CN107337437A - Lightweight periclase hercynite refractory material and preparation method thereof - Google Patents
Lightweight periclase hercynite refractory material and preparation method thereof Download PDFInfo
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- CN107337437A CN107337437A CN201710631762.5A CN201710631762A CN107337437A CN 107337437 A CN107337437 A CN 107337437A CN 201710631762 A CN201710631762 A CN 201710631762A CN 107337437 A CN107337437 A CN 107337437A
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Abstract
The present invention relates to a kind of lightweight periclase hercynite refractory material and preparation method thereof.Its scheme is：Particle diameter using 10 ~ 20wt% particle diameter as 3 ~ 5mm, 30 ~ 40wt% is porous periclase magnesia-alumina spinel ceramic material particle that 1 ~ 2.8mm and 10 ~ 15wt% particle diameter is 0.1 ~ 0.8mm nano aperture for aggregate, using the magnesia powder of the porous periclase magnesia-alumina spinel ceramic material fine powder of 8 ~ 15wt% nano aperture, 10 ~ 15wt% hercynite corundum composite fine powders and 10 ~ 20wt% as matrix, the bonding agent of additional aggregate and 2 ~ 8wt% of matrix sum.Aggregate is first placed in de-airing mixer, vacuumized, bonding agent is added, stirring, closes pumped vacuum systems；Matrix is added, is stirred, is molded, is dried, in 1500 ~ 1650 DEG C of insulations, cooling, produces lightweight periclase hercynite refractory material.The stomata of resulting product is nano-pore, and thermal conductivity factor is low, corrosion resistance is good, hang kliner coating function admirable and thermal shock resistance is high.
Description
Technical field
The invention belongs to Periclase-hercynite refractory material technical field.More particularly to a kind of lightweight periclase-
Hercynite refractory material and preparation method thereof.
Background technology
Periclase-hercynite refractory material due to excellent high-temperature stability and hang kliner coating performance, extensively
Applied to the cement rotary kiln clinkering zone using coal dust as fuel.Existing Periclase-hercynite refractory material is typically with burning
Knot or fused magnesite are made for raw material, and bulk density is larger and thermal conductivity factor is higher, in use, on the one hand can cause water
Mud Kiln Shell Temperature is too high, causes amount of heat to lose, and on the other hand can aggravate the weight of rotary kiln, increase wheel zone cylinder
Body stress, accelerate barrel distortion, increase potential safety hazard.
In order to reduce Kiln Shell Temperature, mitigate wheel zone load, convenient and safe production, refractory material worker has ground
MULTILAYER COMPOSITE refractory material be have issued to substitute conventional dense refractory material.Such as " periclase-magnesium iron hercynite/magnesium olive
Stone composite brick（ZL201510104066）" patented technology, the composite refractory with working lining and thermal insulation layer is prepared for, it is made
Standby complex process, thermal insulation layer intensity is relatively low, and thermal insulation layer easily cracks with compacted zone because hot physical property mismatches, and has a strong impact on
Service life；And for example " a kind of cement rotary kiln low heat conductivity magnesia-hercynite brick and its production method
（ZL201610021949.9）" patented technology, the low heat conduction with fibrous microcellular has been made by pore creating material of polypropylene fibre
Ferro-magnesium-aluminum spinelle fire-resistant material, but air vent aperture is larger, and be insertion shape so that refractory material is easily by sulfide in kiln and salt
The erosion medium resistances such as alkali；For another example " cement rotary kiln lightweight periclase-fireproof magnesia alumina spinel material and preparation method thereof
（ZL201410059476.2）" patented technology, substitute fine and close magnesia, system by raw material of porous square magnesium stone-spinel ceramic material
Obtained the lightweight refractory material of low heat conduction, but the aperture of lightweight refractory material stomata is larger, air permeability is high, resisting sulfide and
The erosiveness of the medium such as saline and alkaline is poor.
The content of the invention
It is contemplated that overcome prior art defect, it is therefore an objective to provide a kind of preparation technology simply and stomata is nano level
The preparation method of lightweight Periclase-hercynite refractory material, the lightweight periclase prepared with this method-iron aluminium point are brilliant
Stone Refractory Thermal Conductivity is low, corrosion resistance is good, hang kliner coating excellent performance and thermal shock resistance can be high.
To achieve the above object, the technical solution adopted by the present invention is：Nano-pore using 10 ~ 20wt% particle diameter as 3 ~ 5mm
Porous periclase-magnesia-alumina spinel ceramic material the particle in footpath, 30 ~ 40wt% particle diameter are porous for 1 ~ 2.8mm nano aperture
Periclase-magnesia-alumina spinel ceramic material particle and 10 ~ 15wt% particle diameter are porous side's magnesium of 0.1 ~ 0.8mm nano aperture
Stone-magnesia-alumina spinel ceramic material particle is aggregate, with the porous side of nano aperture of the 8 ~ 15wt% particle diameter less than 0.074mm
Magnesite-magnesia-alumina spinel ceramic material fine powder, 10 ~ 15wt% hercynite-corundum composite fine powders and 10 ~ 20wt% magnesia
Fine powder is matrix, with 2 ~ 8wt% of the aggregate and matrix sum Al3+Solution is bonding agent.
