CN102503485A - Al2O3-C refractory fired by nitridation and preparation method for Al2O3-C refractory - Google Patents

Al2O3-C refractory fired by nitridation and preparation method for Al2O3-C refractory Download PDF

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Publication number
CN102503485A
CN102503485A CN2011103447672A CN201110344767A CN102503485A CN 102503485 A CN102503485 A CN 102503485A CN 2011103447672 A CN2011103447672 A CN 2011103447672A CN 201110344767 A CN201110344767 A CN 201110344767A CN 102503485 A CN102503485 A CN 102503485A
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fire resistant
resistant materials
nitrogenize
al2o3
refractory
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祝洪喜
彭玮珂
邓承继
朱万政
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Wuhan University of Science and Engineering WUSE
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Wuhan University of Science and Engineering WUSE
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Abstract

The invention relates to an Al2O3-C refractory fired by nitridation and a preparation method for the Al2O3-C refractory. According to the technical scheme, the preparation method comprises the following steps of: mixing 55 to 94 weight percent of corundum, 5 to 20 weight percent of crystalline flake graphite, 1 to 30 weight percent of metal Si fine powder which serve as raw materials, adding a bonding agent in an amount which is 3.5 to 8 percent of the weight of the raw materials, and mixing and grinding for 10 to 30 minutes; and pressing the mixed and ground mixture to form a raw blank of the required Al2O3-C refractory, baking the pressed raw blank at the temperature of between 180 and 220 DEG C, putting into a high-temperature kiln, and keeping the temperature at the temperature of between 1,350 and 1,700 DEG C under the atmosphere of N2 for 1 to 8 hours to obtain the Al2O3-C refractory fired by the nitridation. The Al2O3-C refractory fired by the nitridation comprises a case-hardened Al2O3-C refractory brick, an Al2O3-C protective tube for the continuous casting of molten steel, an Al2O3-C sliding plate for the pouring of the molten steel and a nozzle brick. The Al2O3-C refractory has the characteristics of high strength, oxidation resistance, long service life and high performance of resisting the washing and erosion of high-temperature melts.

