WO2004065327A2 - Produits refractaires non façonnes, notamment betons refractaires, comprenant des fractions non oxydes - Google Patents

Produits refractaires non façonnes, notamment betons refractaires, comprenant des fractions non oxydes Download PDF

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Publication number
WO2004065327A2
WO2004065327A2 PCT/EP2004/000255 EP2004000255W WO2004065327A2 WO 2004065327 A2 WO2004065327 A2 WO 2004065327A2 EP 2004000255 W EP2004000255 W EP 2004000255W WO 2004065327 A2 WO2004065327 A2 WO 2004065327A2
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WO
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Prior art keywords
refractory
weight
composition according
grained
component
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PCT/EP2004/000255
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German (de)
English (en)
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WO2004065327A3 (fr
Inventor
Dirk Uwe RÜSS
Tadeusz Von Rymon Lipinski
Original Assignee
Esk Ceramics Gmbh & Co. Kg
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Priority claimed from DE10354261A external-priority patent/DE10354261A1/de
Application filed by Esk Ceramics Gmbh & Co. Kg filed Critical Esk Ceramics Gmbh & Co. Kg
Publication of WO2004065327A2 publication Critical patent/WO2004065327A2/fr
Publication of WO2004065327A3 publication Critical patent/WO2004065327A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/101—Refractories from grain sized mixtures
    • C04B35/103—Refractories from grain sized mixtures containing non-oxide refractory materials, e.g. carbon
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • C04B35/043—Refractories from grain sized mixtures
    • C04B35/0435—Refractories from grain sized mixtures containing refractory metal compounds other than chromium oxide or chrome ore
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
    • C04B35/443—Magnesium aluminate spinel
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay

