CN111875363A - Preparation method of electrofused mullite containing titanium carbonitride solid solution - Google Patents

Preparation method of electrofused mullite containing titanium carbonitride solid solution Download PDF

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CN111875363A
CN111875363A CN202010687164.1A CN202010687164A CN111875363A CN 111875363 A CN111875363 A CN 111875363A CN 202010687164 A CN202010687164 A CN 202010687164A CN 111875363 A CN111875363 A CN 111875363A
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mullite
titanium carbonitride
solid solution
alumina
medium
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CN111875363B (en
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李勇
岳茜
孙加林
薛文东
蒋朋
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University of Science and Technology Beijing USTB
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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
    • C04B35/16—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 silicates other than clay
    • C04B35/18—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 silicates other than clay rich in aluminium oxide
    • C04B35/185—Mullite 3Al2O3-2SiO2
    • 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
    • C04B35/653—Processes involving a melting step
    • C04B35/657—Processes involving a melting step for manufacturing refractories
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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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3856—Carbonitrides, e.g. titanium carbonitride, zirconium carbonitride

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  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

A preparation method of electrofused mullite containing titanium carbonitride solid solution belongs to the technical field of refractory materials. The invention prepares the electrofused mullite by the medium-low grade alumina in an electric arc furnace through an electric melting method, wherein the alumina content in the medium-low grade alumina is 45-60%, the titanium dioxide content is generally less than 8%, and a titanium carbonitride solid solution is formed in the mullite during the electric melting process and is dissolved in the mullite to obtain the mullite refractory raw material. The mullite prepared by the invention forms acicular crystals, has good crystal structure, is easy to break, has low price of raw materials, realizes the comprehensive utilization of the medium and low grade alumina, and the titanium carbonitride solid solution formed in the electric melting process is a non-oxide ceramic material with excellent performance, thereby being beneficial to the improvement of the performance of the subsequent mullite products.