Description

The Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof
Technical field
The invention belongs to Al 2O 3-C fire resistant materials technical field.Relate in particular to the Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof.
Background technology
Since the seventies in 20th century, because Iron And Steel Industry fast development and The application of new technique press for the good novel refractory of durability to satisfy new demand, people have carried out number of research projects to novel high-performance refractory material.Al 2O 3-C fire resistant materials has obtained applying widely because of it has good wearing quality, especially on metallurgy high temperature equipment such as iron-smelting blast furnace, fish torpedo type iron mixing vehicle, iron ladle, and Al 2O 3-C fire resistant materials is its main high-temperature resistant inner lining material, is in indispensable status.
Al 2O 3The core technology of-C fire resistant materials is at Al 2O 3Introduced C (crystalline flake graphite) in the fire resistant materials (corundum).Because crystalline flake graphite has the good opposing high-temperature slag and the wettability of molten iron and molten steel, thereby can improve Al effectively 2O 3The erosion-resisting characteristics of fire resistant materials.In addition, the thermal conductivity of crystalline flake graphite is good, under the high temperature working conditions, adds crystalline flake graphite and can reduce Al 2O 3Fire resistant materials temperature inside gradient and thermal stresses, and then the anti-thermal shock stability of raising refractory materials are added crystalline flake graphite itself and are had good temperature resistance, therefore, and at Al 2O 3Add crystalline flake graphite in the fire resistant materials and prepare Al 2O 3-C fire resistant materials can improve the use properties of refractory materials comprehensively.Like patent JP57123860 (A), JP61215251 (A), JP1212274 (A), US5746895 (A), CN1424279 (A) etc. has done corresponding explanation.But C (crystalline flake graphite) is oxidized easily under hot conditions, and promptly at high temperature C is lost by burning easily, works as Al 2O 3The C of-C fire resistant materials is oxidized fall after, Al 2O 3The void content of-C fire resistant materials increases and the porosity and looseness that becomes, and the intensity of material obviously reduces, cause material opposing high-temperature fusant washing away and erosional competency reduces, deterioration the use properties of material, greatly influenced Al 2O 3The result of use of-C fire resistant materials.
For solving C (crystalline flake graphite) oxidized problem under hot conditions, people have carried out number of research projects, have extensively adopted at Al 2O 3-C fire resistant materials adds the oxidation inhibitor way, and the material that is used as additive mainly is metal A l, Si, Mg and SiC, Si 3N 4Deng, with the fine powder of these materials separately or mix and add Al to 2O 3In-C the fire resistant materials and even with mechanically mixing, when high temperature oxidation took place, oxidizing reaction at first or with C (crystalline flake graphite) took place in these additives simultaneously, can slow down the oxidising process of C (crystalline flake graphite), but to improving Al 2O 3The bulk strength of-C fire resistant materials is contribution not.
Summary of the invention
Task of the present invention provides that a kind of antioxidant property is good, intensity is high, long service life, opposing high-temperature fusant wash away the Al that burns till with the good nitrogenize of erosion performance 2O 3-C fire resistant materials and preparation method thereof.
For realizing above-mentioned task, the technical scheme that the present invention adopted is: be raw materials mix with the corundum of 55～94wt%, the crystalline flake graphite of 5～20wt% and the metal Si fine powder of 1～30wt% earlier, add the wedding agent of said raw material 3.5～8wt%, mix and ground 10～30 minutes.
The compound that mixes after grinding is pressed into required Al 2O 3The green compact of-C fire resistant materials product, with 180 ~ 220 ℃ of bakings of green compact warp that are pressed into, the high temperature kiln of packing into then is interior in 1350 ~ 1700 ℃ and N again 2Atmospheric condition is incubated 1 ~ 8 hour down, makes the Al that nitrogenize is burnt till 2O 3-C fire resistant materials.
The Al that nitrogenize is burnt till 2O 3-C fire resistant materials comprises typing Al 2O 3-C refractory brick, continuous casting of molten steel are used Al 2O 3-C quality guarantee pillar, pouring molten steel are used Al 2O 3-C matter slide plate and nozzle brick.
In technique scheme: corundum is Al 2O 3The matter refractory raw material, the Al of corundum 2O 3Content>=93wt%; C content>=the 90wt% of crystalline flake graphite; Metal Si fine powder is technical grade metal Si, granularity≤200 orders; N 2Gas is industrial N 2Gas; Wedding agent is a resol or for pitch or for resol and bituminous mixture.
Because adopt technique scheme, the present invention has adopted metal Si fine powder and N 2The pyroreaction of gas is to optimize the structure and the performance of material: at N 2High-temperature ammonolysis burns till the stage under the atmospheric condition, metal Si fine powder and N 2Solid/liquid/gas reactions generates silicon nitride (N 3Si 4), newly-generated silicon nitride (N 3Si 4) in the matrix of material, played well " bridge joint " effect, strengthened the binding between material granule and the fine powder, form firm integral body, increased Al significantly 2O 3The bonding strength that-C fire resistant materials is inner has improved Al 2O 3The erosion resistibility of-C fire resistant materials opposing high-temperature slag and molten iron or molten steel; In the high temperature use, during as if the chance oxidizing condition, the silicon nitride (N of material surface 3Si 4) oxidized back generation SiO 2And the pore on bridge material surface, stop O 2Gas gets into material internal, and the graphite that reaches in the protecting materials is not oxidized, and then reaches the prolongation material purpose in work-ing life.
Therefore, the present invention has overcome traditional Al 2O 3The intensity of-C fire resistant materials is low, in the high temperature use because C (crystalline flake graphite) oxidation and the shortcoming of deterioration material property, have the characteristics good of washing away of intensity height, anti-oxidant, long service life, opposing high-temperature fusant with erosion performance.
