CN104177099B - A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof - Google Patents
A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof Download PDFInfo
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- CN104177099B CN104177099B CN201410405108.9A CN201410405108A CN104177099B CN 104177099 B CN104177099 B CN 104177099B CN 201410405108 A CN201410405108 A CN 201410405108A CN 104177099 B CN104177099 B CN 104177099B
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Abstract
The present invention relates to a kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof.Its technical scheme is: with the γ Al of 45 ~ 65wt%2O3Fine powder, the α Al of 30 ~ 50wt%2O3The nano aluminium oxide micropowder of micropowder and 1 ~ 10wt% was raw material, the water of additional described raw material 40 ~ 80wt%, with planetary ball mill wet grinding 0.5 ~ 3 hour；Again the slip after wet grinding is placed in mould, places 12 ~ 24 hours under room temperature condition, the demoulding；Then it is dried 12 ~ 36 hours under the conditions of 110 ~ 200 DEG C, under the conditions of 1750 ~ 1900 DEG C, is incubated 1 ~ 8 hour, obtains micro-closed pore light-weight corundum fireproof aggregate.Micro-closed pore light-weight corundum fireproof aggregate prepared by the present invention has the advantages that apparent porosity is low, closed porosity is high, bulk density is less, average pore size is little, thermal conductivity is relatively low and slag-resistant erosiveness is strong.
Description
Technical field
The invention belongs to corundum fireproof aggregate technical field.Be specifically related to a kind of micro-closed pore light-weight corundum fireproof aggregate and
Its preparation method.
Background technology
Along with external refining and the development of continuous casting technology, ladle is gradually changed by the splendid attire steel in water container of original function singleness
For the outer liquid steel refining equipment of stove that function is complicated.During current lining material in the ladle uses, it is primarily present two mainly ask
Topic: (1) inner lining material pyroconductivity is higher, causes liquid steel temperature to decline very fast, is unfavorable for that continuous casting produces and is smoothed out, to molten steel
Quality also has considerable influence, and adds energy consumption；(2) inner lining material Spalling resistance energy and slag resistance are the most excellent, special
The diversity not being the different smelting condition lower liner material slag resistance such as slag system, steel grade is bigger.
Working lining refractory material lightweight is the important research direction solving the problems referred to above.First, insulating refractory material
Material is the closer to work surface, and its heat-insulating and energy-saving effect is the best, and working lining refractory material lightweight can effectively reduce ladle heat and scatter and disappear；
Second, owing to light weight refractory material having more pore, can effectively accommodate thermal stress when jump in temperature, promote material
Spalling resistance energy；3rd, when light weight aggregate apparent porosity is relatively low, closed porosity is high, average pore size is little, light weight fire proofed wood
Material slag resistance significantly reduces, it could even be possible to promote material slag resistance.Therefore, the grinding of working lining light weight refractory material
Study carefully the extensive concern by refractories industry.
Refractory aggregate lightweight is to realize the light-weighted main path of working lining refractory material.The light weight aggregate of report at present
Preparation method mainly has: the inorganic matter decomposition methods such as Organic substance decomposition method, foam in place hole creating technology and hydroxide.O.
Lyckfeldt et al. uses starch as bonding agent and foaming agent, is prepared for Woelm Alumina (O. Lyckfeldt, J. M.
F. Ferreira, Processing of porous ceramics by starch consolidation, J. Eur.
Ceram. Soc. 18 (2) (1998) 131 140.), prepared aggregate volume density substantially reduces, but apparent porosity and
Aperture is bigger；S. J. Li et al. use kaolinite as foaming agent, be prepared for porous corundum-mullite aggregate (S. J. Li,
N. Li, Effects of composition and temperature on porosity and pore size
distribution of porous ceramics prepared from Al(OH)3 and kaolinite gangue,
Ceram. Int. 33 (4) (2007) 551-556.), prepared aggregate average pore size is less, but apparent porosity is up to
40%；R. Salom oa et al. utilizes the decomposition in situ of brucite, is prepared for porous corundum-spinel aggregate (R. Salom
oa, M.V. Bôasa, V.C. Pandolfellia, Porous alumina-spinel ceramics for high
Temperature applications, Ceram. Int. 37 (4) (2011) 1393-1399.), prepared aggregate exists
Apparent porosity and aperture aspect are also unable to reach production requirement.