By mentioned component and its content：First the aggregate is placed in de-airing mixer, is evacuated to below 2.0kPa, then
Contain Al described in pouring into3+Solution, stir 10 ~ 15 minutes, close pumped vacuum systems；The matrix is subsequently poured into, is stirred,
Mechanical pressing under the conditions of 100 ~ 200MPa, dry 12 ~ 36 hours under the conditions of 110 ~ 220 DEG C, protected under the conditions of 1500 ~ 1650 DEG C
Temperature 3 ~ 8 hours, cooling, produces lightweight Periclase-hercynite refractory material.
The preparation process of porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is：
The first step, magnesite fine powder is first warming up to 650 ~ 750 DEG C with 1 ~ 1.5 DEG C/min speed, is incubated 3 ~ 6 hours；Again with
1.5 ~ 2 DEG C/min speed is warming up to 820 ~ 900 DEG C, is incubated 2 ~ 5 hours, finally 1000 are warming up to 2 ~ 3 DEG C/min speed ~
1200 DEG C, 3 ~ 7 hours are incubated, cooling, obtains the magnesium oxide powder of high porosity；
Second step, by the high porosity magnesium oxide powder for 63 ~ 91wt%, containing Al3+Solution is 1 ~ 22wt% and aluminium hydroxide
Micro mist is 1 ~ 24wt%, and first the magnesium oxide powder of the high porosity is placed in de-airing mixer, be evacuated to 2.0kPa with
Under, then contain Al by described in3+Solution and the aluminium hydroxide micro powder are poured into de-airing mixer, are stirred 20 ~ 40 minutes, and closing is taken out true
Empty set is united, and obtains compound；
3rd step, the compound is warming up to 100 ~ 200 DEG C, is incubated 5 ~ 9h, cooling, machine is pressed under the conditions of 50 ~ 150MPa
Type, the base substrate after shaping are dried 10 ~ 30 hours under the conditions of 100 ~ 150 DEG C；Then it is warming up to 0.7 ~ 1.7 DEG C/min speed
1050 ~ 1300 DEG C, 3 ~ 5 hours are incubated, then 1400 ~ 1600 DEG C are warming up to 3.5 ~ 5.5 DEG C/min speed, insulation 4 ~ 12 is small
When, cool down, produce porous periclase-magnesia-alumina spinel ceramic material of nano aperture.
The porous periclase of the nano aperture-magnesia-alumina spinel ceramic material obtains different-grain diameter through broken and screening
Ceramic particle and ceramic material fine powder.
It is described to contain Al3+Solution is Alumina gel or is liquor alumini chloridi or is the mixture of Alumina gel and liquor alumini chloridi；
Alumina gel in the mixture: the mass ratio of liquor alumini chloridi is 1:（0.5~2）.
The particle diameter of the hercynite-corundum composite fine powders is less than 0.074mm, and the hercynite-corundum is compound
The Fe of fine powder2O3Content is 39 ~ 45wt%, Al2O3Content is 54 ~ 59wt%, and content of MgO is 1.0 ~ 2.5wt%.
The particle diameter of the magnesia powder is less than 0.074mm, and the content of MgO of the magnesia powder is more than 96wt%.
The solid content of the Alumina gel is 20 ~ 30wt%, the Al of the Alumina gel2O3Content is 10 ~ 15wt%.
AlCl in the liquor alumini chloridi3Content is 11 ~ 15wt%.
The particle diameter of the magnesite fine powder is less than 0.088mm, and the content of MgO of the magnesite fine powder is 44 ~ 50wt%.
The particle diameter of the aluminium hydroxide micro powder is less than 0.006mm, the Al of the aluminium hydroxide micro powder2O3Content be 60 ~
66wt%。
Due to having following good effect compared with prior art using above-mentioned technical proposal, the present invention：
（1）The preparation method of the porous periclase-magnesia-alumina spinel ceramic material for the nano aperture that the present invention uses is：First with
Magnesite fine powder decomposes under the conditions of 650 ~ 750 DEG C produces nanoporous, using its at 820 ~ 1200 DEG C diffusion into the surface and
The transmission course of material of evaporation-cohesion makes to produce neck link between magnesia crystallite, limits the particle re-arrangement of intermediate and final stages of sintering,
The magnesium oxide powder of high porosity is obtained；Introduced again into the magnesium oxide powder of high porosity and contain Al3+Solution, in vacuum bar
Allow solid phase in solution to be enriched in particle neck under part, pass through the magnalium point that reaction in-situ generation expands with certain volume under high temperature
Spar, hinder nano-pore coalescence；Aluminium hydroxide micro powder is added in the magnesium oxide powder of most backward high porosity to fill height
Space between the magnesium oxide powder particle of porosity, it on the one hand can make the stomata nanosizing between magnesium oxide particle, on the other hand
Spinelle neck is formed with magnesia reaction in-situ to be connected, to prevent rearrangement of the magnesium oxide particle in high-temperature sintering process；Institute
The aperture of porous periclase-magnesia-alumina spinel ceramic material of the nano aperture of preparation is nanoscale, has that air permeability is low, volume
The advantages of density is small, thermal conductivity factor is low and intensity is high, so that obtained lightweight Periclase-hercynite refractory material
Thermal conductivity factor is low and corrosion resistance is good.
