WO2013102288A1 - Brique de fond de bain en étain, aluminium, calcium et silicium et son procédé de préparation - Google Patents

Brique de fond de bain en étain, aluminium, calcium et silicium et son procédé de préparation Download PDF

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WO2013102288A1
WO2013102288A1 PCT/CN2012/001713 CN2012001713W WO2013102288A1 WO 2013102288 A1 WO2013102288 A1 WO 2013102288A1 CN 2012001713 W CN2012001713 W CN 2012001713W WO 2013102288 A1 WO2013102288 A1 WO 2013102288A1
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calcium
aluminum
tin
fine powder
siliceous
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PCT/CN2012/001713
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English (en)
Chinese (zh)
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张启山
张瑛
车建壮
李志军
孙文礼
刘杰
冯延春
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淄博工陶耐火材料有限公司
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Publication of WO2013102288A1 publication Critical patent/WO2013102288A1/fr

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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
    • C04B35/44—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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B18/00—Shaping glass in contact with the surface of a liquid
    • C03B18/02—Forming sheets
    • C03B18/16—Construction of the float tank; Use of material for the float tank; Coating or protection of the tank wall
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
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    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5463—Particle size distributions
    • C04B2235/5472—Bimodal, multi-modal or multi-fraction
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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    • C04B2235/725—Metal content
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

