CN114249607A - Fused cast zirconia refractory product and preparation method and application thereof - Google Patents
Fused cast zirconia refractory product and preparation method and application thereof Download PDFInfo
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- 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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- C—CHEMISTRY; METALLURGY
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
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Abstract
The invention provides a fused cast zirconia refractory product and a preparation method and application thereof, the fused cast zirconia refractory product is a fused cast zirconia brick product of an impregnation solution A, and the fused cast zirconia brick product contains a glass phase, wherein the zirconium content is more than or equal to 88 percent or the zirconium content is more than or equal to 92 percent; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium nitrate, zirconium carbonate, ammonium zirconium carbonate or zirconium acetate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3:80-95, and the molar ratio of Si to zirconium is (5-10) to (90-95); adding nitric acid under stirring, and adjusting the pH value to 5-6 to obtain a solution A; wherein the concentration of the solution obtained by dissolving the ethyl silicate in the organic solvent and water is 0.001-0.05 mol/L. By infiltrating the solution comprising the zirconium salt, the exudation of the glass phase in the fused and cast zirconia product is reduced or prevented, while the performance of the fused and cast zirconia product as a refractory product is further improved.
Description
Technical Field
The invention relates to a zirconia refractory product, in particular to a fused cast zirconia refractory product, a preparation method and application thereof. The high-zirconium brick and the glass phase thereof have direct relation with the production of high-purity glass, the vaccine bottle is not closed too much, namely the vaccine bottle is not closed too much because the vitreous body exuded from the wall of the glass melting furnace enters the glass to form impurities, the quality of the zirconia refractory product is directly related to the quality of the vaccine bottle, and the improvement of the quality of the zirconia refractory product is urgent.
Background
The high-zirconium brick and the glass phase thereof have direct relation with the production of high-purity glass, the vaccine bottle is not closed too much, namely the vaccine bottle is not closed too much because the vitreous body exuded from the wall of the glass melting furnace enters the glass to form impurities, the quality of the zirconia refractory product is directly related to the quality of the vaccine bottle, and the improvement of the quality of the zirconia refractory product is urgent.
With zirconium oxide (ZrO)2) Refractory materials, which are the main component, exhibit excellent corrosion resistance to molten glass, and are therefore widely used in the inner wall portion that comes into contact with molten glass in a glass melting furnace. However, its structure is substantially composed of ZrO2High zirconia cast refractory material of crystalline (baddeleyite) with ZrO grown at around 1100 deg.C2The transformation of a crystal from monoclinic to tetragonal, which is characteristic of a crystal, causes abnormal volume expansion and shrinkage accompanying the transformation of the crystal, and particularly, a large-sized refractory material to be actually used has a problem that cracking is likely to occur. Production of ZrO containing 90 mass% or more2The following methods are known as a method for producing a refractory of (1): in the presence of buried ZrO2SiO between crystals2A component for softening the glass is added to a glass phase (hereinafter referred to as matrix glass) as a main component to adjust the viscosity of the glass phase, and ZrO is added to the glass phase2In the temperature range in which the crystallization changes, ZrO is absorbed by the softer matrix glass2Deformation caused by expansion and contraction of crystals. However, since a glass phase is formed, glass is likely to be formed when used in a glass melting furnaceThe glass phase components exude into the glass melting furnace, thereby contaminating the product.
Disclosure of Invention
In order to solve the above problems, the present invention provides a fused cast zirconia refractory product, a method of producing the same, and use thereof, which reduce or prevent the exudation of a glass phase in the fused cast zirconia product by infiltrating a solution containing a zirconium salt, while further improving the performance of the fused cast zirconia product as a refractory product.
The object of the invention is achieved in the following way: a fused cast zirconia refractory product is a fused cast zirconia brick product of an impregnation solution A, wherein the fused cast zirconia brick product contains a glass phase, and the zirconium content is more than or equal to 88 percent or the zirconium content is more than or equal to 92 percent; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium nitrate, zirconium carbonate, ammonium zirconium carbonate or zirconium acetate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3:80-95, and the molar ratio of Si to zirconium is (5-10) to (90-95); adding nitric acid under stirring, and adjusting the pH value to 5-6 to obtain a solution A; wherein the concentration of the solution obtained by dissolving the ethyl silicate in the organic solvent and water is 0.001-0.05 mol/L.
