CN108440004A - A method of introducing silicon carbide-based synthesis material improves Ultra-low carbon Magnesia-carbon material thermal shock resistance - Google Patents
A method of introducing silicon carbide-based synthesis material improves Ultra-low carbon Magnesia-carbon material thermal shock resistance Download PDFInfo
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- CN108440004A CN108440004A CN201810445297.0A CN201810445297A CN108440004A CN 108440004 A CN108440004 A CN 108440004A CN 201810445297 A CN201810445297 A CN 201810445297A CN 108440004 A CN108440004 A CN 108440004A
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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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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
A method of introducing silicon carbide-based synthesis material improves Ultra-low carbon Magnesia-carbon material thermal shock resistance, belongs to Ferrous Metallurgy technical field of fire-resistant material preparation.After titanium dioxide silicon-based mineral or waste residue are sufficiently stirred mixing by the present invention with carbon source, it is placed in high temperature furnace, prepares silicon carbide-based synthesis material under an inert atmosphere；Then according to certain proportioning, silicon carbide-based synthesis material is added in Ultra-low carbon magnesium material raw material and is sufficiently mixed, after molding, drying, high-temperature heat treatment, obtain the Ultra-low carbon Magnesia-carbon material that silicon carbide-based synthesis material improves；Finally, the thermal shock resistance of Ultra-low carbon Magnesia-carbon material is tested in thermal shock experimental furnace.This method improves its thermal shock resistance under the premise of reducing Magnesia-carbon material carbon content, has reached quality requirement of the steel-making to continuous casting process to 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.
Description
Technical field
The invention belongs to Ferrous Metallurgy technical field of fire-resistant material preparation, are related to a kind of high-performance Ultra-low carbon Magnesia-carbon material
Preparation method, in particular to a kind of introducing silicon carbide-based synthesis material and improve the thermal shock resistance of Ultra-low carbon Magnesia-carbon material.
Background technology
With modern steel industrial expansion, the requirement of the high added values steel product such as production ultra-low-carbon steel is increasingly harsh, passes
System Magnesia-carbon material also exposes the problems such as thermal losses is high, to molten steel recarburization, consumption a large amount of graphite resources.The low-carbon of Magnesia-carbon material
It is expected to solve these problems.But with the reduction of carbon content, the thermal shock resistance of Magnesia-carbon material is caused to decline, therefore, if to drop
Low Magnesia-carbon material carbon content, then need to be improved the thermal shock resistance of Magnesia-carbon material, to meet the needs of its practical metallurgical process.
There is abundant titanium dioxide silicon-based mineral and residue resource, typical waste residue to have flyash, iron ore tailings, coal in China
Spoil etc., accumulating amount is increasing, has resulted in problems：It stacks in the arable land for occupying large area；Pollute air, water source and ring
Border；Influence people's health etc..Therefore, silicon carbide-based synthesis material can be made into using short-cut method, had using silicon carbide
The good high-temperature stability and thermal shock resistance having, are added in Ultra-low carbon Magnesia-carbon material, significantly to improve Ultra-low carbon magnesium
The thermal shock resistance of carbon material.
Invention content
Under the premise of reducing Magnesia-carbon material carbon content, improve its thermal shock resistance, the present invention proposes a kind of introducing carbonization
Silicon substrate synthesis material improves the preparation method of Ultra-low carbon Magnesia-carbon material thermal shock resistance.
After the present invention first mixes well titanium dioxide silicon-based mineral or waste residue, carbon source, silicon carbide is prepared under an inert atmosphere
Base synthesis material；Then according to certain proportioning, silicon carbide-based synthesis material and fused magnesite fine powder are mixed well, it is resistance to according to magnesium carbon
The production method of fiery product obtains the good silicon carbide-based synthesis material of thermal shock resistance and changes after molding, drying, high-temperature heat treatment
Kind Ultra-low carbon Magnesia-carbon material.
A method of introducing silicon carbide-based synthesis material improves Ultra-low carbon Magnesia-carbon material thermal shock resistance, according to the following steps into
Row：
Step 1：The preparation of silicon carbide-based synthesis material
(1) titanium dioxide silicon-based mineral or waste residue are mixed well with carbon source；Titanium dioxide silicon-based mineral or waste residue and carbon source
Quality proportioning, the carbon amounts that should be needed according to the purity and carbothermic reduction reaction of raw material calculates, to promote carbothermic reduction reaction abundant
It carries out, is usually added into excessive carbon source.
