CN116143531A - Method for preparing unshaped refractory material by utilizing vanadium-aluminum slag and application - Google Patents
Method for preparing unshaped refractory material by utilizing vanadium-aluminum slag and application Download PDFInfo
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- CN116143531A CN116143531A CN202310183832.0A CN202310183832A CN116143531A CN 116143531 A CN116143531 A CN 116143531A CN 202310183832 A CN202310183832 A CN 202310183832A CN 116143531 A CN116143531 A CN 116143531A
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- vanadium
- aluminum slag
- unshaped refractory
- slag powder
- aluminum
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- 239000002893 slag Substances 0.000 title claims abstract description 141
- PTXMVOUNAHFTFC-UHFFFAOYSA-N alumane;vanadium Chemical compound [AlH3].[V] PTXMVOUNAHFTFC-UHFFFAOYSA-N 0.000 title claims abstract description 131
- 238000000034 method Methods 0.000 title claims abstract description 49
- 239000011819 refractory material Substances 0.000 title claims abstract description 43
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 73
- 239000000203 mixture Substances 0.000 claims description 38
- 239000002245 particle Substances 0.000 claims description 32
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 17
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 14
- 229910052720 vanadium Inorganic materials 0.000 claims description 13
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 13
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 12
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 12
- 239000000292 calcium oxide Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 229910052925 anhydrite Inorganic materials 0.000 claims description 5
- ZOMBKNNSYQHRCA-UHFFFAOYSA-J calcium sulfate hemihydrate Chemical compound O.[Ca+2].[Ca+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZOMBKNNSYQHRCA-UHFFFAOYSA-J 0.000 claims description 5
- 229910052602 gypsum Inorganic materials 0.000 claims description 5
- 239000010440 gypsum Substances 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 12
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 9
- 239000006227 byproduct Substances 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 5
- 239000002910 solid waste Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000003723 Smelting Methods 0.000 abstract description 3
- 238000009825 accumulation Methods 0.000 abstract description 2
- 239000004411 aluminium Substances 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000007767 bonding agent Substances 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910026551 ZrC Inorganic materials 0.000 description 1
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/131—Inorganic additives
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1328—Waste materials; Refuse; Residues without additional clay
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/138—Waste materials; Refuse; Residues from metallurgical processes, e.g. slag, furnace dust, galvanic waste
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D1/00—Casings; Linings; Walls; Roofs
- F27D1/0003—Linings or walls
- F27D1/0006—Linings or walls formed from bricks or layers with a particular composition or specific characteristics
-
- 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
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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- 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
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Dispersion Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
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- General Engineering & Computer Science (AREA)
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Abstract
The invention provides a method for preparing an unshaped refractory material by utilizing vanadium-aluminum slag and application thereof. The method comprises the following steps: taking vanadium-aluminum slag as a raw material, and sequentially crushing, blending, calcining, grinding and mixing to obtain the unshaped refractory material. According to the invention, by taking the vanadium-aluminum alloy smelting byproducts as raw materials, the vanadium-aluminum slag is fully utilized, solid waste accumulation is prevented, resource recycling is realized, the process flow is short, the operation is simple, the safety coefficient is high, more than 85% of the used materials are waste materials generated in the vanadium-aluminum alloy production process, and the prepared unshaped refractory material has good refractory performance and high hardening strength and can be used in various production environments.
Description
Technical Field
The invention belongs to the technical field of refractory materials, relates to a method for preparing a refractory material based on industrial byproducts, and particularly relates to a method for preparing an unshaped refractory material by utilizing vanadium-aluminum slag and application of the unshaped refractory material.
Background
The refractory material is inorganic nonmetallic material with the refractoriness of more than 1580 ℃, and comprises natural ore and various products prepared by a certain process according to a certain purpose and requirement, has certain temperature mechanical property and good volume stability, and is a material necessary for various high-temperature equipment. The refractory material is applied to various fields of national economy such as steel, nonferrous metal, glass, cement, ceramics, petrifaction, machinery, boilers, light industry, electric power, military industry and the like, is an essential basic material for ensuring the industrial production operation and the technical development, and plays an irreplaceable important role in the development of high-temperature industrial production.