Embodiment
Below in conjunction with embodiment, the present invention is done further description, be not restriction to protection domain.
For avoiding repetition, the raw material physics and chemistry technical parameter unification that earlier this embodiment will be related to is described below, and embodiment repeats no more: corundum is Al 2O 3The matter refractory raw material, the Al of corundum 2O 3Content>=93wt%; C content>=the 90wt% of crystalline flake graphite; Metal Si fine powder is technical grade metal Si, granularity≤200 orders; N 2Gas is industrial N 2Gas.
Embodiment 1
The Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof.Be raw materials mix with the corundum of 90～94wt%, the crystalline flake graphite of 5～8wt% and the metal Si fine powder of 1～5wt% earlier, the resol that adds said raw material 4.5～8wt% is made wedding agent, mixes and grinds 20～30 minutes.
The compound that mixes after grinding is pressed into Al 2O 3The green compact of-C matter nozzle brick, with 180 ~ 220 ℃ of bakings of nozzle brick green compact warp that are pressed into, the high temperature kiln of packing into then is interior in 1350 ~ 1400 ℃ and N again 2Atmospheric condition is incubated 6 ~ 8 hours down, makes the Al that nitrogenize is burnt till 2O 3-C matter nozzle brick.
Embodiment 2
The Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof.Is raw materials mix earlier with the corundum of 85～90wt%, the crystalline flake graphite of 5～8wt% and the metal Si fine powder of 5～10wt%, add said raw material 5.5～7wt% resol and bituminous mixture make wedding agent, mixed stone roller 20～30 minutes.
Compound after mixed the stone roller is pressed into pouring molten steel uses Al 2O 3The green compact of-C matter slide plate, with 180 ~ 220 ℃ of bakings of green compact warp that are pressed into, the high temperature kiln of packing into then is interior in 1400 ~ 1450 ℃ and N again 2Down insulation 5 ~ 7 hours of atmospheric condition makes the pouring molten steel that nitrogenize burns till and uses Al 2O 3-C matter slide plate.
Embodiment 3
The Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof.Be raw materials mix with the corundum of 80～85wt%, the crystalline flake graphite of 5～8wt% and the metal Si fine powder of 10～15wt% earlier, the resol and the bituminous mixture that add said raw material 6.0～7.5wt% are made wedding agent, mix and grind 15～25 minutes.
The compound that mixes after grinding is pressed into typing Al 2O 3The green compact of-C refractory brick, with 180 ~ 220 ℃ of bakings of green compact warp that are pressed into, the high temperature kiln of packing into then is interior in 1450 ~ 1500 ℃ and N again 2Atmospheric condition is incubated 4 ~ 6 hours down, makes the typing Al that nitrogenize is burnt till 2O 3-C refractory brick.
Embodiment 4
The Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof.Be raw materials mix with the corundum of 75～80wt%, the crystalline flake graphite of 5～8wt% and the metal Si fine powder of 15～20wt% earlier, the resol that adds said raw material 3.5～5.5wt% is made wedding agent, mixes and grinds 10～20 minutes.
Compound after mixed the stone roller is pressed into continuous casting of molten steel uses Al 2O 3The green compact of-C quality guarantee pillar, with 180 ~ 220 ℃ of bakings of green compact warp that are pressed into, the high temperature kiln of packing into then is interior in 1500 ~ 1550 ℃ and N again 2Down insulation 3 ~ 5 hours of atmospheric condition makes the continuous casting of molten steel that nitrogenize burns till and uses Al 2O 3-C quality guarantee pillar.
Embodiment 5
The Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof.Be raw materials mix with the corundum of 65～70wt%, the crystalline flake graphite of 8～12wt% and the metal Si fine powder of 20～25wt% earlier, the pitch that adds said raw material 6～8wt% is made wedding agent, mixes and grinds 15～25 minutes.Compound after mix grinding is pressed into the green compact of nozzle brick, again with the green compact that are pressed into through 180 ~ 220 ℃ of bakings, in the high temperature kiln of packing into then in 1550 ~ 1600 ℃ and N 2Atmospheric condition is incubated 2 ~ 4 hours down, makes the nozzle brick that nitrogenize is burnt till.
Embodiment 6
The Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof.Be raw materials mix with the corundum of 55～60wt%, the crystalline flake graphite of 12～15wt% and the metal Si fine powder of 25～30wt% earlier, the pitch that adds said raw material 5～7wt% is made wedding agent, mixes and grinds 20～30 minutes.Compound after mixed the stone roller is pressed into pouring molten steel uses Al 2O 3The green compact of-C matter slide plate, with 180 ~ 220 ℃ of bakings of green compact warp that are pressed into, the high temperature kiln of packing into then is interior in 1600 ~ 1650 ℃ and N again 2Down insulation 1 ~ 3 hour of atmospheric condition makes the pouring molten steel that nitrogenize burns till and uses Al 2O 3-C matter slide plate.
Embodiment 7
The Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof.Be raw materials mix with the corundum of 60～65wt%, the crystalline flake graphite of 7～14wt% and the metal Si fine powder of 25～30wt% earlier, the resol that adds said raw material 5～7wt% is made wedding agent, mixes and grinds 20～30 minutes.
Compound after mixed the stone roller is pressed into continuous casting of molten steel uses Al 2O 3The green compact of-C quality guarantee pillar, with 180 ~ 220 ℃ of bakings of green compact warp that are pressed into, the high temperature kiln of packing into then is interior in 1650 ~ 1700 ℃ and N again 2Down insulation 1 ~ 3 hour of atmospheric condition makes the continuous casting of molten steel that nitrogenize burns till and uses Al 2O 3-C quality guarantee pillar.
Embodiment 8
The Al that a kind of nitrogenize is burnt till 2O 3-C fire resistant materials and preparation method thereof.Be raw materials mix with the corundum of 70～75wt%, the crystalline flake graphite of 15～20 wt% and the metal Si fine powder of 10～15wt% earlier, the resol that adds said raw material 4～6wt% is made wedding agent, mixes and grinds 20～30 minutes.
The compound that mixes after grinding is pressed into typing Al 2O 3The green compact of-C refractory brick, with 180 ~ 220 ℃ of bakings of green compact warp that are pressed into, the high temperature kiln of packing into then is interior in 1600 ~ 1650 ℃ and N again 2Atmospheric condition is incubated 2 ~ 4 hours down, makes the typing Al that nitrogenize is burnt till 2O 3-C refractory brick.
 