(2) raw material after mixing is put into high temperature furnace in fully carrying out carbothermic reduction reaction, prepares carbon under an inert atmosphere
SiClx base synthesis material.
Step 2：The preparation for the Ultra-low carbon Magnesia-carbon material that silicon carbide-based synthesis material improves
(1) by fused magnesite, natural graphite, silicon carbide-based synthesis material, phenolic resin according to (92%~95%)：(1%~
2%)：(3%~7%)：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 fully dry at 120 DEG C, under 1200~1600 DEG C of inertia or reducing atmosphere~
8h。
Step 3：The test for the Ultra-low carbon Magnesia-carbon material thermal shock resistance that silicon carbide-based synthesis material after heat treatment improves
(1) the Ultra-low carbon Magnesia-carbon 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；
(2) residual after the flexural strength before Ultra-low carbon Magnesia-carbon material thermal shock and thermal shock 1 time after measuring heat treatment and improving
The ratio of remaining flexural strength, the two is known as strength retention, and strength retention is bigger to indicate that the thermal shock resistance of material is better.
In the step 1 (1), the titanium dioxide silicon-based mineral and waste residue are zircon sand, pyrophyllite, clay, red column
One kind in stone, sillimanite, kyanite, flyash, iron ore tailings, gangue；
In the step 1 (1), the carbon source is one kind in graphite powder, activated carbon and carbon black；
The high temperature furnace is the one kind that can lead in the chamber type electric resistance furnace, tube type resistance furnace and tunnel oven of protective gas；
In the step 1 (2), the carbothermic reduction reaction process needs to be passed through Ar, N2Protection gas, flow are
1.0~3.0Lmin-1；
In the step 1 (2), carbothermic reduction reaction synthesis temperature is 1500~1800 DEG C in the high temperature furnace, is protected
The warm time is 4~10h；
In the step 1 (3), the high temperature furnace is one kind in chamber type electric resistance furnace, tube type resistance furnace or tunnel oven；
In the step 2 (1), the silicon carbide-based synthesis material of additive is silicon carbide-zirconium oxide, silicon carbide-carbon zirconium, carbon
The mass fraction of one kind in SiClx-aluminium oxide, addition is 3%~7%；
In the step 2 (1), the mass fraction of the natural graphite is 1%~2%, the quality point of fused magnesite
Number is 92%~95%, and (additional) mass fraction of phenolic resin is 1%；
In the step 2 (2), the pressure of the compacting biscuit is 150~250MPa；
In the step 3 (1), anti-thermal shock experiment concrete operations are：In 1200 DEG C of high temperature stove heat 30min
Afterwards, it is placed in air hollow cold 30min, is denoted as 1 time；Then it is put back to again in stove and keeps the temperature 30min in 1 200 DEG C, it is empty after taking-up
Cold 30min, for such circulate operation until biscuit fragmentation, anti-thermal shock cycle-index is more, shows that its thermal shock resistance is better；
In 3 described (2), the remaining flexural strength after the described measurement heat treatment after Ultra-low carbon Magnesia-carbon material thermal shock 1 time
With the ratio of the flexural strength before thermal shock, as strength retention, strength retention is higher, shows that its thermal shock resistance is better.
A kind of silicon carbide-based synthesis material of introducing of the present invention improves the method for Ultra-low carbon Magnesia-carbon material thermal shock resistance, reduces
The carbon content of Magnesia-carbon material improves its thermal shock resistance, has reached matter of the steel-making to continuous casting process to related refractory component
Amount requires.With titanium dioxide silicon-based mineral or waste residue (pyrophyllite, clay, andalusite, sillimanite, kyanite, zircon sand, flyash,
Iron ore tailings, gangue) and carbon source (activated carbon, carbon black and graphite powder) be primary raw material, prepare carbon using carbothermic method
SiClx base synthesis material, and then the good Ultra-low carbon Magnesia-carbon material of thermal shock resistance is produced, simple process is easy, and it is raw to be conducive to high-volume
Production.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail.
It is a kind of to introduce silicon carbide-based synthesis material and improve the method for Ultra-low carbon Magnesia-carbon material thermal shock resistance in following embodiment
Process flow chart is as shown in Figure 1.
Embodiment 1
A method of introducing silicon carbide-based synthesis material improves Ultra-low carbon Magnesia-carbon material thermal shock resistance, according to the following steps into
Row：
Step 1：The preparation of silicon carbide-oxidation zirconium synthetic material
(1) carbon black of the zircon sand and 200kg of 1000kg is weighed, and is stirred for being uniformly mixed；
(2) raw material after mixing is put into high temperature furnace, carries out carbon reduction reaction in 1600 DEG C, prepares silicon carbide-oxidation
Aluminium synthesis material.
