CN111348902A - Method for improving oxidation resistance of low-carbon magnesia carbon material - Google Patents
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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
- C04B35/10—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 aluminium oxide
- C04B35/101—Refractories from grain sized mixtures
- C04B35/103—Refractories from grain sized mixtures containing non-oxide refractory materials, e.g. carbon
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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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- 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
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63472—Condensation polymers of aldehydes or ketones
- C04B35/63476—Phenol-formaldehyde condensation polymers
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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
- C04B2235/02—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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- 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
- C04B2235/02—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
- C04B2235/428—Silicon
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Abstract
The invention discloses a method for improving the oxidation resistance of a low-carbon magnesium-carbon material, belonging to the field of refractory materials. The method is characterized in that magnesia, crystalline flake graphite, phenolic resin and polycrystalline silicon waste material which are sintered according to the mass fraction ratio are added in a mixer and fully mixed, wherein the mass fraction ratio of the magnesia to the crystalline flake graphite to the phenolic resin to the polycrystalline silicon waste material is (82% -88%), (4% -7%), (2% -6%), (4% -8%). Then, the milled and mixed raw materials were press-molded in a stainless steel mold. Finally, heat treatment is carried out for 10 hours at 180-200 ℃ to obtain the final product. The invention has the advantages of low cost and obvious oxidation resistance enhancement. Si and SiC in the polycrystalline silicon waste retard the oxidation of carbon and promote the formation of a magnesium oxide dense layer respectively. Can partially or completely replace the antioxidant of the carbon-containing refractory material including the magnesium-carbon material, and has popularization value.
Description
The technical field is as follows:
the invention belongs to the technical field of high-temperature materials, and particularly relates to a method for improving the oxidation resistance of a low-carbon magnesia carbon material.
Background art:
the magnesium-carbon refractory material is one of the most widely researched and applied carbon composite refractory materials, and has attracted extensive attention in the industries such as color, cement and the like besides the steel industry with the most applications. Compared with the traditional refractory material, the magnesia-carbon refractory material has extremely excellent slag resistance and thermal shock resistance. At present, the service life of magnesia carbon bricks (with the carbon content of 12-20%) used for the lining of a converter can even exceed ten thousand heats.
However, with the recent call for domestic industrial transformation, the development goal of the metallurgical industry is also greatly strengthened. Namely, the specific gravity of the specific steel species in the total production of steel is gradually increased. The special steel generally has strict requirements on impurities such as carbon, and the like, so that the development of low-carbon refractory materials such as magnesia carbon bricks and the like is required. Therefore, the magnesium-carbon material industry needs to face and solve the problem of ensuring the performance of the magnesium-carbon material after low carbonization. Because the properties of the magnesium carbon material inevitably deteriorate as the carbon content decreases. Particularly, in the high-temperature service process, once the decarburized layer is formed on the magnesia carbon material with low carbon content, slag and molten metal can easily permeate into the refractory material along pores and grain boundaries, so that the refractory material is corroded and damaged, and even hard spalling occurs.
Obviously, in the trend of the metallurgical industry, the low carbon content of the carbon-containing refractory material is imperative. The oxidation resistance of the low-carbon magnesia carbon material becomes a considerable research hotspot.
The invention content is as follows:
the invention aims to overcome the defect of poor oxidation resistance of the low-carbon magnesia carbon material. A low-carbon magnesium carbon material is prepared by introducing polycrystalline silicon waste materials, and a method for improving the oxidation resistance of the low-carbon magnesium carbon material is provided.
In order to achieve the above object, the present invention adopts the following technical solutions.
A method for improving the oxidation resistance of a low-carbon magnesia carbon material comprises the following specific steps:
firstly, sintering magnesite, carbon, a binder and polycrystalline silicon waste materials according to the mass fraction ratio of (82% -88%), 4% -7%, (2% -6%), and (4% -8%), adding the components, and fully mixing in a mixer. Then, the milled and mixed raw materials were press-molded in a stainless steel mold. And finally, carrying out heat treatment at 180-200 ℃ for 10 h to obtain a final product.
