CN107935611A - A kind of calcium zirconium carbon refractory and preparation method thereof - Google Patents
A kind of calcium zirconium carbon refractory and preparation method thereof Download PDFInfo
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- CN107935611A CN107935611A CN201810005726.2A CN201810005726A CN107935611A CN 107935611 A CN107935611 A CN 107935611A CN 201810005726 A CN201810005726 A CN 201810005726A CN 107935611 A CN107935611 A CN 107935611A
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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
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
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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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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Abstract
The present invention relates to a kind of calcium zirconium carbon refractory and preparation method thereof.Its technical solution is：First using the calcium oxide particle of 60~80wt%, the calcium oxide fine powder of 10~20wt%, the powdered zirconium oxide of 2~10wt% and 1~15wt% graphite as raw material, then the phenolic resin of the additional 2~7wt% of raw material, stir 3~30 minutes, it is compressing；Then by the base substrate after shaping when baking 8~24 is small under the conditions of 150~300 DEG C, cooling, up to calcium zirconium carbon refractory.The baking and the cooling carry out under the conditions of vacuum is 100~1000Pa.Not only fusing point is high, thermodynamic stability is good, vacuum stability is strong, thermal shock resistance is excellent and anti-melt attack ability is excellent for calcium zirconium carbon refractory prepared by the present invention, and prepared calcium zirconium carbon refractory is suitable for metallurgy refractory material, is particularly suitable for vacuum metling refractory material.
Description
Technical field
The invention belongs to technical field of refractory materials.A kind of more particularly to calcium zirconium carbon refractory and preparation method thereof.
Background technology
Refractory composites are the important directions of refractory material development.Carbon containing refractory becomes steel
The industrial important refractory material of iron, such as magnesium carbon and aluminum-carbon refractory material, they be respectively by magnesia, corundum etc. and graphite with
Resin is made of bonding agent.Since graphite is not soaked by slag, thermal conductivity is high, since carbon composite has excellent resistance to slag
It is widely used in the liner of metallurgical furnace and container with thermal shock resistance.In the later stage in last century, refractory material service life it is big
Amplitude improves, and carbon composite refractory has played important function, and magnesium carbon and aluminum-carbon refractory material are in steel-making and refractory for continuous casting
In occupy leading position.
At present, one of main problem that carbon composite refractory faces is, under high temperature, especially under vacuum environment, oxidation
The reaction occurred between thing and graphite destroys the structure of material, greatly weakens the military service performance of material.Such as：Magnesia and
Reaction between graphite often results in the generation of magnesia steam, causes the damage of magnesia particle；Alumina-carbon material is contacted with iron liquid
When, the alumina carbon thermal reduction reaction temperature in material can be reduced to 1550 DEG C.High-temperature vacuum metallurgy is to prepare high-purity high temperature
The main method of alloy and clean steel.Currently used magnesium carbon and aluminum-carbon refractory material high-temperature vacuum smelting process damage
The main problem lifted as restriction high-temperature vacuum smelting process with capabilities of refractory materials.
The content of the invention
It is contemplated that overcome the shortage of prior art, it is therefore an objective to provide a kind of fusing point height, thermodynamic stability is good, vacuum is steady
Qualitative calcium zirconium carbon refractory strong, the excellent and anti-melt attack ability of thermal shock resistance is excellent and preparation method thereof, made system
Product are suitable for metallurgy and are particularly suitable for vacuum metling refractory material with refractory material.
To achieve the above object, the technical solution adopted in the present invention is：First with the calcium oxide particle of 60~80wt%, 10
The calcium oxide fine powder of~20wt%, the powdered zirconium oxide of 2~10wt% and 1~15wt% graphite are raw material, then the additional original
Expect the phenolic resin of 2~7wt%, stir 3~30 minutes, it is compressing；Then by the base substrate after shaping in 150~300 DEG C of bars
When baking 8~24 is small under part, cooling, up to calcium zirconium carbon refractory.
The baking and the cooling carry out under the conditions of vacuum is 100~1000Pa.
The preparation method of the calcium oxide particle is：Added into calcium hydroxide powder and account for the calcium hydroxide powder 0.2
The additive of~2.0wt%, when wet-milling blending 1~5 is small, filtered, drying and grinding, obtain mixed powder.Again by the mixing
Powder is placed in the charging basket of Granulation Equipments, and under conditions of rotating speed is 1000~3000 revs/min, addition accounts for the mixed powder
The water of 8~30wt%, when there is particle formation, is adjusted to 500~1000 revs/min by rotating speed, treats the mixed powder in the charging basket
Body, which is completely converted into particle, to be stopped.Then the particle is inserted in heating furnace, it is small that 1~5 is kept the temperature under the conditions of 1400~1800 DEG C
When；Then nitrogen or argon gas are passed through into stove to room temperature, the flow for being passed through nitrogen or argon gas is 0.5~5 liter/min, up to oxygen
Change calcium particle.
