CN118515470A - Antioxidant low-carbon magnesia carbon brick and preparation process thereof - Google Patents
Antioxidant low-carbon magnesia carbon brick and preparation process thereof Download PDFInfo
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- CN118515470A CN118515470A CN202410985918.XA CN202410985918A CN118515470A CN 118515470 A CN118515470 A CN 118515470A CN 202410985918 A CN202410985918 A CN 202410985918A CN 118515470 A CN118515470 A CN 118515470A
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- magnesia
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- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 365
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 186
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 183
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 143
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 96
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 94
- 239000011449 brick Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 33
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 23
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000003647 oxidation Effects 0.000 claims abstract description 22
- 239000005011 phenolic resin Substances 0.000 claims abstract description 22
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 22
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 21
- 239000010439 graphite Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000005303 weighing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000000748 compression moulding Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 70
- 239000000463 material Substances 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 13
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 12
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052580 B4C Inorganic materials 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910026551 ZrC Inorganic materials 0.000 claims description 8
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 230000003064 anti-oxidating effect Effects 0.000 claims description 8
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 8
- 239000011863 silicon-based powder Substances 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 7
- 229920001187 thermosetting polymer Polymers 0.000 claims description 6
- 239000011819 refractory material Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 21
- 238000000034 method Methods 0.000 description 8
- 239000010410 layer Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 230000002829 reductive effect Effects 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- NFMWFGXCDDYTEG-UHFFFAOYSA-N trimagnesium;diborate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]B([O-])[O-].[O-]B([O-])[O-] NFMWFGXCDDYTEG-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005261 decarburization Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 238000006467 substitution reaction Methods 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
- C04B35/0435—Refractories from grain sized mixtures containing refractory metal compounds other than chromium oxide or chrome ore
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
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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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
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- 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
- C04B2235/3804—Borides
- C04B2235/3813—Refractory metal borides
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
- C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
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Abstract
The invention discloses an antioxidant low-carbon magnesia carbon brick and a preparation process thereof, which belong to the technical field of refractory material production, and firstly, the antioxidant low-carbon magnesia carbon brick comprises the following raw materials in parts by weight: 20-25 parts of fused magnesia with granularity of 3-5 mm; 25-30 parts of fused magnesia with granularity of 1-3 mm; 20-30 parts of fused magnesia with granularity less than or equal to 1 mm; 7-10 parts of flake graphite; 1-4 parts of an antioxidant; 3-4 parts of phenolic resin. Then, the preparation process comprises the following steps: crushing blocky magnesia into fused magnesia with the granularity, weighing the raw materials according to the weight parts, and carrying out high-speed mixing, compression molding, drying and cooling on the fused magnesia, the crystalline flake graphite, the phenolic resin and the antioxidant to obtain the antioxidant low-carbon magnesia carbon brick. The low-carbon magnesia carbon brick prepared by the invention has excellent oxidation resistance (the thickness of the decarburized layer is less than or equal to 5.0mm under the treatment condition of 1400 ℃/2 h).
Description
Technical Field
The invention belongs to the technical field of refractory material production, and particularly relates to an antioxidant low-carbon magnesia carbon brick and a preparation process thereof.
Background
The magnesia carbon brick is mainly composed of magnesia, graphite (or other carbon sources), binding agent and other additives.
Magnesia carbon bricks are widely used in converter linings due to excellent high-temperature mechanical properties, good slag erosion resistance and thermal shock resistance.
However, the higher the carbon content in the magnesia carbon brick, the stronger the heat conduction capability, which causes the temperature of the molten steel to drop rapidly. In addition, when smelting low carbon steel and ultra low carbon steel, the high carbon magnesia carbon bricks can cause molten steel pollution. Therefore, low carbon magnesia carbon bricks are one of the trends in refractory materials.