Preferably, the purity of the sintered magnesite is more than or equal to 98.5%, the granularity is 5-3 mm, 3-1 mm and less than or equal to 0.088 mm in three-minute grade.
Preferably, the carbon is high-purity crystalline flake graphite, the purity is more than or equal to 99.5%, and the granularity is less than or equal to 37 mu m.
Preferably, the binder is a thermosetting phenolic resin, a commercial grade, and has a carbonization rate of about 50%.
Preferably, the polysilicon waste material mainly comprises Si, SiC, polyethylene glycol and a small amount of metal. Before the invention is used, the polysilicon waste is subjected to heat treatment at 800 ℃ and magnetic separation to remove polyethylene glycol and metal impurities. Finally, the waste material containing 60-65% of Si, 30-35% of SiC and 5-10% of impurities is obtained.
Preferably, the forming pressure of the pressed green body is 200-250 MPa. The heat treatment equipment is a multi-channel tunnel kiln.
Compared with the prior art, the invention has the beneficial effects that:
it can be seen that the invention does not need to add an antioxidant in the process of preparing the magnesium-carbon material, which can save a great deal of cost expenditure. The polycrystalline silicon scrap serves as an antioxidant for improving the oxidation resistance of the low-carbon magnesia carbon material. Since the main element Si of the polysilicon scrap is one of the commonly used antioxidants.
The decarburization mechanism of magnesia carbon materials for metallurgical facilities such as converters and electric furnaces is mainly gasification by reaction with oxygen in molten steel (C)(s)+[O]=CO(g)) And finely dividing the reaction mixture with magnesite to form magnesium vapor (C)(s)+MgO(s)=Mg(g)+CO(g)). Therefore, how to control the two reactions has a crucial influence on the oxidation resistance of the magnesium-carbon material during high-temperature service. First, the silicon in the polysilicon residue has a greater affinity for oxygen than carbon and can preferentially react with oxygen (Si)(s)+2[O]=SiO2(s)) Secondly, the silicon carbide in the polysilicon scrap can reduce the carbon in the CO (SiC)(s)+2CO=SiO2(s)+3C(s)) To compensate for carbon loss. Meanwhile, the process can reduce the CO partial pressure, increase the analysis of magnesium steam and contribute to the surface densification of the magnesium-carbon materialFormation of the layer (Mg)(g)+[O]=MgO(s)). Once the compact layer is formed, oxygen in the molten metal cannot enter the magnesium-carbon material, so that carbon of the magnesium-carbon material is protected, and the oxidation resistance is greatly improved.
Description of the drawings:
FIG. 1 is a picture of the shape of a refractory material prepared by adding 5% silicon waste after oxidation at 1200 ℃ for 2 h.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
The oxidation resistance tests of the following examples were all conducted in a box-type resistance furnace. Setting relevant parameters according to preset experiment temperature, putting three groups of low-carbon magnesium-carbon samples with the same composition into a resistance furnace, cooling the furnace to normal temperature after the procedure is finished, and taking out the samples. The decarburized layer ratio was calculated by cutting the carbon film in the radial direction with a cutter and measuring the oxidized radial width of the carbon with a vernier caliper. The oxidation resistance of the material is characterized by taking the average value of three samples.
Example 1
A method for improving the oxidation resistance of a low-carbon magnesia carbon material comprises the following specific steps:
the method comprises the steps of firstly, sintering magnesia, crystalline flake graphite, phenolic resin and polycrystalline silicon waste material according to the mass fraction ratio of 82 percent to 7 percent to 6 percent to 5 percent, adding the components, fully mixing in a mixer, then pressing the mixed raw material in a stainless steel mold under 200 MPa to prepare a green compact with phi of 50 × 50 mm, and finally, preserving heat at 180 ℃ for 10 hours to obtain the final product.
