CN117700233B - Core brick for oxidation-reduction tuyere of anode furnace and preparation method thereof - Google Patents
Core brick for oxidation-reduction tuyere of anode furnace and preparation method thereof Download PDFInfo
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- CN117700233B CN117700233B CN202410167564.8A CN202410167564A CN117700233B CN 117700233 B CN117700233 B CN 117700233B CN 202410167564 A CN202410167564 A CN 202410167564A CN 117700233 B CN117700233 B CN 117700233B
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- 239000011449 brick Substances 0.000 title claims abstract description 115
- 230000033116 oxidation-reduction process Effects 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 127
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 65
- 239000000843 powder Substances 0.000 claims abstract description 60
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000011268 mixed slurry Substances 0.000 claims abstract description 33
- 239000002243 precursor Substances 0.000 claims abstract description 29
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 23
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004327 boric acid Substances 0.000 claims abstract description 21
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 21
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910033181 TiB2 Inorganic materials 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
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- 239000002002 slurry Substances 0.000 claims abstract description 18
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 12
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 239000007767 bonding agent Substances 0.000 claims abstract description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 15
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 13
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- 238000010438 heat treatment Methods 0.000 claims description 9
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- 239000011230 binding agent Substances 0.000 claims description 7
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
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- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 239000004014 plasticizer Substances 0.000 claims description 3
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- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 abstract description 29
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 abstract description 25
- 229910052580 B4C Inorganic materials 0.000 abstract description 17
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 abstract description 17
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- 239000010949 copper Substances 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 229910052593 corundum Inorganic materials 0.000 description 7
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- 230000000694 effects Effects 0.000 description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
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- 229910052710 silicon Inorganic materials 0.000 description 4
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910000423 chromium oxide Inorganic materials 0.000 description 2
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
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Classifications
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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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention belongs to the technical field of refractory materials, and discloses a core brick for an oxidation-reduction tuyere of an anode furnace and a preparation method thereof, wherein the core brick mainly comprises the following raw materials in parts by weight: 85-100 parts of modified silicon carbide fine powder, 8-15 parts of mullite, 2-6 parts of zirconia micro powder, 3-7 parts of calcined alpha alumina micro powder, 2-4 parts of titanium diboride fine powder and 2-5 parts of bonding agent; synthesizing boron nitride and boron carbide precursor gel by using boric acid, melamine and chitosan under the action of a cross-linking agent to coat silicon carbide slurry, and then performing vacuum drying to obtain modified silicon carbide fine powder; and (3) stirring and mixing the modified silicon carbide fine powder with the other raw materials and deionized water to obtain mixed slurry, pouring the mixed slurry into a mould for compression molding, and then sintering at high temperature to obtain the core brick for the oxidation-reduction tuyere of the anode furnace. The core brick prepared by the invention has the advantages of high strength, thermal shock resistance, good slag erosion resistance, high fracture toughness and the like.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a core brick for an oxidation-reduction tuyere of an anode furnace and a preparation method thereof.
Background
The anode furnace is mainly used for refining liquid blister copper, has the advantages of large capacity, high mechanical automation degree, strong controllability, low energy consumption and the like, and is being popularized and used by large-scale copper-smelting factories. The copper smelting anode furnace is mainly used for oxidizing, removing impurities and deoxidizing the blown crude copper so as to obtain refined copper with the purity of more than 99.3 percent. The process of refining copper in the anode furnace mainly comprises four working stages of feeding, oxidizing and deslagging, reducing and casting, wherein the oxidizing and deslagging and the reducing processes are realized by blowing different mediums such as compressed air, nitrogen, natural gas and the like into the copper liquid in stages through core bricks of redox tuyere bricks. The core brick of the redox tuyere brick plays a leading role in the production process of refined copper in the anode furnace, and dominates the contact area of the medium jet flow and the melt, the stirring intensity of a molten pool, the redox reaction rate of impurity elements, the heating rate of the molten pool and the slag skimming effect. Meanwhile, the method is a weaker link of the copper smelting anode furnace, and needs to bear the structural flaking, breaking or burning loss caused by high temperature and scouring and temperature fluctuation. Therefore, strict requirements are put on the core bricks of the oxidation-reduction tuyere bricks of the anode furnace.