The aluminothermic reduction method is one of the most common processes for producing vanadium-aluminum alloy, when preparing the vanadium-aluminum alloy through aluminothermic reduction reaction, a large amount of byproduct alumina is generated, in the production process, in order to reduce the viscosity and melting point of slag liquid and obtain good separation effect of the vanadium-aluminum alloy and slag, a certain proportion of calcium fluoride is usually added into raw materials, and finally the obtained alumina slag usually contains a certain proportion of calcium fluoride. In the actual production process, the mass ratio of the vanadium-aluminum alloy to the slag is about 1:1, and the produced slag is not effectively utilized except for a small part of the slag which is used for filling the thermit reduction reaction furnace body and the rest of the slag is not effectively utilized, so that the economic benefit is seriously influenced.
CN 107287450a discloses a method for efficiently utilizing vanadium-aluminum slag, which comprises: crushing and grinding the vanadium-aluminum slag to obtain powdery vanadium-aluminum slag; dissolving the obtained powdery vanadium-aluminum slag in sulfuric acid solution, filtering to obtain liquid-phase aluminum sulfate solution and solid-phase slag, wherein the aluminum sulfate solution is used for purifying vanadium liquid in the wet vanadium extraction process, and the solid-phase slag is used for knotting refractory lining raw materials of a furnace body. The method can effectively extract aluminum in the vanadium-aluminum slag, realizes the recycling of the vanadium-aluminum slag, but adopts a wet process to pollute seriously, and the residual slag has no cohesiveness, and requires additional addition of a binder when in use.
CN 111247112a discloses a binder based on aluminum-rich slag, which can effectively utilize the aluminum-rich slag, but the addition of the binder such as portland cement during the preparation process severely reduces the refractoriness of mortar, and fails to fully exert the value of the aluminum-rich slag.
CN 114671672a discloses a formulation of unshaped refractory and a preparation method thereof, the formulation of unshaped refractory comprises aggregate and binding agent, the aggregate comprises, by mass, 20-35 parts of bauxite, 10-30 parts of magnesia-alumina spinel, 10-15 parts of silicon oxide, 5-20 parts of zirconium carbide and 38 parts of semisteel jade: the bonding agent comprises 12-26 parts of organic bonding agent, wherein the organic bonding agent adopts random polypropylene or adopts one or more of phenolic resin and absolute ethyl alcohol. According to the formula, the raw materials adopted by the patent for preparing the unshaped refractory material are aggregate and a binding agent, and are not materials such as slag and the like which can be reused.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing an unshaped refractory material by utilizing vanadium-aluminum slag. The method realizes the high-efficiency utilization of the vanadium-aluminum slag.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing an unshaped refractory material from vanadium aluminium slag, the method comprising: taking vanadium-aluminum slag as a raw material, and sequentially crushing, blending, calcining, grinding and mixing to obtain the unshaped refractory material.
According to the invention, the vanadium-aluminum slag is used as a raw material for preparing the refractory material, so that the vanadium-aluminum slag is fully utilized, solid waste is prevented from accumulating, and the recycling of resources is realized. The preparation method has the advantages of short process flow, simple operation and high safety coefficient, more than 85% of the used materials are waste generated in the production process of the vanadium-aluminum alloy, and the prepared unshaped refractory material has good refractory property and high hardening strength and can be used in various production environments.
In a preferred embodiment of the present invention, the refractoriness of the unshaped refractory is 1600 to 1800 ℃, for example, 1600 ℃, 1650 ℃, 1700 ℃, 1750 ℃, or 1800 ℃, but the unshaped refractoriness is not limited to the recited values, and other unshaped values within the numerical range are equally applicable.