Low carbon magnesia carbon bricks generally refer to MgO-C refractory materials having a total carbon content of no more than 8% by weight. However, when the carbon content is reduced, the problem of oxidation exfoliation of magnesia carbon bricks at high temperature is significantly increased, because: carbon in the magnesia carbon bricks can not form a continuous and complete carbon isolation layer in the high-temperature use process, so that the low-carbon magnesia carbon bricks are easy to oxidize and decarbonize under the high-temperature condition, and meanwhile, after the carbon content is reduced, the wettability of molten steel and the magnesia carbon bricks is enhanced, and the oxidation and spalling resistance of the magnesia carbon bricks is obviously reduced along with the erosion and mechanical scouring of the molten steel.
Aiming at the technical problems, the prior art makes the following improvements:
The Chinese patent with the publication number of CN115893990B discloses a low-carbon magnesia carbon brick, which aims to reduce the carbon content and realize the low-carbon aim of the magnesia carbon brick by adding self-made ZrB 2 -C composite powder to replace part or all of crystalline flake graphite, and can effectively protect C from oxidation based on ZrB 2, and B 2O3 generated after the oxidation of ZrB 2 reacts with MgO to generate low-melting magnesium borate, so that pores inside the magnesia carbon brick can be filled, air diffusion is blocked, and the aim of antioxidation is further realized.
The invention further improves the oxidation resistance of the low-carbon magnesia carbon brick on the basis of the prior art.
Disclosure of Invention
The invention provides an antioxidant low-carbon magnesia carbon brick and a preparation process thereof, and aims to improve the antioxidant property of the low-carbon magnesia carbon brick.
The aim of the invention can be achieved by the following technical scheme:
an antioxidant low-carbon magnesia carbon brick comprises the following raw materials in parts by weight:
20-25 parts of fused magnesia with granularity of 3-5 mm;
25-30 parts of fused magnesia with granularity of 1-3 mm;
20-30 parts of fused magnesia with granularity less than or equal to 1 mm;
7-10 parts of flake graphite;
1-4 parts of an antioxidant;
3-4 parts of phenolic resin;
the antioxidant is prepared by the following steps:
Adding absolute ethyl alcohol, al 4SiC4 powder, nickel oxide powder and ZrB 2 powder into pure water under stirring, stirring and mixing for 30min, adding a silane coupling agent into the mixture under stirring, continuing stirring for 30-40 min after the addition is finished, carrying out suction filtration, and drying a solid component to constant weight to obtain the antioxidant.
Further, the dosage ratio of the pure water, the absolute ethyl alcohol, the Al 4SiC4 powder, the nickel oxide powder, the ZrB 2 powder and the silane coupling agent is 100 mL:45-80 mL:17-18 g:3.2-3.5 g:11-12 g:3-5 g.
Further, the silane coupling agent is one of KH-540, KH-550, KH-560 and KH-570.
Further, the Al 4SiC4 powder is prepared by the following steps:
Mixing metal aluminum powder, metal silicon powder and carbon black according to a molar ratio of 4:1:4, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1600-1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain Al 4SiC4 powder.
Further, the ZrB 2 powder is prepared by the following steps:
Weighing zirconium carbide and boron carbide according to a molar ratio of 2:1, mixing, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1600-1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain ZrB 2 powder.
Further, the carbon content of the flake graphite is more than 99.5 weight percent, and the granularity is less than or equal to 0.15mm.
Further, the phenolic resin is PF-5323 type thermosetting phenolic resin.
Further, the preparation process of the antioxidant low-carbon magnesia carbon brick comprises the following steps of:
s1, crushing blocky magnesia into fused magnesia with granularity of 3-5 mm, fused magnesia with granularity of 1-3 mm and fused magnesia with granularity less than or equal to 1 mm;
S2, weighing the raw materials according to the weight parts, carrying out high-speed mixing on the fused magnesia with the granularity of 3-5 mm, the fused magnesia with the granularity of 1-3 mm, the fused magnesia with the granularity of less than or equal to 1mm, crystalline flake graphite, phenolic resin and an antioxidant for 5-10min, carrying out compression molding after mixing to obtain a magnesia carbon brick rough blank, drying the rough blank at the constant temperature of 200 ℃ for 12h, taking out, and cooling to room temperature to obtain the antioxidant low-carbon magnesia carbon brick.