（2）The present invention is in terms of the preparation of lightweight Periclase-hercynite refractory material, by part Alumina gel and chlorine
Change the Al in aluminum solutions3+Ion is filled in porous periclase-magnesium-aluminum spinel ceramic particle table of the nano aperture as aggregate
In face, aggregate surface is partly attached to, contains Al under high temperature3+Solution is formed in situ MgAl with the MgO in aggregate and matrix2O4,
Aggregate surface part holes can be blocked, reduce the connectivity of stomata, the consolidation that and can strengthens between aggregate/matrix is closed；Together
When the hercynite-corundum composite fine powders that are introduced in matrix can be with magnesia powder and porous periclase-magnesium of nano aperture
Aluminium spinel ceramics fine powder reaction in-situ, magnesium-aluminum-iron composite spinelle is formed, the consolidation enhanced between matrix is closed, and is effectively improved
The elevated temperature strength and thermal shock resistance of lightweight Periclase-hercynite refractory material.
Lightweight Periclase-hercynite refractory material prepared by the present invention is after testing：Apparent porosity is 22 ~ 38%；
Bulk density is 2.10 ~ 2.82g/cm3；Average pore size is 300 ~ 2000nm；Compressive resistance is 70 ~ 110MPa.
Therefore, preparation technology of the present invention is simple, the lightweight Periclase-hercynite refractory material prepared with this method
The stomata of product is nanoscale, with thermal conductivity factor is low, corrosion resistance is good, hang kliner coating excellent performance and thermal shock resistance can be high
The features such as.
Embodiment
With reference to embodiment, the invention will be further described, not to the limitation of its protection domain.
It is first that the aggregate in present embodiment, matrix and bonding agent Unify legislation is as follows to avoid repeating, embodiment
In repeat no more：
The porous periclase of the nano aperture-magnesia-alumina spinel ceramic material respectively obtains through broken and screening：
Particle diameter is porous periclase-magnesia-alumina spinel ceramic material particle of 3 ~ 5mm nano aperture；
Particle diameter is porous periclase-magnesia-alumina spinel ceramic material particle of 1 ~ 2.8mm nano aperture；
Particle diameter is porous periclase-magnesia-alumina spinel ceramic material particle of 0.1 ~ 0.8mm nano aperture；
Porous periclase-magnesia-alumina spinel ceramic material fine powder of nano aperture of the particle diameter less than 0.074mm.
Porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is after testing：Apparent porosity is 22 ~ 38%；Body
Product density is 2.12 ~ 2.78g/cm3；Average pore size is 300 ~ 900nm；Thing phase composition is periclase and magnesium aluminate spinel.
The particle diameter of the hercynite-corundum composite fine powders is less than 0.074mm, and the hercynite-corundum is compound
The Fe of fine powder2O3Content is 39 ~ 45wt%, Al2O3Content is 54 ~ 59wt%, and content of MgO is 1.0 ~ 2.5wt%.
The particle diameter of the magnesia powder is less than 0.074mm, and the content of MgO of the magnesia powder is more than 96wt%.
The solid content of the Alumina gel is 20 ~ 30wt%, the Al of the Alumina gel2O3Content is 10 ~ 15wt%.
AlCl in the liquor alumini chloridi3Content is 11 ~ 15wt%.
The particle diameter of the magnesite fine powder is less than 0.088mm, and the content of MgO of the magnesite fine powder is 44 ~ 50wt%.
The particle diameter of the aluminium hydroxide micro powder is less than 0.006mm, the Al of the aluminium hydroxide micro powder2O3Content be 60 ~
66wt%。
Embodiment 1
A kind of lightweight Periclase-hercynite refractory material and preparation method thereof.The preparation method is：
The composition and its content of the lightweight Periclase-hercynite refractory material be：Using 15 ~ 20wt% particle diameter as 3 ~
Porous periclase-magnesia-alumina spinel ceramic material particle of 5mm nano aperture, 30 ~ 37wt% particle diameter are receiving for 1 ~ 2.8mm
Porous periclase-magnesia-alumina spinel ceramic material the particle in metre hole footpath and the nano-pore that 10 ~ 12wt% particle diameter is 0.1 ~ 0.8mm
Porous periclase-magnesia-alumina spinel ceramic material the particle in footpath is aggregate, and 0.074mm nanometer is less than with 8 ~ 10wt% particle diameter
Porous periclase-magnesia-alumina spinel ceramic material the fine powder in aperture, 13 ~ 15wt% hercynite-corundum composite fine powders and 15
~ 20wt% magnesia powder is matrix；With 2 ~ 5wt% of the aggregate and matrix sum Al3+Solution is bonding agent.