Definitions

  • the invention relates to unshaped refractory products, in particular refractory concrete, with non-oxide components.
  • Refractory unshaped products are one of the high-revenue product areas for the steel industry.
  • the proportion of unshaped products in refractory production in the EU is currently around 43%.
  • Japan is a pioneer in this regard, where the masses already account for almost 60%.
  • Unshaped refractory materials account for over 55% of total refractory material production in the United States. Due to the clear technical and economic advantages, refractory masses are becoming increasingly important in industry and are displacing stone deliveries in many areas.
  • Refractory concretes are mixtures of refractory aggregates and binders, mostly delivered dry and processed after the addition of water or another liquid. They are installed by pouring with vibration, pouring without vibration (self-flowing), by poking or, if necessary, by pounding. Binding and hardening take place without heating. After hardening, drying and heating, a furnace lining is created which, in comparison with fireproof masonry, has particularly few joints and is therefore also called “monolithic" (3). Finished parts can also be made from refractory concrete, which are usually thermally pretreated or prebaked.
  • the usual modern liquefied refractory concretes with their low mixing water requirement contain aggregates with grain sizes up to 10 mm, a small proportion of calcium aluminate cement (3 - 5% by weight) of fine-grained additives such as microsilica and / or alumina different rather primary crystal size (specific surface) and fineness, liquefier and setting regulator.
  • Low-cement vibrating refractory concrete with a correct grain structure requires a water addition of 3.5 to 6% by weight. In the case of self-flowing refractory concrete, the water addition is in the range 4.5 to 7% by weight.
  • the calcium aluminate cement used as a binder in the hydraulically bound refractory concretes is often the weakest link in the structure of the refractory concrete.
  • the reason for this is the relatively low-melting eutectics in the CaO-Al 2 0 3 -Si0 2 system .
  • many efforts have been made to reduce the cement content.
  • low-cement refractory concretes or refractory concretes with an extremely low cement content were developed, see above.
  • Parallel to the technological development of refractory concrete based on calcium aluminate the search for new binder systems to replace calcium aluminate cement continues. The technologically relevant developments are:
  • Phosphate binding primarily based on monoaluminium phosphate water glass synthetic resins
  • the fire concrete and door locking compounds are best suited for mechanizing and automating the delivery.
  • the ramming masses and plastic masses, which also belong to the group of unshaped products, are not so cheap in this respect.
  • Modern refractory concrete achieves property values that can exceed that of refractory bricks.
  • Refractory concretes are usually characterized by good corrosion resistance. It is caused, among other things, by a small pore diameter, especially in self-flowing refractory concrete. In many areas of application, for example in the steel industry, this is still not enough, so that people are looking for opportunities for further improvement.
  • One of them is the integration into the material structure of the carbon parts. Primarily graphite and carbon black are used. Similar to shaped stones, the carbon phase brings a significant increase in corrosion resistance. However, due to the poor wettability by water, larger amounts of carbon cannot be easily introduced into a refractory concrete.
  • Carbon-containing concretes also require higher amounts of mixing water, which, however, creates the drying difficulties described above.
  • the use of surface-active substances provides some remedy here.
  • the protection of carbon from burning out of the structure of a refractory concrete has been largely unsolved. After carbon oxidation, pores develop in the material structure, which impair the corrosion resistance.
  • the metallic antioxidants commonly found in molded MAGCARBON (magnesia carbon) stones can only be used to a limited extent. Since the concrete suspensions have a basic character, the metal powders can react with the components and additives dissolved in the mixing water.
  • the resulting hydrogen represents a potential hazard (Hara, T.; Yasuda, N .; Sugiyama, K.; Shimizu, I .: Gas evolution of silicon-containing castables. Taikabutsu Overseas 22 (2002), 2, 114- 117).
  • refractory unshaped masses in particular refractory concrete, which have a significantly improved corrosion resistance compared to conventional products and can be produced on an industrial scale and economically.
  • a refractory mass containing a coarse-grained refractory component (so-called coarse grain) and / or a medium-grained refractory component (so-called medium grain) and / or a fine-grained refractory component (so-called flour) and / or a fine-grained component Refractory component (so-called fine grain) characterized in that the mass is carbon-free and comprises a refractory boron-containing, nitrogen-free component.
  • coarse grain coarse grain
  • medium grain fine-grained refractory component
  • flour fine-grained refractory component
  • fine grain fine grain
  • carbon-free means that no unbound carbon, for example in the form of graphite, carbon black and the like, is present in the material.
  • the invention thus also includes refractory compositions and materials which are produced using a carbon-containing binder, for example resin, tar, pitch. Masses with proportions of chemically bound carbon, such as in refractory carbides, such as silicon carbide, are also part of the invention. All typical, oxidic and non-oxidic, acidic and basic raw materials or their combination are used as coarse-grained, medium-grained, fine-grained and fine-grained refractory components.
