US20180282224A1 - Batch for production of a refractory product, a process for the production of a refractory product, a refractory product as well as the use of a refractory product - Google Patents

Batch for production of a refractory product, a process for the production of a refractory product, a refractory product as well as the use of a refractory product Download PDF

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US20180282224A1
US20180282224A1 US15/543,178 US201515543178A US2018282224A1 US 20180282224 A1 US20180282224 A1 US 20180282224A1 US 201515543178 A US201515543178 A US 201515543178A US 2018282224 A1 US2018282224 A1 US 2018282224A1
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weight
product
batch
refractory product
refractory
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Boro Djuricic
Norbert Freiberger
Jurgen Muhlhausser
Christoph Bauer
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Refractory Intellectual Property GmbH and Co KG
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Refractory Intellectual Property GmbH and Co KG
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Assigned to REFRACTORY INTELLECTUAL PROPERTY GMBH & CO. KG reassignment REFRACTORY INTELLECTUAL PROPERTY GMBH & CO. KG ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BAUER, CHRISTOPH, DJURICIC, BORO, MUHLHAUSSER, JURGEN, FREIBERGER, NORBERT
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Definitions

  • the invention relates to a batch for the production of a refractory product, to a process for the production of a refractory product, to a refractory product as well as to the use of a refractory product.
  • refractory product as used in the context of the invention in particular describes refractory ceramic products with a service temperature of more than 600° C., and preferably refractory substances in accordance with DIN 51060, i.e. substances with a pyrometric cone equivalent of >SK17.
  • the pyrometric cone equivalent may in particular be determined in accordance with DIN EN 993-12.
  • batch describes a composition formed from one or more components from which a refractory product can be produced by means of a heat treatment, i.e. in particular by means of ceramic firing or by melting.
  • Conventional refractory substances for the production of a refractory product are in particular based on the metallic oxides Al 2 O 3 , MgO, SiO 2 , CaO, Cr 2 O 3 and ZrO 2 .
  • batches formed from components or raw materials are prepared which in particular comprise substances consisting of these oxides.
  • refractory substances also comprise raw materials based on non-oxides in addition to raw materials based on the metal oxides mentioned above.
  • non-oxide raw materials of this type may be non-oxide raw materials in the form of metal carbides, metal nitrides, metal borides, metal oxycarbides, metal oxynitrides and metal oxycarbonitrides.
  • refractory substances can be produced with properties which can be used for applications beyond the field of application of conventional refractory ceramic substances based on metallic oxides.
  • the service temperatures, the tolerance to damage and the corrosion resistance of refractory ceramic substances based on a combination of raw materials based on oxides and non-oxides can be substantially improved.
  • Non-oxide-based raw materials are usually synthetic raw materials.
  • non-oxide raw materials of this type are based on alumina and carbon.
  • raw materials based on alumina and carbon are usually melted in an electric arc furnace. The cooled melt is then broken up into pieces and used as raw material for batches for the production of refractory products.
  • the object of the invention is to provide a batch by means of which a refractory product, in particular a so-called non-oxide refractory product, can be produced which is characterized by an extremely small proportion of hydration-sensitive phases, in particular a small proportion of hydration-sensitive phases based on alumina-carbon, such as Al 4 C 3 in particular.
  • a further object of the invention is to provide a batch for the production of a refractory product, in particular a non-oxide refractory product, melting of which produces an extremely small proportion of carbon monoxide.
  • a further object of the invention is to provide a process by means of which a refractory product, in particular a non-oxide refractory product, can be produced with an extremely small proportion of hydration-sensitive phases, in particular of hydration-sensitive phases based on alumina-carbon.
  • a further object of the invention is to provide a process for the production of a refractory product, in particular a non-oxide refractory product, wherein only extremely small proportions of carbon monoxide are produced during the production thereof.
  • a further object of the invention is to provide a refractory product, in particular a non-oxide refractory product, which comprises an extremely small proportion of hydration-sensitive phases, in particular hydration-sensitive phases based on alumina-carbon.
  • the object of the invention is achieved by means of the inventive provision of a batch for the production of a refractory product comprising the following components:
  • At least one silicate component in the form of at least one aluminium silicate or at least one zirconium silicate.
  • the scientific basis for this advantageous effect of these silicates in providing the solution given by the invention has yet to be explained in detail, but there are indications that the presence of silicon suppresses the formation of Al 4 C 3 .