Step 2：The preparation for the Ultra-low carbon Magnesia-carbon material that silicon carbide-aluminium oxide synthesis material improves
(1) fused magnesite of 930kg, the natural graphite of 20kg, silicon carbide-oxidation zirconium synthetic material of 50kg are weighed, and is claimed
The liquid phenolic resin of 10kg is measured, and is stirred for being uniformly mixed；
(2) raw material after mixing is pressed into biscuit；
(3) after fully drying biscuit at 120 DEG C, 4h is heat-treated under 1400 DEG C of argon gas atmospheres.
Step 3：The test for the Ultra-low carbon Magnesia-carbon material thermal shock resistance that silicon carbide-aluminium oxide after heat treatment improves
(1) the Ultra-low carbon Magnesia-carbon material after heat treatment and improvement is placed in 1 200 DEG C of high temperature furnace empty after heating 30min
Cold 30min, back and forth until its rupture, records thermal shock cycle-index；
(2) remaining flexural strength after Ultra-low carbon Magnesia-carbon material thermal shock 1 time after measuring and calculate heat treatment and improving with
The ratio of flexural strength before thermal shock is strength retention.
After testing, the principal crystalline phase of gained synthesis material is β-SiC and m-ZrO2, crystal grain mostly exists with near-spherical；Added
It is added in Ultra-low carbon Magnesia-carbon material, the Ultra-low carbon Magnesia-carbon material that silicon carbide-zirconium oxide improves is made, thermal shock cycle-index is 14
It is secondary, strength retention 38.2%.
Embodiment 2
A method of introducing silicon carbide-based synthesis material improves Ultra-low carbon Magnesia-carbon material thermal shock resistance, different with embodiment 1
Place is：
(1) synthesis material is silicon carbide-carbon zirconium micro mist；
(2) synthesis temperature is 1700 DEG C；
(3) addition of raw material zircon sand and carbon black is respectively 1000kg and 550kg.
After testing, the principal crystalline phase of gained silicon carbide-carbon zirconium synthetic material is β-SiC and ZrC, and micro powder granule size is about
1μm；It is added in Ultra-low carbon Magnesia-carbon material, the Ultra-low carbon Magnesia-carbon material of silicon carbide-carbon zirconium improvement, anti-thermal shock is made
Cycle-index is 12 times, and the conservation rate of intensity is 36.7%.
Embodiment 3
A method of introducing silicon carbide-based synthesis material improves Ultra-low carbon Magnesia-carbon material thermal shock resistance, different with embodiment 1
Place is：
(1) synthesis material is silicon carbide-alumina powder；
(2) raw material for preparing synthesis material is pyrophyllite and activated carbon.
After testing, the principal crystalline phase of the silicon carbide of gained-aluminium oxide synthesis material is β-SiC and α-Al2O3, it is added to
It is ultralow
In carbon Magnesia-carbon material, the Ultra-low carbon Magnesia-carbon material that silicon carbide-aluminium oxide improves is made, thermal shock cycle-index is 12
It is secondary,
Strength retention is 35.6%.
Embodiment 4
A method of introducing silicon carbide-based synthesis material improves Ultra-low carbon Magnesia-carbon material thermal shock resistance, different with embodiment 1
Place is：
(1) synthesis material is silicon carbide-alumina powder；
(2) raw material for preparing synthesis material is flyash and carbon black, and its quality addition is respectively 1000kg and 440kg.
After testing, the principal crystalline phase of gained silicon carbide-aluminium oxide synthesis material is β-SiC and α-Al2O3, and contain on a small quantity
FeSi；Grain uniformity is slightly worse；It is added in Ultra-low carbon Magnesia-carbon material, the Ultra-low carbon that silicon carbide-aluminium oxide improves is made
Magnesia-carbon material, it is 11 times to send out its anti-thermal shock cycle-index, strength retention 33.1%.
