CN112341163A - Addition of C @ Cr3C2Low-carbon magnesia-carbon refractory material of composite powder and preparation method thereof - Google Patents
Addition of C @ Cr3C2Low-carbon magnesia-carbon refractory material of composite powder and preparation method thereof Download PDFInfo
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 142
- 239000000843 powder Substances 0.000 title claims abstract description 101
- 239000002131 composite material Substances 0.000 title claims abstract description 75
- 239000011819 refractory material Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 160
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 82
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 75
- 229910003470 tongbaite Inorganic materials 0.000 claims abstract description 55
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 45
- 239000010439 graphite Substances 0.000 claims abstract description 45
- 239000000203 mixture Substances 0.000 claims abstract description 43
- 238000003756 stirring Methods 0.000 claims abstract description 36
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 26
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000005011 phenolic resin Substances 0.000 claims abstract description 26
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 26
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 239000000654 additive Substances 0.000 claims abstract description 18
- 230000000996 additive effect Effects 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011258 core-shell material Substances 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229920001187 thermosetting polymer Polymers 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 abstract description 22
- 238000007254 oxidation reaction Methods 0.000 abstract description 22
- 239000002893 slag Substances 0.000 abstract description 22
- 238000005245 sintering Methods 0.000 abstract 1
- 230000002829 reductive effect Effects 0.000 description 18
- 239000011651 chromium Substances 0.000 description 12
- 230000003628 erosive effect Effects 0.000 description 12
- 239000000047 product Substances 0.000 description 10
- RWDBMHZWXLUGIB-UHFFFAOYSA-N [C].[Mg] Chemical compound [C].[Mg] RWDBMHZWXLUGIB-UHFFFAOYSA-N 0.000 description 8
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 238000009776 industrial production Methods 0.000 description 5
- 229910021392 nanocarbon Inorganic materials 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000011449 brick Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000005997 Calcium carbide Substances 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 239000009730 ganji Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 description 1
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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
- C04B35/043—Refractories from grain sized mixtures
-
- 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- 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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3839—Refractory metal carbides
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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
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
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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
- 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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- 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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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
Abstract
The invention relates to a method for adding C @ Cr3C2A low-carbon magnesia-carbon refractory material of composite powder and a preparation method thereof. The technical scheme is as follows: 60-80 wt% of fused magnesia aggregate, 10-30 wt% of fused magnesia fine powder, 1-4 wt% of aluminum powder, 1-4 wt% of silicon powder, 1-4 wt% of flake graphite and 1-5 wt% of C @ Cr3C2The composite powder is taken as a raw material, and phenolic resin with the weight percent of 3.5-6 of the raw material is added; firstly, aluminum powder, silicon powder and C @ Cr3C2Premixing the composite powder to obtain a mixture I; adding the fused magnesia aggregate into a stirrer, stirring, adding phenolic resin, stirring, then adding the fused magnesia fine powder and the mixture I, stirring, adding crystalline flake graphite, stirring, press-forming, curing, placing in an air furnace, sintering at 1200-1500 ℃ in a carbon-buried atmosphere, naturally cooling to obtain the additive C @ Cr3C2The low-carbon magnesia-carbon refractory material of the composite powder. The product prepared by the invention has high strength, excellent oxidation resistance and excellent slag resistance.
Description
Technical Field
The invention belongs to the technical field of low-carbon magnesia-carbon refractory materials. In particular toAddition of C @ Cr3C2A low-carbon magnesia-carbon refractory material of composite powder and a preparation method thereof.
Background
Magnesia carbon refractories have been widely used in metallurgical vessels and parts such as alkaline oxygen furnaces, ladles, electric arc furnaces, tapholes, slide plates, nozzles, and continuous casting equipment because of their excellent thermal shock resistance, corrosion resistance, and slag resistance. Because the graphite has a large thermal conductivity coefficient and a low thermal expansion coefficient and is not wetted with slag, the graphite is generally used as a carbon source in the production process of the conventional magnesia carbon refractory material to improve the thermal shock resistance, the corrosion resistance and the slag resistance of the magnesia carbon brick, and the carbon content is generally 12-20 wt%. However, in the actual production process, problems due to too high carbon content are gradually revealed: firstly, high energy losses are also associated with high thermal conductivity of graphite; secondly, the high-content graphite can be more easily carburized into metal in the smelting process, so that the quality of the product is reduced; furthermore, high carbon content will produce more COxGas, not environment friendly; finally, the high carbon content can severely reduce the oxidation resistance of the magnesia carbon brick, and even cause the magnesia carbon brick to form a porous structure, so that slag can more easily permeate and erode the magnesia carbon brick. Therefore, the development of a low-carbon magnesia carbon refractory with good performance has become a trend of the development of the magnesia carbon refractory at present.