The composition of the polycrystalline silicon scrap in this example was 60% Si, 30% SiC and 10% impurity scrap.
The oxidation resistance test results of this example are as follows:
the temperature is kept for 2 hours at 1000 ℃, and the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 17.22 percent. Keeping the temperature at 1200 ℃ for 2 h, wherein the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 25.19 percent. Keeping the temperature at 1400 ℃ for 2 h, wherein the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 37.51%
Example 2
A method for improving the oxidation resistance of a low-carbon magnesia carbon material comprises the following specific steps:
the method comprises the steps of firstly, sintering magnesia, crystalline flake graphite, phenolic resin and polycrystalline silicon waste materials according to the mass fraction ratio of 85 percent to 5 percent to 6 percent to 4 percent, adding the components, fully mixing in a mixer, then pressing the mixed raw materials in a stainless steel mold under the pressure of 220 MPa to form a green compact with the diameter of 50 × 50 mm, and finally, preserving heat at 180 ℃ for 10 hours to obtain the final product.
The composition of the polycrystalline silicon scrap in this example was 62% Si, 30% SiC and 8% impurity scrap.
The oxidation resistance test results of this example are as follows:
the temperature is kept for 2 hours at 1000 ℃, and the percentage of the decarburized layer of the low-carbon magnesia carbon material is 19.73 percent. Keeping the temperature at 1200 ℃ for 2 h, wherein the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 26.49 percent. Keeping the temperature at 1400 ℃ for 2 h, wherein the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 40.12%.
Example 3
A method for improving the oxidation resistance of a low-carbon magnesia carbon material comprises the following specific steps:
the method comprises the steps of firstly, sintering magnesia, crystalline flake graphite, phenolic resin and polycrystalline silicon waste material according to the mass fraction ratio of 88 percent to 4 percent to 2 percent to 6 percent, adding the components, fully mixing in a mixer, then pressing the mixed raw material in a stainless steel mold under the pressure of 250 MPa to prepare a green compact with the diameter of 50 × 50 mm, and finally, preserving heat at the temperature of 200 ℃ for 10 hours to obtain the final product.
The composition of the polycrystalline silicon scrap in this example was 65% Si, 30% SiC and 5% impurity scrap.
The oxidation resistance test results of this example are as follows:
the temperature is kept for 2 hours at 1000 ℃, and the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 18.16 percent. Keeping the temperature at 1200 ℃ for 2 h, wherein the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 25.49 percent. The temperature is kept at 1400 ℃ for 2 h, and the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 38.77 percent.
Example 4
A method for improving the oxidation resistance of a low-carbon magnesia carbon material comprises the following specific steps:
the method comprises the steps of firstly, sintering magnesia, crystalline flake graphite, phenolic resin and polycrystalline silicon waste material according to the mass fraction ratio of 83 percent to 6 percent to 3 percent to 8 percent, adding the components, fully mixing in a mixer, then pressing the mixed raw material in a stainless steel mold under the pressure of 250 MPa to prepare a green compact with the diameter of 50 × 50 mm, and finally, preserving heat at the temperature of 200 ℃ for 10 hours to obtain the final product.
The composition of the polycrystalline silicon scrap in this example was 60% Si, 35% SiC and 5% impurity scrap.
The oxidation resistance test results of this example are as follows:
the temperature is kept for 2 hours at 1000 ℃, and the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 16.28 percent. Keeping the temperature at 1200 ℃ for 2 h, wherein the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 22.94 percent. Keeping the temperature at 1400 ℃ for 2 h, wherein the percentage of the decarburized layer of the low-carbon magnesium-carbon material is 35.41%.
Claims (6)
1. A method for improving the oxidation resistance of a low-carbon magnesia carbon material is characterized by comprising the following specific steps:
firstly, sintering magnesite, carbon, a binder and polycrystalline silicon waste materials in a mass fraction ratio of (82% -88%), of (4% -7%), of (2% -6%) and of (4% -8%) and fully mixing the components in a mixer, then, pressing and molding the ground and mixed raw materials in a stainless steel mold, and finally, carrying out heat treatment at 180-200 ℃ for 10 hours to obtain a final product.