The calcium oxide particle：CaO content >=95wt%, bulk density >=2.8g/cm3, particle diameter is 0.2~7mm.
CaO content >=95wt% of the calcium oxide fine powder, the particle diameter of calcium oxide fine powder is 2~200 μm.
The ZrO of the powdered zirconium oxide2Content >=95wt%, the particle diameter of powdered zirconium oxide is 1~50 μm.
Content >=94wt% of C in the graphite, the particle diameter of graphite is 1~200 μm.
The phenolic resin is one or both of liquid phenolic resin and solid phenolic resin；The phenolic resin
Residual carbon >=40%.
The additive is one kind of zirconium hydroxide powder, Zirconium oxide powder and yttrium oxide powder；The grain of the additive
Footpath is 1~300 μm.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art.
1) the calcium oxide thermodynamic property that the present invention uses is stablized, and partial pressure is extremely low under high temperature, in existing smelting bar
It will not react under part with graphite, so as to improve stability of the material in vacuum environment.In addition, the present invention exists
Graphite is introduced in preparation process, the thermal shock resistance for improving material can be with anti-melt attack performance.
2) present invention is due to adding a certain number of powdered zirconium oxides, and during applied at elevated temperature, square calcium stone (CaO) is brilliant
Alternate formation calcium zirconate combination phase, material mutually form solid-solid directly in conjunction with improving the high-temperature mechanics property of material.By
In the calcium oxide particle for having used comminution granulation to prepare, production technology is not only simplified, improves the production efficiency of product so that calcium
Zirconium carbon refractory is reduced in preparation process by the probability of aquation.
3) calcium oxide particle used in the present invention is made to be granulated, and can directly use, due to the sintering of particle surface
Epidermis is intact, greatly improves the hydration resistance of calcium oxide particle, ensure that calcium zirconium carbon refractory produces raw materials used property
The stability of energy.
Calcium zirconium carbon refractory prepared by the present invention is after testing：Apparent porosity≤10%；Compressive resistance >=20MPa.
Therefore, not only fusing point is high, thermodynamic stability is good, vacuum stability for the calcium zirconium carbon refractory prepared by the present invention
By force, thermal shock resistance and anti-melt attack excellent ability；Made product is suitable for metallurgy and is particularly suitable for vacuum with refractory material
Smelting refractory material.
Embodiment
With reference to embodiment, the present invention will be further described, not to the limitation of its protection domain.
In present embodiment：
CaO content >=95wt% of the calcium oxide fine powder, the particle diameter of calcium oxide fine powder is 2~200 μm；
ZrO2 contents >=95wt% of the powdered zirconium oxide, the particle diameter of powdered zirconium oxide is 1~50 μm；
Content >=94wt% of C in the graphite, the particle diameter of graphite is 1~200 μm；
The Residual carbon of the liquid phenolic resin and solid phenolic resin is >=40%.
Repeated no more in embodiment：
Embodiment 1
A kind of calcium zirconium carbon refractory and preparation method thereof.First calcium oxide particle, the 10~15wt% with 60~70wt%
Calcium oxide fine powder, 5~10wt% powdered zirconium oxide and 8~15wt% graphite be raw material, then the additional raw material 2~
The liquid phenolic resin of 4wt%, is stirred 3~15 minutes, compressing.Then by the base substrate after shaping in 150~220 DEG C of temperature
It is lower baking 16~24 it is small when, cooling, up to calcium zirconium carbon refractory.The baking and cooling vacuum for 700~
Carried out under the conditions of 1000Pa.
