EP3924319A1 - Produit refractaire a haute teneur en zircone - Google Patents

Produit refractaire a haute teneur en zircone

Info

Publication number
EP3924319A1
EP3924319A1 EP20705158.2A EP20705158A EP3924319A1 EP 3924319 A1 EP3924319 A1 EP 3924319A1 EP 20705158 A EP20705158 A EP 20705158A EP 3924319 A1 EP3924319 A1 EP 3924319A1
Authority
EP
European Patent Office
Prior art keywords
less
refractory product
product according
ai2o3
oxide
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.)
Pending
Application number
EP20705158.2A
Other languages
German (de)
English (en)
French (fr)
Inventor
Isabelle Cabodi
Pierrick Fabien VESPA
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.)
Saint Gobain Centre de Recherche et dEtudes Europeen SAS
Original Assignee
Saint Gobain Centre de Recherche et dEtudes Europeen SAS
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.)
Filing date
Publication date
Application filed by Saint Gobain Centre de Recherche et dEtudes Europeen SAS filed Critical Saint Gobain Centre de Recherche et dEtudes Europeen SAS
Publication of EP3924319A1 publication Critical patent/EP3924319A1/fr
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
    • C03B5/42—Details of construction of furnace walls, e.g. to prevent corrosion; Use of materials for furnace walls
    • C03B5/43—Use of materials for furnace walls, e.g. fire-bricks
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    • 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
    • C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/481—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 zirconium or hafnium oxides, zirconates, zircon or hafnates containing silicon, e.g. zircon
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    • 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
    • C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
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    • 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
    • C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/484—Refractories by fusion casting
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    • C04B35/657—Processes involving a melting step for manufacturing refractories
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Definitions

