CN109206144A - A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material - Google Patents
A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material Download PDFInfo
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- CN109206144A CN109206144A CN201811279167.0A CN201811279167A CN109206144A CN 109206144 A CN109206144 A CN 109206144A CN 201811279167 A CN201811279167 A CN 201811279167A CN 109206144 A CN109206144 A CN 109206144A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/22—Investigating strength properties of solid materials by application of mechanical stress by applying steady torsional forces
Abstract
A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material, belong to Ferrous Metallurgy technical field of fire-resistant material preparation.The present invention is by SiO2It after base natural minerals or waste residue and carbon source mix well, is placed in high temperature furnace, SiC base synthesis material is prepared under inertia or reducing atmosphere；Then according to certain proportion, SiC base synthesis material is added in Ultra-low carbon aluminum-carbon refractory material raw material and is sufficiently mixed, after molding, drying, high-temperature heat treatment, obtain the Ultra-low carbon aluminum-carbon refractory material that silicon carbide-based synthesis material improves；Finally, carrying out thermal shock resistance and resistance to slag experiment using thermal shock test furnace and Static crucible method.This method improves its thermal shock resistance and resistance to slag under the premise of reducing aluminum-carbon refractory material carbon content, has reached Ferrous Metallurgy technique to the quality requirement of related refractory component.Simple process is easy, and raw material is cheap and easy to get, it is easy to accomplish produces in enormous quantities, with good economic efficiency and environmental benefit.
Description
Technical field
The invention belongs to Ferrous Metallurgy technical field of fire-resistant material preparation, it is related to a kind of Ultra-low carbon aluminum-carbon refractory material
Preparation and detection method.
Background technique
Aluminium carbon (Al2O3- C) refractory material have good chemical stability, corrosion resistance and thermal shock resistance and high temperature it is strong
Degree, is widely used in blast furnace, continuous casting production (slide plate, long nozzle, submersed nozzle, integral column of sagger) and molten steel pretreatmenting container
Lining etc..However, aluminum-carbon refractory material carbon content (mass fraction) will appear heat transfer generally 10% or so in casting process
Fastly, the serious problems such as thermal loss, release greenhouse gases, therefore R and D Ultra-low carbon aluminum-carbon refractory material is in ecological environment
It is particularly important with Ultra-low carbon steel producer face.
In order to reduce pollution of the carbon to molten steel, steel product quality is improved, the alumina-carbon material of low carbon content is selected to seem especially heavy
It wants.And Ultra-low carbon/low-carbon alumina-carbon material leads to the thermal shock resistance and slag corrosion resistance of fire resistive material product because of the reduction of content of graphite
Property is remarkably decreased.Therefore, while reducing carbon content in aluminum-carbon refractory material, how to improve the thermal shock resistance of refractory material and resist
Scouring becomes one of the research hotspot of carbon containing refractory.
SiC has good high temperature resistance and thermal shock resistance, and its oxidation product SiO2Also have good high temperatures
Energy.Meanwhile SiO at present2Base natural minerals or waste residue are very abundant, and it is multiple thus can to prepare a series of SiC bases through carbothermic method
Micro mist is closed, compared with industrial SiC powder, cost is significantly reduced, and granularity is tiny.It is introduced SiC base synthesis material as additive
To the thermal shock resistance and resistance to slag corrosion that refractory material into Ultra-low carbon alumina-carbon material, can be effectively improved.
Summary of the invention
Under the premise of reducing aluminum-carbon refractory material carbon content, improve the thermal shock resistance and resistance to slag corrosion of refractory material,
The invention proposes the preparations and detection method of a kind of Ultra-low carbon aluminum-carbon refractory material.
The present invention is first by SiO2It after base natural minerals or waste residue, carbon source mix well, is placed in high temperature furnace, in inertia or also
SiC base synthesis material is prepared under originality atmosphere；Then according to certain proportion, SiC base synthesis material and electro-corundum fine powder is abundant
It mixes, obtains thermal shock resistance and resistance to slag after molding, drying, high-temperature heat treatment according to the production method of aluminium carbon refractory product
The Ultra-low carbon aluminum-carbon refractory material that good SiC base synthesis material improves.