The thickness of the fused and cast zirconia product soaked by the solution A is more than or equal to 3 mm.
The thickness of the fused and cast zirconia product infiltrated by the solution A is 3mm-5 mm.
The fused cast zirconia brick product which is not dipped in the solution A is a fused cast zirconia brick.
The fused cast zirconia brick without being impregnated with the solution A is a high-resistance fused cast zirconia brick or a conventional fused cast zirconia brick. For example, because one part of the fused and cast zirconia product is soaked by the solution A, the rest part is not soaked by the solution A, and the fused and cast zirconia product of the non-soaked solution A contains 87 to 95 percent of zirconia, 3 to 11 percent of silicon oxide and Na according to weight percentage2O+Al2O3+TiO2+Fe2O3+K2O≤2%。
The preparation method of the fused cast zirconia refractory product comprises the following steps of (1) preparing a solution A; (2) and spraying the solution A on the fused and cast zirconia product which is not dipped with the solution A, and infiltrating the fused and cast zirconia product.
The preparation method of the fused and cast zirconia refractory product further comprises the following steps of (3) heating the infiltrated fused and cast zirconia product to 200 ℃ for 1-2h, then heating to 700 ℃ to 500 ℃ for calcination for 6-8 h to obtain the fused and cast zirconia refractory product.
And (3) building the fused and cast zirconia product without the solution A on a glass melting kiln, spraying the solution A on the exposed surface of the fused and cast zirconia product without the solution A to enable the solution A to soak the fused and cast zirconia product without the solution A, heating the glass melting kiln to 100-200 ℃ for 1-2h, then heating to 500-700 ℃ for calcination, and obtaining the fused and cast zirconia refractory product with the calcination time of 6-8 hours.
And (3) placing the fused and cast zirconia product without the solution A in a container, enabling the layer of the fused and cast zirconia product without the solution A to face upwards, spraying or pouring the solution A onto the fused and cast zirconia product without the solution A, infiltrating the fused and cast zirconia product without the solution A by the solution A, heating the fused and cast zirconia product in the container to 100-200 ℃ for 1-2h, heating to 500-700 ℃ for calcining, and calcining for 6-8 h.
Use of the fused cast zirconia refractory product.
Compared with the prior art, the fused cast zirconia refractory product, the preparation method and the application thereof reduce or prevent the exudation of the glass phase in the fused cast zirconia product by soaking the solution containing the zirconium salt, and further improve the performance of the fused cast zirconia product as the refractory product. The refractory product obtained by the method has the advantages of stronger temperature resistance, lower apparent porosity, stronger erosion resistance and lower expansion coefficient.
Detailed Description
A fused cast zirconia refractory product is a fused cast zirconia product of an impregnation solution A, wherein the fused cast zirconia product contains a glass phase, and the zirconium content is more than or equal to 88 percent or the zirconium content is more than or equal to 92 percent; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium nitrate, zirconium carbonate, ammonium zirconium carbonate or zirconium acetate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3:80-95, and the molar ratio of Si to zirconium is (5-10) to (90-95); adding nitric acid under stirring, and adjusting the pH value to 5-6 to obtain a solution A; wherein the concentration of the solution obtained by dissolving the ethyl silicate in the organic solvent and water is 0.001-0.05 mol/L.
The thickness of the fused and cast zirconia product soaked by the solution A is more than or equal to 8 mm. The thicker the solution a infiltrates the fused and cast zirconia product, the better, but since the thicker the cost is, it is preferable that the solution a infiltrates the fused and cast zirconia product with a thickness of 10mm to 20 mm.
The fused cast zirconia brick product which is not dipped in the solution A is a fused cast zirconia brick.
The fused cast zirconia brick without being impregnated with the solution A is a high-resistance fused cast zirconia brick or a conventional fused cast zirconia brick. Such as: because one part of the fused and cast zirconia product is soaked by the solution A and the rest part is not soaked by the solution A, in the fused and cast zirconia product of the non-soaked solution A, the zirconia content is 87-95 percent, the silica content is 3-11 percent and Na is calculated by weight percentage2O+Al2O3+TiO2+Fe2O3+K2O≤2%。
The preparation method of the fused cast zirconia refractory product comprises the following steps of (1) preparing a solution A; (2) and spraying the solution A on the fused and cast zirconia product which is not soaked with the solution A, and soaking the fused and cast zirconia product which is not soaked with the solution A. Since the fused cast zirconia refractory product is still to be built on the glass melting furnace finally, when the glass melting furnace is heated, the built fused cast zirconia refractory product can be correspondingly heated, so that the fused cast zirconia refractory product can be heated after the solution A is soaked, but not heated in advance, and the steps of building, spraying the solution A and soaking the solution A are also included.