At present, most of core bricks of the redox tuyere brick of the anode furnace adopt spinel materials, chrome corundum materials and corundum materials, and the redox tuyere brick core bricks of the corundum materials are damaged due to the fact that the corundum thermal expansion coefficient is high and the redox tuyere brick core bricks are easy to crack and peel due to thermal shock, so that the thermal shock resistance and strength of the redox tuyere brick core bricks are reduced, and the service life of the redox tuyere brick core bricks is greatly shortened; the chromium oxide is easy to form hexavalent chromium in the use process, the hexavalent chromium has toxicity, serious injury is caused to human bodies after the chromium oxide contacts the brick, and the used redox tuyere brick core brick can cause serious pollution to the atmosphere and underground water if being improperly treated; the spinel redox tuyere brick is easy to be influenced by local cooling or high temperature change on the surface of spinel, so that the brick blank of the brick is peeled off, and the service life of the redox tuyere brick is shortened. Silicon carbide is a good refractory material, has the advantages of high strength, good high-temperature performance, strong thermal shock resistance, good corrosion resistance and the like, and can not cause environmental pollution in the use process, so that the silicon carbide can be used as the main material of the core brick of the anode furnace redox tuyere brick to overcome the defects of the spinel material, the chrome corundum material and the core brick of the corundum material, but the core brick of the anode furnace redox tuyere brick of the silicon carbide material needs slip casting in the preparation process, and the silicon carbide slurry needs to have good fluidity in the slip casting process, but the silicon carbide powder has high surface energy, so that the silicon carbide powder is easy to agglomerate in an aqueous solution, thereby reducing the fluidity of the silicon carbide slurry, leading to the strength reduction of the silicon carbide core brick of the anode furnace redox tuyere brick, and the silicon carbide has large brittleness and easy damage to external force and easy to fracture and crack, thereby influencing the strength and the service life of the core brick of the anode furnace redox tuyere brick.
Therefore, developing a core brick of the anode furnace redox tuyere brick which meets the use requirements of the anode furnace redox tuyere brick and has high strength, thermal shock resistance, good erosion resistance and low brittleness has important significance in the field.
Disclosure of Invention
In order to solve the technical problems in the prior art, the application aims to provide a core brick for an oxidation-reduction tuyere of an anode furnace and a preparation method thereof. According to the preparation method, boric acid solution, melamine solution and chitosan solution are utilized to synthesize boron nitride and boron carbide precursor gel with a three-dimensional space network structure under the action of cross-linking agent vinyl triethoxysilane, then the boron nitride and boron carbide precursor gel is mixed with silicon carbide slurry to form silicon carbide mixed slurry coated by the boron nitride and boron carbide precursor gel, and then vacuum drying is carried out to obtain modified silicon carbide fine powder; the modified silicon carbide solves the problem that silicon carbide powder is easy to agglomerate in the prior art, and when the core brick is prepared and sintered at high temperature, a precursor coated with the silicon carbide is decomposed in situ to generate boron nitride and boron carbide, the boron nitride has a lamellar structure similar to graphite and has moderate interface bonding strength with the silicon carbide, so that good interface bonding between the boron nitride and the silicon carbide is more favorable, the synergistic toughening effect between multiple interfaces of the silicon carbide is realized, and meanwhile, the generated boron nitride and boron carbide can form a boron carbide-silicon carbide-boron nitride three-dimensional interpenetrating structure with the silicon carbide.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The core brick for the oxidation-reduction tuyere of the anode furnace mainly comprises the following raw materials in parts by weight: 85-100 parts of modified silicon carbide fine powder, 8-15 parts of mullite, 2-6 parts of zirconia micro powder, 3-7 parts of calcined alpha alumina micro powder, 2-4 parts of titanium diboride fine powder and 2-5 parts of bonding agent; the preparation method of the modified silicon carbide specifically comprises the following steps:
(1) Adding boric acid powder into deionized water, stirring at 75-90 ℃ at a rotating speed of 200-300r/min to fully dissolve the boric acid powder and obtain boric acid solution;
(2) Sequentially adding melamine solution and chitosan solution into the boric acid solution obtained in the step (1) under the condition of water bath heating, and performing ultrasonic dispersion, wherein the power of ultrasonic dispersion is 150-200W, the ultrasonic dispersion time is 0.5-1.5h, and stirring at the rotating speed of 150-200r/min until the solution is transparent, so as to obtain a precursor intermediate solution;
(3) Adding a cross-linking agent vinyl triethoxysilane and an initiator potassium persulfate into the precursor intermediate solution obtained in the step (2), and stirring while adding the vinyl triethoxysilane and the initiator potassium persulfate to obtain precursor gel;
(4) Adding dispersing agent polyvinylpyrrolidone and plasticizer tricresyl phosphate into silicon carbide powder, then placing into a ball milling tank, and carrying out planetary wet mixing at the rotating speed of 200-300r/min to obtain prefabricated silicon carbide slurry;
(5) And (3) performing ultrasonic dispersion on the precursor gel obtained in the step (3) and the prefabricated silicon carbide slurry obtained in the step (4), wherein the ultrasonic dispersion power is 80-100W, the ultrasonic dispersion time is 2-5h, so as to obtain modified silicon carbide mixed slurry, and then placing the modified silicon carbide mixed slurry in a vacuum drying oven to perform vacuum drying at 120-150 ℃ for 6-8h, so as to obtain modified silicon carbide fine powder.