A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material, comprising the following steps:
Step 1: the synthesis of SiC base composite micro-powder:
(1) by SiO2Base natural minerals or waste residue, carbon source mix well；
(2) raw material after mixing is put into high temperature furnace and sufficiently carries out carbothermic reduction reaction, under inertia or reducing atmosphere
SiC base synthesis material is prepared；
(3) obtained SiC base synthesis material is kept the temperature into 2h under 700 DEG C of air conditions, removes extra carbon；
Step 2: the preparation for the Ultra-low carbon aluminum-carbon refractory material sample that SiC base synthesis material improves and thermal shock resistance are tested:
(1) by electro-corundum, natural graphite, SiC base synthesis material, phenolic resin according to (85%~95%): (1%~
2%): (2%~10%): 1% quality proportioning weighing, and be uniformly mixed；
(2) raw material after mixing is pressed into biscuit；
(3) 2 are heat-treated after biscuit is sufficiently dry at 120 DEG C, under 1300~1600 DEG C of inertia or reducing atmosphere~
8h；
(4) the Ultra-low carbon aluminum-carbon refractory material after heat treatment and improvement is placed in 1200 DEG C of high temperature furnace and heats 30min
Air-cooled 30min afterwards, back and forth until rupture, records thermal shock cycle-index；
(5) measurement is heat-treated and after the flexural strength before the Ultra-low carbon aluminum-carbon refractory material thermal shock after improvement and thermal shock 1 time
Remaining flexural strength, the latter and the former ratio is known as strength retention, and strength retention is bigger to indicate the anti-of refractory material
Thermal shock resistance is better；
Step 3: the preparation for the Ultra-low carbon aluminium carbon crucible that SiC base synthesis material improves and resistance to slag corrosion are tested:
(1) by electro-corundum, natural graphite, SiC base synthesis material, phenolic resin according to (85%~95%): (1%~
2%): (2%~10%): 1% quality proportioning weighing, and be uniformly mixed；
(2) raw material after mixing is pressed into crucible；
(3) crucible is heat-treated 2~8h after 120 DEG C sufficiently drying under 1300~1600 DEG C of inertia or reducing atmosphere；
(4) 1kg clinker is placed in the Ultra-low carbon aluminium carbon crucible of SiC base synthesis material improvement；
(5) crucible is placed in 2~8h of heat treatment in the high temperature furnace under 1500~1600 DEG C of inert atmospheres；
(6) crucible sets room temperature with furnace natural cooling, and crucible is diametrically longitudinally slit, observes clinker and crucible internal walls
Response situation, the microstructure and clinker for analyzing clinker permeable formation form.
In currently preferred technical solution: in step 1 (1), the SiO2Base natural minerals or waste residue are red column
One of stone, sillimanite, pyrophyllite, clay, kyanite, zircon, flyash, gangue, iron ore tailings.
In currently preferred technical solution: in step 1 (1), the carbon source be active carbon, carbon black, graphite powder and
One of anthracite.
In currently preferred technical solution: the high temperature furnace is the chamber type electric resistance furnace that can lead to protective gas, tubular type electricity
Hinder one of furnace and tunnel oven.
In currently preferred technical solution: in step 1 (2), the carbothermic reduction reaction process needs to be passed through
Ar、N2Gas is protected, flow is 1.0~3.0Lmin-1。
In currently preferred technical solution: in step 1 (2), carbothermic reduction reaction synthesis temperature in the high temperature furnace
Degree is 1550~1750, and DEG C soaking time is 4~10h.
In currently preferred technical solution: in step 2 (1), additive SiC base synthesis material is SiC-Al2O3、SiC-
ZrO2, one of SiC-ZrC, mass fraction is 2%~10%.
In currently preferred technical solution: the mass fraction of the natural graphite is 1%~2%, electro-corundum
Mass fraction is 85%~95%, and (additional) mass fraction of phenolic resin is 1%.