  • the invention relates to a molten refractory product with a high zirconia content as well as a glass melting furnace comprising such a product.
  • Glass melting furnaces generally include a very large number of refractory products, arranged in different places according to their properties. For each part of the furnace, the product chosen will be that which does not cause defects making the glass unusable (which would reduce production yields) and resistant long enough to provide the furnace with a satisfactory life.
  • Figure 1 schematically shows a cross section of a glass melting furnace 10.
  • a tank 12 a metal structure 14 and a superstructure 16 can be distinguished.
  • the vessel 12 intended to contain the molten glass, comprises a vertical side wall 22 and a sole 24.
  • the side wall 22 is conventionally formed of side vessel blocks which extend over the entire height of the vessel, up to an upper edge 25.
  • the superstructure 16 conventionally comprises, at its base, an intermediate layer 18 by which it rests on the metal structure, a side wall 26 resting on the intermediate layer and a vault 28. Burners, not shown, are arranged in the side wall 26. and operate alternately.
  • the intermediate layer 18 comprises, and preferably consists, of nose pieces 20 (“tuckstones” in English).
  • the superstructure parts are subjected to various thermomechanical stresses.
  • This thermal gradient causes a deformation of the material in proportion to its thermal expansion, and that therefore generates stresses (product of this deformation by the modulus of elasticity of the material).
  • These parts also undergo thermal shocks, due to operating accidents of the cooling or the furnace burner systems.
  • the superstructure parts must resist cracking despite very high thermomechanical stresses.
  • the superstructure must also resist corrosion by aggressive furnace vapors and condensate.
  • the superstructure is made of blocks made of a refractory product.
  • molten blocks most often include an intergranular vitreous phase connecting crystallized grains.
  • the problems posed by the sintered blocks and by the fused blocks, and the technical solutions adopted to solve them, are therefore generally different.
  • a composition developed to manufacture a sintered block is therefore not a priori usable as it is to manufacture a molten block, and vice versa.
  • the molten blocks are obtained by melting a mixture of suitable raw materials in an electric arc furnace or by any other suitable technique.
  • the molten material is then conventionally poured into a mold, then solidified.
  • the product obtained then undergoes a controlled cooling cycle to be brought to room temperature without fracturing. This operation is called "annealing" by those skilled in the art.
  • molten blocks with a very high zirconia (THTZ) content are known, which generally contain more than 80%, or even more than 85% by mass of zirconia. They are renowned for their very high resistance to corrosion and their ability not to color the glass produced and not to generate defects in the latter.
  • THTZ very high zirconia
  • EP 403 387 describes molten and cast products with a high zirconia content which contain, in percentages by mass, 4 to 5% of S1O2, approximately 1% of Al2O3, 0.3% of sodium oxide and less than 0.05% of P2O5.
  • FR 2 701 022 describes molten and cast products with a high zirconia content which contain, in weight percentages, 0.05 to 1.0% P2O5 and 0.05 to 1.0% boron oxide B2O3.
  • FR 2 723 583 describes melted and cast products with a high zirconia content which contain, in percentages by mass, 3 to 8% of S1O 2 , 0.1 to 2.0% of Al 2 O 3 , 0.05 to 3, 0% boron oxide B 2 O 3 , 0.05 to 3% BaO + SrO + MgO, 0.05 to 0.6% Na 2 Ü + K 0 and less than 0.3% Fe 2 Ü 3 + Ti0 2 .
  • Melted blocks with a very high zirconia content such as ER 1 195 produced and marketed by the company SEFPRO, are now widely used in glass furnaces. However, their high cost and their properties can limit their use, mainly concentrated on the blocks in contact with the glass, in particular in the most stressed areas of the tank.
  • the present invention aims to meet this need.
  • the invention provides a melted and cast refractory product comprising, in weight percentages based on the oxides and for a total of 100%:
  • a product according to the invention may also include one or more of the following optional features, including when it conforms to the particular embodiments described below and that these optional features are not incompatible with said particular embodiments:
  • the total porosity of the product is less than 10%, or even less than 5%;
  • the oxides represent more than 90%, more than 95%, more than 99%, or even substantially 100% of the mass of the product;
  • the mass content of ZrO ⁇ + HK% is less than 92.0%, or even less than 90.0%, or even less than 89.0% and / or greater than 83.0%, or even greater than 84.0% , or greater than 85.0%;
  • the mass content of S1O2 is greater than 8.4%, or even greater than 8.5%, or even greater than 8.6%, or even greater than 8.8%, or even greater than 9.1% and / or less than 1 1.5%, or even less than 1 1.0%, or even less than 10.8%, or even less than 10.6%;
  • the sum of the contents by mass of boron oxide B2O3, of sodium oxide Na2Ü and of potassium oxide K 0 is greater than 0.65%, or even greater than 0.70%, or even greater than 0.75% and / or less than 1, 20%, even less than 1, 10%, or even less than 1, 00%;
  • the content by mass of boron oxide B2O3 is greater than 0.25%, or even greater than 0.30%, or even greater than 0.35%, or even greater than 0.40% and / or less than 0.85%, less than 0.80%, less than 0.75%, less than 0.70%, less than 0.60%, or even less than 0.55%;
  • the sum of the mass contents of sodium oxide Na2Ü and potassium oxide K 0 is greater than 0.45% and / or less than 0.75%, less than 0.65%;