  • Basic metal oxides such as sintered, melted magnesia, sintered, melted spinel, sintered dolomite, sintered lime, olivine or forsterite are particularly preferred, and masses based on Al 2 O 3 with variable SiO 2 and / or SiC contents are also advantageous. Combinations of these raw materials can also be present.
  • a particularly suitable fire-resistant boron-containing, nitrogen-free component is a compound selected from the group boron carbide BC, refractory borides and their mixtures.
  • Refractory borides are preferably CaB s , TiB 2 , and ZrB 2 . It has been found that also a mixture of several boron-containing, nitrogen-free compounds can be advantageously used '.
  • the boron-containing, nitrogen-free compound is preferably present in amounts from 0.1 to 30% by weight, particularly preferably from 0.5 to 10.0% by weight.
  • the composition according to the invention preferably comprises an additive.
  • additives are preferably metal powders, non-oxides such as, for example, nitrides, carbides, silicides, oxynitrides, oxycarbides, metal fibers, plastic fibers and carbon fibers, and are preferably metal powders Al, Mg, Si and non-oxides such as SiC , A1N, Si 3 N 4 , AlON, SiAlON.
  • the additives are preferably present in amounts of 0.5 to 30% by weight.
  • coarse-grained is preferably to be understood to mean grains> 1 mm, particularly preferably 1-10 mm. Grains of 0.2 to ⁇ 1 mm, preferably 0.2 to 0.5 mm, are used as the middle grain.
  • fine-grained should preferably be understood to mean grains of 0.02 to ⁇ 0.2 mm, particularly preferably 0.02 to 0.1 mm. This grain fraction is usually called flour in technical parlance. Fines are reactive refractory components with an average grain size ⁇ 15 ⁇ m, preferably ⁇ 5 ⁇ m. For example, calcined clay, reactive clay, finely ground, refractory raw materials, microsilica, refractory clay, binding clay are used.
  • the unshaped refractory compositions according to the invention can be bound hydraulically, chemically or ceramic. All binder systems typical in refractory technology are suitable for this purpose. Hydraulic bonding by means of a refractory cement, preferably a calcium aluminate cement, is preferably used in an amount of up to 25% by weight, preferably 1 to 10% by weight.
  • liquid binders common in the refractory industry are suitable for chemical bonding, ie as binders, both water-free and water-containing, for example resins, tar, pitch.
  • the amount of binder is preferably between 0.1 and 50% by weight, preferably between 1 and 10% by weight.
  • Ceramic bonding occurs in the compositions according to the invention when heated to temperatures> 700 ° C. This process is supported by the use of very fine grain fractions.
  • the masses are mixed with up to 40% by weight, preferably ⁇ 10% by weight, of water.
  • Additive is in the range up to max. 5% by weight, preferably ⁇ 1.5% by weight.
  • the coarse-grained component is preferably present in amounts of ⁇ 90% by weight, particularly preferably in amounts of 15 to 80% by weight.
  • the medium-grain component is preferably present in amounts of ⁇ 40% by weight, particularly preferably in amounts of 3 to 20% by weight.
  • the fine-grained component is preferably present in amounts of ⁇ 95% by weight, particularly preferably in amounts of 5 to 80% by weight.
  • the fine-grain component is preferably present in amounts of ⁇ 50% by weight, particularly preferably in amounts of 0.1 to 35% by weight.
  • special metallic and / or non-oxidic substances can be added to the refractory compositions according to the invention. These are preferably compounds selected from the group of metal powders Al, Mg, Si and non-oxides such as SiC, A1N, Si 3 N 4 , A10N, SiAlON.
  • metal fibers For the purpose of reinforcing the structure and / or improving the drying process, the addition of metal fibers is also advantageous.
  • the carbon-free refractory compositions according to the invention are distinguished by a number of positive properties. Due to the relatively high thermal conductivity of the boron-containing additives, they have an improved thermal shock resistance compared to compositions without additives.
  • the boron-containing compounds Due to the high affinity for oxygen, the boron-containing compounds show good oxidation resistance in the material structure. This behavior is supported by the formation of passivation layers on the surface of the material, which make contact with oxygen more difficult.
  • the added boron-containing substances are poorly wetted by ionic melts, which limits the wetting by molten slags. This improves the corrosion resistance and contributes to increasing the durability of these new refractory compounds.
  • a high compression of the material structure is important for the corrosion resistance of the refractory materials. This can include can be improved by an appropriate grain distribution.
  • the following grain structure has proven to be advantageous for the offset according to the invention:
  • Coarse grain component ⁇ 90% by weight> 0.2 mm. Portions of 15 to 80% by weight of the grain fraction 1-10 mm are preferred.
  • Medium grain component ⁇ 40% by weight of the grain fraction 0.2 to 1 mm. Portions of 3 to 20% by weight of the grain fraction 0.2-0.5 mm are preferred.
  • Fine grain component ⁇ 95% by weight ⁇ 0.2 mm, preferably 5 to 80% by weight
  • Fine grain component ⁇ 50% by weight ⁇ 15 ⁇ m, preferably 0.1 to 35% ⁇ 5 ⁇ m
  • refractory compositions according to the invention are produced at the refractory manufacturer or on-site at the refractory user, preferably in the following steps:
  • additives additives and further homogenization of the batch. If necessary, substances are added to the mixture, which take on certain functions in the finished masses. Examples are metal powder and non-oxide materials such as carbides, nitrides, silicides, metal fibers, plastic fibers, carbon fibers, which further improve the resistance to oxidation, strength, drying behavior, corrosion resistance and the thermal shock resistance of the material.
