the range 1350-1400 ° C in the liquid state and is continuously abstechbar by a siphon-like heated tap hole in a Vergießschieb. In a further embodiment, the evaporator is an induction evaporator, which is arranged on a hydraulic platform and designed to be vertically movable over it.

Gemäß einer vorteilhaften Ausführungsform der erfindungsgemäßen Vorrichtung ist die mobile Kondensationskammer horizontal verfahrbar ausgebildet. According to an advantageous embodiment of the device according to the invention, the mobile condensation chamber is designed to be horizontally movable.

In einer weiteren Ausführungsform sind der Induktionsverdampfer und die Kondensationskammer über eine, mit der primären Wasserkühlung und der sekundären Wasserkühlung wirkverbundenen Dampfleitung gasdicht miteinander verbunden. In a further embodiment, the induction evaporator and the condensation chamber are gas-tightly connected to one another via a steam line operatively connected to the primary water cooling and the secondary water cooling.

In einer besonders vorteilhaften Ausführungsform der erfindungemäßen Vorrichtung ist die sekundäre Wasserkühlung innerhalb der Dampfleitung im Dampfstrom über der Kondensationskammer angeordnet. In a particularly advantageous embodiment of the device according to the invention, the secondary water cooling within the steam line is arranged in the vapor stream above the condensation chamber.

Es ist vorgesehen, dass die Dampfleitung mit einer Zuleitung für das Schutzgas (Inertgas) verbunden ist und das Schutzgas (Inertgas) in der Dampfleitung und der Zuleitung im Kreislauf geführt wird, wobei dampfförmiges Mangan durch einen, der Zuleitung zugeordneten, sekundären Kondensator abgeschieden werden kann und das Schutzgas (Inertgas) über die Zuleitung den Induktionsverdampfer und damit dem Dampfstrom wieder zugeführt wird. Dabei ist es vorgesehen, dass auch zusätzliches Inertgas über die Einspeisung dem Kreislauf zugeführt werden kann, um die prozessbedingten Verluste ausgleichen zu können und so die Konzentration im Kreislaufsystem regulieren zu können. It is envisaged that the steam line is connected to a supply line for the protective gas (inert gas) and the protective gas (inert gas) is circulated in the steam line and the supply line, wherein manganese manganese can be separated by a secondary condenser assigned to the feed line and the protective gas (inert gas) via the feed line to the induction evaporator and thus the steam flow is fed back. It is envisaged that additional inert gas can be supplied via the feed to the circuit in order to compensate for the process-related losses and so to be able to regulate the concentration in the circulatory system.

Um die Konzentration an dem Schutzgas (Inertgas) im Kreislauf möglichst konstant zu halten, kann zusätzliches Schutzgas über eine Einspeisung in die Zuleitung eingeleitet werden, wo es über einen sekundären Filter wieder in den Induktionsverdampfer eingespült werden kann. In order to keep the concentration of the protective gas (inert gas) in the circulation as constant as possible, additional protective gas can be introduced via a feed into the supply line, where it can be flushed back into the induction evaporator via a secondary filter.

Die erfindungsgemäße Vorrichtung zur Durchführung des erfindungsgemäßen Verfahrens wird im Folgenden anhand einer beispielhaften Ausführungsform unter Bezugnahme auf die beigefügte Zeichnung näher erläutert. Die einzige Figur zeigt: The device according to the invention for carrying out the method according to the invention is explained in more detail below with reference to an exemplary embodiment with reference to the accompanying drawings. The only figure shows:

Fig. 1 eine schematische Ansicht der Vorrichtung zur Durchführung des Verfahrens als Prozessablaufmodell. Fig. 1 is a schematic view of the apparatus for performing the method as a process flow model.

Wie in der einzigen Figur dargestellt, besteht die Vorrichtung 18 im wesentlichen aus einem Induktionsverdampfer 1 , in dem das eingebrachte FeMn bei einer Temperatur von 1600 - 1700°C im flüssigen Aggregatzustand gehalten wird. Der Induktionsverdampfer 1 ist in dieser Ausführungsform auf einer Hydraulikplattform 9 angeordnet, die es erlaubt diesen zu heben und zu senken. As shown in the single figure, the device 18 consists essentially of an induction evaporator 1, in which the FeMn introduced is kept at a temperature of 1600 - 1700 ° C in the liquid state. The induction evaporator 1 is arranged in this embodiment on a hydraulic platform 9, which allows it to raise and lower.