The preparation method of the fused and cast zirconia refractory product further comprises the following steps of (3) heating the infiltrated fused and cast zirconia product to 200 ℃ for 1-2h, then heating to 700 ℃ to 500 ℃ for calcination for 6-8 h to obtain the fused and cast zirconia refractory product.
And (3) building the fused and cast zirconia product without the solution A on a glass melting kiln, spraying the solution A on the exposed surface of the fused and cast zirconia product to enable the solution A to soak the fused and cast zirconia product without the solution A, heating the glass melting kiln to 100-200 ℃ for 1-2h, then heating to 500-700 ℃ for calcining for 6-8 h to obtain the fused and cast zirconia refractory product.
And (3) placing the fused and cast zirconia product which is not dipped with the solution A in a container, enabling one layer of the fused and cast zirconia product which is not dipped with the solution A to face upwards, spraying or pouring the solution A onto the fused and cast zirconia product which is not dipped with the solution A, soaking the product with the solution A, heating the fused and cast zirconia product in the container to 100-200 ℃ for 1-2h, then heating to 500-700 ℃ for calcination, and calcining for 6-8 h.
Use of the fused cast zirconia refractory product.
Designing, modeling, proportioning, melting, forming, casting, preserving heat, taking out and processing the fused cast zirconia product before dipping the solution A. The fused cast zirconia product before the solution a is not impregnated may be a fused cast high zirconia brick.
(1) Designing: and (3) designing a casting high-zirconium brick model.
(2) Model: and (5) manufacturing a casting high-zirconium brick model.
(3) Preparing materials: weighing the required raw materials according to the weight part ratio requirements of zirconium oxide, hafnium oxide, silicon oxide and sodium oxide, accurately weighing, and uniformly stirring;
the raw material source can be one, two, three or four raw materials which meet the requirements, and the raw materials can be:
(a) desilicated zirconium
The producing area: anhui Anhuo zhongheng
The research and development and production of zirconia series products are specialized, and Australian high-quality raw ore zircon sand is selected as a raw material. The product has the characteristics of high grade, excellent quality, stable and uniform chemical composition and particle distribution, and can meet various process requirements of industries such as ceramics, electronics, aerospace, steel, refractory materials and the like. Wherein, the weight percentage of the zirconia is more than or equal to 98.90 percent.
(b) Zircon sand
The producing area: australia
The australian company, illuka, is the world's largest producer of zircon sand, accounting for 32% of the worldwide production of zirconium metal, about 35.2 million tons. Wherein, the weight percentage of the silicon oxide is more than or equal to 32.64 percent, and the weight percentage of the zirconium oxide is more than or equal to 66.48 percent.
(c) Alkali powder: hubei dicyclo; the weight percentage of the sodium oxide is more than or equal to 54 percent.
(d) High-zirconium brick clinker: waste material from Retiaceae practice group, Inc., Henan province; according to the weight percentage, the silicon oxide is more than or equal to 7.11 percent, the zirconium oxide is more than or equal to 91 percent, and the sodium oxide is more than or equal to 0.85 percent.
(4) Melting: fully stirring and mixing the raw materials, putting the mixture into a three-phase electric furnace, and heating the mixture to 2700-2900 ℃ for melting;
(5) and (3) grouping: and (3) putting the manufactured high-zirconium brick model into a heat preservation box, and filling proper heat preservation materials around the high-zirconium brick model.
(6) Casting: and (4) casting the molten feed liquid into the assembled high-zirconium brick model, and covering the upper part with a heat-insulating material.
(7) And (3) heat preservation: the heat preservation boxes are placed in a centralized manner and cooled naturally;
(8) taking out: after keeping the temperature for a certain number of days, taking the cast high-zirconium brick out of the heat preservation box to obtain a semi-finished product, and preparing for subsequent processing;
(9) processing: and (4) performing cold processing treatment such as cutting, grinding, drilling and the like on the semi-finished high-zirconium brick cooled to room temperature to finally obtain a finished high-zirconium brick.
