CN108033778A - A kind of preparation method of low-carbon fire resisting long nozzle material - Google Patents

A kind of preparation method of low-carbon fire resisting long nozzle material Download PDF

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Publication number
CN108033778A
CN108033778A CN201711173652.5A CN201711173652A CN108033778A CN 108033778 A CN108033778 A CN 108033778A CN 201711173652 A CN201711173652 A CN 201711173652A CN 108033778 A CN108033778 A CN 108033778A
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long nozzle
low
fire resisting
nozzle material
parts
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鲁庭志
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MA'ANSHAN LIRUN METALLURGY MATERIAL CO Ltd
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MA'ANSHAN LIRUN METALLURGY MATERIAL CO Ltd
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    • 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
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    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
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    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
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  • Organic Chemistry (AREA)
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  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a kind of preparation method of low-carbon fire resisting long nozzle material, using crystalline flake graphite as carbon source, ZrO is covered with its surface2Coating, is used as basic castable with fused brown corundum, fused white corundum, carborundum compounding, adds antioxidant, be molded using isostatic pressing process, low-carbon fire resisting long nozzle material is prepared.In flake graphite's surface cladding Zr (OH) in the present invention4Gel, after high temperature sintering, is coated with ZrO2 layers, the wettability and inoxidizability for making modified graphite are improved significantly, and the presence of face coat also improves the antioxygenic property of castable, thermal shock resistance on graphite flakes surface；In addition nanometer ZrO is added2Zirconium ion content is supplemented, improves the fire resistance of product, while is molded using isostatic pressing process, base substrate uniform force, Density Distribution is homogeneous, improves the sintered density of product, has excellent anti-molten steel and slag corrosion performance.