In order to reduce the carbon content in the magnesia-carbon refractory, a great deal of research is carried out by technical personnel at home and abroad: firstly, a nano carbon source is introduced into the low-carbon magnesia carbon refractory material. Bag et al (M.Bag, S.Adakb, R.Sarkara, Study on low carbon containing MgO-C reactivity: Use of nano carbon [ J.]2012,38:2339-2346) uses nano carbon black and crystalline flake graphite as carbon sources to prepare the low-carbon magnesia carbon refractory material, but the cost of the nano carbon black in the method is high, and the nano carbon black is difficult to disperse in raw materials, so that the method is not beneficial to industrial production. Secondly, preparing composite powder of flake graphite and carbide by modifying the flake graphite, and introducing the composite powder into the low-carbon magnesia-carbon refractory material. However, with respect to Cr3C2The application of the powder in the low-carbon magnesia-carbon refractory material is not reported in a public way.
In the Cr-C bodyIn which the compound of chromium and carbon is Cr23C6、Cr7C3And Cr3C2Three kinds of the components are adopted. Chromium carbide generally has high hardness, good wear resistance, excellent oxidation resistance, and excellent erosion resistance. La, etc. (P.Q.La, Q.J.Xue, W.M.Liu, Effects of boron doping on cubic properties of Ni)3Al-Cr7C3 coatings under dry sliding[J]2001,249:93-99) Synthesis of Ni with excellent wear resistance doped with a small amount of boron on carbon Steel by self-propagating high-temperature Synthesis (SHS)3Al-Cr7C3And (4) composite coating. Ganji et al (O.Ganji, S.A.Sajjadi, Z.G.Yang, et al.on the formation and properties of chromium carbide and calcium carbide products on W1 tool of step through Thermally Reactive Dispersion (TRD) [ J.]The Ceramics International 2020,46:25320-25329) adopts a Thermal Reaction Diffusion (TRD) process to synthesize Cr with high hardness on the surface of W1 tool steel7C3And a VC coating. But these applications are mainly related to the high hardness and wear resistance of chromium carbide.
From the viewpoint of oxidation resistance and erosion resistance, chromium carbide can form dense Cr at high temperature2O3A protective film capable of preventing further progress of oxidation; in addition, in the magnesia-carbon refractory, Cr2O3The existence of the chromium carbide can reduce the chemical corrosion of the slag to the magnesia carbon refractory material, and the slag with high viscosity can also reduce the penetration of the slag to the magnesia carbon refractory material and reduce the formation of an altered layer, thereby inhibiting the structural spalling of the magnesia carbon refractory material, which shows that the chromium carbide has potential application value in the field of the magnesia carbon refractory material. Yang et al (Y. Yang, J.Yu, H.Z.ZHao, et al. Cr. al.)7C3:A potential antioxidant for low carbon MgO-C refractories[J]Ceramics International,2020,46:19743-7C3The additive is introduced into the low-carbon magnesia carbon refractory material, so that the erosion resistance of the low-carbon magnesia carbon refractory material is improved, but the mechanical strength of the low-carbon magnesia carbon refractory material prepared by the method is reduced; and, since Cr is contained in7C3Added into the low-carbon magnesia-carbon refractory material as a single additiveIn the material, the effect of improving the oxidation resistance of the low-carbon magnesia carbon refractory material is limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide the C @ Cr adding agent which is simple to operate, low in cost and easy to industrialize3C2Preparation method of low-carbon magnesium-carbon refractory material of composite powder, and C @ Cr-added refractory material prepared by using method3C2The low-carbon magnesium-carbon refractory material of the composite powder has high strength, excellent oxidation resistance and excellent slag resistance.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
step one, 60-80 wt% of fused magnesia aggregate, 10-30 wt% of fused magnesia fine powder, 1-4 wt% of aluminum powder, 1-4 wt% of silicon powder, 1-4 wt% of flake graphite and 1-5 wt% of C @ Cr3C2The composite powder is used as a raw material, and phenolic resin accounting for 3.5-6 wt% of the raw material is added; firstly, the aluminum powder, the silicon powder and the C @ Cr3C2Premixing the composite powder in a mixer to obtain a mixture I, and taking out for later use; and adding the fused magnesia aggregate into a stirrer, stirring for 3-6 min, adding the phenolic resin, stirring for 3-5 min, adding the fused magnesia fine powder and the mixture I, stirring for 3-6 min, finally adding the crystalline flake graphite, and stirring for 5-10 min to obtain a mixture II.