Further, the magnesia content of the blocky magnesia in S1 is more than or equal to 97.5 percent.
Further, the weight ratio of the fused magnesia with the granularity less than or equal to 0.088mm in the fused magnesia with the granularity less than or equal to 1mm in the S2 is 5-10%.
The invention has the beneficial effects that:
the invention provides an antioxidant low-carbon magnesia carbon brick and a preparation process thereof, and the prepared low-carbon magnesia carbon brick has excellent antioxidant performance (the thickness of a decarburized layer is less than or equal to 5.0mm under the treatment condition of 1400 ℃/2 h).
The low-carbon magnesia carbon brick prepared by the invention mainly comprises fused magnesia and carbon components (crystalline graphite), wherein the carbon components are the connection tie of the whole magnesia carbon brick, so that on the basis of preparing a low-carbon magnesia carbon brick product, ensuring the integrity of the carbon components is very critical, namely, the oxidation of the carbon components in the magnesia carbon brick is required to be prevented, on the basis, the occurrence of the oxidation process in the low-carbon magnesia carbon brick can be inhibited by reducing the porosity, and further, the carbon loss in the low-carbon magnesia carbon brick is reduced by reducing CO gas to generate solid carbon, thereby ensuring the stable structure of the finally prepared antioxidant magnesia carbon brick, reducing the deterioration rate of the magnesia carbon brick structure and obviously reducing the thickness of a decarburized layer.
Specifically:
On one hand, the low-carbon magnesia carbon brick comprises the fused magnesia with gradient particle size distribution and the crystalline flake graphite, and further, the fused magnesia consists of the particle size components with gradient distribution, so that the density of the finally prepared low-carbon magnesia carbon brick is ensured, the porosity is reduced, the oxidation process inside the low-carbon magnesia carbon brick is further inhibited, and the oxidation resistance is improved.
On the other hand, the self-made antioxidant is added into the low-carbon magnesia carbon brick, and the self-made antioxidant is prepared by mixing Al 4SiC4 powder, nickel oxide powder and ZrB 2 powder and then modifying the mixture by a silane coupling agent, wherein the Al 4SiC4 powder has the effects of reducing apparent porosity, inhibiting carbon oxidation, improving density, forming a protective layer, improving thermal strength, promoting graphite crystal growth and the like; zrB 2 can be subjected to oxidation reaction under the high temperature condition, and B 2O3,B2O3 which generates a glass state can react with MgO to generate magnesium borate with a low melting point, so that pores in the magnesia carbon brick can be filled, and air diffusion is blocked; the nickel oxide powder can promote the Boudeuard reaction, realize the purpose of reducing CO gas to generate solid carbon to reduce carbon loss in the low-carbon magnesia carbon brick, ensure the stable structure of the anti-magnesia carbon brick, improve the stability of the finally prepared low-carbon magnesia carbon brick, and reduce the occurrence probability of decarburization stripping problems.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1: preparation of an antioxidant:
First, zrB 2 powder was prepared:
Weighing zirconium carbide and boron carbide according to a molar ratio of 2:1, mixing, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1600 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain ZrB 2 powder.
Then, al 4SiC4 powder was prepared:
Mixing metal aluminum powder (100 meshes), metal silicon powder (80 meshes) and carbon black according to a molar ratio of 4:1:4, ball milling for 24 hours under a nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1600 ℃, preserving heat for 4 hours, and cooling to room temperature along with a furnace to obtain Al 4SiC4 powder.
Finally, an antioxidant is prepared:
45mL of absolute ethyl alcohol, 17g of Al 4SiC4 powder, 3.2g of nickel oxide powder (300 meshes) and 11g of ZrB 2 powder are added into 100mL of pure water under stirring, the mixture is stirred and mixed for 30min, 3g of silane coupling agent (KH-540) is added into the mixture under stirring, after the addition is finished, the mixture is stirred for 30min continuously, suction filtration is carried out, and the solid component is dried to constant weight, thus obtaining the antioxidant.