When the core brick for the oxidation-reduction tuyere of the anode furnace is prepared, in order to ensure that the silicon carbide slurry has good fluidity, the agglomeration of silicon carbide particles in the silicon carbide slurry is reduced, the brittleness of the silicon carbide is reduced, the toughness and the strength of the silicon carbide are improved, and the strength and the toughness of the core brick for the oxidation-reduction tuyere of the anode furnace are further improved. According to the preparation method, boric acid is used as a boron source, melamine is used as a nitrogen source, chitosan is used as a carbon source, boron nitride and boron carbide precursor gel with a three-dimensional space network structure are prepared in the presence of cross-linking agent vinyl triethoxysilane and initiator potassium persulfate, and when the three-dimensional space network structure precursor gel is mixed with silicon carbide slurry, modified silicon carbide mixed slurry is formed, namely the three-dimensional space network structure precursor gel coated silicon carbide mixed slurry, the three-dimensional space network structure can form strong steric hindrance on the surfaces of silicon carbide particles, so that the viscosity of the modified silicon carbide mixed slurry is reduced, the aggregation of silicon carbide particles in the modified silicon carbide mixed slurry is reduced, and the strength of silicon carbide is improved; when the modified silicon carbide fine powder is mixed with mullite, zirconia fine powder, calcined alpha alumina fine powder, titanium diboride fine powder and a binding agent to form mixed slurry, the modified silicon carbide is coated by precursor gel with a three-dimensional space network structure, so that agglomeration of silicon carbide particles in the mixed slurry is reduced, and the mechanical property of the silicon carbide is improved; when the mixed slurry is subjected to compression molding and then high-temperature calcination, in the high-temperature calcination process, the precursor coated with the silicon carbide is decomposed in situ to generate boron nitride and boron carbide, and the boron nitride has a graphite-like lamellar structure and moderate interface bonding strength with the silicon carbide, so that good interface bonding between the boron nitride and the silicon carbide is facilitated, the synergistic toughening effect between multiple interfaces of the silicon carbide is realized, and meanwhile, the generated boron nitride and boron carbide can form a boron carbide-silicon carbide-boron nitride three-dimensional interpenetrating structure with the silicon carbide, so that the toughness and strength of a silicon carbide substrate can be effectively improved, and the brittleness of the silicon carbide is reduced.
Further, the SiC content in the silicon carbide fine powder is more than or equal to 99.5 weight percent, and the granularity of the silicon carbide fine powder is 20-30 mu m.
Further, the grain diameter of the mullite is 0.5-15 mu m.
Further, the content of ZrO 2 in the zirconia micropowder is more than or equal to 99wt%, and the granularity of the zirconia micropowder is 10-15 mu m.
Further, the content of alpha-Al 2O3 in the calcined alpha alumina micropowder is more than or equal to 98.3wt%, and the granularity of the calcined alpha alumina micropowder is 2-5 mu m.
Further, the TiB 2 content in the titanium diboride fine powder is more than or equal to 98.6wt%, and the granularity of the titanium diboride fine powder is 8-10 mu m.
Further, the molar ratio of boric acid to melamine to chitosan in the step (2) is (4-6): 1-2): 1-2.5.
Further, the mass ratio of the precursor intermediate solution to the crosslinking agent vinyltriethoxysilane in the step (3) is (1.5-2.8) (2.5-4).
Further, in the step (4), the time of the wet mixing of the planet is 8-10 hours, the used mixing medium is deionized water, and the ball milling medium is silicon carbide balls.