The amorphous refractory preferably has a load softening temperature of 1200 to 1450 ℃, for example, 1200 ℃, 1250 ℃, 1300 ℃,1350 ℃,1400 ℃, or 1450 ℃, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
The compressive strength of the unshaped refractory is preferably 73.2 to 78.5MPa, and may be 73.2MPa, 74MPa, 75MPa, 76MPa, 77MPa or 78.5MPa, for example, but not limited to the values recited, and other values not recited in the numerical range are equally applicable.
The rate of change of the burn line of the unshaped refractory is preferably 0.4 to 0.6%, and may be, for example, 0.4%, 0.45%, 0.5%, 0.55%, or 0.6%, but not limited to the values recited, and other values not recited in the numerical range are equally applicable.
Preferably, the method comprises the steps of:
(1) Crushing the vanadium-aluminum slag to obtain vanadium-aluminum slag powder;
(2) Mixing calcium oxide, calcium fluoride and vanadium-aluminum slag powder obtained in the step (1), and calcining to obtain a first mixture;
(3) Mixing retarder and the first mixture obtained in the step (2), and grinding to obtain a second mixture;
(4) Mixing the second mixture, vanadium-aluminum slag powder and water to obtain an unshaped refractory material;
and (4) obtaining the unshaped refractory materials in different service environments by adjusting the mixing proportion and/or the particle size of the vanadium-aluminum slag powder.
The reason that the unshaped refractory materials with different performances can be obtained by adjusting the addition amount and/or the granularity of the vanadium-aluminum slag powder is as follows: the main component of the vanadium-aluminum slag is aluminum oxide, the melting point of the aluminum oxide is above 2000 ℃, the refractoriness of the unshaped refractory material is increased along with the increase of the vanadium-aluminum slag powder, the unshaped refractory materials with different internal structures can be obtained by adjusting the granularity of the vanadium-aluminum slag, different mechanical properties are shown, and the unshaped refractory material is suitable for different service environments.
Preferably, the average particle size of the vanadium aluminum slag powder in the step (1) is 1 to 10mm, for example, 1mm, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm or 10mm, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The average granularity of the vanadium-aluminum slag powder is 1-10 mm, and excessive granularity can cause excessive porosity of the prepared unshaped refractory material, poor mechanical property and excessively low porosity and poor thermal shock resistance.
Preferably, the vanadium-aluminum slag of the step (1) comprises, in mass percent: calcium fluoride < 20wt%, iron < 1wt%, vanadium < 1wt%, si < 1.5wt%, alumina balance and unavoidable impurities.
Preferably, the mass ratio of the calcium oxide, calcium fluoride and vanadium aluminum slag powder in the step (2) is (2-3): (0-1): (21-26), for example, may be 2:1:21, 2:0:21, 3:0.1:21, 3:1:21, 2:1:26, 3:1:26 or 2.5:0.5:24, but is not limited to the recited values, and other non-recited values in the range of values are equally applicable.
The purpose of adding calcium oxide and calcium fluoride in the method is to adjust the components of the vanadium-aluminum slag and enhance the hydraulicity of the calcined vanadium-aluminum slag.
Preferably, the purity of the calcium oxide is not less than 97%, for example, 97%, 97.5%, 98%, 98.5%, 99% or 99.5%, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
Preferably, the purity of the calcium fluoride is greater than or equal to 98%, for example 98%, 98.5%, 99% or 99.5%, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the temperature of the calcination in the step (2) is 1200 to 1400 ℃, for example, 1200 ℃, 1250 ℃, 1300 ℃,1350 ℃ or 1400 ℃, but the calcination is not limited to the listed values, and other values not listed in the numerical range are equally applicable.
Preferably, the calcination time in step (2) is 20-30 min, for example, 20min, 22min, 24min, 26min, 28min or 30min, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
The invention leads particles to be bonded among powders through calcination, and recrystallization occurs, and too high calcination temperature can lead to serious burning loss, and too low calcination temperature can lead to incomplete reaction, thereby reducing hydraulic property.