The present invention is described in detail below with reference to specific embodiments, it should be noted that the embodiments are only used for further illustration of the present invention, and should not be construed as limiting the scope of the present invention, and those skilled in the art can make modifications and adaptations of the present invention based on the above-mentioned disclosure.
Comparative example 1:
inspecting samples: standard (A) 74X 57X 51 (mm), (B) 74X 57X 23 (mm), and (C) 74X 57X 30 (mm). The fused and cast zirconia product of the unimpregnated solution A was measured in weight percent (ZrO)2+HFO2) 94.92% of SiO23.82%, according to GB/T4984-2007.
Additionally the average properties were measured as: (1) the bulk density is 5.28g/cm3The detection is according to GB/T2997-2015; the apparent porosity is 0.2 percent, and the detection is according to GB/T2997-2015; the normal-temperature compressive strength is 919 Mpa, and the detection is according to GB/T5072-2008 (method 1);
(2) the exudation amount of the glass phase is 0.35 percent under the detection condition of 1500 ℃ multiplied by 4h, and the detection is according to JC/T493-2015 (2017) appendix B. Under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (liquid level line position) is 0.68, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is more than 1420 ℃, and the detection criterion is JC/T805-2013 (2017).
Specifically, the method comprises the following steps: sample a had the following properties: (1) the bulk density is 5.29g/cm3The apparent porosity is 0.2 percent, and the normal-temperature compressive strength is 1109 Mpa;
(2) the exudation amount of the glass phase is 0.37 percent under the detection condition of 1500 ℃ multiplied by 4h, and the detection is according to JC/T493-2015 (2017) appendix B. Under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (liquid level line position) is 0.70, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is more than 1420 ℃, and the detection criterion is JC/T805-2013 (2017).
Sample B had the following properties: (1) the bulk density is 5.27g/cm3The apparent porosity is 0.2 percent, and the normal-temperature compressive strength is 673 Mpa;
(2) the exudation amount of the glass phase is 0.33 percent under the detection condition of 1500 ℃ multiplied by 4h, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (liquid level line position) is 0.66, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is more than 1420 ℃, and the detection criterion is JC/T805-2013 (2017).
Sample C had the following properties: (1) the bulk density is 5.28g/cm3The apparent porosity is 0.2 percent, and the normal-temperature compressive strength is 976 Mpa;
(2) the exudation amount of the glass phase is 0.35 percent under the detection condition of 1500 ℃ multiplied by 4h, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistant speed (mm/24 h) (liquid level line position) is 0.72 and 0.64, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is more than 1420 ℃, and the detection criterion is JC/T805-2013 (2017).
Comparative example 2:
fused cast zirconia product not impregnated with solution a, found: in terms of weight percent, (ZrO)2+HFO2) 89.0% of SiO29.1% of Al in other amounts2O3+TiO2+Fe2O3+K2O+Na2O is 1.9%.
The average properties were measured as: (1) the bulk density is 5.0g/cm3The normal temperature compressive strength is more than or equal to 400 Mpa; the refractoriness under load (0.2 MPa) is more than 1700 ℃, the expansion coefficient (1000 ℃) is 0.65 percent, and the expansion coefficient (1500 ℃) is 0.10 percent;
(2) under the detection condition of 1500 ℃ for 4h, the average glass phase exudation amount is 0.48 percent, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (liquid level line position) is 0.86, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is more than 1350 ℃, and the detection criterion is JC/T805-2013 (2017).
Comparative example 3:
the fused cast zirconia product without impregnating solution a was measured by weight percent: (ZrO)2+HFO2) 93.5% of SiO24.8% of Al, and other contents2O3+TiO2+Fe2O3+K2O+Na2O is 1.7%.
The average properties were measured as: (1) the bulk density is 5.2g/cm3The normal temperature compressive strength is more than or equal to 400 Mpa,the refractoriness under load (0.2 MPa) is more than 1700 ℃, the expansion coefficient (1000 ℃) is 0.70 percent, and the expansion coefficient (1500 ℃) is 0.20 percent;
(2) under the detection condition of 1500 ℃ for 4h, the average glass phase exudation amount is 0.39 percent, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (liquid level line position) is 0.75, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is more than 1420 ℃, and the detection criterion is JC/T805-2013 (2017).
