CN109485442A - A kind of preparation method of stratiform corundum-spinel refractories - Google Patents

A kind of preparation method of stratiform corundum-spinel refractories Download PDF

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Publication number
CN109485442A
CN109485442A CN201910029605.6A CN201910029605A CN109485442A CN 109485442 A CN109485442 A CN 109485442A CN 201910029605 A CN201910029605 A CN 201910029605A CN 109485442 A CN109485442 A CN 109485442A
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corundum
stratiform
spinel
preparation
spinelle
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CN109485442B (en
Inventor
刘国齐
李红霞
杨文刚
陈勇强
于建宾
钱凡
马天飞
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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    • C04B35/803—
    • 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
    • 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
    • C04B35/44—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 aluminates
    • C04B35/443—Magnesium aluminate spinel
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon

Abstract

The invention belongs to technical field of refractory materials, propose a kind of preparation method of stratiform corundum-spinel refractories.A kind of preparation method of the stratiform corundum-spinel refractories proposed: selection liquid ceramic precursor polysilazane is framework material, aluminium secondary butylate is the doping source Al, increase carbon-carbon double bond quantity with divinyl toluene, using hexamethylene as solvent, prepares SiAlCN ceramic forerunner；SiAlCN ceramic forerunner, combined binder and Ni (NO3) 2.6H2O and Al2O3 powder are mixed to get mixture, the molded obtained aluminium oxide green body of mixture cold；Spinelle thin stock is prepared using tape casting；Then hot pressing lamination is used, spinelle thin stock and aluminium oxide green body alternative stacked are prepared into multilayer corundum-spinel green body；Spinelle thin stock prepares the Ultra-low carbon corundum-spinel refractories that multilayer cooperates with enhancing with aluminium oxide green body alternative stacked.The present invention has good thermal shock resistance.