Example 2: preparation of an antioxidant:
First, zrB 2 powder was prepared:
weighing zirconium carbide and boron carbide according to a molar ratio of 2:1, mixing, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1620 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain ZrB 2 powder.
Then, al 4SiC4 powder was prepared:
Mixing metal aluminum powder (100 meshes), metal silicon powder (80 meshes) and carbon black according to a molar ratio of 4:1:4, ball milling for 24 hours under a nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1620 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain Al 4SiC4 powder.
Finally, an antioxidant is prepared:
60mL of absolute ethyl alcohol, 17.5g of Al 4SiC4 powder, 3.3g of nickel oxide powder (300 meshes) and 11.5g of ZrB 2 powder are added into 100mL of pure water under stirring, the mixture is stirred and mixed for 30min, 5g of silane coupling agent (KH-550) is added into the mixture under stirring, after the addition is finished, the mixture is continuously stirred for 40min, suction filtration is carried out, and the solid component is dried to constant weight, so that the antioxidant is obtained.
Example 3: preparation of an antioxidant:
First, zrB 2 powder was prepared:
weighing zirconium carbide and boron carbide according to a molar ratio of 2:1, mixing, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain ZrB 2 powder.
Then, al 4SiC4 powder was prepared:
Mixing metal aluminum powder (100 meshes), metal silicon powder (80 meshes) and carbon black according to a molar ratio of 4:1:4, ball milling for 24 hours under a nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain Al 4SiC4 powder.
Finally, an antioxidant is prepared:
80mL of absolute ethyl alcohol, 18g of Al 4SiC4 powder, 3.4g of nickel oxide powder (300 meshes) and 12g of ZrB 2 powder are added into 100mL of pure water under stirring, the mixture is stirred and mixed for 30min, 5g of silane coupling agent (KH-560) is added into the mixture under stirring, after the addition is finished, stirring is continued for 40min, suction filtration is carried out, and the solid component is dried to constant weight, thus obtaining the antioxidant.
Example 4: preparation of an antioxidant:
First, zrB 2 powder was prepared:
weighing zirconium carbide and boron carbide according to a molar ratio of 2:1, mixing, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain ZrB 2 powder.
Then, al 4SiC4 powder was prepared:
Mixing metal aluminum powder (100 meshes), metal silicon powder (80 meshes) and carbon black according to a molar ratio of 4:1:4, ball milling for 24 hours under a nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain Al 4SiC4 powder.
Finally, an antioxidant is prepared:
80mL of absolute ethyl alcohol, 18g of Al 4SiC4 powder, 3.5g of nickel oxide powder (300 meshes) and 12g of ZrB 2 powder are added into 100mL of pure water under stirring, the mixture is stirred and mixed for 30min, 5g of silane coupling agent (KH-570) is added into the mixture under stirring, after the addition is finished, stirring is continued for 40min, suction filtration is carried out, and the solid component is dried to constant weight, so that the antioxidant is obtained.
Comparative example 1
Preparation of an antioxidant:
Comparative example 1 is a control group of example 3, the nickel oxide powder (300 mesh) of example 3 was removed, the remaining raw materials and the preparation method thereof were kept unchanged, and finally an antioxidant was obtained, namely, the preparation process of the antioxidant was as follows:
First, zrB 2 powder was prepared:
weighing zirconium carbide and boron carbide according to a molar ratio of 2:1, mixing, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain ZrB 2 powder.
Then, al 4SiC4 powder was prepared:
Mixing metal aluminum powder (100 meshes), metal silicon powder (80 meshes) and carbon black according to a molar ratio of 4:1:4, ball milling for 24 hours under a nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain Al 4SiC4 powder.