The main raw materials of comparative example 1 to comparative example 3 are desilicated zirconium, zircon sand, alkali powder and a small amount of fluxing agent. Production area of desilicated zirconium: the Anhui clam is characterized in that Australian high-quality raw ore zircon sand is used as a raw material, and the raw material is high in grade, excellent in quality, stable and uniform in chemical composition and particle distribution. Zircon sand, origin australia; alkali powder: hubei double rings.
The preparation method comprises the following steps: stirring and mixing the raw materials, and putting into an electric furnace; the model and the heat preservation material are reasonably distributed in the heat preservation box; melting by a three-phase electric arc furnace (the highest melting temperature is 2700-3000 ℃), and pouring into a model after the melting is finished; naturally cooling and preserving heat under the condition that the heat preservation material is used for preserving heat (the heat preservation time is 1-2 months); and demolding and cleaning the cooled and annealed semi-finished product, and processing into a brick body with a specified size and surface precision.
Example 1:
a fused cast zirconia refractory product is a fused cast zirconia product of an impregnating solution A, the fused cast zirconia product contains a glass phase, and the fused cast zirconia product A1 before the impregnating solution A is prepared in the same proportion and in the same batch with the sample in the comparative example 1; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium carbonate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3:80, and the molar ratio of Si to zirconium is 5: 90; (ii) a Adding nitric acid under the condition of stirring, and adjusting the pH value to 5 to obtain a solution A; wherein the concentration of the solution obtained by dissolving the ethyl silicate in the organic solvent and the water is 0.05 mol/L. The thickness of the fused and cast zirconia product infiltrated by the solution A is 8 mm.
A preparation method of a fused cast zirconia refractory product comprises the following steps of (1) preparing a solution A; (2) placing the fused and cast zirconia product A1 before the solution A is soaked in the solution A in a container, enabling one surface of the fused and cast zirconia product A1 to face upwards, spraying or pouring the solution A onto the fused and cast zirconia product A1, soaking the fused and cast zirconia product A1 in the solution A, heating the fused and cast zirconia product in the container to 100 ℃ for 2 hours, then heating to 500 ℃ for calcination, and calcining for 6 hours to obtain the fused and cast zirconia refractory product.
In order to determine the product properties, samples were taken from the part of the prepared refractory product that was impregnated with solution a, and samples were taken from the side that was impregnated with solution a, the average properties of the samples being in particular: (1) the average bulk density was 5.28g/cm3The apparent porosity is 0.11 percent, and the normal-temperature compressive strength is 928 Mpa;
(2) the exudation amount of the glass phase is 0.039% under the detection condition of 1500 ℃ multiplied by 4h, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (liquid level line position) is 0.089, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is 1900 ℃, and the detection criterion is JC/T805-2013 (2017). To facilitate comparison of performance effects, the performance and method of testing performance was the same as in comparative example 1.
Example 2:
a fused cast zirconia refractory product is a fused cast zirconia product of an impregnating solution A, the fused cast zirconia product contains a glass phase, and the fused cast zirconia product A2 before the impregnating solution A is not impregnated is prepared in the same proportion and in the same batch as that in the comparative example 1; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium nitrate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3: 95, and the molar ratio of Si to zirconium is 5: 95; adding nitric acid under the condition of stirring, adjusting the pH value to 6 to obtain a solution A, and dissolving ethyl silicate in an organic solvent and water to obtain a solution with the concentration of 0.001 mol/L; the thickness of the fused and cast zirconia product infiltrated by the solution A is 20 mm.
A preparation method of a fused cast zirconia refractory product comprises the following steps of (1) preparing a solution A; (2) and then spraying the solution A on a fused and cast zirconia product A2 which is not dipped in the solution A to soak the fused and cast zirconia product A2, heating the soaked fused and cast zirconia product A2 to 150 ℃ for 1.5 hours, heating to 700 ℃ and calcining for 6 hours to obtain the fused and cast zirconia refractory product.
In order to determine the properties of the product, samples were taken from the part of the prepared refractory product impregnated with solution a, and samples were taken from the side impregnated with solution a, the average properties being in particular: (1) the bulk density is 5.29g/cm3The apparent porosity is 0.09%, and the normal-temperature compressive strength is 985 Mpa;
(2) the exudation amount of the glass phase is 0.021% under the detection condition of 1500 ℃ for 4h, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (liquid level line position) is 0.060 according to the detection criterion of JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is 2020 ℃, and the detection result is JC/T805-2013 (2017). To facilitate comparison of performance effects, the performance and method of testing performance was the same as in comparative example 1.