Further, the preparation method of the core brick for the oxidation-reduction tuyere of the anode furnace comprises the following steps:
S1, weighing the raw materials according to the parts by weight, adding modified silicon carbide fine powder, mullite, zirconia fine powder, calcined alpha alumina fine powder, titanium diboride fine powder, a bonding agent polyacrylic acid and a proper amount of deionized water into a stirring kettle, and fully stirring and uniformly mixing in the stirring kettle to obtain mixed slurry;
s2, pouring the mixed slurry obtained in the step S1 into a mould to be pressed and molded, curing for 12-24 hours at 25-35 ℃, and drying for 15-20 hours at 110-120 ℃ to obtain a green brick of the core brick of the oxidation-reduction tuyere of the anode furnace;
And S3, carrying out heat preservation on the core brick green body of the oxidation-reduction tuyere of the anode furnace obtained in the step S2 for 12-24h high-temperature firing in a nitrogen atmosphere at the temperature of 1670-1750 ℃ at the heating rate of 4-6 ℃/min, and cooling the core brick green body to room temperature along with the furnace to obtain the core brick for the oxidation-reduction tuyere of the anode furnace.
Compared with the prior art, the invention has the positive and beneficial effects that:
(1) According to the preparation method, the modified silicon carbide slurry is obtained by coating the silicon carbide slurry through preparing boron nitride and boron carbide precursor gel with a three-dimensional space network structure, and then the modified silicon carbide slurry is dried at a low temperature to obtain modified silicon carbide fine powder; when the modified silicon carbide fine powder, other raw materials of the core brick and deionized water are stirred and mixed to form mixed slurry, and the mixed slurry is pressed and formed and calcined at high temperature, the core brick for the oxidation-reduction tuyere of the anode furnace is obtained, and the three-dimensional space reticular structure increases the steric hindrance of the surfaces of silicon carbide particles in the mixed slurry, so that the viscosity of the mixed slurry is reduced, the agglomeration of the silicon carbide slurry particles is reduced, the mechanical property of silicon carbide is improved, and the strength of the core brick for the oxidation-reduction tuyere of the anode furnace is further improved; in the high-temperature calcination process, boron nitride and boron carbide precursors in the modified silicon carbide are decomposed in situ to generate boron nitride and boron carbide, the boron nitride has a lamellar structure similar to graphite and has moderate interface bonding strength with the silicon carbide, good interface bonding is formed between the boron nitride and the silicon carbide, the synergistic toughening effect between multiple interfaces of the silicon carbide is realized, and meanwhile, the generated boron nitride and boron carbide can also form a boron carbide-silicon carbide-boron nitride three-dimensional interpenetrating structure with the silicon carbide, so that the brittleness of the silicon carbide can be reduced, and the toughness and the high-temperature fracture strength of the silicon carbide matrix core brick are effectively improved.
(2) The invention prepares the core brick for the oxidation reduction tuyere of the anode furnace by using the raw materials such as modified silicon carbide, mullite, zirconia micropowder, calcined alpha alumina micropowder, titanium diboride micropowder, binding agent and the like; the modified silicon carbide, mullite, zirconia and calcined alpha alumina change the crystal phase structure of the core brick material in the high-temperature sintering process, so that the structure of the core brick material is uniform, no layer crack exists, the strength is high, and the slag erosion resistance and the thermal shock resistance of the core brick are improved; the modified silicon carbide has high strength and low brittleness, so that the strength and toughness of the core brick of the oxidation-reduction tuyere of the anode furnace are improved, and the service life of the core brick of the oxidation-reduction tuyere of the anode furnace is prolonged; meanwhile, mullite can be converted into an A3S2 phase at high temperature, and the A3S2 phase has the advantages of high melting point, small expansion coefficient, good thermal shock resistance, high creep resistance and the like, and the addition of the mullite can improve the high-temperature performance of the core brick; in the high-temperature sintering process of the core brick, when the temperature reaches above 1000 ℃, tiB 2 fine powder can be oxidized slowly, in the oxidation process of TiB 2, tiO 2 phases with very high activity are formed in the core brick, tiO 2-ZrO2、TiO2-Al2O3 solid solutions are formed by reaction with ZrO 2、Al2O3 and the like in the core brick material, strong bonding phases are formed in the core brick, the strength and slag erosion resistance of the core brick are improved, meanwhile, zirconium oxide can form martensitic transformation toughening of zirconium oxide in the high-temperature sintering process, and the thermal shock resistance and high-temperature fracture strength of the core brick of an oxidation reduction tuyere of an anode furnace are improved.