  • a refractory non-oxide product based on alumina-carbon can be produced.
  • the batch therefore has a base component based on alumina (Al 2 O 3 ).
  • the base component may consist of one or more components or raw materials based on alumina.
  • the fact that the base component is said to be “based on” alumina means that it comprises one or more components or raw materials which respectively consist of at least 50% by weight of Al 2 O 3 with respect to the respective components.
  • the base component can in particular consist of one or more of the following components: fused corundum, sintered corundum or calcined alumina.
  • the base component is in the form of calcined alumina.
  • the base components can be present in the batch in a proportion of at least 50% by weight including, for example, in a proportion of at least 55%, 60%, 65%, 70%, 75%, 80%, 82%, 84%, 86%, 88%, 90%, 91%, 92%, 93%, 94% or 95% by weight.
  • the base component may, for example, be present in the batch in a proportion of at most 99%, 98%, 97%, 96%, 95%, 94%, 93%, 92%, 91% or 90% by weight.
  • the at least one silicate component may comprise one or more of the following components or raw materials: at least one silicate component based on aluminium silicate or at least one silicate component based on zirconium silicate.
  • the at least one silicate component includes at least one silicate component based on aluminium silicate and at least one silicate component based on zirconium silicate (mineralogical zircon, ZrSiO 4 ).
  • aluminium silicate as used here generally represents silicates based on the basic oxides Al 2 O 3 and SiO 2 .
  • the term “aluminium silicate” encompasses both aluminosilicates and also aluminium silicates.
  • the silicate component based on aluminium silicate can in particular be in the form of one or more of the following components or raw materials based on aluminium silicate: kaolin, metakaolin, fireclay, pyrophyllite, calcined bauxite or mullite.
  • Kaolin is a natural raw material with kaolinite (Al 4 [(OH) 8
  • Pyrophyllite (Al 2 [(OH) 2
  • Bauxite is an aluminium ore which in particular comprises various aluminium minerals (in particular gibbsite ( ⁇ -Al(OH) 3 ), boehmite ( ⁇ -AlO(OH)), diaspore ( ⁇ -AlO(OH)), iron compounds (haematite (Fe 2 O 3 ) and goethite (FeO(OH)), kaolinite and titanium oxide (anatase (TiO 2 )).
  • Mullite (3 Al 2 O 3 .2 SiO 2 ; 2 Al 2 O 3 .SiO 2 ) can act as the aluminium silicate in the batch of the invention, in particular as a synthetic mullite, especially in the form of at least one of the following components: fused mullite or sintered mullite.
  • Silicate components based on aluminium silicate may, for example, be present in the batch in a proportion of at least 0.5% by weight and for example in a proportion of at most 25% by weight including, for example, in a proportion of at least 1%, 2%, 3% or 4% by weight and also, for example, in a proportion of at most 20%, 15%, 12%, 10%, 9%, 8%, 7% or 6% by weight.
  • the silicate component based on aluminium silicate is in the form of at least one of the raw materials fireclay or kaolin or in the form of the raw materials fireclay and kaolin.
  • Zirconium silicate i.e. ZrSiO 4 ; mineral name “zircon”
  • ZrSiO 4 mineral name “zircon”
  • Zirconium silicate may, for example, be present in the batch in proportions of at least 1% by weight and also, for example, in proportions of at most 35% by weight including, for example, in a proportion of at least 2%, 3%, 4%, 5%, 6% or 7% by weight and also, for example, in a proportion of at most 30%, 25%, 20%, 15%, 12%, 11%, 10% or 9% by weight.
  • the silicate components may, for example, be present in the batch in a proportion of at least 0.5% by weight and, for example, in a proportion of at most 35% by weight including, for example, in a proportion of at least 1%, 2%, 3% or 4% by weight and also, for example, in a proportion of at most 30%, 25%, 20%, 15%, 12%, 11%, 10% or 9% by weight.
  • the carbon component comprises one or more carbon sources, for example at least one of the following carbon sources: graphite, carbon black or petroleum coke.
  • the carbon component is present in the form of graphite.
  • the carbon component is present in the batch in a proportion of at least 0.5% by weight, preferably in a proportion of at most 8.5% by weight including, for example, in a proportion of at least 1%, 2%, 3% or 4% by weight and also, for example, in a proportion of at most 8%, 7%, 6% or 5% by weight.