Example 3
A fused cast zirconia refractory product is a fused cast zirconia product of an impregnating solution A, the fused cast zirconia brick product contains a glass phase, and the fused cast zirconia product A3 before the impregnating solution A is prepared in the same proportion and in the same batch with the sample in the comparative example 1; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding ammonium zirconium carbonate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3:92, and the molar ratio of Si to zirconium is 10: 95; adding nitric acid under stirring, adjusting pH to 5 to obtain solution A, and dissolving ethyl silicate in organic solvent and water to obtain solution with concentration of 0.04 mol/. The thickness of the fused and cast zirconia product infiltrated by the solution A is 10 mm.
A preparation method of a fused cast zirconia refractory product comprises the following steps of (1) preparing a solution A; (2) and building the fused cast zirconia product A3 before the solution A is not dipped in the solution A in the glass melting kiln to be used as the inner wall of the glass melting kiln, spraying the solution A on the fused cast zirconia product A3, infiltrating the fused cast zirconia product A3, heating the infiltrated fused cast zirconia product A3 to 100 ℃ for 1.5 hours, then heating to 500 ℃ for calcination, wherein the calcination time is 8 hours, and obtaining the fused cast zirconia refractory product used as the inner wall of the glass melting kiln.
In order to determine the properties of the product, samples were taken from the part of the prepared refractory product impregnated with solution a, and samples were taken from the side impregnated with solution a, the average properties being in particular: (1) the bulk density is 5.28g/cm3The apparent porosity is 0.11%, and the normal-temperature compressive strength is 976 Mpa;
(2) the exudation amount of the glass phase is 0.026% under 1500 ℃ and 4h detection conditions according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistant speed (mm/24 h) (liquid surface line position) is 0.068, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is 2050 ℃, and the detection criterion is JC/T805-2013 (2017). To facilitate comparison of performance effects, the performance and method of testing performance was the same as in comparative example 1.
Example 4
A fused cast zirconia refractory product is a fused cast zirconia product of an impregnating solution A, the fused cast zirconia brick product contains a glass phase, and the fused cast zirconia product A4 before the impregnating solution A is prepared in the same proportion and in the same batch with the sample in the comparative example 1; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium acetate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3:85, and the molar ratio of Si to zirconium is 10: 90; adding nitric acid under the condition of stirring, adjusting the pH value to 5-6 to obtain a solution A, and dissolving ethyl silicate in an organic solvent and water to obtain a solution with the concentration of 0.002 mol/L. The thickness of the fused and cast zirconia product infiltrated by the solution A is 6 mm.
A preparation method of a fused cast zirconia refractory product comprises the following steps of (1) preparing a solution A; (2) and then spraying the solution A on a fused and cast zirconia product A4 which is not dipped in the solution A to infiltrate the fused and cast zirconia product A4, heating the infiltrated fused and cast zirconia product A4 to 200 ℃ for 1 hour, heating to 700 ℃ for calcination for 8 hours, and thus obtaining the fused and cast zirconia refractory product.
In order to determine the properties of the product, samples were taken from the part of the prepared refractory product impregnated with solution a, and samples were taken from the side impregnated with solution a, the average properties being in particular: (1) the bulk density is 5.29g/cm3The apparent porosity is 0.09%, and the normal-temperature compressive strength is 926 MPa;
(2) the exudation amount of the glass phase is 0.053% under the detection condition of 1500 ℃ multiplied by 4h, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (at a liquid surface line) is 0.082, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is 1920 ℃, and the detection result is JC/T805-2013 (2017). To facilitate comparison of performance effects, the performance and method of testing performance was the same as in comparative example 1.
Example 5
A fused cast zirconia refractory product is a fused cast zirconia product of an impregnating solution A, the fused cast zirconia brick product contains a glass phase, and the fused cast zirconia product A5 before the impregnating solution A is prepared in the same proportion and in the same batch with the sample in the comparative example 1; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium nitrate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3:85, and the molar ratio of Si to zirconium is 7: 93; (2) adding nitric acid under stirring, adjusting pH to 5-6 to obtain solution A, and dissolving ethyl silicate in organic solvent and water to obtain solution with concentration of 0.02 mol/L. The thickness of the fused and cast zirconia product soaked by the solution A is 15 mm.