By mentioned component and its content：First the aggregate is placed in de-airing mixer, is evacuated to below 2.0kPa, then
Contain Al described in pouring into3+Solution, stir 10 ~ 15 minutes, close pumped vacuum systems；The matrix is subsequently poured into, is stirred,
Mechanical pressing under the conditions of 100 ~ 140MPa, dry 12 ~ 24 hours under the conditions of 110 ~ 220 DEG C, protected under the conditions of 1500 ~ 1560 DEG C
Temperature 3 ~ 5 hours, cooling, produces lightweight Periclase-hercynite refractory material.
The preparation process of porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is：
The first step, magnesite fine powder is first warming up to 650 ~ 700 DEG C with 1 ~ 1.5 DEG C/min speed, is incubated 3 ~ 4 hours；Again with
1.5 ~ 2 DEG C/min speed is warming up to 820 ~ 900 DEG C, is incubated 2 ~ 3 hours, is finally warming up to 2.7 ~ 3 DEG C/min speed
1000 ~ 1050 DEG C, 3 ~ 4 hours are incubated, cooling, obtains the magnesium oxide powder of high porosity；
Second step, by the high porosity magnesium oxide powder for 63 ~ 79wt%, containing Al3+Solution is 10 ~ 22wt% and hydroxide
Aluminium micro mist is 10 ~ 24wt%, and first the magnesium oxide powder of the high porosity is placed in de-airing mixer, is evacuated to 2.0kPa
Hereinafter, then by described in Al is contained3+Solution and the aluminium hydroxide micro powder are poured into de-airing mixer, are stirred 20 ~ 40 minutes, closing is taken out
Vacuum system, obtain compound；
3rd step, the compound is warming up to 100 ~ 200 DEG C, is incubated 5 ~ 6h, cooling, machine is pressed under the conditions of 50 ~ 110MPa
Type, the base substrate after shaping are dried 10 ~ 15 hours under the conditions of 100 ~ 150 DEG C；Then it is warming up to 1.3 ~ 1.7 DEG C/min speed
1200 ~ 1300 DEG C, 3 ~ 5 hours are incubated, then 1400 ~ 1450 DEG C are warming up to 5 ~ 5.5 DEG C/min speed, is incubated 4 ~ 6 hours, it is cold
But, porous periclase-magnesia-alumina spinel ceramic material of nano aperture is produced.
It is described to contain Al3+Solution is Alumina gel.
Porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is after testing：Apparent porosity is 32 ~ 38%；Body
Product density is 2.12 ~ 2.26g/cm3；Average pore size is 500 ~ 900nm；Thing phase composition is periclase and magnesium aluminate spinel.
Lightweight Periclase-hercynite refractory material prepared by the present embodiment is after testing：Apparent porosity be 34 ~
38%；Bulk density is 2.10 ~ 2.32g/cm3；Average pore size is 500 ~ 2000nm；Compressive resistance is 70 ~ 90MPa.
Embodiment 2
A kind of lightweight Periclase-hercynite refractory material and preparation method thereof.The preparation method is：
The composition and its content of the lightweight Periclase-hercynite refractory material be：14 ~ 19wt% particle diameter is 3 ~ 5mm
Porous periclase-magnesia-alumina spinel ceramic material particle of nano aperture, 33 ~ 38wt% particle diameter be 1 ~ 2.8mm nano-pore
Porous periclase-magnesia-alumina spinel ceramic material the particle in footpath and 11 ~ 13wt% particle diameter are 0.1 ~ 0.8mm nano aperture
Porous periclase-magnesia-alumina spinel ceramic material particle is aggregate, and 0.074mm nano aperture is less than with 8 ~ 10wt% particle diameter
Porous periclase-magnesia-alumina spinel ceramic material fine powder, 10 ~ 12wt% hercynite-corundum composite fine powders and 12 ~
16wt% magnesia powder is matrix；With 3 ~ 6wt% of the aggregate and matrix sum Al3+Solution is bonding agent.
By mentioned component and its content：First the aggregate is placed in de-airing mixer, is evacuated to below 2.0kPa, then
Contain Al described in pouring into3+Solution, stir 10 ~ 15 minutes, close pumped vacuum systems；The matrix is subsequently poured into, is stirred,
Mechanical pressing under the conditions of 120 ~ 150MPa, dry 20 ~ 30 hours under the conditions of 110 ~ 220 DEG C, protected under the conditions of 1520 ~ 1580 DEG C
Temperature 4 ~ 7 hours, cooling, produces lightweight Periclase-hercynite refractory material.
