WO2006128556A2 - Feuerfestes keramisches produkt - Google Patents

Feuerfestes keramisches produkt Download PDF

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Publication number
WO2006128556A2
WO2006128556A2 PCT/EP2006/004357 EP2006004357W WO2006128556A2 WO 2006128556 A2 WO2006128556 A2 WO 2006128556A2 EP 2006004357 W EP2006004357 W EP 2006004357W WO 2006128556 A2 WO2006128556 A2 WO 2006128556A2
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WO
WIPO (PCT)
Prior art keywords
component
corrosion
product according
compounds
mass
Prior art date
Application number
PCT/EP2006/004357
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English (en)
French (fr)
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WO2006128556A3 (de
Inventor
Robert Treimer
Original Assignee
Refractory Intellectual Property Gmbh & Co. Kg
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Refractory Intellectual Property Gmbh & Co. Kg filed Critical Refractory Intellectual Property Gmbh & Co. Kg
Priority to AU2006254476A priority Critical patent/AU2006254476A1/en
Priority to US11/915,276 priority patent/US20080274870A1/en
Priority to MX2007014894A priority patent/MX2007014894A/es
Priority to EA200702383A priority patent/EA011907B1/ru
Priority to BRPI0611487-3A priority patent/BRPI0611487A2/pt
Priority to CA002611029A priority patent/CA2611029A1/en
Priority to EP06753542A priority patent/EP1888484A2/de
Publication of WO2006128556A2 publication Critical patent/WO2006128556A2/de
Publication of WO2006128556A3 publication Critical patent/WO2006128556A3/de

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    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts

Definitions

  • the invention relates to a refractory ceramic product, in particular a refractory ceramic molded body.
  • Refractory ceramic products both masses and moldings, are used for lining metallurgical melting vessels as well as for use as functional parts, especially in the context of secondary metallurgical processes.
  • the refractory material comes into contact not only with the metallurgical melts but also with corresponding slags. As far as the refractory material is subject to a significant chemical / metallurgical corrosion attack.
  • corrosion inhibitors are known, which are admixtures that are mixed with the offset, with the aid of which the corrosion of the finished product is to be reduced.
  • the invention is so far the object of demonstrating a way to improve the corrosion behavior of refractory ceramic products in the high temperature application (> 1,200 ° C, in particular> 1,500 ° C), without releasing simultaneously environmentally hazardous substances in the application.
  • Extensive testing has found that there are other groups of elements or compounds, as an alternative to chromium oxide, that are non-toxic and drastically reduce the corrosion tendency of an associated fired finished product without adversely affecting the mechanical performance of the products and without adverse effects on the temperature resistance and thermal shock resistance.
  • These include compounds of the transition metals with one another, such as yttrium tungstate, tungstite (Fe, Mn) WO 4 or columbite [(Fe, Mn) (Nb, Ta) 2 ] O 6 .
  • These also include those non-oxidic compounds of transition metals not already included in the above group, such as molybdenum disilicide (MoSi 2 ), Mo 5 Si 3 and FeMo.
  • the said corrosion-inhibiting substances form during firing (see below for selecting a raw material offset) or are added to the finished product, for example by means of infiltration by means of vacuum treatment. They advantageously deposit in the gussets (voids) between the grains of the refractory material (the refractory base component) and contribute to the reduction of corrosive slag attack (especially in the mentioned acid slags). In the binding of hydration-sensitive Ca with a transition metal at the same time the tendency to hydration is lowered. This also applies to non-saturated products.
  • the invention comprises a refractory ceramic product which
  • One or more of the group members bl to b5 can be excluded.
  • the raw material offset must be adjusted accordingly, provided that the corrosion-inhibiting components are not first introduced by impregnation of the finished fired product.
  • the offset thus contains appropriate additives.
  • This group of additives includes, for example, metallic molybdenum, molybdenum compounds, metallic tungsten and tungsten compounds.
  • molybdenum and tungsten are similar to chromium, but both are non-toxic. Both are easily alloyed with other metals such as aluminum, lead, iron, nickel, manganese or chromium. Besides these alloys, other molybdenum and tungsten compounds are suitable for use as additives, for example MoSi 2 , Mo 5 Si 3 , FeMo, WO 3 , WSi 2 or niobium and tantalum compounds.
  • the invention includes ceramic bonded refractory products as well as chemically bonded products.
  • the refractory ceramic products may be monolithic compositions, mortars or the like.
  • the invention relates to the production of refractory ceramic molded parts, for example in the form of stones, plates, sleeves or the like.
  • a suitable base component can at least partially also be a nonbasic basic component, for example from the group: alumina, corundum, ZrO 2 , zirconium silicate (ZrO 2 .SiO 2 ), mullite, TiO 2 .
  • An appropriate offset can be prepared in a conventional manner, for example by mixing the refractory base component with a binder, then shaping (for example by pressing) and fire for sintering, especially at temperatures> 1,200 ° C, but also at temperatures> 1,500 ° C.
  • the corrosion-inhibiting additive is best introduced as a finely ground powder (d 50 ⁇ l SO ⁇ m, in particular ⁇ 100 microns).
  • the additives can be used as primary raw materials. But it is also possible to use recycled materials.
  • Molybdenum-containing additives of the type mentioned can be provided, for example, from spent heating elements by appropriate grinding. Such heating elements consist for example of molybdenum disilicide (MoSi 2 ), sometimes in combination with tungsten compounds.
  • MoSi 2 molybdenum disilicide
  • an inexpensive waste product is available as a raw material for the use according to the invention.
  • the aforementioned corrosion-inhibiting compounds such as calcium molybdate or tungstate are formed during the firing of the products, for example, calcium being advantageously bound.
  • the hydration susceptibility of the finished product decreases.
  • the invention will be explained in more detail below with reference to various embodiments.
  • a dynamic slag test (drip slag test) according to ASTM standard C 768 for bricks from the non-ferrous metal industry was carried out on various refractory materials.
  • the slag had the following composition [in M%] (determination after oxidizing calcination):
  • Example 1 100% by mass sintered magnesia ( ⁇ 6 mm)
  • Example 2 93% by mass sintered magnesia ( ⁇ 6 mm), 7% by mass finely divided
  • Example 3 100% by mass of magnesia chromite
  • Example 4 99.7% by mass of magnesia chromite, 0.3% by mass of FeMo ( ⁇ 100 ⁇ m) The aforementioned slag test yielded the following wear volumes:

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
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Abstract

Die Erfindung betrifft ein feuerfestes keramisches Produkt, das: a) ≥ 93 Masse-% mindestens einer refraktären Grundkomponente und b) ≤ 7 Masse-% mindestens einer korrosionshemmenden Komponente aus der Gruppe: bl) Übergangsmetalle, b2) Verbindungen von Übergangsmetallen untereinander, b3) nicht oxidische Verbindungen von Übergangsmetallen, b4) oxidische Verbindungen von Übergangsmetallen, b5) Verbindungen der Übergangsmetalle mit Ca, Ba, Sr enthält.

Description

Feuerfestes keramisches Produkt
B e s c h r e i b u n g
Die Erfindung betrifft ein feuerfestes keramisches Produkt, insbesondere einen feuerfesten keramischen Formkörper.
Feuerfeste keramische Produkte, und zwar sowohl Massen als auch Formteile, finden zur Auskleidung metallurgischer Schmelzgefäße ebenso Anwendung wie zur Verwendung als Funktionalteile, insbesondere im Rahmen sekundärmetallurgischer Verfahren.
Dies gilt sowohl für Anwendungen in der Eisenmetali-Industrie wie für Anwendungen in der Nichteisenmetall-Industrie. Das feuerfeste Material kommt nicht nur mit den metallurgischen Schmelzen, sondern auch mit korrespondierenden Schlacken in Berührung. Insoweit unterliegt das Feuerfestmaterial einem erheblichen chemischen/metallurgischen Korrosionsangriff.
Unter den bekannten basischen und nicht-basischen Werkstoffsorten zeigen bisher MgCr-Produkte mit Cr2O3 als schützendem Oxid den besten Korrosionsschutz gegenüber einem Angriff von insbesondere sauren, eisensilikatischen - und/oder kupferhältigen Schlacken. Diese Werkstoffsorten haben jedoch aufgrund der Anwesenheit von Chromoxid den Nachteil, dass es zur Freisetzung von toxischem Cr6+ kommen kann.
Es hat deshalb nicht an Versuchen gefehlt, die Korrosionsbeständigkeit feuerfester keramischer Produkte auf anderem Wege zu verbessern.
In diesem Zusammenhang ist die Verwendung so genannter „Korrosionsinhibitoren" bekannt. Es handelt sich hierbei um Zusatzmittel, die dem Versatz zugemischt werden, mit deren Hilfe die Korrosion des fertigen Produktes herabgesetzt werden soll.
Der Erfindung liegt insofern die Aufgabe zugrunde, eine Möglichkeit aufzuzeigen, das Korrosionsverhalten feuerfester keramischer Produkte im Hochtemperatur- Anwendungsbereich (> 1.200° Celsius, insbesondere > 1.500° Celsius) zu verbessern, und zwar ohne gleichzeitig umweltgefährdende Substanzen bei der Anwendung freizusetzen. In umfangreichen Versuchen wurde festgestellt, dass es andere Gruppen von Elementen beziehungsweise Verbindungen als Alternative zum Chromoxid gibt, die nicht toxisch sind und die Korrosionsneigung eines zugehörigen gebrannten fertigen Produktes drastisch herabsetzen, und zwar ohne negative Auswirkungen auf das mechanische Verhalten der Produkte und ohne negative Auswirkungen auf die Temperaturbeständigkeit und Temperaturwechselbeständigkeit.
Diese Gruppen werden im weitesten Sinne definiert durch die Elemente der Übergangsmetalle (gemäß Definition IUPAC, Römpp „Chemielexikon" 9. Auflage, ISBN 3-13-735109-X, Seite 4787 ff.) und deren Verbindungen.
Dazu gehören Verbindungen der Übergangsmetalle untereinander wie Yttriumwolframat, Wolframit (Fe, Mn) WO4 oder Columbit [(Fe, Mn)(Nb, Ta)2]O6.