Preferably, the mass ratio of retarder to first mixture in step (3) is (2-9): 100, which may be, for example, 2:100, 3:100, 4:100, 5:100, 6:100, 7:100, 8:100 or 9:100, but is not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the retarder of step (3) comprises any one or a combination of at least two of calcium sulfate hemihydrate, gypsum or anhydrite, typically but not limited to a combination of calcium sulfate hemihydrate and gypsum, a combination of gypsum and anhydrite, a combination of calcium sulfate hemihydrate and anhydrite, or a combination of calcium sulfate hemihydrate, gypsum and anhydrite.
The retarder has the functions of prolonging the setting time, improving the workability of the unshaped refractory material and effectively improving the application range of the unshaped refractory material.
Preferably, the second mixture of step (3) has an average particle size of 60 to 90 μm, for example 60 μm, 70 μm, 80 μm or 90 μm, but not limited to the values recited, other values not recited in the range of values being equally applicable.
The invention aims to better adapt to different construction environments by limiting the average particle size of the second mixture, and the too large particle size can lead to insufficient contact between the bonding material and the aggregate, poor mechanical properties, too low void ratio and poor thermal shock resistance.
Preferably, the mass ratio of the second mixture, the vanadium-aluminum slag powder and the water in the step (4) is (10-30): (30-80): (10-40), and may be, for example, 20:50:30, 20:40:40, 18:50:20, 25:70:30 or 30:72:40, but not limited to, the recited values, and other non-recited values in the range of values are equally applicable.
Preferably, the vanadium-aluminum slag powder of step (4) includes a first vanadium-aluminum slag powder and a second vanadium-aluminum slag powder.
Preferably, the average particle size of the first vanadium aluminum slag powder is 1 to 3mm, for example, 1mm, 1.5mm, 2mm, 2.5mm or 3mm, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
Preferably, the average particle size of the second vanadium aluminum slag powder is 3 to 10mm, for example, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm or 10mm, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
Preferably, the first vanadium aluminum slag powder and the second vanadium aluminum slag powder are different in particle size.
As a preferred technical scheme of the present invention, the method for preparing the unshaped refractory material by using the vanadium-aluminum slag in the first aspect of the present invention comprises the following steps:
(1) Crushing the vanadium-aluminum slag to obtain vanadium-aluminum slag powder with the granularity of 1-10 mm;
(2) Mixing calcium oxide and calcium fluoride according to the mass ratio of (2-3) to (0-1) to (21-26), and calcining the vanadium-aluminum slag powder obtained in the step (1) at the temperature of 1200-1400 ℃ for 20-30 min to obtain a first mixture;
(3) Mixing retarder and the first mixture obtained in the step (2) according to the mass ratio of (2-9) to 100, and grinding to obtain a second mixture with the average particle size of 60-90 mu m;
(4) Mixing the second mixture, vanadium-aluminum slag powder and water according to the mass ratio of (10-30) to (30-80) to (10-40) to obtain the unshaped refractory material;
wherein the vanadium-aluminum slag powder in the step (4) comprises first vanadium-aluminum slag powder with the average granularity of 1-3 mm and second vanadium-aluminum slag powder with the average granularity of 3-10 mm;
and (4) obtaining the unshaped refractory materials in different service environments by adjusting the mixing proportion and/or the particle size of the vanadium-aluminum slag powder.
In a second aspect, the invention provides the use of an unshaped refractory as provided in the first aspect, the unshaped refractory being useful in any one of a refractory scene of intermediate frequency vacuum induction furnace crucible tying, kiln wall casting or aluminum melting furnace inner wall masonry.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method provided by the invention takes the vanadium-aluminum alloy smelting byproducts as raw materials, fully utilizes the vanadium-aluminum slag, prevents solid waste from accumulating, and realizes the recycling of resources;
(2) The method provided by the invention has the advantages of short process flow, simplicity in operation and high safety coefficient, and is beneficial to industrial production;
(3) The method provided by the invention has the advantages that more than 85% of the used materials are waste generated in the production process of the vanadium-aluminum alloy, and the prepared unshaped refractory material has good refractory property and high hardening strength and can be used in various production environments.