The preparation process of porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is：
The first step, magnesite fine powder is first warming up to 650 ~ 700 DEG C with 1 ~ 1.5 DEG C/min speed, is incubated 4 ~ 5 hours；Again with
1.5 ~ 2 DEG C/min speed is warming up to 820 ~ 900 DEG C, is incubated 3 ~ 4 hours, is finally warming up to 2.5 ~ 2.7 DEG C/min speed
1050 ~ 1100 DEG C, 4 ~ 5 hours are incubated, cooling, obtains the magnesium oxide powder of high porosity；
Second step, by the high porosity magnesium oxide powder for 67 ~ 83wt%, containing Al3+Solution is 7 ~ 19wt% and aluminium hydroxide
Micro mist is 7 ~ 21wt%, and first the magnesium oxide powder of the high porosity is placed in de-airing mixer, be evacuated to 2.0kPa with
Under, then contain Al by described in3+Solution and the aluminium hydroxide micro powder are poured into de-airing mixer, are stirred 20 ~ 40 minutes, and closing is taken out true
Empty set is united, and obtains compound；
3rd step, the compound is warming up to 100 ~ 200 DEG C, is incubated 6 ~ 7h, cooling, machine is pressed under the conditions of 60 ~ 120MPa
Type, the base substrate after shaping are dried 15 ~ 20 hours under the conditions of 100 ~ 150 DEG C；Then it is warming up to 1.1 ~ 1.4 DEG C/min speed
1150 ~ 1250 DEG C, 3 ~ 5 hours are incubated, then 1450 ~ 1500 DEG C are warming up to 4.5 ~ 5 DEG C/min speed, is incubated 6 ~ 8 hours, it is cold
But, porous periclase-magnesia-alumina spinel ceramic material of nano aperture is produced.
It is described to contain Al3+Solution is aluminium chloride.
Porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is after testing：Apparent porosity is 30 ~ 35%；Body
Product density is 2.16 ~ 2.32g/cm3；Average pore size is 500 ~ 800nm；Thing phase composition is periclase and magnesium aluminate spinel.
Lightweight Periclase-hercynite refractory material prepared by the present embodiment is after testing：Apparent porosity be 30 ~
36%；Bulk density is 2.20 ~ 2.38g/cm3；Average pore size is 500 ~ 1800nm；Compressive resistance is 75 ~ 90MPa.
Embodiment 3
A kind of lightweight Periclase-hercynite refractory material and preparation method thereof.The preparation method is：
The composition and its content of the lightweight Periclase-hercynite refractory material be：10 ~ 14wt% particle diameter is 3 ~ 5mm
Porous periclase-magnesia-alumina spinel ceramic material particle of nano aperture, 35 ~ 40wt% particle diameter be 1 ~ 2.8mm nano-pore
Porous periclase-magnesia-alumina spinel ceramic material the particle in footpath and 12 ~ 14wt% particle diameter are 0.1 ~ 0.8mm nano aperture
Porous periclase-magnesia-alumina spinel ceramic material particle is aggregate, and 0.074mm nano aperture is less than with 10 ~ 12wt% particle diameter
Porous periclase-magnesia-alumina spinel ceramic material fine powder, 10 ~ 13wt% hercynite-corundum composite fine powders and 10 ~
15wt% magnesia powder is matrix；With 4 ~ 7wt% of the aggregate and matrix sum Al3+Solution is bonding agent.
By mentioned component and its content：First the aggregate is placed in de-airing mixer, is evacuated to below 2.0kPa, then
Contain Al described in pouring into3+Solution, stir 10 ~ 15 minutes, close pumped vacuum systems；The matrix is subsequently poured into, is stirred,
Mechanical pressing under the conditions of 130 ~ 170MPa, dry 20 ~ 30 hours under the conditions of 110 ~ 220 DEG C, protected under the conditions of 1550 ~ 1600 DEG C
Temperature 5 ~ 8 hours, cooling, produces lightweight Periclase-hercynite refractory material.