The preparation method of the calcium oxide particle is：Added into calcium hydroxide powder and account for the calcium hydroxide powder 0.2
The additive of~2.0wt%, when wet-milling blending 1~5 is small, filtered, drying and grinding, obtain mixed powder.Again by the mixing
Powder is placed in the charging basket of Granulation Equipments, and under conditions of rotating speed is 1000~3000 revs/min, addition accounts for the mixed powder
The water of 8~30wt%, when there is particle formation, is adjusted to 500~1000 revs/min by rotating speed, treats the mixed powder in the charging basket
Body, which is completely converted into particle, to be stopped.Then the particle is inserted in heating furnace, it is small that 1~5 is kept the temperature under the conditions of 1400~1800 DEG C
When；Then nitrogen or argon gas are passed through into stove to room temperature, the flow for being passed through nitrogen or argon gas is 0.5~5 liter/min, up to oxygen
Change calcium particle.The calcium oxide particle：Particle diameter is 0.2~7mm, CaO content >=95wt%, bulk density >=2.8g/cm3.
Additive described in the present embodiment is yttrium oxide powder；The particle diameter of the additive is 1~300 μm.
Calcium zirconium carbon refractory prepared by the present embodiment is after testing：The porosity 9~10%；Compressive resistance for 20~
25MPa。
Embodiment 2
A kind of calcium zirconium carbon refractory and preparation method thereof.First calcium oxide particle, the 13~18wt% with 65~75wt%
Calcium oxide fine powder, 3~8wt% powdered zirconium oxide and 5~13wt% graphite be raw material, then the additional 5~7wt% of raw material
Solid phenolic resin, stir 15~30 minutes, it is compressing.Then the base substrate after shaping is dried at a temperature of 180~260 DEG C
It is roasting 10~18 it is small when, cooling, up to calcium zirconium carbon refractory.The baking and cooling are 400~700P a bars in vacuum
Carried out under part.
The preparation method of calcium oxide particle described in the present embodiment is；In addition to the additive is zirconium hydroxide powder, remaining
It is same as Example 1.
Calcium zirconium carbon refractory prepared by the present embodiment is after testing：The porosity 8~9%；Compressive resistance for 25~
30MPa。
Embodiment 3
A kind of calcium zirconium carbon refractory and preparation method thereof.First calcium oxide particle, the 15~20wt% with 70~80wt%
Calcium oxide fine powder, 2~5wt% powdered zirconium oxide and 1~8wt% graphite be raw material, then the additional 2~4wt% of raw material
Liquid phenolic resin and 1~3wt% solid phenolic resin, stir 15~30 minutes, it is compressing.Then by after shaping
Base substrate is when baking 8~16 is small at a temperature of 220~300 DEG C, cooling, up to calcium zirconium carbon refractory.The baking and cooling are equal
Carried out under the conditions of vacuum is 100~400Pa.
The preparation method of calcium oxide particle described in the present embodiment is；Except the additive be Zirconium oxide powder in addition to, remaining with
Embodiment 1 is identical.
Calcium zirconium carbon refractory prepared by the present embodiment is after testing：The porosity 6~8%；Compressive resistance for 30~
40MPa。
The present invention has following good effect compared with prior art.
1) the calcium oxide thermodynamic property that the present invention uses is stablized, and partial pressure is extremely low under high temperature, in existing smelting bar
It will not react under part with graphite, so as to improve stability of the material in vacuum environment.In addition, the present invention exists
Graphite is introduced in preparation process, the thermal shock resistance for improving material can be with anti-melt attack performance.
2) present invention is due to adding a certain number of powdered zirconium oxides, and during applied at elevated temperature, square calcium stone (CaO) is brilliant
Alternate formation calcium zirconate combination phase, material mutually form solid-solid directly in conjunction with improving the high-temperature mechanics property of material.By
In the calcium oxide particle for having used comminution granulation to prepare, production technology is not only simplified, improves the production efficiency of product so that calcium
Zirconium carbon refractory is reduced in preparation process by the probability of aquation.
3) calcium oxide particle used in the present invention is made to be granulated, and can directly use, due to the sintering of particle surface
Epidermis is intact, greatly improves the hydration resistance of calcium oxide particle, ensure that calcium zirconium carbon refractory produces raw materials used property
The stability of energy.
Calcium zirconium carbon refractory prepared by the present invention is after testing：Apparent porosity≤10%；Compressive resistance >=20MPa.
Therefore, not only fusing point is high, thermodynamic stability is good, vacuum stability for the calcium zirconium carbon refractory prepared by the present invention
By force, thermal shock resistance and anti-melt attack excellent ability；Made product is suitable for metallurgy and is particularly suitable for vacuum with refractory material
Smelting refractory material.