Im Bodenbereich des Induktionsverdampfers 1 ist mindestens ein Spülrohran- schluss 19 vorgesehen, der mit einer Zuleitung 15 verbunden ist und über die ein Schutzgas, in diesem Fall Argon, in den Induktionsverdampfer 1 eingeleitet wird. Das Schutzgas steigt durch die FeMn - Schmelze nach oben, wo es sich mit dem verdampften Anteil des Mangans bei einem Druck von 100 bis 200 mbar in einer Dampfleitung 14 sammelt und in einem Dampfstrom 17, hier als Pfeile dargestellt, abgeführt wird. Die Dampfleitung 14 ist dabei gasdicht mit dem Induktionsverdampfer 1 verbunden. In the bottom region of the induction evaporator 1, at least one flushing pipe connection 19 is provided, which is connected to a supply line 15 and via which a protective gas, in this case argon, is introduced into the induction evaporator 1. The protective gas rises through the FeMn melt, where it collects with the vaporized portion of manganese at a pressure of 100 to 200 mbar in a vapor line 14 and is discharged in a vapor stream 17, shown here as arrows. The steam line 14 is connected in a gas-tight manner to the induction evaporator 1.

Der sich in der Dampfleitung 14 befindliche Dampfstrom 17 wird an einer primären Wasserkühlung 4, die die Dampfleitung von außen ummantelt, vorbeigeleitet und dabei heruntergekühlt. In einer sekundären Wasserkühlung 5 wird der Dampfstrom 17 soweit heruntergekühlt, das ein Aggregatzustandwechsel des Mangans von gasförmig nach flüssig eintritt. Um dies so effizient und schnell wie möglich ausführen zu können, ist dabei vorgesehen, die sekundäre Wasserkühlung 5 innerhalb der Dampfleitung 14 und im Dampfstrom 17 anzuordnen. The steam flow 17 located in the steam line 14 is conducted past a primary water cooling 4, which surrounds the steam line from the outside, and is cooled down at the same time. In a secondary water cooling 5, the steam flow 17 is cooled down to the extent that an aggregate state change of the manganese from gaseous to liquid occurs. In order to do this as efficiently and quickly as possible, it is provided to arrange the secondary water cooling 5 within the steam line 14 and in the steam flow 17.

Die sekundäre Wasserkühlung 5 ist dabei konisch ausgebildet und liegt mit der sich verjüngenden Seite in Richtung des ankommenden Dampfstromes 17. In der Figur ist dies als ein gleichschenkliges Dreieck dargestellt. The secondary water cooling 5 is conical and lies with the tapered side in the direction of the incoming vapor stream 17. In the figure, this is shown as an isosceles triangle.

Unterhalb der sekundären Wasserkühlung 5 ist eine horizontal verfahrbare Kondensationskammer 2 angeordnet. Auch die Kondensationskammer 2 kann gasdicht mit der Dampfleitung 14 verbunden werden. In der horizontal verfahrbar ausgebildeten Kondensationskammer 2 sammelt sich das verflüssigte hochreine Mangan und wird bei einer Temperatur von 1350 bis 1400°C im flüssigen Aggregatzustand gehalten. Below the secondary water cooling 5, a horizontally movable condensation chamber 2 is arranged. The condensation chamber 2 can be connected in a gastight manner to the steam line 14. In the horizontally movable formed condensation chamber 2, the liquefied high-purity manganese collects and is maintained at a temperature of 1350 to 1400 ° C in the liquid state.

Der verfahrbaren Kondensationskammer 2 ist ein siphonartiges Abstichloch 13 zugeordnet. Über das Abstichloch 13 wird das Mangan abgestochen und in eine Gießmaschine 8 aufgegeben. Die Gießmaschine 8 ist gekammert ausgebildet und steht auch unter einer Schutzgasatmosphäre 7 (Argon) und ist mit entsprechenden Vorrichtungsmitteln zur Beaufschlagung und Aufrechterhaltung der Schutzgasatmosphäre ausgerüstet. In der Gießmaschine wird das Mangan zu einem Endprodukt 11 in die entsprechend gewünschten Formate vergossen. Das Endprodukt 11 hat einen Reinheitsgrad von 99,9 % Mangan. The movable condensation chamber 2 is associated with a siphon-like tap hole 13. About the tap hole 13, the manganese is tapped and placed in a casting machine 8. The casting machine 8 is chambered and is also under a protective gas atmosphere 7 (argon) and is equipped with appropriate device means for applying and maintaining the protective gas atmosphere. In the casting machine, the manganese is poured into a final product 11 in the appropriate desired formats. The final product 11 has a purity of 99.9% manganese.