Finally, an antioxidant is prepared:
Adding 80mL of absolute ethyl alcohol, 18g of Al 4SiC4 powder and 12g of ZrB 2 powder into 100mL of pure water under stirring, stirring and mixing for 30min, adding 5g of silane coupling agent (KH-560) under stirring, continuing stirring for 40min after the addition is finished, filtering, and drying the solid component to constant weight to obtain the antioxidant.
Comparative example 2
Preparation of an antioxidant:
Comparative example 2 is a control group of example 3, the silane coupling agent (KH-560) of example 3 was removed, the remaining raw materials and the preparation method thereof were kept unchanged, and finally an antioxidant was obtained, namely, the antioxidant was prepared as follows:
First, zrB 2 powder was prepared:
weighing zirconium carbide and boron carbide according to a molar ratio of 2:1, mixing, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain ZrB 2 powder.
Then, al 4SiC4 powder was prepared:
Mixing metal aluminum powder (100 meshes), metal silicon powder (80 meshes) and carbon black according to a molar ratio of 4:1:4, ball milling for 24 hours under a nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain Al 4SiC4 powder.
Finally, an antioxidant is prepared:
80mL of absolute ethyl alcohol, 18g of Al 4SiC4 powder, 3.4g of nickel oxide powder (300 meshes) and 12g of ZrB 2 powder are added into 100mL of pure water under stirring, the mixture is stirred and mixed for 70min, suction filtration is carried out, and the solid component is dried to constant weight, thus obtaining the antioxidant.
Example 5: preparing an antioxidant low-carbon magnesia carbon brick:
firstly, an antioxidant low-carbon magnesia carbon brick comprises the following raw materials in parts by weight:
20 parts of fused magnesia with granularity of 3-5 mm;
25 parts of fused magnesia with granularity of 1-3 mm;
20 parts of fused magnesia with granularity less than or equal to 1 mm;
7 parts of flake graphite (carbon content is more than 99.5 weight percent, and granularity is less than or equal to 0.15 mm);
1 part of the antioxidant prepared in example 1;
3 parts of a phenolic resin (PF-5323 type thermosetting phenolic resin);
then, the preparation process of the antioxidant low-carbon magnesia carbon brick comprises the following steps:
S1, crushing blocky magnesia with the magnesia content of more than or equal to 97 percent into fused magnesia with the granularity of 3-5 mm, fused magnesia with the granularity of 1-3 mm and fused magnesia with the granularity of less than or equal to 1 mm;
S2, weighing the raw materials according to the weight parts, wherein the weight ratio of the fused magnesia with the granularity less than or equal to 0.088mm in the fused magnesia with the granularity less than or equal to 1mm is 5%, carrying out high-speed mixing on the fused magnesia with the granularity of 3-5 mm, the fused magnesia with the granularity of 1-3 mm, the fused magnesia with the granularity less than or equal to 1mm, flake graphite, phenolic resin and the antioxidant prepared in the example 1, carrying out compression molding after the mixing is completed for 5min, obtaining a magnesia carbon brick rough blank, drying the rough blank at the constant temperature of 200 ℃ for 12h, taking out and cooling to the room temperature, and obtaining the antioxidant low-carbon magnesia carbon brick.