Claims (7)
- A kind of 1. preparation method of calcium zirconium carbon refractory, it is characterised in that first with the calcium oxide particle of 60~80wt%, 10~ The calcium oxide fine powder of 20wt%, the powdered zirconium oxide of 2~10wt% and 1~15wt% graphite are raw material, then the additional raw material 2 The phenolic resin of~7wt%, is stirred 3~30 minutes, compressing；Then by the base substrate after shaping under the conditions of 150~300 DEG C When baking 8~24 is small, cooling, up to calcium zirconium carbon refractory；The baking and the cooling carry out under the conditions of vacuum is 100~1000Pa；The preparation method of the calcium oxide particle is：Into calcium hydroxide powder add account for the calcium hydroxide powder 0.2~ The additive of 2.0wt%, when wet-milling blending 1~5 is small, filtered, drying and grinding, obtain mixed powder；Again by the mixed powder Body is placed in the charging basket of Granulation Equipments, and under conditions of rotating speed is 1000~3000 revs/min, addition accounts for the mixed powder 8 The water of~30wt%, when there is particle formation, is adjusted to 500~1000 revs/min by rotating speed, treats the mixed powder in the charging basket Particle is completely converted into stop；Then the particle is inserted in heating furnace, when insulation 1~5 is small under the conditions of 1400~1800 DEG C； Then nitrogen or argon gas are passed through into stove to room temperature, the flow for being passed through nitrogen or argon gas is 0.5~5 liter/min, up to calcium oxide Particle；The calcium oxide particle：CaO content >=95wt%, bulk density >=2.8g/cm3, particle diameter are 0.2~7mm.
- 2. the preparation method of calcium zirconium carbon refractory according to claim 1, it is characterised in that the calcium oxide fine powder CaO content >=95wt%, the particle diameter of calcium oxide fine powder is 2~200 μm.
- 3. the preparation method of calcium zirconium carbon refractory according to claim 1, it is characterised in that the powdered zirconium oxide ZrO2Content >=95wt%, the particle diameter of powdered zirconium oxide is 1~50 μm.
- 4. the preparation method of calcium zirconium carbon refractory according to claim 1, it is characterised in that the content of C in the graphite >=94wt%, the particle diameter of graphite is 1~200 μm.
- 5. the preparation method of calcium zirconium carbon refractory according to claim 1, it is characterised in that the phenolic resin is liquid One or both of body phenolic resin and solid phenolic resin, Residual carbon >=40% of the phenolic resin.
- 6. the preparation method of calcium zirconium carbon refractory according to claim 1, it is characterised in that the additive is hydrogen-oxygen Change one kind of zirconium powder, Zirconium oxide powder and yttrium oxide powder；The particle diameter of the additive is 1~300 μm.
- 7. a kind of calcium zirconium carbon refractory, it is characterised in that the calcium zirconium carbon refractory is appointed according in claim 1~6 Calcium zirconium carbon refractory prepared by the preparation method of calcium zirconium carbon refractory described in one.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041085A (en) * | 2019-04-08 | 2019-07-23 | 武汉科技大学 | A kind of calcium carbon composite and preparation method thereof |
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| JPH0871715A (en) * | 1994-09-12 | 1996-03-19 | Nippon Steel Corp | Flat nozzle for thin sheet continuous casting |
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| CN106631074A (en) * | 2017-01-05 | 2017-05-10 | 武汉科技大学 | High-calcium-oxide-content calcium oxide material and preparation method thereof |
| CN107056255A (en) * | 2017-01-18 | 2017-08-18 | 武汉科技大学 | A kind of calcium oxide filter and preparation method thereof |
-
2018
- 2018-01-03 CN CN201810005726.2A patent/CN107935611A/en not_active Withdrawn
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| JPH0871715A (en) * | 1994-09-12 | 1996-03-19 | Nippon Steel Corp | Flat nozzle for thin sheet continuous casting |
| CN101096311A (en) * | 2006-06-28 | 2008-01-02 | 宝山钢铁股份有限公司 | Immersion type water gap noumenon material containing calcium oxide |
| CN102910917A (en) * | 2012-10-20 | 2013-02-06 | 江苏苏嘉集团新材料有限公司 | Magnesium-calcium-carbon refractory material |
| CN104829252A (en) * | 2015-04-24 | 2015-08-12 | 沈阳化工大学 | Calcium oxide carbon brick and preparation method thereof |
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| Title |
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| F.NADACHOWSKI: "Refractories based on lime: Development and perspectives", 《CERAMURGIA INTERNATIONAL》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110041085A (en) * | 2019-04-08 | 2019-07-23 | 武汉科技大学 | A kind of calcium carbon composite and preparation method thereof |
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Application publication date: 20180420 |