Step two, pressing and molding the mixture II under the condition of 150-200 MPa, solidifying for 24-48 h under the condition of 200-220 ℃, then placing the mixture in an air furnace, preserving the heat for 2-4 h under the conditions of 1200-1500 ℃ and carbon-embedding atmosphere, and naturally cooling to obtain the additive C @ Cr3C2The low-carbon magnesia-carbon refractory material of the composite powder.
The MgO content of the fused magnesia aggregate is more than or equal to 97 wt%; the granularity of the fused magnesia aggregate is more than or equal to 0.1 and less than or equal to 3 mm.
The MgO content of the fused magnesia fine powder is more than or equal to 97 wt%; the granularity of the fused magnesia fine powder is less than 0.1 mm.
The Al content of the aluminum powder is more than or equal to 99.0 wt%; the granularity of the aluminum powder is less than or equal to 0.15 mm.
The Si content of the silicon powder is more than or equal to 99.0 wt%; the granularity of the silicon powder is less than or equal to 0.15 mm.
The C content of the flake graphite is more than or equal to 97 wt%; the particle size of the flake graphite is less than or equal to 0.15 mm.
The C @ Cr3C2The composite powder is synthesized in situ on the surface of the crystalline flake graphite by adopting a low-temperature liquid phase method, wherein C @ Cr3C2The composite powder is of a core-shell structure, Cr3C2Coating the surface of the crystalline flake graphite with a shell, Cr3C2The content of (B) is 70-90 wt%.
The phenolic resin is thermosetting phenolic resin, the viscosity is 1000-3000 mPa & s, and the content of free phenol is 8-12 wt%.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
the invention mixes the fused magnesia aggregate, fused magnesia fine powder, aluminum powder, silicon powder, crystalline flake graphite, C @ Cr3C2The composite powder and the phenolic resin are mixed, pressed, molded and cured, and then the mixture is placed in an air furnace and sintered at 1200-1500 ℃ under the condition of carbon-embedded atmosphere, so that the process is simple, the preparation period is short, and the industrial production is easy. The main raw materials used in the invention are all available in the market, the price is low, and the production cost is low.
C @ Cr added in the invention3C2Composite powder of Cr3C2The coating is coated on the surface of the crystalline flake graphite, so that the oxidation resistance of the crystalline flake graphite can be obviously improved, and the crystalline flake graphite is endowed with excellent corrosion resistance. Adding C @ Cr3C2The composite powder is added into the low-carbon magnesium-carbon refractory material, so that the oxidation resistance of the product is improved, the loose structure of the low-carbon magnesium-carbon refractory material caused by oxidation is reduced, and the strength of the product is improved; then Cr adopted by the invention3C2Cr generated by reduction under carbon-buried atmosphere2O3Can form MgCr with MgO2O4A ceramic phase, further improving the strength of the article. In addition, Cr2O3Can also reduce the erosion of the slag to the product and improve the slag resistance of the product.
The additive C @ Cr prepared by the invention3C2The low-carbon magnesia-carbon refractory material of the composite powder is tested: the normal-temperature breaking strength is 11-16 MPa; the normal-temperature compressive strength is 42-59 MPa; compared with the existing low-carbon magnesia carbon refractory material, the oxidation depth is reduced by 22-40%, and the slag erosion depth is reduced by 15-25%.