  • the proportion of Al 4 C 3 in a refractory product produced from a batch in accordance with the invention by means of a melting process can be drastically reduced if the proportion of carbon in the batch is adjusted such that the proportion of carbon in the product produced from the batch is less than 2.4% by weight.
  • this target can in particular be reached when the proportion of carbon in the batch is in particular less than 8.5% by weight.
  • the proportion of carbon in the batch can in particular be less than 8.5% by weight including, for example, less than 8%, 7%, 6% or 5% by weight.
  • the proportion of carbon in the batch may be set at more than 0.45% by weight.
  • the silicate component in addition to the base component (in particular in the form of calcined silica), the silicate component (in particular in the form of kaolin, metakaolin, fireclay, pyrophyllite, fired bauxite and/or mullite as well as in the form of zircon) as well as the carbon component (in particular in the form of graphite), the batch may comprise other components, in only a proportion of less than 2% by weight including, for example, in a proportion of less than 1% by weight.
  • all of the components of the batch of the invention are present in grains which are as fine as possible.
  • all of the components of the batch have a mean grain size of less than 1 mm.
  • at least 90% by weight of the components of the batch including, for example, 100% by weight of the components of the batch may have a grain size of less than 1 mm, less than 0.8 mm, less than 0.6 mm or even less than 0.5 mm.
  • the batch of the invention may also react extremely sensitively to certain components.
  • the components of the batch may be fine-tuned so that the amount of certain substances or oxides in the batch does not exceed a specific amount.
  • the batch may comprise the following oxides in the following proportions, wherein the respective proportions may be present in the batch individually or in any combination:
  • a refractory product In order to produce a refractory product from the batch of the invention, it may undergo a heat treatment, in particular by melting. After cooling a melt formed from such a batch of the invention, a refractory product is obtained.
  • the invention also pertains to a process for the production of a refractory product, comprising the following steps:
  • Melting the batch by heat treatment is in particular carried out so that the batch forms a melt.
  • the batch may be melted in an electric arc furnace.
  • the batch may be melted at temperatures of over 2000° C.
  • the batch may be melted in a reducing atmosphere.
  • a reducing atmosphere of this type may be established by the melting per se of the batch of the invention.
  • a refractory product is obtained, in particular in the form of a non-oxide refractory product, for example a refractory product also in the form of a solidified melt.
  • the invention also pertains to a product which in particular is produced by a process in accordance with the invention, in particular a refractory product in the form of a solidified melt.
  • the batch of the invention can be melted in a crucible using an electric arc furnace and then can be cooled and solidified therein, so that a refractory product is obtained in the form of a solidified melt.
  • a product in accordance with the invention is characterized by characteristic phases and properties.
  • the product of the invention may have a very high density, in particular a density of more than 3.3 g/cm 3 including, for example, a density in the range 3.3 to 3.9 g/cm 3 including, for example, a density of at least 3.4 or 3.5 or 3.55 or 3.6 g/cm 3 , and also, for example, a density of at most 3.85 or 3.8 or 3.75 or 3.70 g/cm 3 .
  • the density is approximately 3.62 g/cm 3 .
  • the product in accordance with the invention may preferably have a relatively small open porosity, for example an open porosity of less than 8% by volume including, for example, an open porosity in the range 2% to 8% by volume including, for example, an open porosity of at most 7%, 6% or 5% by volume and also, for example, an open porosity of at least 3% or 3.5% or 4% or 4.5% by volume.
  • the open porosity is approximately 4.85% by volume.
  • the product of the invention may comprise a small proportion of carbon, in particular a proportion of carbon of less than 2.4% by weight including, for example, a proportion of carbon of less than 2.2% or 2.0% or 1.8% or 1.6% or 1.4% or 1.2% or 1.0% by weight or even less than 0.9% by weight.
  • the proportion of carbon in the product of the invention may be at least 0.1% or 0.2% or 0.3% or 0.4% or 0.5% or 0.6% or 0.7% or 0.8% by weight.
  • a particular characteristic of the product of the invention is that it may comprise inclusions of metals and metal alloys.
  • these metals may be metals in the form of metallic aluminium and silicon, since the element aluminium is present in the base component and the element silicon is present in the silicate component of the batch.
  • the metal alloys may in particular be those which comprise at least one of the metals aluminium and silicon, and possibly one or more other metals which are present as elements in the components of the batch, for example titanium (Ti) or iron (Fe), as they are natural impurities in bauxite.