Description

A kind of preparation method of stratiform corundum-spinel refractories
Technical field
The invention belongs to technical field of refractory materials, and in particular to a kind of preparation of stratiform corundum-spinel refractories Method.
Background technique
Traditional carbon containing refractory improves the thermal shock resistance of refractory material, in high temperature although the presence of carbon component Under smelting actions, oxidation, which occurs, for carbon makes to form porous structure in refractory material, reduces the intensity of material, material is caused easily to be melt Scouring and infiltration also affect the content of carbon in steel.The longevity of refractory material is always high temperature industry problems faced, The refractory material long-life for especially meeting advanced steel product smelting is even more huge challenge.Anti-thermal shock, anti-erosion are pollution-free etc. good Good matched structure-function integration novel refractory just becomes the emphasis paid close attention to both at home and abroad.Current research, which is widely used, to be changed Kind refractory material component, addition or in-situ preparation protection equivalent way optimization refractory material anti-erosion, thermodynamics and mechanical performance, But effect of optimization is still single, cannot reach the good unification of structure function always.Laminar composite is used as one kind is bionical to set Meter, fine structure ensure that the excellent comprehensive performance of material.Therefore, the design of stratiform refractory material and preparation also gradually by To attention.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of stratiform corundum-spinel refractories, can solve existing There is the problem of carbon containing refractory carbon content rate high, oxidizable, easy erosion.
In order to achieve the goal above, the technical scheme adopted by the invention is that: a kind of stratiform corundum-spinel refractories Preparation method, including the following steps:
1) selecting liquid ceramic precursor polysilazane is framework material, and aluminium secondary butylate is the doping source Al, with the increasing of divinyl toluene Add carbon-carbon double bond quantity, using hexamethylene as solvent, prepares SiAlCN ceramic forerunner；Liquid phenolic resin and pitch is selected to make For combined binder；Addition forms Ni as Ni (NO3) 2.6H2O of catalyst as additive after decomposing；SiAlCN is made pottery Porcelain presoma, combined binder and Ni (NO3) 2.6H2O and Al2O3 powder are mixed to get mixture, the molded system of mixture cold Obtain aluminium oxide green body；
2) the spinelle thin stock of thickness 1-5mm is prepared using tape casting；Using hot pressing lamination, by spinelle thin stock and aluminium oxide Green body alternative stacked preparation multilayer corundum-spinel green body is warming up in N2 atmosphere furnace with 2~5 DEG C/min rate 1450-1600oC keeps the temperature 60-120min, closes power supply, naturally cools to room temperature；It is raw after the pyrolysis of Sicilian ceramic precursor At continuous ceramic fibre, continuous ceramic fibre forms three-dimensional space network structure inside refractory material；Simultaneously Sicilian ceramic precursor is in pyrolytic process, and the carbonaceous gas of generation is in additive Ni (NO3)2.6H2It is formed after O pyrolysis Ni catalyst under the action of generate further increase material mechanical strength and thermal shock resist carbon fiber；Spinelle thin stock The Ultra-low carbon corundum-spinel refractories that multilayer cooperates with enhancing are prepared with aluminium oxide green body alternative stacked.
The corundum-spinel refractories are multilayered structure.
The corundum-spinel refractories are carbon containing in 1wt% or less.
Component of the mixing package described in step 1) containing following mass percent: Al2O3Powder quality score 80-90wt%, 2-3000 μm of particle size range, combined binder 5-10wt%, SiAlCN ceramic forerunner 5-10wt%, additive is outer Add, additional amount is the 1-2wt% of mixed mixture total mass.
The raw material of the Al2O3 powder forms and weight percent are as follows: 1-3mm plate corundum 15wt%, 0-1mm plate corundum 25wt%, 45 μm of plate corundum 30wt%, 2 μm of Al2O3 fine powder 30wt%.
The combined binder is made of resin and pitch.
Described additive Ni (NO3) 26H2O forms Ni as catalyst, the shape of catalysed promoted carbon fiber after decomposition At.
The thickness 1-5mm of spinelle thin stock described in step 2, the electric smelting spinelle that raw material is 2 μm.
In electric furnace, 1450-1600 is warming up to 2~5 DEG C/min rateoC keeps the temperature 60-120min, closes power supply, from So it is cooled to room temperature.
A kind of preparation method of stratiform corundum-spinel refractories proposed by the present invention, Sicilian ceramic precursor Continuous ceramic fibre is generated after pyrolysis, continuous ceramic fibre forms three-dimensional space network structure inside refractory material, together When in pyrolytic process, the carbonaceous gas of generation under the action of Ni catalyst, generate carbon fiber, also can further improve material The mechanical strength of material and thermal shock are resisted；The formation of three-dimensional space network structure and C fiber, with precursor content, catalyst, heat Treatment conditions are inseparable；The catalytic efficiency of catalyst and temperature, gas concentration, catalyst content are closely related；Ceramic fibre Content and distribution it is very important to the performance of basis material.By regulate and control ceramic setter bulk concentration, content, heat at Temperature, atmosphere are managed, Ultra-low carbon highly heatproof and shockproof Al2O3 base refractory material is prepared.