Während die manganhaltigen Dämpfe im Dampfstrom 17 an der sekundären Wasserkühlung 5 kondensieren, wird über einen Anschluss 20 die Schutzgasatmosphäre mittels einer Vakuumpumpe 3 abgesaugt und wieder in die Zuleitung 15 eingespeist. Das in dem Schutzgas noch befindliche verdampfte Mangan wird in einem sekundären Kondensator 12 heruntergekühlt und von der Schutzgasatmosphäre abgeschieden. Dem sekundären Kondensator 12 steht hierfür eine Vakuumpumpe mit Wasserkühlung 6 zur Verfügung. While the manganese-containing vapors in the vapor stream 17 condense on the secondary water cooling system 5, the protective gas atmosphere is drawn off via a connection 20 by means of a vacuum pump 3 and fed back into the supply line 15. The vaporized manganese still present in the protective gas is cooled down in a secondary condenser 12 and separated from the protective gas atmosphere. The secondary capacitor 12 is for this purpose a vacuum pump with water cooling 6 available.

Das vom Mangandampf gereinigte Schutzgas wird in der Zuleitung 15 im Kreislauf geführt und über eine Einspeisung 16 und ein sekundär Filter 10 wieder in den Induktionsverdampfer geleitet. Über die Einspeisung 16 wird dem Kreislauf durch den Prozessverlauf verlorengegangenes Schutzgas wieder zugeführt, so dass eine stabile Argon - Schutzgasatmosphäre mit jederzeit sichergestellt wird. Bezugszeichenliste The inert gas purified by the manganese vapor is circulated in the supply line 15 and fed back into the induction evaporator via a feed 16 and a secondary filter 10. Via the feed 16, the circulation process returns lost protective gas to the cycle, so that a stable argon protective gas atmosphere is ensured at all times. LIST OF REFERENCE NUMBERS