A preparation method of a fused cast zirconia refractory product comprises the following steps of (1) preparing a solution A; (2) and then spraying the solution A on a fused and cast zirconia product A5 which is not soaked in the solution A to soak the fused and cast zirconia product A5, heating the soaked fused and cast zirconia product A5 to 150 ℃ for 1.5 hours, heating to 550 ℃, and calcining for 7 hours to obtain the fused and cast zirconia refractory product.
In order to determine the properties of the product, samples were taken from the part of the prepared refractory product impregnated with solution a, and samples were taken from the side impregnated with solution a, the average properties being in particular: (1) the bulk density is 5.30g/cm3The apparent porosity is 0.09%, and the normal-temperature compressive strength is 932 MPa;
(2) the exudation amount of the glass phase is 0.023% under the detection condition of 1500 ℃ multiplied by 4h, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistant speed (mm/24 h) (liquid surface line position) is 0.064, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is 1980 ℃, and the detection criterion is JC/T805-2013 (2017). To facilitate comparison of performance effects, the performance and method of testing performance was the same as in comparative example 1.
Example 6:
a fused cast zirconia refractory product is a fused cast zirconia product of an impregnation solution A, the fused cast zirconia product comprises a glass phase, and the fused cast zirconia product D and a sample in a comparative example 2 are prepared in the same proportion and in the same batch; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium carbonate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3:80, and the molar ratio of Si to zirconium is 5: 90; (ii) a Adding nitric acid under the condition of stirring, and adjusting the pH value to 5 to obtain a solution A; wherein the concentration of the solution obtained by dissolving the ethyl silicate in the organic solvent and the water is 0.05 mol/L. The thickness of the fused and cast zirconia product infiltrated by the solution A is 8 mm.
A preparation method of a fused cast zirconia refractory product comprises the following steps of (1) preparing a solution A; (2) placing the fused and cast zirconia product D in a container, enabling one surface of the fused and cast zirconia product D to face upwards, spraying or pouring the solution A onto the fused and cast zirconia product D, infiltrating the fused and cast zirconia product D with the solution A, heating the fused and cast zirconia product in the container to 100 ℃ for 2 hours, then heating to 500 ℃, calcining for 6 hours, and obtaining the fused and cast zirconia refractory product.
In order to determine the properties of the product, samples were taken from the part of the prepared refractory product impregnated with solution a, and samples were taken from the side impregnated with solution a, the average properties being in particular: (1) the bulk density is 5.1g/cm3The normal temperature compressive strength is more than or equal to 400 Mpa, the refractoriness under load (0.2 Mpa) is more than 1700 ℃, the expansion coefficient (1000 ℃) is 0.58 percent, and the expansion coefficient (1500 ℃) is 0.09 percent;
(2) the exudation amount of the glass phase is 0.09% under the detection condition of 1500 ℃ multiplied by 4h, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (liquid level line position) is 0.11, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is 1500 ℃, and the detection criterion is JC/T805-2013 (2017). To facilitate comparison of performance effects, the performance and method of testing performance was the same as in comparative example 2.
Example 7:
a fused cast zirconia refractory product is a fused cast zirconia product of an impregnation solution A, the fused cast zirconia product comprises a glass phase, and the fused cast zirconia product E is prepared in the same proportion and in the same batch as the sample in the comparative example 3; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium nitrate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3: 95, and the molar ratio of Si to zirconium is 5: 95; adding nitric acid under the condition of stirring, adjusting the pH value to 6 to obtain a solution A, and dissolving ethyl silicate in an organic solvent and water to obtain a solution with the concentration of 0.001 mol/L; the thickness of the fused and cast zirconia product infiltrated by the solution A is 20 mm.
A preparation method of a fused cast zirconia refractory product comprises the following steps of (1) preparing a solution A; (2) and then spraying the solution A on the fused and cast zirconia product E, infiltrating the fused and cast zirconia product E, heating the infiltrated fused and cast zirconia product E to 150 ℃ for 1.5 hours, then heating to 700 ℃, and calcining for 6 hours to obtain the fused and cast zirconia refractory product.