Drawings
FIG. 1 is a process flow diagram of the method for preparing the unshaped refractory by utilizing the vanadium-aluminum slag.
Detailed Description
The technical scheme of the invention is further described below by the specific embodiments with reference to the accompanying drawings. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
The compositions of the vanadium-aluminum slag in the following examples and comparative examples include, in mass percent: 18wt% calcium fluoride, 0.85wt% iron, 0.95wt% vanadium, 1.35wt% Si, the balance being alumina and unavoidable impurities.
Example 1
The embodiment provides a method for preparing an unshaped refractory by utilizing vanadium-aluminum slag, which comprises the following steps:
(1) Crushing the vanadium-aluminum slag to obtain vanadium-aluminum slag powder with the granularity of 1-10 mm;
(2) Mixing 2.31kg of calcium oxide, 0.12kg of calcium fluoride and 30kg of the vanadium-aluminum slag powder obtained in the step (1), and calcining at 1400 ℃ for 20min to obtain 32.13kg of a first mixture;
(3) Mixing 1.12kg of anhydrous gypsum with the first mixture obtained in the step (2), and grinding to obtain a second mixture with the average particle size of 80 mu m;
(4) Mixing 33.1kg of the second mixture, vanadium-aluminum slag powder and 13.3kg of water to obtain an unshaped refractory;
wherein the vanadium aluminum slag powder in the step (4) comprises 38kg of a first vanadium aluminum slag powder with an average particle size of 2mm and 40kg of a second vanadium aluminum slag powder with an average particle size of 7 mm.
The refractory material provided by the embodiment can be used for knotting the intermediate frequency vacuum induction furnace crucible.
Example 2
The embodiment provides a method for preparing an unshaped refractory by utilizing vanadium-aluminum slag, which comprises the following steps:
(1) Crushing the vanadium-aluminum slag to obtain vanadium-aluminum slag powder with the granularity of 1-10 mm;
(2) Mixing 2.6kg of calcium oxide, 0.36kg of calcium fluoride and 30kg of the vanadium-aluminum slag powder obtained in the step (1), and calcining at 1350 ℃ for 30min to obtain 31.1kg of a first mixture;
(3) Mixing 1.87kg of anhydrous gypsum with the first mixture obtained in the step (2), and grinding to obtain a second mixture with the average particle size of 60 mu m;
(4) Mixing 32.24kg of the second mixture, vanadium-aluminum slag powder and 30kg of water to obtain an unshaped refractory;
wherein the vanadium aluminum slag powder in the step (4) comprises 30kg of a first vanadium aluminum slag powder with an average particle size of 2mm and 33.25kg of a second vanadium aluminum slag powder with an average particle size of 7 mm.
The refractory material provided by the embodiment can be used for building a vanadium melting tank.
Example 3
The embodiment provides a method for preparing an unshaped refractory by utilizing vanadium-aluminum slag, which comprises the following steps:
(1) Crushing the vanadium-aluminum slag to obtain vanadium-aluminum slag powder with the granularity of 1-10 mm;
(2) Mixing 3.3kg of calcium oxide, 0.91kg of calcium fluoride and 30kg of the vanadium-aluminum slag powder obtained in the step (1), and calcining at 1350 ℃ for 25min to obtain 33.52kg of a first mixture;
(3) Mixing 1.34kg of anhydrous gypsum with the first mixture obtained in the step (2), and grinding to obtain a second mixture with the average particle size of 90 mu m;
(4) Mixing 34.13kg of the second mixture, vanadium-aluminum slag powder and 20kg of water to obtain an unshaped refractory;
wherein the vanadium aluminum slag powder in the step (4) comprises 30kg of a first vanadium aluminum slag powder with an average particle size of 2mm and 33.25kg of a second vanadium aluminum slag powder with an average particle size of 7 mm.
The refractory material provided by the embodiment can be used for building the inner wall of the aluminum melting furnace.