Detailed Description
The technical solutions of the present application will be clearly and completely described below in connection with specific embodiments, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The following examples were conducted under conventional conditions or conditions recommended by the manufacturer, without specifying the specific conditions. The reagents or raw materials used, not specifically described, are of the conventional type used in the art or of the type well known to those skilled in the art, and are of the conventional type commercially available without any indication of the manufacturer.
Examples
The preparation method of the modified silicon carbide fine powder specifically comprises the following steps:
(1) Adding boric acid powder into deionized water, stirring at 75-90 ℃ at a rotating speed of 200-300r/min to fully dissolve the boric acid powder and obtain boric acid solution;
(2) Sequentially adding melamine solution and chitosan solution into the boric acid solution obtained in the step (1) under the water bath heating condition of 60-80 ℃, performing ultrasonic dispersion for 0.5-1.5h under the power condition of 150-200W, and stirring at the rotating speed of 150-200r/min until the solution is transparent, thus obtaining a precursor intermediate solution; wherein the mol ratio of boric acid to melamine to chitosan is (4-6): 1-2): 1-2.5; the mass fraction of boric acid in the boric acid solution is 75-85%, the mass fraction of melamine in the melamine solution is 55-78%, and the mass fraction of chitosan in the chitosan solution is 48-72%;
(3) Sequentially adding a cross-linking agent vinyl triethoxysilane and an initiator potassium persulfate into the precursor intermediate solution obtained in the step (2), and stirring while adding the cross-linking agent vinyl triethoxysilane and the initiator potassium persulfate, wherein the stirring speed is 100-150r/min, so as to obtain precursor gel; wherein the mass ratio of the precursor intermediate solution to the cross-linking agent vinyltriethoxysilane is (1.5-2.8) (2.5-4);
(4) Adding dispersing agent polyvinylpyrrolidone and plasticizer tricresyl phosphate into silicon carbide powder, then placing into a ball milling tank, and carrying out planetary wet mixing at the rotating speed of 200-300r/min to obtain prefabricated silicon carbide slurry; wherein the time of planetary wet mixing is 8-10h, the mixing medium is deionized water, and the ball milling medium is silicon carbide balls;
(5) And (3) performing ultrasonic dispersion on the precursor gel obtained in the step (3) and the prefabricated silicon carbide slurry obtained in the step (4), wherein the ultrasonic power is 80-100W, the ultrasonic dispersion time is 2-5h, so as to obtain modified silicon carbide mixed slurry, and then placing the modified silicon carbide mixed slurry in a vacuum drying oven, and vacuum drying at 120-150 ℃ for 6-8h, so as to obtain modified silicon carbide fine powder.
The silicon carbide fine powders used in the following examples were all modified silicon carbide fine powders prepared in this example.
Specific criteria for the raw material fine powder or micro powder used in the following examples are as follows, and are not described in detail in the following examples: the SiC content in the silicon carbide fine powder is more than or equal to 99.5 weight percent, and the granularity of the silicon carbide fine powder is 20-30 mu m; the grain diameter of the mullite is 0.5-15 mu m; the ZrO 2 content in the zirconia micropowder is more than or equal to 99wt%, and the granularity of the zirconia micropowder is 10-15 mu m; the content of alpha-Al 2O3 in the calcined alpha alumina micropowder is more than or equal to 98.3wt percent, and the granularity of the calcined alpha alumina micropowder is 2-5 mu m; the TiB 2 content in the titanium diboride fine powder is more than or equal to 98.6wt%, and the granularity of the titanium diboride fine powder is 8-10 mu m.
Example 1
The core brick for the oxidation-reduction tuyere of the anode furnace mainly comprises the following raw materials in parts by weight: 85 parts of modified silicon carbide fine powder, 15 parts of mullite, 2 parts of zirconia micro powder, 7 parts of calcined alpha alumina micro powder, 2 parts of titanium diboride fine powder and 5 parts of binding agent polyacrylic acid.