Definitions

  • the invention relates to a tin trough bottom brick and a preparation method thereof, and belongs to the technical field of refractory materials.
  • the tin bath is the key equipment of the float flat glass production line.
  • the molten glass flows into the tin bath, floats on the tin liquid, and forms a smooth plate glass while advancing.
  • the refractory brick used to store the tin liquid is called the tin bath. Bottom brick.
  • Most of the silica fume clay bricks currently used on the market are in the process of use, because N 3 ⁇ 4 0 contained in the glass slowly penetrates into the brick through the tin liquid, forming nepheline and producing volume expansion and thermal stress.
  • the metamorphic layer containing nepheline is increased to a certain thickness, the metamorphic layer will peel off in a sheet form. Since the specific gravity is lower than that of the tin liquid, when the exfoliated pieces float on the tin liquid surface, the glass surface is scratched and the glass defect is caused.
  • the mass percentage of SiO 2 and FeA in the raw material should be less than 1.5%, respectively.
  • the content of 3 is preferably only a small amount.
  • the disadvantage of this brick is that the coarse particles and the fine particles are combined by hydrate. After heat treatment at 1100 °C, the calcium aluminate binding phase still contains a small amount of bound water. During the use of temperature above 1100 °, the combined water will also Overflow, the porosity of the product will increase, which will lead to the risk of use. Summary of the invention
  • An object of the present invention is to provide an aluminum-calcium-silicate tin-slot bottom brick having a low porosity and a high porosity, which has good alkali metal oxide corrosion resistance, low thermal expansion coefficient, low thermal conductivity, and low hydrogen diffusion rate.
  • the invention also provides a reasonably easy preparation method.
  • the aluminum-calcium-silica tin-slot bottom brick (hereinafter referred to as the tin-slot bottom brick) of the present invention has a chemical composition mass percentage including ⁇ 1 66-80%, CaO 17-28%, SiO, 0.5-5%.
  • the impurities in the raw materials exist as the balance, and may contain common mineral impurities such as MgO, N3 ⁇ 40, K-.0, and the like.
  • the preferred chemical composition of the tin bath bottom brick is as follows:
  • the content of ⁇ 1 ⁇ is preferably 67% by mass or more, and more preferably 68% by mass or more. On the other hand, the content is below 79% by mass: ⁇ ', preferably less than 76% by mass.
  • the CaO content of the tin-slot bottom brick is preferably 18% by mass or more, and more preferably 21% by mass or more.
  • the CaO content is preferably 26% by mass or less, and preferably 25% by mass or less.
  • the 5% or more of the mass percentage of the SiO 2 is preferably 1% or more by mass.
  • the content of SiO 2 is preferably 9% or less by mass%, and preferably 7% or less by mass.
  • the MgO content of the tin bath bottom brick is preferably 2.5% or less by mass%, preferably 2.3% or less by mass%, and preferably 2.5% by mass or less.
  • the N3 ⁇ 40 content of the tin-sand brick is preferably less than 1% by mass, preferably less than 0.7% by mass, and preferably less than 0.5% by mass.
  • This tin bottom bricks K 2 0 content of 1% or less in mass percent preferably, in mass percentage is preferably 0.8% or less, a percentage of 0.6% or less is preferred in terms of quality.
  • the 3% or less is preferred, and the mass percentage of 0.4% or less is preferred, and the mass percentage of 0.5% or less is preferred, and the total content of the FeA+Ti0 2 is preferably 0.5% or less.
  • the XRD mineral crystal phase composition of the product is identified as calcium dialuminate, calcium hexaaluminate and calcium aluminum feldspar, which is identified as calcium laurate accounted for 70-90% and calcium aluminum feldspar accounted for 1-25%. It was identified as calcium laurate accounted for 70-90%, calcium hexaaluminate accounted for less than 10%, and feldspar feldspar accounted for 1-25%.
  • the XRD mineral phase was measured by an X-ray diffraction apparatus using Cu-K of rays.
  • the percentages of calcium laurate, calcium hexaaluminate and calcium aluminum feldspar are calculated as follows:
  • ⁇ C42 represents the percentage of calcium laurate in the sample
  • ⁇ C46 represents the percentage of calcium hexaaluminate in the sample
  • ⁇ ?£7 represents the percentage of calcium aluminum feldspar in the sample -
  • J ⁇ s is the calcium diammonate standard substance and the internal standard substance quartz (S). After mixing with a mass ratio of 1:1, the peak intensity of calcium diammonate I (-311) and the internal standard substance of quartz 1 (011) The ratio of peak intensities; S is the calcium hexaaluminate I (114) after mixing the standard material of calcium hexaaluminate with the internal standard substance quartz (S) at a mass ratio of 1:1.
  • the ratio of the 1 (011) peak intensity of the peak material quartz Is the ratio of the peak intensity of the calcium aragonite 1 (211) peak to the 1 (011) peak intensity of the internal standard quartz after mixing with the internal standard material quartz (s) at a mass ratio of 1:1;
  • the internal standard substance quartz (s) is mixed with a mass ratio of 1:1, and the peak intensity of the calcium laurate I (-311) is determined;
  • Igeh is the peak intensity of the calcium aluminum feldspar ⁇ (2 ⁇ ⁇ ) measured after the sample and the internal standard substance quartz (s) are mixed at a mass ratio of 1:1;
  • the porosity of the tin bottom brick is 14-28%. From the viewpoint of pressure resistance and the like, the porosity is preferably 26% or less, and the porosity is 24% or less. In terms of productivity, the porosity is above 16% and the productivity is better, and the porosity is above 18%. In addition, the porosity is calculated by the Archimedean method.
  • the compressive strength of the tin-slot bottom brick is preferably 50 MPa or more, and more preferably 55 MPa or more.
  • the granules of the calcium aluminate having a particle size of 3 to 1 and having a particle diameter of 1 to 0.1.
  • the calcium silicate particles of the calcium silicate are 20 to 35% and the particle diameter is less than 0. 088.
  • the raw material is prepared by a production process of compounding, mixing, molding, and high-temperature firing, and is characterized in that the raw material (weight percentage) comprises: 30-45% of coarse calcium aluminate particles having a particle diameter of 3-1, and a particle diameter of 1 -0. lmm calcium aluminate particles 20-35%, and particle size less than 0. 088 hidden combined fine powder 25-40%. Further, in the present specification, the particle size is determined by a conventional sieve.
  • the porosity of the calcium aluminate raw material is less than 3%
  • the mass percentage of the chemical composition comprises: ⁇ 1 ⁇ 73-79%, CaO 21-27%, 0. 10% or less of FeA, and the balance may include Ti0 2
  • the content of MgO, K 2 O, and Na 2 0 is preferably 1% by mass or less, and more preferably 0.1% by mass or less.
  • the combined fine powder is preferably a mixture comprising a fine powder of calcium aluminate and a fine powder of ⁇ -alumina or a fine powder of a siliceous compound, and is combined with fine powder from the viewpoint of the compressive strength of the tin-bottomed brick.
  • the mixture of the three fine powders is: 0:.
  • the combined fine powder is composed of the above three kinds of fine powders, it is preferable to add a silicon compound fine powder of 0.5 to 5% by mass of the chemical composition of the mixture, and at the same time, according to the mixture of Si0 2 The mass percentage is 0.8-1.
  • ⁇ alumina powder 4 times the addition of ⁇ alumina powder, and the rest is the fine powder of calcium aluminate is preferred.
  • at least one of clay, quartz, diopside and wollastonite is used in combination with the siliceous compound in the fine powder.
  • the green body is formed by isostatic pressing, and the molding pressure of the isostatic pressing is preferably set to 50-200 MPa.
  • a general press Prior to isostatic pressing, a general press can be used for preforming as needed.
  • the manufacturing method of the tin-slot bottom brick since the molding method is not cast molding (including vibration casting molding), it is not necessary to maintain the cast-formed body in a humid environment, which is advantageous for improving productivity.
  • the method for manufacturing the tin-slot bottom brick has the advantages of high product homogeneity and less crack defects in the product because of the isostatic pressing method.
  • the green body is dried and then fired in a kiln.
  • the drying method is not particularly limited, and it is naturally dried, or dried using a drying device. In the case of natural drying, it usually takes several days. Specifically, it can be chosen for 1-3 days.
  • Conditions such as natural drying are preferred.
  • the sintering temperature is preferably 1250-150 CTC, preferably 1270-1470 ° C, and 1300-1450 ° C is preferred.
  • the holding time of the sintering temperature is preferably in 5-50 hours, preferably in 7-45 hours, and preferred in 10-40 hours.
  • the heating rate is preferably 0.1 ° C / hr - 10 Torr / hour, and preferably 0.5 ° C / hr - 5 ° C / hour. Cooling can be performed by natural cooling or by cooling at a certain cooling rate.
  • An example of a preferred firing temperature regime is as follows:
  • the ceasefire cools down and cools naturally.
  • the present invention has the following beneficial effects:
  • the invention adopts dense calcium aluminate as coarse particles and fine particles, and adds ⁇ -alumina powder and siliceous compound powder as a binder, and is formed by isostatic pressing and firing to form calcium aluminate, calcium aluminum yellow feldspar, Calcium hexaaluminate is the main mineral phase product.
  • the product is free of hydrates, has no internal cracking, uniform structure, good resistance to tin liquid penetration, alkali metal oxide corrosion resistance, low thermal expansion rate, low thermal conductivity, low hydrogen diffusion rate, and solves the problem of clay-based tin trough bottom brick.
  • nepheline by the erosion of alkali metal oxides causes the problem of expansion and peeling of the brick body, can improve the service life of the tin tank bottom brick, and can reduce the glass defects generated by the tin tank bottom brick and the heat loss at the bottom of the tin tank.
  • the physical and chemical indexes of raw materials such as calcium aluminate particles, ⁇ -alumina powder, and siliceous compound powder are as follows.
  • Table 1 the raw materials are added to the kneader in the proportions indicated in Table 2, and after mixing for 5-15 minutes, Isostatic pressing under pressure of 50-200Mpa After the specification is dried, the body is naturally dried for 1-3 days, and then a sample of aluminum-calcium-silica tin-slot bottom brick is prepared by firing at 1300 ⁇ - 50 'C, and its chemical composition, mineral phase composition, porosity, bulk density and compressive strength are measured. Physical and chemical properties such as thermal conductivity are shown in Table 2 of the specific examples. Table] Quality Chemical Percent Composition Table of Raw Materials