In sum, all there is the defect that apparent porosity is high, average pore size is big in the most prepared light weight refractory aggregate, difficult
To reach the requirement of actual industrial production.
Summary of the invention
It is contemplated that overcome prior art defect, task is to provide one, and apparent porosity is low, closed porosity is high, volume
Density is less, average pore size is little, thermal conductivity is relatively low and slag-resistant erosiveness is strong micro-closed pore light-weight corundum fireproof aggregate and
Preparation method.
For realizing above-mentioned task, the technical solution adopted in the present invention is: with the γ-Al of 45 ~ 65wt%2O3Fine powder, 30 ~
α-the Al of 50wt%2O3The nano aluminium oxide micropowder of micropowder and 1 ~ 10wt% is raw material, the water of additional described raw material 40 ~ 80wt%, uses
Planetary ball mill wet grinding 0.5 ~ 3 hour；Again the slip after wet grinding is placed in mould, places 12 ~ 24 hours under room temperature condition,
The demoulding；Then it is dried 12 ~ 36 hours under the conditions of 110 ~ 200 DEG C, under the conditions of 1750 ~ 1900 DEG C, is incubated 1 ~ 8 hour, obtains micro-
Closed pore light-weight corundum fireproof aggregate.
Described γ-Al2O3The Al of fine powder2O3Content > 99wt%, particle diameter is 0.045 ~ 0.088mm.
Described α-Al2O3The Al of micropowder2O3Content > 99wt%, particle diameter D50It it is 1 ~ 5 μm.
The Al of described nano aluminium oxide micropowder2O3Content > 99wt%, mean diameter is 20 ~ 50nm.
The mill ball of described planetary ball mill is corundum ball.
Owing to using technique scheme, the present invention compared with prior art has a following good effect:
Owing to nano material has small-size effect, its diffusion coefficient exceeds three orders of magnitude than common material, therefore, originally
Invention introduces nano aluminium oxide micropowder can effectively promote the High-temperature Superplasticity of sintered body.Meanwhile, nano aluminium oxide and micron order
Other α-Al2O3Micropowder and γ-Al2O3Fine powder is collectively forming the double yardstick Sintering Model of nano-micrometer, in high temperature sintering process, by
In the diversity of different grain size alumina raw material sintering character, it is formed in situ internal stress.Additionally, γ-Al2O3Carrying out crystal formation
It also is able to provide certain internal stress during transformation.Under the driving of these internal stress, the High-temperature Superplasticity of sintered body is able to
Playing, crystal boundary quickly spreads, and is enclosed in by pore wherein, and meanwhile, along with the movement of crystal boundary, macroscopic void is divided into small gas
Hole, thus reach to be formed the purpose of micro-closed pore light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by the present invention: bulk density is 2.8 ~ 3.2g/cm3, apparent porosity
Being 2 ~ 10%, average pore size is 0.3 ~ 1 μm.
Therefore, the micro-closed pore light-weight corundum fireproof aggregate prepared by the present invention have that apparent porosity is low, closed porosity is high,
The feature that bulk density is less, average pore size is little, thermal conductivity is relatively low and slag-resistant erosiveness is strong.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described, not limiting of its scope:
For avoiding repeating, first by as follows to the raw material involved by this detailed description of the invention and technological parameter Unify legislation, implement
Example repeats no more:
Described γ-Al2O3The Al of fine powder2O3Content > 99wt%, particle diameter is 0.045 ~ 0.088mm.
Described α-Al2O3The Al of micropowder2O3Content > 99wt%, particle diameter D50It it is 1 ~ 5 μm.
The Al of described nano aluminium oxide micropowder2O3Content > 99wt%, mean diameter is 20 ~ 50nm.
The mill ball of described planetary ball mill is corundum ball.