Description

A kind of preparation method of low-carbon fire resisting long nozzle material
Technical field
The present invention relates to technical field of refractory materials, and in particular to a kind of preparation method of low-carbon fire resisting long nozzle material.
Background technology
Graphite has the characteristics that to be not easy by molten steel and slag wetting, thermal coefficient of expansion is small and thermal conductivity is high, is introduced into In refractory material, the anti-slag erosion ability and thermal shock resistance of refractory material are remarkably improved.At present, carbon containing refractory is in height All multiple locations of the steel and iron industries such as stove furnace bottom and iron tap channel, the liner body of converter, electric furnace and ladle, the mouth of a river, slide plate and stopper obtain Extensive use.
Carbon long runner inner wall process of deteriorating is aoxidized and dissolving forms decarburized layer first for carbon, afterwards being mingled with molten steel The thing FeO and Al in decarburized layer2O3Reaction forms hercynite, and as FeO continues to adhere to, it is rich to form FeO in decarburization layer surface Ji Qu simultaneously generates low melting point phase, causes decarburized layer gradually to deteriorate under the washing away of high speed molten steel；2）Long nozzle slag lining deteriorates Dissolved first into molten steel for carbon, be afterwards the oxide in Tundish Slag erosion material, two processes alternately, so as to lead Deteriorating for long nozzle slag lining material has been caused, has shortened the service life of long nozzle.
Natural flake graphite is small with thermal coefficient of expansion, and thermal conductivity is good, the advantages that being not easy to be soaked by slag, becomes naturally most Preferable carbon source.But crystalline flake graphite density is small, is not soaked with water so that graphite easily floats in castable and is difficult to uniformly divide Dissipate, and graphite is oxidizable at high temperature.
The content of the invention
The present invention provides a kind of preparation method of low-carbon fire resisting long nozzle material, the anti-slag for helping to improve castable is oozed Permeability and corrosion resistance.
A kind of preparation method of low-carbon fire resisting long nozzle material, using crystalline flake graphite as carbon source, ZrO is covered with its surface2Apply Layer, with fused brown corundum, fused white corundum, carborundum compounding be used as basic castable, add antioxidant, using isostatic pressed into Type technological forming, is prepared low-carbon fire resisting long nozzle material.
Wherein, the ZrO2Coating is with Zr (OH)4The mode of hydrogel introduces, and is coated by sol-gel technology In flake graphite's surface, the basic castable further includes a nanometer ZrO2Particle.
Concrete technology step is as follows：
（1）Gel coated graphite：
Take 16-28 parts of ZrOCl2·8H2O is raw material, is added into appropriate distilled water, adds 4-8 parts of polyethylene glycol as scattered Agent, adds 3% Y (NO3)3For stabilizer, after stirring evenly, 8-14 parts of crystalline flake graphites are added, are dispersed with stirring 15-30 minutes, ultrasound Scattered 8-15 minute, after graphite dispersion is uniform, concentrated ammonia liquor is added dropwise until the pH value of solution is to 9-10, be aged 10-15 it is small when after, Washed 3-5 times repeatedly with distilled water, alcohol water coke slurry is then carried out using absolute ethyl alcohol, obtained gel strength converts into ZrO2Content exists The coagulant liquid of 8-10wt%；
（2）Shaping：
By 25-40 parts of fused brown corundums, 15-25 parts of fused white corundums, 8-13 parts of carborundum and 6-12 parts of nanometer ZrO2Particle according to Secondary to be added in above-mentioned coagulant liquid, after mixing, addition antioxidant is compound for strong stirring, after stirring evenly, ageing mixture 10-15 Hour, pour into a mould, be molded using isostatic pressing process under 100-150MPa, in 105-120 DEG C of temperature according to required specification When the lower drying 20-25 of degree is small；
（3）Sintering：
Then blank after shaping is placed in high-temperature cellar, at 1250-1280 DEG C, 1310-1360 DEG C and 1420-1480 DEG C respectively Insulation 1-4 is burnt till when small, is taken out after furnace cooling, you can.
Wherein, the antioxidant is by the B for the Si and 0.4% that mass fraction is 2%4C is formed.
Wherein, the step（2）The nanometer ZrO used2Mean particle size is in 35-45nm.
The present invention has the beneficial effect that：
Using crystalline flake graphite as carbon source in the present invention, in its surface cladding Zr (OH)4Gel, after high temperature sintering, in graphite flakes Surface is coated with ZrO2 layers, and the wettability and inoxidizability for making modified graphite are improved significantly, and improve castable base Bonding state between matter, meanwhile, the presence of face coat also becomes the barrier for preventing oxygen from spreading, and improves the anti-oxidant of castable Performance, thermal shock resistance are also improved, while Zr (OH)4Gel has good dispersiveness, can be risen in castable To the effect of bonding agent, without adding bonding agent, sintering is effectively facilitated；Since the gel strength of introducing is relatively low, in addition add Nanometer ZrO2Zirconium ion content is supplemented, improves the fire resisting erosion-resisting characteristics of product, while be molded using isostatic pressing process, base Body uniform force, Density Distribution is homogeneous, improves the sintered density of product, has excellent anti-molten steel and slag corrosion performance.
Embodiment
A kind of preparation method of low-carbon fire resisting long nozzle material, using crystalline flake graphite as carbon source, ZrO is covered with its surface2Apply Layer, with fused brown corundum, fused white corundum, carborundum compounding be used as basic castable, add antioxidant, using isostatic pressed into Type technological forming, is prepared low-carbon fire resisting long nozzle material.
Wherein, the ZrO2Coating is with Zr (OH)4The mode of hydrogel introduces, and is coated by sol-gel technology In flake graphite's surface, the basic castable further includes a nanometer ZrO2Particle.
Concrete technology step is as follows：
（1）Gel coated graphite：
Take 24 parts of ZrOCl2·8H2O is raw material, is added into appropriate distilled water, adds 6 parts of polyethylene glycol as dispersant, adds Enter 3% Y (NO3)3For stabilizer, after stirring evenly, 8 parts of crystalline flake graphites are added, are dispersed with stirring 30 minutes, ultrasonic disperse 15 minutes, After graphite dispersion is uniform, concentrated ammonia liquor is added dropwise until the pH value of solution is to 9-10, when ageing 12 is small after, washed repeatedly with distilled water 5 times, alcohol water coke slurry is then carried out using absolute ethyl alcohol, obtained gel strength converts into ZrO2Coagulant liquid of the content in 10wt%；
（2）Shaping：
By 35 parts of fused brown corundums, 20 parts of fused white corundums, 8 parts of carborundum and 12 parts of nanometer ZrO2Particle is added sequentially to above-mentioned In coagulant liquid, after mixing, addition antioxidant is compound, after stirring evenly, when ageing mixture 12 is small, according to required rule for strong stirring Lattice size is poured into a mould, and is molded using isostatic pressing process under 100MPa, when drying 24 is small at a temperature of 110 DEG C；
（3）Sintering：
Then blank after shaping is placed in high-temperature cellar, when insulation 1 is small at 1250 DEG C, when insulation 2 is small at 1350 DEG C, 1460 DEG C It is lower insulation 4 it is small when burn till, taken out after furnace cooling, you can.
Wherein, the antioxidant is by the B for the Si and 0.4% that mass fraction is 2%4C is formed.
Wherein, the step（2）The nanometer ZrO used2Mean particle size is in 40nm.