1. Induktionsverdampfer 1. Induction evaporator

2. Kondensationskammer  2nd condensation chamber

3. Vakuumpumpe  3. Vacuum pump

4. primäre Wasserkühlung  4. primary water cooling

5. sekundäre Wasserkühlung  5. secondary water cooling

6. Vakuumpumpe mit Wasserkühlsystem 6. Vacuum pump with water cooling system

7. Argonschutzatmosphäre 7. Argon protective atmosphere

8. Gießmaschine  8. Casting machine

9. Hydraulikplattform  9. Hydraulic platform

10. Sekundärfilter  10. Secondary filter

11. Endprodukt  11. end product

12. sekundär Kondensator  12. Secondary capacitor

13. Abstichloch  13th tap hole

14. Dampfleitung  14th steam line

15. Zuleitung  15. Supply line

16. Einspeisung  16. Feed

17. Dampfstrom  17. Steam flow

18. Vorrichtung  18. Device

19. Spülrohranschluss  19. rinse pipe connection

20. Anschluss  20. Connection

Claims

Patentansprüche claims 1. Verfahren zur Herstellung von technisch reinem Mangan durch Verdampfung von kohlenstoffhaltigem Ferromangan in einem Induktionsvakuumgefäß, dadurch gekennzeichnet, dass das Verfahren unter Vakuum und Temperaturen oberhalb der Liquidus-Temperatur des Mangans ausgeführt wird, wobei eine Pfanne mit flüssigem kohlenstoffhaltigem Ferromangan in einen Induktionsverdampfer (1 ) eingesetzt wird, das Metall unter Vakuum, erzeugt und durch ein Vakuumpumpen- (3) und Filtersystem (10) im Bereich von 10-900 mbar und einer Temperatur im Bereich von > 1248°C rührend mit einem Inertgas verdampft und im weiteren Verlauf der Anlage durch einen primären Kühler (4) mit Wasser gekühlt wird, wobei die Mn-Dämpfe in einer mobilen Kondensationskammer (2) bei Temperaturen im Bereich 1350-1400°C durch einen sekundären Kühler (5) verflüssigt und durch ein siphonartiges beheiztes Abstichloch kontinuierlich in eine Gießmaschine (8) abgestochen und zum Endprodukt (11 ) vergossen werden. 1. A process for the production of technically pure manganese by evaporation of carbonaceous ferromanganese in an induction vacuum vessel, characterized in that the process is carried out under vacuum and temperatures above the liquidus temperature of manganese, wherein a pan with liquid carbonaceous ferromanganese in an induction evaporator (1 ), the metal is generated under vacuum, and by a vacuum pump (3) and filter system (10) in the range of 10-900 mbar and a temperature in the range of> 1248 ° C with an inert inert gas and evaporated in the further course of Is cooled by a primary cooler (4) with water, wherein the Mn vapors in a mobile condensation chamber (2) at temperatures in the range 1350-1400 ° C by a secondary condenser (5) and liquefied by a siphon-like heated taphole continuously in a casting machine (8) tapped and cast to the final product (11). 2. Verfahren nach Anspruch 1 , dadurch gekennzeichnet, dass die Verflüssigung der Mn-Dämpfe kontinuierlich mittels des sekundären Kühlers (5), der im Dampfstrom (17) innerhalb einer Dampfleitung (14) angeordnet und zwecks der Verbesserung des Tropfenabflusses in konischer Form ausgebildet ist, erfolgt. 2. The method according to claim 1, characterized in that the liquefaction of the Mn vapors continuously by means of the secondary cooler (5) which is arranged in the vapor stream (17) within a vapor line (14) and formed for the purpose of improving the droplet drain in a conical shape , he follows. 3. Verfahren Nach Anspruch 1 , dadurch gekennzeichnet, dass das Vakuumpumpensystem zusätzlich mit einem sekundären Wasserkühlsystem (6), einem Kondensator (12) und einem Filter (13) ausgestattet wird. 3. The method according to claim 1, characterized in that the vacuum pump system is additionally equipped with a secondary water cooling system (6), a condenser (12) and a filter (13). 4. Verfahren nach Anspruch 1 , dadurch gekennzeichnet, dass der Ver- dampfungsprozess zusätzlich mit Argon als Inertgas unterstützt wird. 4. The method according to claim 1, characterized in that the evaporation process is additionally supported with argon as an inert gas. 5. Verfahren nach Anspruch 1 , dadurch gekennzeichnet, dass das technische reine Mangan kontinuierlich mit Wasser gekühlt, abgestochen und unter einer Argonschutzgasatmosphäre in eine Gießmaschine (8) aufgegeben wird. 5. The method according to claim 1, characterized in that the technical pure manganese is continuously cooled with water, tapped and placed under an argon protective gas atmosphere in a casting machine (8). 6. Verfahren nach Anspruch 1 , dadurch gekennzeichnet, dass die Verdampfungsrate von Temperatur, Vakuumdruck und Inertgasdurchflussrate gesteuert wird. 6. The method according to claim 1, characterized in that the evaporation rate of temperature, vacuum pressure and inert gas flow rate is controlled. 7. Verfahren nach Anspruch 1 , dadurch gekennzeichnet, dass das Verdampfungsmaterial aus verschiedenen Mn-Konzentrationen besteht. 7. The method according to claim 1, characterized in that the evaporation material consists of different Mn concentrations. 