This embodiment adopts metal Si fine powder and N 2The pyroreaction method of gas is to optimize the structure and the performance of material: at N 2High-temperature ammonolysis under the atmospheric condition burns till the stage, metal Si fine powder and N 2Solid/liquid/gas reactions generates silicon nitride (N 3Si 4), newborn silicon nitride (N 3Si 4) in the matrix of material, played well " bridge joint " effect, strengthened the binding between material granule and the fine powder, form firm integral body, increased Al significantly 2O 3The bonding strength that-C fire resistant materials is inner has improved Al 2O 3The erosion resistibility of-C fire resistant materials opposing high-temperature slag and molten iron or molten steel; In the high temperature use, during as if the chance oxidizing condition, the silicon nitride (N of material surface 3Si 4) oxidized back generation SiO 2And the pore on bridge material surface, can stop O 2Gas gets into material internal, and the graphite that reaches in the protecting materials is not oxidized, and then reaches the prolongation material purpose in work-ing life.
Therefore, this embodiment has overcome traditional Al 2O 3The intensity of-C fire resistant materials is low, in the high temperature use because graphite (C) oxidation and the shortcoming of deterioration material property, Al is burnt till in the nitrogenize of being invented 2O 3What-C fire resistant materials had intensity height, anti-oxidant, an opposing high-temperature fusant washes away characteristics good with erosion performance, long service life.