In currently preferred technical solution: in step 2 (2) and step 3 (2), the briquetting pressure be 150~
250MPa。
In currently preferred technical solution: in the step three (4), the mass fraction of the clinker is respectively as follows:
40%CaO, 40%SiO2, 10%Na2O, 4%MgO, 2%Fe2O3And 4%Al2O3。
In currently preferred technical solution: in the step three (6), the microstructure of slag penetration layer passes through metallographic
Microscopic analysis；The composition of clinker composition and SiC base synthesis material in the slag penetration layer passes through X-ray diffraction analysis；
The preparation and detection method of a kind of Ultra-low carbon aluminum-carbon refractory material of the invention, reduce the carbon of aluminum-carbon refractory material
Content improves the thermal shock resistance and resistance to slag corrosion of refractory material, has reached Ferrous Metallurgy technique to related refractory material portion
The quality requirement of part.With SiO2Base natural minerals or waste residue (andalusite, sillimanite, pyrophyllite, clay, kyanite, zircon,
Flyash, gangue, iron ore tailings) and carbon source (active carbon, carbon black, graphite powder and anthracite) be primary raw material, utilize carbon
Thermal reduction prepares SiC base synthesis material, and then produces thermal shock resistance and the good Ultra-low carbon aluminum-carbon refractory material of resistance to slag, technique
It is simple and easy to do, it is conducive to produce in enormous quantities.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
In following embodiment, a kind of preparation of Ultra-low carbon aluminum-carbon refractory material and process flow chart such as Fig. 1 of detection method
It is shown.
Embodiment 1
A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material, comprising the following steps:
Step 1: SiC-Al2O3The synthesis of composite micro-powder:
(1) pyrophyllite, carbon black are weighed according to the mass ratio of 1000:200, and is stirred and evenly mixed；
(2) raw material after mixing is put into high temperature furnace, carries out carbothermic reduction reaction under 1650 DEG C of heat preservation 4h, argon gas,
Synthesize SiC-Al2O3Composite micro-powder；
(3) by SiC-Al2O3Composite micro-powder keeps the temperature 2h under 700 DEG C of air conditions, to remove extra carbon；
Step 2: SiC-Al2O3The preparation of improved Ultra-low carbon aluminum-carbon refractory material sample and thermal shock resistance are tested:
(1) by electro-corundum, natural graphite, SiC-Al2O3Composite micro-powder according to the quality of 930:20:50 than weighing, it is additional
The liquid phenolic resin of above-mentioned raw materials 1% (mass fraction), and be uniformly mixed；
(2) raw material after mixing is pressed into bar-shaped sample under 200MPa pressure；
(3) sample is heat-treated 2h under 1400 DEG C of argon atmospheres after 120 DEG C sufficiently drying；
(4) sample after heat treatment and improvement is placed in in 1 200 DEG C of high temperature furnace air-cooled 30min after heating 30min, is come
It returns repeatedly until its rupture, records thermal shock cycle-index；
(5) the remaining flexural strength after sample thermal shock 1 time after measuring and calculate heat treatment and improving and resisting before thermal shock
The ratio of intensity is rolled over, is strength retention；
Step 3: SiC-Al2O3The preparation of improved Ultra-low carbon magnesium carbon crucible and resistance to slag are tested:
(1) by electro-corundum, natural graphite, SiC-Al2O3Composite micro-powder according to the quality of 930:20:50 than weighing, it is additional
The liquid phenolic resin of above-mentioned raw materials 1% (mass fraction), and be uniformly mixed；
(2) raw material after mixing is pressed into crucible under 200MPa pressure；
(3) crucible is heat-treated 2h under 1400 DEG C of argon atmospheres after 120 DEG C sufficiently drying；
(4) 1kg clinker is placed in SiC-Al2O3In Ultra-low carbon magnesium carbon crucible after improvement；
(5) crucible is placed under 1500 DEG C of argon atmospheres and is heat-treated 3h；
(6) crucible sets room temperature with furnace natural cooling, and crucible is diametrically longitudinally slit, observes clinker and crucible internal walls
Response situation, the microstructure and clinker for analyzing clinker permeable formation form.
Through detecting, the principal crystalline phase of gained composite micro-powder is β-SiC, α-Al2O3, micro powder granule size is about 1 μm.By its
It is added in Ultra-low carbon aluminum-carbon refractory material, it is found that the thermal shock resistance of made refractory product and resistance to slag are preferable.Its thermal shock circulation
Number is 14 times, strength retention 38.8%, corrodes layer with a thickness of 0.5mm.Clinker and crucible internal walls surface smoother, cover
There is one layer of very thin slag blanket；Contain β-SiC and α-Al in clinker2O3Particle increases the apparent viscosity of clinker, has delayed clinker
Erosion to Ultra-low carbon aluminum-carbon refractory material.
