CN116715530A - Preparation method of spinel carbon material with low thermal expansion rate - Google Patents
Preparation method of spinel carbon material with low thermal expansion rate Download PDFInfo
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- CN116715530A CN116715530A CN202310645274.5A CN202310645274A CN116715530A CN 116715530 A CN116715530 A CN 116715530A CN 202310645274 A CN202310645274 A CN 202310645274A CN 116715530 A CN116715530 A CN 116715530A
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- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 130
- 239000011029 spinel Substances 0.000 title claims abstract description 130
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000002245 particle Substances 0.000 claims abstract description 40
- 238000002156 mixing Methods 0.000 claims abstract description 39
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 18
- 239000010439 graphite Substances 0.000 claims abstract description 18
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000005011 phenolic resin Substances 0.000 claims abstract description 17
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims description 21
- 238000009694 cold isostatic pressing Methods 0.000 claims description 16
- 239000001993 wax Substances 0.000 claims description 12
- 235000013871 bee wax Nutrition 0.000 claims description 8
- 239000012166 beeswax Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000012188 paraffin wax Substances 0.000 claims description 7
- 229910052566 spinel group Inorganic materials 0.000 claims description 4
- 230000035939 shock Effects 0.000 abstract description 6
- 239000011819 refractory material Substances 0.000 abstract description 4
- 238000007781 pre-processing Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 17
- 238000005303 weighing Methods 0.000 description 12
- 238000003723 Smelting Methods 0.000 description 8
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000005245 sintering Methods 0.000 description 6
- RQMIWLMVTCKXAQ-UHFFFAOYSA-N [AlH3].[C] Chemical compound [AlH3].[C] RQMIWLMVTCKXAQ-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C—CHEMISTRY; METALLURGY
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- 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
- C04B2235/425—Graphite
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- C—CHEMISTRY; METALLURGY
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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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
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- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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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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Abstract
The invention belongs to the technical field of refractory materials, and relates to a preparation method of a spinel carbon material with low thermal expansion rate. The preparation method of the spinel carbon material with low thermal expansion rate comprises the steps of preprocessing spinel particles, namely mixing the spinel particles with one of wax, silica sol and PVA, and forming a layer of film on the surfaces of the spinel particles; the addition amount of wax, silica sol and PVA is 1-5% of spinel particles; drying the mixed spinel raw material; according to the mass percentage, the pretreated spinel particles, the crystalline flake graphite, the spinel fine powder and the phenolic resin are mixed in a mixing mill to form spinel carbon raw materials, and the spinel carbon raw materials are dried, cold isostatic pressed and formed and heat treated for 5 hours at 950 ℃ to prepare the spinel carbon material with low thermal expansion rate. The invention reduces the thermal expansion rate of the spinel carbon material product; the thermal shock resistance is good.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a preparation method of a spinel carbon material with a low thermal expansion rate.
Background
The spinel carbon material has high melting point, high strength and excellent molten steel scouring resistance and erosion resistance, can be applied to parts with harsh service environments such as integral stopper rod heads, immersed nozzle bowl parts and the like, and is compounded with the aluminum carbon material for use; however, the thermal expansion rate of the spinel material is too high, the thermal expansion rate of the spinel material with theoretical stoichiometric ratio at 1300 ℃ can reach 8.5%, even if a certain amount of graphite is contained in the spinel carbon material, the thermal expansion rate is reduced, but the thermal expansion rate of the spinel material at 1300 ℃ still exceeds 7%, and the thermal expansion rate of the aluminum carbon material at 1300 ℃ is about 4%. Because of the excessive thermal expansion rate difference between the spinel carbon material and the aluminum carbon material, in addition, the larger the thermal expansion rate of the refractory material is, the worse the thermal shock resistance is; therefore, in the use process, the conditions that the integral stopper rod and the immersed nozzle of the spinel carbon material and the aluminum carbon material are compounded often occur that the joint part is broken, the production is interrupted, and the production efficiency is affected.
Disclosure of Invention
The invention aims to provide a preparation method of a spinel carbon material with low thermal expansion rate, which can improve the stability of a product in use.