  • the mass content of Na2Ü is greater than 0.40%, or even greater than 0.45%, or even greater than 0.50% and / or less than 0.80%, or even less than 0.70%, or even less than 0.60%;
  • K2O is present as an impurity or partially replaces Na2Ü, and the mass content of K 0 is less than 0.70%, or even less than 0.60%, or even less than 0.50%, or even less than 0.40%, or even less than 0.30%;
  • the mass content of Al2O3 is less than 1.9%, or even less than 1.8%, or less than 1.7% and / or greater than 0.5%, or even greater than 0.6%, or even greater than 0.7%, or even greater than 0.9%, greater than 1.0%, or even greater than 1.1%, or even greater than 1.2%;
  • the mass content of Y2O3 is greater than 0.5%, or even greater than 0.7%, or even greater than 0.9%, or even greater than 1.0%, or even greater than 1.1%, and / or less at 1.9%, or even less than 1.8%, or even less than 1.7%, or even less than 1.6%;
  • the total mass content of the “other species” is less than 1.2%, or even less than 1.0%, or even less than 0.6%, or even less than 0.5%, or even less than 0.4%;
  • “other species” consist only of impurities; - The mass content of any “other species” is less than 0.40%, or even less than 0.30%, or even less than 0.20%;
  • the sum of the mass contents of calcium oxide CaO, barium oxide BaO, strontium oxide SrO and magnesium oxide MgO is less than 0.60%, less than 0.50%, less than 0.40% or even less than 0.30%;
  • the mass content of CaO is less than 0.60%, or even less than 0.40%, or even less than 0.30%;
  • the mass content of BaO is less than 0.60%, even less than 0.40%, or even less than 0.30%, less than 0.20%, less than 0.10%, less than 0.05% or substantially zero;
  • the mass content of SrO is less than 0.60%, or even less than 0.40%, or even less than 0.30%, less than 0.20%, less than 0.10%, less than 0.05% or substantially zero;
  • the mass content of MgO is less than 0.60%, or even less than 0.40%, or even less than 0.30%;
  • the mass content of Ta 2 0s is less than 0.20%, less than 0.10%, less than 0.05% or substantially zero;
  • the mass content of Nb 2 0s is less than 0.20%, less than 0.10%, less than 0.05% or substantially zero.
  • the invention provides a molten and cast refractory product comprising, in weight percentages based on the oxides:
  • the invention provides a molten and cast refractory product comprising, in weight percentages based on the oxides:
  • the invention provides a molten and cast refractory product comprising, in weight percentages based on the oxides:
  • AI2O3 1.1% to 1.8%.
  • the invention also relates to a process for manufacturing a refractory product according to the invention, comprising the following successive steps:
  • the oxides for which a minimum content is necessary, or precursors of these oxides are added systematically and methodically.
  • account is taken of the contents of these oxides in the sources of the other oxides where they are present as impurities.
  • the cooling is controlled, preferably so as to be carried out at a rate of less than 20 ° C per hour, preferably at the rate of about 10 ° C per hour.
  • the invention also relates to a glass melting furnace comprising a refractory product according to the invention, or a refractory product manufactured or likely to have been manufactured according to a process according to the invention, in particular in a region not intended to be in. contact with molten glass, in particular in the superstructure, in particular in the vault.
  • a product is conventionally said to be "molten" when it is obtained by a process involving a melting of a charge until a molten material is obtained, then a solidification of this material by cooling.
  • a block is an object all of whose dimensions are greater than 10 mm, preferably greater than 50 mm, preferably greater than 100 mm, and which, unlike a layer, is obtained by a process comprising molding operations and demoulding.
  • a block may for example have a general parallelepipedal shape or else a specific shape suitable for its use. Unless otherwise stated, all the oxide contents in a product according to the invention are percentages by weight on the basis of the oxides.
  • a mass content of an oxide of a metallic element relates to the total content of this element expressed in the form of the most stable oxide, according to the usual convention of the industry.
  • HfC> 2 is not chemically dissociable from ZrC> 2.
  • HfC> 2 is not intentionally added to the feed.
  • HfC> 2 therefore only designates traces of hafnium oxide, this oxide always being naturally present in sources of zirconium oxide at levels generally less than 5%, generally less than 2%.
  • the mass content of HfC> 2 is less than 5%, preferably less than 3%, preferably less than 2%.
  • the total content of zirconium oxide and of traces of hafnium oxide can be designated without distinction by “ZrC> 2” or by “ZrC> 2 + HfC> 2”.
  • HfC> 2 is therefore not included in "other species”.
  • impurities is understood to mean the inevitable constituents introduced with the raw materials or resulting from reactions with these constituents. Impurities are not necessary constituents, but only tolerated. For example, compounds belonging to the group of oxides, nitrides, oxynitrides, carbides, oxycarbons, carbonitrides and metallic species of iron, titanium, vanadium and chromium are impurities.
  • FIG. 1 diagrammatically represents a half-section. cross section of a glass melting furnace.
  • the high content of ZrC> 2 makes it possible to meet the requirements of high resistance to corrosion without generating defects detrimental to the quality of the glass.
  • the hafnium oxide, HfC> 2, present in the product according to the invention is hafnium oxide naturally present in sources of ZrC> 2. Its content in a product according to the invention is therefore less than 5%, generally less than 2%.
  • the presence of S1O2 allows in particular the formation of an intergranular vitreous phase capable of efficiently accommodating the deformations of the zirconia skeleton.