Therefore, the invention has the characteristics of low cost, simple production process and easy industrial production, and the prepared additive C @ Cr3C2The low-carbon magnesium-carbon refractory material of the composite powder has high strength, excellent oxidation resistance and excellent slag resistance.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
C @ Cr addition method3C2A low-carbon magnesia-carbon refractory material of composite powder and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, 60-80 wt% of fused magnesia aggregate, 10-30 wt% of fused magnesia fine powder, 1-4 wt% of aluminum powder, 1-4 wt% of silicon powder, 1-4 wt% of flake graphite and 1-5 wt% of C @ Cr3C2The composite powder is used as a raw material, and phenolic resin accounting for 3.5-6 wt% of the raw material is added; firstly, the aluminum powder, the silicon powder and the C @ Cr3C2Premixing the composite powder in a mixer to obtain a mixture I, and taking out for later use; and adding the fused magnesia aggregate into a stirrer, stirring for 3-6 min, adding the phenolic resin, stirring for 3-5 min, adding the fused magnesia fine powder and the mixture I, stirring for 3-6 min, finally adding the crystalline flake graphite, and stirring for 5-10 min to obtain a mixture II.
Step two, pressing and molding the mixture II under the condition of 150-200 MPa, solidifying for 24-48 h under the condition of 200-220 ℃, then placing the mixture in an air furnace, preserving the heat for 2-4 h under the conditions of 1200-1500 ℃ and carbon-embedding atmosphere, and naturally cooling to obtain the additive C @ Cr3C2The low-carbon magnesia-carbon refractory material of the composite powder.
In this embodiment:
the MgO content of the fused magnesia aggregate is more than or equal to 97 wt%; the granularity of the fused magnesia aggregate is more than or equal to 0.1 and less than or equal to 3 mm.
The MgO content of the fused magnesia fine powder is more than or equal to 97 wt%; the granularity of the fused magnesia fine powder is less than 0.1 mm.
The Al content of the aluminum powder is more than or equal to 99.0 wt%; the granularity of the aluminum powder is less than or equal to 0.15 mm.
The Si content of the silicon powder is more than or equal to 99.0 wt%; the granularity of the silicon powder is less than or equal to 0.15 mm.
The C content of the flake graphite is more than or equal to 97 wt%; the particle size of the flake graphite is less than or equal to 0.15 mm.
The C @ Cr3C2The composite powder is synthesized in situ on the surface of the crystalline flake graphite by adopting a low-temperature liquid phase method, wherein C @ Cr3C2The composite powder is of a core-shell structure, Cr3C2Coating the surface of the crystalline flake graphite with a shell, Cr3C2The content of (B) is 70-90 wt%.
The phenolic resin is thermosetting phenolic resin, the viscosity is 1000-3000 mPa & s, and the content of free phenol is 8-12 wt%.
The detailed description is omitted in the embodiments.
Example 1
C @ Cr addition method3C2A low-carbon magnesia-carbon refractory material of composite powder and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, 60 wt% of fused magnesia aggregate, 30 wt% of fused magnesia fine powder, 4 wt% of aluminum powder, 1 wt% of silicon powder, 4 wt% of flake graphite and 1 wt% of C @ Cr3C2The composite powder is taken as a raw material, and is added with phenolic resin accounting for 3.5 wt% of the raw material; firstly, the aluminum powder, the silicon powder and the C @ Cr3C2Premixing the composite powder in a mixer to obtain a mixture I, and taking out for later use; adding the fused magnesia aggregate into a stirrer, stirring for 3min, adding the phenolic resin, stirring for 5min, adding the fused magnesia fine powder and the mixture I, stirring for 6min, adding the crystalline flake graphite, and stirring for 6min to obtain the fused magnesia aggregateTo a mix II.
Step two, pressing and molding the mixture II under the condition of 150MPa, solidifying for 24 hours at the temperature of 200 ℃, then placing the mixture in an air furnace, preserving the heat for 2 hours at the temperature of 1200 ℃ under the condition of carbon-embedded atmosphere, and naturally cooling to obtain the additive C @ Cr3C2The low-carbon magnesia-carbon refractory material of the composite powder.
The additive C @ Cr prepared by the invention3C2The low-carbon magnesia-carbon refractory material of the composite powder is tested: the normal temperature rupture strength is 11.37 MPa; the normal temperature compressive strength is 42.26 MPa; compared with the existing low-carbon magnesia-carbon refractory material, the oxidation depth is reduced by 22.83 percent, and the slag erosion depth is reduced by 15.46 percent.