Dazu gehören ferner solche nicht oxidische Verbindungen von Übergangsmetallen, die nicht schon in der vorstehenden Gruppe erfasst sind, wie Molybdändisilicid (MoSi2), Mo5Si3 und FeMo.
Insbesondere wurden bei Verbindungen der Übergangsmetalle mit Erdalkalielementen korrosionshemmende Eigenschaften beobachtet.
Die genannten korrosionshemmenden Substanzen bilden sich beim Brand (siehe nachstehende Ausführungen zur Auswahl eines Rohstoffversatzes) oder werden dem fertigen Produkt zugesetzt, zum Beispiel mittels Vakuumbehandlung infiltriert. Sie lagern sich vorteilhaft in den Zwickeln (Hohlräumen) zwischen den Körnern des feuerfesten Materials (der refraktären Grundkomponente) an und tragen zur Verringerung des korrosiven Schlackenangriffs bei (insbesondere bei den genannten sauren Schlacken). Bei der Bindung von hydratationsempfindlichem Ca mit einem Übergangsmetall wird gleichzeitig die Hydratationsneigung herabgesetzt. Dies gilt auch für ungetränkte Produkte.
In ihrer allgemeinsten Ausführungsform umfasst die Erfindung ein feuerfestes keramisches Produkt, das
a) > 93 Masse-% mindestens einer refraktären Grundkomponente und b) < 7 Masse-% mindestens einer korrosionshemmenden Komponente aus der Gruppe: bl) Übergangsmetalle b2) Verbindungen von Übergangsmetallen untereinander b3) nicht oxidische Verbindungen von Übergangsmetallen b4) oxidische Verbindungen von Übergangsmetallen b5) Verbindungen der Übergangsmetalle mit Ca, Ba, Sr enthält.
Dabei können eine oder mehrere der Gruppenmitglieder bl bis b5 ausgeschlossen werden.
Verschiedene Weiterbildungen ergeben sich aus den Merkmalen der Unteransprüche und den sonstigen Beschreibungsunterlagen.
Der Rohstoffversatz ist entsprechend einzustellen, sofern die korrosionshemmenden Komponenten nicht erst durch Tränkung des fertigen gebrannten Produktes eingebracht werden. Der Versatz enthält also entsprechende Zusatzmittel. Zu dieser Gruppe von Zusatzmitteln gehören beispielsweise metallisches Molybdän, Molybdän-Verbindungen, metallisches Wolfram und Wolfram- Verbindungen.
Sowohl Molybdän als auch Wolfram weisen Ähnlichkeiten mit Chrom auf, sind jedoch beide nicht toxisch. Beide sind mit anderen Metallen, wie Aluminium, Blei, Eisen, Nickel, Mangan oder Chrom leicht legierbar. Neben diesen Legierungen sind andere Molybdän - und Wolframverbindungen für die Verwendung als Zusatzmittel geeignet, beispielsweise MoSi2, Mo5Si3, FeMo, WO3, WSi2 oder Niob- und Tantal-Verbindungen.
Ebenso ist es möglich, weitere Komponenten dem Versatz zuzumischen, beispielsweise ein Bindemittel oder Antioxidantien.
Die Erfindung schließt keramisch gebundene feuerfeste Produkte ebenso ein wie chemisch gebundene Produkte. Die feuerfesten keramischen Produkte können monolithische Massen, Mörtel oder dergleichen sein. Insbesondere bezieht sich die Erfindung aber auf die Herstellung feuerfester keramischer Formteile, beispielsweise in Form von Steinen, Platten, Hülsen oder dergleichen.
Soweit Massen angesprochen sind schließt dies auch hydraulisch gebundene Massen ein.