  • the addition of S1O2 must not exceed 12% because this addition is made to the detriment of the zirconia content and can therefore be detrimental to the corrosion resistance.
  • the presence of AC is particularly useful in the formation of a stable glass phase and in the good flowability of the molten material in the mold.
  • AI 03 should be limited because too high a mass content can lead to instability of the glass phase (formation of mullite crystals), particularly in the presence of boron oxide.
  • B2O3 has an adverse effect on the formation of zircon in the product, which may result in an adverse effect on the resistance to thermal cycling.
  • the content by mass of boron oxide B2C> 3 must therefore remain limited.
  • the mass content of Na 2 0 + K 0 is preferably limited in order to limit the flights of raw materials, in particular boron oxide.
  • the oxides Na2O and K0 are considered to have similar effects.
  • At least one of the Na2O and K0 contents is greater than 0.30%, preferably greater than 0.35%, preferably greater than 0.40%.
  • At least one of the Na2O and K0 contents being greater than 0.30%, preferably greater than 0.35%, preferably greater than 0.40%.
  • the mass content of yttrium oxide Y2O3 should be limited to maintain good feasibility.
  • the content by mass of Fe203 + T1O2 is less than 0.50%, preferably less than 0.30%.
  • the P2O5 mass content is less than 0.05%. Indeed, these oxides are harmful and their content must be limited to traces introduced as impurities with the raw materials.
  • the “other species” are the oxide species which are not listed above, namely the species other than ZrC> 2, Hf 0, S1O2, Y2O3, B2O3, AI2O3, Na20, K 0, T1O2 and Fe2C> 3.
  • the "other species” are limited to species whose presence is not not particularly desired and which are generally present as impurities in raw materials.
  • the product according to the invention is in the form of a block.
  • the total porosity of the product according to the invention is less than 15%, or even less than 10%, or even less than 5%, or even less than 2%, or even less than 1%.
  • a product according to the invention can be conventionally manufactured according to steps a. to c. described below:
  • step a. The raw materials are chosen so as to guarantee the oxide contents in the finished product.
  • step b. The melting is preferably carried out thanks to the combined action of a fairly long electric arc, which does not produce any reduction, and of stirring which promotes reoxidation of the products.
  • This process consists in using an electric arc furnace whose arc spurts out between the load and at least one electrode spaced from this load and in adjusting the length of the arc so that its reducing action is reduced to a minimum, while maintaining a oxidizing atmosphere above the molten bath and by stirring said bath, either by the action of the arc itself, or by bubbling an oxidizing gas (air or oxygen, for example) in the bath or even by adding in the bath of substances which give off oxygen, such as peroxides or nitrates.
  • an oxidizing gas air or oxygen, for example
  • step c. The cooling is preferably carried out at a rate of less than 20 ° C per hour, preferably at the rate of about 10 ° C per hour.
  • any conventional process for the manufacture of zirconia-based molten products intended for applications in glass melting furnaces can be carried out, provided that the composition of the starting charge makes it possible to obtain products having a composition in accordance with that of a product according to the invention.
  • ZrO ⁇ is substantially entirely (typically for more than 95% of its mass) in the form of zirconia and S1O2 and AI2O3 are substantially entirely (typically for more than 95% of their masses) in the vitreous phase .
  • the products were prepared according to the conventional arc furnace melting process, then cast to obtain blocks of format 996 mm x 203 mm x 800 mm.
  • MOR modulus of rupture
  • the fracture energy is measured at 1000 ° C, in air, on a sample of dimensions 150x25x25 mm 3 , and having in its middle a triangular notch of angle 60 ° and base 25 mm, placed in a bending assembly 4 points with a distance of 120 mm between the two lower supports and a distance of 40 mm between the two upper supports.
  • the lowering speed of the upper supports is equal to 20 pm / min.
  • Corrosion resistance is measured by spraying a powder consisting of 50% glass cullet, 15% silica, 5% dolomite, and 30% sodium carbonate, at the rate of 180 grams per hour for a total of 20 kilograms on 4 samples of dimensions 1 10x100x30 mm 3 rotated (6 revolutions per minute) in an oven at 1450 ° C.
  • the corroded volume is measured by 3D scanning and this volume is related to the initial volume.
  • the resistance to exudation is measured, in air, on a sample of dimensions 100x100x20 mm 3 .
  • the sample undergoes cycles during which it is brought to 1550 ° C. at a rate of 100 ° C. per hour and then maintained at 1550 ° C. for 6 hours.
  • REx is the percentage of the volume of the silicate phase which has escaped from the sample after two cycles (which is found either on the sample (increase in the volume of the sample) or at the bottom of the crucible), relative to to the initial volume of the sample. It is placed at 1550 ° C, which corresponds substantially to the temperature on the face of the block exposed towards the inside of the tank.
  • Examples 1 and 2 correspond respectively to a conventional AZS product and to a product with a conventional high zirconia content.
  • the remainder corresponds to the content of ZrC> 2 + HfC> 2 as well as to impurities (the content of which is always less than 0.5% in these examples).
  • the level of exudation of the products according to the invention is excellent.
  • the invention therefore provides a product which exhibits remarkable mechanical performance in the environment of a glass melting furnace superstructure, as well as low exudation in service.