The invention adopts the following technical scheme for accomplishing the purposes:
a preparation method of spinel carbon material with low thermal expansion rate comprises the following steps: pretreating spinel particles, namely mixing the spinel particles with one of wax, silica sol and PVA, and forming a layer of film on the surfaces of the spinel particles; the addition amount of wax, silica sol and PVA is 1-5% of spinel particles; drying the mixed spinel raw material; according to the mass percentage, 45 percent of the pretreated spinel particles, 15 percent of crystalline flake graphite, 35 percent of 200-mesh spinel fine powder and 5 percent of phenolic resin are taken, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃ and subjected to cold isostatic pressing under 100mpa pressure, and heat treatment is carried out for 5 hours at 950 ℃ to prepare the spinel carbon material with low thermal expansion rate.
The spinel particles are one of fused spinels and sintered spinels.
The wax is one of paraffin wax and beeswax; when wax is used, the wax is melted into a liquid.
The particle size of the spinel particles is 1-0.2mm.
According to the preparation method of the spinel carbon material with the low thermal expansion rate, one of wax, silica sol and PVA is utilized to mix with spinel particles, a layer of film is formed on the surfaces of the spinel particles after mixing is completed, and then the spinel carbon product is prepared by utilizing the raw materials treated by the method; the heat treatment temperature of the spinel carbon product is above 900 ℃, wax or PVA on the surface of spinel particles can disappear in the heat treatment process, a circle of tiny gaps are formed on the surface of the spinel particles, and a large number of holes are formed on the surface of the spinel particles by silica sol, and the gaps or holes counteract the thermal expansion of the spinel material in the use process, so that the thermal expansion rate of the spinel carbon material product is reduced; according to the related theory of thermal shock fracture and thermal shock damage of the material, the thermal expansion rate of the material is a main factor influencing the thermal shock resistance of the material, and the smaller the thermal expansion rate of the refractory material is, the better the thermal shock resistance is.
Description of the embodiments
The invention will be described in detail with reference to specific examples:
examples
Weighing 100 parts of electrofused spinel (1-0.2 mm) by mass, 1 part of paraffin, melting paraffin into liquid at 90 ℃, mixing in a mixer for 10min, and naturally drying in air for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of electric smelting spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃, subjected to cold isostatic pressing under 100mpa pressure, and subjected to heat treatment for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of sintering spinel (1-0.2 mm) according to mass, melting 3 parts of paraffin into liquid at 90 ℃, mixing in a mixer for 10min, and naturally drying in air for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of sintered spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃ and subjected to cold isostatic pressing under 100mpa pressure, and heat treatment is carried out for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of electrofused spinel (1-0.2 mm) by mass, 5 parts of paraffin, melting paraffin into liquid at 90 ℃, mixing in a mixer for 10min, and naturally drying in air for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of electric smelting spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃, subjected to cold isostatic pressing under 100mpa pressure, and subjected to heat treatment for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of sintering spinel (1-0.2 mm) according to mass, 1 part of beeswax, melting the beeswax into liquid at 90 ℃, mixing in a mixer for 10min, and naturally drying in air for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of sintered spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃ and subjected to cold isostatic pressing under 100mpa pressure, and heat treatment is carried out for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of electrofused spinel (1-0.2 mm) by mass, 3 parts of beeswax, melting the beeswax into liquid at 90 ℃, mixing in a mixer for 10min, and naturally drying in air for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of electric smelting spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃, subjected to cold isostatic pressing under 100mpa pressure, and subjected to heat treatment for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of sintering spinel (1-0.2 mm) according to mass, 5 parts of beeswax, melting the beeswax into liquid at 90 ℃, mixing in a mixer for 10min, and naturally drying in air for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of sintered spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃ and subjected to cold isostatic pressing under 100mpa pressure, and heat treatment is carried out for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of electrofused spinel (1-0.2 mm) by mass, 1 part of silica sol, mixing in a mixing mill for 10min, and drying at 60 ℃ for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of electric smelting spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃, subjected to cold isostatic pressing under 100mpa pressure, and subjected to heat treatment for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of electrofused spinel (1-0.2 mm) by mass, 3 parts of silica sol, mixing in a mixing mill for 10min, and drying at 60 ℃ for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of electric smelting spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃, subjected to cold isostatic pressing under 100mpa pressure, and subjected to heat treatment for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of sintering spinel (1-0.2 mm) by mass, 5 parts of silica sol, mixing in a mixing mill for 10min, and drying at 60 ℃ for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of sintered spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃ and subjected to cold isostatic pressing under 100mpa pressure, and heat treatment is carried out for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of sintering spinel (1-0.2 mm) by mass, 1 part of PVA, mixing in a mixing mill for 10min, and drying at 60 ℃ for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of sintered spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃ and subjected to cold isostatic pressing under 100mpa pressure, and heat treatment is carried out for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of electrofused spinel (1-0.2 mm) by mass, 3 parts of PVA, mixing in a mixer for 10min, and drying at 60 ℃ for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of electric smelting spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃, subjected to cold isostatic pressing under 100mpa pressure, and subjected to heat treatment for 5 hours at 950 ℃ to prepare the spinel carbon product.