  • characteristic inclusions in the product of the invention may be metallic aluminium and metallic silicon as well as, if appropriate, one or more alloys based on the metals aluminium and silicon as well as at least one of the metals titanium and iron, for example at least one of the following alloys: AlSi, AlSiFe, AlSiTi or AlSiTiFe.
  • Inclusions of metallic aluminium or silicon or the metal alloys indicated above may, for example, be present in the product of the invention in proportions of up to 2% by weight.
  • a particular characteristic of these inclusions of metallic aluminium and silicon as well as metal alloys is that they are embedded in the product of the invention, in particular when the product of the invention is in the form of a solidified melt.
  • the density of the product of the invention is high and the porosity is low, so that the inclusions of these metals and metal alloys are protected from the surrounding atmosphere.
  • the product of the invention proves to be a superb raw material for a batch for the production of a carbon-bonded refractory product, in particular for the production of a carbon-bonded product in the form of an alumina-carbon product (in particular a Al 2 O 3 —C brick) or a magnesia-carbon product (in particular a MgO—C brick).
  • alumina-carbon product in particular a Al 2 O 3 —C brick
  • a magnesia-carbon product in particular a MgO—C brick
  • any cracks can be closed by the metallic inclusions and metal alloys, since when they come into contact with the atmosphere, they oxidize and increase in volume and thus close up the cracks which have formed.
  • the refractory product can thus act in a self-healing manner to wear and damage.
  • a batch for the production of a carbon-bonded refractory product of this type does not need any further additions of antioxidant apart from the raw material from the product of the invention.
  • the product of the invention may in particular also contain one or more of the following phases: metal carbides, metal oxycarbides, metal oxycarbonitrides, metal oxynitrides or metal nitrides.
  • these phases may be one or more of the following phases: SiC, Al 4 O 4 C, SiAlON, SiCAlON or Al oxynitride.
  • a product in accordance with the invention may comprise the following phases in the following proportions by weight, respectively individually or in combination:
  • the total weight of the phases Al 4 O 4 C, SiC, SiAlON, SiCAlON, Al oxynitride may be determined substantially or mostly by the proportion by weight of Al 4 O 4 C wherein, for example, the proportion by weight of Al 4 O 4 C in the total weight of the phases Al 4 O 4 C, SiC, SiAlON, SiCAlON, Al oxynitride may be in the range from 0 to 100% by weight, with respect to the total weight of the phases Al 4 O 4 C, SiC, SiAlON, SiCAlON, Al oxynitride.
  • the proportion of the remaining non-oxide phases, in particular the phases SiC, SiAlON and SiCAlON, in the product may advantageously be such that the proportion by weight of Al 4 O 4 C in the total weight of the phases Al 4 O 4 C, SiC, SiAlON, SiCAlON, Al oxynitride with respect to the total weight of the phases Al 4 O 4 C, SiC, SiAlON, SiCAlON and Al oxynitride, may also, for example, be at most 90%, 80%, 70% or 60% by weight and also, for example, at least 10%, 20%, 30% or 40% by weight.
  • the total weight of Al 4 O 4 C may be: at least 0.25% or 0.5% or 1% or 1.5% or 2% or 2.5% or 3% or 3.5% by weight, at most 36%, 33%, 30%, 27%, 25%, 20%, 18%, 16%, 14%, 12%, 10%, 9%, 8%, 7%, 6%, 5% or 4% by weight.
  • the total weight of SiC, SiAlON and SiCAlON in the product of the invention may be: at least 0.25% or 0.5% or 1% or 1.5% or 2% or 2.5% or 3% or 3.5% by weight, at most 30%, 25%, 20%, 18%, 16%, 14%, 12%, 10%, 9%, 8%, 7%, 6%, 5% or 4% by weight.
  • the product of the invention may comprise other phases, in particular in a proportion of at most 2% or 1.5% or 1% by weight.
  • the product of the invention is in particular characterized by isotropic Al 4 O 4 C crystals in particular in the form of islands through the volume of the product.
  • the Al 4 O 4 C crystals in the product of the invention are primarily in the region of the grain boundaries of the grains of Al 2 O 3 .