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EP20705158.2A 2019-02-11 2020-02-11 Produit refractaire a haute teneur en zircone Pending EP3924319A1 (fr)

Applications Claiming Priority (2)

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FR1901334A FR3092579B1 (fr) 2019-02-11 2019-02-11 Produit refractaire a haute teneur en zircone
PCT/EP2020/053472 WO2020165170A1 (fr) 2019-02-11 2020-02-11 Produit refractaire a haute teneur en zircone

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EP (1) EP3924319A1 (zh)
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FR3121677A1 (fr) * 2021-04-07 2022-10-14 Saint-Gobain Centre De Recherches Et D'etudes Europeen Produit réfractaire à haute teneur en zircone

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FR75893E (fr) 1959-06-11 1961-08-18 Electro Refractaire Perfectionnements à la fabrication de produits réfractaires électrofondus contenant des oxydes minéraux
FR1208577A (fr) 1958-07-07 1960-02-24 Electro Refractaire Perfectionnements à la fabrication de produits réfractaires électrofondus contenant des oxydes minéraux
FR82310E (fr) 1962-04-07 1964-01-24 Electro Refractaire Perfectionnements à la fabrication de produits réfractaires électro-fondus contenant des oxydes minéraux
FR2648455B1 (fr) 1989-06-15 1993-04-23 Produits Refractaires Produits refractaires fondus et coules a forte teneur en zircone
FR2701022B1 (fr) 1993-02-03 1998-07-10 Asahi Glass Co Ltd Refractaires coules par fusion a forte teneur en zircone.
US5679612A (en) 1994-08-10 1997-10-21 Toshiba Monofrax Co., Ltd. High-zirconia fused refractories
EP1711445B1 (en) * 2004-01-02 2011-05-25 Refractory Intellectual Property GmbH & Co. KG Fusion - cast zirconia refractory with high electrical resistivity
FR2897862B1 (fr) * 2006-02-24 2008-05-09 Saint Gobain Ct Recherches Produit refractaire fondu et coule a forte teneur en zircone, presentant une resistivite electrique amelioree.
FR2897861B1 (fr) * 2006-02-24 2008-06-13 Saint Gobain Ct Recherches Refractaire a forte teneur en zircone a grande resistivite
KR101706397B1 (ko) * 2009-04-06 2017-02-13 아사히 가라스 가부시키가이샤 고지르코니아질 내화물 및 용융 가마
FR2953825B1 (fr) * 2009-12-16 2013-12-20 Saint Gobain Ct Recherches Produit refractaire a forte teneur en zircone.
FR2984878B1 (fr) * 2011-12-21 2014-02-28 Saint Gobain Ct Recherches Produit refractaire a forte teneur en zircone.
JP5749770B2 (ja) * 2013-08-21 2015-07-15 サンゴバン・ティーエム株式会社 高ジルコニア電気溶融鋳造耐火物
JP5763823B1 (ja) * 2014-10-07 2015-08-12 サンゴバン・ティーエム株式会社 高ジルコニア電気溶融鋳造耐火物

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WO2020165170A1 (fr) 2020-08-20
CN113454045A (zh) 2021-09-28
CN113454045B (zh) 2024-03-08
JP2022520068A (ja) 2022-03-28
FR3092579A1 (fr) 2020-08-14
US20220106213A1 (en) 2022-04-07
JP7274590B2 (ja) 2023-05-16

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