Claims (10)
- Introducing silicon carbide-based synthesis material 1. a kind of and improve the method for Ultra-low carbon Magnesia-carbon material thermal shock resistance, which is characterized in that by with Lower step carries out：Step 1：The preparation of silicon carbide-based synthesis material(1) titanium dioxide silicon-based mineral or waste residue, carbon source are sufficiently stirred mixing；(2) raw material after mixing, which is put into high temperature furnace, fully carries out carbothermic reduction reaction, prepares silicon carbide-based synthesis material；Step 2：The preparation for the Ultra-low carbon Magnesia-carbon material that silicon carbide-based synthesis material improves(1) by fused magnesite, natural graphite, silicon carbide-based synthesis material according to (92%~95%)：(1%~2%)：(3%~ 7%) weighing is matched, and is uniformly mixed；(2) raw material after mixing is pressed into biscuit；(3) after fully drying biscuit at 120 DEG C, 2~8h is heat-treated under 1200~1600 DEG C of inertia or reducing atmosphere.Step 3：The test for the Ultra-low carbon Magnesia-carbon material thermal shock resistance that silicon carbide-based synthesis material improves(1) the Ultra-low carbon Magnesia-carbon material after heat treatment and improvement is placed in 1200 DEG C of high temperature furnace air-cooled after heating 30min 30min, back and forth until rupture, records thermal shock cycle-index；(2) remnants of the flexural strength and thermal shock 1 before Ultra-low carbon Magnesia-carbon material thermal shock hereafter after measuring heat treatment and improving are anti- Intensity is rolled over, the ratio of the two is strength retention.
- 2. preparation method as described in claim 1, which is characterized in that in the step 1 (1), the titanium dioxide silicon substrate Mineral or waste residue are zircon sand, pyrophyllite, clay, andalusite, sillimanite, kyanite, flyash, iron ore tailings, gangue In one kind.
- 3. preparation method as claimed in claim 1 or 2, which is characterized in that in the step 1 (1), the carbon source is stone One kind in ink powder, activated carbon and carbon black.
- 4. preparation method as described in claim 1 or 2, which is characterized in that the high temperature furnace is that can lead to protective gas One kind in chamber type electric resistance furnace, tube type resistance furnace and tunnel oven.
- 5. preparation method as claimed in claim 1 or 2, which is characterized in that in the step 1 (2), the carbon thermal reduction Reaction process needs to be passed through Ar, N2It is 1.0~3.0Lmin to protect gas, flow-1。
- 6. preparation method as claimed in claim 1 or 2, which is characterized in that in the step 1 (2), in the high temperature furnace Carbothermic reduction reaction synthesis temperature is 1500~1800 DEG C, and soaking time is 4~10h.
- 7. preparation method as claimed in claim 1 or 2, which is characterized in that in the step 2 (1), additive is silicon carbide-based Synthesis material is silicon carbide-zirconium oxide, silicon carbide-carbon zirconium, one kind in silicon carbide-aluminium oxide, mass fraction is 3%~ 7%.
- 8. preparation method as described in claim 1, which is characterized in that in the step 2 (1), the natural graphite The mass fraction of mass fraction 1%~2%, fused magnesite is 92%~95%, and the mass fraction (additional) of phenolic resin is 1%.
- 9. preparation method as described in claim 1, which is characterized in that in the step 2 (2), the pressure of the compacting biscuit Power is 150~250MPa.
- 10. preparation method as described in claim 1, which is characterized in that in the step 3 (1), the Ultra-low carbon magnesium carbon Material anti-thermal shock concrete operations：After 1200 DEG C of high temperature stove heat 30min, it is placed in air hollow cold 30min, is denoted as 1 time；So It is put back to again afterwards in stove and keep the temperature 30min in 1200 DEG C, air-cooled 30min after taking-up, such circulate operation is until biscuit fragmentation；Institute In 3 (2) stated, remaining flexural strength after the described measurement heat treatment after Ultra-low carbon Magnesia-carbon material thermal shock 1 time with before thermal shock Flexural strength, ratio are strength retention.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109206144A (en) * | 2018-10-30 | 2019-01-15 | 苏州佳耐材料科技有限公司 | A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material |
| CN110256050A (en) * | 2019-07-05 | 2019-09-20 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of pyrolytic semlting magnesium carbonaceous artesian repairing material |
| CN111348899A (en) * | 2019-07-08 | 2020-06-30 | 营口石兴耐火材料科技有限公司 | Method for enhancing thermal shock resistance of low-carbon magnesia-carbon material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109206144A (en) * | 2018-10-30 | 2019-01-15 | 苏州佳耐材料科技有限公司 | A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material |
| CN110256050A (en) * | 2019-07-05 | 2019-09-20 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of pyrolytic semlting magnesium carbonaceous artesian repairing material |
| CN111348899A (en) * | 2019-07-08 | 2020-06-30 | 营口石兴耐火材料科技有限公司 | Method for enhancing thermal shock resistance of low-carbon magnesia-carbon material |
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Application publication date: 20180824 |