  • the crystals of the phases Al 2 O 3 , Al 4 O 4 C, SiC and SiCAlON in the product of the invention may in particular have the following mean dimensions, wherein at least 90% by weight of the respective crystals including, for example, at least 95% or 100% by weight with respect to the proportion of the respective crystals of the phases mentioned above with respect to the total weight of this phase in the product may be in these ranges:
  • the product may comprise the following oxides in the following respective proportions by weight, wherein the oxides, respectively individually or in combination, may be present in the following respective proportions by weight in the product:
  • the product of the invention makes a highly suitable raw material for the production of a refractory product, in particular a carbon-bonded product.
  • the invention also pertains to the use of a refractory product in accordance with the invention as a raw material for the production of a refractory product, in particular a carbon-bonded product, in particular a refractory alumina-carbon or magnesia-carbon product.
  • the refractory product of the invention can thus be used when the product of the invention, in particular in the form of a solidified melt, is comminuted, in particular into a grainy material, and then used as a raw material for the production of a refractory carbon-bonded product.
  • the calcined silica which in the exemplary embodiment constituted the base component based on alumina, was of high purity, with a proportion of Al 2 O 3 of 99.4% by weight with respect to the weight of the calcined silica.
  • the d 90 value for the grain size was 95 ⁇ m.
  • the carbon component was constituted by graphite.
  • the proportion of carbon was 94.61% by weight with respect to the weight of graphite.
  • the d 90 value for the grain size was 500 ⁇ m.
  • the silicate component based on aluminium silicate, was kaolin, wherein the total proportion of Al 2 O 3 and SiO 2 was 97.6% by weight with respect to the weight of the kaolin.
  • the d 90 value for the grain size was 17.6 ⁇ m.
  • the chemical composition of the batch was as follows:
  • the components of the batch were mixed and melted in a crucible in an electric arc furnace at a temperature of more than 2000° C. for a period of approximately 5 hours.
  • melt was allowed to cool and solidify in the crucible in order to produce a refractory product in the form of a solidified melt.
  • the product comprised the following phases in the following proportions:
  • the proportion of carbon in the product was 0.78% by weight.
  • the density of the product was 3.62 g/cm 3 .
  • the open porosity of the product was 4.85% by volume.
  • the density was determined in accordance with British Standard BS 1902-3.16:1990 with a mercury intrusion pressure for the measurements of 0.52 psia.
  • the open porosity was determined in accordance with British Standard BS 1902-3.16:1990 with a mercury intrusion pressure for the measurements of 0.52 psia and 33000 psia.
  • the proportion of carbon in the product was determined in accordance with DIN EN ISO 21068-2:2008-12.
  • Polished sections were prepared from this product and enlarged electron microscopic images of these samples were produced from these samples, as shown in FIGS. 1 to 3 .
  • the white bar in the bottom right hand corner of the image corresponds to a length of 200 ⁇ m.
  • the phase with reference numeral 1 corresponds to Al 2 O 3 .
  • Reference numeral 2 indicates the non-oxide phases in the form of SiC, Al 4 O 4 C, SiAlON, SiCAlON and Al oxynitride in particular. The isotropic distribution of the non-oxide phases can clearly be discerned.
  • reference numeral 3 indicates pores in the microstructure of the product.
  • reference numeral 1 indicates the major phase in the form of corundum.
  • the phases indicated with reference numerals 4 , 5 and 6 are each non-oxide phases.
  • reference numeral 4 indicates a phase in the form of SiXAlON
  • reference numeral 5 indicates a phase in the form of SiC
  • reference numeral 6 indicates a mixed non-oxide phase.
  • the white bar in the bottom right hand corner of the image indicates a length of 50 ⁇ m.
  • Reference numeral 1 indicates the major phase in the form of corundum, while reference numeral 4 once again indicates a non-oxide phase in the form of SiCAlON and reference numeral 7 indicates a phase in the form of metallic silicon.
US15/543,178 2015-02-09 2015-11-25 Batch for production of a refractory product, a process for the production of a refractory product, a refractory product as well as the use of a refractory product Abandoned US20180282224A1 (en)

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AR103276A1 (es) 2017-04-26
EP3053897A1 (de) 2016-08-10
WO2016128082A1 (de) 2016-08-18
US20190210925A1 (en) 2019-07-11
RU2017121612A3 (es) 2019-05-23
RU2017121612A (ru) 2018-12-20
KR20170115488A (ko) 2017-10-17
MX2017008776A (es) 2017-11-17
CN107108370B (zh) 2021-11-26
US11198647B2 (en) 2021-12-14
BR112017014235A2 (pt) 2018-03-27
TW201628994A (zh) 2016-08-16

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