Die refraktäre Grundkomponente kann mindestens eine basische Grundkomponente sein, beispielsweise aus der Gruppe: Sintermagnesia, Schmelzmagnesia, Magnesia-Chromit, XY2O4-Spinell (mit X = Mg, Fe, Mn, Zn und Y = Al, Fe, Cr), Dolomitsinter etc. Eine geeignete Grundkomponente kann zumindest anteilig auch eine nichtbasische Grundkomponente sein, beispielsweise aus der Gruppe: Tonerde, Korund, ZrO2, Zirkonsilikat (ZrO2 . SiO2), Mullit, TiO2.
Ein entsprechender Versatz kann in üblicher Weise aufbereitet werden, beispielsweise durch Vermischen der refraktären Grundkomponente mit einem Bindemittel, anschließender Formgebung (zum Beispiel durch Pressen) und Brand zur Sinterung, insbesondere bei Temperaturen > 1.200° Celsius, aber auch bei Temperaturen > 1.500° Celsius.
Das korrosionshemmende Zusatzmittel wird am besten als fein gemahlenes Pulver (d50 ≤l SOμm, insbesondere < 100 μm) eingebracht.
Die Zusatzmittel können als Primärrohstoffe eingesetzt werden. Es ist aber ebenso möglich, Recyclingmaterialien zu verwenden. Molybdän-hältige Zusatzmittel der genannten Art lassen sich zum Beispiel aus abgebrannten Heizelementen durch entsprechende Vermahlung bereitstellen. Derartige Heizelemente bestehen beispielsweise aus Molybdän-Disilizid (MoSi2), teilweise auch in Kombination mit Wolfram-Verbindungen. Damit steht ein preiswertes Abfallprodukt als Rohstoff für die erfindungsgemäße Verwendung zur Verfügung.
Im Übrigen bilden sich die genannten korrosionshemmenden Verbindungen wie Ca-Molybdat oder Wolframat während des Brandes der Produkte, wobei zum Beispiel vorteilhaft Calcium gebunden wird. Dabei sinkt die Hydratationsanfälligkeit des fertigen Produktes.
Die Erfindung wird nachstehend anhand verschiedener Ausführungsbeispiele näher erläutert. Dazu wurde an verschiedenen feuerfesten Werkstoffen ein dynamischer Verschlackungstest (drip slag test) gemäß ASTM-Standard C 768 für Steine aus der Nichteisenmetall-Industrie durchgeführt. Die Schlacke hatte folgende Zusammensetzung [in M-%] (Bestimmung nach oxidierender Glühung):
SiO2: 23
Fe2O3: 43
SO3: 9
CuO: 13
PbO: 3
ZnO: 5
Al2O3: 1
Sonstige _3
100
Folgende, bei 1.650° C gebrannte Probenkörper wurden bei einer Versuchstemperatur von 1.480° C an Luft untersucht (Angaben der Korngrößen beziehen sich auf den Versatz):
Beispiel 1 : 100 Masse-% Sintermagnesia (< 6 mm)
Beispiel 2: 93 Masse-% Sintermagnesia (< 6 mm), 7 Masse-% feinteilige
(100 μm) MgO-Suspension, 1 Masse-% MoSi2 (als Pulver < 100 μm)
Beispiel 3 : 100 Masse-% Magnesia-Chromit
Beispiel 4: 99,7 Masse-% Magnesia-Chromit, 0,3 Masse-% FeMo (< 100 μm) Der erwähnte Verschlackungstest erbrachte folgende Verschleißvolumina:
Beispiel 1 : 65 cm3
Beispiel 2: 24 cm3
Beispiel 3: 37 cm3
Beispiel 4: 2,2 cm3
Die Ergebnisse des Verschleißversuches belegen, dass erfindungsgemäße Produkte unter Verwendung der genannten Zusatzmittel beziehungsweise mit den genannten korrosionshemmenden Phasen ein deutlich geringeres Verschleißvolumen aufweisen. Im Fall des Beispiels 4 ist das Verschleißvolumen so gering, dass der entsprechende Stein als nahezu korrosionsresistent gegenüber der aufgetropften fayalitischen Schlacke gelten kann.
Aus den Gruppen der Zusatzmittel (für den Versatz) beziehungsweise Elementen und Verbindungen (im fertigen Produkt) können einzelne oder Untergruppen ausgeschlossen werden.