2. The method for improving the oxidation resistance of the low-carbon magnesia carbon material according to claim 1, wherein the purity of the sintered magnesia is not less than 98.5%, and the granularity is 5-3 mm, 3-1 mm, and not more than 0.088 mm in three-minute grade.
3. The method for improving the oxidation resistance of the low-carbon magnesia carbon material as claimed in claim 1, wherein the carbon is high-purity crystalline flake graphite, the purity is not less than 99.5%, and the particle size is not more than 37 μm.
4. The method of claim 1, wherein the binder is a thermosetting phenolic resin, commercial grade, having a carbonization rate of about 50%.
5. The method for improving the oxidation resistance of the low-carbon magnesium-carbon material as claimed in claim 1, wherein the polycrystalline silicon waste mainly comprises Si, SiC, polyethylene glycol and a small amount of metal, and before the method is used, the polycrystalline silicon waste is subjected to heat treatment at 800 ℃ and magnetic separation to remove polyethylene glycol and metal impurities, so that the waste containing 60% -65% of Si, 30% -35% of SiC and 5% -10% of impurities is finally obtained.
6. The method for improving the oxidation resistance of the low-carbon magnesium-carbon material as claimed in claim 1, wherein the forming pressure of the pressed green body is 200-250 MPa, and the heat treatment equipment is a multichannel tunnel kiln.
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Citations (6)
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|---|---|---|---|---|
| CN101215177A (en) * | 2007-12-29 | 2008-07-09 | 中国钢研科技集团公司 | Low-carbon magnesium oxide base composite fireproof material and preparation method thereof |
| CN102276275A (en) * | 2011-07-21 | 2011-12-14 | 辽宁科技大学 | Method for producing magnesium carbon bricks by using microwave heating technology |
| CN103539465A (en) * | 2013-09-29 | 2014-01-29 | 浙江金磊高温材料股份有限公司 | High-performance magnesia-carbon brick and production method thereof |
| CN105036766A (en) * | 2015-07-04 | 2015-11-11 | 张燕 | Vanadium iron slag-polycrystalline silicon waste refractory castable |
| CN105503212A (en) * | 2015-12-21 | 2016-04-20 | 江苏苏嘉集团新材料有限公司 | Magnesia carbon brick and preparation method thereof |
| CN108484130A (en) * | 2018-06-14 | 2018-09-04 | 营口石元耐火材料有限公司 | A kind of low carbon magnesia carbon brick and preparation method thereof of nano-sized carbon enhancing |
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2019
- 2019-07-04 CN CN201910597778.8A patent/CN111348902A/en active Pending
Patent Citations (6)
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| CN101215177A (en) * | 2007-12-29 | 2008-07-09 | 中国钢研科技集团公司 | Low-carbon magnesium oxide base composite fireproof material and preparation method thereof |
| CN102276275A (en) * | 2011-07-21 | 2011-12-14 | 辽宁科技大学 | Method for producing magnesium carbon bricks by using microwave heating technology |
| CN103539465A (en) * | 2013-09-29 | 2014-01-29 | 浙江金磊高温材料股份有限公司 | High-performance magnesia-carbon brick and production method thereof |
| CN105036766A (en) * | 2015-07-04 | 2015-11-11 | 张燕 | Vanadium iron slag-polycrystalline silicon waste refractory castable |
| CN105503212A (en) * | 2015-12-21 | 2016-04-20 | 江苏苏嘉集团新材料有限公司 | Magnesia carbon brick and preparation method thereof |
| CN108484130A (en) * | 2018-06-14 | 2018-09-04 | 营口石元耐火材料有限公司 | A kind of low carbon magnesia carbon brick and preparation method thereof of nano-sized carbon enhancing |
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