Example 6: preparing an antioxidant low-carbon magnesia carbon brick:
firstly, an antioxidant low-carbon magnesia carbon brick comprises the following raw materials in parts by weight:
22 parts of fused magnesia with granularity of 3-5 mm;
25 parts of fused magnesia with granularity of 1-3 mm;
22 parts of fused magnesia with granularity less than or equal to 1 mm;
8 parts of flake graphite (carbon content is more than 99.5 weight percent, and granularity is less than or equal to 0.15 mm);
2 parts of the antioxidant prepared in example 2;
3 parts of a phenolic resin (PF-5323 type thermosetting phenolic resin);
then, the preparation process of the antioxidant low-carbon magnesia carbon brick comprises the following steps:
S1, crushing blocky magnesia with the magnesia content of more than or equal to 97 percent into fused magnesia with the granularity of 3-5 mm, fused magnesia with the granularity of 1-3 mm and fused magnesia with the granularity of less than or equal to 1 mm;
S2, weighing the raw materials according to the weight parts, wherein the weight ratio of the fused magnesia with the granularity less than or equal to 0.088mm in the fused magnesia with the granularity less than or equal to 1mm is 6%, carrying out high-speed mixing on the fused magnesia with the granularity of 3-5 mm, the fused magnesia with the granularity of 1-3 mm, the fused magnesia with the granularity less than or equal to 1mm, flake graphite, phenolic resin and the antioxidant prepared in the example 2, carrying out compression molding after mixing for 10min, obtaining a magnesia carbon brick rough blank, drying the rough blank at the constant temperature of 200 ℃ for 12h, taking out and cooling to room temperature, and obtaining the antioxidant low-carbon magnesia carbon brick.
Example 7: preparing an antioxidant low-carbon magnesia carbon brick:
firstly, an antioxidant low-carbon magnesia carbon brick comprises the following raw materials in parts by weight:
25 parts of fused magnesia with granularity of 3-5 mm;
25 parts of fused magnesia with granularity of 1-3 mm;
25 parts of fused magnesia with granularity less than or equal to 1 mm;
8 parts of flake graphite (carbon content is more than 99.5 weight percent, and granularity is less than or equal to 0.15 mm);
4 parts of the antioxidant prepared in example 3;
4 parts of a phenolic resin (PF-5323 type thermosetting phenolic resin);
then, the preparation process of the antioxidant low-carbon magnesia carbon brick comprises the following steps:
S1, crushing blocky magnesia with the magnesia content of more than or equal to 97 percent into fused magnesia with the granularity of 3-5 mm, fused magnesia with the granularity of 1-3 mm and fused magnesia with the granularity of less than or equal to 1 mm;
S2, weighing the raw materials according to the weight parts, wherein the weight ratio of the fused magnesia with the granularity less than or equal to 0.088mm in the fused magnesia with the granularity less than or equal to 1mm is 8%, carrying out high-speed mixing on the fused magnesia with the granularity of 3-5 mm, the fused magnesia with the granularity of 1-3 mm, the fused magnesia with the granularity less than or equal to 1mm, flake graphite, phenolic resin and the antioxidant prepared in the example 3, carrying out compression molding after the mixing is completed for 10min, obtaining a magnesia carbon brick rough blank, drying the rough blank at the constant temperature of 200 ℃ for 12h, taking out and cooling to the room temperature, and obtaining the antioxidant low-carbon magnesia carbon brick.
Example 8: preparing an antioxidant low-carbon magnesia carbon brick:
firstly, an antioxidant low-carbon magnesia carbon brick comprises the following raw materials in parts by weight:
25 parts of fused magnesia with granularity of 3-5 mm;
30 parts of fused magnesia with granularity of 1-3 mm;
30 parts of fused magnesia with granularity less than or equal to 1 mm;
10 parts of flake graphite (carbon content is more than 99.5 weight percent, and granularity is less than or equal to 0.15 mm);
4 parts of the antioxidant prepared in example 4;
4 parts of a phenolic resin (PF-5323 type thermosetting phenolic resin);
then, the preparation process of the antioxidant low-carbon magnesia carbon brick comprises the following steps:
S1, crushing blocky magnesia with the magnesia content of more than or equal to 97 percent into fused magnesia with the granularity of 3-5 mm, fused magnesia with the granularity of 1-3 mm and fused magnesia with the granularity of less than or equal to 1 mm;
S2, weighing the raw materials according to the weight parts, wherein the weight ratio of the fused magnesia with the granularity less than or equal to 0.088mm in the fused magnesia with the granularity less than or equal to 1mm is 10 percent, carrying out high-speed mixing on the fused magnesia with the granularity of 3-5 mm, the fused magnesia with the granularity of 1-3 mm, the fused magnesia with the granularity less than or equal to 1mm, flake graphite, phenolic resin and the antioxidant prepared in the example 4, carrying out compression molding after the mixing is completed for 10 minutes, obtaining a magnesia carbon brick rough blank, drying the rough blank at the constant temperature of 200 ℃ for 12 hours, taking out and cooling to the room temperature, and obtaining the antioxidant low-carbon magnesia carbon brick.