The preparation process of porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is：
The first step, magnesite fine powder is first warming up to 700 ~ 750 DEG C with 1 ~ 1.5 DEG C/min speed, is incubated 4 ~ 5 hours；Again with
1.5 ~ 2 DEG C/min speed is warming up to 820 ~ 900 DEG C, is incubated 3 ~ 4 hours, is finally warming up to 2.3 ~ 2.5 DEG C/min speed
1100 ~ 1150 DEG C, 5 ~ 6 hours are incubated, cooling, obtains the magnesium oxide powder of high porosity；
Second step, by the high porosity magnesium oxide powder for 71 ~ 87wt%, containing Al3+Solution is 4 ~ 16wt% and aluminium hydroxide
Micro mist is 4 ~ 18wt%, and first the magnesium oxide powder of the high porosity is placed in de-airing mixer, be evacuated to 2.0kPa with
Under, then contain Al by described in3+Solution and the aluminium hydroxide micro powder are poured into de-airing mixer, are stirred 20 ~ 40 minutes, and closing is taken out true
Empty set is united, and obtains compound；
3rd step, the compound is warming up to 100 ~ 200 DEG C, is incubated 7 ~ 8h, cooling, machine is pressed under the conditions of 70 ~ 130MPa
Type, the base substrate after shaping are dried 20 ~ 25 hours under the conditions of 100 ~ 150 DEG C；Then it is warming up to 0.9 ~ 1.2 DEG C/min speed
1100 ~ 1200 DEG C, 3 ~ 5 hours are incubated, then 1500 ~ 1550 DEG C are warming up to 4 ~ 4.5 DEG C/min speed, is incubated 8 ~ 10 hours,
Cooling, produce porous periclase-magnesia-alumina spinel ceramic material of nano aperture.
It is described to contain Al3+Solution is the mixture of Alumina gel and liquor alumini chloridi；Alumina gel in the mixture: aluminium chloride
The mass ratio of solution is 1:（0.5~2）.
Porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is after testing：Apparent porosity is 26 ~ 32%；Body
Product density is 2.28 ~ 2.56g/cm3；Average pore size is 300 ~ 600nm；Thing phase composition is periclase and magnesium aluminate spinel.
Lightweight Periclase-hercynite refractory material prepared by the present embodiment is after testing：Apparent porosity be 27 ~
34%；Bulk density is 2.32 ~ 2.66g/cm3；Average pore size is 300 ~ 1500nm；Compressive resistance is 80 ~ 100MPa.
Embodiment 4
A kind of lightweight Periclase-hercynite refractory material and preparation method thereof.The preparation method is：
The composition and its content of the lightweight Periclase-hercynite refractory material be：13 ~ 18wt% particle diameter is 3 ~ 5mm
Porous periclase-magnesia-alumina spinel ceramic material particle of nano aperture, 34 ~ 39wt% particle diameter be 1 ~ 2.8mm nano-pore
Porous periclase-magnesia-alumina spinel ceramic material the particle in footpath and 13 ~ 15wt% particle diameter are 0.1 ~ 0.8mm nano aperture
Porous periclase-magnesia-alumina spinel ceramic material particle is aggregate, and 0.074mm nano aperture is less than with 12 ~ 15wt% particle diameter
Porous periclase-magnesia-alumina spinel ceramic material fine powder, 10 ~ 12wt% hercynite-corundum composite fine powders and 10 ~
14wt% magnesia powder is matrix；With 5 ~ 8wt% of the aggregate and matrix sum Al3+Solution is bonding agent.
By mentioned component and its content：First the aggregate is placed in de-airing mixer, is evacuated to below 2.0kPa, then
Contain Al described in pouring into3+Solution, stir 10 ~ 15 minutes, close pumped vacuum systems；The matrix is subsequently poured into, is stirred,
Mechanical pressing under the conditions of 170 ~ 200MPa, dry 24 ~ 36 hours under the conditions of 110 ~ 220 DEG C, protected under the conditions of 1580 ~ 1650 DEG C
Temperature 5 ~ 8 hours, cooling, produces lightweight Periclase-hercynite refractory material.
The preparation process of hole periclase-magnesia-alumina spinel ceramic material more than the nano aperture is：
The first step, magnesite fine powder is first warming up to 700 ~ 750 DEG C with 1 ~ 1.5 DEG C/min speed, is incubated 5 ~ 6 hours；Again with
1.5 ~ 2 DEG C/min speed is warming up to 820 ~ 900 DEG C, is incubated 4 ~ 5 hours, is finally warming up to 2 ~ 2.3 DEG C/min speed
1150 ~ 1200 DEG C, it is incubated 6 ~ 7 hours and cools down, obtain the magnesium oxide powder of high porosity；
Second step, by the high porosity magnesium oxide powder for 75 ~ 91wt%, containing Al3+Solution is 1 ~ 13wt% and aluminium hydroxide
Micro mist is 1 ~ 15wt%, and first the magnesium oxide powder of the high porosity is placed in de-airing mixer, be evacuated to 2.0kPa with
Under, then contain Al by described in3+Solution and the aluminium hydroxide micro powder are poured into de-airing mixer, are stirred 20 ~ 40 minutes, and closing is taken out true
Empty set is united, and obtains compound；
3rd step, the compound is warming up to 100 ~ 200 DEG C, is incubated 8 ~ 9h, cooling, machine is pressed under the conditions of 90 ~ 150MPa
Type, the base substrate after shaping are dried 25 ~ 30 hours under the conditions of 100 ~ 150 DEG C；Then it is warming up to 0.7 ~ 1 DEG C/min speed
1050 ~ 1150 DEG C, 3 ~ 5 hours are incubated, then 1550 ~ 1600 DEG C are warming up to 3.5 ~ 4 DEG C/min speed, is incubated 10 ~ 12 hours,
Cooling, produce porous periclase-magnesia-alumina spinel ceramic material of nano aperture.