Description

Preparation method of electrofused mullite containing titanium carbonitride solid solution
Technical Field
The invention relates to a preparation method of electrofused mullite containing titanium carbonitride solid solution, belonging to the technical field of refractory materials.
Background
The total storage capacity of the bauxite which is proved to be about 21 hundred million tons in China accounts for about 2.5 percent of the total content of the world, and although natural refractory material resources are rich, the per-capita storage capacity of China is lower, and the per-capita storage capacity of the bauxite is about 7.3 percent of the per-capita content of the world. Meanwhile, the problems of overlarge mining quantity and disordered mining, low utilization rate of high-quality bauxite resources, large amount of medium-low grade bauxite and crushed ore which cannot be effectively utilized and the like exist, so that the current situation that the high-quality high-bauxite resources in China are completely consumed is caused, and the continuous development of the refractory material industry in China is severely restricted. The reserves of the medium and low grade alumina in China are huge and account for about 60 percent of the alumina resources, so that the realization of the high-efficiency and comprehensive utilization of the medium and low grade alumina resources is an important way for realizing the sustainable green development of the refractory industry.
The alumina is a mixture of kaolinite, diaspore and gibbsite, and the main chemical component is Al2O3Removing Al2O3In addition, it also contains a certain amount of SiO2、K2O、Na2O、CaO、MgO、TiO2、Fe2O3Al of medium or low grade alumina, compared with high alumina2O3Low content of TiO2The content is higher. Heating the crushed medium-low grade alumina in an electric arc furnace to 2000 ℃, and adding K into the alumina2O、Na2O、CaO、MgO、Fe2O3Reducing to metal and removing to finally form electrofused mullite, and TiO2The titanium carbonitride solid solution generated by the reaction is dissolved in the mullite.
Mullite is a ceramic material with excellent properties, such as high melting point, high creep resistance, high-temperature mechanical stability, and excellent thermal shock resistance and chemical corrosion resistance, but its application is limited due to its low toughness and strength, and in recent years, composite materials combining mullite with some non-oxide materials have been studied.
The titanium carbonitride solid solution is a non-oxide ceramic material with excellent performance, has the characteristics of high melting point, high hardness, corrosion resistance, excellent oxidation resistance and the like, and researches show that the existence of the titanium carbonitride solid solution can obviously enhance the strength and the hardness of the mullite ceramic material and is beneficial to the densification of mullite. Meanwhile, the titanium carbonitride can well resist the erosion of slag and molten steel in the kiln and has good furnace protection effect, but the cost of the titanium carbonitride is too high, so the use of the titanium carbonitride in refractory materials is limited.
Therefore, the method is an important way for continuous, green and efficient development of the refractory industry in the face of the current situation that the high-bauxite resources in China are completely consumed and realizing low-cost preparation of titanium carbonitride so as to be popularized and used in refractory materials on a large scale.
Disclosure of Invention
The invention aims to provide a method for preparing a mullite raw material by using medium-low grade alumina as a raw material through an electric melting method, namely a method for preparing an electric melting mullite raw material containing titanium carbonitride solid solution by using medium-low grade alumina, aiming at the current situation that high-quality alumina resources in China are exhausted, wherein the raw material is low in price, the cost is greatly reduced, and the process is simple and easy to implement.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the mullite refractory raw material is prepared by crushing and finely grinding medium and low-grade alumina and performing an electric melting method, wherein the content of alumina in the medium and low-grade alumina is 45-60%, the content of titanium dioxide is usually less than 8%, and a titanium carbonitride solid solution is formed in the mullite during the electric melting process and is dissolved in the mullite to obtain the mullite refractory raw material.
The electric melting process comprises the steps of mixing, forming, sintering at 800-1200 ℃, heating to 1900-2200 ℃ in an electric arc furnace, controlling the voltage of the electric arc furnace to be 80-140V and the current to be 12000-15000A, and discharging through a chute to be naturally cooled after heating to be molten.
The crushing and fine grinding are to crush the medium-low grade alumina into crushed ore or lump ore, and the granularity of the crushed ore or lump ore is 25-35 mm after the fine grinding.
The main chemical component of the mullite refractory material is Al2O355~80wt.%，SiO245-19 wt.%, titanium carbonitride less than 8.0wt.%, and total content of other impurities less than 3.0 wt.%.
The invention fully utilizes the components in the medium-low grade alumina, converts the titanium dioxide in the alumina into a non-oxide enhanced phase titanium carbonitride solid solution with excellent performance by an electric melting method, and simultaneously prepares the electric melting mullite with a needle-shaped structure and good development.
Positive effects of the invention
1. The invention fully utilizes the titanium oxide in the alumina to prepare the mullite refractory material containing the titanium carbonitride solid solution, and no additional titanium source is needed, thereby reducing the cost;
2. the invention uses the medium-low grade alumina to prepare the mullite, has low raw material price and realizes the comprehensive utilization of resources;
3. the electrofused mullite prepared by the method is an inherent acicular column crystal, is easy to break, and is easy to form maximum compact accumulation in a subsequent mullite product, so that the organization structure of the product is densified.
Drawings
Fig. 1 is a diagram of electrofused mullite acicular crystals of example 1.
Fig. 2 is an electrofused mullite XRD pattern of example 2.
Fig. 3 is the presence of a solid solution of titanium carbonitride in the electrofused mullite of example 3.
Fig. 4 is the morphology of the presence of solid solutions of titanium carbonitride in the electrofused mullite of example 4.
Detailed Description
The technical solution of the present invention is further illustrated by the following examples:
example 1
The raw material of the invention is medium-low grade alumina, wherein the content of alumina is 45-60%, the content of titanium dioxide is about 6%, the alumina is crushed into crushed ore or lump ore, and the granularity is about 30mm after being ground. After mixing and forming, firing at 1000 ℃, heating to 1900 ℃ in an electric arc furnace, controlling the voltage of the electric arc furnace to be 80-140V and the current to be 12000-15000A, heating to be molten, and then discharging from a launder for natural cooling.
Cooling and crushing to obtain the electrofused mullite raw material containing titanium carbonitride solid solution, wherein the main chemical component of the raw material is Al2O372.95%，SiO219.66 percent, 5.79 percent of titanium carbonitride and 1.6 percent of other impurities. As can be seen from fig. 1, the fused mullite has a needle-like crystal structure.
Example 2
The raw material of the invention is medium-low grade alumina, wherein the content of alumina is 45-60%, the content of titanium dioxide is about 6%, the alumina is crushed into crushed ore or lump ore, and the granularity is about 30mm after being ground. Mixing, forming, firing at 1000 ℃, heating to 2000 ℃ in an electric arc furnace, controlling the voltage of the electric arc furnace to be 80-140V and the current to be 12000-15000A, heating to be molten, discharging in a launder and naturally cooling.
Cooling and crushing to obtain the electrofused mullite raw material containing the titanium carbonitride solid solution. The main chemical component of the raw material is Al2O374.35%，SiO219.12 percent, 5.29 percent of titanium carbonitride and 1.24 percent of other impurities. As can be seen from fig. 2, a solid solution of titanium carbonitride was produced in the final product.
Example 3
The raw material of the invention is medium-low grade alumina, wherein the content of alumina is 45-60%, the content of titanium dioxide is about 6%, the alumina is crushed into crushed ore or lump ore, and the granularity is about 30mm after being ground. Mixing, forming, firing at 1000 ℃, heating to 2100 ℃ in an electric arc furnace, controlling the voltage of the electric arc furnace to be 80-140V and the current to be 12000-15000A, heating to melting, discharging in a launder, and naturally cooling.
Cooling and crushing to obtain the electrofused mullite raw material containing the titanium carbonitride solid solution. The main chemical component of the raw material is Al2O373.38%，SiO219.16 percent, 5.99 percent of titanium carbonitride and 1.47 percent of other impurities. As can be seen from fig. 3, titanium carbonitride is solid-dissolved in the raw material of electrofused mullite.
Example 4
The raw material of the invention is medium-low grade alumina, wherein the content of alumina is 45-60%, the content of titanium dioxide is about 6%, the alumina is crushed into crushed ore or lump ore, and the granularity is about 30mm after being ground. After mixing and forming, firing at 1000 ℃, heating to 2200 ℃ in an electric arc furnace, controlling the voltage of the electric arc furnace to be 80-140V and the current to be 12000-15000A, heating to be molten, discharging in a launder and naturally cooling.
Cooling and crushing to obtain the electrofused mullite raw material containing the titanium carbonitride solid solution. The main chemical component of the raw material is Al2O372.13%，SiO219.43 percent, 6.24 percent of titanium carbonitride and 2.2 percent of other impurities. As can be seen from fig. 4, the titanium carbonitride solid solution is granular in the electrofused mullite.