Comparative example 3
Preparing an antioxidant low-carbon magnesia carbon brick:
Comparative example 3 is a control group of example 7, the antioxidant prepared in example 7 and starting material example 3 is replaced by Al 4SiC4 powder prepared in example 3, and the rest materials and preparation method are kept unchanged, so that the antioxidant low-carbon magnesia carbon brick is finally obtained.
Comparative example 4
Preparing an antioxidant low-carbon magnesia carbon brick:
Comparative example 4 is a control group of example 7, the antioxidant prepared in example 7 and starting material example 3 is replaced by ZrB 2 powder prepared in example 3, and the rest materials and preparation method are kept unchanged, so that the antioxidant low-carbon magnesia carbon brick is finally obtained.
Comparative example 5
Preparing an antioxidant low-carbon magnesia carbon brick:
Comparative example 5 is a control group of example 7, the antioxidant prepared in example 7 and the antioxidant prepared in example 3 is replaced by the antioxidant prepared in comparative example 1, and the rest raw materials and the preparation method are kept unchanged, so that the antioxidant low-carbon magnesia carbon brick is finally obtained.
Comparative example 6
Preparing an antioxidant low-carbon magnesia carbon brick:
Comparative example 6 is a control group of example 7, the antioxidant prepared in example 7 and the antioxidant prepared in example 3 is replaced by the antioxidant prepared in comparative example 2, and the rest raw materials and the preparation method are kept unchanged, so that the antioxidant low-carbon magnesia carbon brick is finally obtained.
The oxidation resistance test was performed on the oxidation resistant low carbon magnesia carbon bricks prepared in examples 5 to 8 and comparative examples 3 to 6, and the oxidation resistance test procedure was as follows, and the test results are shown in table 1:
Oxidation resistance: the oxidation resistance tests of the oxidation resistant low carbon magnesia carbon bricks prepared in examples 5 to 8 and comparative examples 3 to 6 of the present invention were carried out with reference to the related procedures of the oxidation resistance test in GB/T17732-2008, test method for compact shaped carbon refractory products.
Specifically: the antioxidation low-carbon magnesia carbon bricks prepared in examples 5 to 8 and comparative examples 3 to 6 were taken out in 10 pieces, respectively, and 80 pieces of the antioxidation low-carbon magnesia carbon bricks were cut into cylinders having diameters and heights of 50mm, respectively, and were used as test samples for the antioxidation performance test. And then placing the sample in a heating furnace for oxidation resistance test, wherein the test temperature is set to 1400 ℃, the heating rate of the heating furnace is set to 4 ℃/min, the temperature is kept for 2 hours after the temperature is raised to the test temperature, after the temperature is kept, the sample is cooled to room temperature along with the furnace, the thickness (mm) of a decarburized layer of the sample is measured, and the thickness (mm) is recorded in the following table 1, wherein the smaller the thickness of the decarburized layer is, the better the oxidation resistance is, and the worse the contrary is.
TABLE 1 results of antioxidant property test
| Project | Example 5 | Example 6 | Example 7 | Example 8 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 |
| Thickness of decarburized layer (mm) | ≤5.0 | ≤4.4 | ≤4.2 | ≤4.5 | ≤8.2 | ≤10.4 | ≤7.2 | ≤5.8 |
As can be seen from table 1, the antioxidant prepared by the invention can significantly improve the oxidation resistance of the low-carbon magnesia carbon brick.