  • metal powder and non-oxide materials such as carbides, nitrides, silicides, metal fibers, plastic fibers, carbon fibers, which further improve the resistance to oxidation, strength, drying behavior, corrosion resistance and the thermal shock resistance of the material.
  • the homogenized mixture is ready for use and can be made using techniques familiar in refractory technology, e.g. Pouring, vibrating, spraying, door locking, pounding, etc., are processed into a monolithic refractory lining or a functional mass.
  • Prefabricated components can also be produced from the refractory materials according to the invention.
  • the masses produced as described above are brought into a metal, or wood , or plastic mold.
  • the mass can be further compacted by subsequent vibration, pounding, pressing, etc.
  • the component is shaped and dried and / or tempered at 80 to 700 ° C. If necessary, the dried or tempered component can be fired.
  • the firing conditions essentially depend on the chemical and mineralogical composition of the refractory mass as well as the shape and geometry of the component.
  • the prefabricated components according to the invention are ready for use.
  • the unshaped refractory compositions according to the invention can be used in the furnaces and plants of the non-ferrous industry, steel industry, cement industry, glass industry, waste incineration plants, etc.
  • test specimens 50x50 mm were produced from the masses. The The test specimens were produced by pouring them into a plastic mold, curing them at room temperature for 24 hours, and then drying them at 110 ° C. for 24 hours. The dried test specimens were characterized by the determination of the cold compressive strength, KDF, (DIN EN 9935), bulk density, RD, (DIN EN 993) and open porosity, OP, (DIN EN 993). The results obtained are summarized in the table below.
  • a bauxite refractory concrete was made with the following composition:
  • Sintered bauxite (sinter bauxite) is a commercially available product.
  • Sintered corundum T60, calcined alumina CTC 50, alumina cement CA 270 and additives can be obtained, for example, from ALCOA Germany.
  • the mixture was then made into a concrete with 5.7% by weight of mixing water.
  • Cylindrical test crucibles for testing corrosion resistance were made from the concrete. As shown in Example 1, the production was carried out by pouring the liquefied concrete into a plastic mold.
  • the casting mold was constructed in such a way that a round recess with a diameter of 30 mm and a depth of 10 mm was created on one side of the test cylinder.
  • the depression was used to hold a test metal melt.
  • 24 h and drying at 110 ° C, 24 h, 20 g of pure aluminum powder were placed in the well of the crucible.
  • the crucible was then aged at 800 ° C for 72 hours in an electric oven with no air.
  • the test crucible was examined for any signs of corrosion, such as chemical reaction with the metal and infiltration of the metal into the material structure.
  • a crucible test was made from the same refractory concrete without BC addition and examined under the same conditions.
  • the bauxite B 4 C refractory concrete according to the invention showed no infiltration and a significantly better corrosion resistance compared to the Al melt in comparison to the material without boron carbide.
  • the spinel raw materials are a sintered Al 2 0 3 -rich magnesium-aluminum spinel, which is available from ALCOA Germany can be obtained.
  • the other components, calcined spinel / alumina CTC 55, alumina cement and additives can also be obtained from this company.
  • test crucible After cooling, the test crucible was examined for any signs of corrosion, such as chemical reaction with the slag and its infiltration into the material structure. For comparison, a crucible test was made from the same refractory concrete without ZrB 2 and examined under the same conditions.
  • the spinel concrete according to the invention with ZrB 2 addition showed a significantly better infiltration and corrosion resistance compared to the material without addition.
  • the magnesia sinter is a sintered high-purity magnesia, for example from NEDMAG.
  • Titanium boride e.g. titanium di boride
  • the components were dry homogenized and then prepared into a sprayable mass by mixing with 12% by weight Na water glass.
  • the mass was applied to a fired magnesia stone and fired at 1550 ° C for 2 hours. After the fire, the mass adhered very well to the stone surface and showed very good oxidation resistance and corrosion resistance compared to a steel converter slag.
  • the mass is suitable for performing both cold and hot repairs of the refractory deliveries.
  • composition made:
  • Silicon carbide powder ⁇ 45 ⁇ m 12% by weight
  • Sintered corundum raw materials can be obtained from ALCOA Germany.
  • a product from ESK-SiC GmbH was used as silicon carbide powder and a commercially available product was used as silicon powder.
  • the components became dry with 3% by weight of ZrB 2 (from Wacker
  • test crucibles were examined for any signs of corrosion, such as chemical reaction with the slag and its infiltration into the material structure.
  • the Al 2 0 3 SiC ramming mass according to the invention with ZrB 2 showed a significantly better infiltration and corrosion resistance compared to the material without addition.
  • the sources of supply for raw materials, additives and additives are as mentioned in the previous examples.
  • test specimens were determined by determining the cold compressive strength, KDF, (DIN EN 9935), bulk density, RD, (DIN EN 993), open porosity, OP, (DIN EN 993) and thermal shock resistance TWB (DIN EN 993-11). For comparison, test specimens without the addition of steel fibers were produced and examined under the same conditions. After drying, the test specimens had the following characteristic values:

Abstract

La présente invention concerne une masse réfractaire contenant une composante réfractaire à gros grains (grain grossier) et/ou une composante réfractaire à grains de moyenne taille (grain moyen) et/ou une composante réfractaire à petits grains (fines) et/ou une composante réfractaire à très petits grains (grain très fin). L'invention se caractérise en ce que la masse est dépourvue d'hydrocarbures et comprend une composante réfractaire dépourvue d'azote qui comprend du bore.
PCT/EP2004/000255 2003-01-23 2004-01-15 Produits refractaires non façonnes, notamment betons refractaires, comprenant des fractions non oxydes WO2004065327A2 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE10302609.6 2003-01-23
DE10302609 2003-01-23
DE10354261.2 2003-11-20
DE10354261A DE10354261A1 (de) 2003-01-23 2003-11-20 Ungeformte feuerfeste Erzeugnisse, insbesondere Feuerbetone, mit Nichtoxidanteilen

Publications (2)

Publication Number Publication Date
WO2004065327A2 true WO2004065327A2 (fr) 2004-08-05
WO2004065327A3 WO2004065327A3 (fr) 2005-03-24

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013011432A1 (fr) * 2011-07-20 2013-01-24 Saint-Gobain Centre De Recherches Et D'etudes Europeen Canal d'alimentation de verre en fusion
CN102958867A (zh) * 2010-04-28 2013-03-06 新日铁住金株式会社 不定形耐火物用粘结剂、不定形耐火物以及不定形耐火物的施工方法
CN109553423A (zh) * 2017-09-26 2019-04-02 纳米及先进材料研发院有限公司 用于生产耐火混凝土砖的组分及耐火混凝土砖

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JPH06305844A (ja) * 1993-04-28 1994-11-01 Kawasaki Steel Corp ＭｇＯ−レジン系不定形耐火物
JPH0782002A (ja) * 1993-06-23 1995-03-28 Kyushu Refract Co Ltd マグネシア質耐火組成物
CN1113715C (zh) * 2001-08-03 2003-07-09 山西新型炉业集团有限公司 连铸中间包碱性干式工作衬

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102958867A (zh) * 2010-04-28 2013-03-06 新日铁住金株式会社 不定形耐火物用粘结剂、不定形耐火物以及不定形耐火物的施工方法
US8835338B2 (en) 2010-04-28 2014-09-16 Nippon Steel & Sumitomo Metal Corporation Binder for monolithic refractories, monolithic refractory, and construction method of monolithic refractories
WO2013011432A1 (fr) * 2011-07-20 2013-01-24 Saint-Gobain Centre De Recherches Et D'etudes Europeen Canal d'alimentation de verre en fusion
FR2978140A1 (fr) * 2011-07-20 2013-01-25 Saint Gobain Ct Recherches Canal d'alimentation de verre en fusion
US9550692B2 (en) 2011-07-20 2017-01-24 Saint-Gobain Centre De Recherches Et D'etudes Method of manufacturing a feeder channel for molten glass
EA028258B1 (ru) * 2011-07-20 2017-10-31 Сен-Гобен Сантр Де Решерш Э Д'Этюд Эропеэн Способ изготовления подводящего канала для стекловаренной печи и блока основания такого канала
CN109553423A (zh) * 2017-09-26 2019-04-02 纳米及先进材料研发院有限公司 用于生产耐火混凝土砖的组分及耐火混凝土砖
CN109553423B (zh) * 2017-09-26 2021-11-19 纳米及先进材料研发院有限公司 用于生产耐火混凝土砖的组分及耐火混凝土砖

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