Claims (3)

1. A preparation method of electrofused mullite containing titanium carbonitride solid solution is characterized in that middle and low-grade alumina is crushed and ground and is prepared by an electrofusion method, wherein the alumina content of the middle and low-grade alumina is 45% -60%, the titanium dioxide content is less than 8%, and the titanium carbonitride solid solution is formed in the mullite in the electrofusion process and is solid-dissolved in the mullite to obtain the mullite refractory raw material;
the electric melting process comprises the steps of mixing, forming, sintering at 800-1200 ℃, heating to 1900-2200 ℃ in an electric arc furnace, controlling the voltage of the electric arc furnace to be 80-140V and the current to be 12000-15000A, and discharging through a chute to be naturally cooled after heating to be molten.
2. The method for preparing electrofused mullite containing a titanium carbonitride solid solution according to claim 1, wherein the medium-low grade alumina is crushed into crushed ore or lump ore, and the grain size is 25-35 mm after being ground.
3. The method of producing electrofused mullite containing a solid solution of titanium carbonitride according to claim 1 wherein the mullite refractory material has a chemical composition of Al as a main component2O355~80wt.%，SiO245-19 wt.%, titanium carbonitride less than 8.0wt.%, and total content of other impurities less than 3.0 wt.%.
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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN113264779A (en) * 2021-05-26 2021-08-17 贵州华鑫新材料有限公司 Production process of electrofused mullite
CN113461410A (en) * 2021-07-22 2021-10-01 河南熔金高温材料股份有限公司 Al-Al added with titanium nitride coated mullite2O3Sliding plate brick and production method thereof
CN114455956A (en) * 2022-02-10 2022-05-10 中国地质科学院郑州矿产综合利用研究所 Method for preparing electrofused mullite from bauxite under coal
CN114853487A (en) * 2022-05-06 2022-08-05 苏州诺瑞达新材料科技有限公司 Mullite castable based on titanium carbide and tungsten carbide composite
CN116332633A (en) * 2023-03-16 2023-06-27 北京科技大学 Method for synthesizing fused mullite and fused corundum-mullite by taking gangue as raw material

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113264779A (en) * 2021-05-26 2021-08-17 贵州华鑫新材料有限公司 Production process of electrofused mullite
CN113461410A (en) * 2021-07-22 2021-10-01 河南熔金高温材料股份有限公司 Al-Al added with titanium nitride coated mullite2O3Sliding plate brick and production method thereof
CN113461410B (en) * 2021-07-22 2022-09-09 河南熔金高温材料股份有限公司 Al-Al added with titanium nitride coated mullite 2 O 3 Sliding plate brick and production method thereof
CN114455956A (en) * 2022-02-10 2022-05-10 中国地质科学院郑州矿产综合利用研究所 Method for preparing electrofused mullite from bauxite under coal
CN114853487A (en) * 2022-05-06 2022-08-05 苏州诺瑞达新材料科技有限公司 Mullite castable based on titanium carbide and tungsten carbide composite
CN116332633A (en) * 2023-03-16 2023-06-27 北京科技大学 Method for synthesizing fused mullite and fused corundum-mullite by taking gangue as raw material

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