It is described to contain Al3+Solution is the mixture of Alumina gel and liquor alumini chloridi；Alumina gel in the mixture: aluminium chloride
The mass ratio of solution is 1:（0.5~2）.
Porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is after testing：Apparent porosity is 22 ~ 28%；Body
Product density is 2.42 ~ 2.78g/cm3；Average pore size is 300 ~ 600nm；Thing phase composition is periclase and magnesium aluminate spinel.
Lightweight Periclase-hercynite refractory material prepared by the present embodiment is after testing：Apparent porosity be 22 ~
26%；Bulk density is 2.60 ~ 2.82g/cm3；Average pore size is 300nm ~ 1200nm；Compressive resistance is 90 ~ 110MPa.
Present embodiment has following good effect compared with prior art：
（1）The preparation method of the porous periclase-magnesia-alumina spinel ceramic material for the nano aperture that present embodiment uses
It is：Decomposed first with magnesite fine powder under the conditions of 650 ~ 750 DEG C and produce nanoporous, using it at 820 ~ 1200 DEG C table
Face is spread and the transmission course of material of evaporation-cohesion makes to produce neck link between magnesia crystallite, limits intermediate and final stages of sintering
Particle re-arrangement, the magnesium oxide powder of high porosity is obtained；Introduced again into the magnesium oxide powder of high porosity and contain Al3+It is molten
Liquid, allow solid phase in solution to be enriched in particle neck under vacuum, there is certain volume by reaction in-situ generation under high temperature
The magnesium aluminate spinel of expansion, hinder nano-pore coalescence；Aluminium hydroxide is added in the magnesium oxide powder of most backward high porosity
On the one hand micro mist can make the stomata nanometer between magnesium oxide particle to fill the space between the magnesium oxide powder particle of high porosity
Change, on the other hand forming spinelle neck with magnesia reaction in-situ is connected, to prevent magnesium oxide particle in high-temperature sintering process
In rearrangement；The aperture of porous periclase-magnesia-alumina spinel ceramic material of prepared nano aperture is nanoscale, is had saturating
The advantages of manner is low, bulk density is small, thermal conductivity factor is low and intensity is high, so that obtained lightweight periclase-iron aluminium point
Spar Refractory Thermal Conductivity is low and corrosion resistance is good.
（2）Present embodiment is in terms of the preparation of lightweight Periclase-hercynite refractory material, by part aluminium
Al in colloidal sol and liquor alumini chloridi3+Ion is filled in porous periclase-magnesium aluminate spinel pottery of the nano aperture as aggregate
In porcelain particle surface hole, aggregate surface is partly attached to, contains Al under high temperature3+Solution is formed in situ with the MgO in aggregate and matrix
MgAl2O4, aggregate surface part holes can be blocked, reduce the connectivity of stomata, it is solid between and can enhancing aggregate/matrix
With reference to；The hercynite-corundum composite fine powders introduced simultaneously in matrix can be with the porous side of magnesia powder and nano aperture
Magnesite-magnesium-aluminum spinel ceramic fine powder reaction in-situ, magnesium-aluminum-iron composite spinelle being formed, the consolidation enhanced between matrix is closed,
Effectively increase the elevated temperature strength and thermal shock resistance of lightweight Periclase-hercynite refractory material.
Lightweight Periclase-hercynite refractory material prepared by present embodiment is after testing：Apparent porosity
For 22 ~ 38%；Bulk density is 2.10 ~ 2.82g/cm3；Average pore size is 300 ~ 2000nm；Compressive resistance is 70 ~ 110MPa.
Therefore, present embodiment preparation technology is simple, the lightweight Periclase-hercynite prepared with this method
The stomata of fire resistive material product is nanoscale, with thermal conductivity factor is low, corrosion resistance is good, hang kliner coating excellent performance and thermal shock is steady
It is qualitative can it is high the features such as.