Embodiment 1
A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof.γ-Al with 45 ~ 50wt%2O3Fine powder, 45 ~
α-the Al of 50wt%2O3The nano aluminium oxide micropowder of micropowder and 1 ~ 6wt% is raw material, and the water of additional described raw material 40 ~ 60wt%, with row
Celestial body grinding machine wet grinding 1.5 ~ 3 hours；Again the slip after wet grinding is placed in mould, places 12 ~ 24 hours under room temperature condition, de-
Mould；Then it is dried 24 ~ 36 hours under the conditions of 110 ~ 160 DEG C, under the conditions of 1750 ~ 1850 DEG C, is incubated 5 ~ 8 hours, obtains micro-closing
Hole light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by the present embodiment: bulk density is 3.0 ~ 3.2g/cm3；Apparent pore
Rate is 2 ~ 4%；Average pore size is 0.6 ~ 1 μm.
Embodiment 2
A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof.γ-Al with 45 ~ 50wt%2O3Fine powder, 45 ~
α-the Al of 50wt%2O3The nano aluminium oxide micropowder of micropowder and 1 ~ 6wt% is raw material, and the water of additional described raw material 60 ~ 80wt%, with row
Celestial body grinding machine wet grinding 0.5 ~ 1.5 hour；Again the slip after wet grinding is placed in mould, places 12 ~ 24 hours under room temperature condition,
The demoulding；Then it is dried 12 ~ 24 hours under the conditions of 150 ~ 200 DEG C, under the conditions of 1800 ~ 1900 DEG C, is incubated 1 ~ 5 hour, obtains micro-
Closed pore light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by the present embodiment: bulk density is 3.0 ~ 3.1g/cm3；Apparent pore
Rate is 2 ~ 4%；Average pore size is 0.5 ~ 1 μm.
Embodiment 3
A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof.γ-Al with 50 ~ 55wt%2O3Fine powder, 40 ~
α-the Al of 45wt%2O3The nano aluminium oxide micropowder of micropowder and 1 ~ 6wt% is raw material, and the water of additional described raw material 40 ~ 60wt%, with row
Celestial body grinding machine wet grinding 1.5 ~ 3 hours；Again the slip after wet grinding is placed in mould, places 12 ~ 24 hours under room temperature condition, de-
Mould；Then it is dried 24 ~ 36 hours under the conditions of 110 ~ 160 DEG C, under the conditions of 1750 ~ 1850 DEG C, is incubated 5 ~ 8 hours, obtains micro-closing
Hole light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by the present embodiment: bulk density is 3.0 ~ 3.2g/cm3；Apparent pore
Rate is 3 ~ 6%；Average pore size is 0.6 ~ 0.8 μm.
Embodiment 4
A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof.γ-Al with 50 ~ 55wt%2O3Fine powder, 40 ~
α-the Al of 45wt%2O3The nano aluminium oxide micropowder of micropowder and 1 ~ 6wt% is raw material, and the water of additional described raw material 60 ~ 80wt%, with row
Celestial body grinding machine wet grinding 0.5 ~ 1.5 hour；Again the slip after wet grinding is placed in mould, places 12 ~ 24 hours under room temperature condition,
The demoulding；Then it is dried 12 ~ 24 hours under the conditions of 150 ~ 200 DEG C, under the conditions of 1800 ~ 1900 DEG C, is incubated 1 ~ 5 hour, obtains micro-
Closed pore light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by the present embodiment: bulk density is 3.0 ~ 3.1g/cm3；Apparent pore
Rate is 4 ~ 6%；Average pore size is 0.5 ~ 1 μm.
Embodiment 5
A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof.γ-Al with 55 ~ 60wt%2O3Fine powder, 35 ~
α-the Al of 40wt%2O3The nano aluminium oxide micropowder of micropowder and 5 ~ 10wt% is raw material, the water of additional described raw material 40 ~ 60wt%, uses
Planetary ball mill wet grinding 1.5 ~ 3 hours；Again the slip after wet grinding is placed in mould, places 12 ~ 24 hours under room temperature condition,
The demoulding；Then it is dried 24 ~ 36 hours under the conditions of 110 ~ 160 DEG C, under the conditions of 1750 ~ 1850 DEG C, is incubated 5 ~ 8 hours, obtains micro-
Closed pore light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by the present embodiment: bulk density is 2.9 ~ 3.1g/cm3；Apparent pore
Rate is 4 ~ 7%；Average pore size is 0.4 ~ 0.6 μm.