Examples
Weighing 100 parts of sintering spinel (1-0.2 mm) by mass, 5 parts of PVA, mixing in a mixing mill for 10min, and drying at 60 ℃ for 2h; 45 parts of the treated spinel particles, 15 parts of crystalline flake graphite, 35 parts of sintered spinel fine powder (200 meshes) and 5 parts of phenolic resin are weighed, mixed into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃ and subjected to cold isostatic pressing under 100mpa pressure, and subjected to heat treatment for 5 hours at 950 ℃ to prepare the spinel carbon product.
Meanwhile, in order to compare the effects of the present invention, a comparative sample was prepared.
Comparative sample 1: 45 parts of sintered spinel particles, 15 parts of crystalline flake graphite, 35 parts of sintered spinel fine powder (200 meshes) and 5 parts of phenolic resin are mixed into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃, subjected to pressure reduction molding at 100mpa, subjected to cold isostatic pressing, and subjected to heat treatment for 5 hours at 950 ℃ to prepare the spinel carbon product.
Comparative sample 2: 45 parts of electric smelting spinel particles, 15 parts of crystalline flake graphite, 35 parts of electric smelting spinel fine powder (200 meshes) and 5 parts of phenolic resin, mixing the materials into spinel carbon raw materials in a mixing mill, drying the spinel carbon raw materials at 60 ℃ for 6 hours, performing cold isostatic pressing and forming under 100mpa pressure, and performing heat treatment at 950 ℃ for 5 hours to prepare the spinel carbon product.
The thermal expansion rates of the respective schemes in the room temperature-1300 ℃ range are shown in table 1.
Table 1 thermal expansion coefficient of each protocol%
。
Claims (4)
1. A preparation method of spinel carbon material with low thermal expansion rate is characterized by comprising the following steps: the preparation method comprises the following steps: pretreating spinel particles, namely mixing the spinel particles with one of wax, silica sol and PVA, and forming a layer of film on the surfaces of the spinel particles; the addition amount of wax, silica sol and PVA is 1-5% of spinel particles; drying the mixed spinel raw material; according to the mass percentage, 45 percent of the pretreated spinel particles, 15 percent of crystalline flake graphite, 35 percent of 200-mesh spinel fine powder and 5 percent of phenolic resin are taken, the materials are kneaded into spinel carbon raw materials by a mixing mill, dried for 6 hours at 60 ℃ and subjected to cold isostatic pressing under 100mpa pressure, and heat treated for 5 hours at 950 ℃ to prepare the spinel carbon material with low thermal expansion rate.
2. A method for preparing a spinel carbon material with low thermal expansion rate according to claim 1, wherein: the spinel particles are one of fused spinels and sintered spinels.
3. A method for preparing a spinel carbon material with low thermal expansion rate according to claim 1, wherein: the wax is one of paraffin wax and beeswax; when wax is used, the wax is melted into a liquid.
4. A method for preparing a spinel carbon material with low thermal expansion rate according to claim 1, wherein: the particle size of the spinel particles is 1-0.2mm.
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