The preparation method of the core brick for the oxidation-reduction tuyere of the anode furnace comprises the following steps:
Step S1, weighing the raw materials according to the weight parts, and fully and uniformly stirring and mixing modified silicon carbide fine powder, mullite, zirconia fine powder, calcined alpha alumina fine powder, titanium diboride fine powder, a bonding agent polyacrylic acid and 11 weight parts of deionized water in a stirring kettle to obtain mixed slurry;
S2, pouring the mixed slurry obtained in the step S1 into a mould for compression molding, curing for 24 hours at 25 ℃, and drying for 20 hours at 110 ℃ to obtain a core brick green body of an anode furnace redox tuyere;
And S3, carrying out heat preservation and high-temperature firing on the core brick green bricks of the oxidation-reduction tuyere of the anode furnace obtained in the step S2 for 24 hours in a nitrogen atmosphere at the temperature of 1670 ℃ at the heating rate of 4 ℃/min, and cooling the core bricks to room temperature along with the furnace to obtain the core bricks for the oxidation-reduction tuyere of the anode furnace.
Example 2
The core brick for the oxidation-reduction tuyere of the anode furnace mainly comprises the following raw materials in parts by weight: 92 parts of modified silicon carbide fine powder, 12 parts of mullite, 5 parts of zirconia micro powder, 5 parts of calcined alpha alumina micro powder, 3 parts of titanium diboride fine powder and 4 parts of binding agent polyacrylic acid.
The preparation method of the core brick for the oxidation-reduction tuyere of the anode furnace comprises the following steps:
Step S1, weighing the raw materials according to the weight parts, and fully and uniformly stirring and mixing modified silicon carbide fine powder, mullite, zirconia fine powder, calcined alpha alumina fine powder, titanium diboride fine powder, a bonding agent polyacrylic acid and 14 weight parts of deionized water in a stirring kettle to obtain mixed slurry;
S2, pouring the mixed slurry obtained in the step S1 into a mould for compression molding, curing for 19h at 30 ℃, and drying for 18h at 115 ℃ to obtain a core brick green body of an anode furnace redox tuyere;
And S3, the green bricks of the core bricks of the oxidation-reduction tuyere of the anode furnace obtained in the step S2 are subjected to heat preservation and high-temperature firing for 20 hours in a nitrogen atmosphere at 1700 ℃ at a heating rate of 5 ℃/min, and are cooled to room temperature along with the furnace, so that the core bricks of the oxidation-reduction tuyere of the anode furnace are obtained.
Example 3
The core brick for the oxidation-reduction tuyere of the anode furnace mainly comprises the following raw materials in parts by weight: 100 parts of modified silicon carbide fine powder, 8 parts of mullite, 6 parts of zirconia micro powder, 3 parts of calcined alpha alumina micro powder, 4 parts of titanium diboride fine powder and 2 parts of binding agent polyacrylic acid.
The preparation method of the core brick for the oxidation-reduction tuyere of the anode furnace comprises the following steps:
Step S1, weighing the raw materials according to the parts by weight, and fully and uniformly stirring and mixing modified silicon carbide fine powder, mullite, zirconia fine powder, calcined alpha alumina fine powder, titanium diboride fine powder, a bonding agent polyacrylic acid and 16 parts by weight of deionized water in a stirring kettle to obtain mixed slurry;
S2, pouring the mixed slurry obtained in the step S1 into a mould for compression molding, curing for 12 hours at 35 ℃, and drying for 15 hours at 120 ℃ to obtain a core brick green body of an anode furnace redox tuyere;
And S3, the green bricks of the core bricks of the redox tuyere of the anode furnace obtained in the step S2 are subjected to heat preservation in a nitrogen atmosphere at 1750 ℃ for 12h at a heating rate of 6 ℃/min, and are subjected to high-temperature firing, and are cooled to room temperature along with the furnace, so that the core bricks of the redox tuyere of the anode furnace are obtained.
Comparative example 1
The raw materials and preparation method of the core brick for the anode furnace redox tuyere in this comparative example were the same as in example 3 except that the modified silicon carbide fine powder was replaced with an equal weight of unmodified silicon carbide fine powder.
Comparative example 2
The raw materials and preparation method of the core brick for the redox tuyere of the anode furnace in this comparative example were the same as in example 3, except that the modified silicon carbide fine powder was not added with chitosan at the time of preparation.
Comparative example 3
The raw materials and preparation method of the core brick for the redox tuyere of the anode furnace in this comparative example were the same as in example 3, except that the modified silicon carbide fine powder was prepared without adding the crosslinking agent vinyltriethoxysilane.
The core bricks for the redox tuyere of the anode furnace in examples 2 to 4 and comparative examples 1 to 3 were subjected to performance test, and the specific test results are shown in table 1; wherein the thermal shock in the thermal shock cycle time means that the material is firstly heated to 1100 ℃ and is preserved for 30min, and then is put into flowing water for cooling.