Example 2
C @ Cr addition method3C2A low-carbon magnesia-carbon refractory material of composite powder and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, 65 wt% of fused magnesia aggregate, 25 wt% of fused magnesia fine powder, 3 wt% of aluminum powder, 2 wt% of silicon powder, 3 wt% of flake graphite and 2 wt% of C @ Cr3C2The composite powder is taken as a raw material, and is added with phenolic resin accounting for 4.5 wt% of the raw material; firstly, the aluminum powder, the silicon powder and the C @ Cr3C2Premixing the composite powder in a mixer to obtain a mixture I, and taking out for later use; and adding the fused magnesia aggregate into a stirrer, stirring for 4min, adding the phenolic resin, stirring for 4min, adding the fused magnesia fine powder and the mixture I, stirring for 5min, adding the crystalline flake graphite, and stirring for 7min to obtain a mixture II.
Step two, pressing and molding the mixture II under the condition of 160MPa, solidifying for 36 hours at the temperature of 210 ℃, then placing the mixture in an air furnace, preserving the heat for 3 hours at the temperature of 1300 ℃ under the condition of carbon-embedded atmosphere, and naturally cooling to obtain the additive C @ Cr3C2The low-carbon magnesia-carbon refractory material of the composite powder.
The additive C @ Cr prepared by the invention3C2The low-carbon magnesia-carbon refractory material of the composite powder is tested: the normal temperature rupture strength is 12.64 MPa; the normal temperature compressive strength is 57.91 MPa; compared with the prior low-carbon magnesia-carbon refractory materialCompared with the material, the oxidation depth is reduced by 25.36 percent, and the slag erosion depth is reduced by 18.72 percent.
Example 3
C @ Cr addition method3C2A low-carbon magnesia-carbon refractory material of composite powder and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, 70 wt% of fused magnesia aggregate, 20 wt% of fused magnesia fine powder, 2 wt% of aluminum powder, 3 wt% of silicon powder, 2 wt% of flake graphite and 3 wt% of C @ Cr3C2The composite powder is taken as a raw material, and 5 wt% of phenolic resin is added; firstly, the aluminum powder, the silicon powder and the C @ Cr3C2Premixing the composite powder in a mixer to obtain a mixture I, and taking out for later use; and adding the fused magnesia aggregate into a stirrer, stirring for 5min, adding the phenolic resin, stirring for 3min, adding the fused magnesia fine powder and the mixture I, stirring for 4min, adding the crystalline flake graphite, and stirring for 8min to obtain a mixture II.
Step two, pressing and molding the mixture II under the condition of 170MPa, solidifying for 48 hours at the temperature of 220 ℃, then placing the mixture in an air furnace, preserving the heat for 4 hours at the temperature of 1400 ℃ under the condition of carbon-embedded atmosphere, and naturally cooling to obtain the additive C @ Cr3C2The low-carbon magnesia-carbon refractory material of the composite powder.
The additive C @ Cr prepared by the invention3C2The low-carbon magnesia-carbon refractory material of the composite powder is tested: the normal temperature rupture strength is 15.87 MPa; the normal temperature compressive strength is 58.96 MPa; compared with the existing low-carbon magnesia-carbon refractory material, the oxidation depth is reduced by 39.15%, and the slag erosion depth is reduced by 24.92%.
Example 4
C @ Cr addition method3C2A low-carbon magnesia-carbon refractory material of composite powder and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, 75 wt% of fused magnesia aggregate, 15 wt% of fused magnesia fine powder, 1 wt% of aluminum powder, 4 wt% of silicon powder, 1 wt% of flake graphite and 4 wt% of C @ Cr3C2The composite powder is used as raw material, and the raw material is added5.5 wt% of a phenolic resin; firstly, the aluminum powder, the silicon powder and the C @ Cr3C2Premixing the composite powder in a mixer to obtain a mixture I, and taking out for later use; and adding the fused magnesia aggregate into a stirrer, stirring for 6min, adding the phenolic resin, stirring for 4min, adding the fused magnesia fine powder and the mixture I, stirring for 5min, adding the crystalline flake graphite, and stirring for 9min to obtain a mixture II.