Embodiment 2
A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material, with embodiment 1, the difference is that:
(1) pyrophyllite used in step 1 (1) and carbon black are changed to flyash and active carbon, and its quality proportioning is 1000:
500；
(2) SiC-Al is prepared in step 1 (2)2O3The temperature of composite micro-powder is 1600 DEG C；
Through detecting, the principal crystalline phase of gained composite micro-powder is β-SiC, α-Al2O3, also contain a small amount of FeSi；Micro powder granule
Size is about 1 μm.It is added in Ultra-low carbon aluminum-carbon refractory material, finds the thermal shock resistance and resistance to slag of made refractory product
Preferably.Its thermal shock cycle-index is 15 times, strength retention 40.6%, corrodes layer with a thickness of 0.8mm.
Embodiment 3
A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material, with embodiment 1, the difference is that: preparation SiC
The raw material of base synthesis material is gangue and carbon black, quality proportioning 1000:400.
Through detecting, resulting SiC-Al2O3The principal crystalline phase of composite micro-powder is β-SiC, α-Al2O3；Micro powder granule size is about
It is 1 μm.It is added in Ultra-low carbon aluminum-carbon refractory material, it is found that the thermal shock resistance of made refractory product and resistance to slag are preferable.
Its thermal shock cycle-index is 18 times, strength retention 45.6%, corrodes layer with a thickness of 0.5mm.
Embodiment 4
A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material, with embodiment 1, the difference is that:
(1) synthesis material is SiC-ZrO2Composite micro-powder；
(2) raw material for preparing SiC base synthesis material is zircon (ZrSiO4) and carbon black, quality proportioning 1000:200.
Through detecting, resulting SiC-ZrO2The principal crystalline phase of composite micro-powder is β-SiC, m-ZrO2, crystal grain mostly deposited with near-spherical
Average grain diameter is about 1 μm.It is added in Ultra-low carbon aluminum-carbon refractory material, finds the thermal shock resistance of made refractory product
It is preferable with resistance to slag.Clinker and crucible internal walls surface smoother, are covered with one layer of very thin slag blanket；Contain in slag penetration layer
CaZrO3With β-SiC；Contain β-SiC and c-ZrO in clinker2Particle increases the apparent viscosity of clinker, has delayed clinker to super
The erosion of low-carbon aluminum-carbon refractory material.Its thermal shock cycle-index be 22 times, strength retention 55.7%, corrode layer with a thickness of
0.4mm。
Embodiment 5
A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material, with embodiment 1, the difference is that:
(1) synthesis material is SiC-ZrC composite micro-powder；
(2) synthesis temperature is 1700 DEG C；
(3) raw material for preparing SiC base synthesis material is zircon and active carbon, quality proportioning 1000:550.
Through detecting, the principal crystalline phase of resulting SiC-ZrC composite micro-powder is β-SiC and ZrC, and micro powder granule size is about 1 μ
m；Clinker and crucible internal walls surface smoother, are covered with one layer of very thin slag blanket；Contain CaZrO in slag penetration layer3With β-
SiC；Contain β-SiC and c-ZrO in clinker2Particle increases the apparent viscosity of clinker, has delayed clinker to Ultra-low carbon magnesium carbon materials
The erosion of material.Its thermal shock cycle-index is 21 times, strength retention 55.1%, corrodes layer with a thickness of 0.5mm.