Claims (5)

1. a kind of preparation method of low-carbon fire resisting long nozzle material, it is characterised in that using crystalline flake graphite as carbon source, covered on its surface There is ZrO2Coating, is used as basic castable with fused brown corundum, fused white corundum, carborundum compounding, adds antioxidant, use Isostatic pressing process is molded, and low-carbon fire resisting long nozzle material is prepared.
A kind of 2. preparation method of low-carbon fire resisting long nozzle material according to claim 1, it is characterised in that the ZrO2 Coating is with Zr (OH)4The mode of hydrogel introduces, and flake graphite's surface is coated onto by sol-gel technology, described Basic castable further includes a nanometer ZrO2Particle.
A kind of 3. preparation method of low-carbon fire resisting long nozzle material according to claim 1, it is characterised in that concrete technology Step is as follows：
（1）Gel coated graphite：
Take 16-28 parts of ZrOCl2·8H2O is raw material, is added into appropriate distilled water, adds 4-8 parts of polyethylene glycol as scattered Agent, adds 3% Y (NO3)3For stabilizer, after stirring evenly, 8-14 parts of crystalline flake graphites are added, are dispersed with stirring 15-30 minutes, ultrasound Scattered 8-15 minute, after graphite dispersion is uniform, concentrated ammonia liquor is added dropwise until the pH value of solution is to 9-10, be aged 10-15 it is small when after, Washed 3-5 times repeatedly with distilled water, alcohol water coke slurry is then carried out using absolute ethyl alcohol, obtained gel strength converts into ZrO2Content exists The coagulant liquid of 8-10wt%；
（2）Shaping：
By 25-40 parts of fused brown corundums, 15-25 parts of fused white corundums, 8-13 parts of carborundum and 6-12 parts of nanometer ZrO2Particle is successively It is added in above-mentioned coagulant liquid, after mixing, addition antioxidant is compound, and after stirring evenly, ageing mixture 10-15 is small for strong stirring When, pour into a mould, be molded using isostatic pressing process under 100-150MPa, in 105-120 DEG C of temperature according to required specification When lower dry 20-25 is small；
（3）Sintering：
Then blank after shaping is placed in high-temperature cellar, at 1250-1280 DEG C, 1310-1360 DEG C and 1420-1480 DEG C respectively Insulation 1-4 is burnt till when small, is taken out after furnace cooling, you can.
4. the preparation method of a kind of low-carbon fire resisting long nozzle material according to claim 1,3, it is characterised in that described anti- Oxidant is by the B for the Si and 0.4% that mass fraction is 2%4C is formed.
A kind of 5. preparation method of low-carbon fire resisting long nozzle material according to claim 2,3, it is characterised in that the step Suddenly（2）The nanometer ZrO used2Mean particle size is in 35-45nm.
CN201711173652.5A 2017-11-22 2017-11-22 A kind of preparation method of low-carbon fire resisting long nozzle material Pending CN108033778A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110436941A (en) * 2019-09-06 2019-11-12 华北理工大学 A kind of method of modifying of zirconium modification expanded graphite
CN111875357A (en) * 2020-07-30 2020-11-03 海城市金福锋科技有限公司 Anti-oxidation high-fracture-resistance hearth castable and production method thereof
CN112791699A (en) * 2021-01-20 2021-05-14 辽宁科技大学 ZrO (ZrO)2Preparation method of coal tar pitch-based composite activated carbon spheres

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101186456A (en) * 2007-12-06 2008-05-28 上海大学 Method for preparing hydrophilic graphite/oxide composite powder
CN103755364A (en) * 2013-12-30 2014-04-30 江苏苏嘉集团新材料有限公司 Graphite composite fire resistant material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101186456A (en) * 2007-12-06 2008-05-28 上海大学 Method for preparing hydrophilic graphite/oxide composite powder
CN103755364A (en) * 2013-12-30 2014-04-30 江苏苏嘉集团新材料有限公司 Graphite composite fire resistant material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110436941A (en) * 2019-09-06 2019-11-12 华北理工大学 A kind of method of modifying of zirconium modification expanded graphite
CN111875357A (en) * 2020-07-30 2020-11-03 海城市金福锋科技有限公司 Anti-oxidation high-fracture-resistance hearth castable and production method thereof
CN112791699A (en) * 2021-01-20 2021-05-14 辽宁科技大学 ZrO (ZrO)2Preparation method of coal tar pitch-based composite activated carbon spheres

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Application publication date: 20180515