Abstract

La présente invention concerne une brique de fond de bain en étain et un procédé de préparation de celle-ci, la brique de fond de bain en étain étant constituée, en pourcentage en poids, de 66 % à 80 % de Al2O3, de 17 % à 28 % de CaO, de 1,5 % à 5 % de SiO2, le reste étant des impuretés minérales communes. La méthode consiste en une formulation, en un pressage isostatique et en une cuisson à haute température, les pourcentages en poids de la formulation étant de 30 % à 45 % de particules grossières d'aluminate de calcium avec une taille de particule de 3 mm à 1 mm, de 20 % à 35 % de particules moyennes d'aluminate de calcium avec une taille de particule de 1 mm à 0,1 mm, et de 25 % à 40 % de poudre fine de calcium de liaison avec une taille de particule inférieure à 0,088 mm. Le produit présente une bonne résistance à la corrosion à des oxydes de métal alcalin, une faible dilatation thermique, une faible conductivité thermique et un faible taux de diffusion d'hydrogène.
PCT/CN2012/001713 2012-01-06 2012-12-21 Brique de fond de bain en étain, aluminium, calcium et silicium et son procédé de préparation WO2013102288A1 (fr)

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CN102557688B (zh) * 2012-01-06 2013-08-14 淄博工陶耐火材料有限公司 等静压铝钙硅质锡槽底砖的制备方法
CN104909542B (zh) * 2015-05-09 2017-09-22 浙江瑞泰耐火材料科技有限公司 一种锡槽底砖
CN104914020A (zh) * 2015-05-09 2015-09-16 浙江瑞泰耐火材料科技有限公司 锡槽底砖氢扩散度检测装置
CN106518043B (zh) * 2016-11-17 2019-05-14 淄博工陶耐火材料有限公司 低成本铝钙硅质锡槽底砖的制备方法
CN107892579B (zh) * 2017-11-23 2020-10-09 淄博工陶新材料集团有限公司 铝酸钙质玻璃窑炉锡槽吊顶砖及其制备方法
CN116751068B (zh) * 2023-08-18 2023-10-31 山东淄博沈淄耐火材料有限公司 等静压成型铝酸钙锡槽底砖的制备方法

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