In the preparation method of stratiform corundum-spinel refractories of the invention, the component structure of stratiform refractory material, sky Between configuration and state of interface codetermine its anti-thermal shock, anti-erosion, mechanical property；Different structure Al2O3 single layer is selected respectively Refractory material and fine and close high anti-erosion single layer MgAl2O4Material, by the two or three with different-thickness than carrying out alternative stacked；Root According to the intrinsic property of different mono-layer refractories, the novel lamellar refractory material of different spaces configuration and interface cohesion is designed；Control Base preparation process and stratiform refractory material stack technology optimize stratiform refractory material firing process system；It is rigid to prepare stratiform Jade-spinel refractory.
In the preparation method of stratiform corundum-spinel refractories of the invention, corundum-spinel refractories are multilayer Structure, and by three-dimensional ceramic network and fibre reinforced, there is good thermal shock resistance；In addition, phosphorus content is lower than 1wt%, belong to It is most important to the smelting of clean steel in ultralow carbon refractory, it has broad application prospects.
Detailed description of the invention
Fig. 1 is stratiform corundum-spinel structural schematic diagram；
Fig. 2 is that catalysis generates carbon fiber SEM figure.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and detailed description.
Embodiment 1:
The preparation method of the stratiform corundum-spinel refractories of the present embodiment, including the following steps:
1) 1-3mm plate corundum 15wt%, 0-1mm plate corundum 25wt%, 45 μm of plate corundum 30wt% and 2 μm of Al are taken2O3Fine powder 30wt%, high speed are kneaded 15min, obtain mixture；Mixture 80wt% is taken, 10wt% compound additive is added, 10wt% is added SiAlCN presoma, additional 6wt%Ni (NO3)2.6H2O, after high speed is kneaded, cold moudling obtains aluminium oxide green body, thickness 10mm。
2) the spinelle thin stock of thickness 2mm, the electric smelting spinelle that raw material is 2 μm are prepared using tape casting；Using hot pressing Spinelle thin stock and aluminium oxide green body alternative stacked are prepared multilayer corundum-spinel green body, in N by lamination2In atmosphere furnace, 1450-1600 is warming up to 2~5 DEG C/min rateoC keeps the temperature 60-120min.It is then shut off power supply, cooled to room temperature, Up to stratiform corundum-spinel refractories.
The stratiform corundum-spinel refractories porosity obtained by the present embodiment is 15%, 1100oAfter C water cooling, intensity is kept Rate 80%.
Embodiment 2
The stratiform corundum-spinel refractories of the present embodiment, including the following steps:
1) 1-3mm plate corundum 15wt%, 0-1mm plate corundum 25wt%, 45 μm of plate corundum 30wt% and 2 μm of Al are taken2O3Fine powder 30wt%, high speed are kneaded 15min, obtain mixture.Mixture 80wt% is taken, 10wt% compound additive is added, 10wt% is added SiAlCN presoma, additional 6wt%Ni (NO3)2.6H2O, after high speed is kneaded, cold moudling obtains aluminium oxide green body, thickness 10mm。
2) the spinelle thin stock of thickness 5mm, the electric smelting spinelle that raw material is 2 μm are prepared using tape casting；Using hot pressing Spinelle thin stock and aluminium oxide green body alternative stacked are prepared multilayer corundum-spinel green body, in N by lamination2In atmosphere furnace, 1450-1600 is warming up to 2~5 DEG C/min rateoC keeps the temperature 60-120min.It is then shut off power supply, cooled to room temperature, Up to stratiform corundum-spinel refractories.
The stratiform corundum-spinel refractories porosity obtained by the present embodiment is 12%, 1100oAfter C water cooling, intensity is kept Rate 75%.
Embodiment 3
The stratiform corundum-spinel refractories of the present embodiment, including the following steps:
1) 1-3mm plate corundum 15wt%, 0-1mm plate corundum 25wt%, 45 μm of plate corundum 30wt% and 2 μm of Al are taken2O3Fine powder 30wt%, high speed are kneaded 15min, obtain mixture；Mixture 90wt% is taken, 5wt% compound additive is added, 5wt% is added SiAlCN presoma, additional 6wt%Ni (NO3)2.6H2O, after high speed is kneaded, cold moudling obtains aluminium oxide green body, thickness 10mm。
2) the spinelle thin stock of thickness 5mm, the electric smelting spinelle that raw material is 2 μm are prepared using tape casting；Using hot pressing Spinelle thin stock and aluminium oxide green body alternative stacked are prepared multilayer corundum-spinel green body, in N by lamination2In atmosphere furnace, 1450-1600 is warming up to 2~5 DEG C/min rateoC keeps the temperature 60-120min.It is then shut off power supply, cooled to room temperature, Up to stratiform corundum-spinel refractories.
The stratiform corundum-spinel refractories porosity obtained by the present embodiment is 10%, 1100oAfter C water cooling, intensity is kept Rate 70%.
Embodiment 4
The microwave sintering method of the aluminium oxide ceramic ball of the present embodiment, including the following steps:
1) 1-3mm plate corundum 15wt%, 0-1mm plate corundum 25wt%, 45 μm of plate corundum 30wt% and 2 μm of Al are taken2O3Fine powder 30wt%, high speed are kneaded 15min, obtain mixture.Mixture 80wt% is taken, 10wt% compound additive is added, 10wt% is added SiAlCN presoma, additional 6wt%Ni (NO3)2.6H2O, after high speed is kneaded, cold moudling obtains aluminium oxide green body, thickness 10mm。
2) the spinelle thin stock of thickness 2mm, the electric smelting spinelle that raw material is 2 μm are prepared using tape casting；Using hot pressing Spinelle thin stock and aluminium oxide green body alternative stacked are prepared multilayer corundum-spinel green body, in N by lamination2In atmosphere furnace, 1450-1600 is warming up to 2~5 DEG C/min rateoC keeps the temperature 60-120min.It is then shut off power supply, cooled to room temperature, Up to stratiform corundum-spinel refractories.
The stratiform corundum-spinel refractories porosity obtained by the present embodiment is 11%, 1100oAfter C water cooling, intensity is kept Rate 75%.