Claims (10)
1. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material, which comprises the following steps:
Step 1: the synthesis of SiC base composite micro-powder:
(1) by SiO2Base natural minerals or waste residue, carbon source mix well；
(2) raw material after mixing is put into high temperature furnace and sufficiently carries out carbothermic reduction reaction, prepared under inertia or reducing atmosphere
Obtain SiC base synthesis material；
(3) obtained SiC base synthesis material is kept the temperature into 2h under 700 DEG C of air conditions, removes extra carbon；
Step 2: the preparation for the Ultra-low carbon aluminum-carbon refractory material sample that SiC base synthesis material improves and thermal shock resistance are tested:
(1) by electro-corundum, natural graphite, SiC base synthesis material, phenolic resin according to (85%~95%): (1%~2%):
(2%~10%): 1% quality proportioning weighing, and be uniformly mixed；
(2) raw material after mixing is pressed into biscuit；
(3) after sufficiently drying biscuit at 120 DEG C, 2~8h is heat-treated under 1300~1600 DEG C of inertia or reducing atmosphere；
(4) the Ultra-low carbon aluminum-carbon refractory material after heat treatment and improvement is placed in 1200 DEG C of high temperature furnace empty after heating 30min
Cold 30min, back and forth until rupture, records thermal shock cycle-index；
(5) measurement heat treatment and improve after Ultra-low carbon aluminum-carbon refractory material thermal shock before flexural strength and thermal shock 1 time after it is residual
Remaining flexural strength, the latter and the former ratio are known as strength retention, the bigger anti-thermal shock for indicating refractory material of strength retention
Property is better；
Step 3: the preparation for the Ultra-low carbon aluminium carbon crucible that SiC base synthesis material improves and resistance to slag corrosion are tested:
(1) by electro-corundum, natural graphite, SiC base synthesis material, phenolic resin according to (85%~95%): (1%~2%):
(2%~10%): 1% quality proportioning weighing, and be uniformly mixed；
(2) raw material after mixing is pressed into crucible；
(3) crucible is heat-treated 2~8h after 120 DEG C sufficiently drying under 1300~1600 DEG C of inertia or reducing atmosphere；
(4) 1kg clinker is placed in the Ultra-low carbon aluminium carbon crucible of SiC base synthesis material improvement；
(5) crucible is placed in 2~8h of heat treatment in the high temperature furnace under 1500~1600 DEG C of inert atmospheres；
(6) crucible sets room temperature with furnace natural cooling, and crucible is diametrically longitudinally slit, and observation clinker is reacted with crucible internal walls
Situation, the microstructure and clinker for analyzing clinker permeable formation form.
2. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material as described in claim 1, it is characterised in that: in step
In rapid one (1), the SiO2Base natural minerals or waste residue are andalusite, sillimanite, pyrophyllite, clay, kyanite, zirconium English
One of stone, flyash, gangue, iron ore tailings.
3. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material as claimed in claim 1 or 2, it is characterised in that:
In step 1 (1), the carbon source is one of active carbon, carbon black, graphite powder and anthracite.
4. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material as described in claim 1 or 2, feature exist
In: the high temperature furnace is one of the chamber type electric resistance furnace, tube type resistance furnace and tunnel oven that can lead to protective gas.
5. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material as claimed in claim 1 or 2, it is characterised in that:
In step 1 (2), the carbothermic reduction reaction process needs to be passed through Ar, N2Gas is protected, flow is 1.0~3.0L
min-1。
6. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material as claimed in claim 1 or 2, it is characterised in that:
In step 1 (2), in the high temperature furnace carbothermic reduction reaction synthesis temperature be 1550~1750, DEG C soaking time be 4~
10h。
7. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material as claimed in claim 1 or 2, it is characterised in that:
In step 2 (1), additive SiC base synthesis material is SiC-Al2O3、SiC-ZrO2, one of SiC-ZrC, mass fraction
It is 2%~10%.
8. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material as described in claim 1, it is characterised in that: described
The mass fraction of natural graphite be 1%~2%, the mass fraction of electro-corundum is 85%~95%, the quality of phenolic resin
(additional) score is 1%.
9. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material as described in claim 1, it is characterised in that: in step
In rapid two (2) and step 3 (2), the briquetting pressure is 150~250MPa.
10. a kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material as described in claim 1, it is characterised in that: institute
In the step of stating three (4), the mass fraction of the clinker is respectively as follows: 40%CaO, 40%SiO2, 10%Na2O, 4%MgO,
2%Fe2O3And 4%Al2O3。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115160002A (en) * | 2022-07-28 | 2022-10-11 | 中钢集团洛阳耐火材料研究院有限公司 | Silicon carbide-calcium zirconate composite refractory material and preparation method thereof |
| CN115160002B (en) * | 2022-07-28 | 2023-08-29 | 中钢集团洛阳耐火材料研究院有限公司 | Silicon carbide-calcium zirconate composite refractory material and preparation method thereof |
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