Step two, pressing and molding the mixture II under the condition of 180MPa, solidifying for 36 hours at the temperature of 220 ℃, then placing the mixture in an air furnace, preserving the heat for 4 hours at the temperature of 1500 ℃ under the condition of carbon-embedded atmosphere, and naturally cooling to obtain the additive C @ Cr3C2The low-carbon magnesia-carbon refractory material of the composite powder.
The additive C @ Cr prepared by the invention3C2The low-carbon magnesia-carbon refractory material of the composite powder is tested: the normal temperature rupture strength is 14.38 MPa; the normal temperature compressive strength is 46.51 MPa; compared with the existing low-carbon magnesia-carbon refractory material, the oxidation depth is reduced by 33.64%, and the slag erosion depth is reduced by 21.89%.
Example 5
C @ Cr addition method3C2A low-carbon magnesia-carbon refractory material of composite powder and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, 80 wt% of fused magnesia aggregate, 10 wt% of fused magnesia fine powder, 1 wt% of aluminum powder, 3 wt% of silicon powder, 1 wt% of flake graphite and 5 wt% of C @ Cr3C2The composite powder is taken as a raw material, and phenolic resin accounting for 6 wt% of the raw material is added; firstly, the aluminum powder, the silicon powder and the C @ Cr3C2Premixing the composite powder in a mixer to obtain a mixture I, and taking out for later use; and adding the fused magnesia aggregate into a stirrer, stirring for 6min, adding the phenolic resin, stirring for 3min, adding the fused magnesia fine powder and the mixture I, stirring for 4min, adding the crystalline flake graphite, and stirring for 10min to obtain a mixture II.
Step two, the mixture II is pressed and formed under the condition of 200MPa, solidified for 36 hours under the condition of 210 ℃, and then placed in the airKeeping the temperature in a furnace for 3h at 1350 ℃ under the condition of carbon-embedded atmosphere, and naturally cooling to obtain the additive C @ Cr3C2The low-carbon magnesia-carbon refractory material of the composite powder.
The additive C @ Cr prepared by the invention3C2The low-carbon magnesia-carbon refractory material of the composite powder is tested: the normal temperature rupture strength is 13.49 MPa; the normal temperature compressive strength is 48.76 MPa; compared with the existing low-carbon magnesia-carbon refractory material, the oxidation depth is reduced by 28.61%, and the slag erosion depth is reduced by 19.63%.
Compared with the prior art, the specific implementation mode has the following positive effects:
the specific embodiment is that the fused magnesia aggregate, the fused magnesia fine powder, the aluminum powder, the silicon powder, the crystalline flake graphite and the C @ Cr are mixed3C2The composite powder and the phenolic resin are mixed, pressed, molded and cured, and then the mixture is placed in an air furnace and sintered at 1200-1500 ℃ under the condition of carbon-embedded atmosphere, so that the process is simple, the preparation period is short, and the industrial production is easy. The main raw materials used in the embodiment are all available in the market, and the cost is low and the production cost is low.
C @ Cr added in the present embodiment3C2Composite powder of Cr3C2The coating is coated on the surface of the crystalline flake graphite, so that the oxidation resistance of the crystalline flake graphite can be obviously improved, and the crystalline flake graphite is endowed with excellent corrosion resistance. Adding C @ Cr3C2The composite powder is added into the low-carbon magnesium-carbon refractory material, so that the oxidation resistance of the product is improved, the loose structure of the low-carbon magnesium-carbon refractory material caused by oxidation is reduced, and the strength of the product is improved; cr used in the present embodiment3C2Cr generated by reduction under carbon-buried atmosphere2O3Can form MgCr with MgO2O4A ceramic phase, further improving the strength of the article. In addition, Cr2O3Can also reduce the erosion of the slag to the product and improve the slag resistance of the product.
The added C @ Cr prepared by the specific embodiment3C2The low-carbon magnesia-carbon refractory material of the composite powder is tested: the normal-temperature breaking strength is 11-16 MPa; the normal-temperature compressive strength is 42-59 MPa; compared with the prior low-carbon magnesia carbonCompared with the refractory material, the oxidation depth is reduced by 22-40%, and the slag erosion depth is reduced by 15-25%.