Example 4
This example provides a method for preparing an unshaped refractory using vanadium aluminium slag, which differs from example 1 only in that:
in the embodiment, the vanadium-aluminum slag powder in the step (4) is changed into 78kg of first vanadium-aluminum slag powder with the average particle size of 2mm, and the second vanadium-aluminum slag powder is omitted.
Example 5
This example provides a method for preparing an unshaped refractory using vanadium aluminium slag, which differs from example 1 only in that:
in the embodiment, the vanadium-aluminum slag powder in the step (4) is changed into 78kg of second vanadium-aluminum slag powder with the average particle size of 7mm, and the first vanadium-aluminum slag powder is omitted.
Example 6
This example provides a method for preparing an unshaped refractory using vanadium aluminium slag, which differs from example 1 only in that:
in the embodiment, the granularity of the vanadium-aluminum slag powder in the step (1) is changed to 10-20 mm.
Example 7
This example provides a method for preparing an unshaped refractory using vanadium aluminium slag, which differs from example 1 only in that:
the temperature of the calcination in the step (2) is changed to 1150 ℃ in the embodiment.
Example 8
This example provides a method for preparing an unshaped refractory using vanadium aluminium slag, which differs from example 1 only in that:
this example changed the temperature of the calcination in step (2) to 1450 ℃.
Example 9
This example provides a method for preparing an unshaped refractory using vanadium aluminium slag, which differs from example 1 only in that:
in this embodiment, the retarder described in step (3) is omitted.
Detecting the performance of the refractory material;
the refractories provided in examples and comparative examples were subjected to performance tests including refractoriness, compressive strength after hardening, softening temperature under load and rate of change of burn-in line, and the test results are shown in table 1.
TABLE 1
As can be seen from table 1, analysis of examples 1 and 4-5 shows that the simultaneous mixing of the first vanadium aluminum slag powder and the second vanadium aluminum slag powder with different particle sizes during the mixing process is beneficial to obtaining the optimal particle size distribution, so that the prepared unshaped refractory material has better mechanical properties and fire resistance, and the lack of one of them can cause a great reduction in mechanical properties or fire resistance.
In summary, the invention takes the vanadium-aluminum alloy smelting byproducts as raw materials, fully utilizes the vanadium-aluminum slag, prevents solid waste accumulation, realizes resource recycling, has short process flow, simple operation and high safety coefficient, and more than 85% of the used materials are waste materials generated in the vanadium-aluminum alloy production process, so that the prepared unshaped refractory material has good refractory performance and high hardening strength, and can be used in various production environments.
The applicant states that the detailed structural features of the present invention are described by the above embodiments, but the present invention is not limited to the above detailed structural features, i.e. it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope of the present invention and the scope of the disclosure.
The applicant states that the detailed process flow of the present invention is illustrated by the above examples, but the present invention is not limited to the above detailed process flow, i.e. it does not mean that the present invention must be implemented depending on the above detailed process flow. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (10)
1. A method for preparing an unshaped refractory by utilizing vanadium-aluminum slag, which is characterized by comprising the following steps: taking vanadium-aluminum slag as a raw material, and sequentially crushing, blending, calcining, grinding and mixing to obtain the unshaped refractory material.
2. The method for preparing unshaped refractory by utilizing vanadium-aluminum slag according to claim 1, wherein the unshaped refractory has a refractoriness of 1600-1800 ℃;
preferably, the load softening temperature of the unshaped refractory material is 1200-1450 ℃;
preferably, the compressive strength of the unshaped refractory is 73.2-78.5 MPa;
preferably, the rate of change of the burn line of the unshaped refractory is 0.4 to 0.6%.
3. The method for preparing an unshaped refractory using vanadium aluminum slag according to claim 1 or 2, comprising the steps of:
(1) Crushing the vanadium-aluminum slag to obtain vanadium-aluminum slag powder;
(2) Mixing calcium oxide, calcium fluoride and vanadium-aluminum slag powder obtained in the step (1), and calcining to obtain a first mixture;
(3) Mixing retarder and the first mixture obtained in the step (2), and grinding to obtain a second mixture;
(4) Mixing the second mixture, vanadium-aluminum slag powder and water to obtain an unshaped refractory material;
and (4) obtaining the unshaped refractory materials in different service environments by adjusting the mixing proportion and/or the particle size of the vanadium-aluminum slag powder.