Claims (7)

1. Al that nitrogenize is burnt till 2O 3The preparation method of-C fire resistant materials is characterized in that being raw materials mix with the corundum of 55～94wt%, the crystalline flake graphite of 5～20wt% and the metal Si fine powder of 1～30wt% earlier, adds the wedding agent of said raw material 3.5～8wt%, mixes and grinds 10～30 minutes;
The compound that mixes after grinding is pressed into required Al 2O 3The green compact of-C fire resistant materials product, with 180 ~ 220 ℃ of bakings of green compact warp that are pressed into, the high temperature kiln of packing into then is interior in 1350 ~ 1700 ℃ and N again 2Atmospheric condition is incubated 1 ~ 8 hour down, makes the Al that nitrogenize is burnt till 2O 3-C fire resistant materials.
2. the Al that said nitrogenize is burnt till according to claim 1 2O 3The preparation method of-C fire resistant materials is characterized in that the Al that described nitrogenize is burnt till 2O 3-C fire resistant materials comprises typing Al 2O 3-C refractory brick, continuous casting of molten steel are used Al 2O 3-C quality guarantee pillar, pouring molten steel are used Al 2O 3-C matter slide plate and nozzle brick.
3. the Al that said nitrogenize is burnt till according to claim 1 2O 3The preparation method of-C fire resistant materials is characterized in that described corundum is Al 2O 3The matter refractory raw material, the Al of corundum 2O 3Content>=93wt%.
4. the Al that said nitrogenize is burnt till according to claim 1 2O 3The preparation method of-C fire resistant materials is characterized in that the C content>=90wt% of described crystalline flake graphite.
5. the Al that said nitrogenize is burnt till according to claim 1 2O 3The preparation method of-C fire resistant materials is characterized in that described metal Si fine powder is technical grade metal Si, becomes segmentation, granularity≤200 orders through grinding and processing.
6. the Al that said nitrogenize is burnt till according to claim 1 2O 3The preparation method of-C fire resistant materials is characterized in that described wedding agent is a resol or for pitch or for resol and bituminous mixture.
7. the Al that burns till according to each said nitrogenize in the claim 1 ~ 6 2O 3The Al that the prepared nitrogenize of the preparation method of-C fire resistant materials is burnt till 2O 3-C fire resistant materials.
CN2011103447672A 2011-11-04 2011-11-04 Al2O3-C refractory fired by nitridation and preparation method for Al2O3-C refractory Pending CN102503485A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102826863A (en) * 2012-09-13 2012-12-19 北京科技大学 Method for preparing an Al-Cr2O3-Al2O sliding plate by aluminum-chrome slag and sliding plate material
CN104177104A (en) * 2014-08-29 2014-12-03 中钢集团洛阳耐火材料研究院有限公司 Preparation method of titanium nitride-containing in-situ composite aluminum-carbon refractory material
CN107400752A (en) * 2017-09-26 2017-11-28 湖南湘钢瑞泰科技有限公司 Tapping hole assembly and converter
CN107673769A (en) * 2017-09-30 2018-02-09 安徽云天冶金科技股份有限公司 A kind of low silicon Sialon pushing off the slag flashboard and its production method
CN111087229A (en) * 2019-12-05 2020-05-01 宜兴市耐火材料有限公司 Nano-material modified high-oxidation-resistance long nozzle and preparation process thereof

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CN1927508A (en) * 2006-09-25 2007-03-14 山东中齐耐火材料有限公司 Aluminium-carbon stopper for continuous casting

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CN1927508A (en) * 2006-09-25 2007-03-14 山东中齐耐火材料有限公司 Aluminium-carbon stopper for continuous casting

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Title
石凯: "Al/Si复合Al2O3-C材料的高温性能、显微结构及研制", 《中国博士学位论文全文数据库（工程科技I辑）》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102826863A (en) * 2012-09-13 2012-12-19 北京科技大学 Method for preparing an Al-Cr2O3-Al2O sliding plate by aluminum-chrome slag and sliding plate material
CN104177104A (en) * 2014-08-29 2014-12-03 中钢集团洛阳耐火材料研究院有限公司 Preparation method of titanium nitride-containing in-situ composite aluminum-carbon refractory material
CN104177104B (en) * 2014-08-29 2016-01-13 中钢集团洛阳耐火材料研究院有限公司 A kind of preparation method of titaniferous nitride in-situ composite aluminum-carbon refractory material
CN107400752A (en) * 2017-09-26 2017-11-28 湖南湘钢瑞泰科技有限公司 Tapping hole assembly and converter
CN107673769A (en) * 2017-09-30 2018-02-09 安徽云天冶金科技股份有限公司 A kind of low silicon Sialon pushing off the slag flashboard and its production method
CN111087229A (en) * 2019-12-05 2020-05-01 宜兴市耐火材料有限公司 Nano-material modified high-oxidation-resistance long nozzle and preparation process thereof

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Application publication date: 20120620