Claims (8)
- A kind of 1. preparation method of lightweight Periclase-hercynite refractory material, it is characterised in that lightweight side's magnesium The composition and its content of stone-hercynite refractory material be：Using 10 ~ 20wt% particle diameter as the porous of 3 ~ 5mm nano aperture The porous periclase for the nano aperture that periclase-magnesia-alumina spinel ceramic material particle, 30 ~ 40wt% particle diameter are 1 ~ 2.8mm- Magnesia-alumina spinel ceramic material particle and 10 ~ 15wt% particle diameter are porous periclase-magnalium of 0.1 ~ 0.8mm nano aperture Spinel ceramic material particle is aggregate, with porous periclase-magnesium of nano aperture of the 8 ~ 15wt% particle diameter less than 0.074mm The magnesia powder of aluminium spinel ceramics fine material powder, 10 ~ 15wt% hercynite-corundum composite fine powders and 10 ~ 20wt% is Matrix, with 2 ~ 8wt% of the aggregate and matrix sum Al3+Solution is bonding agent；By mentioned component and its content：First the aggregate is placed in de-airing mixer, is evacuated to below 2.0kPa, then pour into It is described to contain Al3+Solution, stir 10 ~ 15 minutes, close pumped vacuum systems；The matrix is subsequently poured into, is stirred, 100 ~ Mechanical pressing under the conditions of 200MPa, under the conditions of 110 ~ 220 DEG C dry 12 ~ 36 hours, under the conditions of 1500 ~ 1650 DEG C be incubated 3 ~ 8 hours, cooling, produce lightweight Periclase-hercynite refractory material；The preparation process of porous periclase-magnesia-alumina spinel ceramic material of the nano aperture is：The first step, magnesite fine powder is first warming up to 650 ~ 750 DEG C with 1 ~ 1.5 DEG C/min speed, is incubated 3 ~ 6 hours；Again with 1.5 ~ 2 DEG C/min speed is warming up to 820 ~ 900 DEG C, is incubated 2 ~ 5 hours, finally 1000 are warming up to 2 ~ 3 DEG C/min speed ~ 1200 DEG C, 3 ~ 7 hours are incubated, cooling, obtains the magnesium oxide powder of high porosity；Second step, by the high porosity magnesium oxide powder for 63 ~ 91wt%, containing Al3+Solution is 1 ~ 22wt% and aluminium hydroxide Micro mist is 1 ~ 24wt%, and first the magnesium oxide powder of the high porosity is placed in de-airing mixer, be evacuated to 2.0kPa with Under, then contain Al by described in3+Solution and the aluminium hydroxide micro powder are poured into de-airing mixer, are stirred 20 ~ 40 minutes, and closing is taken out true Empty set is united, and obtains compound；3rd step, the compound is warming up to 100 ~ 200 DEG C, is incubated 5 ~ 9h, cooling, machine is pressed under the conditions of 50 ~ 150MPa Type, the base substrate after shaping are dried 10 ~ 30 hours under the conditions of 100 ~ 150 DEG C；Then it is warming up to 0.7 ~ 1.7 DEG C/min speed 1050 ~ 1300 DEG C, 3 ~ 5 hours are incubated, then 1400 ~ 1600 DEG C are warming up to 3.5 ~ 5.5 DEG C/min speed, insulation 4 ~ 12 is small When, cool down, produce porous periclase-magnesia-alumina spinel ceramic material of nano aperture；It is described to contain Al3+Solution is Alumina gel or is liquor alumini chloridi or is the mixture of Alumina gel and liquor alumini chloridi；It is described Alumina gel in mixture: the mass ratio of liquor alumini chloridi is 1:（0.5~2）.
- 2. the preparation method of lightweight Periclase-hercynite refractory material according to claim 1, it is characterised in that The particle diameter of the hercynite-corundum composite fine powders is less than 0.074mm, the hercynite-corundum composite fine powders Fe2O3Content is 39 ~ 45wt%, Al2O3Content is 54 ~ 59wt%, and content of MgO is 1.0 ~ 2.5wt%.
- 3. the preparation method of lightweight Periclase-hercynite refractory material according to claim 1, it is characterised in that The particle diameter of the magnesia powder is less than 0.074mm, and the content of MgO of the magnesia powder is more than 96wt%.
- 4. the preparation method of lightweight Periclase-hercynite refractory material according to claim 1, it is characterised in that The solid content of the Alumina gel is 20 ~ 30wt%, the Al of the Alumina gel2O3Content is 10 ~ 15wt%.
- 5. the preparation method of lightweight Periclase-hercynite refractory material according to claim 1, it is characterised in that AlCl in the liquor alumini chloridi3Content is 11 ~ 15wt%.
- 6. the preparation method of lightweight Periclase-hercynite refractory material according to claim 1, it is characterised in that The particle diameter of the magnesite fine powder is less than 0.088mm, and the content of MgO of the magnesite fine powder is 44 ~ 50wt%.
- 7. the preparation method of lightweight Periclase-hercynite refractory material according to claim 1, it is characterised in that The particle diameter of the aluminium hydroxide micro powder is less than 0.006mm, the Al of the aluminium hydroxide micro powder2O3Content is 60 ~ 66wt%.
- 8. a kind of lightweight Periclase-hercynite refractory material, it is characterised in that the lightweight periclase-iron aluminium point is brilliant Stone refractory material is the lightweight Periclase-hercynite refractory material according to any one of claim 1 ~ 7 Lightweight Periclase-hercynite refractory material prepared by preparation method.
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| CN107337437B (en) | 2019-11-22 |
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