In order to determine the properties of the product, samples were taken from the part of the prepared refractory product impregnated with solution a, and samples were taken from the side impregnated with solution a, the average properties being in particular: (1) the bulk density is 5.22g/cm3The normal temperature compressive strength is more than or equal to 400 Mpa, the refractoriness under load (0.2 Mpa) is more than 1700 ℃, the expansion coefficient (1000 ℃) is 0.67 percent, and the expansion coefficient (1500 ℃) is 0.16 percent;
(2) the exudation amount of the glass phase is 0.022% under the detection condition of 1500 ℃ multiplied by 4h, and the detection is according to JC/T493-2015 (2017) appendix B; under the detection condition of 1500 ℃ and 36h of common soda-lime glass, the static molten glass erosion resistance speed (mm/24 h) (liquid level line position) is 0.062, and the detection basis is JC/T806-2013 (2017); the glass phase exudation temperature (the detection condition is primary analysis) is 1990 ℃, and the detection result is JC/T805-2013 (2017). To facilitate comparison of performance effects, the performance and method of testing performance was the same as in comparative example 3.
While the preferred embodiments of the present invention have been described, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A fused cast zirconia refractory product characterized by: the fused cast zirconia brick product is a fused cast zirconia brick product of the dipping solution A, and the fused cast zirconia product contains a glass phase, wherein the zirconium content is more than or equal to 88 percent or the zirconium content is more than or equal to 92 percent; solution a contains a zirconium salt, solution a being the following: dissolving ethyl silicate in an organic solvent and water; adding zirconium nitrate, zirconium carbonate, ammonium zirconium carbonate or zirconium acetate, dissolving and uniformly stirring, wherein the volume ratio of the organic solvent to water is 3:80-95, and the molar ratio of Si to zirconium is (5-10) to (90-95); adding nitric acid under stirring, and adjusting the pH value to 5-6 to obtain a solution A; wherein the concentration of the solution obtained by dissolving the ethyl silicate in the organic solvent and water is 0.001-0.05 mol/L.
2. The fused-cast zirconia refractory product according to claim 1, characterized in that: the thickness of the fused and cast zirconia product soaked by the solution A is more than or equal to 8 mm.
3. The fused-cast zirconia refractory product according to claim 2, characterized in that: the thickness of the fused and cast zirconia product soaked by the solution A is 10mm-20 mm.
4. The fused-cast zirconia refractory product according to claim 1, characterized in that: the fused cast zirconia brick product which is not dipped in the solution A is a fused cast zirconia brick.
5. The fused-cast zirconia refractory product according to claim 2, characterized in that: according to the weight percentage, because one part of the fused and cast zirconia product is soaked by the solution A, the rest part is not soaked by the solution A, in the fused and cast zirconia product of the non-soaked solution A, according to the weight percentage, the zirconia content is 87-95 percent, the silica content is 3-11 percent, and Na2O+Al2O3+TiO2+Fe2O3+K2O≤2%。
6. The method for producing a fused-cast zirconia refractory product according to any one of claims 1 to 5, characterized in that: the method comprises the following steps of (1) preparing a solution A; (2) and spraying the solution A on the fused and cast zirconia product which is not dipped with the solution A, and infiltrating the fused and cast zirconia product.
7. The method of producing a fused-cast zirconia refractory product according to claim 6, characterized in that: the method further comprises the following steps of (3) heating the infiltrated fused and cast zirconia product to 100-200 ℃ for 1-2h, then heating to 500-700 ℃ for calcining for 6-8 h to obtain the fused and cast zirconia refractory product.
8. The method of producing a fused-cast zirconia refractory product according to claim 7, characterized in that: and (3) building the fused and cast zirconia product without the solution A on a glass melting kiln, spraying the solution A on the exposed surface of the fused and cast zirconia product without the solution A to enable the solution A to soak the fused and cast zirconia product without the solution A, heating the glass melting kiln to 100-200 ℃ for 1-2h, then heating to 500-700 ℃ for calcination, and obtaining the fused and cast zirconia refractory product with the calcination time of 6-8 hours.
9. The method of producing a fused-cast zirconia refractory product according to claim 7, characterized in that: and (3) placing the fused and cast zirconia product without the solution A in a container, enabling the layer of the fused and cast zirconia product without the solution A to face upwards, spraying or pouring the solution A onto the fused and cast zirconia product without the solution A, infiltrating the fused and cast zirconia product without the solution A by the solution A, heating the fused and cast zirconia product in the container to 100-200 ℃ for 1-2h, heating to 500-700 ℃ for calcining, and calcining for 6-8 h.
10. Use of a fused-cast zirconia refractory product according to any one of claims 1 to 9.
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