Embodiment 6
A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof.γ-Al with 55 ~ 60wt%2O3Fine powder, 35 ~
α-the Al of 40wt%2O3The nano aluminium oxide micropowder of micropowder and 5 ~ 10wt% is raw material, the water of additional described raw material 60 ~ 80wt%, uses
Planetary ball mill wet grinding 0.5 ~ 1.5 hour；Again the slip after wet grinding is placed in mould, under room temperature condition, places 12 ~ 24 little
Time, the demoulding；Then it is dried 12 ~ 24 hours under the conditions of 150 ~ 200 DEG C, under the conditions of 1800 ~ 1900 DEG C, is incubated 1 ~ 5 hour, i.e.
Obtain micro-closed pore light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by the present embodiment: bulk density is 2.9 ~ 3.0g/cm3；Apparent pore
Rate is 5 ~ 8%；Average pore size is 0.5 ~ 0.7 μm.
Embodiment 7
A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof.γ-Al with 60 ~ 65wt%2O3Fine powder, 30 ~
α-the Al of 35wt%2O3The nano aluminium oxide micropowder of micropowder and 5 ~ 10wt% is raw material, the water of additional described raw material 40 ~ 60wt%, uses
Planetary ball mill wet grinding 1.5 ~ 3 hours；Again the slip after wet grinding is placed in mould, places 12 ~ 24 hours under room temperature condition,
The demoulding；Then it is dried 24 ~ 36 hours under the conditions of 110 ~ 160 DEG C, under the conditions of 1750 ~ 1850 DEG C, is incubated 5 ~ 8 hours, obtains micro-
Closed pore light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by the present embodiment: bulk density is 2.9 ~ 3.1g/cm3；Apparent pore
Rate is 5 ~ 9%；Average pore size is 0.3 ~ 0.6 μm.
Embodiment 8
A kind of micro-closed pore light-weight corundum fireproof aggregate and preparation method thereof.γ-Al with 60 ~ 65wt%2O3Fine powder, 30 ~
α-the Al of 35wt%2O3The nano aluminium oxide micropowder of micropowder and 5 ~ 10wt% is raw material, the water of additional described raw material 60 ~ 80wt%, uses
Planetary ball mill wet grinding 0.5 ~ 1.5 hour；Again the slip after wet grinding is placed in mould, under room temperature condition, places 12 ~ 24 little
Time, the demoulding；Then it is dried 12 ~ 24 hours under the conditions of 150 ~ 200 DEG C, under the conditions of 1800 ~ 1900 DEG C, is incubated 1 ~ 5 hour, i.e.
Obtain micro-closed pore light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by the present embodiment: bulk density is 2.8 ~ 3.0g/cm3；Apparent pore
Rate is 6 ~ 10%；Average pore size is 0.3 ~ 0.6 μm.
Owing to using technique scheme, this detailed description of the invention compared with prior art has a following good effect:
Owing to nano material has small-size effect, its diffusion coefficient exceeds three orders of magnitude than common material, therefore, draws
Enter nano aluminium oxide micropowder and can effectively promote the High-temperature Superplasticity of sintered body.Meanwhile, the α of nano aluminium oxide and micron level-
Al2O3Micropowder and γ-Al2O3Fine powder is collectively forming the double yardstick Sintering Model of nano-micrometer, in high temperature sintering process, due to difference
The diversity of granularity alumina raw material sintering character, is formed in situ internal stress.Additionally, γ-Al2O3When carrying out crystal conversion
It also is able to provide certain internal stress.Under the driving of these internal stress, the High-temperature Superplasticity of sintered body is played, brilliant
Boundary quickly spreads, and is enclosed in by pore wherein, and meanwhile, along with the movement of crystal boundary, macroscopic void is divided into Minute pores, thus reaches
To the purpose forming micro-closed pore light-weight corundum fireproof aggregate.
Micro-closed pore light-weight corundum fireproof aggregate prepared by this detailed description of the invention: bulk density is 2.8 ~ 3.2g/cm3,
Apparent porosity is 2 ~ 10%, and average pore size is 0.3 ~ 1 μm.
Therefore, the micro-closed pore light-weight corundum fireproof aggregate prepared by this detailed description of the invention has that apparent porosity is low, remains silent
The feature that the porosity is high, bulk density is less, average pore size is little, thermal conductivity is relatively low and slag-resistant erosiveness is strong.