Claims

Feuerfestes keramisches ProduktA n s p r ü c h e
1. Feuerfestes keramisches Produkt, das a) > 93 Masse-% mindestens einer refraktären Grundkomponente und b) < 7 Masse-% mindestens einer korrosionshemmenden Komponente aus der Gruppe: bl) Übergangsmetalle b2) Verbindungen von Übergangsmetalien untereinander b3) nicht oxidische Verbindungen von Übergangsmetallen b4) oxidische Verbindungen von Übergangsmetallen b5) Verbindungen der Übergangsmetalle mit Ca, Ba, Sr enthält.
2. Produkt nach Anspruch 1 , bei dem der Anteil der korrosionshemmenden Komponente < 5 Masse-% beträgt.
3. Produkt nach Anspruch 1 , bei dem der Anteil der korrosionshemmenden Komponente < 3 Masse-% beträgt.
4. Produkt nach Anspruch 1 , bei dem der Anteil der korrosions- hemmenden Komponente < 2 Masse-% beträgt.
5. Produkt nach Anspruch 1 , bei dem der Anteil der korrosions- hemmenden Komponente < 1 Masse-% beträgt.
6. Produkt nach Anspruch 1 , bei dem der Anteil der korrosions- hemmenden Komponente < 0,5 Masse-% beträgt.
7. Produkt nach Anspruch 1, mit mindestens einer korrosionshemmenden Komponente aus der Gruppe: Ca-, Ba-, Sr-Molybdat, -Wolframat, -Niobat, -Tantalat.
8. Produkt nach Anspruch 1 , bei dem mindestens eine refraktäre Grundkomponente eine basische Grundkomponente ist.
9. Produkt nach Anspruch 8, bei dem die basische Grundkomponente aus der Gruppe: Sintermagnesia, Schmelzmagnesia, Magnesia-Chromit, XY2θ4-Spinell, Dolomitsinter stammt.
10. Produkt nach Anspruch 1 , bei dem mindestens eine refraktäre Grundkomponente eine nicht-basische Grundkomponente ist.
11. Produkt nach Anspruch 10, bei dem die nicht-basische
Grundkomponente zumindest anteilig aus der Gruppe: Tonerde, Korund, ZrO2, Zirkonsilikat, Mullit, TiO2 stammt.
12. Produkt nach Anspruch 1 , dessen korrosionshemmende Komponente(n) keine nicht-oxidischen Verbindungen von Zr, Ti, Cr, Hf, Fe und keine Verbindungen dieser Elemente mit Ca enthält (enthalten).
13. Produkt nach Anspruch 1 mit einem Verschleißvolumen nach ASTM- C 768 von < 50 cm3.
14. Produkt nach Anspruch 1 mit einem Verschleißvolumen nach ASTM- C 768 von < 30 cm3.
PCT/EP2006/004357 2005-05-30 2006-05-10 Feuerfestes keramisches produkt WO2006128556A2 (de)

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US11/915,276 US20080274870A1 (en) 2005-05-30 2006-05-10 Refractory Ceramic Product
MX2007014894A MX2007014894A (es) 2005-05-30 2006-05-10 Producto refractario de ceramica.
EA200702383A EA011907B1 (ru) 2005-05-30 2006-05-10 Огнеупорный керамический продукт
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ZA200710245B (en) 2008-11-26
EP1888484A2 (de) 2008-02-20
AU2006254476A1 (en) 2006-12-07
EA200702383A1 (ru) 2008-06-30
EA011907B1 (ru) 2009-06-30
CA2611029A1 (en) 2006-12-07
US20080274870A1 (en) 2008-11-06
CN101189198A (zh) 2008-05-28
MX2007014894A (es) 2008-02-11
BRPI0611487A2 (pt) 2010-11-23

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