Table 1 results of Performance test of core bricks for redox tuyeres of anode furnace in examples 2 to 4 and comparative examples 1 to 3
| High temperature breaking Strength (MPa, 1200 ℃ C.) | Normal temperature compressive strength (MPa) | Flexural strength (MPa) | Softening temperature under load (0.2 MPa. Times.T 0.6. DEG C.) | Fracture toughness (MPa m 1/2) | Number of thermal shock cycles | 1600 ℃ Static crucible method slag resistance experiment erosion index (%) | |
| Example 2 | 6.3 | 92 | 33 | 1670 | 8.6 | 31 | 2 |
| Example 3 | 6.7 | 95 | 36 | 1700 | 8.9 | 34 | 1.8 |
| Example 4 | 6.4 | 93 | 35 | 1685 | 8.7 | 32 | 1.9 |
| Comparative example 1 | 4.9 | 82 | 28 | 1640 | 7.5 | 27 | 2.3 |
| Comparative example 2 | 5.5 | 86 | 31 | 1655 | 8.1 | 30 | 2.1 |
| Comparative example 3 | 5.2 | 85 | 29 | 1650 | 7.8 | 29 | 2.2 |
As can be seen from the data in Table 1, the application generates the precursor solution of boron nitride and boron carbide by utilizing the reaction of boric acid solution, melamine solution and chitosan solution, and simultaneously, chitosan is subjected to covalent crosslinking among chitosan molecules under the action of vinyl triethoxysilane serving as a crosslinking agent to synthesize chitosan hydrogel with a three-dimensional space network structure; when the modified silicon carbide fine powder, mullite, zirconia fine powder, calcined alpha alumina fine powder, titanium diboride fine powder, binding agent polyacrylic acid and deionized water are stirred and mixed to form mixed slurry, pressed and formed, and calcined at high temperature, the core brick for the oxidation-reduction tuyere of the anode furnace is subjected to three-dimensional space reticular structure, so that the steric hindrance on the surface of silicon carbide particles in the mixed slurry is increased, the viscosity of the mixed slurry is reduced, the agglomeration of the silicon carbide slurry particles is reduced, the mechanical property of silicon carbide is improved, and the strength of the core brick for the oxidation-reduction tuyere of the anode furnace is further improved; in the high-temperature calcination process, boron nitride and boron carbide precursors in the modified silicon carbide are decomposed in situ to generate boron nitride and boron carbide, and the boron nitride has a lamellar structure similar to graphite and has moderate interface bonding strength with the silicon carbide, so that good interface bonding is formed between the boron nitride and the silicon carbide, the synergistic toughening effect between multiple interfaces of the silicon carbide is realized, and meanwhile, the generated boron nitride and boron carbide generate synergistic effect to form a boron carbide-silicon carbide-boron nitride three-dimensional interpenetrating structure with the silicon carbide, and the structure greatly reduces the brittleness of the silicon carbide, thereby effectively improving the toughness and high-temperature fracture strength of the silicon carbide matrix core brick of the oxidation-reduction tuyere of the anode furnace; the modified silicon carbide, mullite, zirconia and calcined alpha alumina change the crystal phase structure of the core brick material of the anode furnace redox tuyere in the high-temperature sintering process, so that the structure of the core brick material is uniform, no layer cracks and high in strength, the slag erosion resistance and the thermal shock resistance of the core brick of the anode furnace redox tuyere are improved, the strength and the brittleness of the modified silicon carbide are low, the strength and the fracture toughness of the core brick of the anode furnace redox tuyere are improved, and the service life of the core brick of the anode furnace redox tuyere is prolonged.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present application have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the application, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The core brick for the oxidation-reduction tuyere of the anode furnace is characterized by mainly comprising the following raw materials in parts by weight: 85-100 parts of modified silicon carbide fine powder, 8-15 parts of mullite, 2-6 parts of zirconia micro powder, 3-7 parts of calcined alpha alumina micro powder, 2-4 parts of titanium diboride fine powder and 2-5 parts of binding agent polyacrylic acid; the preparation method of the modified silicon carbide specifically comprises the following steps:
(1) Adding boric acid powder into deionized water, stirring at 75-90 ℃ at a rotating speed of 200-300r/min to fully dissolve the boric acid powder and obtain boric acid solution;