It should be noted that in this document, terms such as "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 invention 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 spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (10)
1. An antioxidant low-carbon magnesia carbon brick is characterized by comprising the following raw materials in parts by weight:
20-25 parts of fused magnesia with granularity of 3-5 mm;
25-30 parts of fused magnesia with granularity of 1-3 mm;
20-30 parts of fused magnesia with granularity less than or equal to 1 mm;
7-10 parts of flake graphite;
1-4 parts of an antioxidant;
3-4 parts of phenolic resin;
the antioxidant is prepared by the following steps:
Adding absolute ethyl alcohol, al 4SiC4 powder, nickel oxide powder and ZrB 2 powder into pure water under stirring, stirring and mixing for 30min, adding a silane coupling agent into the mixture under stirring, continuing stirring for 30-40 min after the addition is finished, carrying out suction filtration, and drying a solid component to constant weight to obtain the antioxidant.
2. The antioxidation low-carbon magnesia carbon brick according to claim 1, wherein the dosage ratio of pure water, absolute ethyl alcohol, al 4SiC4 powder, nickel oxide powder, zrB 2 powder and silane coupling agent is 100 mL:45-80 mL:17-18 g:3.2-3.5 g:11-12 g:3-5 g.
3. The antioxidant low carbon magnesia carbon brick of claim 1, wherein the silane coupling agent is one of KH-540, KH-550, KH-560 and KH-570.
4. The antioxidation low-carbon magnesia carbon brick according to claim 1, wherein the Al 4SiC4 powder is prepared by the steps of:
Mixing metal aluminum powder, metal silicon powder and carbon black according to a molar ratio of 4:1:4, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1600-1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain Al 4SiC4 powder.
5. The antioxidation low-carbon magnesia carbon brick according to claim 1, wherein the ZrB 2 powder is prepared by the steps of:
Weighing zirconium carbide and boron carbide according to a molar ratio of 2:1, mixing, ball milling for 24 hours under nitrogen atmosphere to obtain a mixed material, heating the mixed material to 1600-1650 ℃ in a vacuum furnace, preserving heat for 4 hours, and cooling to room temperature along with the furnace to obtain ZrB 2 powder.
6. The antioxidation low-carbon magnesia carbon brick according to claim 1, wherein the carbon content of the crystalline flake graphite is more than 99.5wt% and the granularity is less than or equal to 0.15mm.
7. An oxidation resistant low carbon magnesia carbon brick according to claim 1, wherein the phenolic resin is a PF-5323 type thermosetting phenolic resin.
8. The process for preparing the antioxidant low-carbon magnesia carbon brick according to claim 1, which is characterized by comprising the following steps:
s1, crushing blocky magnesia into fused magnesia with granularity of 3-5 mm, fused magnesia with granularity of 1-3 mm and fused magnesia with granularity less than or equal to 1 mm;
S2, weighing the raw materials according to the weight parts, carrying out high-speed mixing on the fused magnesia with the granularity of 3-5 mm, the fused magnesia with the granularity of 1-3 mm, the fused magnesia with the granularity of less than or equal to 1mm, crystalline flake graphite, phenolic resin and an antioxidant for 5-10min, carrying out compression molding after mixing to obtain a magnesia carbon brick rough blank, drying the rough blank at the constant temperature of 200 ℃ for 12h, taking out, and cooling to room temperature to obtain the antioxidant low-carbon magnesia carbon brick.
9. The process for preparing the antioxidant low-carbon magnesia carbon brick according to claim 8, wherein the magnesia content of the blocky magnesia in S1 is more than or equal to 97.5%.
10. The process for preparing the antioxidant low-carbon magnesia carbon brick according to claim 8, wherein the weight ratio of the fused magnesia with the granularity less than or equal to 0.088mm in the fused magnesia with the granularity less than or equal to 1mm in S2 is 5-10%.
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| CN119390428A (en) * | 2025-01-02 | 2025-02-07 | 弘祥中科(辽宁)耐材有限公司 | Low-carbon magnesia carbon brick and preparation method thereof |
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