Claims (8)

1. a kind of preparation method of stratiform corundum-spinel refractories, it is characterised in that: include the following steps:
1) selecting liquid ceramic precursor polysilazane is framework material, and aluminium secondary butylate is the doping source Al, with the increasing of divinyl toluene Add carbon-carbon double bond quantity, using hexamethylene as solvent, prepares SiAlCN ceramic forerunner；Liquid phenolic resin and pitch is selected to make For combined binder；Addition forms Ni as Ni (NO3) 2.6H2O of catalyst as additive after decomposing；SiAlCN is made pottery Porcelain presoma, combined binder and Ni (NO3) 2.6H2O and Al2O3 powder are mixed to get mixture, the molded system of mixture cold Obtain aluminium oxide green body；
2) the spinelle thin stock of thickness 1-5mm, the electric smelting spinelle that base raw material is 2 μm are prepared using tape casting；Using hot pressing Spinelle thin stock and aluminium oxide green body alternative stacked are prepared multilayer corundum-spinel green body by lamination, in N2 atmosphere furnace, It is warming up to 1450-1600oC with 2~5 DEG C/min rate, keeps the temperature 60-120min, power supply is closed, naturally cools to room temperature； Continuous ceramic fibre is generated after the pyrolysis of Sicilian ceramic precursor, continuous ceramic fibre forms three inside refractory material Dimension space network structure；Sicilian ceramic precursor is in pyrolytic process simultaneously, and the carbonaceous gas of generation is in additive Ni (NO3) 2.6H2O generates the mechanical strength and thermal shock for further increasing material under the action of being formed by Ni catalyst after being pyrolyzed The carbon fiber of resistance；Spinelle thin stock prepares the ultralow carbo-corundum-that multilayer cooperates with enhancing with aluminium oxide green body alternative stacked Spinel refractory.
2. a kind of preparation method of stratiform corundum-spinel refractories as described in claim 1, it is characterised in that: described Corundum-spinel refractories are multilayered structure.
3. a kind of preparation method of stratiform corundum-spinel refractories as described in claim 1, it is characterised in that: described Corundum-spinel refractories are carbon containing in 1wt% or less.
4. a kind of preparation method of stratiform corundum-spinel refractories as described in claim 1, it is characterised in that: step 1) component of the mixing package containing following mass percent described in: Al2O3 powder quality score 80-90wt%, particle size range 2-3000 μm, combined binder 5-10wt%, SiAlCN ceramic forerunner 5-10wt%, additive be it is additional, additional amount is mixed The 1-2wt% of mixture total mass.
5. a kind of preparation method of stratiform corundum-spinel refractories as described in claim 1, it is characterised in that: described Al2O3 powder raw material composition and weight percent are as follows: 1-3mm plate corundum 15wt%, 0-1mm plate corundum 25wt%, 45 μm Plate corundum 30wt%, 2 μm of Al2O3 fine powder 30wt%.
6. a kind of preparation method of stratiform corundum-spinel refractories as described in claim 1, it is characterised in that: described Additive Ni (NO3) 26H2O forms Ni as catalyst, the formation of catalysed promoted carbon fiber after decomposition.
7. a kind of preparation method of stratiform corundum-spinel refractories as described in claim 1, it is characterised in that: step 2) the thickness 1-5mm of spinelle thin stock described in, the electric smelting spinelle that raw material is 2 μm.
8. a kind of preparation method of stratiform corundum-spinel refractories as described in claim 1, it is characterised in that: in electricity In furnace, 1450-1600 is warming up to 2~5 DEG C/min rateoC keeps the temperature 60-120min, closes power supply, naturally cools to room temperature.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101863673A (en) * 2010-06-07 2010-10-20 长兴锅炉耐火器材厂 Magnesia-alumina spinel structure heat insulation integral composite brick and preparation method thereof
CN101870585A (en) * 2010-07-06 2010-10-27 中国人民解放军国防科学技术大学 Preparation method of Si-Al-C-N ceramic precursor
CN103880449A (en) * 2014-03-27 2014-06-25 中钢集团洛阳耐火材料研究院有限公司 Preparation method of low-carbon aluminum-carbon refractory material for use in continuous casting

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101863673A (en) * 2010-06-07 2010-10-20 长兴锅炉耐火器材厂 Magnesia-alumina spinel structure heat insulation integral composite brick and preparation method thereof
CN101870585A (en) * 2010-07-06 2010-10-27 中国人民解放军国防科学技术大学 Preparation method of Si-Al-C-N ceramic precursor
CN103880449A (en) * 2014-03-27 2014-06-25 中钢集团洛阳耐火材料研究院有限公司 Preparation method of low-carbon aluminum-carbon refractory material for use in continuous casting

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
INGO GÖTSCHEL ET AL.: ""Tape Casting of Al2O3 , MgO, and MgAl2O4 for the Manufacture of Multilayer Composites for Refractory Applications "", 《INTERNATIONAL JOURNAL OF APPLIED CERAMIC TECHNOLOGY》 *
朱芷颐: ""添加 Ni、Co 对 Al2O3-C 耐火材料显微组织结构及性能的影响"", 《内蒙古科技大学硕士论文》 *

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