(2) Sequentially adding melamine solution and chitosan solution into the boric acid solution obtained in the step (1) under the condition of water bath heating, and performing ultrasonic dispersion, wherein the power of ultrasonic dispersion is 150-200W, the ultrasonic dispersion time is 0.5-1.5h, and stirring and mixing at the rotating speed of 150-200r/min until the solution is transparent, so as to obtain a precursor intermediate solution;
(3) Adding vinyl triethoxysilane and initiator potassium persulfate into the precursor intermediate solution obtained in the step (2), and stirring while adding the vinyl triethoxysilane and the initiator potassium persulfate to obtain precursor gel;
(4) Adding dispersing agent polyvinylpyrrolidone and plasticizer tricresyl phosphate into silicon carbide powder, then placing into a ball milling tank, and carrying out planetary wet mixing at the rotating speed of 200-300r/min to obtain prefabricated silicon carbide slurry;
(5) Performing ultrasonic dispersion on the precursor gel obtained in the step (3) and the prefabricated silicon carbide slurry obtained in the step (4), wherein the power of ultrasonic dispersion is 80-100W, the ultrasonic dispersion time is 2-5h, so as to obtain modified silicon carbide mixed slurry, and then placing the modified silicon carbide mixed slurry in a vacuum drying oven to perform vacuum drying at 120-150 ℃ for 6-8h, so as to obtain modified silicon carbide fine powder;
the molar ratio of boric acid to melamine to chitosan in the step (2) is (4-6): 1-2): 1-2.5;
The mass ratio of the precursor intermediate solution to the vinyltriethoxysilane in the step (3) is (1.5-2.8) (2.5-4).
2. The core brick for an oxidation-reduction tuyere of an anode furnace according to claim 1, wherein the SiC content in the silicon carbide fine powder is not less than 99.5wt%, and the granularity of the silicon carbide fine powder is 20-30 μm.
3. The core brick for an anode furnace redox tuyere according to claim 1, wherein the grain size of the mullite is 0.5-15 μm.
4. The core brick for an oxidation-reduction tuyere of an anode furnace according to claim 1, wherein the content of ZrO 2 in the zirconia fine powder is not less than 99wt%, and the grain size of the zirconia fine powder is 10-15 μm.
5. The core brick for an oxidation-reduction tuyere of an anode furnace according to claim 1, wherein the content of alpha-Al 2O3 in the calcined alpha alumina fine powder is not less than 98.3wt%, and the particle size of the calcined alpha alumina fine powder is 2-5 μm.
6. The core brick for an oxidation-reduction tuyere of an anode furnace according to claim 1, wherein the TiB 2 content in the titanium diboride fine powder is not less than 98.6wt%, and the granularity of the titanium diboride fine powder is 8-10 μm.
7. The core brick for the oxidation-reduction tuyere of the anode furnace according to claim 1, wherein the time of the planetary wet mixing in the step (4) is 8-10h, the mixing medium used for the planetary wet mixing is deionized water, and the ball milling medium used for the planetary wet mixing is silicon carbide balls.
8. A method for producing a core brick for an anode furnace redox tuyere according to any of claims 1-7, characterized by comprising the steps of:
S1, weighing the raw materials according to the parts by weight, adding modified silicon carbide fine powder, mullite, zirconia fine powder, calcined alpha alumina fine powder, titanium diboride fine powder, a bonding agent polyacrylic acid and a proper amount of deionized water into a stirring kettle, and fully stirring and uniformly mixing in the stirring kettle to obtain mixed slurry;
s2, pouring the mixed slurry obtained in the step S1 into a mould to be pressed and molded, curing for 12-24 hours at 25-35 ℃, and drying for 15-20 hours at 110-120 ℃ to obtain a green brick of the core brick of the oxidation-reduction tuyere of the anode furnace;
And S3, carrying out heat preservation on the core brick green body of the oxidation-reduction tuyere of the anode furnace obtained in the step S2 for 12-24h high-temperature firing in a nitrogen atmosphere at the temperature of 1670-1750 ℃ at the heating rate of 4-6 ℃/min, and cooling the core brick green body to room temperature along with the furnace to obtain the core brick for the oxidation-reduction tuyere of the anode furnace.
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| AT189111B (en) * | 1948-02-26 | 1957-02-25 | Carborundum Co | Products and objects made of silicon carbide as well as raw materials and processes for their manufacture |
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