Claims (2)
1. the preparation method of a micro-closed pore light-weight corundum fireproof aggregate, it is characterised in that with the γ-Al of 45～65wt%2O3Carefully
α-the Al of powder, 30～50wt%2O3Micropowder and 1～10wt% nano aluminium oxide micropowder be raw material, additional described raw material 40～
The water of 80wt%, with planetary ball mill wet grinding 0.5～3 hours；Again the slip after wet grinding is placed in mould, under room temperature condition
Place 12～24 hours, the demoulding；Then it is dried 12～36 hours under the conditions of 110～200 DEG C, under the conditions of 1750～1900 DEG C
It is incubated 1～8 hour, obtains micro-closed pore light-weight corundum fireproof aggregate；
Described γ-Al2O3The Al of fine powder2O3Content > 99wt%, particle diameter is 0.045～0.088mm；
Described α-Al2O3The Al of micropowder2O3Content > 99wt%, particle diameter D50It is 1～5 μm；
The Al of described nano aluminium oxide micropowder2O3Content > 99wt%, mean diameter is 20～50nm.
The preparation method of micro-closed pore light-weight corundum fireproof aggregate the most according to claim 1, it is characterised in that described planet
The mill ball of ball mill is corundum ball.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105060901B (en) * | 2015-07-24 | 2017-07-11 | 武汉科技大学 | A kind of light-weight corundum fireproof aggregate and preparation method thereof |
| CN104944996B (en) * | 2015-07-24 | 2017-08-08 | 武汉科技大学 | A kind of light-weight corundum composite fire aggregate and preparation method thereof |
| CN105236937B (en) * | 2015-09-01 | 2018-05-11 | 武汉科技大学 | A kind of isometrical micropore corundum complex phase ball of light weight and preparation method thereof |
| CN105237014B (en) * | 2015-11-06 | 2017-11-17 | 武汉科技大学 | A kind of micro- closed pore corundum multiple phase refractory material of lightweight and preparation method thereof |
| CN106431440B (en) * | 2016-10-17 | 2019-07-09 | 武汉科技大学 | A kind of micro- closed pore alumina refractory aggregate of light weight and preparation method thereof |
| CN106478078B (en) * | 2016-10-17 | 2019-07-09 | 武汉科技大学 | A kind of light weight alumina refractory aggregate and preparation method thereof containing micro- hole of holding one's breath |
| CN106747556B (en) * | 2016-11-24 | 2019-12-10 | 武汉科技大学 | Nano closed-cell light-weight corundum complex-phase refractory aggregate and preparation method thereof |
| CN106587956B (en) * | 2016-11-24 | 2019-12-10 | 武汉科技大学 | Nanocrystalline inner-hole light-weight corundum complex-phase refractory aggregate and preparation method thereof |
| WO2022144013A1 (en) * | 2020-12-31 | 2022-07-07 | 郑州轻工业大学 | Corundum-based micro-nano-porous heat insulating refractory material and preparation method therefor |
| CN115231908A (en) * | 2022-07-05 | 2022-10-25 | 洛阳欧斯特建材有限公司 | High-purity alumina brick for preparing lithium battery anode material kiln and preparation method thereof |
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| CN102659426A (en) * | 2012-04-20 | 2012-09-12 | 武汉科技大学 | Micro-porous high-strength anti-corrosion corundum refractory aggregate and preparation method thereof |
| CN103833383A (en) * | 2012-11-26 | 2014-06-04 | 东北大学 | Corundum-magnesium aluminum spinelle-textured refractory aggregate with closed-hole structure and preparation method of refractory aggregate |
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| CN102659426A (en) * | 2012-04-20 | 2012-09-12 | 武汉科技大学 | Micro-porous high-strength anti-corrosion corundum refractory aggregate and preparation method thereof |
| CN103833383A (en) * | 2012-11-26 | 2014-06-04 | 东北大学 | Corundum-magnesium aluminum spinelle-textured refractory aggregate with closed-hole structure and preparation method of refractory aggregate |
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Application publication date: 20141203 Assignee: Wuhan University of science and Technology Business Incubator Co.,Ltd. Assignor: WUHAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2020420000003 Denomination of invention: A kind of micro closed cell lightweight corundum refractory aggregate and its preparation method Granted publication date: 20160727 License type: Common License Record date: 20201021 |
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