8. Verfahren nach Anspruch 7, dadurch gekennzeichnet, dass das Verdampfungsmaterial kontinuierlich oder diskontinuierlich in den Induktionsverdampfer (1 ) chargiert wird. 8. The method according to claim 7, characterized in that the evaporation material is charged continuously or discontinuously in the induction evaporator (1). 9. Vorrichtung zum Durchführen des Verfahrens gemäß den Ansprüchen 1 bis 8, gekennzeichnet durch einen Verdampfer (1 ) in dem die Manganlegierung eingesetzt wird, das Metall unter Vakuum, erzeugt und durch ein Vakuumpumpen- (3) und Filtersystem (13) im Bereich von 10-900 mbar und einer Temperatur im Bereich von > 1248°C rührend mit Argon als Schutzgas verdampfbar ist und über eine primäre Wasserkühlung (4) und über eine sekundäre Wasserkühlung (5) gekühlt wird, wobei die Mn-Dämpfe in einer mobilen Kondensationskammer (2) bei Temperaturen im Bereich 1350-1400°C im flüssigen Aggregatzustand gesammelt werden und durch ein siphonartiges beheiztes Abstichloch (13) kontinuierlich in eine Vergießmaschine (8) abstechbar ist. 9. Apparatus for carrying out the method according to claims 1 to 8, characterized by an evaporator (1) in which the manganese alloy is used, the metal under vacuum, generated and by a vacuum pump (3) and filter system (13) in the range of 10-900 mbar and a temperature in the range of> 1248 ° C is stirred with argon as a protective gas and is cooled by a primary water cooling (4) and a secondary water cooling (5), wherein the Mn vapors in a mobile condensation chamber ( 2) are collected in the liquid state at temperatures in the range 1350-1400 ° C and continuously by a siphon-like heated taphole (13) in a Vergießmaschine (8) is abstechbar. 10. Vorrichtung nach Anspruch 9, dadurch gekennzeichnet, dass der Ver- dampfer (1 ) ein Induktionsverdampfer ist, der auf einer Hydraulikplattform (9) angeordnet ist und über diese vertikal verfahrbar ausgebildet ist. 10. Apparatus according to claim 9, characterized in that the steamer (1) is an induction evaporator, which is arranged on a hydraulic platform (9) and is designed to be vertically movable over this. 11. Vorrichtung gemäß Anspruch 9, dadurch gekennzeichnet, dass die mobile Kondensationskammer (2) horizontal verfahrbar ausgebildet ist. 11. The device according to claim 9, characterized in that the mobile condensation chamber (2) is designed to be horizontally movable. 12. Vorrichtung gemäß Anspruch 10 und 11 , dadurch gekennzeichnet, dass der Induktionsverdampfer (1 ) und die Kondensationskammer (2) miteinander über eine, mit der primären Wasserkühlung (4) und der sekundären Wasserkühlung (5) wirkverbundenen Dampfleitung (14), gasdicht verbunden sind. 12. The apparatus according to claim 10 and 11, characterized in that the induction evaporator (1) and the condensation chamber (2) connected to each other via a, with the primary water cooling (4) and the secondary water cooling (5) operatively connected to the steam line (14), gas-tight are. 13. Vorrichtung gemäß Anspruch 12, dadurch gekennzeichnet, dass die sekundäre Wasserkühlung (5) innerhalb der Dampfleitung (14) im Dampfstrom (17) über der Kondensationskammer (2) angeordnet ist. 13. The apparatus according to claim 12, characterized in that the secondary water cooling (5) within the vapor line (14) in the vapor stream (17) above the condensation chamber (2) is arranged. 14. Vorrichtung gemäß Anspruch 13, dadurch gekennzeichnet, dass die14. The apparatus according to claim 13, characterized in that the Dampfleitung (14) mit einer Zuleitung (15) für das Schutzgas verbunden ist, und das Schutzgas in der Dampfleitung (14) und der Zuleitung (15) im Kreislauf geführt wird, wobei dampfförmiges Mangan durch einen, der Zuleitung (15) zugeordneten, sekundär Kondensator (12) abscheidbar ist und das Schutzgas über die Zuleitung (15) den Induktionsverdampfer (1 ) dem Kreislauf wieder zugeführt wird. Steam line (14) is connected to a supply line (15) for the protective gas, and the protective gas in the steam line (14) and the supply line (15) is circulated, wherein manganese manganese by a, the supply line (15) associated, secondary Capacitor (12) can be deposited and the protective gas via the feed line (15) the induction evaporator (1) is supplied to the circuit again. 15. Vorrichtung gemäß Anspruch 14, dadurch gekennzeichnet, dass das15. The apparatus according to claim 14, characterized in that the Schutzgas aus der Kondensationskammer (2) über eine Einspeisung (16) erneut in die Zuleitung (15) einleitbar ist und über einen sekundären Filter (10) in den Induktionsverdampfer (1) einspülbar und zusätzliches Schutzgas ebenfalls über die Einspeisung (16) dem Dampfstrom (17) zuleitbar ist. Inert gas from the condensation chamber (2) via a feed (16) again in the supply line (15) can be introduced and via a secondary filter (10) in the induction evaporator (1) einspülbar and additional inert gas also via the feed (16) the steam flow ( 17) is zulleitbar.
EP14789775.5A 2013-09-25 2014-08-14 Production of high-grade manganese from ferromanganese by means of vaporization in a vacuum induction plant Active EP3049543B1 (en)

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