Therefore, the specific implementation mode has the characteristics of low cost, simple production process and easy industrial production, and the prepared C @ Cr additive3C2The low-carbon magnesium-carbon refractory material of the composite powder has high strength, excellent oxidation resistance and excellent slag resistance.
Claims (9)
1. C @ Cr addition method3C2The preparation method of the low-carbon magnesia-carbon refractory material of the composite powder is characterized by comprising the following steps:
step one, 60-80 wt% of fused magnesia aggregate, 10-30 wt% of fused magnesia fine powder, 1-4 wt% of aluminum powder, 1-4 wt% of silicon powder, 1-4 wt% of flake graphite and 1-5 wt% of C @ Cr3C2The composite powder is used as a raw material, and phenolic resin accounting for 3.5-6 wt% of the raw material is added; firstly, the aluminum powder, the silicon powder and the C @ Cr3C2Premixing the composite powder in a mixer to obtain a mixture I, and taking out for later use; adding the fused magnesia aggregate into a stirrer, stirring for 3-6 min, adding the phenolic resin, stirring for 3-5 min, adding the fused magnesia fine powder and the mixture I, stirring for 3-6 min, finally adding the crystalline flake graphite, and stirring for 5-10 min to obtain a mixture II;
step two, pressing and molding the mixture II under the condition of 150-200 MPa, solidifying for 24-48 h under the condition of 200-220 ℃, then placing the mixture in an air furnace, preserving the heat for 2-4 h under the conditions of 1200-1500 ℃ and carbon-embedding atmosphere, and naturally cooling to obtain the additive C @ Cr3C2The low-carbon magnesia-carbon refractory material of the composite powder.
2. The addition of C @ Cr as claimed in claim 13C2The preparation method of the low-carbon magnesia carbon refractory material of the composite powder is characterized in that the MgO content of the fused magnesia aggregate is more than or equal to 97 wt%; the granularity of the fused magnesia aggregate is more than or equal to 0.1 and less than or equal to 3 mm.
3. The addition of C @ Cr as claimed in claim 13C2The preparation method of the low-carbon magnesia-carbon refractory material of the composite powder is characterized in that the MgO content of the fused magnesia fine powder is more than or equal to 97 wt%; the granularity of the fused magnesia fine powder is less than 0.1 mm.
4. The addition of C @ Cr as claimed in claim 13C2The preparation method of the low-carbon magnesia-carbon refractory material of the composite powder is characterized in that the Al content of the aluminum powder is more than or equal to 99.0 wt%; the granularity of the aluminum powder is less than or equal to 0.15 mm.
5. The addition of C @ Cr as claimed in claim 13C2The preparation method of the low-carbon magnesia-carbon refractory material of the composite powder is characterized in that the Si content of the silicon powder is more than or equal to 99.0 wt%; the granularity of the silicon powder is less than or equal to 0.15 mm.
6. The addition of C @ Cr as claimed in claim 13C2The preparation method of the low-carbon magnesia-carbon refractory material of the composite powder is characterized in that the C content of the crystalline flake graphite is more than or equal to 97 wt%; the particle size of the flake graphite is less than or equal to 0.15 mm.
7. The addition of C @ Cr as claimed in claim 13C2The preparation method of the low-carbon magnesia-carbon refractory material of the composite powder is characterized in that C @ Cr3C2The composite powder is synthesized in situ on the surface of the crystalline flake graphite by adopting a low-temperature liquid phase method, wherein C @ Cr3C2The composite powder is of a core-shell structure, Cr3C2Coating the surface of the crystalline flake graphite with a shell, Cr3C2The content of (B) is 70-90 wt%.
8. The addition of C @ Cr as claimed in claim 13C2The preparation method of the low-carbon magnesia-carbon refractory material of the composite powder is characterized in that the phenolic resin is thermosetting phenolic resin, the viscosity is 1000-3000 mPa.s, and the content of free phenol is 8-12 wt%.
9. C @ Cr addition method3C2The low-carbon magnesia-carbon refractory material of the composite powder is characterized in that C @ Cr is added3C2The low-carbon magnesia-carbon refractory material of the composite powder is prepared by adding C @ Cr according to any one of claims 1 to 83C2C @ Cr-added low-carbon magnesia-carbon refractory material prepared by preparation method of composite powder3C2The low-carbon magnesia-carbon refractory material of the composite powder.
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