4. A method for producing an unshaped refractory using a vanadium aluminum slag according to claim 3, wherein the average particle size of the vanadium aluminum slag powder in the step (1) is 1 to 10mm;
preferably, the vanadium-aluminum slag of the step (1) comprises, in mass percent: calcium fluoride < 20wt%, iron < 1wt%, vanadium < 1wt%, si < 1.5wt%, alumina balance and unavoidable impurities.
5. The method for producing unshaped refractory using vanadium-aluminum slag as claimed in claim 3 or 4, wherein the mass ratio of the calcium oxide, calcium fluoride and vanadium-aluminum slag powder in the step (2) is (2-3): (0-1): (21-26);
preferably, the purity of the calcium oxide is more than or equal to 97%;
preferably, the purity of the calcium fluoride is more than or equal to 98 percent.
6. The method for preparing an unshaped refractory using vanadium-aluminum slag according to any one of claims 3 to 5, wherein the temperature of the calcination in the step (2) is 1200 to 1400 ℃;
preferably, the calcination time in the step (2) is 20-30 min.
7. The method for preparing unshaped refractory by utilizing vanadium-aluminum slag according to any one of claims 3 to 6, wherein the mass ratio of retarder to first mixture in the step (3) is (2-9) 100;
preferably, the retarder of step (3) comprises any one or a combination of at least two of calcium sulfate hemihydrate, gypsum or anhydrite;
preferably, the second mixture of step (3) has an average particle size of 60 to 90 μm.
8. The method for preparing unshaped refractory by utilizing vanadium-aluminum slag according to any one of claims 3 to 7, wherein the mass ratio of the second mixture, vanadium-aluminum slag powder and water in the step (4) is (10-30): (30-80): (10-40);
preferably, the vanadium-aluminum slag powder of step (4) comprises a first vanadium-aluminum slag powder and a second vanadium-aluminum slag powder;
preferably, the average particle size of the first vanadium-aluminum slag powder is 1-3 mm;
preferably, the average particle size of the second vanadium-aluminum slag powder is 3-10 mm;
preferably, the first vanadium aluminum slag powder and the second vanadium aluminum slag powder are different in particle size.
9. The method for preparing an unshaped refractory using vanadium-aluminum slag according to any one of claims 1 to 8, wherein the method comprises the steps of:
(1) Crushing the vanadium-aluminum slag to obtain vanadium-aluminum slag powder with the average granularity of 1-10 mm;
(2) Mixing calcium oxide and calcium fluoride according to the mass ratio of (2-3) to (0-1) to (21-26), and calcining the vanadium-aluminum slag powder obtained in the step (1) at the temperature of 1200-1400 ℃ for 20-30 min to obtain a first mixture;
(3) Mixing retarder and the first mixture obtained in the step (2) according to the mass ratio of (2-9) to 100, and grinding to obtain a second mixture with the average particle size of 60-90 mu m;
(4) Mixing the second mixture, vanadium-aluminum slag powder and water according to the mass ratio of (10-30) to (30-80) to (10-40) to obtain the unshaped refractory material;
wherein the vanadium-aluminum slag powder in the step (4) comprises first vanadium-aluminum slag powder with the average granularity of 1-3 mm and second vanadium-aluminum slag powder with the average granularity of 3-10 mm;
and (4) obtaining the unshaped refractory materials in different service environments by adjusting the mixing proportion and/or the particle size of the vanadium-aluminum slag powder.
10. Use of an unshaped refractory according to any one of claims 1 to 9, wherein the unshaped refractory is used in any one of refractory scenes in intermediate frequency vacuum induction furnace crucible knotting, kiln wall casting or aluminum melting furnace inner wall masonry.
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